#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:58:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179272 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/92/4319259.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_4319259
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 Mo N2 O2 S4'
_chemical_formula_weight         648.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.3500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3994(13)
_cell_length_b                   13.8728(12)
_cell_length_c                   18.0505(16)
_cell_measurement_temperature    233(2)
_cell_volume                     3310.5(5)
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13929
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed by SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0344
_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)+(0.0380P)²+0.3095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                3189
_reflns_number_total             4338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001046w_2.cif
_cod_data_source_block           '[NEt4]2[3]'
_cod_database_code               4319259
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Mo1 Mo 0.23513(3) 0.37545(3) 0.197211(19) 0.02863(12) Uani 1 1 d . . .
S1 S 0.16853(8) 0.52184(8) 0.11685(6) 0.0358(3) Uani 1 1 d . . .
S2 S 0.37674(8) 0.41735(8) 0.16054(6) 0.0388(3) Uani 1 1 d . . .
S3 S 0.27659(9) 0.20259(8) 0.20052(7) 0.0419(3) Uani 1 1 d . . .
S4 S 0.06443(8) 0.30602(8) 0.14073(7) 0.0416(3) Uani 1 1 d . . .
O1 O 0.3948(2) 0.3611(2) 0.37375(19) 0.0583(9) Uani 1 1 d . . .
O2 O 0.1564(2) 0.4808(2) 0.31109(18) 0.0574(9) Uani 1 1 d . . .
N1 N 0.4135(3) 0.6897(2) 0.3417(2) 0.0416(9) Uani 1 1 d . . .
N2 N 0.1287(3) 0.1965(2) 0.4015(2) 0.0410(9) Uani 1 1 d . . .
C1 C 0.3367(3) 0.3669(3) 0.3055(3) 0.0444(11) Uani 1 1 d . . .
C2 C 0.1845(3) 0.4403(3) 0.2670(2) 0.0415(11) Uani 1 1 d . . .
C3 C 0.2562(3) 0.5632(3) 0.0783(2) 0.0325(10) Uani 1 1 d . . .
C4 C 0.3445(3) 0.5191(3) 0.0969(2) 0.0329(10) Uani 1 1 d . . .
C5 C 0.2214(3) 0.6528(3) 0.0262(3) 0.0483(12) Uani 1 1 d . . .
H5A H 0.2722 0.6715 0.0071 0.072 Uiso 1 1 calc R . .
H5B H 0.2108 0.7042 0.0576 0.072 Uiso 1 1 calc R . .
H5C H 0.1593 0.6392 -0.0189 0.072 Uiso 1 1 calc R . .
C6 C 0.4286(3) 0.5517(3) 0.0724(3) 0.0514(12) Uani 1 1 d . . .
H6A H 0.4067 0.6070 0.0379 0.077 Uiso 1 1 calc R . .
H6B H 0.4454 0.5004 0.0442 0.077 Uiso 1 1 calc R . .
H6C H 0.4871 0.5683 0.1198 0.077 Uiso 1 1 calc R . .
C7 C 0.1631(4) 0.1367(3) 0.1606(3) 0.0441(12) Uani 1 1 d . . .
C8 C 0.0729(4) 0.1805(3) 0.1349(3) 0.0438(12) Uani 1 1 d . . .
C9 C 0.1778(4) 0.0280(3) 0.1599(3) 0.0707(16) Uani 1 1 d . . .
H9A H 0.1130 -0.0031 0.1374 0.106 Uiso 1 1 calc R . .
H9B H 0.2145 0.0056 0.2140 0.106 Uiso 1 1 calc R . .
H9C H 0.2153 0.0130 0.1276 0.106 Uiso 1 1 calc R . .
C10 C -0.0282(4) 0.1292(4) 0.0997(3) 0.0712(16) Uani 1 1 d . . .
H10A H -0.0172 0.0611 0.0982 0.107 Uiso 1 1 calc R . .
H10B H -0.0660 0.1522 0.0459 0.107 Uiso 1 1 calc R . .
H10C H -0.0653 0.1417 0.1326 0.107 Uiso 1 1 calc R . .
C11 C 0.5226(3) 0.6558(3) 0.3817(3) 0.0509(13) Uani 1 1 d . . .
H11A H 0.5649 0.7003 0.3675 0.061 Uiso 1 1 calc R . .
H11B H 0.5433 0.6588 0.4398 0.061 Uiso 1 1 calc R . .
C12 C 0.5421(4) 0.5547(3) 0.3594(3) 0.0681(15) Uani 1 1 d . . .
H12A H 0.6127 0.5398 0.3867 0.102 Uiso 1 1 calc R . .
H12B H 0.5231 0.5509 0.3021 0.102 Uiso 1 1 calc R . .
H12C H 0.5030 0.5094 0.3752 0.102 Uiso 1 1 calc R . .
C13 C 0.4128(3) 0.7904(3) 0.3726(3) 0.0507(13) Uani 1 1 d . . .
H13A H 0.4614 0.8289 0.3606 0.061 Uiso 1 1 calc R . .
H13B H 0.4355 0.7877 0.4308 0.061 Uiso 1 1 calc R . .
C14 C 0.3113(4) 0.8411(4) 0.3382(3) 0.0745(16) Uani 1 1 d . . .
H14A H 0.3180 0.9047 0.3607 0.112 Uiso 1 1 calc R . .
H14B H 0.2630 0.8052 0.3515 0.112 Uiso 1 1 calc R . .
H14C H 0.2885 0.8454 0.2806 0.112 Uiso 1 1 calc R . .
C15 C 0.3429(3) 0.6243(3) 0.3619(3) 0.0541(12) Uani 1 1 d . . .
H15A H 0.3448 0.5609 0.3400 0.065 Uiso 1 1 calc R . .
H15B H 0.2745 0.6488 0.3349 0.065 Uiso 1 1 calc R . .
C16 C 0.3656(4) 0.6136(4) 0.4514(3) 0.0739(16) Uani 1 1 d . . .
H16A H 0.3167 0.5714 0.4581 0.111 Uiso 1 1 calc R . .
H16B H 0.3623 0.6756 0.4738 0.111 Uiso 1 1 calc R . .
H16C H 0.4321 0.5870 0.4787 0.111 Uiso 1 1 calc R . .
C17 C 0.3779(3) 0.6872(3) 0.2508(3) 0.0514(13) Uani 1 1 d . . .
H17A H 0.3824 0.6212 0.2345 0.062 Uiso 1 1 calc R . .
H17B H 0.3071 0.7055 0.2272 0.062 Uiso 1 1 calc R . .
C18 C 0.4350(4) 0.7511(4) 0.2156(3) 0.0612(14) Uani 1 1 d . . .
H18A H 0.4073 0.7441 0.1580 0.092 Uiso 1 1 calc R . .
H18B H 0.5051 0.7328 0.2373 0.092 Uiso 1 1 calc R . .
H18C H 0.4291 0.8171 0.2293 0.092 Uiso 1 1 calc R . .
C19 C 0.2099(3) 0.1912(3) 0.3688(3) 0.0486(12) Uani 1 1 d . . .
H19A H 0.2271 0.2564 0.3593 0.058 Uiso 1 1 calc R . .
H19B H 0.1825 0.1585 0.3171 0.058 Uiso 1 1 calc R . .
C20 C 0.3055(3) 0.1404(4) 0.4223(3) 0.0701(16) Uani 1 1 d . . .
H20A H 0.3528 0.1408 0.3969 0.105 Uiso 1 1 calc R . .
H20B H 0.2900 0.0750 0.4306 0.105 Uiso 1 1 calc R . .
H20C H 0.3344 0.1729 0.4733 0.105 Uiso 1 1 calc R . .
C21 C 0.0406(4) 0.2484(3) 0.3375(3) 0.0621(15) Uani 1 1 d . . .
H21A H 0.0164 0.2101 0.2885 0.075 Uiso 1 1 calc R . .
H21B H 0.0643 0.3095 0.3254 0.075 Uiso 1 1 calc R . .
C22 C -0.0473(4) 0.2675(4) 0.3626(4) 0.094(2) Uani 1 1 d . . .
H22A H -0.1004 0.3005 0.3198 0.141 Uiso 1 1 calc R . .
H22B H -0.0244 0.3066 0.4103 0.141 Uiso 1 1 calc R . .
H22C H -0.0725 0.2073 0.3733 0.141 Uiso 1 1 calc R . .
C23 C 0.0991(4) 0.0980(4) 0.4184(3) 0.0644(15) Uani 1 1 d . . .
H23A H 0.1554 0.0706 0.4635 0.077 Uiso 1 1 calc R . .
H23B H 0.0428 0.1043 0.4347 0.077 Uiso 1 1 calc R . .
C24 C 0.0699(4) 0.0298(4) 0.3494(4) 0.089(2) Uani 1 1 d . . .
H24A H 0.0511 -0.0310 0.3649 0.133 Uiso 1 1 calc R . .
H24B H 0.1261 0.0206 0.3342 0.133 Uiso 1 1 calc R . .
H24C H 0.0136 0.0557 0.3045 0.133 Uiso 1 1 calc R . .
C25 C 0.1672(4) 0.2510(4) 0.4812(3) 0.0674(16) Uani 1 1 d . . .
H25A H 0.1146 0.2511 0.5020 0.081 Uiso 1 1 calc R . .
H25B H 0.2248 0.2166 0.5196 0.081 Uiso 1 1 calc R . .
C26 C 0.1986(5) 0.3546(4) 0.4760(3) 0.0866(19) Uani 1 1 d . . .
H26A H 0.2217 0.3838 0.5284 0.130 Uiso 1 1 calc R . .
H26B H 0.1417 0.3899 0.4392 0.130 Uiso 1 1 calc R . .
H26C H 0.2521 0.3554 0.4570 0.130 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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 Mo1 C1 72.25(19) . . yes
C2 Mo1 S2 129.94(13) . . yes
C1 Mo1 S2 84.84(13) . . yes
C2 Mo1 S4 82.95(13) . . yes
C1 Mo1 S4 129.08(13) . . yes
S2 Mo1 S4 141.69(4) . . yes
C2 Mo1 S1 80.71(13) . . yes
C1 Mo1 S1 127.69(13) . . yes
S2 Mo1 S1 79.42(4) . . yes
S4 Mo1 S1 89.24(4) . . yes
C2 Mo1 S3 126.40(13) . . yes
C1 Mo1 S3 80.58(14) . . yes
S2 Mo1 S3 91.02(4) . . yes
S4 Mo1 S3 79.72(4) . . yes
S1 Mo1 S3 148.38(4) . . yes
C3 S1 Mo1 109.22(14) . . yes
C4 S2 Mo1 109.51(14) . . yes
C7 S3 Mo1 108.61(16) . . yes
C8 S4 Mo1 109.43(17) . . yes
C13 N1 C15 111.3(4) . . yes
C13 N1 C17 111.9(3) . . yes
C15 N1 C17 106.1(3) . . yes
C13 N1 C11 105.5(3) . . yes
C15 N1 C11 111.6(3) . . yes
C17 N1 C11 110.5(3) . . yes
C23 N2 C19 111.3(4) . . yes
C23 N2 C21 111.7(3) . . yes
C19 N2 C21 105.6(3) . . yes
C23 N2 C25 106.7(4) . . yes
C19 N2 C25 110.2(4) . . yes
C21 N2 C25 111.4(4) . . yes
O1 C1 Mo1 176.1(4) . . yes
O1 C1 C2 123.2(4) . . yes
Mo1 C1 C2 53.60(16) . . yes
O2 C2 Mo1 178.0(4) . . yes
O2 C2 C1 124.1(3) . . yes
Mo1 C2 C1 54.16(17) . . yes
C4 C3 C5 125.5(4) . . yes
C4 C3 S1 120.9(3) . . yes
C5 C3 S1 113.5(3) . . yes
C3 C4 C6 125.8(4) . . yes
C3 C4 S2 120.8(3) . . yes
C6 C4 S2 113.3(3) . . yes
C8 C7 C9 124.5(4) . . yes
C8 C7 S3 121.4(3) . . yes
C9 C7 S3 114.1(4) . . yes
C7 C8 C10 124.7(4) . . yes
C7 C8 S4 120.8(3) . . yes
C10 C8 S4 114.5(4) . . yes
C12 C11 N1 115.2(4) . . yes
N1 C13 C14 115.2(4) . . yes
N1 C15 C16 115.6(4) . . yes
C18 C17 N1 115.8(3) . . yes
N2 C19 C20 115.2(4) . . yes
N2 C21 C22 113.4(4) . . yes
C24 C23 N2 114.8(4) . . yes
C26 C25 N2 114.6(4) . . 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
Mo1 C2 1.911(5) . yes
Mo1 C1 1.925(5) . yes
Mo1 S2 2.4503(11) . yes
Mo1 S4 2.4540(11) . yes
Mo1 S1 2.4588(11) . yes
Mo1 S3 2.4662(12) . yes
S1 C3 1.761(4) . yes
S2 C4 1.762(4) . yes
S3 C7 1.758(5) . yes
S4 C8 1.751(5) . yes
O1 C1 1.186(5) . yes
O2 C2 1.171(5) . yes
N1 C13 1.506(5) . yes
N1 C15 1.511(5) . yes
N1 C17 1.514(5) . yes
N1 C11 1.520(5) . yes
N2 C23 1.498(5) . yes
N2 C19 1.505(5) . yes
N2 C21 1.517(5) . yes
N2 C25 1.522(6) . yes
C1 C2 2.262(7) . yes
C3 C4 1.330(5) . yes
C3 C5 1.518(5) . yes
C4 C6 1.513(5) . yes
C7 C8 1.339(6) . yes
C7 C9 1.524(6) . yes
C8 C10 1.516(6) . yes
C11 C12 1.516(6) . yes
C13 C14 1.516(6) . yes
C15 C16 1.523(6) . yes
C17 C18 1.510(6) . yes
C19 C20 1.507(6) . yes
C21 C22 1.527(7) . yes
C23 C24 1.486(7) . yes
C25 C26 1.520(7) . yes
