# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

###################################################################
### X-ray Crystallographic Data for 2_CH2Cl2_100K, 3, 4_MeOH_100K
### 4_MeOH_200K, and 5
###################################################################
data_global
loop_
_publ_author_name
_publ_author_email
_publ_author_address
'Brian S. Dolinar' ? ?
'John F. Berry' ? ?

_publ_contact_author_address     ?
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
;
data_2_CH2Cl2_100K
_audit_creation_date             2013-12-18
_audit_creation_method           
;
  Olex2 1.2-alpha
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H16 Mo2 N4 S8, C H2 Cl2'
_chemical_formula_sum            'C17 H18 Cl2 Mo2 N4 S8'
_chemical_formula_weight         797.61
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.322(6)
_cell_length_b                   10.791(4)
_cell_length_c                   16.081(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.44(3)
_cell_angle_gamma                90
_cell_volume                     2730.3(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.91
_cell_measurement_theta_min      2.29
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7348
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0812 before and 0.0623 after correction.
The Ratio of minimum to maximum transmission is 0.7348.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.046
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35363
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.942
_diffrn_reflns_theta_min         1.294
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ ω and 0.5\ φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4343
_reflns_number_total             5323
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5323
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      1.296
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+26.4048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1167
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H15A(0.039) H15B(0.039) H11A(0.024) H11B(0.024) H14A(0.042)
 H14B(0.042) H10A(0.025) H10B(0.025) H2A(0.028) H2B(0.028) H6A(0.03) H6B(0.03)
 H7A(0.031) H7B(0.031) H3A(0.027) H3B(0.027) H1SA(0.036) H1SB(0.036)
 Fixed X: H15A(0.5248) H15B(0.4729) H11A(-0.0675) H11B(-0.0145) H14A(0.3958)
 H14B(0.4426) H10A(0.0827) H10B(0.0315) H2A(0.3271) H2B(0.3887) H6A(0.0965)
 H6B(0.0426) H7A(0.1451) H7B(0.1937) H3A(0.2914) H3B(0.2323) H1SA(0.323)
 H1SB(0.2673)
 Fixed Y: H15A(0.2294) H15B(0.2863) H11A(0.3854) H11B(0.3026) H14A(0.1114)
 H14B(0.0593) H10A(0.4538) H10B(0.5344) H2A(0.0637) H2B(0.0008) H6A(0.4675)
 H6B(0.545) H7A(0.6871) H7B(0.618) H3A(-0.1455) H3B(-0.0876) H1SA(0.6932)
 H1SB(0.8167)
 Fixed Z: H15A(0.089) H15B(-0.0024) H11A(-0.1001) H11B(-0.151) H14A(-0.0289)
 H14B(0.0659) H10A(-0.1341) H10B(-0.0798) H2A(0.4383) H2B(0.3868) H6A(0.3838)
 H6B(0.3017) H7A(0.3205) H7B(0.4086) H3A(0.3348) H3B(0.3908) H1SA(0.141)
 H1SB(0.1161)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo2 Mo 0.17335(4) 0.21367(5) 0.14278(3) 0.01591(14) Uani 1 1 d . . . . .
Mo1 Mo 0.26574(4) 0.35674(5) 0.17543(3) 0.01726(15) Uani 1 1 d . . . . .
S3 S 0.07442(11) 0.29216(15) 0.22438(10) 0.0180(3) Uani 1 1 d . . . . .
S6 S -0.02943(13) 0.15225(18) 0.01218(11) 0.0283(4) Uani 1 1 d . . . . .
S5 S 0.20584(11) 0.49376(17) 0.05003(11) 0.0215(4) Uani 1 1 d . . . . .
S2 S 0.12234(12) -0.07453(17) 0.20192(11) 0.0260(4) Uani 1 1 d . . . . .
S1 S 0.35881(11) 0.26243(17) 0.30832(11) 0.0227(4) Uani 1 1 d . . . . .
S4 S 0.32772(12) 0.60630(18) 0.30664(12) 0.0275(4) Uani 1 1 d . . . . .
S7 S 0.24620(12) 0.08727(17) 0.05471(11) 0.0241(4) Uani 1 1 d . . . . .
S8 S 0.44479(12) 0.4771(2) 0.13233(13) 0.0328(5) Uani 1 1 d . . . . .
N4 N 0.3473(4) 0.2787(6) 0.1048(3) 0.0242(13) Uani 1 1 d . . . . .
N2 N 0.1997(4) 0.4538(5) 0.2551(3) 0.0152(11) Uani 1 1 d . . . . .
N3 N 0.0981(3) 0.3075(5) 0.0288(3) 0.0165(12) Uani 1 1 d . . . . .
C4 C 0.2067(4) -0.0146(6) 0.2677(4) 0.0179(14) Uani 1 1 d . . . . .
C12 C 0.0181(4) 0.2666(6) -0.0193(4) 0.0191(14) Uani 1 1 d . . . . .
N1 N 0.2352(4) 0.1009(5) 0.2527(3) 0.0191(12) Uani 1 1 d . . . . .
C15 C 0.4673(5) 0.2488(8) 0.0520(5) 0.0327(19) Uani 1 1 d . . . . .
H15A H 0.5248 0.2294 0.0890 0.039 Uiso 1 1 calc R U . . .
H15B H 0.4729 0.2863 -0.0024 0.039 Uiso 1 1 calc R U . . .
C11 C -0.0109(4) 0.3497(6) -0.0972(4) 0.0204(14) Uani 1 1 d . . . . .
H11A H -0.0675 0.3854 -0.1001 0.024 Uiso 1 1 calc R U . . .
H11B H -0.0145 0.3026 -0.1510 0.024 Uiso 1 1 calc R U . . .
C14 C 0.4125(5) 0.1312(9) 0.0334(5) 0.035(2) Uani 1 1 d . . . . .
H14A H 0.3958 0.1114 -0.0289 0.042 Uiso 1 1 calc R U . . .
H14B H 0.4426 0.0593 0.0659 0.042 Uiso 1 1 calc R U . . .
C1 C 0.3063(4) 0.1297(6) 0.3135(4) 0.0196(14) Uani 1 1 d . . . . .
C10 C 0.0562(4) 0.4521(6) -0.0855(4) 0.0206(15) Uani 1 1 d . . . . .
H10A H 0.0827 0.4538 -0.1341 0.025 Uiso 1 1 calc R U . . .
H10B H 0.0315 0.5344 -0.0798 0.025 Uiso 1 1 calc R U . . .
C2 C 0.3305(5) 0.0320(7) 0.3816(4) 0.0235(15) Uani 1 1 d . . . . .
H2A H 0.3271 0.0637 0.4383 0.028 Uiso 1 1 calc R U . . .
H2B H 0.3887 0.0008 0.3868 0.028 Uiso 1 1 calc R U . . .
C6 C 0.0989(5) 0.5086(7) 0.3295(4) 0.0246(16) Uani 1 1 d . . . . .
H6A H 0.0965 0.4675 0.3838 0.030 Uiso 1 1 calc R U . . .
H6B H 0.0426 0.5450 0.3017 0.030 Uiso 1 1 calc R U . . .
C5 C 0.1259(4) 0.4189(6) 0.2698(4) 0.0177(14) Uani 1 1 d . . . . .
C8 C 0.2325(5) 0.5573(6) 0.3029(4) 0.0209(15) Uani 1 1 d . . . . .
C13 C 0.3360(5) 0.1680(7) 0.0649(4) 0.0253(16) Uani 1 1 d . . . . .
C7 C 0.1681(5) 0.6067(7) 0.3460(5) 0.0262(16) Uani 1 1 d . . . . .
H7A H 0.1451 0.6871 0.3205 0.031 Uiso 1 1 calc R U . . .
H7B H 0.1937 0.6180 0.4086 0.031 Uiso 1 1 calc R U . . .
C3 C 0.2642(5) -0.0686(7) 0.3480(4) 0.0224(15) Uani 1 1 d . . . . .
H3A H 0.2914 -0.1455 0.3348 0.027 Uiso 1 1 calc R U . . .
H3B H 0.2323 -0.0876 0.3908 0.027 Uiso 1 1 calc R U . . .
C9 C 0.1196(4) 0.4137(6) -0.0023(4) 0.0163(13) Uani 1 1 d . . . . .
C16 C 0.4211(5) 0.3365(8) 0.0982(4) 0.0281(17) Uani 1 1 d . . . . .
Cl2S Cl 0.34873(13) 0.7849(2) 0.02201(12) 0.0345(4) Uani 1 1 d . . . . .
Cl1S Cl 0.40076(14) 0.8641(2) 0.20163(12) 0.0366(5) Uani 1 1 d . . . . .
C1S C 0.3243(5) 0.7804(8) 0.1223(4) 0.0298(17) Uani 1 1 d . . . . .
H1SA H 0.3230 0.6932 0.1410 0.036 Uiso 1 1 calc R U . . .
H1SB H 0.2673 0.8167 0.1161 0.036 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Mo2 Mo1 2.1242(10) . ?
Mo2 S3 2.4850(18) . ?
Mo2 S7 2.4853(19) . ?
Mo2 N3 2.167(5) . ?
Mo2 N1 2.162(6) . ?
Mo1 S5 2.4818(19) . ?
Mo1 S1 2.486(2) . ?
Mo1 N4 2.138(6) . ?
Mo1 N2 2.152(5) . ?
S3 C5 1.668(7) . ?
S6 C12 1.610(7) . ?
S5 C9 1.675(7) . ?
S2 C4 1.631(7) . ?
S1 C1 1.683(7) . ?
S4 C8 1.627(8) . ?
S7 C13 1.676(8) . ?
S8 C16 1.624(9) . ?
N4 C13 1.346(10) . ?
N4 C16 1.386(10) . ?
N2 C5 1.342(9) . ?
N2 C8 1.381(8) . ?
N3 C12 1.400(9) . ?
N3 C9 1.334(8) . ?
C4 N1 1.374(9) . ?
C4 C3 1.497(9) . ?
C12 C11 1.510(9) . ?
N1 C1 1.339(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C14 1.535(12) . ?
C15 C16 1.521(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.532(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.520(10) . ?
C1 C2 1.496(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.514(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.526(10) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C5 1.510(9) . ?
C6 C7 1.519(10) . ?
C8 C7 1.502(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
Cl2S C1S 1.762(7) . ?
Cl1S C1S 1.776(8) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?

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
Mo1 Mo2 S3 98.06(5) . . ?
Mo1 Mo2 S7 97.11(6) . . ?
Mo1 Mo2 N3 94.28(15) . . ?
Mo1 Mo2 N1 93.48(16) . . ?
S3 Mo2 S7 164.74(6) . . ?
N3 Mo2 S3 89.19(15) . . ?
N3 Mo2 S7 91.36(15) . . ?
N1 Mo2 S3 89.32(15) . . ?
N1 Mo2 S7 88.08(15) . . ?
N1 Mo2 N3 172.2(2) . . ?
Mo2 Mo1 S5 97.58(6) . . ?
Mo2 Mo1 S1 98.40(6) . . ?
Mo2 Mo1 N4 94.81(17) . . ?
Mo2 Mo1 N2 93.79(15) . . ?
S5 Mo1 S1 163.88(6) . . ?
N4 Mo1 S5 88.24(16) . . ?
N4 Mo1 S1 88.34(16) . . ?
N4 Mo1 N2 171.2(2) . . ?
N2 Mo1 S5 92.41(14) . . ?
N2 Mo1 S1 88.63(15) . . ?
C5 S3 Mo2 100.8(2) . . ?
C9 S5 Mo1 101.4(2) . . ?
C1 S1 Mo1 100.8(2) . . ?
C13 S7 Mo2 101.4(3) . . ?
C13 N4 Mo1 125.3(5) . . ?
C13 N4 C16 111.9(6) . . ?
C16 N4 Mo1 122.7(5) . . ?
C5 N2 Mo1 125.7(4) . . ?
C5 N2 C8 111.2(5) . . ?
C8 N2 Mo1 123.0(4) . . ?
C12 N3 Mo2 123.7(4) . . ?
C9 N3 Mo2 124.9(4) . . ?
C9 N3 C12 111.3(5) . . ?
N1 C4 S2 120.8(5) . . ?
N1 C4 C3 109.9(6) . . ?
C3 C4 S2 129.2(5) . . ?
N3 C12 S6 121.6(5) . . ?
N3 C12 C11 108.2(6) . . ?
C11 C12 S6 130.2(5) . . ?
C4 N1 Mo2 123.2(4) . . ?
C1 N1 Mo2 126.3(5) . . ?
C1 N1 C4 110.5(6) . . ?
H15A C15 H15B 108.7 . . ?
C14 C15 H15A 110.6 . . ?
C14 C15 H15B 110.6 . . ?
C16 C15 H15A 110.6 . . ?
C16 C15 H15B 110.6 . . ?
C16 C15 C14 105.7(6) . . ?
C12 C11 H11A 110.6 . . ?
C12 C11 H11B 110.6 . . ?
C12 C11 C10 105.6(5) . . ?
H11A C11 H11B 108.7 . . ?
C10 C11 H11A 110.6 . . ?
C10 C11 H11B 110.6 . . ?
C15 C14 H14A 111.4 . . ?
C15 C14 H14B 111.4 . . ?
H14A C14 H14B 109.2 . . ?
C13 C14 C15 101.9(7) . . ?
C13 C14 H14A 111.4 . . ?
C13 C14 H14B 111.4 . . ?
N1 C1 S1 121.0(5) . . ?
N1 C1 C2 112.3(6) . . ?
C2 C1 S1 126.7(5) . . ?
C11 C10 H10A 111.3 . . ?
C11 C10 H10B 111.3 . . ?
H10A C10 H10B 109.2 . . ?
C9 C10 C11 102.1(5) . . ?
C9 C10 H10A 111.3 . . ?
C9 C10 H10B 111.3 . . ?
C1 C2 H2A 111.3 . . ?
C1 C2 H2B 111.3 . . ?
C1 C2 C3 102.6(5) . . ?
H2A C2 H2B 109.2 . . ?
C3 C2 H2A 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H6A C6 H6B 109.1 . . ?
C5 C6 H6A 111.1 . . ?
C5 C6 H6B 111.1 . . ?
C5 C6 C7 103.2(6) . . ?
C7 C6 H6A 111.1 . . ?
C7 C6 H6B 111.1 . . ?
N2 C5 S3 121.6(5) . . ?
N2 C5 C6 111.1(6) . . ?
C6 C5 S3 127.3(5) . . ?
N2 C8 S4 120.5(5) . . ?
N2 C8 C7 109.2(6) . . ?
C7 C8 S4 130.3(5) . . ?
N4 C13 S7 120.9(5) . . ?
N4 C13 C14 111.8(7) . . ?
C14 C13 S7 127.4(6) . . ?
C6 C7 H7A 110.8 . . ?
C6 C7 H7B 110.8 . . ?
C8 C7 C6 104.6(6) . . ?
C8 C7 H7A 110.8 . . ?
C8 C7 H7B 110.8 . . ?
H7A C7 H7B 108.9 . . ?
C4 C3 C2 104.5(6) . . ?
C4 C3 H3A 110.8 . . ?
C4 C3 H3B 110.8 . . ?
C2 C3 H3A 110.8 . . ?
C2 C3 H3B 110.8 . . ?
H3A C3 H3B 108.9 . . ?
N3 C9 S5 121.6(5) . . ?
N3 C9 C10 112.3(6) . . ?
C10 C9 S5 126.0(5) . . ?
N4 C16 S8 121.8(6) . . ?
N4 C16 C15 108.2(7) . . ?
C15 C16 S8 129.9(6) . . ?
Cl2S C1S Cl1S 110.9(4) . . ?
Cl2S C1S H1SA 109.5 . . ?
Cl2S C1S H1SB 109.5 . . ?
Cl1S C1S H1SA 109.5 . . ?
Cl1S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo2 S3 C5 N2 1.6(6) . . . . ?
Mo2 S3 C5 C6 -179.2(5) . . . . ?
Mo2 S7 C13 N4 -6.8(6) . . . . ?
Mo2 S7 C13 C14 173.0(6) . . . . ?
Mo2 N3 C12 S6 6.4(7) . . . . ?
Mo2 N3 C12 C11 -175.6(4) . . . . ?
Mo2 N3 C9 S5 -5.3(8) . . . . ?
Mo2 N3 C9 C10 176.9(4) . . . . ?
Mo2 N1 C1 S1 -1.9(8) . . . . ?
Mo2 N1 C1 C2 178.6(4) . . . . ?
Mo1 S5 C9 N3 2.4(6) . . . . ?
Mo1 S5 C9 C10 179.8(5) . . . . ?
Mo1 S1 C1 N1 1.6(6) . . . . ?
Mo1 S1 C1 C2 -178.9(5) . . . . ?
Mo1 N4 C13 S7 9.2(8) . . . . ?
Mo1 N4 C13 C14 -170.7(4) . . . . ?
Mo1 N4 C16 S8 -8.7(8) . . . . ?
Mo1 N4 C16 C15 174.0(4) . . . . ?
Mo1 N2 C5 S3 -1.2(8) . . . . ?
Mo1 N2 C5 C6 179.5(4) . . . . ?
Mo1 N2 C8 S4 -4.3(7) . . . . ?
Mo1 N2 C8 C7 176.2(4) . . . . ?
S6 C12 C11 C10 172.2(5) . . . . ?
S2 C4 N1 Mo2 -0.1(8) . . . . ?
S2 C4 N1 C1 -178.4(5) . . . . ?
S2 C4 C3 C2 -179.2(5) . . . . ?
S1 C1 C2 C3 -175.5(5) . . . . ?
S4 C8 C7 C6 -170.7(6) . . . . ?
N2 C8 C7 C6 8.7(7) . . . . ?
N3 C12 C11 C10 -5.6(7) . . . . ?
C4 N1 C1 S1 176.4(5) . . . . ?
C4 N1 C1 C2 -3.2(8) . . . . ?
C12 N3 C9 S5 171.7(5) . . . . ?
C12 N3 C9 C10 -6.0(7) . . . . ?
C12 C11 C10 C9 2.1(7) . . . . ?
N1 C4 C3 C2 1.7(7) . . . . ?
N1 C1 C2 C3 4.0(7) . . . . ?
C15 C14 C13 S7 173.3(5) . . . . ?
C15 C14 C13 N4 -6.9(8) . . . . ?
C11 C10 C9 S5 -175.5(5) . . . . ?
C11 C10 C9 N3 2.1(7) . . . . ?
C14 C15 C16 S8 -178.0(6) . . . . ?
C14 C15 C16 N4 -0.9(8) . . . . ?
C1 C2 C3 C4 -3.2(7) . . . . ?
C5 N2 C8 S4 171.4(5) . . . . ?
C5 N2 C8 C7 -8.0(7) . . . . ?
C5 C6 C7 C8 -6.1(7) . . . . ?
C8 N2 C5 S3 -176.9(5) . . . . ?
C8 N2 C5 C6 3.8(7) . . . . ?
C13 N4 C16 S8 173.7(5) . . . . ?
C13 N4 C16 C15 -3.6(8) . . . . ?
C7 C6 C5 S3 -177.5(5) . . . . ?
C7 C6 C5 N2 1.8(7) . . . . ?
C3 C4 N1 Mo2 179.1(4) . . . . ?
C3 C4 N1 C1 0.8(7) . . . . ?
C9 N3 C12 S6 -170.8(5) . . . . ?
C9 N3 C12 C11 7.3(7) . . . . ?
C16 N4 C13 S7 -173.3(5) . . . . ?
C16 N4 C13 C14 6.8(8) . . . . ?
C16 C15 C14 C13 4.4(7) . . . . ?

_shelx_estimated_absorpt_T_max   0.924
_shelx_estimated_absorpt_T_min   0.804
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_database_code_depnum_ccdc_archive 'CCDC 983531'
###################################################################
### X-ray Crystallographic Data for 2_CH2Cl2_100K, 3, 4_MeOH_100K
### 4_MeOH_200K, and 5
###################################################################
data_global
loop_
_publ_author_name
_publ_author_email
_publ_author_address
'Brian S. Dolinar' ? ?
'John F. Berry' ? ?

_publ_contact_author_address     ?
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
;

### END 2
data_3_100K
_audit_creation_date             2013-12-18
_audit_creation_method           
;
  Olex2 1.2-alpha
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_chemical_name_common            ?
_chemical_formula_moiety         'C14 H18 Mo2 N2 O4 S4'
_chemical_formula_sum            'C14 H18 Mo2 N2 O4 S4'
_chemical_formula_weight         598.42
_chemical_melting_point          ?
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   8.4950(2)
_cell_length_b                   7.4672(2)
_cell_length_c                   15.4637(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.6340(10)
_cell_angle_gamma                90.00
_cell_volume                     949.10(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8454
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5157
_cell_measurement_theta_min      2.7227
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  0.8253
_exptl_absorpt_correction_T_min  0.6567
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.073
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2908
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         2.48
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60° ω and 0.6° φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_reflns_number_gt                2514
_reflns_number_total             2908
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2908
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0241
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0154P)²+2.0690P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0573
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2A(0.019) H2B(0.019) H3A(0.02) H3B(0.02) H4A(0.02) H4B(0.02)
 H7A(0.022) H7B(0.022) H7C(0.022)
 Fixed X: H2A(0.2876) H2B(0.1473) H3A(0.0409) H3B(0.0072) H4A(0.7374)
 H4B(0.8814) H7A(0.077) H7B(-0.0237) H7C(0.055)
 Fixed Y: H2A(0.5069) H2B(0.509) H3A(0.431) H3B(0.2749) H4A(-0.2794) H4B(-
 0.1359) H7A(-0.3664) H7B(-0.1921) H7C(-0.2048)
 Fixed Z: H2A(-0.2009) H2B(-0.1484) H3A(-0.3039) H3B(-0.2393) H4A(0.3308)
 H4B(0.3456) H7A(0.03) H7B(-0.0115) H7C(0.0939)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.51456(2) 0.07005(3) 0.060687(13) 0.00879(5) Uani 1 1 d . . .
S1 S 0.35648(7) 0.33796(8) -0.00542(4) 0.01137(11) Uani 1 1 d . . .
S2 S 0.63196(8) 0.10444(9) 0.26224(4) 0.01673(13) Uani 1 1 d . . .
O1 O 0.3013(2) -0.0460(2) 0.08249(11) 0.0115(3) Uani 1 1 d . . .
O2 O 0.7336(2) 0.1868(2) 0.04808(11) 0.0121(3) Uani 1 1 d . . .
N1 N 0.6557(2) -0.1349(3) 0.14425(13) 0.0108(4) Uani 1 1 d . . .
C1 C 0.3015(3) 0.2940(3) -0.11526(15) 0.0106(4) Uani 1 1 d . . .
C2 C 0.2098(3) 0.4309(3) -0.17940(16) 0.0159(5) Uani 1 1 d . . .
H2A H 0.2876 0.5069 -0.2009 0.019 Uiso 1 1 calc R . .
H2B H 0.1473 0.5090 -0.1484 0.019 Uiso 1 1 calc R . .
C3 C 0.0932(3) 0.3403(3) -0.25919(17) 0.0164(5) Uani 1 1 d . . .
H3A H 0.0409 0.4310 -0.3039 0.020 Uiso 1 1 calc R . .
H3B H 0.0072 0.2749 -0.2393 0.020 Uiso 1 1 calc R . .
C4 C 0.8064(3) -0.2098(4) 0.30002(17) 0.0170(5) Uani 1 1 d . . .
H4A H 0.7374 -0.2794 0.3308 0.020 Uiso 1 1 calc R . .
H4B H 0.8814 -0.1359 0.3456 0.020 Uiso 1 1 calc R . .
C5 C 0.7003(3) -0.0889(3) 0.23329(16) 0.0119(4) Uani 1 1 d . . .
C6 C 0.2220(3) -0.1518(3) 0.02277(16) 0.0118(4) Uani 1 1 d . . .
C7 C 0.0695(3) -0.2360(3) 0.03485(17) 0.0149(5) Uani 1 1 d . . .
H7A H 0.0770 -0.3664 0.0300 0.022 Uiso 1 1 calc R . .
H7B H -0.0237 -0.1921 -0.0115 0.022 Uiso 1 1 calc R . .
H7C H 0.0550 -0.2048 0.0939 0.022 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
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 Mo1 2.1080(4) 3_655 ?
Mo1 S1 2.4813(6) . ?
Mo1 O1 2.1108(16) . ?
Mo1 O2 2.1083(17) . ?
Mo1 N1 2.160(2) . ?
S1 C1 1.676(2) . ?
S2 C5 1.659(2) . ?
O1 C6 1.271(3) . ?
O2 C6 1.273(3) 3_655 ?
N1 C1 1.352(3) 3_655 ?
N1 C5 1.376(3) . ?
C1 N1 1.352(3) 3_655 ?
C1 C2 1.498(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.531(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.532(4) 3_655 ?
C4 C3 1.532(4) 3_655 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.491(3) . ?
C6 O2 1.273(3) 3_655 ?
C6 C7 1.494(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
Mo1 Mo1 S1 95.955(18) 3_655 . ?
Mo1 Mo1 O1 91.49(5) 3_655 . ?
Mo1 Mo1 O2 91.76(5) 3_655 . ?
Mo1 Mo1 N1 95.95(5) 3_655 . ?
O1 Mo1 S1 89.99(5) . . ?
O1 Mo1 N1 89.00(7) . . ?
O2 Mo1 S1 91.54(5) . . ?
O2 Mo1 O1 176.24(6) . . ?
O2 Mo1 N1 88.79(7) . . ?
N1 Mo1 S1 168.08(5) . . ?
C1 S1 Mo1 104.06(8) . . ?
C6 O1 Mo1 117.25(15) . . ?
C6 O2 Mo1 117.06(15) 3_655 . ?
C1 N1 Mo1 125.41(16) 3_655 . ?
C1 N1 C5 121.5(2) 3_655 . ?
C5 N1 Mo1 113.13(16) . . ?
N1 C1 S1 118.59(17) 3_655 . ?
N1 C1 C2 121.2(2) 3_655 . ?
C2 C1 S1 120.16(18) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 C3 110.7(2) . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C2 C3 H3A 110.2 . . ?
C2 C3 H3B 110.2 . . ?
C2 C3 C4 107.4(2) . 3_655 ?
H3A C3 H3B 108.5 . . ?
C4 C3 H3A 110.2 3_655 . ?
C4 C3 H3B 110.2 3_655 . ?
C3 C4 H4A 108.8 3_655 . ?
C3 C4 H4B 108.8 3_655 . ?
H4A C4 H4B 107.7 . . ?
C5 C4 C3 113.7(2) . 3_655 ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
N1 C5 S2 117.41(18) . . ?
N1 C5 C4 120.5(2) . . ?
C4 C5 S2 122.12(18) . . ?
O1 C6 O2 122.4(2) . 3_655 ?
O1 C6 C7 119.2(2) . . ?
O2 C6 C7 118.4(2) 3_655 . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 Mo1 S1 C1 -1.51(8) 3_655 . . . ?
Mo1 Mo1 O1 C6 -1.49(16) 3_655 . . . ?
Mo1 Mo1 O2 C6 3.03(16) 3_655 . . 3_655 ?
Mo1 Mo1 N1 C1 -0.29(19) 3_655 . . 3_655 ?
Mo1 Mo1 N1 C5 179.86(15) 3_655 . . . ?
Mo1 S1 C1 N1 1.96(19) . . . 3_655 ?
Mo1 S1 C1 C2 -176.83(17) . . . . ?
Mo1 O1 C6 O2 -0.6(3) . . . 3_655 ?
Mo1 O1 C6 C7 -179.50(16) . . . . ?
Mo1 N1 C5 S2 3.4(2) . . . . ?
Mo1 N1 C5 C4 -176.40(17) . . . . ?
S1 Mo1 O1 C6 94.47(16) . . . . ?
S1 Mo1 O2 C6 -92.98(16) . . . 3_655 ?
S1 Mo1 N1 C1 176.34(18) . . . 3_655 ?
S1 Mo1 N1 C5 -3.5(4) . . . . ?
S1 C1 C2 C3 -147.66(18) . . . . ?
O1 Mo1 S1 C1 -93.00(9) . . . . ?
O1 Mo1 O2 C6 153.0(10) . . . 3_655 ?
O1 Mo1 N1 C1 91.11(19) . . . 3_655 ?
O1 Mo1 N1 C5 -88.75(16) . . . . ?
O2 Mo1 S1 C1 90.43(9) . . . . ?
O2 Mo1 O1 C6 -151.5(10) . . . . ?
O2 Mo1 N1 C1 -91.93(19) . . . 3_655 ?
O2 Mo1 N1 C5 88.21(16) . . . . ?
N1 Mo1 S1 C1 -178.1(3) . . . . ?
N1 Mo1 O1 C6 -97.41(17) . . . . ?
N1 Mo1 O2 C6 98.95(17) . . . 3_655 ?
N1 C1 C2 C3 33.6(3) 3_655 . . . ?
C1 N1 C5 S2 -176.45(17) 3_655 . . . ?
C1 N1 C5 C4 3.7(3) 3_655 . . . ?
C1 C2 C3 C4 -54.6(3) . . . 3_655 ?
C3 C4 C5 S2 -158.17(19) 3_655 . . . ?
C3 C4 C5 N1 21.6(3) 3_655 . . . ?
_database_code_depnum_ccdc_archive 'CCDC 983532'
###################################################################
### X-ray Crystallographic Data for 2_CH2Cl2_100K, 3, 4_MeOH_100K
### 4_MeOH_200K, and 5
###################################################################
data_global
loop_
_publ_author_name
_publ_author_email
_publ_author_address
'Brian S. Dolinar' ? ?
'John F. Berry' ? ?

_publ_contact_author_address     ?
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
;

### END 3
data_4a_CH2Cl2_100K

_audit_creation_date             2013-12-18
_audit_creation_method           
;
  Olex2 1.2-alpha
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H16 Mo2 N4 O4 S4, 2(C H2 Cl2)'
_chemical_formula_sum            'C18 H20 Cl4 Mo2 N4 O4 S4'
_chemical_formula_weight         818.30
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.101(4)
_cell_length_b                   20.553(10)
_cell_length_c                   7.445(4)
_cell_angle_alpha                90
_cell_angle_beta                 110.31(2)
_cell_angle_gamma                90
_cell_volume                     1305.9(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3794
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.39
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7377
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1094 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.7377.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.018
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14742
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         1.982
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5° ω and 0.5° φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2416
_reflns_number_total             2981
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0366
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+3.0059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0884
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2A(0.022) H2B(0.022) H3A(0.019) H3B(0.019) H6A(0.028) H6B(0.028)
 H7A(0.026) H7B(0.026) H9AA(0.055) H9AB(0.055) H9BC(0.055) H9BD(0.055)
 H9CE(0.055) H9CF(0.055)
 Fixed X: H2A(0.745) H2B(0.5645) H3A(0.5305) H3B(0.7176) H6A(1.0288)
 H6B(1.0753) H7A(1.0391) H7B(0.9921) H9AA(0.7947) H9AB(0.8307) H9BC(0.7774)
 H9BD(0.8099) H9CE(0.8267) H9CF(0.7974)
 Fixed Y: H2A(0.2969) H2B(0.2736) H3A(0.3168) H3B(0.3267) H6A(0.6062)
 H6B(0.5358) H7A(0.5735) H7B(0.6438) H9AA(0.6561) H9AB(0.6829) H9BC(0.7147)
 H9BD(0.6465) H9CE(0.6938) H9CF(0.6515)
 Fixed Z: H2A(0.3424) H2B(0.2717) H3A(0.5322) H3B(0.62) H6A(0.2326)
 H6B(0.3319) H7A(0.598) H7B(0.4986) H9AA(0.8087) H9AB(1.0212) H9BC(0.7749)
 H9BD(0.8859) H9CE(1.022) H9CF(0.8313)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.49406(4) 0.51498(2) 0.13529(4) 0.00865(10) Uani 1 1 d . . . . .
S1 S 0.57584(13) 0.36959(4) -0.03742(13) 0.0140(2) Uani 1 1 d . . . . .
S2 S 0.78777(12) 0.51581(5) -0.03991(14) 0.0159(2) Uani 1 1 d . . . . .
O1 O 0.6121(3) 0.45019(13) 0.5959(4) 0.0152(6) Uani 1 1 d . . . . .
O2 O 0.7250(4) 0.59866(15) 0.5466(4) 0.0232(7) Uani 1 1 d . . . . .
N1 N 0.5669(4) 0.42292(14) 0.2813(4) 0.0101(6) Uani 1 1 d . . . . .
N2 N 0.7319(4) 0.54915(15) 0.2713(4) 0.0124(7) Uani 1 1 d . . . . .
C1 C 0.5896(5) 0.36932(18) 0.1926(5) 0.0120(8) Uani 1 1 d . . . . .
C2 C 0.6363(5) 0.31060(19) 0.3232(6) 0.0182(9) Uani 1 1 d . . . . .
H2A H 0.7450 0.2969 0.3424 0.022 Uiso 1 1 calc R U . . .
H2B H 0.5645 0.2736 0.2717 0.022 Uiso 1 1 calc R U . . .
C3 C 0.6218(5) 0.33633(18) 0.5093(5) 0.0154(8) Uani 1 1 d . . . . .
H3A H 0.5305 0.3168 0.5322 0.019 Uiso 1 1 calc R U . . .
H3B H 0.7176 0.3267 0.6200 0.019 Uiso 1 1 calc R U . . .
C4 C 0.6002(5) 0.40908(18) 0.4771(5) 0.0112(7) Uani 1 1 d . . . . .
C5 C 0.8347(5) 0.54510(19) 0.1824(6) 0.0152(8) Uani 1 1 d . . . . .
C6 C 0.9958(5) 0.5708(2) 0.3007(6) 0.0235(10) Uani 1 1 d . . . . .
H6A H 1.0288 0.6062 0.2326 0.028 Uiso 1 1 calc R U . . .
H6B H 1.0753 0.5358 0.3319 0.028 Uiso 1 1 calc R U . . .
C7 C 0.9706(5) 0.5965(2) 0.4825(6) 0.0217(9) Uani 1 1 d . . . . .
H7A H 1.0391 0.5735 0.5980 0.026 Uiso 1 1 calc R U . . .
H7B H 0.9921 0.6438 0.4986 0.026 Uiso 1 1 calc R U . . .
C8 C 0.7988(5) 0.58226(19) 0.4471(6) 0.0159(8) Uani 1 1 d . . . . .
Cl1 Cl 1.03983(18) 0.69920(9) 0.9261(2) 0.0545(4) Uani 1 1 d D . . . .
Cl2 Cl 0.7334(3) 0.76209(10) 0.8046(4) 0.0304(6) Uani 0.578(3) 1 d D . P A 1
Cl2A Cl 0.7995(11) 0.7286(5) 1.0866(13) 0.089(3) Uiso 0.219(2) 1 d D . P A 2
Cl2B Cl 0.7398(13) 0.7598(7) 0.754(2) 0.089(3) Uiso 0.203(3) 1 d D . P A 3
C9 C 0.8404(5) 0.6930(3) 0.8958(8) 0.0459(15) Uani 1 1 d D . . . .
H9AA H 0.7947 0.6561 0.8087 0.055 Uiso 0.578(3) 1 calc R U P A 1
H9AB H 0.8307 0.6829 1.0212 0.055 Uiso 0.578(3) 1 calc R U P A 1
H9BC H 0.7774 0.7147 0.7749 0.055 Uiso 0.219(2) 1 calc R U P A 2
H9BD H 0.8099 0.6465 0.8859 0.055 Uiso 0.219(2) 1 calc R U P A 2
H9CE H 0.8267 0.6938 1.0220 0.055 Uiso 0.203(3) 1 calc R U P A 3
H9CF H 0.7974 0.6515 0.8313 0.055 Uiso 0.203(3) 1 calc R U P A 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Mo1 2.1447(11) 3_665 ?
Mo1 S1 2.4985(15) 3_665 ?
Mo1 S2 2.4937(16) 3_665 ?
Mo1 N1 2.168(3) . ?
Mo1 N2 2.164(3) . ?
S1 Mo1 2.4986(15) 3_665 ?
S1 C1 1.673(4) . ?
S2 Mo1 2.4936(16) 3_665 ?
S2 C5 1.672(4) . ?
O1 C4 1.200(5) . ?
O2 C8 1.208(5) . ?
N1 C1 1.336(5) . ?
N1 C4 1.411(5) . ?
N2 C5 1.322(5) . ?
N2 C8 1.412(5) . ?
C1 C2 1.515(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.531(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.516(5) . ?
C5 C6 1.519(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.542(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.521(6) . ?
Cl1 C9 1.754(5) . ?
Cl2 C9 1.723(5) . ?
Cl2A C9 1.749(7) . ?
Cl2B C9 1.779(8) . ?
C9 H9AA 0.9900 . ?
C9 H9AB 0.9900 . ?
C9 H9BC 0.9900 . ?
C9 H9BD 0.9900 . ?
C9 H9CE 0.9900 . ?
C9 H9CF 0.9900 . ?

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
Mo1 Mo1 S1 95.13(3) 3_665 3_665 ?
Mo1 Mo1 S2 92.40(4) 3_665 3_665 ?
Mo1 Mo1 N1 96.54(9) 3_665 . ?
Mo1 Mo1 N2 99.46(9) 3_665 . ?
S2 Mo1 S1 91.45(4) 3_665 3_665 ?
N1 Mo1 S1 167.82(8) . 3_665 ?
N1 Mo1 S2 91.54(9) . 3_665 ?
N2 Mo1 S1 86.58(9) . 3_665 ?
N2 Mo1 S2 168.10(9) . 3_665 ?
N2 Mo1 N1 88.07(12) . . ?
C1 S1 Mo1 102.87(13) . 3_665 ?
C5 S2 Mo1 104.91(15) . 3_665 ?
C1 N1 Mo1 123.0(2) . . ?
C1 N1 C4 109.2(3) . . ?
C4 N1 Mo1 127.7(2) . . ?
C5 N2 Mo1 120.8(3) . . ?
C5 N2 C8 110.0(3) . . ?
C8 N2 Mo1 129.0(3) . . ?
N1 C1 S1 122.2(3) . . ?
N1 C1 C2 113.4(3) . . ?
C2 C1 S1 124.3(3) . . ?
C1 C2 H2A 111.3 . . ?
C1 C2 H2B 111.3 . . ?
C1 C2 C3 102.3(3) . . ?
H2A C2 H2B 109.2 . . ?
C3 C2 H2A 111.3 . . ?
C3 C2 H2B 111.3 . . ?
C2 C3 H3A 110.9 . . ?
C2 C3 H3B 110.9 . . ?
H3A C3 H3B 108.9 . . ?
C4 C3 C2 104.2(3) . . ?
C4 C3 H3A 110.9 . . ?
C4 C3 H3B 110.9 . . ?
O1 C4 N1 123.5(3) . . ?
O1 C4 C3 127.2(3) . . ?
N1 C4 C3 109.4(3) . . ?
N2 C5 S2 122.4(3) . . ?
N2 C5 C6 113.3(3) . . ?
C6 C5 S2 124.2(3) . . ?
C5 C6 H6A 111.2 . . ?
C5 C6 H6B 111.2 . . ?
C5 C6 C7 102.7(4) . . ?
H6A C6 H6B 109.1 . . ?
C7 C6 H6A 111.2 . . ?
C7 C6 H6B 111.2 . . ?
C6 C7 H7A 111.0 . . ?
C6 C7 H7B 111.0 . . ?
H7A C7 H7B 109.0 . . ?
C8 C7 C6 103.8(3) . . ?
C8 C7 H7A 111.0 . . ?
C8 C7 H7B 111.0 . . ?
O2 C8 N2 123.4(4) . . ?
O2 C8 C7 126.6(4) . . ?
N2 C8 C7 109.9(3) . . ?
Cl1 C9 Cl2B 108.4(5) . . ?
Cl1 C9 H9AA 108.7 . . ?
Cl1 C9 H9AB 108.7 . . ?
Cl1 C9 H9BC 109.3 . . ?
Cl1 C9 H9BD 109.3 . . ?
Cl1 C9 H9CE 110.0 . . ?
Cl1 C9 H9CF 110.0 . . ?
Cl2 C9 Cl1 114.1(3) . . ?
Cl2 C9 H9AA 108.7 . . ?
Cl2 C9 H9AB 108.7 . . ?
Cl2A C9 Cl1 111.6(4) . . ?
Cl2A C9 H9BC 109.3 . . ?
Cl2A C9 H9BD 109.3 . . ?
Cl2B C9 H9CE 110.0 . . ?
Cl2B C9 H9CF 110.0 . . ?
H9AA C9 H9AB 107.6 . . ?
H9BC C9 H9BD 108.0 . . ?
H9CE C9 H9CF 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 S1 C1 N1 -0.8(4) 3_665 . . . ?
Mo1 S1 C1 C2 -177.5(3) 3_665 . . . ?
Mo1 S2 C5 N2 -0.8(4) 3_665 . . . ?
Mo1 S2 C5 C6 -179.4(3) 3_665 . . . ?
Mo1 N1 C1 S1 4.4(5) . . . . ?
Mo1 N1 C1 C2 -178.6(3) . . . . ?
Mo1 N1 C4 O1 -10.4(6) . . . . ?
Mo1 N1 C4 C3 171.2(3) . . . . ?
Mo1 N2 C5 S2 1.8(5) . . . . ?
Mo1 N2 C5 C6 -179.4(3) . . . . ?
Mo1 N2 C8 O2 -2.8(6) . . . . ?
Mo1 N2 C8 C7 -179.8(3) . . . . ?
S1 C1 C2 C3 -177.3(3) . . . . ?
S2 C5 C6 C7 175.4(3) . . . . ?
N1 C1 C2 C3 5.7(5) . . . . ?
N2 C5 C6 C7 -3.4(5) . . . . ?
C1 N1 C4 O1 168.6(4) . . . . ?
C1 N1 C4 C3 -9.8(4) . . . . ?
C1 C2 C3 C4 -10.7(4) . . . . ?
C2 C3 C4 O1 -165.4(4) . . . . ?
C2 C3 C4 N1 12.9(4) . . . . ?
C4 N1 C1 S1 -174.7(3) . . . . ?
C4 N1 C1 C2 2.3(5) . . . . ?
C5 N2 C8 O2 171.8(4) . . . . ?
C5 N2 C8 C7 -5.1(5) . . . . ?
C5 C6 C7 C8 0.2(4) . . . . ?
C6 C7 C8 O2 -174.0(4) . . . . ?
C6 C7 C8 N2 2.8(5) . . . . ?
C8 N2 C5 S2 -173.4(3) . . . . ?
C8 N2 C5 C6 5.4(5) . . . . ?

_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.681
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-3
_database_code_depnum_ccdc_archive 'CCDC 983533'
###################################################################
### X-ray Crystallographic Data for 2_CH2Cl2_100K, 3, 4_MeOH_100K
### 4_MeOH_200K, and 5
###################################################################
data_global
loop_
_publ_author_name
_publ_author_email
_publ_author_address
'Brian S. Dolinar' ? ?
'John F. Berry' ? ?

_publ_contact_author_address     ?
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
;

### END 4a-CH2Cl2(100K)

data_4a_MeOH_100K

_audit_creation_date             2014-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C8 H8 Mo N2 O2 S2), 2(C H4 O)'
_chemical_formula_sum            'C18 H24 Mo2 N4 O6 S4'
_chemical_formula_weight         712.53
_chemical_melting_point          ?
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'
Mo Mo -1.6832 0.6857 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.990(3)
_cell_length_b                   14.717(7)
_cell_length_c                   10.048(4)
_cell_angle_alpha                89.646(17)
_cell_angle_beta                 112.528(13)
_cell_angle_gamma                88.73(2)
_cell_volume                     1227.6(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2864
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      4.08
_shelx_estimated_absorpt_T_max   0.933
_shelx_estimated_absorpt_T_min   0.933
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.647639
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1181 before and 0.0457 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1181 before and 0.0492 after correction.
 The Ratio of minimum to maximum transmission is 0.72.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 18764 reflections, Rint = 0.0800
 (9312 with I > 3sig(I), Rint = 0.0684)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8926
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         3.507
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5\ ω and 0.5\ φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6636
_reflns_number_total             8926
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         8926
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0516
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0669P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1269
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(O5A)=Sof(H5A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(O5)=Sof(H5)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,
 H11B), C14(H14A,H14B), C15(H15A,H15B)
3.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C)
3.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O5A(H5A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.57476(5) 1.03524(4) 0.59394(6) 0.01693(15) Uani 1 1 d . . . . .
S1 S 0.39378(17) 1.01068(12) 0.72627(19) 0.0237(4) Uani 1 1 d . . . . .
S2 S 0.73615(16) 0.89483(11) 0.70622(19) 0.0209(4) Uani 1 1 d . . . . .
O1 O 0.0962(5) 0.8230(4) 0.3119(7) 0.0405(15) Uani 1 1 d . . . . .
O2 O 0.3897(5) 0.7454(3) 0.2639(6) 0.0298(12) Uani 1 1 d . . . . .
O5 O 0.7190(17) 1.0910(8) 0.8658(15) 0.032(4) Uani 0.52(2) 1 d . . P A 1
H5 H 0.7125 1.1480 0.8611 0.048 Uiso 0.52(2) 1 calc GR . P A 1
O5A O 0.7959(18) 1.0752(8) 0.8446(13) 0.029(4) Uani 0.48(2) 1 d . . P A 2
H5A H 0.8193 1.1225 0.8104 0.043 Uiso 0.48(2) 1 calc GR . P A 2
N1 N 0.2463(5) 0.9219(4) 0.4880(6) 0.0220(13) Uani 1 1 d . . . . .
N2 N 0.5287(5) 0.8299(4) 0.4639(6) 0.0190(12) Uani 1 1 d . . . . .
C1 C 0.2498(6) 0.9465(4) 0.6154(8) 0.0211(14) Uani 1 1 d . . . . .
C2 C 0.1154(7) 0.9065(5) 0.6518(9) 0.0307(18) Uani 1 1 d . . . . .
H2A H 0.0438 0.9549 0.6644 0.037 Uiso 1 1 calc R . . . .
H2B H 0.1590 0.8683 0.7404 0.037 Uiso 1 1 calc R . . . .
C3 C 0.0263(7) 0.8493(5) 0.5190(9) 0.0310(18) Uani 1 1 d . . . . .
H3A H 0.0257 0.7846 0.5466 0.037 Uiso 1 1 calc R . . . .
H3B H -0.0863 0.8718 0.4691 0.037 Uiso 1 1 calc R . . . .
C4 C 0.1205(7) 0.8607(5) 0.4250(9) 0.0255(16) Uani 1 1 d . . . . .
C5 C 0.6483(7) 0.8122(4) 0.5911(8) 0.0212(14) Uani 1 1 d . . . . .
C6 C 0.6918(7) 0.7129(4) 0.6172(8) 0.0234(15) Uani 1 1 d . . . . .
H6A H 0.6791 0.6907 0.7053 0.028 Uiso 1 1 calc R . . . .
H6B H 0.8040 0.7004 0.6262 0.028 Uiso 1 1 calc R . . . .
C7 C 0.5719(7) 0.6699(5) 0.4834(8) 0.0254(15) Uani 1 1 d . . . . .
H7A H 0.6284 0.6315 0.4360 0.031 Uiso 1 1 calc R . . . .
H7B H 0.4969 0.6316 0.5085 0.031 Uiso 1 1 calc R . . . .
C8 C 0.4824(7) 0.7472(5) 0.3863(8) 0.0223(15) Uani 1 1 d . . . . .
C17 C 0.878(2) 1.0623(12) 0.9644(18) 0.044(6) Uani 0.52(2) 1 d . . P A 1
H17A H 0.9495 1.0553 0.9114 0.067 Uiso 0.52(2) 1 calc GR . P A 1
H17B H 0.8725 1.0041 1.0097 0.067 Uiso 0.52(2) 1 calc GR . P A 1
H17C H 0.9214 1.1081 1.0389 0.067 Uiso 0.52(2) 1 calc GR . P A 1
C17A C 0.781(2) 1.0951(12) 0.975(2) 0.030(5) Uani 0.48(2) 1 d . . P A 2
H17D H 0.7043 1.1459 0.9606 0.045 Uiso 0.48(2) 1 calc GR . P A 2
H17E H 0.8867 1.1117 1.0465 0.045 Uiso 0.48(2) 1 calc GR . P A 2
H17F H 0.7433 1.0416 1.0100 0.045 Uiso 0.48(2) 1 calc GR . P A 2
Mo2 Mo 0.56756(5) 0.45997(4) 0.09423(6) 0.01632(15) Uani 1 1 d . . . . .
S3 S 0.73714(16) 0.58892(11) 0.21936(19) 0.0215(4) Uani 1 1 d . . . . .
S4 S 0.37407(16) 0.49278(11) 0.21327(19) 0.0201(3) Uani 1 1 d . . . . .
O3 O 0.4111(5) 0.7647(3) -0.2181(6) 0.0292(12) Uani 1 1 d . . . . .
O4 O 0.0963(5) 0.6882(4) -0.2125(6) 0.0328(12) Uani 1 1 d . . . . .
O6 O 0.6940(5) 0.3916(4) 0.3612(6) 0.0327(12) Uani 1 1 d . . . . .
H6 H 0.692(9) 0.326(6) 0.323(10) 0.05(2) Uiso 1 1 d . . . . .
N3 N 0.5442(5) 0.6687(4) -0.0248(6) 0.0190(12) Uani 1 1 d . . . . .
N4 N 0.2434(5) 0.5890(4) -0.0274(6) 0.0182(12) Uani 1 1 d . . . . .
C9 C 0.6616(6) 0.6777(4) 0.1074(8) 0.0203(14) Uani 1 1 d . . . . .
C10 C 0.7116(7) 0.7747(5) 0.1395(8) 0.0270(16) Uani 1 1 d . . . . .
H10A H 0.8279 0.7807 0.1609 0.032 Uiso 1 1 calc R . . . .
H10B H 0.6883 0.7973 0.2224 0.032 Uiso 1 1 calc R . . . .
C11 C 0.6097(9) 0.8262(5) 0.0014(9) 0.0380(19) Uani 1 1 d . . . . .
H11A H 0.5413 0.8739 0.0204 0.046 Uiso 1 1 calc R . . . .
H11B H 0.6786 0.8548 -0.0431 0.046 Uiso 1 1 calc R . . . .
C12 C 0.5078(7) 0.7535(5) -0.0947(8) 0.0255(16) Uani 1 1 d . . . . .
C13 C 0.2376(6) 0.5644(4) 0.0978(7) 0.0185(14) Uani 1 1 d . . . . .
C14 C 0.0983(7) 0.6081(5) 0.1245(8) 0.0238(15) Uani 1 1 d . . . . .
H14A H 0.1367 0.6463 0.2113 0.029 Uiso 1 1 calc R . . . .
H14B H 0.0259 0.5617 0.1363 0.029 Uiso 1 1 calc R . . . .
C15 C 0.0139(7) 0.6655(5) -0.0108(9) 0.0278(16) Uani 1 1 d . . . . .
H15A H -0.0969 0.6446 -0.0638 0.033 Uiso 1 1 calc R . . . .
H15B H 0.0088 0.7303 0.0133 0.033 Uiso 1 1 calc R . . . .
C16 C 0.1158(6) 0.6522(5) -0.0993(8) 0.0227(15) Uani 1 1 d . . . . .
C18 C 0.8438(8) 0.4101(6) 0.4745(9) 0.038(2) Uani 1 1 d . . . . .
H18A H 0.9273 0.4158 0.4348 0.056 Uiso 1 1 calc GR . . . .
H18B H 0.8737 0.3604 0.5458 0.056 Uiso 1 1 calc GR . . . .
H18C H 0.8336 0.4671 0.5207 0.056 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Mo1 2.1420(13) 2_676 ?
Mo1 S1 2.4948(19) . ?
Mo1 S2 2.4965(19) . ?
Mo1 N1 2.172(5) 2_676 ?
Mo1 N2 2.152(5) 2_676 ?
S1 C1 1.664(7) . ?
S2 C5 1.674(7) . ?
O1 C4 1.213(9) . ?
O2 C8 1.194(8) . ?
O5 H5 0.8400 . ?
O5 C17 1.45(2) . ?
O5A H5A 0.8400 . ?
O5A C17A 1.40(3) . ?
N1 Mo1 2.172(5) 2_676 ?
N1 C1 1.322(9) . ?
N1 C4 1.412(8) . ?
N2 Mo1 2.152(5) 2_676 ?
N2 C5 1.337(8) . ?
N2 C8 1.430(9) . ?
C1 C2 1.518(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.535(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.502(10) . ?
C5 C6 1.499(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.518(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.496(10) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
Mo2 Mo2 2.1439(13) 2_665 ?
Mo2 S3 2.4890(19) . ?
Mo2 S4 2.5009(18) . ?
Mo2 N3 2.155(5) 2_665 ?
Mo2 N4 2.165(5) 2_665 ?
S3 C9 1.671(7) . ?
S4 C13 1.673(6) . ?
O3 C12 1.219(9) . ?
O4 C16 1.200(8) . ?
O6 H6 1.04(9) . ?
O6 C18 1.425(8) . ?
N3 Mo2 2.155(5) 2_665 ?
N3 C9 1.354(8) . ?
N3 C12 1.397(9) . ?
N4 Mo2 2.165(5) 2_665 ?
N4 C13 1.328(9) . ?
N4 C16 1.418(8) . ?
C9 C10 1.506(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.524(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.516(10) . ?
C13 C14 1.510(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.518(10) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.512(10) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

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
Mo1 Mo1 S1 94.26(6) 2_676 . ?
Mo1 Mo1 S2 92.80(6) 2_676 . ?
Mo1 Mo1 N1 97.17(16) 2_676 2_676 ?
Mo1 Mo1 N2 99.25(15) 2_676 2_676 ?
S1 Mo1 S2 90.98(6) . . ?
N1 Mo1 S1 168.08(17) 2_676 . ?
N1 Mo1 S2 91.83(15) 2_676 . ?
N2 Mo1 S1 89.06(15) 2_676 . ?
N2 Mo1 S2 167.92(15) 2_676 . ?
N2 Mo1 N1 85.8(2) 2_676 2_676 ?
C1 S1 Mo1 103.5(3) . . ?
C5 S2 Mo1 104.6(2) . . ?
C17 O5 H5 109.5 . . ?
C17A O5A H5A 109.5 . . ?
C1 N1 Mo1 122.4(4) . 2_676 ?
C1 N1 C4 109.6(6) . . ?
C4 N1 Mo1 127.8(5) . 2_676 ?
C5 N2 Mo1 121.3(4) . 2_676 ?
C5 N2 C8 109.4(5) . . ?
C8 N2 Mo1 129.2(4) . 2_676 ?
N1 C1 S1 122.5(5) . . ?
N1 C1 C2 113.2(6) . . ?
C2 C1 S1 124.3(6) . . ?
C1 C2 H2A 111.3 . . ?
C1 C2 H2B 111.3 . . ?
C1 C2 C3 102.6(6) . . ?
H2A C2 H2B 109.2 . . ?
C3 C2 H2A 111.3 . . ?
C3 C2 H2B 111.3 . . ?
C2 C3 H3A 110.9 . . ?
C2 C3 H3B 110.9 . . ?
H3A C3 H3B 108.9 . . ?
C4 C3 C2 104.3(5) . . ?
C4 C3 H3A 110.9 . . ?
C4 C3 H3B 110.9 . . ?
O1 C4 N1 123.6(6) . . ?
O1 C4 C3 126.2(6) . . ?
N1 C4 C3 110.2(7) . . ?
N2 C5 S2 121.8(5) . . ?
N2 C5 C6 113.2(6) . . ?
C6 C5 S2 125.0(5) . . ?
C5 C6 H6A 111.2 . . ?
C5 C6 H6B 111.2 . . ?
C5 C6 C7 102.7(5) . . ?
H6A C6 H6B 109.1 . . ?
C7 C6 H6A 111.2 . . ?
C7 C6 H6B 111.2 . . ?
C6 C7 H7A 110.6 . . ?
C6 C7 H7B 110.6 . . ?
H7A C7 H7B 108.7 . . ?
C8 C7 C6 105.8(6) . . ?
C8 C7 H7A 110.6 . . ?
C8 C7 H7B 110.6 . . ?
O2 C8 N2 122.9(6) . . ?
O2 C8 C7 128.8(6) . . ?
N2 C8 C7 108.3(6) . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5A C17A H17D 109.5 . . ?
O5A C17A H17E 109.5 . . ?
O5A C17A H17F 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
Mo2 Mo2 S3 93.55(6) 2_665 . ?
Mo2 Mo2 S4 93.68(5) 2_665 . ?
Mo2 Mo2 N3 98.73(15) 2_665 2_665 ?
Mo2 Mo2 N4 98.10(15) 2_665 2_665 ?
S3 Mo2 S4 91.21(6) . . ?
N3 Mo2 S3 167.62(15) 2_665 . ?
N3 Mo2 S4 89.57(14) 2_665 . ?
N3 Mo2 N4 86.58(19) 2_665 2_665 ?
N4 Mo2 S3 90.16(14) 2_665 . ?
N4 Mo2 S4 168.04(16) 2_665 . ?
C9 S3 Mo2 104.3(2) . . ?
C13 S4 Mo2 103.8(2) . . ?
C18 O6 H6 112(4) . . ?
C9 N3 Mo2 121.2(4) . 2_665 ?
C9 N3 C12 109.2(5) . . ?
C12 N3 Mo2 129.5(4) . 2_665 ?
C13 N4 Mo2 122.0(4) . 2_665 ?
C13 N4 C16 109.6(5) . . ?
C16 N4 Mo2 128.4(5) . 2_665 ?
N3 C9 S3 122.0(5) . . ?
N3 C9 C10 112.5(6) . . ?
C10 C9 S3 125.5(5) . . ?
C9 C10 H10A 111.0 . . ?
C9 C10 H10B 111.0 . . ?
C9 C10 C11 103.7(5) . . ?
H10A C10 H10B 109.0 . . ?
C11 C10 H10A 111.0 . . ?
C11 C10 H10B 111.0 . . ?
C10 C11 H11A 111.0 . . ?
C10 C11 H11B 111.0 . . ?
H11A C11 H11B 109.0 . . ?
C12 C11 C10 103.8(6) . . ?
C12 C11 H11A 111.0 . . ?
C12 C11 H11B 111.0 . . ?
O3 C12 N3 123.4(6) . . ?
O3 C12 C11 125.9(7) . . ?
N3 C12 C11 110.7(6) . . ?
N4 C13 S4 122.4(4) . . ?
N4 C13 C14 113.3(6) . . ?
C14 C13 S4 124.3(5) . . ?
C13 C14 H14A 111.2 . . ?
C13 C14 H14B 111.2 . . ?
C13 C14 C15 103.0(6) . . ?
H14A C14 H14B 109.1 . . ?
C15 C14 H14A 111.2 . . ?
C15 C14 H14B 111.2 . . ?
C14 C15 H15A 110.8 . . ?
C14 C15 H15B 110.8 . . ?
H15A C15 H15B 108.9 . . ?
C16 C15 C14 104.8(5) . . ?
C16 C15 H15A 110.8 . . ?
C16 C15 H15B 110.8 . . ?
O4 C16 N4 123.6(6) . . ?
O4 C16 C15 127.2(6) . . ?
N4 C16 C15 109.2(6) . . ?
O6 C18 H18A 109.5 . . ?
O6 C18 H18B 109.5 . . ?
O6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 S1 C1 N1 -1.7(6) . . . . ?
Mo1 S1 C1 C2 175.2(5) . . . . ?
Mo1 S2 C5 N2 5.7(6) . . . . ?
Mo1 S2 C5 C6 -173.9(5) . . . . ?
Mo1 N1 C1 S1 -1.3(7) 2_676 . . . ?
Mo1 N1 C1 C2 -178.5(4) 2_676 . . . ?
Mo1 N1 C4 O1 0.0(10) 2_676 . . . ?
Mo1 N1 C4 C3 179.1(4) 2_676 . . . ?
Mo1 N2 C5 S2 -5.7(8) 2_676 . . . ?
Mo1 N2 C5 C6 173.9(4) 2_676 . . . ?
Mo1 N2 C8 O2 11.4(10) 2_676 . . . ?
Mo1 N2 C8 C7 -169.9(4) 2_676 . . . ?
S1 C1 C2 C3 -176.2(5) . . . . ?
S2 C5 C6 C7 177.7(5) . . . . ?
N1 C1 C2 C3 0.9(7) . . . . ?
N2 C5 C6 C7 -2.0(8) . . . . ?
C1 N1 C4 O1 -175.2(6) . . . . ?
C1 N1 C4 C3 3.9(7) . . . . ?
C1 C2 C3 C4 1.4(7) . . . . ?
C2 C3 C4 O1 175.9(7) . . . . ?
C2 C3 C4 N1 -3.2(7) . . . . ?
C4 N1 C1 S1 174.2(4) . . . . ?
C4 N1 C1 C2 -3.0(7) . . . . ?
C5 N2 C8 O2 -172.1(6) . . . . ?
C5 N2 C8 C7 6.6(7) . . . . ?
C5 C6 C7 C8 5.7(7) . . . . ?
C6 C7 C8 O2 171.0(7) . . . . ?
C6 C7 C8 N2 -7.6(7) . . . . ?
C8 N2 C5 S2 177.5(5) . . . . ?
C8 N2 C5 C6 -2.8(8) . . . . ?
Mo2 S3 C9 N3 -5.6(6) . . . . ?
Mo2 S3 C9 C10 173.7(5) . . . . ?
Mo2 S4 C13 N4 2.3(6) . . . . ?
Mo2 S4 C13 C14 -176.9(5) . . . . ?
Mo2 N3 C9 S3 4.9(7) 2_665 . . . ?
Mo2 N3 C9 C10 -174.4(4) 2_665 . . . ?
Mo2 N3 C12 O3 -7.4(10) 2_665 . . . ?
Mo2 N3 C12 C11 175.1(5) 2_665 . . . ?
Mo2 N4 C13 S4 -0.7(7) 2_665 . . . ?
Mo2 N4 C13 C14 178.6(4) 2_665 . . . ?
Mo2 N4 C16 O4 -0.1(10) 2_665 . . . ?
Mo2 N4 C16 C15 -179.8(4) 2_665 . . . ?
S3 C9 C10 C11 178.5(5) . . . . ?
S4 C13 C14 C15 179.9(5) . . . . ?
N3 C9 C10 C11 -2.2(8) . . . . ?
N4 C13 C14 C15 0.7(7) . . . . ?
C9 N3 C12 O3 176.7(6) . . . . ?
C9 N3 C12 C11 -0.8(8) . . . . ?
C9 C10 C11 C12 1.6(7) . . . . ?
C10 C11 C12 O3 -178.0(7) . . . . ?
C10 C11 C12 N3 -0.6(8) . . . . ?
C12 N3 C9 S3 -178.8(4) . . . . ?
C12 N3 C9 C10 1.9(7) . . . . ?
C13 N4 C16 O4 177.1(6) . . . . ?
C13 N4 C16 C15 -2.7(7) . . . . ?
C13 C14 C15 C16 -2.1(7) . . . . ?
C14 C15 C16 O4 -176.8(7) . . . . ?
C14 C15 C16 N4 3.0(7) . . . . ?
C16 N4 C13 S4 -178.1(5) . . . . ?
C16 N4 C13 C14 1.2(7) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 983534'
###################################################################
### X-ray Crystallographic Data for 2_CH2Cl2_100K, 3, 4_MeOH_100K
### 4_MeOH_200K, and 5
###################################################################
data_global
loop_
_publ_author_name
_publ_author_email
_publ_author_address
'Brian S. Dolinar' ? ?
'John F. Berry' ? ?

_publ_contact_author_address     ?
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
;


### END 4a_MeOH_100K
data_4a_MeOH_200K

_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H16 Mo2 N4 O4 S4, 2(C H4 O)'
_chemical_formula_sum            'C18 H24 Mo2 N4 O6 S4'
_chemical_formula_weight         712.53
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.0133(5)
_cell_length_b                   14.7157(12)
_cell_length_c                   10.0976(7)
_cell_angle_alpha                90
_cell_angle_beta                 111.403(4)
_cell_angle_gamma                90
_cell_volume                     1246.95(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      72.35
_cell_measurement_theta_min      5.27
_shelx_estimated_absorpt_T_max   0.485
_shelx_estimated_absorpt_T_min   0.333
_exptl_absorpt_coefficient_mu    11.745
_exptl_absorpt_correction_T_max  0.6221
_exptl_absorpt_correction_T_min  0.4880
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0440 before and 0.0344 after correction.
The Ratio of minimum to maximum transmission is 0.7844.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.072
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20908
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.392
_diffrn_reflns_theta_min         5.271
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\ ω and 0.6\ φ scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2323
_reflns_number_total             2451
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2012.14-3 (Bruker-AXS, 2012)'
_computing_data_reduction        'SAINT+ Ver. 7.68A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2451
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0182
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0244P)²+0.8012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0454
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-C9 \\sim O3A-C9A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3 \\sim O3A \\sim C9A \\sim C9: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O3A)=Sof(H3AA)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(1)
 Sof(O3)=Sof(H3)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B)
5.b Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9(H9A,H9B,H9C)
5.c Idealised tetrahedral OH refined as rotating group:
 O3A(H3AA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.56805(2) 0.46223(2) 0.09294(2) 0.02065(6) Uani 1 1 d . . . . .
S1 S 0.73365(6) 0.59576(4) 0.21180(5) 0.02957(11) Uani 1 1 d . . . . .
S2 S 0.37782(6) 0.49305(4) 0.21537(5) 0.02869(11) Uani 1 1 d . . . . .
O1 O 0.4035(2) 0.76149(12) -0.21794(19) 0.0485(4) Uani 1 1 d . . . . .
O2 O 0.0956(2) 0.67863(15) -0.2068(2) 0.0551(5) Uani 1 1 d . . . . .
N1 N 0.53964(19) 0.66900(11) -0.02667(18) 0.0248(3) Uani 1 1 d . . . . .
N2 N 0.24509(19) 0.58441(11) -0.02282(18) 0.0256(3) Uani 1 1 d . . . . .
C1 C 0.6548(2) 0.68194(14) 0.0998(2) 0.0272(4) Uani 1 1 d . . . . .
C2 C 0.7022(3) 0.78018(15) 0.1300(3) 0.0373(5) Uani 1 1 d . . . . .
H2A H 0.8158 0.7893 0.1441 0.045 Uiso 1 1 calc R . . . .
H2B H 0.6835 0.8019 0.2154 0.045 Uiso 1 1 calc R . . . .
C3 C 0.5940(4) 0.82857(16) -0.0029(3) 0.0462(6) Uani 1 1 d . . . . .
H3A H 0.5230 0.8719 0.0202 0.055 Uiso 1 1 calc R . . . .
H3B H 0.6572 0.8620 -0.0492 0.055 Uiso 1 1 calc R . . . .
C4 C 0.4989(3) 0.75353(15) -0.0978(2) 0.0334(5) Uani 1 1 d . . . . .
C5 C 0.2404(2) 0.56092(14) 0.1024(2) 0.0274(4) Uani 1 1 d . . . . .
C6 C 0.1025(3) 0.60279(17) 0.1319(3) 0.0365(5) Uani 1 1 d . . . . .
H6A H 0.1406 0.6422 0.2172 0.044 Uiso 1 1 calc R . . . .
H6B H 0.0315 0.5554 0.1457 0.044 Uiso 1 1 calc R . . . .
C7 C 0.0180(3) 0.65816(17) -0.0022(3) 0.0409(5) Uani 1 1 d . . . . .
H7A H -0.0919 0.6357 -0.0521 0.049 Uiso 1 1 calc R . . . .
H7B H 0.0135 0.7232 0.0211 0.049 Uiso 1 1 calc R . . . .
C8 C 0.1180(3) 0.64462(16) -0.0925(3) 0.0352(5) Uani 1 1 d . . . . .
O3A O 0.778(3) 0.4152(10) 0.3476(14) 0.059(5) Uani 0.148(8) 1 d . . P A 2
H3AA H 0.8556 0.3852 0.3428 0.088 Uiso 0.148(8) 1 calc GR . P A 2
C9A C 0.776(4) 0.408(3) 0.484(2) 0.057(5) Uani 0.148(8) 1 d . . P A 2
H9AA H 0.8850 0.4096 0.5541 0.085 Uiso 0.148(8) 1 calc GR . P A 2
H9AB H 0.7247 0.3510 0.4935 0.085 Uiso 0.148(8) 1 calc GR . P A 2
H9AC H 0.7154 0.4593 0.5019 0.085 Uiso 0.148(8) 1 calc GR . P A 2
O3 O 0.6918(4) 0.39623(19) 0.3582(3) 0.0491(8) Uani 0.852(8) 1 d . . P A 1
H3 H 0.691(5) 0.339(3) 0.335(4) 0.073(14) Uiso 0.852(8) 1 d . . P A 1
C9 C 0.8335(6) 0.4196(5) 0.4685(5) 0.0722(17) Uani 0.852(8) 1 d . . P A 1
H9A H 0.9182 0.4276 0.4304 0.108 Uiso 0.852(8) 1 calc GR . P A 1
H9B H 0.8633 0.3711 0.5399 0.108 Uiso 0.852(8) 1 calc GR . P A 1
H9C H 0.8183 0.4764 0.5126 0.108 Uiso 0.852(8) 1 calc GR . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Mo1 2.1408(3) 3_665 ?
Mo1 S1 2.4944(5) . ?
Mo1 S2 2.4941(5) . ?
Mo1 N1 2.1553(16) 3_665 ?
Mo1 N2 2.1632(16) 3_665 ?
S1 C1 1.675(2) . ?
S2 C5 1.674(2) . ?
O1 C4 1.209(3) . ?
O2 C8 1.206(3) . ?
N1 Mo1 2.1552(16) 3_665 ?
N1 C1 1.333(3) . ?
N1 C4 1.416(3) . ?
N2 Mo1 2.1632(16) 3_665 ?
N2 C5 1.326(3) . ?
N2 C8 1.416(3) . ?
C1 C2 1.507(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.518(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.508(3) . ?
C5 C6 1.511(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.525(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.510(3) . ?
O3A H3AA 0.8400 . ?
O3A C9A 1.394(10) . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
O3 H3 0.87(4) . ?
O3 C9 1.397(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

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
Mo1 Mo1 S1 93.646(16) 3_665 . ?
Mo1 Mo1 S2 93.588(15) 3_665 . ?
Mo1 Mo1 N1 98.28(5) 3_665 3_665 ?
Mo1 Mo1 N2 98.23(5) 3_665 3_665 ?
S2 Mo1 S1 90.984(18) . . ?
N1 Mo1 S1 167.91(5) 3_665 . ?
N1 Mo1 S2 90.21(4) 3_665 . ?
N1 Mo1 N2 86.00(6) 3_665 3_665 ?
N2 Mo1 S1 90.39(4) 3_665 . ?
N2 Mo1 S2 167.99(5) 3_665 . ?
C1 S1 Mo1 103.86(7) . . ?
C5 S2 Mo1 104.02(7) . . ?
C1 N1 Mo1 122.03(14) . 3_665 ?
C1 N1 C4 109.13(17) . . ?
C4 N1 Mo1 128.71(14) . 3_665 ?
C5 N2 Mo1 121.93(14) . 3_665 ?
C5 N2 C8 109.57(17) . . ?
C8 N2 Mo1 128.44(14) . 3_665 ?
N1 C1 S1 121.93(16) . . ?
N1 C1 C2 113.27(19) . . ?
C2 C1 S1 124.79(16) . . ?
C1 C2 H2A 111.1 . . ?
C1 C2 H2B 111.1 . . ?
C1 C2 C3 103.18(18) . . ?
H2A C2 H2B 109.1 . . ?
C3 C2 H2A 111.1 . . ?
C3 C2 H2B 111.1 . . ?
C2 C3 H3A 110.8 . . ?
C2 C3 H3B 110.8 . . ?
H3A C3 H3B 108.9 . . ?
C4 C3 C2 104.55(18) . . ?
C4 C3 H3A 110.8 . . ?
C4 C3 H3B 110.8 . . ?
O1 C4 N1 123.5(2) . . ?
O1 C4 C3 126.7(2) . . ?
N1 C4 C3 109.80(19) . . ?
N2 C5 S2 122.15(16) . . ?
N2 C5 C6 113.36(19) . . ?
C6 C5 S2 124.48(17) . . ?
C5 C6 H6A 111.2 . . ?
C5 C6 H6B 111.2 . . ?
C5 C6 C7 102.86(18) . . ?
H6A C6 H6B 109.1 . . ?
C7 C6 H6A 111.2 . . ?
C7 C6 H6B 111.2 . . ?
C6 C7 H7A 110.8 . . ?
C6 C7 H7B 110.8 . . ?
H7A C7 H7B 108.9 . . ?
C8 C7 C6 104.53(18) . . ?
C8 C7 H7A 110.8 . . ?
C8 C7 H7B 110.8 . . ?
O2 C8 N2 123.9(2) . . ?
O2 C8 C7 126.5(2) . . ?
N2 C8 C7 109.62(19) . . ?
C9A O3A H3AA 109.5 . . ?
O3A C9A H9AA 109.5 . . ?
O3A C9A H9AB 109.5 . . ?
O3A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C9 O3 H3 112(3) . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 S1 C1 N1 -5.52(18) . . . . ?
Mo1 S1 C1 C2 173.49(16) . . . . ?
Mo1 S2 C5 N2 2.06(18) . . . . ?
Mo1 S2 C5 C6 -176.68(16) . . . . ?
Mo1 N1 C1 S1 4.6(2) 3_665 . . . ?
Mo1 N1 C1 C2 -174.55(13) 3_665 . . . ?
Mo1 N1 C4 O1 -8.1(3) 3_665 . . . ?
Mo1 N1 C4 C3 173.15(15) 3_665 . . . ?
Mo1 N2 C5 S2 -0.3(2) 3_665 . . . ?
Mo1 N2 C5 C6 178.52(13) 3_665 . . . ?
Mo1 N2 C8 O2 0.9(3) 3_665 . . . ?
Mo1 N2 C8 C7 -179.36(14) 3_665 . . . ?
S1 C1 C2 C3 -179.04(17) . . . . ?
S2 C5 C6 C7 179.21(16) . . . . ?
N1 C1 C2 C3 0.0(2) . . . . ?
N2 C5 C6 C7 0.4(2) . . . . ?
C1 N1 C4 O1 176.0(2) . . . . ?
C1 N1 C4 C3 -2.8(2) . . . . ?
C1 C2 C3 C4 -1.6(2) . . . . ?
C2 C3 C4 O1 -176.0(2) . . . . ?
C2 C3 C4 N1 2.7(3) . . . . ?
C4 N1 C1 S1 -179.20(14) . . . . ?
C4 N1 C1 C2 1.7(2) . . . . ?
C5 N2 C8 O2 178.1(2) . . . . ?
C5 N2 C8 C7 -2.1(2) . . . . ?
C5 C6 C7 C8 -1.5(2) . . . . ?
C6 C7 C8 O2 -178.0(2) . . . . ?
C6 C7 C8 N2 2.3(3) . . . . ?
C8 N2 C5 S2 -177.78(15) . . . . ?
C8 N2 C5 C6 1.1(2) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 983535'
###################################################################
### X-ray Crystallographic Data for 2_CH2Cl2_100K, 3, 4_MeOH_100K
### 4_MeOH_200K, and 5
###################################################################
data_global
loop_
_publ_author_name
_publ_author_email
_publ_author_address
'Brian S. Dolinar' ? ?
'John F. Berry' ? ?

_publ_contact_author_address     ?
_publ_contact_author_email       berry@chem.wisc.edu
_publ_contact_author_name        'John F. Berry'
_publ_contact_author_phone       ?
_publ_section_references         
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122
;


### END 4a_MeOH_200K
data_5_100K
_audit_creation_date             2013-12-18
_audit_creation_method           
;
  Olex2 1.2-alpha
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_publ_contact_author_address     ?
_publ_contact_author_email       ?
_publ_contact_author_phone       ?
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H14 Mo2 N2 O6 S2'
_chemical_formula_sum            'C12 H14 Mo2 N2 O6 S2'
_chemical_formula_weight         538.25
_chemical_melting_point          ?
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'
Mo Mo -1.6832 0.6857 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_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'

_cell_length_a                   5.450(2)
_cell_length_b                   8.227(3)
_cell_length_c                   18.268(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.805(15)
_cell_angle_gamma                90
_cell_volume                     813.3(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3858
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.25
_exptl_absorpt_coefficient_mu    1.831
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1707 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.9033.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.198
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.025
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.736
_diffrn_reflns_theta_min         2.246
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.5° ω and 0.5° φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1448
_reflns_number_total             1548
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.090
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.509
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1548
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0570
_refine_ls_restrained_S_all      1.491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+15.4147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1337
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2A(0.024) H2B(0.024) H3A(0.025) H3B(0.025) H6A(0.022) H6B(0.022)
 H6C(0.022)
 Fixed X: H2A(0.5066) H2B(0.3466) H3A(-0.005) H3B(0.1542) H6A(0.0914)
 H6B(0.2296) H6C(-0.029)
 Fixed Y: H2A(0.4096) H2B(0.5076) H3A(0.4047) H3B(0.3119) H6A(0.3997)
 H6B(0.3188) H6C(0.2469)
 Fixed Z: H2A(0.2999) H2B(0.3543) H3A(0.2947) H3B(0.2386) H6A(0.6132)
 H6B(0.6865) H6C(0.6498)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.33098(13) -0.04016(10) 0.47154(4) 0.0099(2) Uani 1 1 d . . . . .
S1 S 0.6948(4) 0.2905(3) 0.45314(14) 0.0197(5) Uani 1 1 d . U . . .
O1 O -0.0597(12) 0.0719(8) 0.3130(4) 0.0207(15) Uani 1 1 d . U . . .
O2 O 0.1372(10) 0.1035(7) 0.5435(3) 0.0083(11) Uani 1 1 d . U . . .
O3 O 0.4932(10) 0.1817(8) 0.6036(3) 0.0117(12) Uani 1 1 d . U . . .
N1 N 0.2865(12) 0.1523(9) 0.3913(4) 0.0115(13) Uani 1 1 d . U . . .
C1 C 0.4429(16) 0.2757(12) 0.3919(5) 0.0167(14) Uani 1 1 d . U . . .
C2 C 0.3756(17) 0.3998(13) 0.3328(5) 0.0197(16) Uani 1 1 d . U . . .
H2A H 0.5066 0.4096 0.2999 0.024 Uiso 1 1 calc R U . . .
H2B H 0.3466 0.5076 0.3543 0.024 Uiso 1 1 calc R U . . .
C3 C 0.1360(18) 0.3304(13) 0.2913(5) 0.0205(16) Uani 1 1 d . U . . .
H3A H -0.0050 0.4047 0.2947 0.025 Uiso 1 1 calc R U . . .
H3B H 0.1542 0.3119 0.2386 0.025 Uiso 1 1 calc R U . . .
C4 C 0.0998(17) 0.1716(12) 0.3302(5) 0.0172(15) Uani 1 1 d . U . . .
C5 C 0.2594(15) 0.1854(11) 0.5941(5) 0.0100(13) Uani 1 1 d . U . . .
C6 C 0.1265(16) 0.2972(12) 0.6398(5) 0.0147(18) Uani 1 1 d . U . . .
H6A H 0.0914 0.3997 0.6132 0.022 Uiso 1 1 calc R U . . .
H6B H 0.2296 0.3188 0.6865 0.022 Uiso 1 1 calc R U . . .
H6C H -0.0290 0.2469 0.6498 0.022 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 Mo1 2.1113(16) 3_656 ?
Mo1 S1 2.490(3) 3_656 ?
Mo1 O2 2.137(6) . ?
Mo1 O3 2.115(6) 3_656 ?
Mo1 N1 2.151(8) . ?
S1 Mo1 2.490(3) 3_656 ?
S1 C1 1.669(9) . ?
O1 C4 1.209(11) . ?
O2 C5 1.267(10) . ?
O3 Mo1 2.115(6) 3_656 ?
O3 C5 1.266(10) . ?
N1 C1 1.326(12) . ?
N1 C4 1.428(11) . ?
C1 C2 1.499(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.540(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.511(14) . ?
C5 C6 1.487(12) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
Mo1 Mo1 S1 95.16(7) 3_656 3_656 ?
Mo1 Mo1 O2 89.42(16) 3_656 . ?
Mo1 Mo1 O3 93.21(16) 3_656 3_656 ?
Mo1 Mo1 N1 97.3(2) 3_656 . ?
O2 Mo1 S1 93.06(17) . 3_656 ?
O2 Mo1 N1 89.3(2) . . ?
O3 Mo1 S1 87.89(18) 3_656 3_656 ?
O3 Mo1 O2 177.1(2) 3_656 . ?
O3 Mo1 N1 89.2(3) 3_656 . ?
N1 Mo1 S1 167.4(2) . 3_656 ?
C1 S1 Mo1 102.4(4) . 3_656 ?
C5 O2 Mo1 119.2(5) . . ?
C5 O3 Mo1 116.7(5) . 3_656 ?
C1 N1 Mo1 122.5(6) . . ?
C1 N1 C4 108.6(8) . . ?
C4 N1 Mo1 128.8(6) . . ?
N1 C1 S1 122.6(7) . . ?
N1 C1 C2 114.4(8) . . ?
C2 C1 S1 123.0(7) . . ?
C1 C2 H2A 111.2 . . ?
C1 C2 H2B 111.2 . . ?
C1 C2 C3 102.9(8) . . ?
H2A C2 H2B 109.1 . . ?
C3 C2 H2A 111.2 . . ?
C3 C2 H2B 111.2 . . ?
C2 C3 H3A 111.0 . . ?
C2 C3 H3B 111.0 . . ?
H3A C3 H3B 109.0 . . ?
C4 C3 C2 103.8(8) . . ?
C4 C3 H3A 111.0 . . ?
C4 C3 H3B 111.0 . . ?
O1 C4 N1 123.5(9) . . ?
O1 C4 C3 126.4(8) . . ?
N1 C4 C3 110.1(8) . . ?
O2 C5 C6 119.3(7) . . ?
O3 C5 O2 121.4(8) . . ?
O3 C5 C6 119.1(8) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 S1 C1 N1 0.0(8) 3_656 . . . ?
Mo1 S1 C1 C2 -179.5(7) 3_656 . . . ?
Mo1 O2 C5 O3 -1.2(11) . . . . ?
Mo1 O2 C5 C6 174.4(6) . . . . ?
Mo1 O3 C5 O2 2.5(11) 3_656 . . . ?
Mo1 O3 C5 C6 -173.2(6) 3_656 . . . ?
Mo1 N1 C1 S1 2.2(11) . . . . ?
Mo1 N1 C1 C2 -178.3(6) . . . . ?
Mo1 N1 C4 O1 -3.7(13) . . . . ?
Mo1 N1 C4 C3 177.1(6) . . . . ?
S1 C1 C2 C3 179.1(7) . . . . ?
N1 C1 C2 C3 -0.4(11) . . . . ?
C1 N1 C4 O1 175.3(9) . . . . ?
C1 N1 C4 C3 -3.9(10) . . . . ?
C1 C2 C3 C4 -1.9(10) . . . . ?
C2 C3 C4 O1 -175.6(10) . . . . ?
C2 C3 C4 N1 3.5(10) . . . . ?
C4 N1 C1 S1 -176.9(7) . . . . ?
C4 N1 C1 C2 2.7(11) . . . . ?

_shelx_estimated_absorpt_T_max   0.956
_shelx_estimated_absorpt_T_min   0.906
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-3
### END 4b_100K

# start Validation Reply Form
_vrf_PLAT021_4a_MeOH_100K        
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      1.555       
RESPONSE: The final refinement was run against HKLF5 data.
;
_vrf_PLAT094_4a_MeOH_200K        
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.08       
RESPONSE: The maximum peak is in the vicinity of the heaviest atoms (Mo)
It was interpreted as noise.
;
# end Validation Reply Form
### END CIF
_database_code_depnum_ccdc_archive 'CCDC 983536'
