#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/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 W₆S₈L₆ 
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       '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  0.0331
_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/[σ²(Fo²)+(0.0900P)²+0.0000P] where P=(Fo²+2Fc²)/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_original_sg_symbol_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_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) . ?
