#------------------------------------------------------------------------------
#$Date: 2015-03-08 06:11:26 +0200 (Sun, 08 Mar 2015) $
#$Revision: 133647 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/00/40/1004000.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_1004000
loop_
_publ_author_name
'Jin, Song'
'Zhou, Ran'
'Scheuer, Ellen M.'
'Adamchuk, Jennifer'
'Rayburn, Lori L.'
'DiSalvo, Francis J.'
_publ_contact_author
; 
Prof. Francis J. DiSalvo 
Department of Chemistry and Chemical Biology 
Cornell University 
Ithaca, NY 14853 
;
_publ_contact_author_email       fjd3@cornell.edu
_publ_contact_author_fax         607-255-4137
_publ_contact_author_phone       607-255-7238
_publ_section_title
;
Synthesis, Characterization, and Ligand Exchange Studies of W~6~S~8~L~6~ 
Cluster Compounds
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2666
_journal_page_last               2674
_journal_paper_doi               10.1021/ic001314q
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'W6 S8 (CH5N)6'
_chemical_formula_sum            'C6 H30 N6 S8 W6'
_chemical_formula_weight         1545.94
_chemical_melting_point          ?
_chemical_name_common            'Tungsten sulfide cluster with'
_chemical_name_systematic
;
octakis(mu!3$-sulfido)-hexakis(methylamine)-hexa-tungsten
;
_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-97
_cell_angle_alpha                103.7320(10)
_cell_angle_beta                 116.6220(10)
_cell_angle_gamma                106.2650(10)
_cell_formula_units_Z            1
_cell_length_a                   9.0847(5)
_cell_length_b                   9.1602(5)
_cell_length_c                   9.5660(5)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     619.10(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       '\w 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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4234
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    28.438
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.074905
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.147
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.921
_refine_diff_density_min         -5.048
_refine_diff_density_rms         0.652
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                1789
_reflns_number_total             1987
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_cif_authors_sg_H-M          P-1
_cod_database_code               1004000
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.97011(6) 0.77966(6) 0.41202(6) 0.0086(2) Uani 1 1 d . . .
W2 W 0.89130(6) 0.98906(6) 0.27547(6) 0.0086(2) Uani 1 1 d . . .
W3 W 0.76642(6) 0.91450(6) 0.46528(6) 0.0085(2) Uani 1 1 d . . .
S5 S 0.7108(4) 1.1175(4) 0.3413(4) 0.0137(7) Uani 1 1 d . . .
S4 S 0.6591(4) 0.7105(4) 0.1837(4) 0.0163(7) Uani 1 1 d . . .
S6 S 1.0930(4) 0.8690(4) 0.2456(4) 0.0127(7) Uani 1 1 d . . .
S7 S 0.8608(4) 0.7279(4) 0.5959(4) 0.0147(7) Uani 1 1 d . . .
N1 N 0.9158(14) 0.5077(13) 0.2976(13) 0.020(2) Uani 1 1 d . . .
H1A H 1.009(10) 0.5026(14) 0.350(6) 0.025 Uiso 1 1 calc R . .
H1B H 0.846(8) 0.454(6) 0.315(2) 0.025 Uiso 1 1 calc R . .
N2 N 0.7514(13) 0.9588(13) -0.0043(12) 0.016(2) Uani 1 1 d . . .
H2A H 0.671(9) 0.981(3) -0.025(3) 0.019 Uiso 1 1 calc R . .
H2B H 0.820(8) 1.022(7) -0.0109(14) 0.019 Uiso 1 1 calc R . .
N3 N 0.4802(13) 0.8050(13) 0.4117(12) 0.016(2) Uani 1 1 d . . .
H3A H 0.4877(14) 0.851(5) 0.503(9) 0.019 Uiso 1 1 calc R . .
H3B H 0.416(7) 0.834(3) 0.339(7) 0.019 Uiso 1 1 calc R . .
C1 C 0.8424(17) 0.4249(16) 0.1118(14) 0.020(3) Uani 1 1 d . . .
H1B H 0.8249 0.3086 0.0814 0.030 Uiso 1 1 calc R . .
H1C H 0.9296 0.4852 0.0880 0.030 Uiso 1 1 calc R . .
H1D H 0.7243 0.4259 0.0432 0.030 Uiso 1 1 calc R . .
C2 C 0.6814(18) 0.7909(19) -0.1366(15) 0.030(4) Uani 1 1 d . . .
H2B H 0.6252 0.7916 -0.2509 0.045 Uiso 1 1 calc R . .
H2C H 0.5892 0.7079 -0.1332 0.045 Uiso 1 1 calc R . .
H2D H 0.7833 0.7618 -0.1137 0.045 Uiso 1 1 calc R . .
C3 C 0.3792(17) 0.6218(17) 0.3483(17) 0.025(3) Uani 1 1 d . . .
H3B H 0.2586 0.5943 0.3317 0.037 Uiso 1 1 calc R . .
H3C H 0.4492 0.5851 0.4329 0.037 Uiso 1 1 calc R . .
H3D H 0.3629 0.5645 0.2382 0.037 Uiso 1 1 calc R . .
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 0.0055(3) 0.0094(4) 0.0077(3) 0.0008(2) 0.0036(2) 0.0016(2)
W2 0.0050(3) 0.0118(4) 0.0062(3) 0.0019(2) 0.0031(2) 0.0021(3)
W3 0.0035(3) 0.0109(4) 0.0083(3) 0.0020(2) 0.0035(2) 0.0013(2)
S5 0.0094(14) 0.0211(17) 0.0149(15) 0.0087(13) 0.0079(12) 0.0091(13)
S4 0.0082(14) 0.0145(17) 0.0105(15) -0.0033(13) 0.0009(12) 0.0000(13)
S6 0.0091(14) 0.0173(16) 0.0113(14) 0.0031(13) 0.0069(12) 0.0055(13)
S7 0.0137(15) 0.0171(17) 0.0167(15) 0.0094(14) 0.0100(13) 0.0063(14)
N1 0.014(5) 0.013(6) 0.021(6) -0.002(5) 0.009(5) 0.000(5)
N2 0.017(5) 0.020(6) 0.014(5) 0.005(5) 0.012(4) 0.006(5)
N3 0.012(5) 0.018(6) 0.016(5) 0.005(4) 0.009(4) 0.006(5)
C1 0.015(6) 0.015(7) 0.010(6) -0.008(5) 0.003(5) 0.001(5)
C2 0.023(7) 0.052(10) 0.007(6) 0.006(6) 0.004(5) 0.020(7)
C3 0.015(6) 0.026(8) 0.030(7) 0.013(6) 0.012(6) 0.004(6)
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
N1 W1 S4 90.2(3) . . ?
N1 W1 S7 92.0(3) . . ?
S4 W1 S7 90.12(10) . . ?
N1 W1 S5 96.4(3) . 2_776 ?
S4 W1 S5 173.40(10) . 2_776 ?
S7 W1 S5 88.96(10) . 2_776 ?
N1 W1 S6 95.0(3) . . ?
S4 W1 S6 90.85(10) . . ?
S7 W1 S6 172.99(10) . . ?
S5 W1 S6 89.28(10) 2_776 . ?
N1 W1 W2 133.4(3) . . ?
S4 W1 W2 57.31(8) . . ?
S7 W1 W2 117.76(6) . . ?
S5 W1 W2 117.65(7) 2_776 . ?
S6 W1 W2 57.45(6) . . ?
N1 W1 W3 131.7(3) . . ?
S4 W1 W3 56.94(7) . . ?
S7 W1 W3 57.71(6) . . ?
S5 W1 W3 117.38(6) 2_776 . ?
S6 W1 W3 117.48(6) . . ?
W2 W1 W3 60.112(18) . . ?
N1 W1 W3 138.3(3) . 2_776 ?
S4 W1 W3 117.44(8) . 2_776 ?
S7 W1 W3 116.78(8) . 2_776 ?
S5 W1 W3 57.49(8) 2_776 2_776 ?
S6 W1 W3 56.81(7) . 2_776 ?
W2 W1 W3 60.187(18) . 2_776 ?
W3 W1 W3 90.02(2) . 2_776 ?
N1 W1 W2 136.4(3) . 2_776 ?
S4 W1 W2 117.01(7) . 2_776 ?
S7 W1 W2 57.15(8) . 2_776 ?
S5 W1 W2 57.29(7) 2_776 2_776 ?
S6 W1 W2 116.43(7) . 2_776 ?
W2 W1 W2 90.02(2) . 2_776 ?
W3 W1 W2 60.111(17) . 2_776 ?
W3 W1 W2 59.641(18) 2_776 2_776 ?
N2 W2 S4 90.4(3) . . ?
N2 W2 S7 96.6(3) . 2_776 ?
S4 W2 S7 172.95(10) . 2_776 ?
N2 W2 S6 91.9(2) . . ?
S4 W2 S6 90.94(10) . . ?
S7 W2 S6 89.43(10) 2_776 . ?
N2 W2 S5 94.6(2) . . ?
S4 W2 S5 89.95(10) . . ?
S7 W2 S5 88.89(10) 2_776 . ?
S6 W2 S5 173.39(9) . . ?
N2 W2 W1 131.6(2) . . ?
S4 W2 W1 57.09(7) . . ?
S7 W2 W1 117.65(7) 2_776 . ?
S6 W2 W1 57.82(7) . . ?
S5 W2 W1 117.67(7) . . ?
N2 W2 W3 133.6(2) . . ?
S4 W2 W3 56.84(7) . . ?
S7 W2 W3 117.00(7) 2_776 . ?
S6 W2 W3 117.75(7) . . ?
S5 W2 W3 57.71(7) . . ?
W1 W2 W3 60.003(18) . . ?
N2 W2 W3 136.2(2) . 2_776 ?
S4 W2 W3 117.29(7) . 2_776 ?
S7 W2 W3 57.43(7) 2_776 2_776 ?
S6 W2 W3 56.95(7) . 2_776 ?
S5 W2 W3 117.01(7) . 2_776 ?
W1 W2 W3 60.262(19) . 2_776 ?
W3 W2 W3 90.00(2) . 2_776 ?
N2 W2 W1 138.4(2) . 2_776 ?
S4 W2 W1 116.92(7) . 2_776 ?
S7 W2 W1 56.89(7) 2_776 2_776 ?
S6 W2 W1 116.52(7) . 2_776 ?
S5 W2 W1 57.44(7) . 2_776 ?
W1 W2 W1 89.98(2) . 2_776 ?
W3 W2 W1 60.125(19) . 2_776 ?
W3 W2 W1 59.594(17) 2_776 2_776 ?
N3 W3 S4 90.8(3) . . ?
N3 W3 S6 95.3(3) . 2_776 ?
S4 W3 S6 173.96(10) . 2_776 ?
N3 W3 S7 94.3(3) . . ?
S4 W3 S7 89.84(10) . . ?
S6 W3 S7 89.51(10) 2_776 . ?
N3 W3 S5 92.9(3) . . ?
S4 W3 S5 90.09(10) . . ?
S6 W3 S5 89.81(10) 2_776 . ?
S7 W3 S5 172.82(10) . . ?
N3 W3 W1 133.4(2) . . ?
S4 W3 W1 57.18(7) . . ?
S6 W3 W1 117.76(6) 2_776 . ?
S7 W3 W1 57.04(7) . . ?
S5 W3 W1 117.32(6) . . ?
N3 W3 W2 132.9(3) . . ?
S4 W3 W2 57.30(8) . . ?
S6 W3 W2 117.92(8) 2_776 . ?
S7 W3 W2 116.86(7) . . ?
S5 W3 W2 57.48(7) . . ?
W1 W3 W2 59.885(18) . . ?
N3 W3 W2 137.1(3) . 2_776 ?
S4 W3 W2 117.44(6) . 2_776 ?
S6 W3 W2 57.48(6) 2_776 2_776 ?
S7 W3 W2 57.03(8) . 2_776 ?
S5 W3 W2 116.93(7) . 2_776 ?
W1 W3 W2 60.296(17) . 2_776 ?
W2 W3 W2 90.00(2) . 2_776 ?
N3 W3 W1 136.5(2) . 2_776 ?
S4 W3 W1 117.49(8) . 2_776 ?
S6 W3 W1 57.71(8) 2_776 2_776 ?
S7 W3 W1 116.53(8) . 2_776 ?
S5 W3 W1 57.41(7) . 2_776 ?
W1 W3 W1 89.98(2) . 2_776 ?
W2 W3 W1 60.235(19) . 2_776 ?
W2 W3 W1 59.553(18) 2_776 2_776 ?
W2 S5 W1 65.28(7) . 2_776 ?
W2 S5 W3 64.80(7) . . ?
W1 S5 W3 65.10(7) 2_776 . ?
W3 S4 W1 65.88(7) . . ?
W3 S4 W2 65.87(8) . . ?
W1 S4 W2 65.60(8) . . ?
W3 S6 W2 65.57(7) 2_776 . ?
W3 S6 W1 65.48(7) 2_776 . ?
W2 S6 W1 64.73(7) . . ?
W1 S7 W2 65.95(8) . 2_776 ?
W1 S7 W3 65.26(8) . . ?
W2 S7 W3 65.54(8) 2_776 . ?
C1 N1 W1 118.9(8) . . ?
C2 N2 W2 116.0(8) . . ?
C3 N3 W3 119.2(7) . . ?
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
W1 N1 2.276(10) . ?
W1 S4 2.442(3) . ?
W1 S7 2.450(3) . ?
W1 S5 2.479(3) 2_776 ?
W1 S6 2.479(3) . ?
W1 W2 2.6493(7) . ?
W1 W3 2.6525(6) . ?
W1 W3 2.6684(7) 2_776 ?
W1 W2 2.6714(7) 2_776 ?
W2 N2 2.293(9) . ?
W2 S4 2.449(3) . ?
W2 S7 2.458(3) 2_776 ?
W2 S6 2.469(2) . ?
W2 S5 2.474(3) . ?
W2 W3 2.6554(7) . ?
W2 W3 2.6664(7) 2_776 ?
W2 W1 2.6714(7) 2_776 ?
W3 N3 2.265(10) . ?
W3 S4 2.436(3) . ?
W3 S6 2.455(3) 2_776 ?
W3 S7 2.469(3) . ?
W3 S5 2.481(3) . ?
W3 W2 2.6664(7) 2_776 ?
W3 W1 2.6684(7) 2_776 ?
S5 W1 2.479(3) 2_776 ?
S6 W3 2.455(3) 2_776 ?
S7 W2 2.458(3) 2_776 ?
N1 C1 1.481(15) . ?
N2 C2 1.476(16) . ?
N3 C3 1.477(17) . ?