Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2003

data_global

_publ_contact_author_email       suriel@posta.unizar.es

_publ_contact_author_name        'Dr Santiago Uriel'
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?
_publ_contact_author_address     
;
Department of Organic Chemistry
C.P.S. Universidad de Zaragoza
Marķa de Luna 3
Zaragoza
50015
SPAIN
;

_publ_section_title              
;
Synthesis and Third-order Nonlinear Optical
Properties of [Mo3(m3-S)(m2-S2)3]4+ Clusters with Maleonitriledithiolate,
Oxalate and Thiocyanate Ligands
;

loop_
_publ_author_name
'Santiago Uriel'
'Juan M. Garriga'
'Mark Humphrey'
'Rosa Llusar'
'Nigel T. Lucas'
S.Marek
;
A.J.Usher
;
'Cristian Vicent'

data_(TBA)2[Mo3S7(mnt)3]
_database_code_CSD               211454

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H72 Mo3 N8 S13'
_chemical_formula_weight         1417.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   16.019(3)
_cell_length_b                   27.534(5)
_cell_length_c                   15.050(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.949(4)
_cell_angle_gamma                90.00
_cell_volume                     6557(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2904
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_absorpt_correction_T_min  1.195624
_exptl_absorpt_correction_T_max  1.955922
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11665
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         20.81
_reflns_number_total             3519
_reflns_number_gt                2203
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w==1/[\s^2^(Fo^2^)+(0.0955P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3519
_refine_ls_number_parameters     296
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1651
_refine_ls_wR_factor_gt          0.1437
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.01502(7) 0.0000 0.69455(9) 0.0488(4) Uani 1 2 d S . .
Mo2 Mo 0.16534(5) 0.05006(3) 0.73306(6) 0.0510(4) Uani 1 1 d . . .
S1 S 0.1057(2) 0.0000 0.8345(3) 0.0535(10) Uani 1 2 d S . .
S3 S 0.02286(17) 0.09053(10) 0.7044(2) 0.0634(8) Uani 1 1 d . . .
S2 S 0.06563(16) 0.05940(10) 0.59809(19) 0.0592(8) Uani 1 1 d . . .
S5 S 0.2962(2) 0.0000 0.7702(3) 0.0679(12) Uani 1 2 d S . .
S4 S 0.2401(2) 0.0000 0.6418(3) 0.0647(12) Uani 1 2 d S . .
S6 S -0.0865(2) 0.0000 0.7995(3) 0.0698(13) Uani 1 2 d S . .
S7 S -0.1150(2) 0.0000 0.5789(3) 0.0651(12) Uani 1 2 d S . .
S8 S 0.20595(18) 0.09508(10) 0.8728(2) 0.0651(9) Uani 1 1 d . . .
S9 S 0.23815(19) 0.11802(12) 0.6678(2) 0.0768(10) Uani 1 1 d . . .
N1 N -0.3133(11) 0.0000 0.8185(15) 0.163(9) Uani 1 2 d S . .
N2 N -0.3474(8) 0.0000 0.5512(12) 0.098(6) Uani 1 2 d S . .
N3 N 0.3508(8) 0.2311(5) 0.7169(11) 0.149(6) Uani 1 1 d . . .
N4 N 0.3200(9) 0.2028(5) 0.9741(9) 0.140(6) Uani 1 1 d . . .
C1 C -0.1858(9) 0.0000 0.7320(13) 0.063(5) Uani 1 2 d S . .
C2 C -0.1959(9) 0.0000 0.6414(14) 0.067(5) Uani 1 2 d S . .
C3 C -0.2585(12) 0.0000 0.7791(14) 0.091(6) Uani 1 2 d S . .
C4 C -0.2824(11) 0.0000 0.5900(13) 0.069(5) Uani 1 2 d S . .
C5 C 0.2603(7) 0.1459(4) 0.8422(10) 0.073(4) Uani 1 1 d . . .
C6 C 0.2713(6) 0.1549(4) 0.7593(9) 0.069(3) Uani 1 1 d . . .
C8 C 0.3153(9) 0.1981(5) 0.7375(10) 0.094(4) Uani 1 1 d . . .
C7 C 0.2919(9) 0.1786(5) 0.9145(11) 0.096(4) Uani 1 1 d . . .
N10 N 0.0000 -0.1874(4) 1.0000 0.060(3) Uani 1 2 d S . .
C10 C -0.0221(10) -0.2224(6) 1.0707(10) 0.121(5) Uiso 1 1 d . . .
H10A H -0.0725 -0.2398 1.0442 0.145 Uiso 1 1 calc R . .
H10B H 0.0231 -0.2462 1.0813 0.145 Uiso 1 1 calc R . .
C11 C -0.0358(12) -0.2059(7) 1.1532(12) 0.155(7) Uiso 1 1 d . . .
H11A H -0.0781 -0.1804 1.1458 0.186 Uiso 1 1 calc R . .
H11B H 0.0160 -0.1928 1.1864 0.186 Uiso 1 1 calc R . .
C12 C -0.0671(13) -0.2498(8) 1.2055(13) 0.160(8) Uani 1 1 d . . .
H12A H -0.1213 -0.2617 1.1757 0.192 Uiso 1 1 calc R . .
H12B H -0.0266 -0.2762 1.2110 0.192 Uiso 1 1 calc R . .
C13 C -0.0744(12) -0.2289(6) 1.2950(14) 0.166(8) Uani 1 1 d . . .
H13A H -0.0927 -0.2537 1.3325 0.249 Uiso 1 1 calc R . .
H13B H -0.1147 -0.2029 1.2878 0.249 Uiso 1 1 calc R . .
H13C H -0.0203 -0.2168 1.3225 0.249 Uiso 1 1 calc R . .
C14 C -0.0663(9) -0.1518(5) 0.9562(10) 0.111(5) Uiso 1 1 d . . .
H14A H -0.0780 -0.1296 1.0027 0.133 Uiso 1 1 calc R . .
H14B H -0.0407 -0.1329 0.9133 0.133 Uiso 1 1 calc R . .
C15 C -0.1429(15) -0.1682(8) 0.9125(15) 0.206(10) Uiso 1 1 d . . .
H15A H -0.1757 -0.1821 0.9552 0.247 Uiso 1 1 calc R . .
H15B H -0.1345 -0.1930 0.8689 0.247 Uiso 1 1 calc R . .
C16 C -0.1924(11) -0.1212(6) 0.8618(11) 0.142(7) Uani 1 1 d . . .
H16A H -0.2024 -0.0966 0.9049 0.170 Uiso 1 1 calc R . .
H16B H -0.1603 -0.1071 0.8187 0.170 Uiso 1 1 calc R . .
C17 C -0.2705(14) -0.1415(9) 0.8175(13) 0.226(12) Uani 1 1 d . . .
H17A H -0.3038 -0.1165 0.7847 0.339 Uiso 1 1 calc R . .
H17B H -0.3011 -0.1551 0.8615 0.339 Uiso 1 1 calc R . .
H17C H -0.2588 -0.1665 0.7766 0.339 Uiso 1 1 calc R . .
N20 N 0.5000 0.1250(5) 0.5000 0.077(4) Uani 1 2 d S . .
C20 C 0.4947(7) 0.0927(5) 0.5826(11) 0.094(5) Uani 1 1 d . . .
H20A H 0.4435 0.0735 0.5694 0.113 Uiso 1 1 calc R . .
H20B H 0.5419 0.0702 0.5884 0.113 Uiso 1 1 calc R . .
C21 C 0.4948(8) 0.1153(6) 0.6700(10) 0.104(5) Uani 1 1 d . . .
H21A H 0.4465 0.1368 0.6673 0.124 Uiso 1 1 calc R . .
H21B H 0.5457 0.1345 0.6857 0.124 Uiso 1 1 calc R . .
C22 C 0.4907(11) 0.0758(7) 0.7432(11) 0.138(6) Uiso 1 1 d . . .
H22A H 0.4398 0.0566 0.7269 0.165 Uiso 1 1 calc R . .
H22B H 0.5388 0.0542 0.7449 0.165 Uiso 1 1 calc R . .
C23 C 0.4909(11) 0.0973(7) 0.8356(12) 0.174(8) Uiso 1 1 d . . .
H23A H 0.4876 0.0717 0.8782 0.260 Uiso 1 1 calc R . .
H23B H 0.4431 0.1185 0.8344 0.260 Uiso 1 1 calc R . .
H23C H 0.5420 0.1155 0.8530 0.260 Uiso 1 1 calc R . .
C24 C 0.4216(6) 0.1579(4) 0.4834(8) 0.076(4) Uani 1 1 d . . .
H24A H 0.4183 0.1758 0.5382 0.091 Uiso 1 1 calc R . .
H24B H 0.4294 0.1813 0.4373 0.091 Uiso 1 1 calc R . .
C25 C 0.3398(6) 0.1329(4) 0.4556(9) 0.076(4) Uani 1 1 d . . .
H25A H 0.3302 0.1095 0.5011 0.091 Uiso 1 1 calc R . .
H25B H 0.3407 0.1157 0.3996 0.091 Uiso 1 1 calc R . .
C26 C 0.2689(7) 0.1708(5) 0.4435(9) 0.094(4) Uani 1 1 d . . .
H26A H 0.2782 0.1932 0.3963 0.112 Uiso 1 1 calc R . .
H26B H 0.2714 0.1893 0.4988 0.112 Uiso 1 1 calc R . .
C27 C 0.1796(7) 0.1482(6) 0.4194(9) 0.116(5) Uani 1 1 d . . .
H27A H 0.1379 0.1736 0.4132 0.174 Uiso 1 1 calc R . .
H27B H 0.1695 0.1264 0.4663 0.174 Uiso 1 1 calc R . .
H27C H 0.1760 0.1307 0.3638 0.174 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0315(8) 0.0432(8) 0.0702(10) 0.000 0.0032(6) 0.000
Mo2 0.0360(6) 0.0509(6) 0.0636(7) 0.0002(5) 0.0001(4) -0.0058(4)
S1 0.045(2) 0.052(3) 0.062(3) 0.000 0.0050(19) 0.000
S3 0.0504(17) 0.0472(18) 0.090(2) -0.0012(16) 0.0015(16) 0.0016(14)
S2 0.0428(16) 0.0581(19) 0.072(2) 0.0063(16) -0.0049(14) -0.0059(14)
S5 0.042(2) 0.085(3) 0.074(3) 0.000 0.000(2) 0.000
S4 0.044(2) 0.084(3) 0.066(3) 0.000 0.008(2) 0.000
S6 0.043(2) 0.080(3) 0.088(3) 0.000 0.013(2) 0.000
S7 0.030(2) 0.075(3) 0.087(3) 0.000 -0.003(2) 0.000
S8 0.0561(18) 0.062(2) 0.074(2) -0.0071(16) -0.0008(15) -0.0114(15)
S9 0.065(2) 0.078(2) 0.085(2) 0.0143(19) 0.0046(17) -0.0251(17)
N1 0.064(13) 0.23(2) 0.21(2) 0.000 0.052(14) 0.000
N2 0.026(8) 0.087(12) 0.175(17) 0.000 -0.003(10) 0.000
N3 0.109(11) 0.114(12) 0.213(16) 0.036(11) -0.007(10) -0.054(9)
N4 0.153(13) 0.139(12) 0.128(11) -0.053(10) 0.020(9) -0.079(10)
C1 0.041(10) 0.053(10) 0.092(13) 0.000 -0.002(10) 0.000
C2 0.029(9) 0.045(10) 0.122(16) 0.000 -0.001(10) 0.000
C3 0.046(12) 0.105(16) 0.128(18) 0.000 0.028(12) 0.000
C4 0.050(12) 0.047(10) 0.119(16) 0.000 0.037(11) 0.000
C5 0.060(8) 0.061(8) 0.093(10) -0.004(8) -0.007(7) -0.014(6)
C6 0.043(7) 0.066(9) 0.094(10) 0.007(8) -0.005(7) -0.015(6)
C8 0.088(11) 0.076(10) 0.112(12) 0.008(9) -0.006(9) -0.020(9)
C7 0.091(11) 0.073(10) 0.123(13) -0.012(10) 0.009(9) -0.022(8)
N10 0.065(8) 0.040(7) 0.071(9) 0.000 0.003(7) 0.000
C12 0.156(17) 0.16(2) 0.152(17) 0.077(17) -0.005(15) -0.041(15)
C13 0.166(19) 0.122(16) 0.21(2) 0.062(17) 0.017(18) 0.032(14)
C16 0.143(15) 0.145(16) 0.119(14) 0.012(12) -0.041(12) 0.060(13)
C17 0.20(2) 0.35(4) 0.122(17) 0.03(2) 0.002(16) -0.05(2)
N20 0.048(9) 0.063(10) 0.119(13) 0.000 0.012(8) 0.000
C20 0.038(7) 0.081(11) 0.160(15) 0.033(10) 0.008(9) -0.003(7)
C21 0.073(10) 0.133(14) 0.107(12) 0.027(11) 0.022(9) 0.018(9)
C24 0.056(8) 0.059(8) 0.109(10) 0.010(7) 0.001(7) 0.010(7)
C25 0.038(7) 0.075(9) 0.115(10) 0.012(7) 0.014(7) -0.007(6)
C26 0.074(9) 0.103(11) 0.099(10) 0.010(9) -0.003(8) 0.010(8)
C27 0.049(8) 0.156(15) 0.136(13) 0.032(11) -0.009(8) -0.002(9)

_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 S1 2.366(4) . ?
Mo1 S2 2.410(3) . ?
Mo1 S2 2.410(3) 6 ?
Mo1 S6 2.437(4) . ?
Mo1 S7 2.498(4) . ?
Mo1 S3 2.499(3) 6 ?
Mo1 S3 2.499(3) . ?
Mo1 Mo2 2.7569(13) . ?
Mo1 Mo2 2.7569(13) 6 ?
Mo2 S1 2.366(3) . ?
Mo2 S4 2.394(3) . ?
Mo2 S2 2.395(3) . ?
Mo2 S8 2.440(3) . ?
Mo2 S9 2.486(3) . ?
Mo2 S5 2.498(3) . ?
Mo2 S3 2.516(3) . ?
Mo2 Mo2 2.7570(19) 6 ?
S1 Mo2 2.366(3) 6 ?
S3 S2 2.026(4) . ?
S5 S4 2.001(6) . ?
S5 Mo2 2.498(3) 6 ?
S4 Mo2 2.394(3) 6 ?
S6 C1 1.749(16) . ?
S7 C2 1.716(17) . ?
S8 C5 1.746(12) . ?
S9 C6 1.727(13) . ?
N1 C3 1.13(2) . ?
N2 C4 1.111(19) . ?
N3 C8 1.141(15) . ?
N4 C7 1.153(16) . ?
C1 C2 1.35(2) . ?
C1 C3 1.45(2) . ?
C2 C4 1.48(2) . ?
C5 C6 1.310(14) . ?
C5 C7 1.442(18) . ?
C6 C8 1.446(17) . ?
N10 C14 1.517(14) 2_557 ?
N10 C14 1.517(14) . ?
N10 C10 1.519(15) . ?
N10 C10 1.519(15) 2_557 ?
C10 C11 1.373(18) . ?
C11 C12 1.57(2) . ?
C12 C13 1.48(2) . ?
C14 C15 1.37(2) . ?
C15 C16 1.64(2) . ?
C16 C17 1.44(2) . ?
N20 C24 1.536(12) 2_656 ?
N20 C24 1.536(12) . ?
N20 C20 1.542(14) 2_656 ?
N20 C20 1.542(14) . ?
C20 C21 1.455(16) . ?
C21 C22 1.557(19) . ?
C22 C23 1.513(19) . ?
C24 C25 1.480(14) . ?
C25 C26 1.533(15) . ?
C26 C27 1.550(15) . ?

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
S1 Mo1 S2 108.60(10) . . ?
S1 Mo1 S2 108.60(10) . 6 ?
S2 Mo1 S2 85.49(14) . 6 ?
S1 Mo1 S6 78.59(14) . . ?
S2 Mo1 S6 135.36(8) . . ?
S2 Mo1 S6 135.36(8) 6 . ?
S1 Mo1 S7 161.90(14) . . ?
S2 Mo1 S7 84.39(10) . . ?
S2 Mo1 S7 84.39(10) 6 . ?
S6 Mo1 S7 83.30(15) . . ?
S1 Mo1 S3 85.93(7) . 6 ?
S2 Mo1 S3 133.96(11) . 6 ?
S2 Mo1 S3 48.71(10) 6 6 ?
S6 Mo1 S3 89.66(7) . 6 ?
S7 Mo1 S3 94.02(7) . 6 ?
S1 Mo1 S3 85.93(7) . . ?
S2 Mo1 S3 48.71(10) . . ?
S2 Mo1 S3 133.96(11) 6 . ?
S6 Mo1 S3 89.66(7) . . ?
S7 Mo1 S3 94.02(7) . . ?
S3 Mo1 S3 171.81(15) 6 . ?
S1 Mo1 Mo2 54.37(8) . . ?
S2 Mo1 Mo2 54.73(7) . . ?
S2 Mo1 Mo2 95.82(8) 6 . ?
S6 Mo1 Mo2 120.86(10) . . ?
S7 Mo1 Mo2 138.83(8) . . ?
S3 Mo1 Mo2 116.88(7) 6 . ?
S3 Mo1 Mo2 56.95(7) . . ?
S1 Mo1 Mo2 54.37(8) . 6 ?
S2 Mo1 Mo2 95.82(8) . 6 ?
S2 Mo1 Mo2 54.73(7) 6 6 ?
S6 Mo1 Mo2 120.86(10) . 6 ?
S7 Mo1 Mo2 138.83(8) . 6 ?
S3 Mo1 Mo2 56.95(7) 6 6 ?
S3 Mo1 Mo2 116.88(7) . 6 ?
Mo2 Mo1 Mo2 60.00(5) . 6 ?
S1 Mo2 S4 108.85(8) . . ?
S1 Mo2 S2 109.09(12) . . ?
S4 Mo2 S2 84.38(12) . . ?
S1 Mo2 S8 79.62(10) . . ?
S4 Mo2 S8 134.17(12) . . ?
S2 Mo2 S8 136.86(11) . . ?
S1 Mo2 S9 162.66(11) . . ?
S4 Mo2 S9 84.24(10) . . ?
S2 Mo2 S9 82.89(10) . . ?
S8 Mo2 S9 83.08(11) . . ?
S1 Mo2 S5 86.73(11) . . ?
S4 Mo2 S5 48.23(13) . . ?
S2 Mo2 S5 132.44(12) . . ?
S8 Mo2 S5 89.17(11) . . ?
S9 Mo2 S5 94.29(10) . . ?
S1 Mo2 S3 85.54(10) . . ?
S4 Mo2 S3 132.66(12) . . ?
S2 Mo2 S3 48.65(10) . . ?
S8 Mo2 S3 92.06(10) . . ?
S9 Mo2 S3 93.88(10) . . ?
S5 Mo2 S3 171.82(10) . . ?
S1 Mo2 Mo1 54.36(9) . . ?
S4 Mo2 Mo1 95.15(8) . . ?
S2 Mo2 Mo1 55.23(7) . . ?
S8 Mo2 Mo1 122.83(8) . . ?
S9 Mo2 Mo1 137.85(8) . . ?
S5 Mo2 Mo1 116.50(6) . . ?
S3 Mo2 Mo1 56.36(7) . . ?
S1 Mo2 Mo2 54.37(6) . 6 ?
S4 Mo2 Mo2 54.85(6) . 6 ?
S2 Mo2 Mo2 96.16(7) . 6 ?
S8 Mo2 Mo2 120.52(7) . 6 ?
S9 Mo2 Mo2 138.82(8) . 6 ?
S5 Mo2 Mo2 56.51(5) . 6 ?
S3 Mo2 Mo2 116.29(7) . 6 ?
Mo1 Mo2 Mo2 60.00(2) . 6 ?
Mo1 S1 Mo2 71.26(11) . 6 ?
Mo1 S1 Mo2 71.26(11) . . ?
Mo2 S1 Mo2 71.26(12) 6 . ?
S2 S3 Mo1 63.34(11) . . ?
S2 S3 Mo2 62.54(10) . . ?
Mo1 S3 Mo2 66.69(8) . . ?
S3 S2 Mo2 68.80(12) . . ?
S3 S2 Mo1 67.95(12) . . ?
Mo2 S2 Mo1 70.04(8) . . ?
S4 S5 Mo2 63.16(13) . 6 ?
S4 S5 Mo2 63.16(13) . . ?
Mo2 S5 Mo2 66.97(10) 6 . ?
S5 S4 Mo2 68.61(14) . . ?
S5 S4 Mo2 68.61(14) . 6 ?
Mo2 S4 Mo2 70.30(11) . 6 ?
C1 S6 Mo1 105.2(7) . . ?
C2 S7 Mo1 103.7(6) . . ?
C5 S8 Mo2 104.9(5) . . ?
C6 S9 Mo2 103.4(4) . . ?
C2 C1 C3 120.9(15) . . ?
C2 C1 S6 122.8(13) . . ?
C3 C1 S6 116.2(14) . . ?
C1 C2 C4 119.0(15) . . ?
C1 C2 S7 125.0(12) . . ?
C4 C2 S7 116.0(14) . . ?
N1 C3 C1 178(2) . . ?
N2 C4 C2 180(2) . . ?
C6 C5 C7 121.1(12) . . ?
C6 C5 S8 123.3(10) . . ?
C7 C5 S8 115.6(11) . . ?
C5 C6 C8 121.0(12) . . ?
C5 C6 S9 125.3(10) . . ?
C8 C6 S9 113.8(10) . . ?
N3 C8 C6 176.8(18) . . ?
N4 C7 C5 176.4(18) . . ?
C14 N10 C14 99.7(13) 2_557 . ?
C14 N10 C10 109.2(8) 2_557 . ?
C14 N10 C10 119.4(8) . . ?
C14 N10 C10 119.4(8) 2_557 2_557 ?
C14 N10 C10 109.2(8) . 2_557 ?
C10 N10 C10 101.0(13) . 2_557 ?
C11 C10 N10 120.7(14) . . ?
C10 C11 C12 107.9(17) . . ?
C13 C12 C11 103.5(18) . . ?
C15 C14 N10 120.6(15) . . ?
C14 C15 C16 107.1(17) . . ?
C17 C16 C15 103.4(18) . . ?
C24 N20 C24 107.9(12) 2_656 . ?
C24 N20 C20 108.9(6) 2_656 2_656 ?
C24 N20 C20 110.8(6) . 2_656 ?
C24 N20 C20 110.8(6) 2_656 . ?
C24 N20 C20 108.9(6) . . ?
C20 N20 C20 109.5(15) 2_656 . ?
C21 C20 N20 119.3(12) . . ?
C20 C21 C22 110.2(14) . . ?
C23 C22 C21 112.4(16) . . ?
C25 C24 N20 116.0(9) . . ?
C24 C25 C26 108.9(9) . . ?
C25 C26 C27 113.3(11) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        20.81
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.121

#======== END

data_(TBA)2[Mo3S7(oxalate)3]
_database_code_CSD               211455

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         (TBA)2[Mo3S7(oxalate)3]
_chemical_formula_sum            'C54 H108 Br Mo3 N3 O12 S7'
_chemical_formula_weight         1583.58

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'
Br Br -0.2901 2.4595 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   25.229(9)
_cell_length_b                   23.162(8)
_cell_length_c                   12.495(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7301(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3288
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_type   'Bruker SADABS'
_exptl_absorpt_correction_T_min  1.294179
_exptl_absorpt_correction_T_max  1.959358
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48435
_diffrn_reflns_av_R_equivalents  0.0989
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         23.26
_reflns_number_total             5394
_reflns_number_gt                4218
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w==1/[\s^2^(Fo^2^)+(0.0611P)^2^+67.2672P] where P==(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5394
_refine_ls_number_parameters     355
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0610
_refine_ls_wR_factor_ref         0.1591
_refine_ls_wR_factor_gt          0.1475
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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 0.12366(2) 0.19115(3) 0.07429(5) 0.0220(2) Uani 1 1 d . . .
Br1 Br 0.21280(4) 0.2500 0.35277(8) 0.0302(3) Uani 1 2 d S . .
S1 S 0.05272(11) 0.2500 0.0159(2) 0.0252(6) Uani 1 2 d S . .
C1 C 0.1726(4) 0.0814(4) 0.0082(8) 0.044(2) Uani 1 1 d . . .
O1 O 0.1770(2) 0.1209(2) 0.0800(5) 0.0374(14) Uani 1 1 d . . .
Mo2 Mo 0.05542(4) 0.2500 0.20416(7) 0.0224(3) Uani 1 2 d S . .
S2 S 0.18112(11) 0.2500 -0.0458(2) 0.0301(7) Uani 1 2 d S . .
O2 O 0.1019(2) 0.1412(2) -0.0569(4) 0.0362(14) Uani 1 1 d . . .
C2 C 0.1296(4) 0.0950(4) -0.0775(8) 0.043(2) Uani 1 1 d . . .
S3 S 0.19978(10) 0.2500 0.1148(2) 0.0239(6) Uani 1 2 d S . .
O3 O 0.1989(3) 0.0378(3) 0.0015(6) 0.072(2) Uani 1 1 d . . .
C3 C -0.0225(5) 0.2500 0.3787(10) 0.051(4) Uani 1 2 d S . .
S4 S 0.05626(9) 0.14273(9) 0.18832(18) 0.0359(5) Uani 1 1 d . . .
O4 O 0.1232(3) 0.0654(3) -0.1573(6) 0.066(2) Uani 1 1 d . . .
C4 C -0.0556(5) 0.2500 0.2751(10) 0.035(3) Uani 1 2 d S . .
S5 S 0.11935(7) 0.18023(8) 0.26608(15) 0.0258(4) Uani 1 1 d . . .
O5 O 0.0269(3) 0.2500 0.3647(6) 0.044(2) Uani 1 2 d S . .
O6 O -0.0264(3) 0.2500 0.1874(6) 0.0334(19) Uani 1 2 d S . .
O7 O -0.0451(4) 0.2500 0.4656(8) 0.103(5) Uani 1 2 d S . .
O8 O -0.1032(3) 0.2500 0.2758(7) 0.040(2) Uani 1 2 d S . .
N1 N -0.1653(5) 0.0915(5) 0.2602(12) 0.034(3) Uani 0.582(8) 1 d P A 1
C50 C -0.2082(7) 0.0452(8) 0.2475(18) 0.046(6) Uiso 0.582(8) 1 d P A 1
C51 C -0.2616(8) 0.0605(9) 0.2114(17) 0.047(6) Uiso 0.582(8) 1 d P A 1
C52 C -0.2923(8) 0.0017(10) 0.2222(19) 0.068(6) Uiso 0.582(8) 1 d P A 1
C53 C -0.3509(15) 0.0101(16) 0.208(3) 0.152(13) Uiso 0.582(8) 1 d P A 1
C54 C -0.1176(6) 0.0566(7) 0.2934(13) 0.047(4) Uiso 0.582(8) 1 d P A 1
C55 C -0.0692(8) 0.0932(8) 0.3324(16) 0.063(5) Uiso 0.582(8) 1 d P A 1
C56 C -0.0269(9) 0.0538(10) 0.3778(19) 0.080(6) Uiso 0.582(8) 1 d P A 1
C57 C 0.0130(11) 0.0829(12) 0.458(2) 0.109(9) Uiso 0.582(8) 1 d P A 1
C58 C -0.1819(6) 0.1354(7) 0.3434(17) 0.031(4) Uiso 0.582(8) 1 d P A 1
C59 C -0.1893(6) 0.1112(6) 0.4582(12) 0.037(4) Uiso 0.582(8) 1 d P A 1
C60 C -0.1922(7) 0.1617(7) 0.5390(15) 0.045(4) Uiso 0.582(8) 1 d P A 1
C61 C -0.2082(9) 0.1490(10) 0.6456(19) 0.084(7) Uiso 0.582(8) 1 d P A 1
C62 C -0.1525(8) 0.1275(9) 0.1576(16) 0.054(5) Uiso 0.582(8) 1 d P A 1
C63 C -0.1366(11) 0.0910(12) 0.058(2) 0.096(8) Uiso 0.582(8) 1 d P A 1
C64 C -0.075(2) 0.114(2) 0.024(5) 0.25(3) Uiso 0.582(8) 1 d P A 1
C65 C -0.055(2) 0.082(2) -0.073(5) 0.56(8) Uiso 0.582(8) 1 d PR A 1
N2 N 0.0899(4) 0.2500 0.6530(9) 0.086(6) Uani 1 2 d S . 2
C70 C 0.1382(10) 0.2071(11) 0.708(2) 0.071(7) Uiso 0.50 1 d P . 2
C71 C 0.1699(11) 0.1734(11) 0.628(2) 0.060(7) Uiso 0.50 1 d P . 2
C72 C 0.2226(12) 0.1551(13) 0.688(2) 0.098(9) Uiso 0.50 1 d P . 2
C73 C 0.2536(16) 0.1235(18) 0.621(3) 0.133(13) Uiso 0.50 1 d P . 2
C74 C 0.1106(8) 0.2836(9) 0.5726(17) 0.051(5) Uiso 0.50 1 d P . 2
C75 C 0.1466(13) 0.3280(13) 0.633(2) 0.075(9) Uiso 0.50 1 d P . 2
C76 C 0.1592(10) 0.3734(11) 0.555(2) 0.072(7) Uiso 0.50 1 d P . 2
C77 C 0.1977(12) 0.4206(13) 0.602(2) 0.095(9) Uiso 0.50 1 d P . 2
C78 C 0.0566(9) 0.1976(10) 0.5860(19) 0.066(6) Uiso 0.50 1 d P . 2
C79 C 0.0310(10) 0.1460(11) 0.658(2) 0.071(7) Uiso 0.50 1 d P . 2
C80 C -0.0010(14) 0.1090(19) 0.587(3) 0.154(15) Uiso 0.50 1 d P . 2
C81 C -0.0070(14) 0.0319(19) 0.658(3) 0.33(4) Uiso 0.50 1 d PR . 2
C82 C 0.0585(7) 0.2640(8) 0.7470(14) 0.049(5) Uiso 0.50 1 d P . 2
C83 C 0.0148(12) 0.3082(13) 0.700(2) 0.090(8) Uiso 0.50 1 d P . 2
C84 C -0.0153(14) 0.3285(16) 0.794(3) 0.116(11) Uiso 0.50 1 d P . 2
C85 C -0.0576(18) 0.3737(19) 0.750(4) 0.157(15) Uiso 0.50 1 d P . 2
N3 N -0.1688(8) 0.1073(10) 0.1916(19) 0.042(5) Uiso 0.418(8) 1 d P . 3
C100 C -0.1910(10) 0.1352(11) 0.094(2) 0.056(7) Uiso 0.418(8) 1 d P . 3
C101 C -0.1577(12) 0.1868(13) 0.053(2) 0.074(8) Uiso 0.418(8) 1 d P . 3
C102 C -0.1772(14) 0.2043(16) -0.053(3) 0.095(11) Uiso 0.418(8) 1 d P . 3
C103 C -0.141(2) 0.2500 -0.081(4) 0.204(19) Uiso 0.837(16) 2 d SP . 3
C104 C -0.1813(10) 0.1488(11) 0.288(2) 0.051(7) Uiso 0.418(8) 1 d P . 3
C105 C -0.1701(10) 0.1252(11) 0.392(2) 0.046(7) Uiso 0.418(8) 1 d P . 3
C106 C -0.1755(10) 0.1713(11) 0.483(2) 0.050(6) Uiso 0.418(8) 1 d P . 3
C107 C -0.1554(15) 0.1628(16) 0.584(3) 0.101(11) Uiso 0.418(8) 1 d P . 3
C108 C -0.1141(10) 0.0911(12) 0.187(2) 0.060(7) Uiso 0.418(8) 1 d P . 3
C109 C -0.0983(11) 0.0620(12) 0.080(2) 0.064(7) Uiso 0.418(8) 1 d P . 3
C110 C -0.043(2) 0.048(3) 0.085(5) 0.17(2) Uiso 0.418(8) 1 d P . 3
C111 C -0.0178(17) 0.014(2) -0.021(4) 0.129(16) Uiso 0.418(8) 1 d P . 3
C112 C -0.2051(8) 0.0495(9) 0.2083(19) 0.019(5) Uiso 0.418(8) 1 d P . 3
C113 C -0.2587(9) 0.0717(11) 0.177(2) 0.035(6) Uiso 0.418(8) 1 d P . 3
C114 C -0.2989(7) 0.0203(8) 0.1778(15) 0.019(4) Uiso 0.418(8) 1 d P . 3
C115 C -0.3460(10) 0.0358(11) 0.108(2) 0.060(7) Uiso 0.418(8) 1 d P . 3

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0258(4) 0.0212(4) 0.0189(4) -0.0032(3) -0.0041(3) 0.0015(3)
Br1 0.0312(6) 0.0415(7) 0.0178(6) 0.000 -0.0046(5) 0.000
S1 0.0259(14) 0.0283(15) 0.0215(14) 0.000 -0.0054(12) 0.000
C1 0.047(5) 0.040(6) 0.045(6) -0.011(5) -0.014(5) 0.011(5)
O1 0.044(3) 0.031(3) 0.038(3) -0.013(3) -0.013(3) 0.017(3)
Mo2 0.0192(5) 0.0277(5) 0.0202(5) 0.000 -0.0007(4) 0.000
S2 0.0306(15) 0.0464(18) 0.0133(14) 0.000 0.0001(11) 0.000
O2 0.047(3) 0.032(3) 0.030(3) -0.013(3) -0.014(3) 0.005(3)
C2 0.053(6) 0.031(5) 0.044(6) -0.013(5) -0.005(5) 0.005(4)
S3 0.0237(14) 0.0331(15) 0.0148(13) 0.000 -0.0009(11) 0.000
O3 0.087(5) 0.040(4) 0.088(6) -0.031(4) -0.034(5) 0.035(4)
C3 0.033(8) 0.094(12) 0.027(7) 0.000 0.004(6) 0.000
S4 0.0366(12) 0.0292(11) 0.0419(13) 0.0052(10) -0.0060(10) -0.0116(9)
O4 0.089(6) 0.055(4) 0.055(5) -0.032(4) -0.026(4) 0.021(4)
C4 0.025(7) 0.033(7) 0.048(8) 0.000 0.004(6) 0.000
S5 0.0295(10) 0.0257(10) 0.0223(10) 0.0070(8) -0.0023(8) -0.0017(8)
O5 0.016(4) 0.087(7) 0.029(5) 0.000 0.001(4) 0.000
O6 0.021(4) 0.051(5) 0.028(4) 0.000 -0.004(4) 0.000
O7 0.025(5) 0.246(18) 0.039(6) 0.000 0.003(5) 0.000
O8 0.023(5) 0.051(5) 0.047(5) 0.000 -0.001(4) 0.000
N1 0.036(7) 0.011(6) 0.055(9) -0.013(6) 0.014(6) -0.002(5)
N2 0.027(6) 0.213(18) 0.018(6) 0.000 -0.009(5) 0.000

_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 O2 2.081(5) . ?
Mo1 O1 2.113(5) . ?
Mo1 S1 2.365(2) . ?
Mo1 S3 2.409(2) . ?
Mo1 S5 2.412(2) . ?
Mo1 S4 2.486(2) . ?
Mo1 S2 2.492(2) . ?
Mo1 Mo1 2.7260(16) 7_565 ?
Mo1 Mo2 2.7304(11) . ?
S1 Mo2 2.353(3) . ?
S1 Mo1 2.365(2) 7_565 ?
C1 O3 1.211(10) . ?
C1 O1 1.287(10) . ?
C1 C2 1.556(12) . ?
Mo2 O6 2.075(7) . ?
Mo2 O5 2.131(8) . ?
Mo2 S5 2.411(2) 7_565 ?
Mo2 S5 2.411(2) . ?
Mo2 S4 2.492(2) . ?
Mo2 S4 2.492(2) 7_565 ?
Mo2 Mo1 2.7304(11) 7_565 ?
S2 S3 2.061(4) . ?
S2 Mo1 2.492(2) 7_565 ?
O2 C2 1.305(10) . ?
C2 O4 1.220(10) . ?
S3 Mo1 2.409(2) 7_565 ?
C3 O7 1.226(16) . ?
C3 O5 1.259(15) . ?
C3 C4 1.542(18) . ?
S4 S5 2.057(3) . ?
C4 O8 1.200(13) . ?
C4 O6 1.320(14) . ?
N1 C54 1.51(2) . ?
N1 C58 1.513(19) . ?
N1 C50 1.53(2) . ?
N1 C62 1.56(2) . ?
C50 C51 1.46(3) . ?
C51 C52 1.57(3) . ?
C52 C53 1.50(4) . ?
C54 C55 1.57(2) . ?
C55 C56 1.51(3) . ?
C56 C57 1.57(3) . ?
C58 C59 1.55(2) . ?
C59 C60 1.55(2) . ?
C60 C61 1.42(3) . ?
C62 C63 1.56(3) . ?
C63 C64 1.69(6) . ?
C64 C65 1.5130 . ?
N2 C74 1.37(2) 7_565 ?
N2 C74 1.37(2) . ?
N2 C82 1.45(2) . ?
N2 C82 1.45(2) 7_565 ?
N2 C78 1.70(2) . ?
N2 C78 1.70(2) 7_565 ?
N2 C70 1.72(3) 7_565 ?
N2 C70 1.72(3) . ?
C70 C75 1.26(4) 7_565 ?
C70 C71 1.50(4) . ?
C70 C74 1.85(3) 7_565 ?
C70 C70 1.99(5) 7_565 ?
C71 C75 0.59(3) 7_565 ?
C71 C76 1.44(4) 7_565 ?
C71 C72 1.58(4) . ?
C71 C74 1.93(3) 7_565 ?
C72 C73 1.36(4) . ?
C73 C77 1.76(5) 7_565 ?
C74 C78 1.44(3) 7_565 ?
C74 C74 1.56(4) 7_565 ?
C74 C75 1.57(4) . ?
C74 C70 1.85(3) 7_565 ?
C74 C71 1.93(3) 7_565 ?
C75 C71 0.59(3) 7_565 ?
C75 C70 1.26(4) 7_565 ?
C75 C76 1.46(4) . ?
C76 C71 1.44(4) 7_565 ?
C76 C77 1.57(4) . ?
C77 C73 1.76(5) 7_565 ?
C78 C74 1.44(3) 7_565 ?
C78 C79 1.63(3) . ?
C78 C83 1.78(4) 7_565 ?
C79 C83 1.25(3) 7_565 ?
C79 C80 1.47(4) . ?
C80 C81 1.9993 . ?
C82 C82 0.65(4) 7_565 ?
C82 C83 1.61(3) . ?
C83 C79 1.25(3) 7_565 ?
C83 C84 1.47(4) . ?
C83 C78 1.78(4) 7_565 ?
C84 C85 1.60(5) . ?
N3 C108 1.43(3) . ?
N3 C100 1.49(3) . ?
N3 C104 1.57(3) . ?
N3 C112 1.63(3) . ?
C100 C101 1.55(4) . ?
C101 C102 1.47(4) . ?
C102 C103 1.45(4) . ?
C103 C102 1.45(4) 7_565 ?
C104 C105 1.44(4) . ?
C105 C106 1.57(3) . ?
C106 C107 1.38(4) . ?
C108 C109 1.56(4) . ?
C109 C110 1.43(6) . ?
C110 C111 1.66(7) . ?
C111 C111 1.22(8) 5 ?
C112 C113 1.50(3) . ?
C113 C114 1.56(3) . ?
C114 C115 1.52(3) . ?

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
O2 Mo1 O1 76.5(2) . . ?
O2 Mo1 S1 82.99(16) . . ?
O1 Mo1 S1 159.47(16) . . ?
O2 Mo1 S3 133.69(18) . . ?
O1 Mo1 S3 85.43(16) . . ?
S1 Mo1 S3 110.00(6) . . ?
O2 Mo1 S5 135.45(17) . . ?
O1 Mo1 S5 85.08(16) . . ?
S1 Mo1 S5 109.43(8) . . ?
S3 Mo1 S5 83.48(8) . . ?
O2 Mo1 S4 91.17(18) . . ?
O1 Mo1 S4 93.97(18) . . ?
S1 Mo1 S4 85.36(8) . . ?
S3 Mo1 S4 132.85(8) . . ?
S5 Mo1 S4 49.64(7) . . ?
O2 Mo1 S2 89.04(18) . . ?
O1 Mo1 S2 94.06(18) . . ?
S1 Mo1 S2 86.53(9) . . ?
S3 Mo1 S2 49.71(9) . . ?
S5 Mo1 S2 132.98(8) . . ?
S4 Mo1 S2 171.79(8) . . ?
O2 Mo1 Mo1 123.79(16) . 7_565 ?
O1 Mo1 Mo1 140.34(16) . 7_565 ?
S1 Mo1 Mo1 54.81(4) . 7_565 ?
S3 Mo1 Mo1 55.54(4) . 7_565 ?
S5 Mo1 Mo1 96.02(5) . 7_565 ?
S4 Mo1 Mo1 116.82(5) . 7_565 ?
S2 Mo1 Mo1 56.84(4) . 7_565 ?
O2 Mo1 Mo2 125.43(16) . . ?
O1 Mo1 Mo2 140.00(16) . . ?
S1 Mo1 Mo2 54.43(7) . . ?
S3 Mo1 Mo2 95.46(6) . . ?
S5 Mo1 Mo2 55.49(5) . . ?
S4 Mo1 Mo2 56.85(6) . . ?
S2 Mo1 Mo2 116.84(5) . . ?
Mo1 Mo1 Mo2 60.05(2) 7_565 . ?
Mo2 S1 Mo1 70.73(7) . 7_565 ?
Mo2 S1 Mo1 70.73(7) . . ?
Mo1 S1 Mo1 70.39(8) 7_565 . ?
O3 C1 O1 126.4(8) . . ?
O3 C1 C2 120.2(8) . . ?
O1 C1 C2 113.4(7) . . ?
C1 O1 Mo1 117.9(5) . . ?
O6 Mo2 O5 76.1(3) . . ?
O6 Mo2 S1 82.6(2) . . ?
O5 Mo2 S1 158.6(2) . . ?
O6 Mo2 S5 134.26(9) . 7_565 ?
O5 Mo2 S5 85.61(16) . 7_565 ?
S1 Mo2 S5 109.89(7) . 7_565 ?
O6 Mo2 S5 134.26(9) . . ?
O5 Mo2 S5 85.61(16) . . ?
S1 Mo2 S5 109.89(7) . . ?
S5 Mo2 S5 84.19(10) 7_565 . ?
O6 Mo2 S4 90.03(6) . . ?
O5 Mo2 S4 94.45(6) . . ?
S1 Mo2 S4 85.46(6) . . ?
S5 Mo2 S4 133.48(8) 7_565 . ?
S5 Mo2 S4 49.58(7) . . ?
O6 Mo2 S4 90.03(6) . 7_565 ?
O5 Mo2 S4 94.45(6) . 7_565 ?
S1 Mo2 S4 85.46(6) . 7_565 ?
S5 Mo2 S4 49.58(7) 7_565 7_565 ?
S5 Mo2 S4 133.48(8) . 7_565 ?
S4 Mo2 S4 170.84(11) . 7_565 ?
O6 Mo2 Mo1 124.57(17) . 7_565 ?
O5 Mo2 Mo1 140.55(13) . 7_565 ?
S1 Mo2 Mo1 54.84(6) . 7_565 ?
S5 Mo2 Mo1 55.55(5) 7_565 7_565 ?
S5 Mo2 Mo1 95.95(6) . 7_565 ?
S4 Mo2 Mo1 116.43(6) . 7_565 ?
S4 Mo2 Mo1 56.62(6) 7_565 7_565 ?
O6 Mo2 Mo1 124.57(17) . . ?
O5 Mo2 Mo1 140.55(13) . . ?
S1 Mo2 Mo1 54.84(6) . . ?
S5 Mo2 Mo1 95.95(6) 7_565 . ?
S5 Mo2 Mo1 55.55(5) . . ?
S4 Mo2 Mo1 56.62(6) . . ?
S4 Mo2 Mo1 116.43(6) 7_565 . ?
Mo1 Mo2 Mo1 59.89(4) 7_565 . ?
S3 S2 Mo1 63.05(9) . . ?
S3 S2 Mo1 63.05(9) . 7_565 ?
Mo1 S2 Mo1 66.32(8) . 7_565 ?
C2 O2 Mo1 118.1(5) . . ?
O4 C2 O2 123.4(8) . . ?
O4 C2 C1 122.8(8) . . ?
O2 C2 C1 113.8(7) . . ?
S2 S3 Mo1 67.25(9) . . ?
S2 S3 Mo1 67.25(9) . 7_565 ?
Mo1 S3 Mo1 68.92(8) . 7_565 ?
O7 C3 O5 125.7(12) . . ?
O7 C3 C4 119.5(11) . . ?
O5 C3 C4 114.9(11) . . ?
S5 S4 Mo1 63.32(8) . . ?
S5 S4 Mo2 63.15(8) . . ?
Mo1 S4 Mo2 66.52(6) . . ?
O8 C4 O6 124.4(12) . . ?
O8 C4 C3 122.4(11) . . ?
O6 C4 C3 113.2(10) . . ?
S4 S5 Mo2 67.28(9) . . ?
S4 S5 Mo1 67.04(8) . . ?
Mo2 S5 Mo1 68.96(6) . . ?
C3 O5 Mo2 117.7(8) . . ?
C4 O6 Mo2 118.2(7) . . ?
C54 N1 C58 113.1(14) . . ?
C54 N1 C50 102.5(12) . . ?
C58 N1 C50 110.2(12) . . ?
C54 N1 C62 110.3(11) . . ?
C58 N1 C62 105.3(12) . . ?
C50 N1 C62 115.8(15) . . ?
C51 C50 N1 120.8(16) . . ?
C50 C51 C52 102.6(17) . . ?
C53 C52 C51 111(2) . . ?
N1 C54 C55 114.7(13) . . ?
C56 C55 C54 109.9(16) . . ?
C55 C56 C57 116(2) . . ?
N1 C58 C59 115.3(14) . . ?
C60 C59 C58 109.7(13) . . ?
C61 C60 C59 117.9(16) . . ?
C63 C62 N1 114.9(16) . . ?
C62 C63 C64 105(3) . . ?
C65 C64 C63 111(3) . . ?
C74 N2 C74 69.0(17) 7_565 . ?
C74 N2 C82 157.6(12) 7_565 . ?
C74 N2 C82 132.2(11) . . ?
C74 N2 C82 132.2(11) 7_565 7_565 ?
C74 N2 C82 157.6(12) . 7_565 ?
C82 N2 C82 25.8(14) . 7_565 ?
C74 N2 C78 54.7(11) 7_565 . ?
C74 N2 C78 103.5(13) . . ?
C82 N2 C78 106.8(12) . . ?
C82 N2 C78 88.2(11) 7_565 . ?
C74 N2 C78 103.5(13) 7_565 7_565 ?
C74 N2 C78 54.7(11) . 7_565 ?
C82 N2 C78 88.2(11) . 7_565 ?
C82 N2 C78 106.8(12) 7_565 7_565 ?
C78 N2 C78 91.3(16) . 7_565 ?
C74 N2 C70 110.6(13) 7_565 7_565 ?
C74 N2 C70 72.4(12) . 7_565 ?
C82 N2 C70 86.1(12) . 7_565 ?
C82 N2 C70 101.0(12) 7_565 7_565 ?
C78 N2 C70 164.5(13) . 7_565 ?
C78 N2 C70 97.9(11) 7_565 7_565 ?
C74 N2 C70 72.4(12) 7_565 . ?
C74 N2 C70 110.6(13) . . ?
C82 N2 C70 101.0(12) . . ?
C82 N2 C70 86.1(11) 7_565 . ?
C78 N2 C70 97.9(11) . . ?
C78 N2 C70 164.5(13) 7_565 . ?
C70 N2 C70 70.6(17) 7_565 . ?
C75 C70 C71 22.7(17) 7_565 . ?
C75 C70 N2 101(2) 7_565 . ?
C71 C70 N2 114.1(19) . . ?
C75 C70 C74 56.8(18) 7_565 7_565 ?
C71 C70 C74 69.3(16) . 7_565 ?
N2 C70 C74 45.2(9) . 7_565 ?
C75 C70 C70 130.1(18) 7_565 7_565 ?
C71 C70 C70 121.3(14) . 7_565 ?
N2 C70 C70 54.7(8) . 7_565 ?
C74 C70 C70 83.3(10) 7_565 7_565 ?
C75 C71 C76 81(5) 7_565 7_565 ?
C75 C71 C70 55(4) 7_565 . ?
C76 C71 C70 135(3) 7_565 . ?
C75 C71 C72 140(6) 7_565 . ?
C76 C71 C72 105(2) 7_565 . ?
C70 C71 C72 106(2) . . ?
C75 C71 C74 45(4) 7_565 7_565 ?
C76 C71 C74 90.9(18) 7_565 7_565 ?
C70 C71 C74 63.8(15) . 7_565 ?
C72 C71 C74 164(2) . 7_565 ?
C73 C72 C71 110(3) . . ?
C72 C73 C77 86(3) . 7_565 ?
N2 C74 C78 74.0(14) . 7_565 ?
N2 C74 C74 55.5(9) . 7_565 ?
C78 C74 C74 107.5(12) 7_565 7_565 ?
N2 C74 C75 103.9(17) . . ?
C78 C74 C75 107.1(19) 7_565 . ?
C74 C74 C75 131.1(14) 7_565 . ?
N2 C74 C70 62.4(12) . 7_565 ?
C78 C74 C70 102.4(17) 7_565 7_565 ?
C74 C74 C70 96.7(10) 7_565 7_565 ?
C75 C74 C70 42.5(14) . 7_565 ?
N2 C74 C71 109.0(15) . 7_565 ?
C78 C74 C71 122.5(18) 7_565 7_565 ?
C74 C74 C71 121.1(10) 7_565 7_565 ?
C75 C74 C71 15.6(14) . 7_565 ?
C70 C74 C71 46.9(12) 7_565 7_565 ?
C71 C75 C70 102(5) 7_565 7_565 ?
C71 C75 C76 76(5) 7_565 . ?
C70 C75 C76 173(3) 7_565 . ?
C71 C75 C74 119(5) 7_565 . ?
C70 C75 C74 81(2) 7_565 . ?
C76 C75 C74 106(2) . . ?
C71 C76 C75 23.5(14) 7_565 . ?
C71 C76 C77 100(2) 7_565 . ?
C75 C76 C77 113(2) . . ?
C76 C77 C73 98(2) . 7_565 ?
C74 C78 C79 131(2) 7_565 . ?
C74 C78 N2 51.2(12) 7_565 . ?
C79 C78 N2 116.8(17) . . ?
C74 C78 C83 133(2) 7_565 7_565 ?
C79 C78 C83 42.9(13) . 7_565 ?
N2 C78 C83 87.3(15) . 7_565 ?
C83 C79 C80 125(3) 7_565 . ?
C83 C79 C78 75(2) 7_565 . ?
C80 C79 C78 109(2) . . ?
C79 C80 C81 107(2) . . ?
C82 C82 N2 77.1(7) 7_565 . ?
C82 C82 C83 129.3(12) 7_565 . ?
N2 C82 C83 102.7(15) . . ?
C79 C83 C84 104(3) 7_565 . ?
C79 C83 C82 118(2) 7_565 . ?
C84 C83 C82 105(2) . . ?
C79 C83 C78 62.2(19) 7_565 7_565 ?
C84 C83 C78 165(3) . 7_565 ?
C82 C83 C78 80.7(16) . 7_565 ?
C83 C84 C85 106(3) . . ?
C108 N3 C100 116(2) . . ?
C108 N3 C104 112.4(19) . . ?
C100 N3 C104 106.5(19) . . ?
C108 N3 C112 109.3(19) . . ?
C100 N3 C112 104.5(17) . . ?
C104 N3 C112 107.0(19) . . ?
N3 C100 C101 113(2) . . ?
C102 C101 C100 109(3) . . ?
C103 C102 C101 102(3) . . ?
C102 C103 C102 94(4) . 7_565 ?
C105 C104 N3 115(2) . . ?
C104 C105 C106 112(2) . . ?
C107 C106 C105 122(3) . . ?
N3 C108 C109 113(2) . . ?
C110 C109 C108 108(3) . . ?
C109 C110 C111 116(4) . . ?
C111 C111 C110 101(6) 5 . ?
C113 C112 N3 100.9(17) . . ?
C112 C113 C114 108.7(19) . . ?
C115 C114 C113 108.9(18) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.937
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.160