#------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/01/4300133.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_4300133
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            'C70 H78 Mo2 N2 O2 P2 S10'
_chemical_formula_weight         1553.76
_chemical_name_systematic
; 
 [Mo2(??S)2(S2C2Me2)4](PPh4)2(2DMF) 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 107.9420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.9620(3)
_cell_length_b                   16.0040(3)
_cell_length_c                   15.915
_cell_measurement_temperature    213(2)
_cell_volume                     3625.55(10)
_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  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23596
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.723
_exptl_crystal_colour            'Dark blue-green'
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       plate
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_obs   1.248
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         8689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_restrained_S_obs      1.248
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         0.089
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0642
_refine_ls_wR_factor_obs         0.0588
_reflns_number_observed          5175
_reflns_number_total             8689
_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^)+(0.0150P)^2^+0.0000P] 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^)+(0.0150P)^2^+0.0000P] 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        3625.48(10)
_cod_database_code               4300133
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.59458(2) 0.957109(14) 0.524996(15) 0.02194(7) Uani 1 d . .
S1 S 0.54929(5) 0.82085(4) 0.46216(5) 0.0294(2) Uani 1 d . .
S2 S 0.70943(5) 0.93424(4) 0.44613(5) 0.0305(2) Uani 1 d . .
S3 S 0.68561(6) 0.88597(5) 0.66058(5) 0.0347(2) Uani 1 d . .
S4 S 0.69482(5) 1.06837(4) 0.60083(5) 0.0326(2) Uani 1 d . .
S5 S 0.46137(5) 0.92750(4) 0.56620(5) 0.0269(2) Uani 1 d . .
P1 P 0.27379(5) 0.58940(4) 0.45333(5) 0.0247(2) Uani 1 d . .
O1 O 0.9892(2) 0.83374(14) 0.67633(14) 0.0511(6) Uani 1 d . .
N1 N 0.9988(2) 0.9666(2) 0.6295(2) 0.0482(7) Uani 1 d . .
C1 C 0.6259(2) 0.7847(2) 0.4070(2) 0.0304(7) Uani 1 d . .
C2 C 0.6956(2) 0.8351(2) 0.4003(2) 0.0281(7) Uani 1 d . .
C3 C 0.7710(2) 0.9531(2) 0.7243(2) 0.0333(7) Uani 1 d . .
C4 C 0.7748(2) 1.0322(2) 0.6976(2) 0.0335(7) Uani 1 d . .
C5 C 0.6063(3) 0.6979(2) 0.3670(3) 0.0445(10) Uani 1 d . .
H5A H 0.5798(27) 0.6995(23) 0.3085(26) 0.095(16) Uiso 1 d . .
H5B H 0.5661(24) 0.6648(20) 0.3933(21) 0.066(11) Uiso 1 d . .
H5C H 0.6628(27) 0.6679(23) 0.3816(24) 0.089(15) Uiso 1 d . .
C6 C 0.7642(3) 0.8112(3) 0.3502(3) 0.0525(11) Uani 1 d . .
H6A H 0.7349(27) 0.7778(24) 0.2981(26) 0.098(15) Uiso 1 d . .
H6B H 0.8040(36) 0.8529(29) 0.3477(31) 0.140(22) Uiso 1 d . .
H6C H 0.8106(41) 0.7790(34) 0.3904(37) 0.184(29) Uiso 1 d . .
C7 C 0.8385(3) 0.9163(3) 0.8075(3) 0.0532(11) Uani 1 d . .
H7A H 0.8786(33) 0.9550(26) 0.8448(30) 0.122(19) Uiso 1 d . .
H7B H 0.8824(34) 0.8865(28) 0.8000(30) 0.123(21) Uiso 1 d . .
H7C H 0.8128(31) 0.8927(27) 0.8400(30) 0.118(20) Uiso 1 d . .
C8 C 0.8469(3) 1.0961(3) 0.7498(3) 0.0609(12) Uani 1 d . .
H8A H 0.9045(30) 1.0824(24) 0.7540(27) 0.094(17) Uiso 1 d . .
H8B H 0.8502(33) 1.0951(27) 0.8091(32) 0.130(20) Uiso 1 d . .
H8C H 0.8379(30) 1.1565(27) 0.7261(27) 0.118(18) Uiso 1 d . .
C9 C 0.3688(2) 0.5896(2) 0.5554(2) 0.0252(6) Uani 1 d . .
C10 C 0.3628(2) 0.5360(2) 0.6237(2) 0.0314(7) Uani 1 d . .
H10A H 0.3155(19) 0.4939(16) 0.6154(17) 0.036(9) Uiso 1 d . .
C11 C 0.4314(2) 0.5398(2) 0.7051(2) 0.0396(8) Uani 1 d . .
H11A H 0.4288(20) 0.5074(17) 0.7456(18) 0.037(9) Uiso 1 d . .
C12 C 0.5038(3) 0.5962(2) 0.7190(2) 0.0438(9) Uani 1 d . .
H12A H 0.5478(21) 0.5998(18) 0.7705(20) 0.049(10) Uiso 1 d . .
C13 C 0.5098(2) 0.6491(2) 0.6521(2) 0.0417(9) Uani 1 d . .
H13A H 0.5579(21) 0.6855(17) 0.6659(19) 0.046(10) Uiso 1 d . .
C14 C 0.4423(2) 0.6458(2) 0.5703(2) 0.0327(8) Uani 1 d . .
H14A H 0.4481(21) 0.6799(17) 0.5294(19) 0.046(10) Uiso 1 d . .
C15 C 0.1826(2) 0.6578(2) 0.4642(2) 0.0270(7) Uani 1 d . .
C16 C 0.1085(2) 0.6802(2) 0.3894(2) 0.0342(8) Uani 1 d . .
H16A H 0.1090(18) 0.6641(15) 0.3355(16) 0.027(8) Uiso 1 d . .
C17 C 0.0357(2) 0.7287(2) 0.3985(2) 0.0409(8) Uani 1 d . .
H17A H -0.0132(18) 0.7416(15) 0.3471(17) 0.030(8) Uiso 1 d . .
C18 C 0.0356(2) 0.7556(2) 0.4805(2) 0.0439(9) Uani 1 d . .
H18A H -0.0148(22) 0.7882(18) 0.4877(19) 0.055(10) Uiso 1 d . .
C19 C 0.1090(3) 0.7353(2) 0.5547(2) 0.0447(9) Uani 1 d . .
H19A H 0.1082(21) 0.7525(17) 0.6079(19) 0.047(10) Uiso 1 d . .
C20 C 0.1829(2) 0.6865(2) 0.5469(2) 0.0385(8) Uani 1 d . .
H20A H 0.2314(21) 0.6693(18) 0.5952(19) 0.055(11) Uiso 1 d . .
C21 C 0.3104(2) 0.6259(2) 0.3622(2) 0.0243(6) Uani 1 d . .
C22 C 0.3215(2) 0.7117(2) 0.3532(2) 0.0307(7) Uani 1 d . .
H22A H 0.3129(18) 0.7516(15) 0.3958(17) 0.034(8) Uiso 1 d . .
C23 C 0.3486(2) 0.7415(2) 0.2827(2) 0.0367(8) Uani 1 d . .
H23A H 0.3529(19) 0.7988(16) 0.2779(17) 0.034(8) Uiso 1 d . .
C24 C 0.3624(2) 0.6869(2) 0.2211(2) 0.0376(8) Uani 1 d . .
H24A H 0.3715(19) 0.7073(16) 0.1695(18) 0.043(9) Uiso 1 d . .
C25 C 0.3510(2) 0.6024(2) 0.2291(2) 0.0404(9) Uani 1 d . .
H25A H 0.3521(21) 0.5672(17) 0.1869(19) 0.049(10) Uiso 1 d . .
C26 C 0.3243(2) 0.5714(2) 0.2997(2) 0.0336(8) Uani 1 d . .
H26A H 0.3204(20) 0.5148(17) 0.3031(17) 0.040(9) Uiso 1 d . .
C27 C 0.2296(2) 0.4843(2) 0.4330(2) 0.0286(7) Uani 1 d . .
C28 C 0.2921(3) 0.4197(2) 0.4315(2) 0.0373(8) Uani 1 d . .
H28A H 0.3560(19) 0.4325(15) 0.4446(17) 0.030(8) Uiso 1 d . .
C29 C 0.2604(3) 0.3384(2) 0.4124(2) 0.0501(10) Uani 1 d . .
H29A H 0.2987(22) 0.2983(19) 0.4034(21) 0.059(12) Uiso 1 d . .
C30 C 0.1670(3) 0.3214(2) 0.3960(2) 0.0630(12) Uani 1 d . .
H30A H 0.1470(25) 0.2649(22) 0.3868(22) 0.083(13) Uiso 1 d . .
C31 C 0.1046(3) 0.3835(3) 0.3988(3) 0.0672(13) Uani 1 d . .
H31A H 0.0417(25) 0.3726(21) 0.3897(23) 0.075(13) Uiso 1 d . .
C32 C 0.1357(2) 0.4660(2) 0.4170(2) 0.0467(9) Uani 1 d . .
H32A H 0.0943(19) 0.5088(16) 0.4206(18) 0.037(9) Uiso 1 d . .
C33 C 0.9523(3) 0.8971(2) 0.6367(2) 0.0389(8) Uani 1 d . .
H33A H 0.8854(20) 0.9014(16) 0.6046(17) 0.039(9) Uiso 1 d . .
C34 C 1.1013(3) 0.9710(4) 0.6701(4) 0.0775(15) Uani 1 d . .
H34A H 1.1274(36) 0.9933(30) 0.6234(33) 0.158(23) Uiso 1 d . .
H34B H 1.0972(29) 1.0171(24) 0.7039(27) 0.090(18) Uiso 1 d . .
H34C H 1.1234(29) 0.9112(25) 0.6861(27) 0.108(18) Uiso 1 d . .
C35 C 0.9489(4) 1.0389(3) 0.5842(3) 0.0695(13) Uani 1 d . .
H35A H 0.9773(21) 1.0534(17) 0.5367(20) 0.053(10) Uiso 1 d . .
H35B H 0.9622(33) 1.0848(27) 0.6222(31) 0.128(20) Uiso 1 d . .
H35C H 0.8780(36) 1.0383(32) 0.5577(33) 0.156(24) Uiso 1 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
S5 Mo1 S5 99.30(2) . 3_676 ?
S5 Mo1 S4 117.74(3) . . ?
S5 Mo1 S4 77.00(3) 3_676 . ?
S5 Mo1 S1 77.11(3) . . ?
S5 Mo1 S1 117.15(3) 3_676 . ?
S4 Mo1 S1 158.92(3) . . ?
S5 Mo1 S2 155.53(3) . . ?
S5 Mo1 S2 88.48(2) 3_676 . ?
S4 Mo1 S2 86.57(3) . . ?
S1 Mo1 S2 78.69(2) . . ?
S5 Mo1 S3 87.09(3) . . ?
S5 Mo1 S3 155.45(3) 3_676 . ?
S4 Mo1 S3 79.05(3) . . ?
S1 Mo1 S3 87.35(3) . . ?
S2 Mo1 S3 95.43(3) . . ?
S5 Mo1 Mo1 49.76(2) . 3_676 ?
S5 Mo1 Mo1 49.53(2) 3_676 3_676 ?
S4 Mo1 Mo1 100.65(2) . 3_676 ?
S1 Mo1 Mo1 100.43(2) . 3_676 ?
S2 Mo1 Mo1 132.93(2) . 3_676 ?
S3 Mo1 Mo1 131.64(2) . 3_676 ?
C1 S1 Mo1 111.40(10) . . ?
C2 S2 Mo1 109.94(10) . . ?
C3 S3 Mo1 109.64(10) . . ?
C4 S4 Mo1 110.63(10) . . ?
Mo1 S5 Mo1 80.70(2) . 3_676 ?
C21 P1 C9 112.07(13) . . ?
C21 P1 C15 107.95(12) . . ?
C9 P1 C15 108.91(13) . . ?
C21 P1 C27 110.14(12) . . ?
C9 P1 C27 107.95(13) . . ?
C15 P1 C27 109.80(13) . . ?
C33 N1 C35 120.4(4) . . ?
C33 N1 C34 120.2(4) . . ?
C35 N1 C34 119.3(4) . . ?
C2 C1 C5 124.6(3) . . ?
C2 C1 S1 119.1(2) . . ?
C5 C1 S1 116.3(2) . . ?
C1 C2 C6 123.5(3) . . ?
C1 C2 S2 120.6(2) . . ?
C6 C2 S2 115.9(3) . . ?
C4 C3 C7 124.2(3) . . ?
C4 C3 S3 119.6(2) . . ?
C7 C3 S3 116.2(3) . . ?
C3 C4 C8 123.3(3) . . ?
C3 C4 S4 120.8(2) . . ?
C8 C4 S4 115.9(3) . . ?
C14 C9 C10 119.9(3) . . ?
C14 C9 P1 121.4(2) . . ?
C10 C9 P1 118.4(2) . . ?
C11 C10 C9 119.4(3) . . ?
C12 C11 C10 120.0(3) . . ?
C11 C12 C13 120.8(3) . . ?
C14 C13 C12 120.0(3) . . ?
C13 C14 C9 119.9(3) . . ?
C20 C15 C16 119.3(3) . . ?
C20 C15 P1 120.7(2) . . ?
C16 C15 P1 120.0(2) . . ?
C17 C16 C15 119.9(3) . . ?
C18 C17 C16 120.4(3) . . ?
C17 C18 C19 120.4(3) . . ?
C18 C19 C20 120.0(3) . . ?
C19 C20 C15 119.9(3) . . ?
C26 C21 C22 119.7(3) . . ?
C26 C21 P1 121.7(2) . . ?
C22 C21 P1 118.5(2) . . ?
C23 C22 C21 119.5(3) . . ?
C24 C23 C22 120.3(3) . . ?
C25 C24 C23 120.6(3) . . ?
C24 C25 C26 119.9(3) . . ?
C21 C26 C25 120.0(3) . . ?
C32 C27 C28 119.2(3) . . ?
C32 C27 P1 121.9(3) . . ?
C28 C27 P1 118.9(2) . . ?
C29 C28 C27 120.8(3) . . ?
C30 C29 C28 119.4(4) . . ?
C29 C30 C31 120.9(4) . . ?
C30 C31 C32 120.2(4) . . ?
C27 C32 C31 119.6(4) . . ?
O1 C33 N1 124.4(3) . . ?
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 S5 2.3308(7) . ?
Mo1 S5 2.3387(7) 3_676 ?
Mo1 S4 2.4002(8) . ?
Mo1 S1 2.4077(7) . ?
Mo1 S2 2.4476(7) . ?
Mo1 S3 2.4487(8) . ?
Mo1 Mo1 3.0235(5) 3_676 ?
S1 C1 1.743(3) . ?
S2 C2 1.732(3) . ?
S3 C3 1.737(3) . ?
S4 C4 1.732(3) . ?
S5 Mo1 2.3387(7) 3_676 ?
P1 C21 1.798(3) . ?
P1 C9 1.799(3) . ?
P1 C15 1.799(3) . ?
P1 C27 1.800(3) . ?
O1 C33 1.232(4) . ?
N1 C33 1.335(4) . ?
N1 C35 1.444(5) . ?
N1 C34 1.471(5) . ?
C1 C2 1.347(4) . ?
C1 C5 1.520(4) . ?
C2 C6 1.530(4) . ?
C3 C4 1.342(4) . ?
C3 C7 1.516(4) . ?
C4 C8 1.532(5) . ?
C9 C14 1.384(4) . ?
C9 C10 1.408(4) . ?
C10 C11 1.384(4) . ?
C11 C12 1.375(5) . ?
C12 C13 1.383(5) . ?
C13 C14 1.381(4) . ?
C15 C20 1.393(4) . ?
C15 C16 1.400(4) . ?
C16 C17 1.380(4) . ?
C17 C18 1.374(4) . ?
C18 C19 1.381(5) . ?
C19 C20 1.389(4) . ?
C21 C26 1.386(4) . ?
C21 C22 1.397(4) . ?
C22 C23 1.389(4) . ?
C23 C24 1.376(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.395(4) . ?
C27 C32 1.380(4) . ?
C27 C28 1.399(4) . ?
C28 C29 1.385(4) . ?
C29 C30 1.368(5) . ?
C30 C31 1.374(6) . ?
C31 C32 1.400(5) . ?
