#------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/01/4000187.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_4000187
_journal_name_full               'Chemistry of Materials'
_journal_year                    2002
_chemical_formula_moiety         '(Et4N)5 W6 S8 (CN)6'
_chemical_formula_sum            'C46 H100 N11 S8 W6'
_chemical_formula_weight         2166.95
_chemical_name_common            'Tungsten sulfide cluster with cyanide'
_chemical_name_systematic
;
octakis(mu!3$-sulfido)-hexakis(cyano)
-hexa-tungsten pentakis(tetraethalammonium) salt
;
_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
_cell_angle_alpha                97.934(7)
_cell_angle_beta                 105.571(6)
_cell_angle_gamma                114.065(6)
_cell_formula_units_Z            1
_cell_length_a                   12.056(3)
_cell_length_b                   12.236(3)
_cell_length_c                   12.574(4)
_cell_measurement_temperature    173(2)
_cell_volume                     1565.6(8)
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Bruker SMART CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17046
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    11.284
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.710514
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.298
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1025
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.067
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6385
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_obs          0.0321
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0296P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0658
_refine_ls_wR_factor_obs         0.0624
_reflns_number_observed          5310
_reflns_number_total             6385
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0296P)^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^)+(0.0296P)^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               4000187
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
W1 W 0.52367(3) 0.14057(2) 0.10976(2) 0.01716(7) Uani 1 d . .
W2 W 0.39524(2) -0.10936(2) 0.06653(2) 0.01705(7) Uani 1 d . .
W3 W 0.65142(2) 0.00522(2) 0.10414(2) 0.01775(7) Uani 1 d . .
S4 S 0.5598(2) 0.02977(15) 0.25296(12) 0.0232(4) Uani 1 d . .
S5 S 0.2891(2) 0.02657(15) 0.06690(13) 0.0234(4) Uani 1 d . .
S6 S 0.4761(2) 0.22145(15) -0.05657(13) 0.0241(4) Uani 1 d . .
S7 S 0.7529(2) 0.22972(15) 0.12918(13) 0.0244(4) Uani 1 d . .
C1 C 0.5577(6) 0.3013(6) 0.2427(5) 0.0237(15) Uani 1 d . .
N1 N 0.5796(6) 0.3837(5) 0.3153(4) 0.0322(14) Uani 1 d . .
C2 C 0.2684(6) -0.2438(6) 0.1340(5) 0.0216(14) Uani 1 d . .
N2 N 0.1977(6) -0.3180(5) 0.1636(5) 0.0300(13) Uani 1 d . .
C3 C 0.8277(7) 0.0258(6) 0.2324(5) 0.027(2) Uani 1 d . .
N3 N 0.9243(6) 0.0458(6) 0.3045(5) 0.038(2) Uani 1 d . .
N4 N 0.1692(5) 0.3275(5) -0.0057(4) 0.0223(12) Uani 1 d . .
C41 C 0.0738(7) 0.3004(7) 0.0571(6) 0.043(2) Uani 1 d . .
H41A H 0.1067(7) 0.3744(7) 0.1225(6) 0.051 Uiso 1 calc R .
H41B H -0.0105(7) 0.2877(7) 0.0041(6) 0.051 Uiso 1 calc R .
C42 C 0.0508(9) 0.1882(9) 0.1020(7) 0.064(3) Uani 1 d . .
H42A H -0.0116(9) 0.1770(9) 0.1412(7) 0.096 Uiso 1 calc R .
H42B H 0.1332(9) 0.2007(9) 0.1563(7) 0.096 Uiso 1 calc R .
H42C H 0.0158(9) 0.1138(9) 0.0377(7) 0.096 Uiso 1 calc R .
C43 C 0.1657(8) 0.4312(6) -0.0567(6) 0.036(2) Uani 1 d . .
H43A H 0.1923(8) 0.5053(6) 0.0062(6) 0.044 Uiso 1 calc R .
H43B H 0.0751(8) 0.4046(6) -0.1070(6) 0.044 Uiso 1 calc R .
C44 C 0.2537(9) 0.4676(7) -0.1264(7) 0.051(2) Uani 1 d . .
H44A H 0.2472(9) 0.5350(7) -0.1572(7) 0.076 Uiso 1 calc R .
H44B H 0.2266(9) 0.3952(7) -0.1901(7) 0.076 Uiso 1 calc R .
H44C H 0.3439(9) 0.4960(7) -0.0768(7) 0.076 Uiso 1 calc R .
C45 C 0.1292(6) 0.2109(6) -0.0989(5) 0.0251(15) Uani 1 d . .
H45A H 0.1929(6) 0.2303(6) -0.1383(5) 0.030 Uiso 1 calc R .
H45B H 0.1330(6) 0.1454(6) -0.0620(5) 0.030 Uiso 1 calc R .
C46 C -0.0054(7) 0.1599(7) -0.1877(6) 0.039(2) Uani 1 d . .
H66A H -0.0241(7) 0.0853(7) -0.2446(6) 0.058 Uiso 1 calc R .
H66B H -0.0096(7) 0.2232(7) -0.2264(6) 0.058 Uiso 1 calc R .
H66C H -0.0696(7) 0.1382(7) -0.1500(6) 0.058 Uiso 1 calc R .
C47 C 0.3047(6) 0.3638(6) 0.0750(5) 0.0252(15) Uani 1 d . .
H47A H 0.3598(6) 0.3668(6) 0.0285(5) 0.030 Uiso 1 calc R .
H47B H 0.2997(6) 0.2974(6) 0.1133(5) 0.030 Uiso 1 calc R .
C48 C 0.3714(7) 0.4872(6) 0.1670(5) 0.030(2) Uani 1 d . .
H48A H 0.4580(7) 0.5020(6) 0.2144(5) 0.045 Uiso 1 calc R .
H48B H 0.3196(7) 0.4849(6) 0.2156(5) 0.045 Uiso 1 calc R .
H48C H 0.3799(7) 0.5545(6) 0.1306(5) 0.045 Uiso 1 calc R .
N5 N 0.6389(5) -0.2030(5) 0.4990(4) 0.0245(12) Uani 1 d . .
C51 C 0.7546(7) -0.1479(6) 0.4621(6) 0.035(2) Uani 1 d . .
H51A H 0.8345(7) -0.1254(6) 0.5278(6) 0.042 Uiso 1 calc R .
H51B H 0.7610(7) -0.0700(6) 0.4435(6) 0.042 Uiso 1 calc R .
C52 C 0.7498(8) -0.2338(7) 0.3580(6) 0.047(2) Uani 1 d . .
H52A H 0.8280(8) -0.1912(7) 0.3399(6) 0.071 Uiso 1 calc R .
H52B H 0.6724(8) -0.2548(7) 0.2917(6) 0.071 Uiso 1 calc R .
H52C H 0.7460(8) -0.3104(7) 0.3760(6) 0.071 Uiso 1 calc R .
C53 C 0.6105(7) -0.3314(6) 0.5116(5) 0.029(2) Uani 1 d . .
H53A H 0.5888(7) -0.3867(6) 0.4357(5) 0.035 Uiso 1 calc R .
H53B H 0.5325(7) -0.3642(6) 0.5333(5) 0.035 Uiso 1 calc R .
C54 C 0.7196(8) -0.3387(7) 0.5990(7) 0.045(2) Uani 1 d . .
H54A H 0.6922(8) -0.4254(7) 0.6010(7) 0.067 Uiso 1 calc R .
H54B H 0.7404(8) -0.2865(7) 0.6752(7) 0.067 Uiso 1 calc R .
H54C H 0.7968(8) -0.3090(7) 0.5774(7) 0.067 Uiso 1 calc R .
C55 C 0.6676(7) -0.1180(6) 0.6140(5) 0.028(2) Uani 1 d . .
H55A H 0.5962(7) -0.1588(6) 0.6424(5) 0.033 Uiso 1 calc R .
H55B H 0.7488(7) -0.1081(6) 0.6702(5) 0.033 Uiso 1 calc R .
C56 C 0.6822(7) 0.0097(6) 0.6095(6) 0.037(2) Uani 1 d . .
H56A H 0.7005(7) 0.0588(6) 0.6863(6) 0.055 Uiso 1 calc R .
H56B H 0.6014(7) 0.0012(6) 0.5557(6) 0.055 Uiso 1 calc R .
H56C H 0.7542(7) 0.0520(6) 0.5835(6) 0.055 Uiso 1 calc R .
C57 C 0.5190(7) -0.2136(6) 0.4085(5) 0.029(2) Uani 1 d . .
H57A H 0.5410(7) -0.1320(6) 0.3921(5) 0.035 Uiso 1 calc R .
H57B H 0.4974(7) -0.2753(6) 0.3366(5) 0.035 Uiso 1 calc R .
C58 C 0.4015(7) -0.2510(7) 0.4408(6) 0.038(2) Uani 1 d . .
H58A H 0.3296(7) -0.2554(7) 0.3780(6) 0.058 Uiso 1 calc R .
H58B H 0.4206(7) -0.1893(7) 0.5106(6) 0.058 Uiso 1 calc R .
H58C H 0.3769(7) -0.3329(7) 0.4551(6) 0.058 Uiso 1 calc R .
N6 N 0.0000 -0.5000 0.5000 0.030(2) Uiso 1 d SD .
C61 C -0.0533(13) -0.5185(13) 0.3725(9) 0.028(3) Uiso 0.50 d PD 1
H61A H -0.0800(13) -0.4537(13) 0.3583(9) 0.034 Uiso 0.50 calc PR 1
H61B H -0.1315(13) -0.6009(13) 0.3362(9) 0.034 Uiso 0.50 calc PR 1
C62 C 0.0507(21) -0.5112(19) 0.3153(16) 0.033(5) Uiso 0.50 d PD 1
H62A H 0.0129(21) -0.5236(19) 0.2325(16) 0.050 Uiso 0.50 calc PR 1
H62B H 0.0761(21) -0.5763(19) 0.3280(16) 0.050 Uiso 0.50 calc PR 1
H62C H 0.1276(21) -0.4292(19) 0.3500(16) 0.050 Uiso 0.50 calc PR 1
C63 C 0.0293(16) -0.6030(14) 0.5304(15) 0.060(5) Uiso 0.50 d PD 2
H63A H 0.0658(16) -0.5873(14) 0.6148(15) 0.072 Uiso 0.50 calc PR 2
H63B H 0.0904(16) -0.6134(14) 0.4959(15) 0.072 Uiso 0.50 calc PR 2
C64 C -0.1244(18) -0.7317(16) 0.4698(18) 0.058(6) Uiso 0.50 d PD 2
H64A H -0.1183(18) -0.8062(16) 0.4840(18) 0.087 Uiso 0.50 calc PR 2
H64B H -0.1586(18) -0.7436(16) 0.3868(18) 0.087 Uiso 0.50 calc PR 2
H64C H -0.1829(18) -0.7178(16) 0.5046(18) 0.087 Uiso 0.50 calc PR 2
C65 C -0.1234(16) -0.6254(14) 0.4431(16) 0.069(6) Uiso 0.50 d PD 3
H65A H -0.1522(16) -0.6454(14) 0.3582(16) 0.083 Uiso 0.50 calc PR 3
H65B H -0.1950(16) -0.6254(14) 0.4674(16) 0.083 Uiso 0.50 calc PR 3
C66 C -0.0756(22) -0.7279(18) 0.4914(20) 0.065(7) Uiso 0.50 d PD 3
H64D H -0.1490(22) -0.8123(18) 0.4593(20) 0.098 Uiso 0.50 calc PR 3
H64E H -0.0464(22) -0.7054(18) 0.5756(20) 0.098 Uiso 0.50 calc PR 3
H64F H -0.0040(22) -0.7252(18) 0.4672(20) 0.098 Uiso 0.50 calc PR 3
C67 C 0.1050(13) -0.5049(14) 0.4609(11) 0.036(3) Uiso 0.50 d PD 4
H67A H 0.1200(13) -0.5744(14) 0.4808(11) 0.043 Uiso 0.50 calc PR 4
H67B H 0.1868(13) -0.4263(14) 0.5025(11) 0.043 Uiso 0.50 calc PR 4
C68 C 0.0700(24) -0.5236(21) 0.3262(16) 0.045(7) Uiso 0.50 d PD 4
H62D H 0.1415(24) -0.5262(21) 0.3048(16) 0.068 Uiso 0.50 calc PR 4
H62E H 0.0568(24) -0.4541(21) 0.3062(16) 0.068 Uiso 0.50 calc PR 4
H62F H -0.0098(24) -0.6021(21) 0.2846(16) 0.068 Uiso 0.50 calc PR 4
