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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1026544'
_audit_update_record             
;
2014-09-29 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H72 Br2 Mo12 N6 O52 S'
_chemical_formula_weight         3052.39

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   11.225(2)
_cell_length_b                   31.408(6)
_cell_length_c                   13.382(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.79(3)
_cell_angle_gamma                90.00
_cell_volume                     4561.5(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2960.0
_exptl_absorpt_coefficient_mu    2.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_process_details   
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43451
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.40
_reflns_number_total             10353
_reflns_number_gt                8965
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0286P)²+9.2553P] where P=(Fo²+2Fc²)/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         10353
_refine_ls_number_parameters     632
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0685
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_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
S1 S 0.5000 0.0000 1.0000 0.01771(19) Uani 1 2 d S . .
Mo1 Mo 0.23500(2) -0.067832(9) 0.91662(2) 0.02845(7) Uani 1 1 d . . .
Mo2 Mo 0.23481(2) 0.037208(9) 0.80617(2) 0.02698(7) Uani 1 1 d . . .
Mo3 Mo 0.48376(3) 0.109428(9) 0.91691(3) 0.03089(7) Uani 1 1 d . . .
Mo4 Mo 0.52788(2) 0.026079(9) 0.74430(2) 0.02703(7) Uani 1 1 d . . .
Mo5 Mo 0.78089(2) -0.025284(9) 0.92954(2) 0.02337(6) Uani 1 1 d . . .
Mo6 Mo 0.50163(2) -0.083528(9) 0.81673(2) 0.02537(7) Uani 1 1 d . . .
Br1 Br 1.09996(7) 0.277538(18) 0.24808(5) 0.0607(2) Uani 0.7624(14) 1 d P A 1
Br2 Br 0.73694(17) 0.18985(6) 0.06747(13) 0.0466(6) Uani 0.2376(14) 1 d P A 2
O1 O 0.5417(3) 0.04375(12) 1.0348(3) 0.0180(8) Uani 0.50 1 d P . .
O2 O 0.4582(3) 0.02863(12) 0.9075(3) 0.0174(8) Uani 0.50 1 d P . .
O3 O 0.3644(3) -0.00061(12) 0.9693(3) 0.0174(8) Uani 0.50 1 d P . .
O4 O 0.5512(3) -0.01386(12) 0.9191(3) 0.0173(8) Uani 0.50 1 d P . .
O5 O 0.8130(3) -0.04567(8) 1.0615(2) 0.0560(9) Uani 1 1 d . . .
O6 O 0.9078(2) -0.03452(10) 0.8926(3) 0.0550(8) Uani 1 1 d . . .
O7 O 0.6780(2) -0.06881(8) 0.8712(2) 0.0474(7) Uani 1 1 d . . .
O8 O 0.5376(3) -0.11276(13) 0.9531(3) 0.0703(11) Uani 1 1 d . . .
O9 O 0.5113(3) -0.12389(9) 0.7400(2) 0.0570(9) Uani 1 1 d . . .
O10 O 0.3383(3) -0.10030(13) 1.0146(2) 0.0669(11) Uani 1 1 d . . .
O11 O 0.3405(2) -0.08365(13) 0.8236(2) 0.0637(10) Uani 1 1 d . . .
O12 O 0.4891(2) -0.03628(9) 0.7359(2) 0.0449(7) Uani 1 1 d . . .
O13 O 0.1128(2) -0.09844(9) 0.8738(2) 0.0437(6) Uani 1 1 d . . .
O14 O 0.2002(4) -0.01896(8) 0.8188(2) 0.0580(9) Uani 1 1 d . . .
O15 O 0.1904(4) -0.03209(9) 1.0083(2) 0.0632(10) Uani 1 1 d . . .
O16 O 0.3476(3) 0.02824(10) 0.7307(3) 0.0672(11) Uani 1 1 d . . .
O17 O 0.1122(2) 0.05534(9) 0.72010(19) 0.0405(6) Uani 1 1 d . . .
O18 O 0.3285(3) 0.08996(11) 0.8567(3) 0.0694(11) Uani 1 1 d . . .
O19 O 0.4797(3) 0.15959(8) 0.8802(3) 0.0491(7) Uani 1 1 d . . .
O20 O 0.5355(3) 0.07866(11) 0.8047(3) 0.0712(12) Uani 1 1 d . . .
O21 O 0.6840(2) 0.00994(8) 0.8118(2) 0.0455(7) Uani 1 1 d . . .
O22 O 0.5384(3) 0.03635(10) 0.6256(2) 0.0466(7) Uani 1 1 d . . .
O23 O 0.6763(2) 0.20009(7) 0.51777(19) 0.0311(5) Uani 1 1 d . . .
O24 O 0.7051(2) 0.11421(7) 0.45895(19) 0.0293(5) Uani 1 1 d . . .
O25 O 0.9453(2) 0.08422(7) 0.47420(19) 0.0305(5) Uani 1 1 d . . .
O26 O 1.1355(2) 0.12943(8) 0.56602(18) 0.0309(5) Uani 1 1 d . . .
O27 O 1.1097(2) 0.21375(8) 0.63725(18) 0.0331(5) Uani 1 1 d . . .
O28 O 0.8649(2) 0.24752(8) 0.5878(2) 0.0404(6) Uani 1 1 d . . .
N1 N 0.9084(2) 0.17426(9) 0.4823(2) 0.0272(6) Uani 1 1 d . . .
H1A H 0.9835 0.1645 0.5122 0.041 Uiso 1 1 calc R . .
H1B H 0.8542 0.1531 0.4749 0.041 Uiso 1 1 calc R . .
H1C H 0.8885 0.1946 0.5216 0.041 Uiso 1 1 calc R . .
N2 N 0.2891(4) 0.19029(15) 0.3690(4) 0.0791(15) Uani 1 1 d . . .
N3 N 0.9004(4) 0.14381(13) 0.6886(3) 0.0549(9) Uani 1 1 d . . .
C1 C 0.7582(3) 0.26914(11) 0.5421(3) 0.0351(8) Uani 1 1 d . . .
C2 C 0.7469(4) 0.31307(12) 0.5321(3) 0.0453(10) Uani 1 1 d . . .
H2 H 0.8155 0.3304 0.5560 0.054 Uiso 1 1 calc R . .
C3 C 0.6327(5) 0.33116(13) 0.4863(3) 0.0500(11) Uani 1 1 d . . .
H3 H 0.6254 0.3605 0.4786 0.060 Uiso 1 1 calc R . .
C4 C 0.5311(4) 0.30575(13) 0.4525(3) 0.0457(10) Uani 1 1 d . . .
H4 H 0.4548 0.3181 0.4235 0.055 Uiso 1 1 calc R . .
C5 C 0.5409(4) 0.26129(12) 0.4610(3) 0.0358(8) Uani 1 1 d . . .
H5 H 0.4718 0.2442 0.4373 0.043 Uiso 1 1 calc R . .
C6 C 0.6542(3) 0.24326(11) 0.5049(3) 0.0304(7) Uani 1 1 d . . .
C7 C 0.5735(3) 0.17242(11) 0.4789(3) 0.0330(7) Uani 1 1 d . . .
H7A H 0.5459 0.1749 0.4043 0.040 Uiso 1 1 calc R . .
H7B H 0.5058 0.1803 0.5079 0.040 Uiso 1 1 calc R . .
C8 C 0.6131(3) 0.12723(11) 0.5087(3) 0.0333(8) Uani 1 1 d . . .
H8A H 0.6455 0.1254 0.5831 0.040 Uiso 1 1 calc R . .
H8B H 0.5424 0.1084 0.4888 0.040 Uiso 1 1 calc R . .
C9 C 0.7404(3) 0.07105(10) 0.4843(3) 0.0308(7) Uani 1 1 d . . .
H9A H 0.6694 0.0526 0.4618 0.037 Uiso 1 1 calc R . .
H9B H 0.7713 0.0681 0.5586 0.037 Uiso 1 1 calc R . .
C10 C 0.8391(3) 0.05818(10) 0.4320(3) 0.0297(7) Uani 1 1 d . . .
H10A H 0.8595 0.0283 0.4448 0.036 Uiso 1 1 calc R . .
H10B H 0.8105 0.0625 0.3580 0.036 Uiso 1 1 calc R . .
C11 C 1.0556(3) 0.07201(10) 0.4555(2) 0.0265(6) Uani 1 1 d . . .
C12 C 1.0694(3) 0.03886(11) 0.3908(3) 0.0323(7) Uani 1 1 d . . .
H12 H 1.0010 0.0233 0.3555 0.039 Uiso 1 1 calc R . .
C13 C 1.1871(4) 0.02877(12) 0.3787(3) 0.0385(8) Uani 1 1 d . . .
H13 H 1.1965 0.0067 0.3352 0.046 Uiso 1 1 calc R . .
C14 C 1.2881(3) 0.05165(13) 0.4314(3) 0.0407(9) Uani 1 1 d . . .
H14 H 1.3660 0.0446 0.4243 0.049 Uiso 1 1 calc R . .
C15 C 1.2745(3) 0.08529(12) 0.4952(3) 0.0354(8) Uani 1 1 d . . .
H15 H 1.3434 0.1006 0.5303 0.042 Uiso 1 1 calc R . .
C16 C 1.1594(3) 0.09607(11) 0.5069(2) 0.0280(7) Uani 1 1 d . . .
C17 C 1.2388(3) 0.15416(12) 0.6231(3) 0.0348(8) Uani 1 1 d . . .
H17A H 1.2727 0.1710 0.5761 0.042 Uiso 1 1 calc R . .
H17B H 1.3029 0.1355 0.6621 0.042 Uiso 1 1 calc R . .
C18 C 1.1931(3) 0.18284(12) 0.6951(3) 0.0371(8) Uani 1 1 d . . .
H18A H 1.1515 0.1660 0.7368 0.045 Uiso 1 1 calc R . .
H18B H 1.2623 0.1972 0.7412 0.045 Uiso 1 1 calc R . .
C19 C 1.0605(4) 0.24026(12) 0.7049(3) 0.0405(9) Uani 1 1 d . . .
H19A H 1.1270 0.2554 0.7519 0.049 Uiso 1 1 calc R . .
H19B H 1.0197 0.2226 0.7457 0.049 Uiso 1 1 calc R . .
C20 C 0.9702(3) 0.27159(12) 0.6428(3) 0.0415(9) Uani 1 1 d . . .
H20A H 0.9463 0.2922 0.6880 0.050 Uiso 1 1 calc R . .
H20B H 1.0067 0.2867 0.5947 0.050 Uiso 1 1 calc R . .
C21 C 0.9069(3) 0.19201(10) 0.3796(3) 0.0277(7) Uani 1 1 d . . .
C22 C 0.9919(4) 0.22301(11) 0.3719(3) 0.0374(8) Uani 1 1 d . A .
H22 H 1.0494 0.2332 0.4299 0.045 Uiso 1 1 calc R . .
C23 C 0.9870(5) 0.23828(13) 0.2725(4) 0.0562(13) Uani 1 1 d . . .
C24 C 0.8996(5) 0.22356(18) 0.1863(3) 0.0663(16) Uani 1 1 d . A .
H24 H 0.8971 0.2344 0.1211 0.080 Uiso 1 1 calc R B 2
C25 C 0.8175(5) 0.19321(18) 0.1975(3) 0.0590(13) Uani 1 1 d . . .
C26 C 0.8204(4) 0.17699(13) 0.2938(3) 0.0410(9) Uani 1 1 d . A .
H26 H 0.7646 0.1561 0.3010 0.049 Uiso 1 1 calc R . .
C27 C 0.1458(4) 0.13705(13) 0.2482(3) 0.0447(9) Uani 1 1 d . . .
H27A H 0.0894 0.1252 0.2839 0.067 Uiso 1 1 calc R . .
H27B H 0.1935 0.1146 0.2291 0.067 Uiso 1 1 calc R . .
H27C H 0.1004 0.1516 0.1872 0.067 Uiso 1 1 calc R . .
C28 C 0.2272(4) 0.16685(14) 0.3152(4) 0.0479(10) Uani 1 1 d . . .
C29 C 0.8852(5) 0.08932(15) 0.8295(4) 0.0598(13) Uani 1 1 d . . .
H29A H 0.9571 0.0912 0.8865 0.090 Uiso 1 1 calc R . .
H29B H 0.8788 0.0611 0.8012 0.090 Uiso 1 1 calc R . .
H29C H 0.8132 0.0955 0.8532 0.090 Uiso 1 1 calc R . .
C30 C 0.8949(4) 0.11989(13) 0.7502(3) 0.0407(9) Uani 1 1 d . . .


_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
S1 O4 1.417(4) . ?
S1 O4 1.417(4) 3_657 ?
S1 O3 1.472(4) 3_657 ?
S1 O3 1.472(4) . ?
S1 O1 1.488(4) . ?
S1 O1 1.488(4) 3_657 ?
S1 O2 1.505(4) . ?
S1 O2 1.505(4) 3_657 ?
Mo1 O13 1.653(2) . ?
Mo1 O10 1.824(3) . ?
Mo1 O15 1.824(3) . ?
Mo1 O11 1.989(3) . ?
Mo1 O14 1.990(3) . ?
Mo2 O17 1.654(2) . ?
Mo2 O14 1.824(3) . ?
Mo2 O16 1.832(3) . ?
Mo2 O18 1.986(3) . ?
Mo2 O5 1.995(3) 3_657 ?
Mo3 O19 1.648(3) . ?
Mo3 O8 1.819(3) 3_657 ?
Mo3 O18 1.829(3) . ?
Mo3 O20 1.993(3) . ?
Mo3 O10 1.994(3) 3_657 ?
Mo4 O22 1.655(3) . ?
Mo4 O21 1.826(3) . ?
Mo4 O20 1.831(3) . ?
Mo4 O16 1.986(3) . ?
Mo4 O12 2.003(3) . ?
Mo4 O2 2.502(4) . ?
Mo5 O6 1.649(3) . ?
Mo5 O5 1.826(3) . ?
Mo5 O7 1.830(3) . ?
Mo5 O15 1.977(3) 3_657 ?
Mo5 O21 2.004(3) . ?
Mo5 O3 2.506(4) 3_657 ?
Mo6 O9 1.652(3) . ?
Mo6 O12 1.820(3) . ?
Mo6 O11 1.834(3) . ?
Mo6 O7 1.982(3) . ?
Mo6 O8 1.990(3) . ?
Mo6 O1 2.497(4) 3_657 ?
Br1 C23 1.856(5) . ?
Br2 C25 1.748(5) . ?
Br2 C24 2.345(7) . ?
O1 O4 1.636(5) 3_657 ?
O1 O3 1.726(5) 3_657 ?
O1 O2 1.787(6) . ?
O1 Mo6 2.497(4) 3_657 ?
O2 O4 1.677(5) . ?
O2 O3 1.755(5) . ?
O3 O4 1.615(5) 3_657 ?
O3 O1 1.726(5) 3_657 ?
O3 Mo5 2.506(4) 3_657 ?
O4 O3 1.615(5) 3_657 ?
O4 O1 1.636(5) 3_657 ?
O5 Mo2 1.995(3) 3_657 ?
O8 Mo3 1.819(3) 3_657 ?
O10 Mo3 1.994(3) 3_657 ?
O15 Mo5 1.977(3) 3_657 ?
O23 C6 1.381(4) . ?
O23 C7 1.432(4) . ?
O24 C8 1.425(4) . ?
O24 C9 1.429(4) . ?
O25 C11 1.379(4) . ?
O25 C10 1.437(4) . ?
O26 C16 1.380(4) . ?
O26 C17 1.442(4) . ?
O27 C18 1.431(4) . ?
O27 C19 1.440(4) . ?
O28 C1 1.376(5) . ?
O28 C20 1.438(4) . ?
N1 C21 1.479(4) . ?
N2 C28 1.134(6) . ?
N3 C30 1.129(5) . ?
C1 C2 1.389(5) . ?
C1 C6 1.405(5) . ?
C2 C3 1.393(6) . ?
C3 C4 1.371(6) . ?
C4 C5 1.403(5) . ?
C5 C6 1.379(5) . ?
C7 C8 1.510(5) . ?
C9 C10 1.508(5) . ?
C11 C12 1.388(5) . ?
C11 C16 1.412(5) . ?
C12 C13 1.407(5) . ?
C13 C14 1.375(6) . ?
C14 C15 1.391(5) . ?
C15 C16 1.383(5) . ?
C17 C18 1.502(5) . ?
C19 C20 1.502(6) . ?
C21 C26 1.384(5) . ?
C21 C22 1.386(5) . ?
C22 C23 1.402(6) . ?
C23 C24 1.389(8) . ?
C24 C25 1.360(8) . ?
C25 C26 1.377(6) . ?
C27 C28 1.448(6) . ?
C29 C30 1.456(6) . ?

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
O4 S1 O4 180.000(1) . 3_657 ?
O4 S1 O3 68.0(2) . 3_657 ?
O4 S1 O3 112.0(2) 3_657 3_657 ?
O4 S1 O3 112.0(2) . . ?
O4 S1 O3 68.0(2) 3_657 . ?
O3 S1 O3 180.00(8) 3_657 . ?
O4 S1 O1 111.5(2) . . ?
O4 S1 O1 68.5(2) 3_657 . ?
O3 S1 O1 71.4(2) 3_657 . ?
O3 S1 O1 108.6(2) . . ?
O4 S1 O1 68.5(2) . 3_657 ?
O4 S1 O1 111.5(2) 3_657 3_657 ?
O3 S1 O1 108.6(2) 3_657 3_657 ?
O3 S1 O1 71.4(2) . 3_657 ?
O1 S1 O1 180.00(11) . 3_657 ?
O4 S1 O2 70.0(2) . . ?
O4 S1 O2 110.0(2) 3_657 . ?
O3 S1 O2 107.7(2) 3_657 . ?
O3 S1 O2 72.3(2) . . ?
O1 S1 O2 73.3(2) . . ?
O1 S1 O2 106.7(2) 3_657 . ?
O4 S1 O2 110.0(2) . 3_657 ?
O4 S1 O2 70.0(2) 3_657 3_657 ?
O3 S1 O2 72.3(2) 3_657 3_657 ?
O3 S1 O2 107.7(2) . 3_657 ?
O1 S1 O2 106.7(2) . 3_657 ?
O1 S1 O2 73.3(2) 3_657 3_657 ?
O2 S1 O2 180.0(2) . 3_657 ?
O13 Mo1 O10 104.06(16) . . ?
O13 Mo1 O15 104.18(16) . . ?
O10 Mo1 O15 95.39(15) . . ?
O13 Mo1 O11 102.25(15) . . ?
O10 Mo1 O11 86.52(13) . . ?
O15 Mo1 O11 152.16(16) . . ?
O13 Mo1 O14 102.39(15) . . ?
O10 Mo1 O14 152.37(16) . . ?
O15 Mo1 O14 85.77(12) . . ?
O11 Mo1 O14 80.16(13) . . ?
O17 Mo2 O14 103.79(15) . . ?
O17 Mo2 O16 103.81(16) . . ?
O14 Mo2 O16 95.51(15) . . ?
O17 Mo2 O18 102.94(16) . . ?
O14 Mo2 O18 151.94(16) . . ?
O16 Mo2 O18 86.28(12) . . ?
O17 Mo2 O5 101.99(14) . 3_657 ?
O14 Mo2 O5 86.26(12) . 3_657 ?
O16 Mo2 O5 152.89(16) . 3_657 ?
O18 Mo2 O5 79.97(14) . 3_657 ?
O19 Mo3 O8 103.29(17) . 3_657 ?
O19 Mo3 O18 103.73(17) . . ?
O8 Mo3 O18 95.58(16) 3_657 . ?
O19 Mo3 O20 103.30(17) . . ?
O8 Mo3 O20 152.09(17) 3_657 . ?
O18 Mo3 O20 86.22(13) . . ?
O19 Mo3 O10 102.90(15) . 3_657 ?
O8 Mo3 O10 85.98(13) 3_657 3_657 ?
O18 Mo3 O10 152.19(16) . 3_657 ?
O20 Mo3 O10 79.99(14) . 3_657 ?
O22 Mo4 O21 103.56(14) . . ?
O22 Mo4 O20 103.94(18) . . ?
O21 Mo4 O20 95.81(14) . . ?
O22 Mo4 O16 103.09(16) . . ?
O21 Mo4 O16 151.78(16) . . ?
O20 Mo4 O16 86.63(12) . . ?
O22 Mo4 O12 101.82(14) . . ?
O21 Mo4 O12 85.63(11) . . ?
O20 Mo4 O12 153.06(16) . . ?
O16 Mo4 O12 80.00(12) . . ?
O22 Mo4 O2 161.21(14) . . ?
O21 Mo4 O2 92.95(13) . . ?
O20 Mo4 O2 64.90(15) . . ?
O16 Mo4 O2 62.63(15) . . ?
O12 Mo4 O2 88.17(13) . . ?
O6 Mo5 O5 104.86(17) . . ?
O6 Mo5 O7 103.89(16) . . ?
O5 Mo5 O7 95.60(13) . . ?
O6 Mo5 O15 103.08(17) . 3_657 ?
O5 Mo5 O15 86.66(11) . 3_657 ?
O7 Mo5 O15 151.36(15) . 3_657 ?
O6 Mo5 O21 101.45(15) . . ?
O5 Mo5 O21 152.56(14) . . ?
O7 Mo5 O21 85.43(11) . . ?
O15 Mo5 O21 79.92(12) 3_657 . ?
O6 Mo5 O3 161.90(15) . 3_657 ?
O5 Mo5 O3 65.56(14) . 3_657 ?
O7 Mo5 O3 92.63(14) . 3_657 ?
O15 Mo5 O3 62.31(14) 3_657 3_657 ?
O21 Mo5 O3 87.00(13) . 3_657 ?
O9 Mo6 O12 105.31(16) . . ?
O9 Mo6 O11 104.55(17) . . ?
O12 Mo6 O11 95.94(13) . . ?
O9 Mo6 O7 100.94(14) . . ?
O12 Mo6 O7 86.96(11) . . ?
O11 Mo6 O7 152.54(15) . . ?
O9 Mo6 O8 100.70(17) . . ?
O12 Mo6 O8 152.58(16) . . ?
O11 Mo6 O8 85.71(12) . . ?
O7 Mo6 O8 79.66(13) . . ?
O9 Mo6 O1 159.24(16) . 3_657 ?
O12 Mo6 O1 93.63(13) . 3_657 ?
O11 Mo6 O1 64.31(15) . 3_657 ?
O7 Mo6 O1 88.27(13) . 3_657 ?
O8 Mo6 O1 62.39(14) . 3_657 ?
C25 Br2 C24 35.1(2) . . ?
S1 O1 O4 53.71(18) . 3_657 ?
S1 O1 O3 53.89(17) . 3_657 ?
O4 O1 O3 90.8(3) 3_657 3_657 ?
S1 O1 O2 53.79(17) . . ?
O4 O1 O2 88.7(3) 3_657 . ?
O3 O1 O2 86.4(2) 3_657 . ?
S1 O1 Mo6 127.0(2) . 3_657 ?
O4 O1 Mo6 73.5(2) 3_657 3_657 ?
O3 O1 Mo6 131.5(2) 3_657 3_657 ?
O2 O1 Mo6 136.9(2) . 3_657 ?
S1 O2 O4 52.56(18) . . ?
S1 O2 O3 52.99(17) . . ?
O4 O2 O3 88.5(3) . . ?
S1 O2 O1 52.89(17) . . ?
O4 O2 O1 87.7(2) . . ?
O3 O2 O1 85.5(2) . . ?
S1 O2 Mo4 126.7(2) . . ?
O4 O2 Mo4 74.30(19) . . ?
O3 O2 Mo4 138.9(2) . . ?
O1 O2 Mo4 129.5(2) . . ?
S1 O3 O4 54.42(18) . 3_657 ?
S1 O3 O1 54.75(18) . 3_657 ?
O4 O3 O1 91.8(3) 3_657 3_657 ?
S1 O3 O2 54.75(18) . . ?
O4 O3 O2 90.5(3) 3_657 . ?
O1 O3 O2 87.2(2) 3_657 . ?
S1 O3 Mo5 127.9(2) . 3_657 ?
O4 O3 Mo5 73.65(19) 3_657 3_657 ?
O1 O3 Mo5 139.4(2) 3_657 3_657 ?
O2 O3 Mo5 129.5(2) . 3_657 ?
S1 O4 O3 57.61(19) . 3_657 ?
S1 O4 O1 57.8(2) . 3_657 ?
O3 O4 O1 95.3(3) 3_657 3_657 ?
S1 O4 O2 57.47(19) . . ?
O3 O4 O2 93.8(3) 3_657 . ?
O1 O4 O2 92.9(3) 3_657 . ?
Mo5 O5 Mo2 141.32(19) . 3_657 ?
Mo5 O7 Mo6 142.48(17) . . ?
Mo3 O8 Mo6 143.6(2) 3_657 . ?
Mo1 O10 Mo3 142.11(19) . 3_657 ?
Mo6 O11 Mo1 141.6(2) . . ?
Mo6 O12 Mo4 141.36(16) . . ?
Mo2 O14 Mo1 142.76(17) . . ?
Mo1 O15 Mo5 143.2(2) . 3_657 ?
Mo2 O16 Mo4 141.9(2) . . ?
Mo3 O18 Mo2 142.30(19) . . ?
Mo4 O20 Mo3 141.3(2) . . ?
Mo4 O21 Mo5 143.34(17) . . ?
C6 O23 C7 116.6(3) . . ?
C8 O24 C9 110.6(2) . . ?
C11 O25 C10 117.6(2) . . ?
C16 O26 C17 117.7(3) . . ?
C18 O27 C19 110.8(3) . . ?
C1 O28 C20 118.5(3) . . ?
O28 C1 C2 125.5(3) . . ?
O28 C1 C6 115.0(3) . . ?
C2 C1 C6 119.6(4) . . ?
C1 C2 C3 119.9(4) . . ?
C4 C3 C2 120.2(4) . . ?
C3 C4 C5 120.8(4) . . ?
C6 C5 C4 119.2(4) . . ?
C5 C6 O23 124.9(3) . . ?
C5 C6 C1 120.4(3) . . ?
O23 C6 C1 114.7(3) . . ?
O23 C7 C8 108.6(3) . . ?
O24 C8 C7 110.2(3) . . ?
O24 C9 C10 109.6(3) . . ?
O25 C10 C9 107.4(3) . . ?
O25 C11 C12 124.8(3) . . ?
O25 C11 C16 115.5(3) . . ?
C12 C11 C16 119.7(3) . . ?
C11 C12 C13 119.9(3) . . ?
C14 C13 C12 119.9(3) . . ?
C13 C14 C15 120.4(3) . . ?
C16 C15 C14 120.5(3) . . ?
O26 C16 C15 125.1(3) . . ?
O26 C16 C11 115.4(3) . . ?
C15 C16 C11 119.5(3) . . ?
O26 C17 C18 107.6(3) . . ?
O27 C18 C17 110.0(3) . . ?
O27 C19 C20 110.1(3) . . ?
O28 C20 C19 106.8(3) . . ?
C26 C21 C22 121.9(4) . . ?
C26 C21 N1 118.8(3) . . ?
C22 C21 N1 119.3(3) . . ?
C21 C22 C23 116.8(4) . . ?
C24 C23 C22 121.5(4) . . ?
C24 C23 Br1 116.4(4) . . ?
C22 C23 Br1 122.1(4) . . ?
C25 C24 C23 119.8(4) . . ?
C25 C24 Br2 47.7(3) . . ?
C23 C24 Br2 167.4(4) . . ?
C24 C25 C26 120.5(5) . . ?
C24 C25 Br2 97.2(4) . . ?
C26 C25 Br2 142.3(5) . . ?
C25 C26 C21 119.6(4) . . ?
N2 C28 C27 178.5(5) . . ?
N3 C30 C29 178.8(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.40
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.132
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1026545'
_audit_update_record             
;
2014-09-29 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            ' C60 H72 Cl2 Mo12 N6 O52 S'
_chemical_formula_weight         2963.49

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'
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   11.273(2)
_cell_length_b                   31.417(6)
_cell_length_c                   13.312(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.12(3)
_cell_angle_gamma                90.00
_cell_volume                     4551.4(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2888.0
_exptl_absorpt_coefficient_mu    1.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_process_details   
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43588
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.42
_reflns_number_total             10350
_reflns_number_gt                8582
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0187P)²+17.0916P] where P=(Fo²+2Fc²)/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         10350
_refine_ls_number_parameters     632
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.003
_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
S1 S 0.5000 1.0000 0.0000 0.0166(2) Uani 1 2 d S . .
Mo1 Mo 0.47184(3) 1.024444(12) 0.25780(3) 0.02488(8) Uani 1 1 d . . .
Mo2 Mo 0.76294(3) 1.037651(11) 0.19663(3) 0.02627(9) Uani 1 1 d . . .
Mo3 Mo 0.50099(3) 0.915455(11) 0.18229(3) 0.02424(8) Uani 1 1 d . . .
Mo4 Mo 0.22114(3) 0.972975(11) 0.06936(3) 0.02264(8) Uani 1 1 d . . .
Mo5 Mo 0.76655(3) 0.933321(12) 0.08381(3) 0.02850(9) Uani 1 1 d . . .
Mo6 Mo 0.48820(3) 0.891041(11) -0.08618(3) 0.02970(9) Uani 1 1 d . . .
Cl1 Cl 1.0796(3) 0.72657(8) 0.2457(2) 0.0606(9) Uani 0.569(4) 1 d P A 1
Cl2 Cl 0.7332(3) 0.81427(10) 0.0817(2) 0.0491(10) Uani 0.431(4) 1 d P A 2
O1 O 0.5415(5) 0.95573(16) 0.0332(4) 0.0194(11) Uani 0.50 1 d P . .
O2 O 0.6369(5) 1.00049(16) 0.0318(4) 0.0173(10) Uani 0.50 1 d P . .
O3 O 0.5400(5) 1.02752(16) 0.0941(4) 0.0185(10) Uani 0.50 1 d P . .
O4 O 0.5496(4) 1.01394(16) -0.0812(4) 0.0185(10) Uani 0.50 1 d P . .
O5 O 0.0945(3) 0.96292(12) 0.1047(3) 0.0546(11) Uani 1 1 d . . .
O6 O 0.1903(5) 0.95294(11) -0.0642(3) 0.0589(12) Uani 1 1 d . . .
O7 O 0.3251(3) 0.92947(11) 0.1272(3) 0.0449(9) Uani 1 1 d . . .
O8 O 0.3162(3) 1.00792(10) 0.1886(3) 0.0414(8) Uani 1 1 d . . .
O9 O 0.4867(4) 0.84130(11) -0.1256(3) 0.0484(9) Uani 1 1 d . . .
O10 O 0.4669(3) 0.88664(17) 0.0442(3) 0.0716(15) Uani 1 1 d . . .
O11 O 0.4933(4) 0.87484(11) 0.2588(3) 0.0536(11) Uani 1 1 d . . .
O12 O 0.5120(3) 0.96226(11) 0.2650(3) 0.0426(9) Uani 1 1 d . . .
O13 O 0.4615(3) 1.03405(13) 0.3775(3) 0.0485(10) Uani 1 1 d . . .
O14 O 0.4621(3) 1.07722(13) 0.1982(4) 0.0657(13) Uani 1 1 d . . .
O15 O 0.6645(3) 0.90093(17) -0.0168(3) 0.0672(14) Uani 1 1 d . . .
O16 O 0.6617(3) 0.91630(16) 0.1759(3) 0.0649(13) Uani 1 1 d . . .
O17 O 0.6509(3) 1.02744(13) 0.2715(4) 0.0642(13) Uani 1 1 d . . .
O18 O 0.6673(3) 1.09020(13) 0.1472(4) 0.0652(13) Uani 1 1 d . . .
O19 O 0.8850(3) 1.05571(11) 0.2839(2) 0.0383(8) Uani 1 1 d . . .
O20 O 0.8096(5) 0.96953(11) -0.0075(3) 0.0630(13) Uani 1 1 d . . .
O21 O 0.8002(5) 0.98143(11) 0.1832(3) 0.0609(13) Uani 1 1 d . . .
O22 O 0.8893(3) 0.90310(11) 0.1269(3) 0.0388(8) Uani 1 1 d . . .
O23 O 0.9456(3) 0.91554(10) 0.4752(2) 0.0301(7) Uani 1 1 d . . .
O24 O 0.7056(3) 0.88609(9) 0.4622(2) 0.0284(6) Uani 1 1 d . . .
O25 O 0.6763(3) 0.80054(9) 0.5250(2) 0.0300(7) Uani 1 1 d . . .
O26 O 0.8652(3) 0.75321(10) 0.5932(3) 0.0392(8) Uani 1 1 d . . .
O27 O 1.1103(3) 0.78586(10) 0.6397(2) 0.0319(7) Uani 1 1 d . . .
O28 O 1.1348(3) 0.86985(9) 0.5653(2) 0.0291(6) Uani 1 1 d . . .
N1 N 0.9066(3) 0.82585(11) 0.4839(3) 0.0259(7) Uani 1 1 d . . .
H1A H 0.8513 0.8125 0.5096 0.039 Uiso 1 1 calc R . .
H1B H 0.8886 0.8535 0.4772 0.039 Uiso 1 1 calc R . .
H1C H 0.9810 0.8225 0.5269 0.039 Uiso 1 1 calc R . .
N2 N 0.2894(5) 0.80761(19) 0.3640(5) 0.0777(18) Uani 1 1 d . . .
N3 N 0.4065(5) 0.64240(15) 0.1920(4) 0.0485(11) Uani 1 1 d . . .
C1 C 1.1580(4) 0.90323(13) 0.5053(3) 0.0262(8) Uani 1 1 d . . .
C2 C 1.2726(4) 0.91363(15) 0.4932(4) 0.0343(10) Uani 1 1 d . . .
H2 H 1.3413 0.8982 0.5283 0.041 Uiso 1 1 calc R . .
C3 C 1.2854(5) 0.94718(16) 0.4286(4) 0.0392(11) Uani 1 1 d . . .
H3 H 1.3626 0.9540 0.4205 0.047 Uiso 1 1 calc R . .
C4 C 1.1840(5) 0.97030(15) 0.3767(4) 0.0372(11) Uani 1 1 d . . .
H4 H 1.1927 0.9924 0.3328 0.045 Uiso 1 1 calc R . .
C5 C 1.0680(4) 0.96050(13) 0.3901(3) 0.0303(9) Uani 1 1 d . . .
H5 H 0.9997 0.9762 0.3552 0.036 Uiso 1 1 calc R . .
C6 C 1.0546(4) 0.92765(13) 0.4549(3) 0.0251(8) Uani 1 1 d . . .
C7 C 0.8391(4) 0.94180(14) 0.4333(3) 0.0285(9) Uani 1 1 d . . .
H7A H 0.8089 0.9373 0.3589 0.034 Uiso 1 1 calc R . .
H7B H 0.8601 0.9716 0.4455 0.034 Uiso 1 1 calc R . .
C8 C 0.7425(4) 0.92933(13) 0.4876(4) 0.0299(9) Uani 1 1 d . . .
H8A H 0.7753 0.9322 0.5623 0.036 Uiso 1 1 calc R . .
H8B H 0.6720 0.9480 0.4660 0.036 Uiso 1 1 calc R . .
C9 C 0.6143(4) 0.87312(15) 0.5132(4) 0.0349(10) Uani 1 1 d . . .
H9A H 0.5441 0.8921 0.4935 0.042 Uiso 1 1 calc R . .
H9B H 0.6478 0.8751 0.5880 0.042 Uiso 1 1 calc R . .
C10 C 0.5741(4) 0.82866(14) 0.4845(4) 0.0322(10) Uani 1 1 d . . .
H10A H 0.5063 0.8213 0.5135 0.039 Uiso 1 1 calc R . .
H10B H 0.5465 0.8259 0.4094 0.039 Uiso 1 1 calc R . .
C11 C 0.6542(4) 0.75753(14) 0.5104(3) 0.0301(9) Uani 1 1 d . . .
C12 C 0.5413(5) 0.73925(16) 0.4654(3) 0.0358(10) Uani 1 1 d . . .
H12 H 0.4720 0.7563 0.4425 0.043 Uiso 1 1 calc R . .
C13 C 0.5319(6) 0.69527(17) 0.4547(4) 0.0459(13) Uani 1 1 d . . .
H13 H 0.4558 0.6828 0.4254 0.055 Uiso 1 1 calc R . .
C14 C 0.6352(6) 0.66990(16) 0.4876(4) 0.0497(14) Uani 1 1 d . . .
H14 H 0.6288 0.6405 0.4787 0.060 Uiso 1 1 calc R . .
C15 C 0.7483(5) 0.68823(15) 0.5337(4) 0.0419(12) Uani 1 1 d . . .
H15 H 0.8173 0.6710 0.5558 0.050 Uiso 1 1 calc R . .
C16 C 0.7591(4) 0.73155(15) 0.5468(4) 0.0339(10) Uani 1 1 d . . .
C17 C 0.9701(5) 0.72893(15) 0.6471(4) 0.0405(12) Uani 1 1 d . . .
H17A H 1.0041 0.7136 0.5978 0.049 Uiso 1 1 calc R . .
H17B H 0.9470 0.7085 0.6933 0.049 Uiso 1 1 calc R . .
C18 C 1.0624(5) 0.75968(16) 0.7081(4) 0.0393(11) Uani 1 1 d . . .
H18A H 1.0241 0.7775 0.7502 0.047 Uiso 1 1 calc R . .
H18B H 1.1291 0.7442 0.7544 0.047 Uiso 1 1 calc R . .
C19 C 1.1936(4) 0.81715(16) 0.6968(3) 0.0362(11) Uani 1 1 d . . .
H19A H 1.2629 0.8032 0.7439 0.043 Uiso 1 1 calc R . .
H19B H 1.1524 0.8344 0.7379 0.043 Uiso 1 1 calc R . .
C20 C 1.2382(4) 0.84504(15) 0.6224(4) 0.0327(10) Uani 1 1 d . . .
H20A H 1.3033 0.8636 0.6603 0.039 Uiso 1 1 calc R . .
H20B H 1.2701 0.8277 0.5750 0.039 Uiso 1 1 calc R . .
C21 C 0.9049(4) 0.80791(14) 0.3818(3) 0.0287(9) Uani 1 1 d . . .
C22 C 0.9887(5) 0.77695(14) 0.3751(4) 0.0362(11) Uani 1 1 d . A .
H22 H 1.0455 0.7669 0.4342 0.043 Uiso 1 1 calc R . .
C23 C 0.9853(7) 0.76112(19) 0.2757(6) 0.063(2) Uani 1 1 d . . .
C24 C 0.8997(8) 0.7749(3) 0.1889(5) 0.074(2) Uani 1 1 d . A .
H24 H 0.8971 0.7634 0.1240 0.089 Uiso 1 1 calc R . .
C25 C 0.8183(7) 0.8057(2) 0.1984(4) 0.0606(19) Uani 1 1 d . . .
C26 C 0.8186(5) 0.82319(16) 0.2945(4) 0.0371(11) Uani 1 1 d . A .
H26 H 0.7630 0.8444 0.3002 0.045 Uiso 1 1 calc R . .
C27 C 0.1436(5) 0.86159(17) 0.2472(4) 0.0443(12) Uani 1 1 d . . .
H28A H 0.0871 0.8468 0.1917 0.066 Uiso 1 1 calc R . .
H28B H 0.1904 0.8816 0.2186 0.066 Uiso 1 1 calc R . .
H28C H 0.0988 0.8765 0.2885 0.066 Uiso 1 1 calc R . .
C28 C 0.2263(5) 0.83111(17) 0.3122(5) 0.0446(12) Uani 1 1 d . . .
C29 C 0.3887(6) 0.5880(2) 0.3333(5) 0.0593(16) Uani 1 1 d . . .
H30A H 0.3221 0.5962 0.3619 0.089 Uiso 1 1 calc R . .
H30B H 0.4639 0.5876 0.3876 0.089 Uiso 1 1 calc R . .
H30C H 0.3730 0.5602 0.3028 0.089 Uiso 1 1 calc R . .
C30 C 0.3992(5) 0.61862(17) 0.2536(4) 0.0395(11) Uani 1 1 d . . .


_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
S1 O4 1.410(5) . ?
S1 O4 1.410(5) 3_675 ?
S1 O2 1.491(5) 3_675 ?
S1 O2 1.491(5) . ?
S1 O3 1.492(5) 3_675 ?
S1 O3 1.492(5) . ?
S1 O1 1.497(5) . ?
S1 O1 1.497(5) 3_675 ?
Mo1 O13 1.656(3) . ?
Mo1 O14 1.829(4) . ?
Mo1 O8 1.831(3) . ?
Mo1 O17 1.981(4) . ?
Mo1 O12 2.002(3) . ?
Mo1 O3 2.494(5) . ?
Mo2 O19 1.653(3) . ?
Mo2 O17 1.830(4) . ?
Mo2 O21 1.835(4) . ?
Mo2 O18 1.988(4) . ?
Mo2 O6 1.989(4) 3_675 ?
Mo3 O11 1.649(3) . ?
Mo3 O12 1.822(3) . ?
Mo3 O16 1.835(4) . ?
Mo3 O7 1.977(3) . ?
Mo3 O10 1.995(4) . ?
Mo3 O1 2.494(5) . ?
Mo4 O5 1.645(3) . ?
Mo4 O6 1.832(3) . ?
Mo4 O7 1.834(3) . ?
Mo4 O20 1.978(3) 3_675 ?
Mo4 O8 1.997(3) . ?
Mo4 O2 2.488(5) 3_675 ?
Mo5 O22 1.652(3) . ?
Mo5 O20 1.820(4) . ?
Mo5 O15 1.830(4) . ?
Mo5 O21 1.979(3) . ?
Mo5 O16 1.986(4) . ?
Mo6 O9 1.647(3) . ?
Mo6 O10 1.818(4) . ?
Mo6 O18 1.827(4) 3_675 ?
Mo6 O15 1.985(4) . ?
Mo6 O14 1.992(4) 3_675 ?
Cl1 C23 1.640(6) . ?
Cl2 C25 1.622(6) . ?
O1 O4 1.647(7) 3_675 ?
O1 O2 1.774(7) . ?
O1 O3 1.784(7) 3_675 ?
O2 O4 1.625(7) . ?
O2 O3 1.754(7) . ?
O2 Mo4 2.488(5) 3_675 ?
O3 O4 1.629(7) 3_675 ?
O3 O1 1.784(7) 3_675 ?
O4 O3 1.629(7) 3_675 ?
O4 O1 1.647(7) 3_675 ?
O6 Mo2 1.989(4) 3_675 ?
O14 Mo6 1.992(4) 3_675 ?
O18 Mo6 1.827(4) 3_675 ?
O20 Mo4 1.978(3) 3_675 ?
O23 C6 1.378(5) . ?
O23 C7 1.444(5) . ?
O24 C9 1.432(5) . ?
O24 C8 1.435(5) . ?
O25 C11 1.378(5) . ?
O25 C10 1.440(5) . ?
O26 C16 1.375(6) . ?
O26 C17 1.433(5) . ?
O27 C18 1.433(5) . ?
O27 C19 1.433(6) . ?
O28 C1 1.383(5) . ?
O28 C20 1.443(5) . ?
N1 C21 1.467(5) . ?
N2 C28 1.127(7) . ?
N3 C30 1.128(6) . ?
C1 C2 1.382(6) . ?
C1 C6 1.410(6) . ?
C2 C3 1.391(7) . ?
C3 C4 1.378(7) . ?
C4 C5 1.400(7) . ?
C5 C6 1.378(6) . ?
C7 C8 1.508(6) . ?
C9 C10 1.487(6) . ?
C11 C12 1.383(7) . ?
C11 C16 1.414(6) . ?
C12 C13 1.390(7) . ?
C13 C14 1.385(8) . ?
C14 C15 1.387(8) . ?
C15 C16 1.374(7) . ?
C17 C18 1.495(7) . ?
C19 C20 1.504(7) . ?
C21 C22 1.375(6) . ?
C21 C26 1.392(6) . ?
C22 C23 1.405(8) . ?
C23 C24 1.368(11) . ?
C24 C25 1.361(11) . ?
C25 C26 1.392(8) . ?
C27 C28 1.453(7) . ?
C29 C30 1.459(7) . ?

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
O4 S1 O4 180.0(4) . 3_675 ?
O4 S1 O2 111.9(3) . 3_675 ?
O4 S1 O2 68.1(3) 3_675 3_675 ?
O4 S1 O2 68.1(3) . . ?
O4 S1 O2 111.9(3) 3_675 . ?
O2 S1 O2 180.0 3_675 . ?
O4 S1 O3 68.2(3) . 3_675 ?
O4 S1 O3 111.8(3) 3_675 3_675 ?
O2 S1 O3 72.0(3) 3_675 3_675 ?
O2 S1 O3 108.0(3) . 3_675 ?
O4 S1 O3 111.8(3) . . ?
O4 S1 O3 68.2(3) 3_675 . ?
O2 S1 O3 108.0(3) 3_675 . ?
O2 S1 O3 72.0(3) . . ?
O3 S1 O3 180.0(3) 3_675 . ?
O4 S1 O1 111.1(3) . . ?
O4 S1 O1 68.9(3) 3_675 . ?
O2 S1 O1 107.2(3) 3_675 . ?
O2 S1 O1 72.8(3) . . ?
O3 S1 O1 73.3(3) 3_675 . ?
O3 S1 O1 106.7(3) . . ?
O4 S1 O1 68.9(3) . 3_675 ?
O4 S1 O1 111.1(3) 3_675 3_675 ?
O2 S1 O1 72.8(3) 3_675 3_675 ?
O2 S1 O1 107.2(3) . 3_675 ?
O3 S1 O1 106.7(3) 3_675 3_675 ?
O3 S1 O1 73.3(3) . 3_675 ?
O1 S1 O1 180.000(2) . 3_675 ?
O13 Mo1 O14 103.9(2) . . ?
O13 Mo1 O8 103.71(18) . . ?
O14 Mo1 O8 95.60(17) . . ?
O13 Mo1 O17 103.2(2) . . ?
O14 Mo1 O17 86.64(15) . . ?
O8 Mo1 O17 151.58(19) . . ?
O13 Mo1 O12 101.74(18) . . ?
O14 Mo1 O12 153.22(19) . . ?
O8 Mo1 O12 85.55(14) . . ?
O17 Mo1 O12 80.21(15) . . ?
O13 Mo1 O3 161.60(19) . . ?
O14 Mo1 O3 65.4(2) . . ?
O8 Mo1 O3 92.57(17) . . ?
O17 Mo1 O3 62.61(19) . . ?
O12 Mo1 O3 87.84(16) . . ?
O19 Mo2 O17 104.12(19) . . ?
O19 Mo2 O21 103.3(2) . . ?
O17 Mo2 O21 95.30(19) . . ?
O19 Mo2 O18 103.17(19) . . ?
O17 Mo2 O18 86.21(16) . . ?
O21 Mo2 O18 152.3(2) . . ?
O19 Mo2 O6 101.95(18) . 3_675 ?
O17 Mo2 O6 152.7(2) . 3_675 ?
O21 Mo2 O6 86.34(15) . 3_675 ?
O18 Mo2 O6 80.20(17) . 3_675 ?
O11 Mo3 O12 104.95(19) . . ?
O11 Mo3 O16 104.5(2) . . ?
O12 Mo3 O16 95.96(17) . . ?
O11 Mo3 O7 101.09(18) . . ?
O12 Mo3 O7 87.00(14) . . ?
O16 Mo3 O7 152.43(19) . . ?
O11 Mo3 O10 100.9(2) . . ?
O12 Mo3 O10 152.8(2) . . ?
O16 Mo3 O10 85.38(16) . . ?
O7 Mo3 O10 79.95(16) . . ?
O11 Mo3 O1 159.1(2) . . ?
O12 Mo3 O1 94.22(17) . . ?
O16 Mo3 O1 64.43(19) . . ?
O7 Mo3 O1 88.04(17) . . ?
O10 Mo3 O1 61.85(19) . . ?
O5 Mo4 O6 104.6(2) . . ?
O5 Mo4 O7 104.1(2) . . ?
O6 Mo4 O7 95.19(17) . . ?
O5 Mo4 O20 102.9(2) . 3_675 ?
O6 Mo4 O20 86.62(14) . 3_675 ?
O7 Mo4 O20 151.5(2) . 3_675 ?
O5 Mo4 O8 101.76(18) . . ?
O6 Mo4 O8 152.55(19) . . ?
O7 Mo4 O8 85.67(14) . . ?
O20 Mo4 O8 80.12(15) 3_675 . ?
O5 Mo4 O2 161.2(2) . 3_675 ?
O6 Mo4 O2 64.91(19) . 3_675 ?
O7 Mo4 O2 92.67(18) . 3_675 ?
O20 Mo4 O2 62.37(19) 3_675 3_675 ?
O8 Mo4 O2 87.64(16) . 3_675 ?
O22 Mo5 O20 104.2(2) . . ?
O22 Mo5 O15 104.1(2) . . ?
O20 Mo5 O15 94.88(19) . . ?
O22 Mo5 O21 102.10(18) . . ?
O20 Mo5 O21 86.05(15) . . ?
O15 Mo5 O21 152.6(2) . . ?
O22 Mo5 O16 102.13(19) . . ?
O20 Mo5 O16 152.4(2) . . ?
O15 Mo5 O16 86.59(16) . . ?
O21 Mo5 O16 80.44(18) . . ?
O9 Mo6 O10 103.8(2) . . ?
O9 Mo6 O18 103.6(2) . 3_675 ?
O10 Mo6 O18 95.7(2) . 3_675 ?
O9 Mo6 O15 102.9(2) . . ?
O10 Mo6 O15 86.18(16) . . ?
O18 Mo6 O15 152.2(2) 3_675 . ?
O9 Mo6 O14 102.6(2) . 3_675 ?
O10 Mo6 O14 152.3(2) . 3_675 ?
O18 Mo6 O14 85.99(16) 3_675 3_675 ?
O15 Mo6 O14 80.04(18) . 3_675 ?
S1 O1 O4 53.0(2) . 3_675 ?
S1 O1 O2 53.4(2) . . ?
O4 O1 O2 89.2(3) 3_675 . ?
S1 O1 O3 53.2(2) . 3_675 ?
O4 O1 O3 88.8(3) 3_675 3_675 ?
O2 O1 O3 85.4(3) . 3_675 ?
S1 O1 Mo3 126.8(3) . . ?
O4 O1 Mo3 73.9(3) 3_675 . ?
O2 O1 Mo3 130.4(3) . . ?
O3 O1 Mo3 138.6(3) 3_675 . ?
S1 O2 O4 53.6(2) . . ?
S1 O2 O3 54.0(2) . . ?
O4 O2 O3 90.6(3) . . ?
S1 O2 O1 53.7(2) . . ?
O4 O2 O1 89.6(3) . . ?
O3 O2 O1 85.7(3) . . ?
S1 O2 Mo4 127.9(3) . 3_675 ?
O4 O2 Mo4 74.4(3) . 3_675 ?
O3 O2 Mo4 131.4(3) . 3_675 ?
O1 O2 Mo4 138.5(3) . 3_675 ?
S1 O3 O4 53.5(2) . 3_675 ?
S1 O3 O2 53.9(2) . . ?
O4 O3 O2 90.5(3) 3_675 . ?
S1 O3 O1 53.5(2) . 3_675 ?
O4 O3 O1 89.1(3) 3_675 3_675 ?
O2 O3 O1 85.6(3) . 3_675 ?
S1 O3 Mo1 128.1(3) . . ?
O4 O3 Mo1 74.8(3) 3_675 . ?
O2 O3 Mo1 140.0(3) . . ?
O1 O3 Mo1 130.0(3) 3_675 . ?
S1 O4 O2 58.3(3) . . ?
S1 O4 O3 58.3(3) . 3_675 ?
O2 O4 O3 95.7(4) . 3_675 ?
S1 O4 O1 58.0(3) . 3_675 ?
O2 O4 O1 94.6(4) . 3_675 ?
O3 O4 O1 94.1(4) 3_675 3_675 ?
Mo4 O6 Mo2 141.4(2) . 3_675 ?
Mo4 O7 Mo3 142.3(2) . . ?
Mo1 O8 Mo4 143.2(2) . . ?
Mo6 O10 Mo3 143.5(3) . . ?
Mo3 O12 Mo1 141.3(2) . . ?
Mo1 O14 Mo6 141.4(3) . 3_675 ?
Mo5 O15 Mo6 142.1(2) . . ?
Mo3 O16 Mo5 141.8(3) . . ?
Mo2 O17 Mo1 142.2(3) . . ?
Mo6 O18 Mo2 142.2(2) 3_675 . ?
Mo5 O20 Mo4 143.2(3) . 3_675 ?
Mo2 O21 Mo5 142.3(2) . . ?
C6 O23 C7 117.4(3) . . ?
C9 O24 C8 111.0(3) . . ?
C11 O25 C10 116.9(3) . . ?
C16 O26 C17 118.0(4) . . ?
C18 O27 C19 111.1(3) . . ?
C1 O28 C20 117.8(3) . . ?
C2 C1 O28 124.7(4) . . ?
C2 C1 C6 119.8(4) . . ?
O28 C1 C6 115.5(4) . . ?
C1 C2 C3 120.1(4) . . ?
C4 C3 C2 120.2(5) . . ?
C3 C4 C5 120.0(4) . . ?
C6 C5 C4 120.2(4) . . ?
C5 C6 O23 125.3(4) . . ?
C5 C6 C1 119.6(4) . . ?
O23 C6 C1 115.1(4) . . ?
O23 C7 C8 107.3(3) . . ?
O24 C8 C7 109.5(3) . . ?
O24 C9 C10 110.7(4) . . ?
O25 C10 C9 108.6(4) . . ?
O25 C11 C12 125.4(4) . . ?
O25 C11 C16 114.5(4) . . ?
C12 C11 C16 120.1(4) . . ?
C11 C12 C13 119.6(5) . . ?
C14 C13 C12 120.3(5) . . ?
C13 C14 C15 120.1(5) . . ?
C16 C15 C14 120.6(5) . . ?
C15 C16 O26 125.8(5) . . ?
C15 C16 C11 119.3(5) . . ?
O26 C16 C11 114.8(4) . . ?
O26 C17 C18 107.1(4) . . ?
O27 C18 C17 110.5(4) . . ?
O27 C19 C20 109.6(4) . . ?
O28 C20 C19 107.4(4) . . ?
C22 C21 C26 122.2(4) . . ?
C22 C21 N1 119.2(4) . . ?
C26 C21 N1 118.6(4) . . ?
C21 C22 C23 117.4(5) . . ?
C24 C23 C22 121.6(6) . . ?
C24 C23 Cl1 111.3(5) . . ?
C22 C23 Cl1 127.1(6) . . ?
C25 C24 C23 119.4(5) . . ?
C24 C25 C26 121.8(6) . . ?
C24 C25 Cl2 105.9(5) . . ?
C26 C25 Cl2 132.3(7) . . ?
C25 C26 C21 117.6(5) . . ?
N2 C28 C27 178.8(7) . . ?
N3 C30 C29 179.5(7) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.155
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1026546'
_audit_update_record             
;
2014-09-29 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            ' C60 H72 F2 Mo12 N6 O52 S'
_chemical_formula_weight         2930.59

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'
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'
F F 0.0171 0.0103 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   11.310(2)
_cell_length_b                   31.231(6)
_cell_length_c                   13.308(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.06(3)
_cell_angle_gamma                90.00
_cell_volume                     4539.1(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2856.0
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_process_details   
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43398
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.43
_reflns_number_total             10297
_reflns_number_gt                9363
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0500P)²+11.3728P] where P=(Fo²+2Fc²)/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         10297
_refine_ls_number_parameters     632
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1010
_refine_ls_wR_factor_gt          0.0981
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.002
_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
S1 S 0.5000 0.5000 1.0000 0.0185(2) Uani 1 2 d S . .
Mo1 Mo 0.49943(3) 0.585500(9) 0.81949(2) 0.02387(8) Uani 1 1 d . . .
Mo2 Mo 0.52765(3) 0.476155(10) 0.74203(2) 0.02595(8) Uani 1 1 d . . .
Mo3 Mo 0.23816(3) 0.462568(10) 0.80355(3) 0.02856(8) Uani 1 1 d . . .
Mo4 Mo 0.77764(3) 0.527364(10) 0.93095(2) 0.02486(8) Uani 1 1 d . . .
Mo5 Mo 0.23477(3) 0.567337(10) 0.91743(3) 0.02862(8) Uani 1 1 d . . .
Mo6 Mo 0.48861(3) 0.390479(10) 0.91196(3) 0.02881(8) Uani 1 1 d . . .
F1 F 0.2823(4) 0.67704(16) 0.8803(3) 0.0582(16) Uani 0.673(8) 1 d P A 1
F2 F -0.0474(14) 0.7679(4) 0.7395(11) 0.092(5) Uani 0.327(8) 1 d P A 2
O1 O 0.4597(4) 0.54366(14) 0.9679(4) 0.0193(9) Uani 0.50 1 d P . .
O2 O 0.3626(4) 0.50033(14) 0.9675(4) 0.0195(9) Uani 0.50 1 d P . .
O3 O 0.4616(4) 0.47158(14) 0.9067(4) 0.0193(9) Uani 0.50 1 d P . .
O4 O 0.5484(4) 0.51519(14) 0.9183(4) 0.0193(9) Uani 0.50 1 d P . .
O5 O 0.3361(3) 0.59949(16) 1.0190(3) 0.0618(12) Uani 1 1 d . . .
O6 O 0.1126(3) 0.59804(11) 0.8750(3) 0.0419(7) Uani 1 1 d . . .
O7 O 0.1912(5) 0.53025(10) 1.0084(3) 0.0705(14) Uani 1 1 d . . .
O8 O 0.2006(5) 0.51886(10) 0.8173(2) 0.0658(13) Uani 1 1 d . . .
O9 O 0.3391(3) 0.58427(15) 0.8259(3) 0.0591(11) Uani 1 1 d . . .
O10 O 0.1166(3) 0.44446(10) 0.7161(2) 0.0384(7) Uani 1 1 d . . .
O11 O 0.3334(3) 0.40970(12) 0.8511(4) 0.0669(13) Uani 1 1 d . . .
O12 O 0.4668(3) 0.38552(16) 1.0422(3) 0.0652(12) Uani 1 1 d . . .
O13 O 0.4870(3) 0.34047(10) 0.8706(3) 0.0483(8) Uani 1 1 d . . .
O14 O 0.5379(3) 0.42296(13) 0.8001(4) 0.0690(13) Uani 1 1 d . . .
O15 O 0.3501(3) 0.47333(12) 0.7288(4) 0.0670(13) Uani 1 1 d . . .
O16 O 0.5372(3) 0.46703(12) 0.6220(2) 0.0467(8) Uani 1 1 d . . .
O17 O 0.6831(3) 0.49279(10) 0.8110(3) 0.0447(8) Uani 1 1 d . . .
O18 O 0.4880(3) 0.53872(10) 0.7358(3) 0.0447(8) Uani 1 1 d . . .
O19 O 0.5065(3) 0.62677(11) 0.7434(3) 0.0570(10) Uani 1 1 d . . .
O20 O 0.6745(3) 0.57150(10) 0.8740(3) 0.0466(8) Uani 1 1 d . . .
O21 O 0.8087(5) 0.54734(10) 1.0645(3) 0.0643(12) Uani 1 1 d . . .
O22 O 0.9040(3) 0.53783(11) 0.8959(3) 0.0517(9) Uani 1 1 d . . .
O23 O 0.3259(2) 0.69858(9) 0.4723(2) 0.0332(6) Uani 1 1 d . . .
O24 O 0.2966(2) 0.61287(8) 0.5367(2) 0.0309(6) Uani 1 1 d . . .
O25 O 0.0570(2) 0.58333(9) 0.5247(2) 0.0317(6) Uani 1 1 d . . .
O26 O -0.1315(2) 0.62913(9) 0.4344(2) 0.0313(6) Uani 1 1 d . . .
O27 O -0.1079(3) 0.71341(9) 0.3601(2) 0.0333(6) Uani 1 1 d . . .
O28 O 0.1362(3) 0.74636(9) 0.4058(3) 0.0421(7) Uani 1 1 d . . .
N1 N 0.0958(3) 0.67298(10) 0.5130(2) 0.0282(6) Uani 1 1 d . . .
H1A H 0.1505 0.6861 0.4862 0.042 Uiso 1 1 calc R . .
H1B H 0.0210 0.6774 0.4720 0.042 Uiso 1 1 calc R . .
H1C H 0.1113 0.6450 0.5177 0.042 Uiso 1 1 calc R . .
N2 N 0.7137(5) 0.69443(19) 0.6384(6) 0.086(2) Uani 1 1 d . . .
N3 N 0.0933(4) 0.64106(16) 0.3067(3) 0.0549(11) Uani 1 1 d . . .
C1 C 0.2418(4) 0.76782(13) 0.4521(3) 0.0354(9) Uani 1 1 d . . .
C2 C 0.2530(5) 0.81185(14) 0.4659(4) 0.0452(11) Uani 1 1 d . . .
H2 H 0.1842 0.8292 0.4440 0.054 Uiso 1 1 calc R . .
C3 C 0.3650(6) 0.83018(15) 0.5116(4) 0.0529(13) Uani 1 1 d . . .
H3 H 0.3709 0.8597 0.5216 0.064 Uiso 1 1 calc R . .
C4 C 0.4684(5) 0.80499(16) 0.5424(4) 0.0477(11) Uani 1 1 d . . .
H4 H 0.5443 0.8176 0.5709 0.057 Uiso 1 1 calc R . .
C5 C 0.4588(4) 0.76040(14) 0.5306(3) 0.0374(9) Uani 1 1 d . . .
H5 H 0.5280 0.7433 0.5524 0.045 Uiso 1 1 calc R . .
C6 C 0.3463(4) 0.74197(12) 0.4865(3) 0.0310(8) Uani 1 1 d . . .
C7 C 0.4276(4) 0.67082(13) 0.5130(4) 0.0359(9) Uani 1 1 d . . .
H7A H 0.4555 0.6740 0.5880 0.043 Uiso 1 1 calc R . .
H7B H 0.4948 0.6781 0.4834 0.043 Uiso 1 1 calc R . .
C8 C 0.3874(4) 0.62538(13) 0.4856(4) 0.0365(9) Uani 1 1 d . . .
H8A H 0.3544 0.6229 0.4109 0.044 Uiso 1 1 calc R . .
H8B H 0.4574 0.6064 0.5063 0.044 Uiso 1 1 calc R . .
C9 C 0.2599(4) 0.56944(12) 0.5126(3) 0.0312(8) Uani 1 1 d . . .
H9A H 0.3302 0.5507 0.5349 0.037 Uiso 1 1 calc R . .
H9B H 0.2276 0.5662 0.4380 0.037 Uiso 1 1 calc R . .
C10 C 0.1635(3) 0.55725(12) 0.5668(3) 0.0303(8) Uani 1 1 d . . .
H10A H 0.1429 0.5272 0.5554 0.036 Uiso 1 1 calc R . .
H10B H 0.1935 0.5621 0.6411 0.036 Uiso 1 1 calc R . .
C11 C -0.0511(3) 0.57164(12) 0.5461(3) 0.0283(7) Uani 1 1 d . . .
C12 C -0.0638(4) 0.53869(13) 0.6123(3) 0.0344(8) Uani 1 1 d . . .
H12 H 0.0042 0.5229 0.6473 0.041 Uiso 1 1 calc R . .
C13 C -0.1798(4) 0.52926(14) 0.6262(3) 0.0404(10) Uani 1 1 d . . .
H13 H -0.1885 0.5073 0.6710 0.049 Uiso 1 1 calc R . .
C14 C -0.2798(4) 0.55208(15) 0.5746(4) 0.0422(10) Uani 1 1 d . . .
H14 H -0.3567 0.5451 0.5828 0.051 Uiso 1 1 calc R . .
C15 C -0.2678(4) 0.58599(15) 0.5091(3) 0.0384(9) Uani 1 1 d . . .
H15 H -0.3362 0.6017 0.4747 0.046 Uiso 1 1 calc R . .
C16 C -0.1546(3) 0.59596(12) 0.4960(3) 0.0288(7) Uani 1 1 d . . .
C17 C -0.2350(3) 0.65364(14) 0.3774(3) 0.0350(8) Uani 1 1 d . . .
H17A H -0.2677 0.6708 0.4247 0.042 Uiso 1 1 calc R . .
H17B H -0.2991 0.6347 0.3393 0.042 Uiso 1 1 calc R . .
C18 C -0.1909(4) 0.68208(14) 0.3033(3) 0.0370(9) Uani 1 1 d . . .
H18A H -0.1502 0.6649 0.2616 0.044 Uiso 1 1 calc R . .
H18B H -0.2603 0.6962 0.2568 0.044 Uiso 1 1 calc R . .
C19 C -0.0610(4) 0.73971(15) 0.2916(4) 0.0408(10) Uani 1 1 d . . .
H19A H -0.1277 0.7552 0.2453 0.049 Uiso 1 1 calc R . .
H19B H -0.0224 0.7219 0.2495 0.049 Uiso 1 1 calc R . .
C20 C 0.0305(4) 0.77078(14) 0.3531(4) 0.0424(10) Uani 1 1 d . . .
H20A H 0.0526 0.7917 0.3072 0.051 Uiso 1 1 calc R . .
H20B H -0.0033 0.7858 0.4031 0.051 Uiso 1 1 calc R . .
C21 C 0.1032(3) 0.69036(12) 0.6173(3) 0.0295(7) Uani 1 1 d . . .
C22 C 0.1898(4) 0.67382(14) 0.7012(3) 0.0370(9) Uani 1 1 d . A .
H22 H 0.2424 0.6519 0.6931 0.044 Uiso 1 1 calc R . .
C23 C 0.1952(5) 0.69125(16) 0.7983(4) 0.0464(11) Uani 1 1 d . . .
C24 C 0.1172(6) 0.72295(17) 0.8127(4) 0.0563(14) Uani 1 1 d . A .
H24 H 0.1230 0.7340 0.8787 0.068 Uiso 1 1 calc R . .
C25 C 0.0290(6) 0.73822(17) 0.7261(5) 0.0590(15) Uani 1 1 d . . .
C26 C 0.0226(5) 0.72263(14) 0.6273(4) 0.0434(10) Uani 1 1 d . A .
H26 H -0.0341 0.7335 0.5694 0.052 Uiso 1 1 calc R . .
C27 C 0.8590(5) 0.63940(17) 0.7526(4) 0.0490(11) Uani 1 1 d . . .
H27A H 0.9162 0.6293 0.7159 0.073 Uiso 1 1 calc R . .
H27B H 0.8125 0.6157 0.7679 0.073 Uiso 1 1 calc R . .
H27C H 0.9027 0.6528 0.8164 0.073 Uiso 1 1 calc R . .
C28 C 0.7774(4) 0.66998(17) 0.6892(4) 0.0491(12) Uani 1 1 d . . .
C29 C 0.1085(6) 0.5865(2) 0.1651(5) 0.0636(15) Uani 1 1 d . . .
H29A H 0.0630 0.5970 0.0984 0.095 Uiso 1 1 calc R . .
H29B H 0.0760 0.5594 0.1787 0.095 Uiso 1 1 calc R . .
H29C H 0.1929 0.5832 0.1653 0.095 Uiso 1 1 calc R . .
C30 C 0.0989(4) 0.61699(15) 0.2455(4) 0.0404(10) Uani 1 1 d . . .


_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
S1 O4 1.420(5) 3_667 ?
S1 O4 1.420(5) . ?
S1 O1 1.466(4) . ?
S1 O1 1.466(4) 3_667 ?
S1 O3 1.495(4) 3_667 ?
S1 O3 1.495(4) . ?
S1 O2 1.501(4) . ?
S1 O2 1.501(4) 3_667 ?
Mo1 O19 1.654(3) . ?
Mo1 O18 1.821(3) . ?
Mo1 O9 1.837(3) . ?
Mo1 O20 1.972(3) . ?
Mo1 O12 1.997(3) 3_667 ?
Mo1 O1 2.504(5) . ?
Mo2 O16 1.653(3) . ?
Mo2 O14 1.824(3) . ?
Mo2 O17 1.834(3) . ?
Mo2 O15 1.972(3) . ?
Mo2 O18 2.002(3) . ?
Mo2 O3 2.497(5) . ?
Mo3 O10 1.653(3) . ?
Mo3 O8 1.829(3) . ?
Mo3 O15 1.833(4) . ?
Mo3 O11 1.983(3) . ?
Mo3 O21 1.986(4) 3_667 ?
Mo4 O22 1.648(3) . ?
Mo4 O21 1.829(3) . ?
Mo4 O20 1.837(3) . ?
Mo4 O7 1.966(3) 3_667 ?
Mo4 O17 1.993(3) . ?
Mo4 O2 2.491(5) 3_667 ?
Mo5 O6 1.656(3) . ?
Mo5 O5 1.829(3) . ?
Mo5 O7 1.833(4) . ?
Mo5 O9 1.976(4) . ?
Mo5 O8 1.987(3) . ?
Mo6 O13 1.655(3) . ?
Mo6 O12 1.819(4) . ?
Mo6 O11 1.833(3) . ?
Mo6 O5 1.981(3) 3_667 ?
Mo6 O14 1.996(4) . ?
F1 C23 1.342(7) . ?
F2 C25 1.310(12) . ?
O1 O4 1.605(6) . ?
O1 O3 1.741(6) 3_667 ?
O1 O2 1.742(6) . ?
O2 O4 1.662(6) 3_667 ?
O2 O3 1.784(6) . ?
O2 Mo4 2.491(5) 3_667 ?
O3 O4 1.662(6) . ?
O3 O1 1.741(6) 3_667 ?
O4 O2 1.662(6) 3_667 ?
O5 Mo6 1.981(3) 3_667 ?
O7 Mo4 1.966(3) 3_667 ?
O12 Mo1 1.997(3) 3_667 ?
O21 Mo3 1.986(4) 3_667 ?
O23 C6 1.379(5) . ?
O23 C7 1.430(5) . ?
O24 C8 1.426(5) . ?
O24 C9 1.430(5) . ?
O25 C11 1.376(5) . ?
O25 C10 1.441(4) . ?
O26 C16 1.387(5) . ?
O26 C17 1.439(4) . ?
O27 C19 1.428(5) . ?
O27 C18 1.429(5) . ?
O28 C1 1.369(5) . ?
O28 C20 1.438(5) . ?
N1 C21 1.472(5) . ?
N2 C28 1.143(7) . ?
N3 C30 1.122(6) . ?
C1 C2 1.389(6) . ?
C1 C6 1.406(6) . ?
C2 C3 1.379(8) . ?
C3 C4 1.380(8) . ?
C4 C5 1.402(6) . ?
C5 C6 1.381(6) . ?
C7 C8 1.506(6) . ?
C9 C10 1.505(5) . ?
C11 C12 1.386(5) . ?
C11 C16 1.410(5) . ?
C12 C13 1.404(6) . ?
C13 C14 1.362(7) . ?
C14 C15 1.400(6) . ?
C15 C16 1.371(6) . ?
C17 C18 1.505(6) . ?
C19 C20 1.498(7) . ?
C21 C22 1.380(6) . ?
C21 C26 1.388(6) . ?
C22 C23 1.388(6) . ?
C23 C24 1.372(8) . ?
C24 C25 1.398(9) . ?
C25 C26 1.385(7) . ?
C27 C28 1.439(7) . ?
C29 C30 1.456(7) . ?

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
O4 S1 O4 180.000(2) 3_667 . ?
O4 S1 O1 112.4(3) 3_667 . ?
O4 S1 O1 67.6(3) . . ?
O4 S1 O1 67.6(3) 3_667 3_667 ?
O4 S1 O1 112.4(3) . 3_667 ?
O1 S1 O1 180.000(2) . 3_667 ?
O4 S1 O3 69.5(3) 3_667 3_667 ?
O4 S1 O3 110.5(3) . 3_667 ?
O1 S1 O3 72.0(3) . 3_667 ?
O1 S1 O3 108.0(3) 3_667 3_667 ?
O4 S1 O3 110.5(3) 3_667 . ?
O4 S1 O3 69.5(3) . . ?
O1 S1 O3 108.0(3) . . ?
O1 S1 O3 72.0(3) 3_667 . ?
O3 S1 O3 180.0(3) 3_667 . ?
O4 S1 O2 69.3(3) 3_667 . ?
O4 S1 O2 110.7(3) . . ?
O1 S1 O2 71.9(2) . . ?
O1 S1 O2 108.1(2) 3_667 . ?
O3 S1 O2 106.9(2) 3_667 . ?
O3 S1 O2 73.1(3) . . ?
O4 S1 O2 110.7(3) 3_667 3_667 ?
O4 S1 O2 69.3(3) . 3_667 ?
O1 S1 O2 108.1(2) . 3_667 ?
O1 S1 O2 71.9(2) 3_667 3_667 ?
O3 S1 O2 73.1(3) 3_667 3_667 ?
O3 S1 O2 106.9(2) . 3_667 ?
O2 S1 O2 180.000(1) . 3_667 ?
O19 Mo1 O18 104.94(19) . . ?
O19 Mo1 O9 104.5(2) . . ?
O18 Mo1 O9 95.60(16) . . ?
O19 Mo1 O20 101.22(18) . . ?
O18 Mo1 O20 87.25(13) . . ?
O9 Mo1 O20 152.43(18) . . ?
O19 Mo1 O12 100.6(2) . 3_667 ?
O18 Mo1 O12 153.29(19) . 3_667 ?
O9 Mo1 O12 85.48(14) . 3_667 ?
O20 Mo1 O12 80.11(15) . 3_667 ?
O19 Mo1 O1 159.51(19) . . ?
O18 Mo1 O1 93.70(16) . . ?
O9 Mo1 O1 64.59(17) . . ?
O20 Mo1 O1 87.88(16) . . ?
O12 Mo1 O1 62.62(17) 3_667 . ?
O16 Mo2 O14 103.9(2) . . ?
O16 Mo2 O17 103.71(17) . . ?
O14 Mo2 O17 95.68(16) . . ?
O16 Mo2 O15 103.1(2) . . ?
O14 Mo2 O15 87.03(14) . . ?
O17 Mo2 O15 151.52(19) . . ?
O16 Mo2 O18 101.47(17) . . ?
O14 Mo2 O18 153.60(19) . . ?
O17 Mo2 O18 85.38(12) . . ?
O15 Mo2 O18 80.09(14) . . ?
O16 Mo2 O3 161.40(17) . . ?
O14 Mo2 O3 64.93(19) . . ?
O17 Mo2 O3 92.51(16) . . ?
O15 Mo2 O3 62.98(18) . . ?
O18 Mo2 O3 88.68(15) . . ?
O10 Mo3 O8 103.11(19) . . ?
O10 Mo3 O15 104.25(19) . . ?
O8 Mo3 O15 95.12(19) . . ?
O10 Mo3 O11 102.90(18) . . ?
O8 Mo3 O11 152.8(2) . . ?
O15 Mo3 O11 86.08(15) . . ?
O10 Mo3 O21 101.80(18) . 3_667 ?
O8 Mo3 O21 86.49(15) . 3_667 ?
O15 Mo3 O21 152.8(2) . 3_667 ?
O11 Mo3 O21 80.54(17) . 3_667 ?
O22 Mo4 O21 104.2(2) . . ?
O22 Mo4 O20 103.83(18) . . ?
O21 Mo4 O20 94.93(16) . . ?
O22 Mo4 O7 102.8(2) . 3_667 ?
O21 Mo4 O7 86.84(14) . 3_667 ?
O20 Mo4 O7 152.0(2) . 3_667 ?
O22 Mo4 O17 101.83(17) . . ?
O21 Mo4 O17 152.97(19) . . ?
O20 Mo4 O17 85.69(13) . . ?
O7 Mo4 O17 80.48(15) 3_667 . ?
O22 Mo4 O2 160.79(18) . 3_667 ?
O21 Mo4 O2 65.18(18) . 3_667 ?
O20 Mo4 O2 93.35(16) . 3_667 ?
O7 Mo4 O2 62.05(18) 3_667 3_667 ?
O17 Mo4 O2 87.80(16) . 3_667 ?
O6 Mo5 O5 103.97(19) . . ?
O6 Mo5 O7 104.3(2) . . ?
O5 Mo5 O7 94.78(18) . . ?
O6 Mo5 O9 102.37(17) . . ?
O5 Mo5 O9 87.04(15) . . ?
O7 Mo5 O9 152.0(2) . . ?
O6 Mo5 O8 102.29(19) . . ?
O5 Mo5 O8 152.8(2) . . ?
O7 Mo5 O8 85.57(15) . . ?
O9 Mo5 O8 80.44(17) . . ?
O13 Mo6 O12 104.1(2) . . ?
O13 Mo6 O11 103.6(2) . . ?
O12 Mo6 O11 95.58(19) . . ?
O13 Mo6 O5 103.13(18) . 3_667 ?
O12 Mo6 O5 86.48(15) . 3_667 ?
O11 Mo6 O5 151.78(19) . 3_667 ?
O13 Mo6 O14 102.3(2) . . ?
O12 Mo6 O14 152.4(2) . . ?
O11 Mo6 O14 85.72(15) . . ?
O5 Mo6 O14 79.97(17) 3_667 . ?
S1 O1 O4 54.9(2) . . ?
S1 O1 O3 54.8(2) . 3_667 ?
O4 O1 O3 91.4(3) . 3_667 ?
S1 O1 O2 55.0(2) . . ?
O4 O1 O2 91.7(3) . . ?
O3 O1 O2 87.4(3) 3_667 . ?
S1 O1 Mo1 127.5(3) . . ?
O4 O1 Mo1 72.9(2) . . ?
O3 O1 Mo1 138.3(3) 3_667 . ?
O2 O1 Mo1 130.2(3) . . ?
S1 O2 O4 53.0(2) . 3_667 ?
S1 O2 O1 53.1(2) . . ?
O4 O2 O1 89.6(3) 3_667 . ?
S1 O2 O3 53.3(2) . . ?
O4 O2 O3 88.0(3) 3_667 . ?
O1 O2 O3 85.6(3) . . ?
S1 O2 Mo4 126.8(3) . 3_667 ?
O4 O2 Mo4 73.9(2) 3_667 3_667 ?
O1 O2 Mo4 139.3(3) . 3_667 ?
O3 O2 Mo4 129.4(3) . 3_667 ?
S1 O3 O4 53.1(2) . . ?
S1 O3 O1 53.2(2) . 3_667 ?
O4 O3 O1 89.6(3) . 3_667 ?
S1 O3 O2 53.6(2) . . ?
O4 O3 O2 88.3(3) . . ?
O1 O3 O2 85.9(3) 3_667 . ?
S1 O3 Mo2 127.3(3) . . ?
O4 O3 Mo2 74.3(2) . . ?
O1 O3 Mo2 131.4(3) 3_667 . ?
O2 O3 Mo2 137.3(3) . . ?
S1 O4 O1 57.6(2) . . ?
S1 O4 O2 57.6(2) . 3_667 ?
O1 O4 O2 94.6(3) . 3_667 ?
S1 O4 O3 57.4(2) . . ?
O1 O4 O3 94.3(3) . . ?
O2 O4 O3 92.8(3) 3_667 . ?
Mo5 O5 Mo6 142.1(2) . 3_667 ?
Mo5 O7 Mo4 143.0(3) . 3_667 ?
Mo3 O8 Mo5 142.1(2) . . ?
Mo1 O9 Mo5 142.1(2) . . ?
Mo6 O11 Mo3 142.4(2) . . ?
Mo6 O12 Mo1 143.0(2) . 3_667 ?
Mo2 O14 Mo6 141.2(3) . . ?
Mo3 O15 Mo2 142.3(3) . . ?
Mo2 O17 Mo4 143.07(19) . . ?
Mo1 O18 Mo2 141.12(19) . . ?
Mo4 O20 Mo1 141.92(19) . . ?
Mo4 O21 Mo3 141.1(2) . 3_667 ?
C6 O23 C7 117.0(3) . . ?
C8 O24 C9 110.8(3) . . ?
C11 O25 C10 117.9(3) . . ?
C16 O26 C17 117.1(3) . . ?
C19 O27 C18 111.0(3) . . ?
C1 O28 C20 118.5(3) . . ?
O28 C1 C2 125.7(4) . . ?
O28 C1 C6 115.2(4) . . ?
C2 C1 C6 119.1(4) . . ?
C3 C2 C1 120.7(5) . . ?
C2 C3 C4 120.3(4) . . ?
C3 C4 C5 119.9(5) . . ?
C6 C5 C4 119.8(4) . . ?
O23 C6 C5 124.8(4) . . ?
O23 C6 C1 115.1(4) . . ?
C5 C6 C1 120.2(4) . . ?
O23 C7 C8 108.5(3) . . ?
O24 C8 C7 110.6(3) . . ?
O24 C9 C10 109.6(3) . . ?
O25 C10 C9 107.9(3) . . ?
O25 C11 C12 125.0(4) . . ?
O25 C11 C16 115.6(3) . . ?
C12 C11 C16 119.4(4) . . ?
C11 C12 C13 119.6(4) . . ?
C14 C13 C12 120.4(4) . . ?
C13 C14 C15 120.5(4) . . ?
C16 C15 C14 119.7(4) . . ?
C15 C16 O26 124.8(4) . . ?
C15 C16 C11 120.3(4) . . ?
O26 C16 C11 114.9(3) . . ?
O26 C17 C18 107.3(3) . . ?
O27 C18 C17 110.0(3) . . ?
O27 C19 C20 110.0(4) . . ?
O28 C20 C19 107.0(3) . . ?
C22 C21 C26 122.7(4) . . ?
C22 C21 N1 118.6(4) . . ?
C26 C21 N1 118.7(4) . . ?
C21 C22 C23 117.1(4) . . ?
F1 C23 C24 119.2(5) . . ?
F1 C23 C22 118.2(5) . . ?
C24 C23 C22 122.6(5) . . ?
C23 C24 C25 118.5(5) . . ?
F2 C25 C26 120.2(9) . . ?
F2 C25 C24 118.9(8) . . ?
C26 C25 C24 120.8(5) . . ?
C25 C26 C21 118.2(5) . . ?
N2 C28 C27 179.2(7) . . ?
N3 C30 C29 178.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.679
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.188
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/. 
# 
# Audit and citation data items have may been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1026547'
_audit_update_record             
;
2014-09-29 deposited with the CCDC.
2014-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H74 I2 Mo12 N6 O52 S'
_chemical_formula_weight         3148.40

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'
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'
I I -0.4742 1.8119 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   11.113(2)
_cell_length_b                   31.240(6)
_cell_length_c                   13.533(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.97(3)
_cell_angle_gamma                90.00
_cell_volume                     4559.2(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3036.0
_exptl_absorpt_coefficient_mu    2.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_process_details   
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43779
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.42
_reflns_number_total             10328
_reflns_number_gt                9089
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0390P)²+12.8561P] where P=(Fo²+2Fc²)/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         10328
_refine_ls_number_parameters     622
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.003
_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
S1 S 0.5000 0.0000 1.0000 0.0154(2) Uani 1 2 d S . .
Mo1 Mo 0.21522(3) 0.022757(10) 1.07234(2) 0.02016(7) Uani 1 1 d . . .
Mo2 Mo 0.49294(3) 0.083069(10) 1.18196(2) 0.02203(7) Uani 1 1 d . . .
Mo3 Mo 0.47563(3) 0.110310(10) 0.91886(3) 0.02611(8) Uani 1 1 d . . .
Mo4 Mo 0.23817(3) -0.070547(10) 0.92053(2) 0.02374(8) Uani 1 1 d . . .
Mo5 Mo 0.23063(3) 0.035579(10) 0.81137(2) 0.02404(8) Uani 1 1 d . . .
Mo6 Mo 0.52740(3) 0.027767(11) 0.74762(2) 0.02447(8) Uani 1 1 d . . .
I1 I 1.13217(4) 0.283869(10) 0.25328(3) 0.04992(10) Uani 1 1 d . . .
N1 N 0.9083(3) 0.17518(10) 0.4767(2) 0.0231(6) Uani 1 1 d . . .
H1A H 0.9762 0.1837 0.5220 0.035 Uiso 1 1 calc R . .
H1B H 0.9075 0.1467 0.4729 0.035 Uiso 1 1 calc R . .
H1C H 0.8414 0.1842 0.4958 0.035 Uiso 1 1 calc R . .
N2 N 0.8806(5) 0.14767(16) 0.6815(3) 0.0544(12) Uani 1 1 d . . .
N3 N 0.7804(4) 0.31393(17) 0.8813(4) 0.0650(14) Uani 1 1 d . . .
O1 O 0.5395(4) 0.04359(14) 1.0334(3) 0.0166(9) Uani 0.50 1 d P . .
O2 O 0.4459(4) 0.01372(15) 1.0820(3) 0.0165(9) Uani 0.50 1 d P . .
O3 O 0.3649(4) -0.00232(14) 0.9706(3) 0.0152(9) Uani 0.50 1 d P . .
O4 O 0.4550(4) 0.02951(15) 0.9099(3) 0.0173(9) Uani 0.50 1 d P . .
O5 O 0.4792(3) 0.12326(11) 1.2580(3) 0.0511(10) Uani 1 1 d . . .
O6 O 0.5080(3) 0.03527(10) 1.2610(3) 0.0490(9) Uani 1 1 d . . .
O7 O 0.3149(3) -0.01242(10) 1.1873(3) 0.0490(10) Uani 1 1 d . . .
O8 O 0.0872(3) 0.03068(11) 1.1109(3) 0.0489(9) Uani 1 1 d . . .
O9 O 0.6547(3) 0.08477(15) 1.1730(3) 0.0573(11) Uani 1 1 d . . .
O10 O 0.3163(3) 0.06705(11) 1.1293(3) 0.0510(10) Uani 1 1 d . . .
O11 O 0.1904(5) -0.03534(10) 1.0116(2) 0.0563(11) Uani 1 1 d . . .
O12 O 0.1167(3) -0.10223(12) 0.8801(3) 0.0460(8) Uani 1 1 d . . .
O13 O 0.1810(4) 0.04343(9) 0.9424(2) 0.0498(10) Uani 1 1 d . . .
O14 O 0.4553(3) 0.11282(16) 1.0480(3) 0.0634(13) Uani 1 1 d . . .
O15 O 0.3217(3) 0.08938(14) 0.8613(4) 0.0725(15) Uani 1 1 d . . .
O16 O 0.6558(3) 0.10275(15) 0.9845(3) 0.0569(11) Uani 1 1 d . . .
O17 O 0.1993(4) -0.02133(10) 0.8238(2) 0.0527(10) Uani 1 1 d . . .
O18 O 0.1065(3) 0.05325(11) 0.7272(2) 0.0389(7) Uani 1 1 d . . .
O19 O 0.3461(3) 0.02817(13) 0.7366(4) 0.0671(14) Uani 1 1 d . . .
O20 O 0.5310(3) 0.08057(14) 0.8077(4) 0.0680(14) Uani 1 1 d . . .
O21 O 0.4658(3) 0.16105(9) 0.8836(3) 0.0424(8) Uani 1 1 d . . .
O22 O 0.5381(3) 0.03877(11) 0.6303(2) 0.0382(7) Uani 1 1 d . . .
O23 O 0.9416(2) 0.08368(9) 0.4724(2) 0.0291(6) Uani 1 1 d . . .
O24 O 0.6994(2) 0.11469(8) 0.4496(2) 0.0260(5) Uani 1 1 d . . .
O25 O 0.6711(2) 0.20203(9) 0.5011(2) 0.0284(6) Uani 1 1 d . . .
O26 O 0.8588(3) 0.24985(9) 0.5756(2) 0.0360(7) Uani 1 1 d . . .
O27 O 1.1031(3) 0.21435(9) 0.6338(2) 0.0295(6) Uani 1 1 d . . .
O28 O 1.1314(2) 0.12795(9) 0.5690(2) 0.0298(6) Uani 1 1 d . . .
C1 C 1.1579(4) 0.09447(13) 0.5112(3) 0.0269(8) Uani 1 1 d . . .
C2 C 1.2760(4) 0.08343(15) 0.5026(3) 0.0339(9) Uani 1 1 d . . .
H2 H 1.3446 0.0986 0.5389 0.041 Uiso 1 1 calc R . .
C3 C 1.2920(4) 0.04978(15) 0.4398(3) 0.0370(10) Uani 1 1 d . . .
H3 H 1.3715 0.0425 0.4350 0.044 Uiso 1 1 calc R . .
C4 C 1.1915(4) 0.02707(14) 0.3845(3) 0.0346(9) Uani 1 1 d . . .
H4 H 1.2030 0.0050 0.3416 0.042 Uiso 1 1 calc R . .
C5 C 1.0715(4) 0.03773(13) 0.3937(3) 0.0305(8) Uani 1 1 d . . .
H5 H 1.0034 0.0224 0.3572 0.037 Uiso 1 1 calc R . .
C6 C 1.0546(4) 0.07108(12) 0.4570(3) 0.0260(8) Uani 1 1 d . . .
C7 C 0.8350(4) 0.05789(12) 0.4274(3) 0.0277(8) Uani 1 1 d . . .
H7A H 0.8537 0.0278 0.4403 0.033 Uiso 1 1 calc R . .
H7B H 0.8107 0.0624 0.3544 0.033 Uiso 1 1 calc R . .
C8 C 0.7322(4) 0.07145(13) 0.4756(3) 0.0292(8) Uani 1 1 d . . .
H8A H 0.6606 0.0531 0.4518 0.035 Uiso 1 1 calc R . .
H8B H 0.7593 0.0686 0.5490 0.035 Uiso 1 1 calc R . .
C9 C 0.6052(4) 0.12898(13) 0.4978(3) 0.0302(8) Uani 1 1 d . . .
H9A H 0.6364 0.1276 0.5712 0.036 Uiso 1 1 calc R . .
H9B H 0.5338 0.1102 0.4790 0.036 Uiso 1 1 calc R . .
C10 C 0.5664(4) 0.17394(13) 0.4673(3) 0.0297(8) Uani 1 1 d . . .
H10A H 0.5368 0.1757 0.3938 0.036 Uiso 1 1 calc R . .
H10B H 0.4996 0.1825 0.4977 0.036 Uiso 1 1 calc R . .
C11 C 0.6474(4) 0.24499(13) 0.4937(3) 0.0278(8) Uani 1 1 d . . .
C12 C 0.5321(4) 0.26346(13) 0.4535(3) 0.0304(8) Uani 1 1 d . . .
H12 H 0.4633 0.2462 0.4283 0.036 Uiso 1 1 calc R . .
C13 C 0.5198(5) 0.30819(15) 0.4510(3) 0.0401(10) Uani 1 1 d . . .
H13 H 0.4426 0.3205 0.4241 0.048 Uiso 1 1 calc R . .
C14 C 0.6209(5) 0.33408(14) 0.4881(4) 0.0446(11) Uani 1 1 d . . .
H14 H 0.6122 0.3637 0.4853 0.054 Uiso 1 1 calc R . .
C15 C 0.7371(5) 0.31553(14) 0.5301(3) 0.0386(10) Uani 1 1 d . . .
H15 H 0.8053 0.3330 0.5555 0.046 Uiso 1 1 calc R . .
C16 C 0.7508(4) 0.27162(13) 0.5339(3) 0.0308(8) Uani 1 1 d . . .
C17 C 0.9624(4) 0.27336(13) 0.6343(3) 0.0356(9) Uani 1 1 d . . .
H17A H 0.9348 0.2938 0.6780 0.043 Uiso 1 1 calc R . .
H17B H 1.0035 0.2888 0.5896 0.043 Uiso 1 1 calc R . .
C18 C 1.0499(4) 0.24140(15) 0.6974(3) 0.0366(10) Uani 1 1 d . . .
H18A H 1.1154 0.2565 0.7451 0.044 Uiso 1 1 calc R . .
H18B H 1.0053 0.2240 0.7362 0.044 Uiso 1 1 calc R . .
C19 C 1.1843(4) 0.18305(15) 0.6938(3) 0.0353(9) Uani 1 1 d . . .
H19A H 1.1391 0.1667 0.7339 0.042 Uiso 1 1 calc R . .
H19B H 1.2525 0.1974 0.7402 0.042 Uiso 1 1 calc R . .
C20 C 1.2342(4) 0.15344(14) 0.6257(3) 0.0341(9) Uani 1 1 d . . .
H20A H 1.2706 0.1698 0.5794 0.041 Uiso 1 1 calc R . .
H20B H 1.2977 0.1350 0.6661 0.041 Uiso 1 1 calc R . .
C21 C 0.9082(3) 0.19322(12) 0.3765(3) 0.0223(7) Uani 1 1 d . . .
C22 C 0.9958(4) 0.22401(13) 0.3687(3) 0.0280(8) Uani 1 1 d . . .
H22 H 1.0535 0.2334 0.4263 0.034 Uiso 1 1 calc R . .
C23 C 0.9953(4) 0.24047(13) 0.2728(3) 0.0339(9) Uani 1 1 d . . .
C24 C 0.9066(5) 0.22674(15) 0.1870(3) 0.0386(10) Uani 1 1 d . . .
H24 H 0.9050 0.2383 0.1234 0.046 Uiso 1 1 calc R . .
C25 C 0.8212(4) 0.19584(16) 0.1971(3) 0.0397(10) Uani 1 1 d . . .
H25 H 0.7634 0.1863 0.1396 0.048 Uiso 1 1 calc R . .
C26 C 0.8203(4) 0.17880(13) 0.2918(3) 0.0308(8) Uani 1 1 d . . .
H26 H 0.7623 0.1582 0.2983 0.037 Uiso 1 1 calc R . .
C27 C 0.8777(5) 0.09041(17) 0.8198(4) 0.0490(12) Uani 1 1 d . . .
H28A H 0.8081 0.0959 0.8484 0.073 Uiso 1 1 calc R . .
H28B H 0.9529 0.0918 0.8726 0.073 Uiso 1 1 calc R . .
H28C H 0.8698 0.0625 0.7895 0.073 Uiso 1 1 calc R . .
C28 C 0.8814(4) 0.12273(15) 0.7417(3) 0.0360(9) Uani 1 1 d . . .
C29 C 0.6443(5) 0.36547(17) 0.7517(4) 0.0453(11) Uani 1 1 d . . .
H30A H 0.6000 0.3496 0.6936 0.068 Uiso 1 1 calc R . .
H30B H 0.6952 0.3867 0.7303 0.068 Uiso 1 1 calc R . .
H30C H 0.5863 0.3793 0.7836 0.068 Uiso 1 1 calc R . .
C30 C 0.7221(4) 0.33660(17) 0.8237(4) 0.0443(11) Uani 1 1 d . . .


_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
S1 O2 1.450(4) . ?
S1 O2 1.450(4) 3_657 ?
S1 O3 1.460(4) 3_657 ?
S1 O3 1.460(4) . ?
S1 O1 1.468(5) . ?
S1 O1 1.468(5) 3_657 ?
S1 O4 1.514(5) . ?
S1 O4 1.514(5) 3_657 ?
Mo1 O8 1.648(3) . ?
Mo1 O13 1.825(3) . ?
Mo1 O10 1.831(3) . ?
Mo1 O11 1.984(3) . ?
Mo1 O7 2.006(3) . ?
Mo2 O5 1.654(3) . ?
Mo2 O6 1.821(3) . ?
Mo2 O9 1.832(3) . ?
Mo2 O10 1.984(3) . ?
Mo2 O14 1.989(3) . ?
Mo2 O1 2.517(5) . ?
Mo3 O21 1.652(3) . ?
Mo3 O14 1.818(4) . ?
Mo3 O15 1.821(4) . ?
Mo3 O20 1.988(4) . ?
Mo3 O16 1.998(3) . ?
Mo4 O12 1.656(3) . ?
Mo4 O16 1.823(3) 3_657 ?
Mo4 O11 1.823(3) . ?
Mo4 O9 1.986(3) 3_657 ?
Mo4 O17 1.998(3) . ?
Mo5 O18 1.657(3) . ?
Mo5 O17 1.827(3) . ?
Mo5 O19 1.830(4) . ?
Mo5 O15 1.994(3) . ?
Mo5 O13 1.995(3) . ?
Mo6 O22 1.657(3) . ?
Mo6 O7 1.825(3) 3_657 ?
Mo6 O20 1.835(4) . ?
Mo6 O19 1.984(3) . ?
Mo6 O6 2.006(3) 3_657 ?
Mo6 O4 2.515(5) . ?
I1 C23 2.101(4) . ?
N1 C21 1.468(5) . ?
N2 C28 1.125(6) . ?
N3 C30 1.133(7) . ?
O1 O2 1.649(6) . ?
O1 O3 1.680(6) 3_657 ?
O1 O4 1.764(6) . ?
O2 O3 1.638(6) . ?
O2 O4 1.730(6) 3_657 ?
O3 O1 1.680(6) 3_657 ?
O3 O4 1.750(6) . ?
O4 O2 1.730(6) 3_657 ?
O6 Mo6 2.006(3) 3_657 ?
O7 Mo6 1.825(3) 3_657 ?
O9 Mo4 1.986(3) 3_657 ?
O16 Mo4 1.823(3) 3_657 ?
O23 C6 1.379(5) . ?
O23 C7 1.440(4) . ?
O24 C8 1.421(5) . ?
O24 C9 1.433(5) . ?
O25 C11 1.367(5) . ?
O25 C10 1.441(4) . ?
O26 C16 1.377(5) . ?
O26 C17 1.433(5) . ?
O27 C18 1.433(5) . ?
O27 C19 1.441(5) . ?
O28 C1 1.380(5) . ?
O28 C20 1.451(5) . ?
C1 C2 1.389(6) . ?
C1 C6 1.409(5) . ?
C2 C3 1.390(6) . ?
C3 C4 1.381(7) . ?
C4 C5 1.409(6) . ?
C5 C6 1.390(6) . ?
C7 C8 1.506(6) . ?
C9 C10 1.498(6) . ?
C11 C12 1.391(6) . ?
C11 C16 1.416(6) . ?
C12 C13 1.404(6) . ?
C13 C14 1.377(7) . ?
C14 C15 1.404(7) . ?
C15 C16 1.380(6) . ?
C17 C18 1.507(7) . ?
C19 C20 1.503(6) . ?
C21 C26 1.389(5) . ?
C21 C22 1.390(5) . ?
C22 C23 1.395(6) . ?
C23 C24 1.397(7) . ?
C24 C25 1.383(7) . ?
C25 C26 1.390(6) . ?
C27 C28 1.470(7) . ?
C29 C30 1.450(7) . ?

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 S1 O2 180.00(18) . 3_657 ?
O2 S1 O3 111.5(2) . 3_657 ?
O2 S1 O3 68.5(2) 3_657 3_657 ?
O2 S1 O3 68.5(2) . . ?
O2 S1 O3 111.5(2) 3_657 . ?
O3 S1 O3 180.0 3_657 . ?
O2 S1 O1 68.8(3) . . ?
O2 S1 O1 111.2(3) 3_657 . ?
O3 S1 O1 70.0(2) 3_657 . ?
O3 S1 O1 110.0(2) . . ?
O2 S1 O1 111.2(3) . 3_657 ?
O2 S1 O1 68.8(3) 3_657 3_657 ?
O3 S1 O1 110.0(2) 3_657 3_657 ?
O3 S1 O1 70.0(2) . 3_657 ?
O1 S1 O1 180.00(13) . 3_657 ?
O2 S1 O4 108.6(3) . . ?
O2 S1 O4 71.4(3) 3_657 . ?
O3 S1 O4 107.9(3) 3_657 . ?
O3 S1 O4 72.1(3) . . ?
O1 S1 O4 72.5(3) . . ?
O1 S1 O4 107.5(3) 3_657 . ?
O2 S1 O4 71.4(3) . 3_657 ?
O2 S1 O4 108.6(3) 3_657 3_657 ?
O3 S1 O4 72.1(3) 3_657 3_657 ?
O3 S1 O4 107.9(3) . 3_657 ?
O1 S1 O4 107.5(3) . 3_657 ?
O1 S1 O4 72.5(3) 3_657 3_657 ?
O4 S1 O4 180.0(3) . 3_657 ?
O8 Mo1 O13 104.9(2) . . ?
O8 Mo1 O10 104.0(2) . . ?
O13 Mo1 O10 95.87(16) . . ?
O8 Mo1 O11 102.98(19) . . ?
O13 Mo1 O11 87.04(13) . . ?
O10 Mo1 O11 151.12(19) . . ?
O8 Mo1 O7 101.17(18) . . ?
O13 Mo1 O7 152.72(18) . . ?
O10 Mo1 O7 85.40(13) . . ?
O11 Mo1 O7 79.38(14) . . ?
O5 Mo2 O6 105.4(2) . . ?
O5 Mo2 O9 105.0(2) . . ?
O6 Mo2 O9 96.34(17) . . ?
O5 Mo2 O10 100.54(18) . . ?
O6 Mo2 O10 86.95(14) . . ?
O9 Mo2 O10 152.29(19) . . ?
O5 Mo2 O14 100.5(2) . . ?
O6 Mo2 O14 152.58(19) . . ?
O9 Mo2 O14 85.41(14) . . ?
O10 Mo2 O14 79.53(16) . . ?
O5 Mo2 O1 159.55(19) . . ?
O6 Mo2 O1 93.45(17) . . ?
O9 Mo2 O1 64.32(17) . . ?
O10 Mo2 O1 88.06(17) . . ?
O14 Mo2 O1 62.60(17) . . ?
O21 Mo3 O14 102.82(19) . . ?
O21 Mo3 O15 103.4(2) . . ?
O14 Mo3 O15 96.0(2) . . ?
O21 Mo3 O20 103.93(19) . . ?
O14 Mo3 O20 151.8(2) . . ?
O15 Mo3 O20 86.49(15) . . ?
O21 Mo3 O16 103.36(18) . . ?
O14 Mo3 O16 85.51(15) . . ?
O15 Mo3 O16 152.2(2) . . ?
O20 Mo3 O16 79.70(17) . . ?
O12 Mo4 O16 103.9(2) . 3_657 ?
O12 Mo4 O11 103.70(19) . . ?
O16 Mo4 O11 95.78(17) 3_657 . ?
O12 Mo4 O9 102.81(18) . 3_657 ?
O16 Mo4 O9 86.60(14) 3_657 3_657 ?
O11 Mo4 O9 152.0(2) . 3_657 ?
O12 Mo4 O17 102.32(18) . . ?
O16 Mo4 O17 152.57(19) 3_657 . ?
O11 Mo4 O17 85.77(14) . . ?
O9 Mo4 O17 79.79(15) 3_657 . ?
O18 Mo5 O17 104.01(18) . . ?
O18 Mo5 O19 103.9(2) . . ?
O17 Mo5 O19 95.89(18) . . ?
O18 Mo5 O15 102.8(2) . . ?
O17 Mo5 O15 151.8(2) . . ?
O19 Mo5 O15 85.86(15) . . ?
O18 Mo5 O13 101.96(16) . . ?
O17 Mo5 O13 86.44(14) . . ?
O19 Mo5 O13 152.61(19) . . ?
O15 Mo5 O13 79.74(16) . . ?
O22 Mo6 O7 103.55(17) . 3_657 ?
O22 Mo6 O20 103.9(2) . . ?
O7 Mo6 O20 96.11(18) 3_657 . ?
O22 Mo6 O19 103.50(19) . . ?
O7 Mo6 O19 151.3(2) 3_657 . ?
O20 Mo6 O19 86.59(15) . . ?
O22 Mo6 O6 101.90(17) . 3_657 ?
O7 Mo6 O6 85.54(13) 3_657 3_657 ?
O20 Mo6 O6 153.01(19) . 3_657 ?
O19 Mo6 O6 79.67(16) . 3_657 ?
O22 Mo6 O4 160.81(16) . . ?
O7 Mo6 O4 93.24(17) 3_657 . ?
O20 Mo6 O4 64.59(19) . . ?
O19 Mo6 O4 62.11(18) . . ?
O6 Mo6 O4 88.43(16) 3_657 . ?
S1 O1 O2 55.1(2) . . ?
S1 O1 O3 54.8(2) . 3_657 ?
O2 O1 O3 92.5(3) . 3_657 ?
S1 O1 O4 55.0(2) . . ?
O2 O1 O4 89.7(3) . . ?
O3 O1 O4 88.6(3) 3_657 . ?
S1 O1 Mo2 126.6(3) . . ?
O2 O1 Mo2 71.8(2) . . ?
O3 O1 Mo2 130.9(3) 3_657 . ?
O4 O1 Mo2 135.6(3) . . ?
S1 O2 O3 56.0(2) . . ?
S1 O2 O1 56.1(2) . . ?
O3 O2 O1 93.7(3) . . ?
S1 O2 O4 56.1(2) . 3_657 ?
O3 O2 O4 91.1(3) . 3_657 ?
O1 O2 O4 90.7(3) . 3_657 ?
S1 O3 O2 55.4(2) . . ?
S1 O3 O1 55.2(2) . 3_657 ?
O2 O3 O1 93.0(3) . 3_657 ?
S1 O3 O4 55.4(2) . . ?
O2 O3 O4 90.5(3) . . ?
O1 O3 O4 89.0(3) 3_657 . ?
S1 O4 O2 52.6(2) . 3_657 ?
S1 O4 O3 52.5(2) . . ?
O2 O4 O3 87.4(3) 3_657 . ?
S1 O4 O1 52.5(2) . . ?
O2 O4 O1 87.1(3) 3_657 . ?
O3 O4 O1 86.1(3) . . ?
S1 O4 Mo6 125.2(3) . . ?
O2 O4 Mo6 72.8(2) 3_657 . ?
O3 O4 Mo6 137.5(3) . . ?
O1 O4 Mo6 128.5(3) . . ?
Mo2 O6 Mo6 141.4(2) . 3_657 ?
Mo6 O7 Mo1 143.5(2) 3_657 . ?
Mo2 O9 Mo4 141.7(2) . 3_657 ?
Mo1 O10 Mo2 142.6(2) . . ?
Mo4 O11 Mo1 142.9(2) . . ?
Mo1 O13 Mo5 140.8(2) . . ?
Mo3 O14 Mo2 143.9(2) . . ?
Mo3 O15 Mo5 142.7(3) . . ?
Mo4 O16 Mo3 141.9(2) 3_657 . ?
Mo5 O17 Mo4 142.5(2) . . ?
Mo5 O19 Mo6 142.6(3) . . ?
Mo6 O20 Mo3 141.1(3) . . ?
C6 O23 C7 117.5(3) . . ?
C8 O24 C9 110.8(3) . . ?
C11 O25 C10 116.6(3) . . ?
C16 O26 C17 118.6(3) . . ?
C18 O27 C19 110.8(3) . . ?
C1 O28 C20 117.9(3) . . ?
O28 C1 C2 124.8(4) . . ?
O28 C1 C6 115.4(3) . . ?
C2 C1 C6 119.7(4) . . ?
C1 C2 C3 120.1(4) . . ?
C4 C3 C2 120.9(4) . . ?
C3 C4 C5 119.3(4) . . ?
C6 C5 C4 120.2(4) . . ?
O23 C6 C5 124.8(4) . . ?
O23 C6 C1 115.5(3) . . ?
C5 C6 C1 119.7(4) . . ?
O23 C7 C8 107.0(3) . . ?
O24 C8 C7 109.6(3) . . ?
O24 C9 C10 111.1(3) . . ?
O25 C10 C9 109.1(3) . . ?
O25 C11 C12 125.4(4) . . ?
O25 C11 C16 115.1(4) . . ?
C12 C11 C16 119.5(4) . . ?
C11 C12 C13 119.8(4) . . ?
C14 C13 C12 120.7(4) . . ?
C13 C14 C15 119.6(4) . . ?
C16 C15 C14 120.5(4) . . ?
O26 C16 C15 125.7(4) . . ?
O26 C16 C11 114.4(4) . . ?
C15 C16 C11 119.8(4) . . ?
O26 C17 C18 107.3(3) . . ?
O27 C18 C17 110.7(3) . . ?
O27 C19 C20 110.2(3) . . ?
O28 C20 C19 107.6(3) . . ?
C26 C21 C22 121.8(4) . . ?
C26 C21 N1 118.8(3) . . ?
C22 C21 N1 119.4(3) . . ?
C21 C22 C23 118.7(4) . . ?
C22 C23 C24 120.2(4) . . ?
C22 C23 I1 121.0(3) . . ?
C24 C23 I1 118.7(3) . . ?
C25 C24 C23 119.7(4) . . ?
C24 C25 C26 121.0(4) . . ?
C21 C26 C25 118.5(4) . . ?
N2 C28 C27 177.9(6) . . ?
N3 C30 C29 178.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.862
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.169
