# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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/access/V1 
# 
# Audit and citation data items may have 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_100k
_database_code_depnum_ccdc_archive 'CCDC 1037985'
_audit_update_record             
;
2014-12-08 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(TT-TTF)3(PMo12O40)
;
_chemical_name_common            (TT-TTF)3(PMo12O40)
_chemical_melting_point          '423, decomposed'
_chemical_formula_moiety         'C67 H36 Cl2 Mo12 O40 P S36'
_chemical_formula_sum            'C67 H36 Cl2 Mo12 O40 P S36'
_chemical_formula_weight         3888.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   23.7742(3)
_cell_length_b                   23.7742(3)
_cell_length_c                   13.7571(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6733.94(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    14432
_cell_measurement_theta_min      3.4150
_cell_measurement_theta_max      28.4620

_exptl_crystal_description       'hexagonal block'
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3774
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_T_max  0.7790
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
The black hexagonal single crystals were obtained by diffusion method.
In a typical procedure, In a typical condition, a dichloromethane 
solution (5 mL) of TT-TTF (6 mg, 0.010 mmol) was placed at the bottom layer 
of a glass tube, freshly distilled acetonitrile (CH3CN, 5 mL) 
was added dropwisely into the tube as the middle layer, and the solution 
of phosphomolybdic acid (PMA, 30mg, 0.016 mmol) in CH3CN (2 mL) was slowly 
charged into the tube as the upper layer. The tube was then placed in the 
dark hood and kept quietly. After around one week, the black hexagonal single 
crystals (see Figure S7) of (TT-TTF)3[PMo12O40](CH2Cl2) 
were obtained (2.4 mg, yield: 11%). It should be noted that in this 
synthesis, the microcrystals were simultaneously formed to show the 
hexagonal shapes, similar to those obtained in the mixed solution 
of TT-TTF : PMA = 1 : 1 in CH2Cl2-CH3CN (v/v, 7 : 3).The bulk crystals 
were dried in vacuo at 60 oC for 6 hours before the X-ray single crystal
diffraction measurement, that is to remove the solvent molecules in the 
nano-channel formed by thienyl groups
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27533
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         28.66
_reflns_number_total             10406
_reflns_number_gt                8903
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    SIR2004
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Mercury
_computing_publication_material  Mercury

_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.
 The thienyl groups in this complex show the orientational disorder, which
 cannot be suppressed even at lower temperature. Thus, the disorder is caused
 by statistic reason rather than the rotational one. It should be noted that 
 the rotational disorder of thienyl groups have also been observed in the 
 crystal structure of neutral TT-TTF (J. Sun, et al., Chem. Eur. J. 
 2013, 19, 12517), and those of the inclusion complex [(TT-TTF)-C60] 
 (which will be published in due course).
;

_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)+(0.0150P)²+5.4269P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10406
_refine_ls_number_parameters     516
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0569
_refine_ls_wR_factor_gt          0.0527
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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
C1 C 0.87527(13) 0.49704(13) 0.55008(19) 0.0149(5) Uani 1 1 d . . .
C2 C 0.90647(12) 0.46141(13) 0.53802(18) 0.0144(5) Uani 1 1 d . . .
C3 C 0.81734(13) 0.56136(14) 0.5179(2) 0.0188(6) Uani 1 1 d . . .
C4 C 0.83863(12) 0.57568(13) 0.6107(2) 0.0161(6) Uani 1 1 d . . .
C5 C 0.94775(12) 0.38934(12) 0.46846(18) 0.0135(5) Uani 1 1 d . . .
C6 C 0.96507(12) 0.39750(13) 0.56406(18) 0.0138(5) Uani 1 1 d . . .
C7 C 0.83424(16) 0.64893(17) 0.3812(3) 0.0365(8) Uani 1 1 d . . .
C8 C 0.90309(14) 0.67573(14) 0.7376(2) 0.0227(6) Uani 1 1 d . . .
C9 C 0.93867(13) 0.35838(13) 0.27874(18) 0.0137(5) Uani 1 1 d . . .
C10 C 1.00238(13) 0.37516(13) 0.74004(19) 0.0166(6) Uani 1 1 d . . .
C11 C 0.85184(17) 0.6401(2) 0.2909(3) 0.0433(10) Uani 1 1 d . . .
H11 H 0.8314 0.6005 0.2585 0.052 Uiso 1 1 calc R . .
C12 C 0.9041(2) 0.6969(3) 0.2514(4) 0.0654(15) Uani 1 1 d . . .
H12 H 0.9222 0.6993 0.1905 0.078 Uiso 1 1 calc R . .
C13 C 0.9244(2) 0.7471(3) 0.3128(4) 0.0824(18) Uani 1 1 d . . .
H13 H 0.9584 0.7886 0.2989 0.099 Uiso 1 1 calc R . .
C14 C 0.92655(14) 0.66714(15) 0.8274(3) 0.0317(8) Uani 1 1 d . . .
H14 H 0.9034 0.6331 0.8706 0.038 Uiso 1 1 calc R . .
C15 C 0.99086(17) 0.71842(17) 0.8413(3) 0.0400(9) Uani 1 1 d . . .
H15 H 1.0155 0.7209 0.8954 0.048 Uiso 1 1 calc R . .
C16 C 1.01385(17) 0.76347(17) 0.7704(3) 0.0428(9) Uani 1 1 d . . .
H16 H 1.0551 0.8000 0.7709 0.051 Uiso 1 1 calc R . .
C18 C 0.93548(13) 0.40614(14) 0.1287(2) 0.0187(6) Uani 1 1 d . . .
H18 H 0.9499 0.4347 0.0763 0.022 Uiso 1 1 calc R A 1
C19 C 0.87548(14) 0.35442(14) 0.1420(2) 0.0211(6) Uani 1 1 d . E .
H19 H 0.8429 0.3446 0.0966 0.025 Uiso 1 1 calc R B 1
C21 C 0.96685(14) 0.35511(14) 0.9048(2) 0.0223(6) Uani 1 1 d . . .
H21 H 0.9443 0.3383 0.9626 0.027 Uiso 1 1 calc R C 1
C22 C 1.02467(15) 0.41131(15) 0.9032(2) 0.0258(7) Uani 1 1 d . F .
H22 H 1.0460 0.4373 0.9566 0.031 Uiso 1 1 calc R D 1
S1 S 0.83186(3) 0.50601(4) 0.45674(5) 0.02012(15) Uani 1 1 d . . .
S2 S 0.87565(3) 0.53439(3) 0.65731(5) 0.01436(13) Uani 1 1 d . . .
S3 S 0.90777(3) 0.42846(3) 0.42676(5) 0.01458(13) Uani 1 1 d . . .
S4 S 0.94466(3) 0.44569(3) 0.63259(5) 0.01464(13) Uani 1 1 d . . .
S5 S 0.77297(4) 0.59186(4) 0.45749(6) 0.02684(17) Uani 1 1 d . . .
S6 S 0.82529(4) 0.62673(4) 0.68783(5) 0.02137(15) Uani 1 1 d . . .
S7 S 0.96540(3) 0.34275(3) 0.38887(5) 0.01479(13) Uani 1 1 d . E .
S8 S 1.01030(4) 0.36526(4) 0.61551(5) 0.02458(17) Uani 1 1 d . F .
S9 S 0.88183(6) 0.72743(5) 0.41879(10) 0.0696(4) Uani 1 1 d . . .
S10 S 0.95863(4) 0.74607(4) 0.67916(7) 0.0409(2) Uani 1 1 d . . .
C17A C 0.9726(5) 0.4078(6) 0.2129(10) 0.026(3) Uani 0.536(4) 1 d P E 1
H17A H 1.0157 0.4395 0.2220 0.031 Uiso 0.536(4) 1 calc PR E 1
S11A S 0.86079(17) 0.30917(17) 0.2389(3) 0.0178(6) Uani 0.536(4) 1 d P E 1
C20A C 1.0476(9) 0.4238(8) 0.8017(16) 0.026(4) Uani 0.534(4) 1 d P F 1
H20A H 1.0867 0.4591 0.7814 0.031 Uiso 0.534(4) 1 calc PR F 1
S12A S 0.93739(16) 0.31669(16) 0.7974(2) 0.0181(6) Uani 0.534(4) 1 d P F 1
C17B C 0.8779(7) 0.3267(7) 0.2347(13) 0.024(4) Uani 0.464(4) 1 d P E 2
H17B H 0.8421 0.2910 0.2622 0.029 Uiso 0.464(4) 1 calc PR E 2
S11B S 0.99286(17) 0.4211(2) 0.2081(3) 0.0155(7) Uani 0.464(4) 1 d P E 2
C20B C 0.9540(6) 0.3338(6) 0.8072(11) 0.021(3) Uani 0.466(4) 1 d P F 2
H20B H 0.9169 0.2957 0.7886 0.025 Uiso 0.466(4) 1 calc PR F 2
S12B S 1.0613(3) 0.4396(3) 0.7997(5) 0.0222(9) Uani 0.466(4) 1 d P F 2
Mo1 Mo 0.745953(10) 0.326092(10) 0.687752(15) 0.00975(5) Uani 1 1 d . . .
Mo2 Mo 0.759388(11) 0.420889(11) 1.112038(16) 0.01155(5) Uani 1 1 d . . .
Mo3 Mo 0.837281(10) 0.431827(10) 0.896207(16) 0.01032(5) Uani 1 1 d . . .
Mo4 Mo 0.758779(10) 0.252928(10) 0.920827(16) 0.01087(5) Uani 1 1 d . . .
O1 O 0.6667 0.3333 0.7917(2) 0.0109(6) Uani 1 3 d S . .
O2 O 0.60472(8) 0.33086(8) 0.94053(12) 0.0103(4) Uani 1 1 d . . .
O3 O 0.80755(8) 0.40009(8) 0.77503(12) 0.0121(4) Uani 1 1 d . . .
O4 O 0.74930(8) 0.27434(8) 0.78185(12) 0.0123(4) Uani 1 1 d . . .
O5 O 0.83279(8) 0.44174(8) 1.04180(12) 0.0136(4) Uani 1 1 d . . .
O6 O 0.73618(8) 0.23685(8) 1.04963(12) 0.0138(4) Uani 1 1 d . . .
O7 O 0.66584(8) 0.26863(8) 0.63662(12) 0.0119(4) Uani 1 1 d . . .
O8 O 0.72996(8) 0.33403(8) 1.12557(13) 0.0144(4) Uani 1 1 d . . .
O9 O 0.81044(8) 0.34152(8) 0.93309(12) 0.0131(4) Uani 1 1 d . . .
O10 O 0.82772(8) 0.50501(8) 0.88788(12) 0.0132(4) Uani 1 1 d . . .
O11 O 0.79742(8) 0.32730(8) 0.60292(13) 0.0154(4) Uani 1 1 d . . .
O12 O 0.78872(9) 0.45226(9) 1.22212(13) 0.0178(4) Uani 1 1 d . . .
O13 O 0.91824(8) 0.46455(9) 0.88699(13) 0.0168(4) Uani 1 1 d . . .
O14 O 0.81273(8) 0.22749(9) 0.90980(13) 0.0152(4) Uani 1 1 d . . .
P P 0.6667 0.3333 0.90321(8) 0.0085(2) Uani 1 3 d S . .
C01 C 0.6667 0.3333 0.3951(4) 0.0407(15) Uani 1 3 d S . .
Cl Cl 0.73790(6) 0.33395(6) 0.38660(9) 0.0311(3) Uani 0.67 1 d P . .


_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
C1 C2 1.387(4) . ?
C1 S2 1.719(3) . ?
C1 S1 1.726(3) . ?
C2 S3 1.727(3) . ?
C2 S4 1.731(3) . ?
C3 C4 1.352(4) . ?
C3 S1 1.736(3) . ?
C3 S5 1.759(3) . ?
C4 S2 1.736(3) . ?
C4 S6 1.756(3) . ?
C5 C6 1.363(3) . ?
C5 S3 1.727(3) . ?
C5 S7 1.751(3) . ?
C6 S4 1.730(3) . ?
C6 S8 1.752(3) . ?
C7 C11 1.360(5) . ?
C7 S9 1.708(4) . ?
C7 S5 1.757(4) . ?
C8 C14 1.411(4) . ?
C8 S10 1.726(3) . ?
C8 S6 1.759(3) . ?
C9 C17A 1.379(13) . ?
C9 C17B 1.390(16) . ?
C9 S11B 1.704(4) . ?
C9 S11A 1.712(4) . ?
C9 S7 1.753(3) . ?
C10 C20A 1.404(19) . ?
C10 C20B 1.419(15) . ?
C10 S12A 1.671(4) . ?
C10 S12B 1.685(7) . ?
C10 S8 1.752(3) . ?
C11 C12 1.410(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.340(7) . ?
C12 H12 0.9300 . ?
C13 S9 1.702(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.413(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.347(5) . ?
C15 H15 0.9300 . ?
C16 S10 1.711(4) . ?
C16 H16 0.9300 . ?
C18 C19 1.351(4) . ?
C18 C17A 1.444(14) . ?
C18 S11B 1.642(4) . ?
C18 H18 0.9300 . ?
C19 C17B 1.450(18) . ?
C19 S11A 1.637(5) . ?
C19 H19 0.9300 . ?
C21 C22 1.356(4) . ?
C21 C20B 1.414(14) . ?
C21 S12A 1.694(4) . ?
C21 H21 0.9300 . ?
C22 C20A 1.47(2) . ?
C22 S12B 1.630(7) . ?
C22 H22 0.9300 . ?
C17A H17A 0.9300 . ?
C20A H20A 0.9300 . ?
C17B H17B 0.9300 . ?
C20B H20B 0.9300 . ?
Mo1 O11 1.6808(17) . ?
Mo1 O4 1.8148(17) . ?
Mo1 O7 1.8403(17) . ?
Mo1 O7 2.0149(17) 2_655 ?
Mo1 O3 2.0260(17) . ?
Mo1 O1 2.4394(17) . ?
Mo2 O12 1.6781(18) . ?
Mo2 O8 1.8286(18) . ?
Mo2 O5 1.8330(18) . ?
Mo2 O8 2.0004(17) 2_655 ?
Mo2 O6 2.0139(17) 2_655 ?
Mo2 O2 2.4660(16) 3_665 ?
Mo3 O13 1.6819(17) . ?
Mo3 O3 1.8206(17) . ?
Mo3 O10 1.8676(17) . ?
Mo3 O9 1.9759(17) . ?
Mo3 O5 2.0257(17) . ?
Mo3 O2 2.4108(17) 3_665 ?
Mo4 O14 1.6762(17) . ?
Mo4 O6 1.8355(17) . ?
Mo4 O9 1.8402(17) . ?
Mo4 O10 1.9799(17) 3_665 ?
Mo4 O4 2.0200(17) . ?
Mo4 O2 2.4338(16) 2_655 ?
O1 P 1.534(3) . ?
O1 Mo1 2.4394(17) 3_665 ?
O1 Mo1 2.4394(17) 2_655 ?
O2 P 1.5329(17) . ?
O2 Mo3 2.4108(17) 2_655 ?
O2 Mo4 2.4338(16) 3_665 ?
O2 Mo2 2.4660(16) 2_655 ?
O6 Mo2 2.0139(17) 3_665 ?
O7 Mo1 2.0149(17) 3_665 ?
O8 Mo2 2.0004(17) 3_665 ?
O10 Mo4 1.9799(17) 2_655 ?
P O2 1.5329(17) 2_655 ?
P O2 1.5329(17) 3_665 ?
C01 Cl 1.6903(13) . ?
C01 Cl 1.6903(13) 3_665 ?
C01 Cl 1.6903(13) 2_655 ?

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
C2 C1 S2 123.5(2) . . ?
C2 C1 S1 121.5(2) . . ?
S2 C1 S1 115.07(15) . . ?
C1 C2 S3 121.3(2) . . ?
C1 C2 S4 122.7(2) . . ?
S3 C2 S4 115.98(15) . . ?
C4 C3 S1 117.2(2) . . ?
C4 C3 S5 124.6(2) . . ?
S1 C3 S5 118.10(16) . . ?
C3 C4 S2 116.0(2) . . ?
C3 C4 S6 124.8(2) . . ?
S2 C4 S6 119.02(16) . . ?
C6 C5 S3 116.9(2) . . ?
C6 C5 S7 122.8(2) . . ?
S3 C5 S7 120.23(15) . . ?
C5 C6 S4 117.1(2) . . ?
C5 C6 S8 122.4(2) . . ?
S4 C6 S8 120.42(15) . . ?
C11 C7 S9 111.0(3) . . ?
C11 C7 S5 128.8(3) . . ?
S9 C7 S5 120.2(2) . . ?
C14 C8 S10 112.5(2) . . ?
C14 C8 S6 127.3(2) . . ?
S10 C8 S6 120.11(18) . . ?
C17A C9 C17B 100.4(8) . . ?
C17A C9 S11B 10.5(6) . . ?
C17B C9 S11B 110.6(7) . . ?
C17A C9 S11A 110.1(5) . . ?
C17B C9 S11A 9.8(7) . . ?
S11B C9 S11A 120.1(2) . . ?
C17A C9 S7 129.0(5) . . ?
C17B C9 S7 130.6(7) . . ?
S11B C9 S7 118.84(19) . . ?
S11A C9 S7 120.98(18) . . ?
C20A C10 C20B 101.5(10) . . ?
C20A C10 S12A 114.1(9) . . ?
C20B C10 S12A 12.6(5) . . ?
C20A C10 S12B 8.1(10) . . ?
C20B C10 S12B 109.3(5) . . ?
S12A C10 S12B 122.0(3) . . ?
C20A C10 S8 127.8(9) . . ?
C20B C10 S8 130.4(5) . . ?
S12A C10 S8 117.80(19) . . ?
S12B C10 S8 120.1(3) . . ?
C7 C11 C12 113.4(4) . . ?
C7 C11 H11 123.3 . . ?
C12 C11 H11 123.3 . . ?
C13 C12 C11 111.2(5) . . ?
C13 C12 H12 124.4 . . ?
C11 C12 H12 124.4 . . ?
C12 C13 S9 113.3(4) . . ?
C12 C13 H13 123.4 . . ?
S9 C13 H13 123.4 . . ?
C8 C14 C15 109.2(3) . . ?
C8 C14 H14 125.4 . . ?
C15 C14 H14 125.4 . . ?
C16 C15 C14 114.9(4) . . ?
C16 C15 H15 122.5 . . ?
C14 C15 H15 122.5 . . ?
C15 C16 S10 112.5(3) . . ?
C15 C16 H16 123.8 . . ?
S10 C16 H16 123.8 . . ?
C19 C18 C17A 105.6(5) . . ?
C19 C18 S11B 119.5(3) . . ?
C17A C18 S11B 14.2(5) . . ?
C19 C18 H18 127.2 . . ?
C17A C18 H18 127.2 . . ?
S11B C18 H18 113.3 . . ?
C18 C19 C17B 105.6(6) . . ?
C18 C19 S11A 119.3(3) . . ?
C17B C19 S11A 13.9(6) . . ?
C18 C19 H19 120.4 . . ?
C17B C19 H19 134.0 . . ?
S11A C19 H19 120.4 . . ?
C22 C21 C20B 105.6(6) . . ?
C22 C21 S12A 117.4(3) . . ?
C20B C21 S12A 11.7(6) . . ?
C22 C21 H21 121.3 . . ?
C20B C21 H21 133.1 . . ?
S12A C21 H21 121.3 . . ?
C21 C22 C20A 107.7(7) . . ?
C21 C22 S12B 119.3(3) . . ?
C20A C22 S12B 11.8(8) . . ?
C21 C22 H22 126.2 . . ?
C20A C22 H22 126.2 . . ?
S12B C22 H22 114.5 . . ?
C1 S1 C3 95.21(13) . . ?
C1 S2 C4 95.83(13) . . ?
C5 S3 C2 95.13(13) . . ?
C6 S4 C2 94.85(13) . . ?
C7 S5 C3 99.45(14) . . ?
C4 S6 C8 101.52(13) . . ?
C5 S7 C9 100.34(12) . . ?
C6 S8 C10 101.86(12) . . ?
C13 S9 C7 91.1(3) . . ?
C16 S10 C8 90.87(17) . . ?
C9 C17A C18 114.5(7) . . ?
C9 C17A H17A 122.7 . . ?
C18 C17A H17A 122.7 . . ?
C19 S11A C9 90.5(2) . . ?
C10 C20A C22 110.7(11) . . ?
C10 C20A H20A 124.7 . . ?
C22 C20A H20A 124.7 . . ?
C10 S12A C21 90.13(19) . . ?
C9 C17B C19 113.8(8) . . ?
C9 C17B H17B 123.1 . . ?
C19 C17B H17B 123.1 . . ?
C18 S11B C9 90.4(2) . . ?
C21 C20B C10 114.5(7) . . ?
C21 C20B H20B 122.7 . . ?
C10 C20B H20B 122.7 . . ?
C22 S12B C10 91.2(3) . . ?
O11 Mo1 O4 103.21(8) . . ?
O11 Mo1 O7 102.81(8) . . ?
O4 Mo1 O7 98.59(8) . . ?
O11 Mo1 O7 99.93(8) . 2_655 ?
O4 Mo1 O7 154.44(7) . 2_655 ?
O7 Mo1 O7 86.61(10) . 2_655 ?
O11 Mo1 O3 101.11(8) . . ?
O4 Mo1 O3 84.74(7) . . ?
O7 Mo1 O3 154.36(7) . . ?
O7 Mo1 O3 80.28(7) 2_655 . ?
O11 Mo1 O1 170.87(8) . . ?
O4 Mo1 O1 85.82(7) . . ?
O7 Mo1 O1 74.16(6) . . ?
O7 Mo1 O1 71.47(6) 2_655 . ?
O3 Mo1 O1 80.79(6) . . ?
O12 Mo2 O8 104.44(8) . . ?
O12 Mo2 O5 103.17(8) . . ?
O8 Mo2 O5 97.70(8) . . ?
O12 Mo2 O8 101.58(8) . 2_655 ?
O8 Mo2 O8 85.09(10) . 2_655 ?
O5 Mo2 O8 153.51(7) . 2_655 ?
O12 Mo2 O6 99.03(8) . 2_655 ?
O8 Mo2 O6 154.67(7) . 2_655 ?
O5 Mo2 O6 85.95(7) . 2_655 ?
O8 Mo2 O6 80.97(7) 2_655 2_655 ?
O12 Mo2 O2 169.70(8) . 3_665 ?
O8 Mo2 O2 85.65(7) . 3_665 ?
O5 Mo2 O2 72.94(7) . 3_665 ?
O8 Mo2 O2 81.06(6) 2_655 3_665 ?
O6 Mo2 O2 71.40(6) 2_655 3_665 ?
O13 Mo3 O3 103.89(8) . . ?
O13 Mo3 O10 102.04(8) . . ?
O3 Mo3 O10 97.30(8) . . ?
O13 Mo3 O9 101.25(8) . . ?
O3 Mo3 O9 86.40(7) . . ?
O10 Mo3 O9 154.75(7) . . ?
O13 Mo3 O5 97.78(8) . . ?
O3 Mo3 O5 157.13(7) . . ?
O10 Mo3 O5 85.08(7) . . ?
O9 Mo3 O5 82.26(7) . . ?
O13 Mo3 O2 168.61(8) . 3_665 ?
O3 Mo3 O2 87.35(7) . 3_665 ?
O10 Mo3 O2 74.29(7) . 3_665 ?
O9 Mo3 O2 80.97(6) . 3_665 ?
O5 Mo3 O2 71.33(6) . 3_665 ?
O14 Mo4 O6 102.09(8) . . ?
O14 Mo4 O9 103.19(8) . . ?
O6 Mo4 O9 96.21(8) . . ?
O14 Mo4 O10 100.64(8) . 3_665 ?
O6 Mo4 O10 88.65(8) . 3_665 ?
O9 Mo4 O10 154.06(7) . 3_665 ?
O14 Mo4 O4 101.96(8) . . ?
O6 Mo4 O4 155.27(7) . . ?
O9 Mo4 O4 83.86(7) . . ?
O10 Mo4 O4 81.31(7) 3_665 . ?
O14 Mo4 O2 171.93(7) . 2_655 ?
O6 Mo4 O2 74.93(7) . 2_655 ?
O9 Mo4 O2 84.68(7) . 2_655 ?
O10 Mo4 O2 71.98(6) 3_665 2_655 ?
O4 Mo4 O2 80.47(6) . 2_655 ?
P O1 Mo1 125.87(5) . . ?
P O1 Mo1 125.87(5) . 3_665 ?
Mo1 O1 Mo1 89.13(8) . 3_665 ?
P O1 Mo1 125.87(5) . 2_655 ?
Mo1 O1 Mo1 89.13(8) . 2_655 ?
Mo1 O1 Mo1 89.13(8) 3_665 2_655 ?
P O2 Mo3 125.44(9) . 2_655 ?
P O2 Mo4 126.34(9) . 3_665 ?
Mo3 O2 Mo4 89.27(6) 2_655 3_665 ?
P O2 Mo2 125.84(10) . 2_655 ?
Mo3 O2 Mo2 89.70(5) 2_655 2_655 ?
Mo4 O2 Mo2 88.44(5) 3_665 2_655 ?
Mo3 O3 Mo1 149.86(10) . . ?
Mo1 O4 Mo4 153.41(10) . . ?
Mo2 O5 Mo3 126.03(9) . . ?
Mo4 O6 Mo2 125.11(9) . 3_665 ?
Mo1 O7 Mo1 125.20(9) . 3_665 ?
Mo2 O8 Mo2 152.11(10) . 3_665 ?
Mo4 O9 Mo3 152.66(10) . . ?
Mo3 O10 Mo4 124.40(9) . 2_655 ?
O2 P O2 109.37(7) 2_655 3_665 ?
O2 P O2 109.37(7) 2_655 . ?
O2 P O2 109.37(7) 3_665 . ?
O2 P O1 109.57(7) 2_655 . ?
O2 P O1 109.57(7) 3_665 . ?
O2 P O1 109.57(7) . . ?
Cl C01 Cl 119.53(5) . 3_665 ?
Cl C01 Cl 119.53(5) . 2_655 ?
Cl C01 Cl 119.53(5) 3_665 2_655 ?

_diffrn_measured_fraction_theta_max 0.900
_diffrn_reflns_theta_full        26.3154
_diffrn_measured_fraction_theta_full 0.9984
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.102
_exptl_crystal_recrystallization_method 
'The crystals were obtained by slow diffusion of two components through a three-layer technique'
_chemical_properties_physical    Heat-sensitive
_exptl_crystal_preparation       'Magnetic properties'
