#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:57:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179271 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/91/4319151.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_4319151
loop_
_publ_author_name
'Benoît Domercq'
'Claude Coulon'
'Marc Fourmigué'
_publ_section_title
;
 A Density Functional Study of the Highly Adaptable Molecular Structure of
 Mo(V) and W(V) Dithiolene Complexes: From Three-Dimensional
 Antiferromagnet to Spin Ladder
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              371
_journal_page_last               378
_journal_paper_doi               10.1021/ic000550y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C13 H10 As F6 S5 W'
_chemical_formula_weight         699.28
_chemical_name_common            Cp2W(dmit)AsF6
_chemical_name_systematic
; 
 Bis(cyclopentadienyl)(1,3-dithiole-2-thione-4,5-dithiolato)tungsten(V)
 hexafluoroarsenate
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                   9.0293(18)
_cell_length_b                   20.568(4)
_cell_length_c                   10.264(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.0
_cell_volume                     1906.2(6)
_computing_cell_refinement       'SELECT, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'area detector'
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9180
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    8.382
_exptl_absorpt_correction_T_max  0.7268
_exptl_absorpt_correction_T_min  0.3192
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.3466
_exptl_crystal_size_mid          0.1156
_exptl_crystal_size_min          0.0384
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0181P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0375
_reflns_number_gt                943
_reflns_number_total             1040
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000550y_3.cif
_cod_data_source_block           wdmas
_cod_original_cell_volume        1906.2(7)
_cod_database_code               4319151
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.0000 0.177551(13) 0.7500 0.03576(10) Uani 1 4 d S . .
S1 S 0.0000 0.26542(7) 0.59185(14) 0.0679(5) Uani 1 2 d S . .
S2 S 0.0000 0.40972(6) 0.60875(13) 0.0501(3) Uani 1 2 d S . .
S3 S 0.0000 0.53535(10) 0.7500 0.0655(6) Uani 1 4 d S . .
C1 C 0.0000 0.3341(2) 0.6826(5) 0.0397(11) Uani 1 2 d S . .
C2 C 0.0000 0.4554(4) 0.7500 0.0486(19) Uani 1 4 d S . .
C3 C 0.2503(7) 0.1915(4) 0.7500 0.095(3) Uani 1 2 d S . .
H3 H 0.2890 0.2334 0.7500 0.114 Uiso 1 2 calc SR . .
C4 C 0.2144(5) 0.1525(3) 0.6403(5) 0.0824(15) Uani 1 1 d . . .
H4 H 0.2250 0.1643 0.5533 0.099 Uiso 1 1 calc R . .
C5 C 0.1628(5) 0.0962(2) 0.6843(5) 0.0849(16) Uani 1 1 d . . .
H5 H 0.1314 0.0618 0.6323 0.102 Uiso 1 1 calc R . .
As1 As 0.0000 0.11034(4) 0.2500 0.04581(19) Uani 1 4 d S . .
F1 F 0.0000 0.0551(4) 0.3722(9) 0.111(4) Uani 0.50 2 d SP . .
F2 F 0.0000 0.1675(5) 0.3628(10) 0.135(5) Uani 0.50 2 d SP . .
F3 F 0.1301(9) 0.1510(5) 0.3321(9) 0.149(3) Uani 0.50 1 d P . .
F4 F 0.1262(9) 0.0677(5) 0.3250(9) 0.163(4) Uani 0.50 1 d P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
As As 0.0499 2.0058 '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
C3 W1 C3 165.5(4) 3_556 . ?
C3 W1 C4 36.16(16) 3_556 12 ?
C3 W1 C4 149.75(15) . 12 ?
C3 W1 C4 149.75(15) 3_556 . ?
C3 W1 C4 36.16(16) . . ?
C4 W1 C4 114.8(3) 12 . ?
C3 W1 C4 149.75(15) 3_556 10_557 ?
C3 W1 C4 36.16(16) . 10_557 ?
C4 W1 C4 154.1(3) 12 10_557 ?
C4 W1 C4 58.7(3) . 10_557 ?
C3 W1 C4 36.16(16) 3_556 3_556 ?
C3 W1 C4 149.75(15) . 3_556 ?
C4 W1 C4 58.7(3) 12 3_556 ?
C4 W1 C4 154.1(3) . 3_556 ?
C4 W1 C4 114.8(3) 10_557 3_556 ?
C3 W1 C5 57.6(2) 3_556 12 ?
C3 W1 C5 135.8(2) . 12 ?
C4 W1 C5 33.37(16) 12 12 ?
C4 W1 C5 103.2(2) . 12 ?
C4 W1 C5 120.9(3) 10_557 12 ?
C4 W1 C5 56.55(17) 3_556 12 ?
C3 W1 C5 57.6(2) 3_556 3_556 ?
C3 W1 C5 135.8(2) . 3_556 ?
C4 W1 C5 56.55(17) 12 3_556 ?
C4 W1 C5 120.9(3) . 3_556 ?
C4 W1 C5 103.2(2) 10_557 3_556 ?
C4 W1 C5 33.37(16) 3_556 3_556 ?
C5 W1 C5 33.7(3) 12 3_556 ?
C3 W1 C5 135.8(2) 3_556 10_557 ?
C3 W1 C5 57.6(2) . 10_557 ?
C4 W1 C5 120.9(3) 12 10_557 ?
C4 W1 C5 56.55(17) . 10_557 ?
C4 W1 C5 33.37(16) 10_557 10_557 ?
C4 W1 C5 103.2(2) 3_556 10_557 ?
C5 W1 C5 88.0(3) 12 10_557 ?
C5 W1 C5 78.3(2) 3_556 10_557 ?
C3 W1 C5 135.8(2) 3_556 . ?
C3 W1 C5 57.6(2) . . ?
C4 W1 C5 103.2(2) 12 . ?
C4 W1 C5 33.37(16) . . ?
C4 W1 C5 56.55(17) 10_557 . ?
C4 W1 C5 120.9(3) 3_556 . ?
C5 W1 C5 78.3(2) 12 . ?
C5 W1 C5 88.0(3) 3_556 . ?
C5 W1 C5 33.7(3) 10_557 . ?
C3 W1 S1 84.61(14) 3_556 . ?
C3 W1 S1 84.61(14) . . ?
C4 W1 S1 80.74(14) 12 . ?
C4 W1 S1 80.74(14) . . ?
C4 W1 S1 119.62(16) 10_557 . ?
C4 W1 S1 119.62(16) 3_556 . ?
C5 W1 S1 109.97(14) 12 . ?
C5 W1 S1 136.76(11) 3_556 . ?
C5 W1 S1 136.76(11) 10_557 . ?
C5 W1 S1 109.97(14) . . ?
C3 W1 S1 84.61(14) 3_556 10_557 ?
C3 W1 S1 84.61(14) . 10_557 ?
C4 W1 S1 119.62(16) 12 10_557 ?
C4 W1 S1 119.62(16) . 10_557 ?
C4 W1 S1 80.74(14) 10_557 10_557 ?
C4 W1 S1 80.74(14) 3_556 10_557 ?
C5 W1 S1 136.76(11) 12 10_557 ?
C5 W1 S1 109.97(14) 3_556 10_557 ?
C5 W1 S1 109.97(14) 10_557 10_557 ?
C5 W1 S1 136.76(11) . 10_557 ?
S1 W1 S1 83.86(7) . 10_557 ?
C1 S1 W1 104.69(17) . . ?
C2 S2 C1 97.0(3) . . ?
C1 C1 S1 123.38(17) 10_557 . ?
C1 C1 S2 115.99(17) 10_557 . ?
S1 C1 S2 120.6(3) . . ?
S3 C2 S2 123.0(2) . 10_557 ?
S3 C2 S2 123.0(2) . . ?
S2 C2 S2 114.1(4) 10_557 . ?
C4 C3 C4 104.9(6) 10_557 . ?
C4 C3 W1 72.7(3) 10_557 . ?
C4 C3 W1 72.7(3) . . ?
C5 C4 C3 107.6(5) . . ?
C5 C4 W1 74.5(3) . . ?
C3 C4 W1 71.2(3) . . ?
C4 C5 C5 109.9(3) . 10_557 ?
C4 C5 W1 72.1(3) . . ?
C5 C5 W1 73.17(13) 10_557 . ?
F4 As1 F4 115.0(7) . 3 ?
F4 As1 F4 88.7(8) . 12 ?
F4 As1 F4 56.3(7) 3 12 ?
F4 As1 F4 56.3(7) . 10_556 ?
F4 As1 F4 88.7(8) 3 10_556 ?
F4 As1 F4 115.0(7) 12 10_556 ?
F4 As1 F2 93.0(4) . . ?
F4 As1 F2 135.6(4) 3 . ?
F4 As1 F2 93.0(4) 12 . ?
F4 As1 F2 135.6(4) 10_556 . ?
F4 As1 F2 135.6(4) . 10_556 ?
F4 As1 F2 93.0(4) 3 10_556 ?
F4 As1 F2 135.6(4) 12 10_556 ?
F4 As1 F2 93.0(4) 10_556 10_556 ?
F2 As1 F2 89.1(8) . 10_556 ?
F4 As1 F3 62.6(4) . . ?
F4 As1 F3 177.1(5) 3 . ?
F4 As1 F3 121.5(4) 12 . ?
F4 As1 F3 90.9(5) 10_556 . ?
F2 As1 F3 44.7(4) . . ?
F2 As1 F3 89.9(3) 10_556 . ?
F4 As1 F3 90.9(5) . 10_556 ?
F4 As1 F3 121.5(4) 3 10_556 ?
F4 As1 F3 177.1(5) 12 10_556 ?
F4 As1 F3 62.6(4) 10_556 10_556 ?
F2 As1 F3 89.9(3) . 10_556 ?
F2 As1 F3 44.7(4) 10_556 10_556 ?
F3 As1 F3 60.6(6) . 10_556 ?
F4 As1 F3 177.1(5) . 3 ?
F4 As1 F3 62.6(4) 3 3 ?
F4 As1 F3 90.9(5) 12 3 ?
F4 As1 F3 121.5(4) 10_556 3 ?
F2 As1 F3 89.9(3) . 3 ?
F2 As1 F3 44.7(4) 10_556 3 ?
F3 As1 F3 120.0(7) . 3 ?
F3 As1 F3 89.4(7) 10_556 3 ?
F4 As1 F3 121.5(4) . 12 ?
F4 As1 F3 90.9(5) 3 12 ?
F4 As1 F3 62.6(4) 12 12 ?
F4 As1 F3 177.1(5) 10_556 12 ?
F2 As1 F3 44.7(4) . 12 ?
F2 As1 F3 89.9(3) 10_556 12 ?
F3 As1 F3 89.4(7) . 12 ?
F3 As1 F3 120.0(7) 10_556 12 ?
F3 As1 F3 60.6(6) 3 12 ?
F4 As1 F1 89.3(3) . 10_556 ?
F4 As1 F1 44.7(4) 3 10_556 ?
F4 As1 F1 89.4(3) 12 10_556 ?
F4 As1 F1 44.7(4) 10_556 10_556 ?
F2 As1 F1 176.7(5) . 10_556 ?
F2 As1 F1 87.6(5) 10_556 10_556 ?
F3 As1 F1 135.2(4) . 10_556 ?
F3 As1 F1 87.8(4) 10_556 10_556 ?
F3 As1 F1 87.8(4) 3 10_556 ?
F3 As1 F1 135.2(4) 12 10_556 ?
F4 As1 F1 44.7(4) . . ?
F4 As1 F1 89.4(3) 3 . ?
F4 As1 F1 44.7(4) 12 . ?
F4 As1 F1 89.4(3) 10_556 . ?
F2 As1 F1 87.6(5) . . ?
F2 As1 F1 176.7(5) 10_556 . ?
F3 As1 F1 87.8(4) . . ?
F3 As1 F1 135.2(4) 10_556 . ?
F3 As1 F1 135.2(4) 3 . ?
F3 As1 F1 87.8(4) 12 . ?
F1 As1 F1 95.6(7) 10_556 . ?
F4 F1 F4 128.4(11) . 12 ?
F4 F1 As1 65.0(6) . . ?
F4 F1 As1 65.0(6) 12 . ?
F3 F2 F3 136.9(11) 12 . ?
F3 F2 As1 68.5(6) 12 . ?
F3 F2 As1 68.5(6) . . ?
F2 F3 As1 66.8(5) . . ?
F2 F3 F3 104.4(7) . 10_556 ?
As1 F3 F3 59.7(3) . 10_556 ?
F2 F3 F4 105.1(8) . . ?
As1 F3 F4 57.6(3) . . ?
F3 F3 F4 87.5(5) 10_556 . ?
F1 F4 F4 112.5(6) . 10_556 ?
F1 F4 As1 70.3(5) . . ?
F4 F4 As1 61.8(3) 10_556 . ?
F1 F4 F3 102.0(8) . . ?
F4 F4 F3 92.5(5) 10_556 . ?
As1 F4 F3 59.8(4) . . ?
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 C3 2.279(6) 3_556 ?
W1 C3 2.279(6) . ?
W1 C4 2.298(4) 12 ?
W1 C4 2.298(4) . ?
W1 C4 2.298(4) 10_557 ?
W1 C4 2.298(4) 3_556 ?
W1 C5 2.328(4) 12 ?
W1 C5 2.328(4) 3_556 ?
W1 C5 2.328(4) 10_557 ?
W1 C5 2.328(4) . ?
W1 S1 2.4293(14) . ?
W1 S1 2.4293(14) 10_557 ?
S1 C1 1.693(5) . ?
S2 C2 1.728(4) . ?
S2 C1 1.729(5) . ?
S3 C2 1.643(7) . ?
C1 C1 1.384(10) 10_557 ?
C2 S2 1.728(4) 10_557 ?
C3 C4 1.421(6) 10_557 ?
C3 C4 1.421(6) . ?
C4 C5 1.329(7) . ?
C5 C5 1.348(10) 10_557 ?
As1 F4 1.631(7) . ?
As1 F4 1.631(7) 3 ?
As1 F4 1.631(7) 12 ?
As1 F4 1.631(7) 10_556 ?
As1 F2 1.650(8) . ?
As1 F2 1.650(8) 10_556 ?
As1 F3 1.670(7) . ?
As1 F3 1.670(7) 10_556 ?
As1 F3 1.670(7) 3 ?
As1 F3 1.670(7) 12 ?
As1 F1 1.693(8) 10_556 ?
As1 F1 1.693(8) . ?
F1 F4 1.265(11) . ?
F1 F4 1.266(11) 12 ?
F2 F3 1.263(10) 12 ?
F2 F3 1.263(10) . ?
F3 F3 1.686(19) 10_556 ?
F3 F4 1.714(12) . ?
F4 F4 1.539(19) 10_556 ?
