data_4000187
_journal_name_full 'Chemistry of Materials'
_journal_year    2002
_chemical_name_systematic
;
octakis(mu!3$-sulfido)-hexakis(cyano)
-hexa-tungsten pentakis(tetraethalammonium) salt
;
_chemical_name_common             'Tungsten sulfide cluster with cyanide'
_chemical_formula_moiety          '(Et4N)5 W6 S8 (CN)6'
_chemical_formula_sum             'C46 H100 N11 S8 W6'
_chemical_formula_weight          2166.95
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P -1'
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
_cell_length_a                    12.056(3)
_cell_length_b                    12.236(3)
_cell_length_c                    12.574(4)
_cell_angle_alpha                 97.934(7)
_cell_angle_beta                  105.571(6)
_cell_angle_gamma                 114.065(6)
_cell_volume                      1565.6(8)
_cell_formula_units_Z             1
_cell_measurement_temperature     173(2)
_exptl_crystal_description        block
_exptl_crystal_colour             green
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       'NOT MEASURED'
_exptl_crystal_density_diffrn     2.298
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1025
_exptl_absorpt_coefficient_mu     11.284
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.710514
_exptl_absorpt_correction_T_max   1
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        'Bruker SMART CCD'
_diffrn_measurement_method        '\w scans'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             17046
_diffrn_reflns_av_R_equivalents   0.0328
_diffrn_reflns_av_sigmaI/netI     0.0421
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          2.54
_diffrn_reflns_theta_max          26.49
_reflns_number_total              6385
_reflns_number_observed           5310
_reflns_observed_criterion        >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     noref
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          6385
_refine_ls_number_parameters      313
_refine_ls_number_restraints      18
_refine_ls_R_factor_all           0.0451
_refine_ls_R_factor_obs           0.0321
_refine_ls_wR_factor_all          0.0658
_refine_ls_wR_factor_obs          0.0624
_refine_ls_goodness_of_fit_all    1.067
_refine_ls_goodness_of_fit_obs    1.115
_refine_ls_restrained_S_all       1.072
_refine_ls_restrained_S_obs       1.120
_refine_ls_shift/esd_max          -0.001
_refine_ls_shift/esd_mean         0.000
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
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
W1 0.02215(15) 0.01631(13) 0.01348(12) 0.00428(9) 0.00752(10) 0.00864(12)
W2 0.02115(15) 0.01693(13) 0.01317(12) 0.00505(9) 0.00765(10) 0.00779(12)
W3 0.02050(15) 0.01865(14) 0.01424(12) 0.00527(10) 0.00648(10) 0.00891(12)
S4 0.0311(10) 0.0257(9) 0.0130(7) 0.0060(6) 0.0084(7) 0.0130(8)
S5 0.0236(9) 0.0270(9) 0.0238(8) 0.0075(7) 0.0124(7) 0.0130(8)
S6 0.0310(10) 0.0214(9) 0.0230(8) 0.0092(7) 0.0104(7) 0.0137(8)
S7 0.0232(9) 0.0197(8) 0.0189(8) -0.0006(6) 0.0033(7) 0.0040(8)
C1 0.028(4) 0.024(4) 0.020(3) 0.010(3) 0.007(3) 0.013(3)
N1 0.044(4) 0.030(3) 0.022(3) 0.001(3) 0.010(3) 0.019(3)
C2 0.028(4) 0.024(4) 0.013(3) 0.005(3) 0.007(3) 0.013(3)
N2 0.038(4) 0.025(3) 0.030(3) 0.016(3) 0.022(3) 0.009(3)
C3 0.029(4) 0.028(4) 0.022(3) 0.001(3) 0.012(3) 0.013(3)
N3 0.033(4) 0.051(4) 0.031(3) 0.009(3) 0.003(3) 0.027(4)
N4 0.021(3) 0.024(3) 0.018(3) 0.000(2) 0.005(2) 0.011(3)
C41 0.031(5) 0.059(5) 0.028(4) -0.006(4) 0.016(3) 0.014(4)
C42 0.049(6) 0.076(7) 0.042(5) 0.025(5) 0.020(5) 0.001(5)
C43 0.048(5) 0.025(4) 0.032(4) 0.001(3) 0.001(4) 0.025(4)
C44 0.078(7) 0.026(4) 0.042(5) 0.016(4) 0.016(5) 0.020(5)
C45 0.027(4) 0.021(3) 0.022(3) 0.000(3) 0.010(3) 0.008(3)
C46 0.036(5) 0.041(5) 0.028(4) -0.008(3) 0.006(3) 0.017(4)
C47 0.020(4) 0.027(4) 0.023(3) 0.005(3) 0.006(3) 0.007(3)
C48 0.029(4) 0.025(4) 0.029(4) 0.007(3) 0.007(3) 0.010(3)
N5 0.032(3) 0.020(3) 0.019(3) 0.005(2) 0.010(2) 0.009(3)
C51 0.037(5) 0.033(4) 0.038(4) 0.015(3) 0.021(4) 0.015(4)
C52 0.071(6) 0.046(5) 0.046(5) 0.018(4) 0.043(5) 0.031(5)
C53 0.037(4) 0.022(4) 0.031(4) 0.011(3) 0.016(3) 0.013(4)
C54 0.048(5) 0.036(5) 0.057(5) 0.019(4) 0.018(4) 0.026(4)
C55 0.032(4) 0.031(4) 0.017(3) -0.002(3) 0.007(3) 0.015(4)
C56 0.038(5) 0.027(4) 0.039(4) -0.001(3) 0.013(4) 0.014(4)
C57 0.040(5) 0.024(4) 0.017(3) 0.006(3) 0.003(3) 0.012(4)
C58 0.029(4) 0.034(4) 0.035(4) 0.012(3) -0.005(3) 0.008(4)