#------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/01/4300121.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_4300121
loop_
_publ_author_name
'Booyong S. Lim'
'James P. Donahue'
'R. H. Holm'
_publ_contact_author             R.H.Holm
_publ_contact_author_address
;
   R.H.Holm
   Dept. of Chemistry and Chemical Biology 
   Harvard University 
   Cambridge, MA 02138
   USA
;
_publ_contact_author_email       holm@chemistry.harvard.edu
_publ_section_title
;
Synthesis and Structures of Bis(dithiolene)molybdenum Complexes Related to
the Active Sites of the DMSO Reductase Enzyme Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              263
_journal_page_last               273
_journal_paper_doi               10.1021/ic9908672
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C22 H41 Mo N2 S6'
_chemical_formula_weight         621.87
_chemical_name_systematic
; 
 [Mo(S2C2Me2)3](Et4N)(MeCN)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 105.347(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6185(14)
_cell_length_b                   24.159(3)
_cell_length_c                   13.256(2)
_cell_measurement_temperature    213(2)
_cell_volume                     2970.5(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12646
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.877
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       Thin_Plate
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3881
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.027
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_obs          0.0438
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0731P)²+2.1444P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1319
_refine_ls_wR_factor_obs         0.1161
_reflns_number_observed          2737
_reflns_number_total             3885
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+2.1444P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+2.1444P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2970.4(7)
_cod_database_code               4300121
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo -0.48801(5) 0.34443(2) 0.59700(4) 0.0399(2) Uani 1 d . .
S1 S -0.7260(2) 0.36372(8) 0.60790(14) 0.0587(5) Uani 1 d . .
S2 S -0.4380(2) 0.37185(8) 0.77504(13) 0.0560(5) Uani 1 d . .
S3 S -0.6050(2) 0.26972(8) 0.4918(2) 0.0663(6) Uani 1 d . .
S4 S -0.3172(2) 0.27362(8) 0.6624(2) 0.0625(5) Uani 1 d . .
S5 S -0.5630(2) 0.39493(8) 0.43814(14) 0.0587(5) Uani 1 d . .
S6 S -0.2762(2) 0.39691(9) 0.6073(2) 0.0650(6) Uani 1 d . .
N1 N -0.1748(5) 0.3070(2) 0.3145(4) 0.0456(13) Uani 1 d . .
C3 C -0.5005(8) 0.2107(3) 0.5208(6) 0.058(2) Uani 1 d . .
C4 C -0.3721(8) 0.2127(3) 0.5956(6) 0.055(2) Uani 1 d . .
C9 C -0.5580(10) 0.1597(3) 0.4579(7) 0.090(3) Uani 1 d . .
H3A H -0.6496(10) 0.1679(3) 0.4101(7) 0.135 Uiso 1 calc R .
H3B H -0.5693(10) 0.1305(3) 0.5042(7) 0.135 Uiso 1 calc R .
H3C H -0.4915(10) 0.1482(3) 0.4192(7) 0.135 Uiso 1 calc R .
C10 C -0.2734(9) 0.1636(3) 0.6266(7) 0.080(2) Uani 1 d . .
H4A H -0.1896(9) 0.1744(3) 0.6804(7) 0.121 Uiso 1 calc R .
H4B H -0.2446(9) 0.1505(3) 0.5669(7) 0.121 Uiso 1 calc R .
H4C H -0.3232(9) 0.1346(3) 0.6524(7) 0.121 Uiso 1 calc R .
C1 C -0.7208(7) 0.3912(3) 0.7294(5) 0.054(2) Uani 1 d . .
C2 C -0.5935(7) 0.3953(3) 0.8026(5) 0.051(2) Uani 1 d . .
C7 C -0.8636(8) 0.4104(4) 0.7436(7) 0.089(3) Uani 1 d . .
H7A H -0.9384(8) 0.4031(4) 0.6810(7) 0.134 Uiso 1 calc R .
H7B H -0.8593(8) 0.4495(4) 0.7578(7) 0.134 Uiso 1 calc R .
H7C H -0.8841(8) 0.3910(4) 0.8012(7) 0.134 Uiso 1 calc R .
C8 C -0.5764(9) 0.4202(3) 0.9093(6) 0.082(2) Uani 1 d . .
H8A H -0.4769(9) 0.4188(3) 0.9480(6) 0.123 Uiso 1 calc R .
H8B H -0.6334(9) 0.3997(3) 0.9459(6) 0.123 Uiso 1 calc R .
H8C H -0.6082(9) 0.4580(3) 0.9021(6) 0.123 Uiso 1 calc R .
C5 C -0.4286(7) 0.4412(3) 0.4297(5) 0.049(2) Uani 1 d . .
C6 C -0.3023(7) 0.4419(3) 0.5043(5) 0.052(2) Uani 1 d . .
C11 C -0.4650(8) 0.4783(3) 0.3350(6) 0.075(2) Uani 1 d . .
H11A H -0.5607(8) 0.4701(3) 0.2934(6) 0.113 Uiso 1 calc R .
H11B H -0.3975(8) 0.4721(3) 0.2943(6) 0.113 Uiso 1 calc R .
H11C H -0.4601(8) 0.5162(3) 0.3571(6) 0.113 Uiso 1 calc R .
C12 C -0.1812(7) 0.4819(3) 0.5047(7) 0.076(2) Uani 1 d . .
H12A H -0.1020(7) 0.4750(3) 0.5648(7) 0.114 Uiso 1 calc R .
H12B H -0.2147(7) 0.5191(3) 0.5073(7) 0.114 Uiso 1 calc R .
H12C H -0.1500(7) 0.4769(3) 0.4422(7) 0.114 Uiso 1 calc R .
C13 C -0.3107(9) 0.2988(4) 0.3438(7) 0.063(3) Uani 0.687(5) d P 1
H13A H -0.3721(9) 0.3309(4) 0.3230(7) 0.076 Uiso 0.687(5) calc PR 1
H13B H -0.2903(9) 0.2950(4) 0.4192(7) 0.076 Uiso 0.687(5) calc PR 1
C13A C -0.2431(9) 0.2550(4) 0.2539(7) 0.063(3) Uani 0.313(5) d PR 2
H13A H -0.1785(9) 0.2236(4) 0.2728(7) 0.076 Uiso 0.313(5) d PR 2
H13B H -0.2632(9) 0.2610(4) 0.1791(7) 0.076 Uiso 0.313(5) d PR 2
C14 C -0.3943(9) 0.2438(4) 0.2879(8) 0.105(3) Uani 1 d . .
H14A H -0.4823(9) 0.2389(4) 0.3082(8) 0.158 Uiso 0.50 d PR 1
H14B H -0.4160(9) 0.2479(4) 0.2134(8) 0.158 Uiso 0.50 d PR 1
H14C H -0.3337(9) 0.2120(4) 0.3091(8) 0.158 Uiso 0.50 d PR 1
H14D H -0.4439(9) 0.2117(4) 0.2533(8) 0.158 Uiso 0.50 d PR 2
H14E H -0.3713(9) 0.2385(4) 0.3623(8) 0.158 Uiso 0.50 d PR 2
H14F H -0.4551(9) 0.2757(4) 0.2691(8) 0.158 Uiso 0.50 d PR 2
C15 C -0.1018(10) 0.3583(4) 0.3661(8) 0.066(3) Uani 0.687(5) d P 1
H15A H -0.1695(10) 0.3888(4) 0.3480(8) 0.079 Uiso 0.687(5) calc PR 1
H15B H -0.0802(10) 0.3532(4) 0.4413(8) 0.079 Uiso 0.687(5) calc PR 1
C15A C -0.0449(10) 0.3203(4) 0.2895(8) 0.066(3) Uani 0.313(5) d PR 2
H15A H -0.0653(10) 0.3236(4) 0.2140(8) 0.079 Uiso 0.313(5) d PR 2
H15B H 0.0213(10) 0.2895(4) 0.3103(8) 0.079 Uiso 0.313(5) d PR 2
C16 C 0.0328(8) 0.3746(4) 0.3399(7) 0.090(3) Uani 1 d . .
H16A H 0.0694(8) 0.4079(4) 0.3770(7) 0.135 Uiso 0.50 d PR 1
H16B H 0.1030(8) 0.3457(4) 0.3600(7) 0.135 Uiso 0.50 d PR 1
H16C H 0.0133(8) 0.3810(4) 0.2660(7) 0.135 Uiso 0.50 d PR 1
H16D H 0.1185(8) 0.3796(4) 0.3168(7) 0.135 Uiso 0.50 d PR 2
H16E H -0.0293(8) 0.4061(4) 0.3194(7) 0.135 Uiso 0.50 d PR 2
H16F H 0.0584(8) 0.3710(4) 0.4147(7) 0.135 Uiso 0.50 d PR 2
C17 C -0.1987(10) 0.3103(5) 0.1970(7) 0.068(3) Uani 0.687(5) d P 1
H17A H -0.2407(10) 0.2761(5) 0.1643(7) 0.081 Uiso 0.687(5) calc PR 1
H17B H -0.1077(10) 0.3162(5) 0.1800(7) 0.081 Uiso 0.687(5) calc PR 1
C17A C -0.2878(10) 0.3546(5) 0.2880(7) 0.068(3) Uani 0.313(5) d PR 2
H17A H -0.2526(10) 0.3883(5) 0.3259(7) 0.081 Uiso 0.313(5) d PR 2
H17B H -0.3779(10) 0.3438(5) 0.3022(7) 0.081 Uiso 0.313(5) d PR 2
C18 C -0.3072(11) 0.3618(4) 0.1552(8) 0.139(5) Uani 1 d . .
H18A H -0.3249(11) 0.3646(4) 0.0806(8) 0.209 Uiso 0.50 d PR 1
H18B H -0.3968(11) 0.3561(4) 0.1727(8) 0.209 Uiso 0.50 d PR 1
H18C H -0.2631(11) 0.3954(4) 0.1872(8) 0.209 Uiso 0.50 d PR 1
H18D H -0.3759(11) 0.3903(4) 0.1264(8) 0.209 Uiso 0.50 d PR 2
H18E H -0.2150(11) 0.3716(4) 0.1452(8) 0.209 Uiso 0.50 d PR 2
H18F H -0.3387(11) 0.3274(4) 0.1205(8) 0.209 Uiso 0.50 d PR 2
C19 C -0.0718(10) 0.2577(4) 0.3452(8) 0.065(3) Uani 0.687(5) d P 1
H19A H 0.0166(10) 0.2650(4) 0.3254(8) 0.078 Uiso 0.687(5) calc PR 1
H19B H -0.1159(10) 0.2247(4) 0.3086(8) 0.078 Uiso 0.687(5) calc PR 1
C19A C -0.1573(10) 0.2976(4) 0.4340(8) 0.065(3) Uani 0.313(5) d PR 2
H19A H -0.2483(10) 0.2862(4) 0.4460(8) 0.078 Uiso 0.313(5) d PR 2
H19B H -0.1252(10) 0.3312(4) 0.4733(8) 0.078 Uiso 0.313(5) d PR 2
C20 C -0.0363(10) 0.2480(4) 0.4682(7) 0.104(3) Uani 1 d . .
H20A H 0.0273(10) 0.2168(4) 0.4864(7) 0.156 Uiso 0.50 d PR 1
H20B H 0.0098(10) 0.2803(4) 0.5041(7) 0.156 Uiso 0.50 d PR 1
H20C H -0.1235(10) 0.2408(4) 0.4882(7) 0.156 Uiso 0.50 d PR 1
H20D H -0.0213(10) 0.2400(4) 0.5412(7) 0.156 Uiso 0.50 d PR 2
H20E H -0.0693(10) 0.2153(4) 0.4279(7) 0.156 Uiso 0.50 d PR 2
H20F H 0.0527(10) 0.2601(4) 0.4556(7) 0.156 Uiso 0.50 d PR 2
C21 C 0.3362(13) 0.0082(5) 0.3563(14) 0.203(6) Uani 1 d DU .
H21A H 0.2814(13) -0.0073(5) 0.2912(14) 0.304 Uiso 1 d R .
H21B H 0.3381(13) 0.0478(5) 0.3505(14) 0.304 Uiso 1 d R .
H21C H 0.2924(13) -0.0018(5) 0.4109(14) 0.304 Uiso 1 d R .
C22 C 0.4824(13) -0.0130(5) 0.3800(15) 0.203(6) Uani 1 d DU .
N2 N 0.5971(14) -0.0292(6) 0.4115(17) 0.517(27) Uani 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'
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
S4 Mo1 S6 82.13(7) . . ?
S4 Mo1 S3 80.86(7) . . ?
S6 Mo1 S3 134.94(8) . . ?
S4 Mo1 S5 135.49(7) . . ?
S6 Mo1 S5 80.29(6) . . ?
S3 Mo1 S5 83.34(7) . . ?
S4 Mo1 S2 84.24(7) . . ?
S6 Mo1 S2 81.28(7) . . ?
S3 Mo1 S2 137.36(7) . . ?
S5 Mo1 S2 132.23(7) . . ?
S4 Mo1 S1 134.78(7) . . ?
S6 Mo1 S1 135.85(8) . . ?
S3 Mo1 S1 82.56(7) . . ?
S5 Mo1 S1 83.22(6) . . ?
S2 Mo1 S1 80.21(6) . . ?
C1 S1 Mo1 109.9(2) . . ?
C2 S2 Mo1 110.0(2) . . ?
C3 S3 Mo1 109.8(3) . . ?
C4 S4 Mo1 109.8(3) . . ?
C5 S5 Mo1 109.4(2) . . ?
C6 S6 Mo1 110.5(2) . . ?
C13 N1 C15 109.4(6) . . ?
C13 N1 C17 112.0(6) . . ?
C15 N1 C17 110.5(7) . . ?
C13 N1 C19 112.5(6) . . ?
C15 N1 C19 109.2(6) . . ?
C17 N1 C19 103.0(6) . . ?
C15A N1 C13A 110.2(6) . . ?
C15A N1 C17A 112.7(6) . . ?
C13A N1 C17A 108.0(6) . . ?
C15A N1 C19A 114.0(6) . . ?
C13A N1 C19A 109.1(6) . . ?
C17A N1 C19A 102.5(5) . . ?
C4 C3 C9 124.0(7) . . ?
C4 C3 S3 119.6(5) . . ?
C9 C3 S3 116.4(6) . . ?
C3 C4 C10 123.6(7) . . ?
C3 C4 S4 119.9(5) . . ?
C10 C4 S4 116.5(6) . . ?
C2 C1 C7 124.7(7) . . ?
C2 C1 S1 119.6(5) . . ?
C7 C1 S1 115.6(6) . . ?
C1 C2 C8 123.9(6) . . ?
C1 C2 S2 119.7(5) . . ?
C8 C2 S2 116.4(5) . . ?
C6 C5 C11 124.7(6) . . ?
C6 C5 S5 120.2(5) . . ?
C11 C5 S5 115.1(5) . . ?
C5 C6 C12 123.7(6) . . ?
C5 C6 S6 119.4(5) . . ?
C12 C6 S6 116.9(5) . . ?
N1 C13 C14 110.9(7) . . ?
N1 C13A C14 106.0(6) . . ?
C16 C15 N1 116.5(8) . . ?
N1 C15A C16 116.2(7) . . ?
N1 C17 C18 107.5(8) . . ?
N1 C17A C18 100.7(6) . . ?
N1 C19 C20 109.5(7) . . ?
N1 C19A C20 105.2(6) . . ?
N2 C22 C21 171.4(22) . . ?
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 S4 2.371(2) . ?
Mo1 S6 2.372(2) . ?
Mo1 S3 2.375(2) . ?
Mo1 S5 2.375(2) . ?
Mo1 S2 2.375(2) . ?
Mo1 S1 2.378(2) . ?
S1 C1 1.730(7) . ?
S2 C2 1.727(7) . ?
S3 C3 1.728(7) . ?
S4 C4 1.726(7) . ?
S5 C5 1.734(6) . ?
S6 C6 1.711(7) . ?
N1 C15A 1.413(11) . ?
N1 C13 1.472(10) . ?
N1 C15 1.499(10) . ?
N1 C17 1.515(10) . ?
N1 C19 1.533(10) . ?
N1 C13A 1.540(11) . ?
N1 C17A 1.558(12) . ?
N1 C19A 1.565(11) . ?
C3 C4 1.364(9) . ?
C3 C9 1.510(9) . ?
C4 C10 1.508(9) . ?
C1 C2 1.350(9) . ?
C1 C7 1.509(9) . ?
C2 C8 1.505(9) . ?
C5 C6 1.348(9) . ?
C5 C11 1.506(9) . ?
C6 C12 1.512(9) . ?
C13 C14 1.627(12) . ?
C13A C14 1.655(11) . ?
C15 C16 1.480(12) . ?
C15A C16 1.570(12) . ?
C17 C18 1.625(13) . ?
C17A C18 1.729(14) . ?
C19 C20 1.592(13) . ?
C19A C20 1.648(12) . ?
C21 C22 1.4505(11) . ?
C22 N2 1.1410(11) . ?
