#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:58:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179272 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/92/4319263.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_4319263
loop_
_publ_author_name
'Dmitry V. Fomitchev'
'Booyong S. Lim'
'R. H. Holm'
_publ_contact_author
;
       R.H. Holm
       Department of Chemistry and Chemical Biology
       Harvard University
       Cambridge, MA 02138
       USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_contact_author_fax         '+1 (617) 496-9289'
_publ_contact_author_phone       '+1 (617) 495-0853'
_publ_section_title
;
 Electron Distribution in the Nonclassical Bis(dithiolene) Electron
 Transfer Series [M(CO)2(S2C2Me2)2]0/1-/2- (M = Mo, W): Assessment by
 Structural, Spectroscopic, and Density Functional Theory Results
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              645
_journal_page_last               654
_journal_paper_doi               10.1021/ic001046w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C22 H41 N2 S6 W'
_chemical_formula_weight         709.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.096(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6566(14)
_cell_length_b                   23.791(3)
_cell_length_c                   13.4302(19)
_cell_measurement_temperature    233(2)
_cell_volume                     2964.5(7)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area detector system'
_diffrn_measurement_method       'rotation around ο axis, 0.3 deg/frame'
_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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12323
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    4.333
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed by SADABS'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.532
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3874
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0520P)²+20.2246P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                3632
_reflns_number_total             3874
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001046w_6.cif
_cod_data_source_block           '[Et4N][11]MeCN'
_cod_database_code               4319263
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 -0.48768(3) 0.341831(12) 0.59586(2) 0.03319(15) Uani 1 1 d . . .
S1 S -0.7244(2) 0.36365(11) 0.60504(17) 0.0502(5) Uani 1 1 d . . .
S2 S -0.4352(2) 0.37243(11) 0.77030(17) 0.0524(6) Uani 1 1 d . . .
S3 S -0.6095(3) 0.26529(10) 0.49382(19) 0.0583(6) Uani 1 1 d . . .
S4 S -0.3226(2) 0.26854(10) 0.6666(2) 0.0602(6) Uani 1 1 d . . .
S5 S -0.5595(2) 0.39096(11) 0.43619(18) 0.0544(6) Uani 1 1 d . . .
S6 S -0.2706(2) 0.39059(12) 0.60408(19) 0.0607(7) Uani 1 1 d . . .
N1 N -0.1735(7) 0.3075(3) 0.3123(5) 0.0392(15) Uani 1 1 d . . .
C3 C -0.4978(10) 0.2064(3) 0.5178(7) 0.049(2) Uani 1 1 d . . .
C4 C -0.3717(10) 0.2083(3) 0.5933(7) 0.048(2) Uani 1 1 d . . .
C9 C -0.5552(14) 0.1558(4) 0.4523(10) 0.081(4) Uani 1 1 d . . .
H3A H -0.6470 0.1647 0.4050 0.122 Uiso 1 1 calc R . .
H3B H -0.5664 0.1253 0.4962 0.122 Uiso 1 1 calc R . .
H3C H -0.4890 0.1451 0.4140 0.122 Uiso 1 1 calc R . .
C10 C -0.2696(12) 0.1593(4) 0.6226(10) 0.068(3) Uani 1 1 d . . .
H4A H -0.1861 0.1706 0.6764 0.103 Uiso 1 1 calc R . .
H4B H -0.2407 0.1473 0.5631 0.103 Uiso 1 1 calc R . .
H4C H -0.3168 0.1289 0.6469 0.103 Uiso 1 1 calc R . .
C1 C -0.7177(9) 0.3895(4) 0.7266(7) 0.048(2) Uani 1 1 d . . .
C2 C -0.5902(9) 0.3940(3) 0.7998(6) 0.046(2) Uani 1 1 d . . .
C7 C -0.8610(11) 0.4089(5) 0.7404(9) 0.080(3) Uani 1 1 d . . .
H7A H -0.9362 0.4017 0.6780 0.120 Uiso 1 1 calc R . .
H7B H -0.8566 0.4485 0.7550 0.120 Uiso 1 1 calc R . .
H7C H -0.8808 0.3889 0.7969 0.120 Uiso 1 1 calc R . .
C8 C -0.5717(12) 0.4190(5) 0.9050(7) 0.069(3) Uani 1 1 d . . .
H8A H -0.4719 0.4175 0.9435 0.103 Uiso 1 1 calc R . .
H8B H -0.6280 0.3981 0.9410 0.103 Uiso 1 1 calc R . .
H8C H -0.6034 0.4574 0.8978 0.103 Uiso 1 1 calc R . .
C5 C -0.4283(8) 0.4395(3) 0.4304(7) 0.0432(19) Uani 1 1 d . . .
C6 C -0.3011(8) 0.4393(3) 0.5061(7) 0.045(2) Uani 1 1 d . . .
C11 C -0.4645(11) 0.4785(4) 0.3387(8) 0.067(3) Uani 1 1 d . . .
H11A H -0.5602 0.4707 0.2964 0.100 Uiso 1 1 calc R . .
H11B H -0.3971 0.4729 0.2988 0.100 Uiso 1 1 calc R . .
H11C H -0.4591 0.5167 0.3624 0.100 Uiso 1 1 calc R . .
C12 C -0.1798(10) 0.4805(4) 0.5087(8) 0.061(3) Uani 1 1 d . . .
H12A H -0.1008 0.4734 0.5689 0.092 Uiso 1 1 calc R . .
H12B H -0.2139 0.5182 0.5113 0.092 Uiso 1 1 calc R . .
H12C H -0.1480 0.4758 0.4475 0.092 Uiso 1 1 calc R . .
C13 C -0.3102(12) 0.3026(5) 0.3413(10) 0.055(3) Uani 0.710(14) 1 d P A 1
H13A H -0.3683 0.3359 0.3186 0.066 Uiso 0.710(14) 1 calc PR A 1
H13B H -0.2893 0.3002 0.4161 0.066 Uiso 0.710(14) 1 calc PR A 1
C13A C -0.2427(12) 0.2588(5) 0.2514(10) 0.055(3) Uani 0.29 1 d PR A 2
H13A H -0.1781 0.2275 0.2702 0.066 Uiso 0.290(14) 1 d PR A 2
H13B H -0.2627 0.2649 0.1766 0.066 Uiso 0.290(14) 1 d PR A 2
C14 C -0.3989(13) 0.2482(6) 0.2899(11) 0.097(4) Uani 1 1 d . . .
H14A H -0.4869 0.2434 0.3101 0.146 Uiso 0.50 1 d PR A 1
H14B H -0.4206 0.2524 0.2153 0.146 Uiso 0.50 1 d PR A 1
H14C H -0.3383 0.2165 0.3110 0.146 Uiso 0.50 1 d PR A 1
H14D H -0.4485 0.2162 0.2553 0.146 Uiso 0.50 1 d PR A 2
H14E H -0.3759 0.2429 0.3642 0.146 Uiso 0.50 1 d PR A 2
H14F H -0.4597 0.2802 0.2710 0.146 Uiso 0.50 1 d PR A 2
C15 C -0.0971(13) 0.3598(5) 0.3616(10) 0.057(3) Uani 0.710(14) 1 d P A 1
H15A H -0.1620 0.3914 0.3411 0.069 Uiso 0.710(14) 1 calc PR A 1
H15B H -0.0755 0.3560 0.4362 0.069 Uiso 0.710(14) 1 calc PR A 1
C15A C -0.0401(13) 0.3218(5) 0.2849(10) 0.057(3) Uani 0.29 1 d PR A 2
H15A H -0.0605 0.3251 0.2095 0.069 Uiso 0.290(14) 1 d PR A 2
H15B H 0.0260 0.2910 0.3058 0.069 Uiso 0.290(14) 1 d PR A 2
C16 C 0.0400(11) 0.3727(5) 0.3346(9) 0.081(3) Uani 1 1 d . . .
H16A H 0.0766 0.4060 0.3717 0.122 Uiso 0.50 1 d PR A 1
H16B H 0.1103 0.3437 0.3547 0.122 Uiso 0.50 1 d PR A 1
H16C H 0.0205 0.3791 0.2607 0.122 Uiso 0.50 1 d PR A 1
H16D H 0.1258 0.3776 0.3116 0.122 Uiso 0.50 1 d PR A 2
H16E H -0.0221 0.4041 0.3142 0.122 Uiso 0.50 1 d PR A 2
H16F H 0.0656 0.3691 0.4094 0.122 Uiso 0.50 1 d PR A 2
C17 C -0.1949(14) 0.3084(6) 0.1954(9) 0.061(4) Uani 0.710(14) 1 d P A 1
H17A H -0.2408 0.2739 0.1642 0.073 Uiso 0.710(14) 1 calc PR A 1
H17B H -0.1028 0.3119 0.1801 0.073 Uiso 0.710(14) 1 calc PR A 1
C17A C -0.2840(14) 0.3527(6) 0.2864(9) 0.061(4) Uani 0.29 1 d PR A 2
H17A H -0.2488 0.3864 0.3243 0.073 Uiso 0.290(14) 1 d PR A 2
H17B H -0.3741 0.3418 0.3006 0.073 Uiso 0.290(14) 1 d PR A 2
C18 C -0.2975(17) 0.3626(7) 0.1503(11) 0.136(7) Uani 1 1 d . . .
H18A H -0.3152 0.3654 0.0757 0.204 Uiso 0.50 1 d PR A 1
H18B H -0.3871 0.3569 0.1678 0.204 Uiso 0.50 1 d PR A 1
H18C H -0.2534 0.3962 0.1823 0.204 Uiso 0.50 1 d PR A 1
H18D H -0.3662 0.3911 0.1215 0.204 Uiso 0.50 1 d PR A 2
H18E H -0.2053 0.3724 0.1403 0.204 Uiso 0.50 1 d PR A 2
H18F H -0.3290 0.3282 0.1156 0.204 Uiso 0.50 1 d PR A 2
C19 C -0.0744(14) 0.2583(5) 0.3490(10) 0.062(4) Uani 0.710(14) 1 d P A 1
H19A H 0.0158 0.2646 0.3322 0.074 Uiso 0.710(14) 1 calc PR A 1
H19B H -0.1181 0.2245 0.3136 0.074 Uiso 0.710(14) 1 calc PR A 1
C19A C -0.1600(14) 0.2982(5) 0.4378(10) 0.062(4) Uani 0.29 1 d PR A 2
H19A H -0.2510 0.2868 0.4498 0.074 Uiso 0.290(14) 1 d PR A 2
H19B H -0.1278 0.3318 0.4771 0.074 Uiso 0.290(14) 1 d PR A 2
C20 C -0.0438(14) 0.2502(6) 0.4715(10) 0.097(4) Uani 1 1 d . . .
H20A H 0.0198 0.2191 0.4897 0.145 Uiso 0.50 1 d PR A 1
H20B H 0.0023 0.2826 0.5074 0.145 Uiso 0.50 1 d PR A 1
H20C H -0.1310 0.2431 0.4915 0.145 Uiso 0.50 1 d PR A 1
H20D H -0.0288 0.2422 0.5445 0.145 Uiso 0.50 1 d PR A 2
H20E H -0.0768 0.2175 0.4312 0.145 Uiso 0.50 1 d PR A 2
H20F H 0.0452 0.2624 0.4589 0.145 Uiso 0.50 1 d PR A 2
C21 C 0.3433(15) 0.0080(6) 0.351(2) 0.185(7) Uani 1 1 d DU . .
H21A H 0.2885 -0.0075 0.2864 0.277 Uiso 1 1 d R . .
H21B H 0.3452 0.0475 0.3457 0.277 Uiso 1 1 d R . .
H21C H 0.2994 -0.0021 0.4061 0.277 Uiso 1 1 d R . .
C22 C 0.4920(15) -0.0108(7) 0.378(2) 0.185(7) Uani 1 1 d DU . .
N2 N 0.6079(16) -0.0243(9) 0.416(2) 0.58(5) Uani 1 1 d D . .
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
S2 W1 S5 132.17(9) . . yes
S2 W1 S6 81.94(9) . . yes
S5 W1 S6 80.45(8) . . yes
S2 W1 S4 83.93(9) . . yes
S5 W1 S4 135.98(9) . . yes
S6 W1 S4 81.59(9) . . yes
S2 W1 S1 80.04(8) . . yes
S5 W1 S1 83.98(8) . . yes
S6 W1 S1 137.74(9) . . yes
S4 W1 S1 133.39(9) . . yes
S2 W1 S3 137.65(9) . . yes
S5 W1 S3 83.26(9) . . yes
S6 W1 S3 133.57(10) . . yes
S4 W1 S3 80.72(8) . . yes
S1 W1 S3 82.45(9) . . yes
C1 S1 W1 110.0(3) . . yes
C2 S2 W1 110.9(3) . . yes
C3 S3 W1 109.0(3) . . yes
C4 S4 W1 109.4(3) . . yes
C5 S5 W1 109.6(3) . . yes
C6 S6 W1 109.4(3) . . yes
C13A N1 C15A 109.6(7) . . yes
C13A N1 C13 77.5(6) . . yes
C15A N1 C13 171.3(9) . . yes
C13A N1 C17A 104.7(8) . . yes
C15A N1 C17A 113.4(8) . . yes
C13 N1 C17A 58.9(7) . . yes
C13A N1 C15 172.1(8) . . yes
C15A N1 C15 64.1(5) . . yes
C13 N1 C15 108.4(8) . . yes
C17A N1 C15 74.9(7) . . yes
C13A N1 C19 73.6(8) . . yes
C15A N1 C19 74.9(8) . . yes
C13 N1 C19 112.6(9) . . yes
C17A N1 C19 171.4(9) . . yes
C15 N1 C19 108.0(8) . . yes
C13A N1 C17 61.7(7) . . yes
C15A N1 C17 67.6(7) . . yes
C13 N1 C17 113.3(8) . . yes
C17A N1 C17 82.3(7) . . yes
C15 N1 C17 110.6(8) . . yes
C19 N1 C17 103.8(8) . . yes
C13A N1 C19A 110.7(8) . . yes
C15A N1 C19A 117.0(8) . . yes
C13 N1 C19A 63.3(7) . . yes
C17A N1 C19A 100.6(7) . . yes
C15 N1 C19A 76.9(7) . . yes
C19 N1 C19A 72.6(6) . . yes
C17 N1 C19A 172.4(8) . . yes
C4 C3 C9 125.0(9) . . yes
C4 C3 S3 119.7(6) . . yes
C9 C3 S3 115.3(8) . . yes
C3 C4 C10 124.0(8) . . yes
C3 C4 S4 120.2(6) . . yes
C10 C4 S4 115.8(7) . . yes
C2 C1 C7 124.5(9) . . yes
C2 C1 S1 120.2(6) . . yes
C7 C1 S1 115.2(7) . . yes
C1 C2 C8 124.3(8) . . yes
C1 C2 S2 118.9(6) . . yes
C8 C2 S2 116.7(7) . . yes
C6 C5 C11 124.9(8) . . yes
C6 C5 S5 118.9(6) . . yes
C11 C5 S5 116.2(7) . . yes
C5 C6 C12 123.0(8) . . yes
C5 C6 S6 120.2(6) . . yes
C12 C6 S6 116.8(7) . . yes
N1 C13 C14 111.1(9) . . yes
N1 C13A C14 104.3(8) . . yes
C13 C14 C13A 66.8(6) . . yes
C16 C15 N1 115.0(10) . . yes
N1 C15A C16 117.1(10) . . yes
C15A C16 C15 63.8(6) . . yes
N1 C17 C18 106.6(10) . . yes
N1 C17A C18 100.2(9) . . yes
C17 C18 C17A 69.9(6) . . yes
N1 C19 C20 110.4(10) . . yes
C20 C19A N1 103.7(9) . . yes
C19A C20 C19 72.8(7) . . yes
N2 C22 C21 168(3) . . yes
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 S2 2.370(2) . yes
W1 S5 2.371(2) . yes
W1 S6 2.372(2) . yes
W1 S4 2.376(2) . yes
W1 S1 2.381(2) . yes
W1 S3 2.384(2) . yes
S1 C1 1.729(9) . yes
S2 C2 1.728(8) . yes
S3 C3 1.742(9) . yes
S4 C4 1.729(9) . yes
S5 C5 1.733(8) . yes
S6 C6 1.716(9) . yes
N1 C13A 1.468(13) . yes
N1 C15A 1.474(14) . yes
N1 C13 1.481(13) . yes
N1 C17A 1.485(15) . yes
N1 C15 1.502(13) . yes
N1 C19 1.506(14) . yes
N1 C17 1.526(13) . yes
N1 C19A 1.669(15) . yes
C3 C4 1.352(13) . yes
C3 C9 1.504(13) . yes
C4 C10 1.507(13) . yes
C1 C2 1.350(12) . yes
C1 C7 1.518(12) . yes
C2 C8 1.498(12) . yes
C5 C6 1.360(12) . yes
C5 C11 1.503(12) . yes
C6 C12 1.520(11) . yes
C13 C14 1.599(17) . yes
C13A C14 1.743(16) . yes
C15 C16 1.498(16) . yes
C15A C16 1.492(16) . yes
C17 C18 1.64(2) . yes
C17A C18 1.812(19) . yes
C19 C20 1.601(18) . yes
C19A C20 1.575(17) . yes
C21 C22 1.4501(11) . yes
C22 N2 1.1405(11) . yes
