#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:58:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179272 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/92/4319261.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_4319261
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            'C26 H52 N2 O2 S4 W'
_chemical_formula_weight         736.79
_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                 113.4720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4185(10)
_cell_length_b                   13.8166(10)
_cell_length_c                   18.0792(16)
_cell_measurement_temperature    233(2)
_cell_volume                     3303.6(4)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.1006
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21286
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    3.773
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed by SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.828
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0393P)²+4.5517P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                6485
_reflns_number_total             7980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001046w_4.cif
_cod_data_source_block           '[Et4N]2[6]'
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4319261
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 0.536242(12) 0.124219(12) 0.800285(9) 0.02592(7) Uani 1 1 d . . .
S1 S 0.57517(10) 0.29742(9) 0.79828(8) 0.0383(3) Uani 1 1 d . . .
S2 S 0.42440(10) 0.19332(9) 0.85862(8) 0.0388(3) Uani 1 1 d . . .
S3 S 0.55137(8) -0.02098(8) 0.88241(7) 0.0324(2) Uani 1 1 d . . .
S4 S 0.71413(8) 0.08279(9) 0.83689(7) 0.0353(2) Uani 1 1 d . . .
C1 C 0.4154(3) 0.0570(4) 0.7305(3) 0.0323(9) Uani 1 1 d . . .
C2 C 0.5289(4) 0.1328(3) 0.6916(3) 0.0363(10) Uani 1 1 d . . .
O1 O 0.3435(3) 0.0173(3) 0.6855(2) 0.0467(9) Uani 1 1 d . . .
O2 O 0.5178(3) 0.1374(3) 0.6234(2) 0.0490(10) Uani 1 1 d . . .
C5 C 0.6775(3) -0.0607(3) 0.9225(3) 0.0306(9) Uani 1 1 d . . .
C6 C 0.7474(3) -0.0177(4) 0.9026(3) 0.0338(9) Uani 1 1 d . . .
C9 C 0.6954(4) -0.1486(4) 0.9758(3) 0.0450(12) Uani 1 1 d . . .
H9A H 0.7654 -0.1666 0.9955 0.083(3) Uiso 1 1 calc R . .
H9B H 0.6544 -0.2011 0.9453 0.083(3) Uiso 1 1 calc R . .
H9C H 0.6779 -0.1339 1.0205 0.083(3) Uiso 1 1 calc R . .
C3 C 0.5042(4) 0.3642(4) 0.8409(3) 0.0428(12) Uani 1 1 d . . .
C4 C 0.4408(4) 0.3204(4) 0.8666(3) 0.0429(12) Uani 1 1 d . . .
C10 C 0.8555(4) -0.0483(4) 0.9277(3) 0.0465(12) Uani 1 1 d . . .
H10A H 0.8690 -0.1029 0.9633 0.083(3) Uiso 1 1 calc R . .
H10B H 0.8993 0.0043 0.9549 0.083(3) Uiso 1 1 calc R . .
H10C H 0.8673 -0.0660 0.8808 0.083(3) Uiso 1 1 calc R . .
C8 C 0.3767(6) 0.3723(5) 0.9031(4) 0.067(2) Uani 1 1 d . . .
H8A H 0.3902 0.4405 0.9052 0.083(3) Uiso 1 1 calc R . .
H8B H 0.3927 0.3485 0.9566 0.083(3) Uiso 1 1 calc R . .
H8C H 0.3065 0.3610 0.8705 0.083(3) Uiso 1 1 calc R . .
N2 N 0.2280(3) 0.3054(3) 0.6001(2) 0.0376(9) Uani 1 1 d . . .
N1 N 0.9271(3) 0.3106(3) 0.8425(2) 0.0350(8) Uani 1 1 d . . .
C15 C 0.8570(4) 0.3449(4) 0.8823(3) 0.0461(12) Uani 1 1 d . . .
H15A H 0.8000 0.3009 0.8672 0.083(3) Uiso 1 1 calc R . .
H15B H 0.8933 0.3411 0.9404 0.083(3) Uiso 1 1 calc R . .
C11 C 0.9579(4) 0.2066(4) 0.8712(3) 0.0463(12) Uani 1 1 d . . .
H11A H 0.9927 0.2074 0.9295 0.083(3) Uiso 1 1 calc R . .
H11B H 0.8968 0.1686 0.8581 0.083(3) Uiso 1 1 calc R . .
C17 C 1.0182(4) 0.3769(4) 0.8637(4) 0.0471(13) Uani 1 1 d . . .
H17A H 1.0595 0.3536 0.8361 0.083(3) Uiso 1 1 calc R . .
H17B H 0.9945 0.4411 0.8430 0.083(3) Uiso 1 1 calc R . .
C25 C 0.3419(4) 0.3095(4) 0.6311(3) 0.0439(12) Uani 1 1 d . . .
H25A H 0.3676 0.3394 0.6841 0.083(3) Uiso 1 1 calc R . .
H25B H 0.3675 0.2437 0.6378 0.083(3) Uiso 1 1 calc R . .
C13 C 0.8737(4) 0.3149(4) 0.7512(3) 0.0461(12) Uani 1 1 d . . .
H13A H 0.9211 0.2959 0.7281 0.083(3) Uiso 1 1 calc R . .
H13B H 0.8543 0.3815 0.7355 0.083(3) Uiso 1 1 calc R . .
C16 C 0.8175(5) 0.4459(5) 0.8606(4) 0.0590(16) Uani 1 1 d . . .
H16A H 0.7745 0.4617 0.8881 0.083(3) Uiso 1 1 calc R . .
H16B H 0.7794 0.4502 0.8034 0.083(3) Uiso 1 1 calc R . .
H16C H 0.8731 0.4904 0.8765 0.083(3) Uiso 1 1 calc R . .
C19 C 0.1828(5) 0.4071(5) 0.5856(5) 0.0629(19) Uani 1 1 d . . .
H19A H 0.1938 0.4359 0.5409 0.083(3) Uiso 1 1 calc R . .
H19B H 0.1103 0.4018 0.5699 0.083(3) Uiso 1 1 calc R . .
C21 C 0.2048(5) 0.2514(5) 0.6637(4) 0.0599(17) Uani 1 1 d . . .
H21A H 0.2306 0.2884 0.7134 0.083(3) Uiso 1 1 calc R . .
H21B H 0.2398 0.1897 0.6741 0.083(3) Uiso 1 1 calc R . .
C26 C 0.3834(5) 0.3627(5) 0.5798(5) 0.0649(19) Uani 1 1 d . . .
H26A H 0.4560 0.3617 0.6048 0.083(3) Uiso 1 1 calc R . .
H26B H 0.3602 0.4285 0.5736 0.083(3) Uiso 1 1 calc R . .
H26C H 0.3610 0.3324 0.5278 0.083(3) Uiso 1 1 calc R . .
C12 C 1.0240(6) 0.1566(5) 0.8371(4) 0.0626(17) Uani 1 1 d . . .
H12A H 1.0382 0.0920 0.8583 0.083(3) Uiso 1 1 calc R . .
H12B H 1.0862 0.1917 0.8515 0.083(3) Uiso 1 1 calc R . .
H12C H 0.9900 0.1538 0.7794 0.083(3) Uiso 1 1 calc R . .
C14 C 0.7797(5) 0.2513(5) 0.7151(3) 0.0588(16) Uani 1 1 d . . .
H14A H 0.7510 0.2580 0.6575 0.083(3) Uiso 1 1 calc R . .
H14B H 0.7309 0.2709 0.7360 0.083(3) Uiso 1 1 calc R . .
H14C H 0.7980 0.1849 0.7291 0.083(3) Uiso 1 1 calc R . .
C18 C 1.0843(6) 0.3852(6) 0.9526(4) 0.070(2) Uani 1 1 d . . .
H18A H 1.1400 0.4277 0.9601 0.083(3) Uiso 1 1 calc R . .
H18B H 1.1096 0.3224 0.9738 0.083(3) Uiso 1 1 calc R . .
H18C H 1.0453 0.4109 0.9805 0.083(3) Uiso 1 1 calc R . .
C23 C 0.1866(5) 0.2527(6) 0.5197(3) 0.0619(17) Uani 1 1 d . . .
H23A H 0.2066 0.2880 0.4820 0.083(3) Uiso 1 1 calc R . .
H23B H 0.1134 0.2538 0.4988 0.083(3) Uiso 1 1 calc R . .
C7 C 0.5205(6) 0.4733(4) 0.8425(4) 0.0641(18) Uani 1 1 d . . .
H7A H 0.4799 0.5043 0.8667 0.083(3) Uiso 1 1 calc R . .
H7B H 0.5014 0.4967 0.7885 0.083(3) Uiso 1 1 calc R . .
H7C H 0.5905 0.4876 0.8735 0.083(3) Uiso 1 1 calc R . .
C24 C 0.2214(7) 0.1464(6) 0.5224(5) 0.077(2) Uani 1 1 d . . .
H24A H 0.1919 0.1190 0.4693 0.083(3) Uiso 1 1 calc R . .
H24B H 0.2002 0.1100 0.5582 0.083(3) Uiso 1 1 calc R . .
H24C H 0.2938 0.1443 0.5415 0.083(3) Uiso 1 1 calc R . .
C20 C 0.2238(8) 0.4723(5) 0.6550(5) 0.088(3) Uani 1 1 d . . .
H20A H 0.1927 0.5348 0.6405 0.083(3) Uiso 1 1 calc R . .
H20B H 0.2955 0.4784 0.6712 0.083(3) Uiso 1 1 calc R . .
H20C H 0.2101 0.4464 0.6989 0.083(3) Uiso 1 1 calc R . .
C22 C 0.0912(6) 0.2333(6) 0.6392(6) 0.093(3) Uani 1 1 d . . .
H22A H 0.0810 0.1996 0.6818 0.083(3) Uiso 1 1 calc R . .
H22B H 0.0655 0.1948 0.5910 0.083(3) Uiso 1 1 calc R . .
H22C H 0.0561 0.2941 0.6294 0.083(3) 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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 '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
C2 W1 C1 72.3(2) . . yes
C2 W1 S2 129.61(14) . . yes
C1 W1 S2 83.74(13) . . yes
C2 W1 S4 85.19(15) . . yes
C1 W1 S4 129.73(14) . . yes
S2 W1 S4 140.78(4) . . yes
C2 W1 S3 128.47(14) . . yes
C1 W1 S3 80.90(14) . . yes
S2 W1 S3 88.46(4) . . yes
S4 W1 S3 79.29(4) . . yes
C2 W1 S1 81.13(15) . . yes
C1 W1 S1 127.50(14) . . yes
S2 W1 S1 79.64(4) . . yes
S4 W1 S1 90.62(4) . . yes
S3 W1 S1 146.94(4) . . yes
C3 S1 W1 109.05(19) . . yes
C4 S2 W1 109.43(19) . . yes
C5 S3 W1 109.46(16) . . yes
C6 S4 W1 109.91(16) . . yes
O1 C1 W1 177.0(4) . . yes
O1 C1 C2 123.3(4) . . yes
W1 C1 C2 53.75(17) . . yes
O2 C2 W1 175.7(4) . . yes
O2 C2 C1 122.2(4) . . yes
W1 C2 C1 53.98(17) . . yes
C6 C5 C9 125.1(4) . . yes
C6 C5 S3 121.2(3) . . yes
C9 C5 S3 113.6(4) . . yes
C5 C6 C10 126.6(5) . . yes
C5 C6 S4 119.9(3) . . yes
C10 C6 S4 113.4(4) . . yes
C4 C3 C7 124.5(5) . . yes
C4 C3 S1 121.0(4) . . yes
C7 C3 S1 114.5(5) . . yes
C3 C4 C8 124.2(5) . . yes
C3 C4 S2 120.9(4) . . yes
C8 C4 S2 114.9(5) . . yes
C23 N2 C21 111.6(5) . . yes
C23 N2 C25 109.2(4) . . yes
C21 N2 C25 105.8(4) . . yes
C23 N2 C19 107.5(5) . . yes
C21 N2 C19 111.9(4) . . yes
C25 N2 C19 110.9(4) . . yes
C13 N1 C17 105.2(4) . . yes
C13 N1 C15 110.7(4) . . yes
C17 N1 C15 111.2(4) . . yes
C13 N1 C11 111.0(4) . . yes
C17 N1 C11 112.0(4) . . yes
C15 N1 C11 106.7(4) . . yes
C16 C15 N1 114.8(4) . . yes
C12 C11 N1 116.1(5) . . yes
C18 C17 N1 115.4(5) . . yes
C26 C25 N2 115.8(5) . . yes
N1 C13 C14 114.9(4) . . yes
C20 C19 N2 114.9(6) . . yes
N2 C21 C22 113.2(6) . . yes
N2 C23 C24 115.2(5) . . 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 C2 1.928(5) . yes
W1 C1 1.934(5) . yes
W1 S2 2.4452(12) . yes
W1 S4 2.4478(11) . yes
W1 S3 2.4533(11) . yes
W1 S1 2.4616(12) . yes
S1 C3 1.766(6) . yes
S2 C4 1.770(5) . yes
S3 C5 1.757(5) . yes
S4 C6 1.765(5) . yes
C1 O1 1.168(6) . yes
C1 C2 2.277(7) . yes
C2 O2 1.181(6) . yes
C5 C6 1.337(7) . yes
C5 C9 1.506(7) . yes
C6 C10 1.500(6) . yes
C3 C4 1.325(8) . yes
C3 C7 1.524(7) . yes
C4 C8 1.513(7) . yes
N2 C23 1.520(8) . yes
N2 C21 1.517(6) . yes
N2 C25 1.510(6) . yes
N2 C19 1.527(7) . yes
N1 C13 1.520(6) . yes
N1 C17 1.521(7) . yes
N1 C15 1.531(7) . yes
N1 C11 1.531(7) . yes
C15 C16 1.499(9) . yes
C11 C12 1.497(9) . yes
C17 C18 1.512(9) . yes
C25 C26 1.485(8) . yes
C13 C14 1.526(8) . yes
C19 C20 1.464(11) . yes
C21 C22 1.537(10) . yes
C23 C24 1.545(10) . yes
