#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:03:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179360 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/57/4325781.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_4325781
loop_
_publ_author_name
'Stephen Sproules'
'Priyabrata Banerjee'
'Thomas Weyhermüller'
'Yong Yan'
'James P. Donahue'
'Karl Wieghardt'
_publ_section_title
;
 Monoanionic Molybdenum and Tungsten Tris(dithiolene) Complexes: A
 Multifrequency EPR Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7106
_journal_page_last               7122
_journal_paper_doi               10.1021/ic2006265
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C12 N6 S6 W, 2(C24 H20 P)'
_chemical_formula_sum            'C60 H40 N6 P2 S6 W'
_chemical_formula_weight         1283.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9080(3)
_cell_length_b                   15.1931(3)
_cell_length_c                   18.3256(3)
_cell_measurement_temperature    100(2)
_cell_volume                     5542.84(16)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method
'1522 images at 0.5 deg. stepwise rotation in omega and phi, 30 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            127250
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.414
_exptl_absorpt_correction_T_max  0.8687
_exptl_absorpt_correction_T_min  0.5726
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.084
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         12210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0284P)²+5.6302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0715
_reflns_number_gt                9432
_reflns_number_total             12210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2006265_si_002_6.cif
_cod_data_source_block           6
_cod_database_code               4325781
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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
W1 W 0.0000 0.170945(6) 0.2500 0.01755(3) Uani 1 2 d S
S1 S 0.04911(2) 0.20314(3) 0.36600(2) 0.02150(8) Uani 1 1 d .
C1 C 0.11643(9) 0.27357(11) 0.35138(10) 0.0204(3) Uani 1 1 d .
S2 S 0.09005(2) 0.26096(3) 0.20706(2) 0.02097(8) Uani 1 1 d .
C2 C 0.13329(9) 0.30013(11) 0.28279(10) 0.0210(3) Uani 1 1 d .
C3 C 0.18973(10) 0.35683(13) 0.27070(12) 0.0260(4) Uani 1 1 d .
N4 N 0.23506(11) 0.40312(14) 0.26134(11) 0.0367(4) Uani 1 1 d .
C5 C 0.15309(9) 0.30177(12) 0.41448(11) 0.0238(3) Uani 1 1 d .
N6 N 0.18181(10) 0.32238(12) 0.46612(11) 0.0324(4) Uani 1 1 d .
S11 S 0.04924(2) 0.05348(3) 0.18341(3) 0.02216(8) Uani 1 1 d .
C11 C 0.02147(10) -0.04535(12) 0.22099(11) 0.0245(3) Uani 1 1 d .
C12 C 0.04405(11) -0.12553(14) 0.18771(12) 0.0315(4) Uani 1 1 d .
N13 N 0.06269(12) -0.18865(14) 0.15984(13) 0.0447(5) Uani 1 1 d .
P20 P 0.13249(2) 0.66381(3) 0.40612(3) 0.01824(8) Uani 1 1 d .
C21 C 0.18340(9) 0.62557(12) 0.48063(10) 0.0202(3) Uani 1 1 d .
C22 C 0.21272(11) 0.68350(13) 0.53052(11) 0.0275(4) Uani 1 1 d .
H22 H 0.2023 0.7445 0.5291 0.033 Uiso 1 1 calc R
C23 C 0.25725(13) 0.65105(15) 0.58215(13) 0.0365(5) Uani 1 1 d .
H23 H 0.2770 0.6902 0.6164 0.044 Uiso 1 1 calc R
C24 C 0.27327(12) 0.56254(14) 0.58445(12) 0.0328(4) Uani 1 1 d .
H24 H 0.3040 0.5412 0.6200 0.039 Uiso 1 1 calc R
C25 C 0.24438(10) 0.50480(13) 0.53465(11) 0.0274(4) Uani 1 1 d .
H25 H 0.2556 0.4440 0.5360 0.033 Uiso 1 1 calc R
C26 C 0.19929(9) 0.53569(12) 0.48316(10) 0.0229(3) Uani 1 1 d .
H26 H 0.1791 0.4961 0.4496 0.028 Uiso 1 1 calc R
C31 C 0.11464(9) 0.77897(11) 0.41798(10) 0.0209(3) Uani 1 1 d .
C32 C 0.08086(10) 0.80935(13) 0.48030(11) 0.0264(4) Uani 1 1 d .
H32 H 0.0663 0.7690 0.5166 0.032 Uiso 1 1 calc R
C33 C 0.06884(11) 0.89906(13) 0.48854(12) 0.0288(4) Uani 1 1 d .
H33 H 0.0449 0.9197 0.5300 0.035 Uiso 1 1 calc R
C34 C 0.09147(10) 0.95846(13) 0.43670(12) 0.0289(4) Uani 1 1 d .
H34 H 0.0835 1.0196 0.4430 0.035 Uiso 1 1 calc R
C35 C 0.12575(10) 0.92874(13) 0.37575(11) 0.0270(4) Uani 1 1 d .
H35 H 0.1415 0.9697 0.3406 0.032 Uiso 1 1 calc R
C36 C 0.13726(10) 0.83908(12) 0.36570(11) 0.0231(3) Uani 1 1 d .
H36 H 0.1604 0.8189 0.3235 0.028 Uiso 1 1 calc R
C41 C 0.17965(9) 0.64852(12) 0.32381(10) 0.0194(3) Uani 1 1 d .
C42 C 0.14794(10) 0.66044(13) 0.25609(10) 0.0254(4) Uani 1 1 d .
H42 H 0.1013 0.6736 0.2538 0.030 Uiso 1 1 calc R
C43 C 0.18537(11) 0.65273(14) 0.19248(11) 0.0285(4) Uani 1 1 d .
H43 H 0.1645 0.6614 0.1464 0.034 Uiso 1 1 calc R
C44 C 0.25331(11) 0.63241(13) 0.19612(11) 0.0280(4) Uani 1 1 d .
H44 H 0.2788 0.6279 0.1524 0.034 Uiso 1 1 calc R
C45 C 0.28433(10) 0.61862(12) 0.26275(11) 0.0252(4) Uani 1 1 d .
H45 H 0.3305 0.6031 0.2644 0.030 Uiso 1 1 calc R
C46 C 0.24820(9) 0.62747(11) 0.32708(10) 0.0209(3) Uani 1 1 d .
H46 H 0.2697 0.6194 0.3729 0.025 Uiso 1 1 calc R
C51 C 0.05763(8) 0.59726(11) 0.39847(10) 0.0199(3) Uani 1 1 d .
C52 C -0.00227(9) 0.62105(13) 0.43312(11) 0.0242(3) Uani 1 1 d .
H52 H -0.0053 0.6751 0.4589 0.029 Uiso 1 1 calc R
C53 C -0.05749(9) 0.56495(14) 0.42955(12) 0.0269(4) Uani 1 1 d .
H53 H -0.0981 0.5806 0.4535 0.032 Uiso 1 1 calc R
C54 C -0.05363(9) 0.48622(13) 0.39114(11) 0.0266(4) Uani 1 1 d .
H54 H -0.0915 0.4483 0.3890 0.032 Uiso 1 1 calc R
C55 C 0.00571(9) 0.46288(13) 0.35586(12) 0.0262(4) Uani 1 1 d .
H55 H 0.0082 0.4093 0.3292 0.031 Uiso 1 1 calc R
C56 C 0.06160(9) 0.51832(12) 0.35964(11) 0.0238(3) Uani 1 1 d .
H56 H 0.1022 0.5024 0.3359 0.029 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'
P P 0.1023 0.0942 '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
S11 W1 S11 82.50(2) . 3
S11 W1 S2 155.492(15) . 3
S11 W1 S2 87.200(16) 3 3
S11 W1 S2 87.200(16) . .
S11 W1 S2 155.492(15) 3 .
S2 W1 S2 110.13(2) 3 .
S11 W1 S1 116.237(16) . .
S11 W1 S1 82.276(15) 3 .
S2 W1 S1 84.076(15) 3 .
S2 W1 S1 82.463(15) . .
S11 W1 S1 82.276(15) . 3
S11 W1 S1 116.238(16) 3 3
S2 W1 S1 82.464(15) 3 3
S2 W1 S1 84.075(16) . 3
S1 W1 S1 156.38(2) . 3
C1 S1 W1 107.74(6) . .
C2 C1 C5 122.03(17) . .
C2 C1 S1 121.02(14) . .
C5 C1 S1 116.94(14) . .
C2 S2 W1 107.75(6) . .
C1 C2 C3 120.93(17) . .
C1 C2 S2 120.87(14) . .
C3 C2 S2 118.08(15) . .
N4 C3 C2 179.4(3) . .
N6 C5 C1 178.1(2) . .
C11 S11 W1 108.29(7) . .
C11 C11 C12 121.85(13) 3 .
C11 C11 S11 120.46(7) 3 .
C12 C11 S11 117.67(16) . .
N13 C12 C11 178.5(3) . .
C41 P20 C21 107.59(8) . .
C41 P20 C31 109.35(8) . .
C21 P20 C31 109.52(9) . .
C41 P20 C51 107.12(8) . .
C21 P20 C51 110.08(8) . .
C31 P20 C51 113.01(8) . .
C22 C21 C26 119.84(17) . .
C22 C21 P20 121.96(14) . .
C26 C21 P20 117.84(14) . .
C23 C22 C21 119.32(18) . .
C24 C23 C22 120.9(2) . .
C23 C24 C25 119.9(2) . .
C26 C25 C24 120.11(19) . .
C25 C26 C21 119.92(17) . .
C36 C31 C32 119.82(17) . .
C36 C31 P20 119.27(14) . .
C32 C31 P20 120.86(14) . .
C33 C32 C31 119.52(18) . .
C34 C33 C32 120.49(19) . .
C35 C34 C33 120.06(18) . .
C34 C35 C36 120.42(19) . .
C35 C36 C31 119.66(18) . .
C46 C41 C42 120.30(17) . .
C46 C41 P20 120.21(14) . .
C42 C41 P20 119.45(14) . .
C43 C42 C41 119.33(19) . .
C42 C43 C44 120.07(19) . .
C45 C44 C43 120.69(18) . .
C44 C45 C46 120.23(19) . .
C45 C46 C41 119.34(18) . .
C56 C51 C52 120.10(16) . .
C56 C51 P20 118.26(13) . .
C52 C51 P20 121.57(14) . .
C53 C52 C51 119.58(18) . .
C54 C53 C52 120.45(18) . .
C53 C54 C55 120.08(17) . .
C54 C55 C56 119.93(18) . .
C51 C56 C55 119.85(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 S11 2.3738(5) .
W1 S11 2.3738(5) 3
W1 S2 2.3881(4) 3
W1 S2 2.3882(4) .
W1 S1 2.3903(4) .
W1 S1 2.3904(4) 3
S1 C1 1.7357(18) .
C1 C2 1.362(3) .
C1 C5 1.433(3) .
S2 C2 1.7382(19) .
C2 C3 1.433(3) .
C3 N4 1.157(3) .
C5 N6 1.149(3) .
S11 C11 1.742(2) .
C11 C11 1.364(4) 3
C11 C12 1.434(3) .
C12 N13 1.148(3) .
P20 C41 1.7919(18) .
P20 C21 1.7969(18) .
P20 C31 1.7986(18) .
P20 C51 1.8064(17) .
C21 C22 1.397(3) .
C21 C26 1.402(3) .
C22 C23 1.387(3) .
C23 C24 1.383(3) .
C24 C25 1.390(3) .
C25 C26 1.384(3) .
C31 C36 1.398(3) .
C31 C32 1.403(3) .
C32 C33 1.392(3) .
C33 C34 1.386(3) .
C34 C35 1.385(3) .
C35 C36 1.394(3) .
C41 C46 1.403(2) .
C41 C42 1.404(3) .
C42 C43 1.388(3) .
C43 C44 1.389(3) .
C44 C45 1.384(3) .
C45 C46 1.388(3) .
C51 C56 1.397(3) .
C51 C52 1.399(2) .
C52 C53 1.393(3) .
C53 C54 1.390(3) .
C54 C55 1.393(3) .
C55 C56 1.397(3) .
