# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 990544'
_audit_update_record             
;
2014-03-07 deposited with the CCDC.
2015-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[V2(PS3)2(mu-Se2)(mu-Se)][PPh4]2'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C91 H72 N3 O0.25 P4 S6 Se3 V2'
_chemical_formula_weight         1866.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2/c

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

_cell_length_a                   23.551(19)
_cell_length_b                   13.683(11)
_cell_length_c                   27.38(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.212(14)
_cell_angle_gamma                90.00
_cell_volume                     8710(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8083
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.40

_exptl_crystal_description       column
_exptl_crystal_colour            reddish-purple
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3780
_exptl_absorpt_coefficient_mu    1.732
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.4179
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            61983
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.1019
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         0.88
_diffrn_reflns_theta_max         28.49
_reflns_number_total             21294
_reflns_number_gt                11361
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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)+(0.0712P)²+12.4001P] 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         21294
_refine_ls_number_parameters     996
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1840
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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
Se1 Se 0.28614(3) 0.70568(4) 0.25292(2) 0.03752(15) Uani 1 1 d . . .
Se2 Se 0.23176(3) 0.88292(4) 0.15065(2) 0.04123(16) Uani 1 1 d . . .
Se3 Se 0.32864(3) 0.86616(4) 0.14877(2) 0.04281(16) Uani 1 1 d . . .
V1 V 0.29820(4) 0.87439(6) 0.23407(3) 0.0315(2) Uani 1 1 d . . .
V2 V 0.27203(4) 0.71329(7) 0.16481(3) 0.0334(2) Uani 1 1 d . . .
S1 S 0.30732(7) 1.05353(10) 0.22922(5) 0.0402(3) Uani 1 1 d . . .
P3 P 0.50984(6) 1.31912(11) 0.08240(5) 0.0357(3) Uani 1 1 d . . .
P2 P 0.25474(6) 0.54300(10) 0.16553(5) 0.0328(3) Uani 1 1 d . . .
P1 P 0.31385(6) 0.91084(10) 0.32060(5) 0.0328(3) Uani 1 1 d . . .
S2 S 0.20083(6) 0.89931(11) 0.25973(6) 0.0425(4) Uani 1 1 d . . .
S3 S 0.40328(6) 0.85726(12) 0.25509(6) 0.0418(4) Uani 1 1 d . . .
S5 S 0.16457(6) 0.68717(11) 0.16387(6) 0.0421(4) Uani 1 1 d . . .
S4 S 0.24711(7) 0.68890(11) 0.07492(5) 0.0437(4) Uani 1 1 d . . .
S6 S 0.36974(7) 0.64660(12) 0.16464(7) 0.0491(4) Uani 1 1 d . . .
P4 P -0.00896(7) 1.25085(12) 0.09728(6) 0.0440(4) Uani 1 1 d . . .
C21 C 0.2594(3) 0.8573(4) 0.35271(19) 0.0380(13) Uani 1 1 d . . .
C16 C 0.3003(2) 1.1012(4) 0.2878(2) 0.0360(13) Uani 1 1 d . . .
C11 C 0.3037(2) 1.0421(4) 0.3294(2) 0.0367(13) Uani 1 1 d . . .
C41 C 0.2220(2) 0.5021(4) 0.1033(2) 0.0345(12) Uani 1 1 d . . .
C61 C 0.3198(2) 0.4700(4) 0.1821(2) 0.0384(13) Uani 1 1 d . . .
C94 C 0.4407(2) 1.3485(4) 0.0443(2) 0.0370(13) Uani 1 1 d . . .
C51 C 0.2010(2) 0.5111(4) 0.20393(18) 0.0322(12) Uani 1 1 d . . .
C93 C 0.5607(2) 1.2783(4) 0.0439(2) 0.0387(13) Uani 1 1 d . . .
C46 C 0.2209(2) 0.5703(4) 0.06446(19) 0.0357(13) Uani 1 1 d . . .
C36 C 0.4247(2) 0.8606(4) 0.3199(2) 0.0379(13) Uani 1 1 d . . .
C33 C 0.4654(3) 0.8828(5) 0.4209(3) 0.062(2) Uani 1 1 d . . .
H33A H 0.4792 0.8918 0.4547 0.075 Uiso 1 1 calc R . .
C31 C 0.3872(2) 0.8846(4) 0.3522(2) 0.0373(13) Uani 1 1 d . . .
C66 C 0.3711(2) 0.5242(4) 0.1835(2) 0.0397(14) Uani 1 1 d . . .
C108 C 0.0586(2) 1.1973(4) 0.1261(2) 0.0428(14) Uani 1 1 d . . .
C26 C 0.2056(3) 0.8563(4) 0.3214(2) 0.0442(14) Uani 1 1 d . . .
C92 C 0.4990(2) 1.2219(4) 0.1233(2) 0.0383(13) Uani 1 1 d . . .
C107 C -0.0620(3) 1.2012(5) 0.1309(3) 0.0512(16) Uani 1 1 d . . .
C91 C 0.5694(3) 1.1801(5) 0.0370(2) 0.0441(14) Uani 1 1 d . . .
H91A H 0.5506 1.1337 0.0540 0.053 Uiso 1 1 calc R . .
C12 C 0.2987(3) 1.0821(5) 0.3761(2) 0.0490(16) Uani 1 1 d . . .
H12A H 0.3014 1.0415 0.4041 0.059 Uiso 1 1 calc R . .
C62 C 0.3229(3) 0.3695(5) 0.1913(2) 0.0491(16) Uani 1 1 d . . .
H62A H 0.2887 0.3330 0.1888 0.059 Uiso 1 1 calc R . .
C56 C 0.1574(2) 0.5822(4) 0.1988(2) 0.0405(14) Uani 1 1 d . . .
C90 C 0.3963(3) 1.3864(5) 0.0666(2) 0.0491(16) Uani 1 1 d . . .
H90A H 0.4019 1.3965 0.1009 0.059 Uiso 1 1 calc R . .
C42 C 0.2010(3) 0.4082(5) 0.0937(2) 0.0456(15) Uani 1 1 d . . .
H42A H 0.2022 0.3638 0.1200 0.055 Uiso 1 1 calc R . .
C32 C 0.4075(3) 0.8973(5) 0.4028(2) 0.0533(17) Uani 1 1 d . . .
H32A H 0.3820 0.9156 0.4244 0.064 Uiso 1 1 calc R . .
C45 C 0.1981(3) 0.5382(5) 0.0165(2) 0.0486(15) Uani 1 1 d . . .
H45A H 0.1971 0.5816 -0.0102 0.058 Uiso 1 1 calc R . .
C89 C 0.5388(2) 1.4268(4) 0.1158(2) 0.0389(13) Uani 1 1 d . . .
C15 C 0.2915(3) 1.2018(4) 0.2931(2) 0.0460(15) Uani 1 1 d . . .
H15A H 0.2898 1.2431 0.2655 0.055 Uiso 1 1 calc R . .
C43 C 0.1782(3) 0.3782(5) 0.0457(2) 0.0553(17) Uani 1 1 d . . .
H43A H 0.1640 0.3144 0.0395 0.066 Uiso 1 1 calc R . .
C22 C 0.2642(3) 0.8261(5) 0.4014(2) 0.0499(16) Uani 1 1 d . . .
H22A H 0.3002 0.8260 0.4220 0.060 Uiso 1 1 calc R . .
C14 C 0.2855(3) 1.2409(5) 0.3385(3) 0.0558(17) Uani 1 1 d . . .
H14A H 0.2786 1.3082 0.3412 0.067 Uiso 1 1 calc R . .
C35 C 0.4834(3) 0.8432(4) 0.3396(3) 0.0519(17) Uani 1 1 d . . .
H35A H 0.5091 0.8235 0.3185 0.062 Uiso 1 1 calc R . .
C88 C 0.6077(4) 1.5038(6) 0.1789(3) 0.088(3) Uani 1 1 d . . .
H88A H 0.6405 1.4991 0.2033 0.105 Uiso 1 1 calc R . .
C52 C 0.1983(3) 0.4314(5) 0.2353(2) 0.0489(16) Uani 1 1 d . . .
H52A H 0.2289 0.3864 0.2402 0.059 Uiso 1 1 calc R . .
C13 C 0.2896(3) 1.1822(5) 0.3804(3) 0.0575(18) Uani 1 1 d . . .
H13A H 0.2863 1.2097 0.4113 0.069 Uiso 1 1 calc R . .
C87 C 0.4827(3) 1.0664(5) 0.1860(3) 0.0555(17) Uani 1 1 d . . .
H87A H 0.4769 1.0150 0.2074 0.067 Uiso 1 1 calc R . .
C63 C 0.3755(3) 0.3224(5) 0.2042(3) 0.0606(19) Uani 1 1 d . . .
H63A H 0.3769 0.2548 0.2103 0.073 Uiso 1 1 calc R . .
C64 C 0.4251(3) 0.3760(5) 0.2079(2) 0.0585(19) Uani 1 1 d . . .
H64A H 0.4607 0.3445 0.2173 0.070 Uiso 1 1 calc R . .
C25 C 0.1563(3) 0.8248(6) 0.3400(3) 0.068(2) Uani 1 1 d . . .
H25A H 0.1201 0.8237 0.3197 0.082 Uiso 1 1 calc R . .
C86 C 0.6059(3) 1.1492(5) 0.0050(2) 0.0514(17) Uani 1 1 d . . .
H86A H 0.6112 1.0821 0.0000 0.062 Uiso 1 1 calc R . .
C106 C -0.0242(3) 1.2168(5) 0.0332(3) 0.0509(16) Uani 1 1 d . . .
C85 C 0.4461(3) 1.1765(5) 0.1207(3) 0.063(2) Uani 1 1 d . . .
H85A H 0.4148 1.1981 0.0975 0.075 Uiso 1 1 calc R . .
C34 C 0.5029(3) 0.8551(5) 0.3895(3) 0.062(2) Uani 1 1 d . . .
H34A H 0.5419 0.8443 0.4021 0.074 Uiso 1 1 calc R . .
C65 C 0.4243(3) 0.4752(5) 0.1983(2) 0.0517(17) Uani 1 1 d . . .
H65A H 0.4590 0.5103 0.2014 0.062 Uiso 1 1 calc R . .
C105 C -0.0063(3) 1.3815(5) 0.1008(3) 0.0522(17) Uani 1 1 d . . .
C84 C 0.5358(4) 1.1086(6) 0.1891(3) 0.073(2) Uani 1 1 d . . .
H84A H 0.5666 1.0852 0.2122 0.087 Uiso 1 1 calc R . .
C104 C 0.0352(3) 1.4309(6) 0.0796(3) 0.076(2) Uani 1 1 d . . .
H10A H 0.0613 1.3955 0.0639 0.091 Uiso 1 1 calc R . .
C83 C 0.3358(3) 1.3934(6) -0.0123(3) 0.066(2) Uani 1 1 d . . .
H83A H 0.3000 1.4080 -0.0315 0.080 Uiso 1 1 calc R . .
C103 C 0.0616(3) 1.0976(5) 0.1286(3) 0.079(3) Uani 1 1 d . . .
H10B H 0.0301 1.0602 0.1137 0.095 Uiso 1 1 calc R . .
C82 C 0.6343(3) 1.2173(6) -0.0196(2) 0.0597(19) Uani 1 1 d . . .
H82A H 0.6595 1.1967 -0.0409 0.072 Uiso 1 1 calc R . .
C102 C 0.1040(3) 1.2528(5) 0.1500(2) 0.0517(16) Uani 1 1 d . . .
H10C H 0.1020 1.3214 0.1501 0.062 Uiso 1 1 calc R . .
C23 C 0.2154(4) 0.7950(6) 0.4198(3) 0.073(2) Uani 1 1 d . . .
H23A H 0.2183 0.7738 0.4528 0.088 Uiso 1 1 calc R . .
C101 C 0.1103(3) 1.0507(5) 0.1528(3) 0.080(3) Uani 1 1 d . . .
H10D H 0.1120 0.9821 0.1537 0.096 Uiso 1 1 calc R . .
C55 C 0.1098(3) 0.5657(6) 0.2226(3) 0.0609(19) Uani 1 1 d . . .
H55A H 0.0795 0.6112 0.2190 0.073 Uiso 1 1 calc R . .
C100 C 0.1535(3) 1.2037(5) 0.1742(2) 0.0538(17) Uani 1 1 d . . .
H10E H 0.1851 1.2404 0.1896 0.065 Uiso 1 1 calc R . .
C81 C 0.4325(3) 1.3339(5) -0.0061(2) 0.0523(16) Uani 1 1 d . . .
H81A H 0.4626 1.3087 -0.0212 0.063 Uiso 1 1 calc R . .
C80 C 0.5806(4) 1.5897(6) 0.1696(3) 0.070(2) Uani 1 1 d . . .
H80A H 0.5942 1.6454 0.1879 0.083 Uiso 1 1 calc R . .
C79 C 0.4387(4) 1.0987(5) 0.1522(3) 0.076(2) Uani 1 1 d . . .
H79A H 0.4026 1.0685 0.1499 0.091 Uiso 1 1 calc R . .
C78 C 0.5442(3) 1.1851(6) 0.1584(3) 0.067(2) Uani 1 1 d . . .
H78A H 0.5809 1.2135 0.1609 0.081 Uiso 1 1 calc R . .
C44 C 0.1771(3) 0.4449(5) 0.0078(3) 0.0582(18) Uani 1 1 d . . .
H44A H 0.1616 0.4263 -0.0247 0.070 Uiso 1 1 calc R . .
C77 C 0.5894(3) 1.3464(5) 0.0189(3) 0.0586(18) Uani 1 1 d . . .
H77A H 0.5842 1.4136 0.0236 0.070 Uiso 1 1 calc R . .
C99 C 0.1561(3) 1.1051(5) 0.1756(3) 0.0556(17) Uani 1 1 d . . .
H99A H 0.1893 1.0737 0.1920 0.067 Uiso 1 1 calc R . .
C76 C 0.3796(3) 1.3565(6) -0.0350(2) 0.065(2) Uani 1 1 d . . .
H76A H 0.3739 1.3466 -0.0694 0.078 Uiso 1 1 calc R . .
C75 C 0.5867(4) 1.4216(6) 0.1517(3) 0.090(3) Uani 1 1 d . . .
H75A H 0.6057 1.3614 0.1580 0.108 Uiso 1 1 calc R . .
C74 C 0.3439(3) 1.4091(5) 0.0382(3) 0.0573(18) Uani 1 1 d . . .
H74A H 0.3140 1.4351 0.0532 0.069 Uiso 1 1 calc R . .
C73 C 0.5116(3) 1.5154(5) 0.1066(3) 0.066(2) Uani 1 1 d . . .
H73A H 0.4789 1.5210 0.0821 0.079 Uiso 1 1 calc R . .
C98 C 0.0383(4) 1.5316(7) 0.0816(4) 0.097(3) Uani 1 1 d . . .
H98A H 0.0677 1.5643 0.0686 0.117 Uiso 1 1 calc R . .
C53 C 0.1518(3) 0.4173(5) 0.2593(3) 0.0616(19) Uani 1 1 d . . .
H53A H 0.1509 0.3637 0.2806 0.074 Uiso 1 1 calc R . .
C72 C 0.6255(3) 1.3145(6) -0.0126(3) 0.067(2) Uani 1 1 d . . .
H72A H 0.6444 1.3607 -0.0297 0.081 Uiso 1 1 calc R . .
C97 C -0.0468(4) 1.4339(6) 0.1217(4) 0.086(3) Uani 1 1 d . . .
H97A H -0.0761 1.4022 0.1352 0.104 Uiso 1 1 calc R . .
C24 C 0.1626(4) 0.7954(6) 0.3891(3) 0.083(3) Uani 1 1 d . . .
H24A H 0.1299 0.7750 0.4020 0.100 Uiso 1 1 calc R . .
C71 C 0.5331(4) 1.5965(5) 0.1337(3) 0.085(3) Uani 1 1 d . . .
H71A H 0.5147 1.6572 0.1274 0.101 Uiso 1 1 calc R . .
C96 C -0.0422(5) 1.5363(7) 0.1216(4) 0.118(4) Uani 1 1 d . . .
H96A H -0.0689 1.5738 0.1357 0.142 Uiso 1 1 calc R . .
C95 C -0.0001(5) 1.5823(7) 0.1017(5) 0.114(4) Uani 1 1 d . . .
H95A H 0.0018 1.6509 0.1023 0.137 Uiso 1 1 calc R . .
C118 C -0.0769(3) 1.2490(6) 0.0056(3) 0.065(2) Uani 1 1 d . . .
H11A H -0.1025 1.2860 0.0211 0.078 Uiso 1 1 calc R . .
C117 C 0.0129(3) 1.1642(6) 0.0099(3) 0.070(2) Uani 1 1 d . . .
H11B H 0.0478 1.1424 0.0283 0.084 Uiso 1 1 calc R . .
C54 C 0.1070(3) 0.4820(6) 0.2519(3) 0.072(2) Uani 1 1 d . . .
H54A H 0.0741 0.4703 0.2664 0.086 Uiso 1 1 calc R . .
C116 C -0.0568(4) 1.2202(6) 0.1813(3) 0.077(2) Uani 1 1 d . . .
H11C H -0.0283 1.2631 0.1968 0.092 Uiso 1 1 calc R . .
C115 C -0.1034(3) 1.1346(6) 0.1095(3) 0.077(2) Uani 1 1 d . . .
H11E H -0.1066 1.1192 0.0757 0.092 Uiso 1 1 calc R . .
C114 C -0.0910(4) 1.2262(7) -0.0443(3) 0.084(3) Uani 1 1 d . . .
H11F H -0.1264 1.2458 -0.0625 0.101 Uiso 1 1 calc R . .
C113 C 0.0006(4) 1.1422(7) -0.0397(3) 0.093(3) Uani 1 1 d . . .
H11G H 0.0269 1.1067 -0.0553 0.111 Uiso 1 1 calc R . .
N1 N 0.6694(4) 0.9095(8) -0.0231(3) 0.119(3) Uani 1 1 d . . .
C112 C -0.0942(4) 1.1753(7) 0.2080(4) 0.091(3) Uani 1 1 d . . .
H11H H -0.0911 1.1891 0.2420 0.109 Uiso 1 1 calc R . .
C111 C -0.0518(5) 1.1739(7) -0.0666(3) 0.089(3) Uani 1 1 d . . .
H11I H -0.0605 1.1593 -0.1006 0.106 Uiso 1 1 calc R . .
C110 C -0.1356(4) 1.1112(7) 0.1867(4) 0.094(3) Uani 1 1 d . . .
H11J H -0.1608 1.0816 0.2057 0.113 Uiso 1 1 calc R . .
C109 C -0.1395(4) 1.0914(8) 0.1378(4) 0.104(4) Uani 1 1 d . . .
H10F H -0.1676 1.0471 0.1230 0.125 Uiso 1 1 calc R . .
C128 C 0.2155(5) 0.4883(8) 0.3747(3) 0.092(3) Uani 1 1 d . . .
C121 C 0.7232(4) 0.8437(7) -0.0923(4) 0.104(3) Uani 1 1 d . . .
H12B H 0.6956 0.8219 -0.1203 0.156 Uiso 1 1 calc R . .
H12E H 0.7477 0.7895 -0.0795 0.156 Uiso 1 1 calc R . .
H12K H 0.7465 0.8958 -0.1026 0.156 Uiso 1 1 calc R . .
C125 C 0.2199(4) 0.9182(7) 0.0012(4) 0.094(3) Uani 1 1 d D . .
N2 N 0.1431(5) 1.0510(9) 0.0114(5) 0.171(5) Uani 1 1 d . . .
O1 O 0.0000 0.7766(12) 0.2500 0.128(8) Uani 0.50 2 d SP . .
C126 C 0.0165(8) 0.8352(18) 0.2156(7) 0.101(7) Uani 0.50 1 d P . .
H12C H 0.0570 0.8237 0.2132 0.121 Uiso 0.50 1 calc PR . .
H12D H -0.0066 0.8222 0.1832 0.121 Uiso 0.50 1 calc PR . .
C127 C 0.0094(7) 0.9207(15) 0.2284(10) 0.129(11) Uani 0.50 1 d P . .
H12H H -0.0187 0.9533 0.2034 0.155 Uiso 0.50 1 calc PR . .
H12I H 0.0458 0.9565 0.2313 0.155 Uiso 0.50 1 calc PR . .
C122 C 0.6919(4) 0.8806(7) -0.0528(4) 0.083(3) Uani 1 1 d . . .
C124 C 0.1761(4) 0.9949(7) 0.0075(4) 0.100(3) Uani 1 1 d D . .
N3 N 0.1977(5) 0.4249(8) 0.3938(3) 0.139(4) Uani 1 1 d . . .
C129 C 0.2345(6) 0.5702(8) 0.3500(4) 0.134(5) Uani 1 1 d . . .
H12F H 0.2691 0.5966 0.3695 0.202 Uiso 1 1 calc R . .
H12G H 0.2047 0.6198 0.3458 0.202 Uiso 1 1 calc R . .
H12J H 0.2426 0.5502 0.3178 0.202 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 V2 2.384(2) . ?
Se1 V1 2.392(2) . ?
Se2 Se3 2.302(2) . ?
Se2 V2 2.514(2) . ?
Se2 V1 2.5565(19) . ?
Se3 V1 2.553(2) . ?
Se3 V2 2.5560(19) . ?
V1 P1 2.391(2) . ?
V1 S3 2.461(3) . ?
V1 S1 2.466(3) . ?
V1 S2 2.527(2) . ?
V1 V2 2.909(2) . ?
V2 P2 2.366(3) . ?
V2 S4 2.460(3) . ?
V2 S6 2.476(2) . ?
V2 S5 2.552(3) . ?
S1 C16 1.763(6) . ?
P3 C92 1.785(6) . ?
P3 C93 1.805(6) . ?
P3 C89 1.808(6) . ?
P3 C94 1.832(6) . ?
P2 C51 1.823(5) . ?
P2 C61 1.824(6) . ?
P2 C41 1.842(6) . ?
P1 C21 1.822(6) . ?
P1 C11 1.833(6) . ?
P1 C31 1.838(6) . ?
S2 C26 1.775(6) . ?
S3 C36 1.767(6) . ?
S5 C56 1.749(6) . ?
S4 C46 1.743(6) . ?
S6 C66 1.752(6) . ?
P4 C105 1.790(7) . ?
P4 C106 1.796(7) . ?
P4 C107 1.799(7) . ?
P4 C108 1.813(6) . ?
C21 C22 1.388(8) . ?
C21 C26 1.410(8) . ?
C16 C11 1.390(7) . ?
C16 C15 1.403(8) . ?
C11 C12 1.414(8) . ?
C41 C42 1.387(8) . ?
C41 C46 1.411(7) . ?
C61 C62 1.398(8) . ?
C61 C66 1.413(8) . ?
C94 C81 1.378(8) . ?
C94 C90 1.392(8) . ?
C51 C52 1.397(8) . ?
C51 C56 1.406(8) . ?
C93 C91 1.378(8) . ?
C93 C77 1.393(8) . ?
C46 C45 1.406(8) . ?
C36 C31 1.386(8) . ?
C36 C35 1.420(8) . ?
C33 C34 1.381(10) . ?
C33 C32 1.389(9) . ?
C31 C32 1.404(8) . ?
C66 C65 1.422(8) . ?
C108 C103 1.366(9) . ?
C108 C102 1.389(8) . ?
C26 C25 1.407(9) . ?
C92 C85 1.384(8) . ?
C92 C78 1.406(8) . ?
C107 C116 1.389(10) . ?
C107 C115 1.394(9) . ?
C91 C86 1.387(8) . ?
C12 C13 1.393(9) . ?
C62 C63 1.391(9) . ?
C56 C55 1.403(8) . ?
C90 C74 1.384(9) . ?
C42 C43 1.400(8) . ?
C45 C44 1.376(9) . ?
C89 C75 1.375(9) . ?
C89 C73 1.376(8) . ?
C15 C14 1.381(9) . ?
C43 C44 1.379(9) . ?
C22 C23 1.392(9) . ?
C14 C13 1.392(9) . ?
C35 C34 1.378(9) . ?
C88 C80 1.343(11) . ?
C88 C75 1.396(10) . ?
C52 C53 1.377(9) . ?
C87 C79 1.348(10) . ?
C87 C84 1.366(10) . ?
C63 C64 1.370(10) . ?
C64 C65 1.383(9) . ?
C25 C24 1.390(10) . ?
C86 C82 1.383(9) . ?
C106 C117 1.367(9) . ?
C106 C118 1.416(9) . ?
C85 C79 1.398(9) . ?
C105 C97 1.388(10) . ?
C105 C104 1.388(9) . ?
C84 C78 1.377(9) . ?
C104 C98 1.381(11) . ?
C83 C76 1.382(10) . ?
C83 C74 1.383(10) . ?
C103 C101 1.387(9) . ?
C82 C72 1.365(10) . ?
C102 C100 1.414(9) . ?
C23 C24 1.385(11) . ?
C101 C99 1.375(10) . ?
C55 C54 1.405(10) . ?
C100 C99 1.351(9) . ?
C81 C76 1.399(9) . ?
C80 C71 1.368(11) . ?
C77 C72 1.376(9) . ?
C73 C71 1.385(10) . ?
C98 C95 1.328(13) . ?
C53 C54 1.367(10) . ?
C97 C96 1.405(12) . ?
C96 C95 1.361(13) . ?
C118 C114 1.388(11) . ?
C117 C113 1.376(11) . ?
C116 C112 1.376(11) . ?
C115 C109 1.373(11) . ?
C114 C111 1.385(12) . ?
C113 C111 1.402(12) . ?
N1 C122 1.113(11) . ?
C112 C110 1.372(13) . ?
C110 C109 1.355(13) . ?
C128 N3 1.126(12) . ?
C128 C129 1.418(13) . ?
C121 C122 1.489(13) . ?
C125 C124 1.4996(13) . ?
N2 C124 1.109(11) . ?
O1 C126 1.34(2) 2 ?
O1 C126 1.34(2) . ?
C126 C127 1.24(3) . ?
C127 C127 1.33(4) 2 ?

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
V2 Se1 V1 75.03(4) . . ?
Se3 Se2 V2 63.94(3) . . ?
Se3 Se2 V1 63.15(5) . . ?
V2 Se2 V1 70.01(4) . . ?
Se2 Se3 V1 63.30(3) . . ?
Se2 Se3 V2 62.07(5) . . ?
V1 Se3 V2 69.41(4) . . ?
P1 V1 Se1 89.56(5) . . ?
P1 V1 S3 78.37(6) . . ?
Se1 V1 S3 90.42(5) . . ?
P1 V1 S1 81.09(6) . . ?
Se1 V1 S1 170.12(6) . . ?
S3 V1 S1 90.82(6) . . ?
P1 V1 S2 72.49(6) . . ?
Se1 V1 S2 85.75(5) . . ?
S3 V1 S2 150.62(7) . . ?
S1 V1 S2 88.37(6) . . ?
P1 V1 Se3 153.43(6) . . ?
Se1 V1 Se3 102.43(4) . . ?
S3 V1 Se3 77.92(6) . . ?
S1 V1 Se3 87.42(5) . . ?
S2 V1 Se3 131.34(5) . . ?
P1 V1 Se2 148.31(6) . . ?
Se1 V1 Se2 99.20(4) . . ?
S3 V1 Se2 131.46(6) . . ?
S1 V1 Se2 87.28(5) . . ?
S2 V1 Se2 77.84(7) . . ?
Se3 V1 Se2 53.55(6) . . ?
P1 V1 V2 141.90(6) . . ?
Se1 V1 V2 52.36(5) . . ?
S3 V1 V2 100.40(5) . . ?
S1 V1 V2 136.83(6) . . ?
S2 V1 V2 100.17(6) . . ?
Se3 V1 V2 55.34(4) . . ?
Se2 V1 V2 54.31(4) . . ?
P2 V2 Se1 86.84(5) . . ?
P2 V2 S4 82.00(6) . . ?
Se1 V2 S4 168.17(6) . . ?
P2 V2 S6 78.36(7) . . ?
Se1 V2 S6 90.39(6) . . ?
S4 V2 S6 91.21(7) . . ?
P2 V2 Se2 148.15(6) . . ?
Se1 V2 Se2 100.63(4) . . ?
S4 V2 Se2 86.98(5) . . ?
S6 V2 Se2 131.89(6) . . ?
P2 V2 S5 71.97(5) . . ?
Se1 V2 S5 88.94(5) . . ?
S4 V2 S5 83.88(6) . . ?
S6 V2 S5 150.32(7) . . ?
Se2 V2 S5 77.22(5) . . ?
P2 V2 Se3 154.50(6) . . ?
Se1 V2 Se3 102.57(4) . . ?
S4 V2 Se3 89.23(5) . . ?
S6 V2 Se3 77.93(7) . . ?
Se2 V2 Se3 53.99(6) . . ?
S5 V2 Se3 131.04(6) . . ?
P2 V2 V1 139.43(6) . . ?
Se1 V2 V1 52.61(4) . . ?
S4 V2 V1 138.32(6) . . ?
S6 V2 V1 100.40(6) . . ?
Se2 V2 V1 55.68(5) . . ?
S5 V2 V1 102.65(5) . . ?
Se3 V2 V1 55.25(5) . . ?
C16 S1 V1 107.29(19) . . ?
C92 P3 C93 108.1(3) . . ?
C92 P3 C89 111.7(3) . . ?
C93 P3 C89 108.4(3) . . ?
C92 P3 C94 108.6(3) . . ?
C93 P3 C94 110.3(3) . . ?
C89 P3 C94 109.7(3) . . ?
C51 P2 C61 111.0(3) . . ?
C51 P2 C41 103.6(2) . . ?
C61 P2 C41 105.9(2) . . ?
C51 P2 V2 112.14(18) . . ?
C61 P2 V2 113.7(2) . . ?
C41 P2 V2 109.78(19) . . ?
C21 P1 C11 102.3(3) . . ?
C21 P1 C31 112.1(3) . . ?
C11 P1 C31 105.2(3) . . ?
C21 P1 V1 112.69(19) . . ?
C11 P1 V1 109.38(19) . . ?
C31 P1 V1 114.2(2) . . ?
C26 S2 V1 107.3(2) . . ?
C36 S3 V1 110.35(19) . . ?
C56 S5 V2 107.0(2) . . ?
C46 S4 V2 108.19(18) . . ?
C66 S6 V2 108.9(2) . . ?
C105 P4 C106 108.1(3) . . ?
C105 P4 C107 111.8(3) . . ?
C106 P4 C107 110.8(3) . . ?
C105 P4 C108 111.1(3) . . ?
C106 P4 C108 110.1(3) . . ?
C107 P4 C108 104.9(3) . . ?
C22 C21 C26 120.6(6) . . ?
C22 C21 P1 129.2(5) . . ?
C26 C21 P1 110.1(4) . . ?
C11 C16 C15 118.4(5) . . ?
C11 C16 S1 121.9(4) . . ?
C15 C16 S1 119.7(4) . . ?
C16 C11 C12 121.0(5) . . ?
C16 C11 P1 117.0(4) . . ?
C12 C11 P1 122.0(4) . . ?
C42 C41 C46 120.5(5) . . ?
C42 C41 P2 122.6(4) . . ?
C46 C41 P2 116.8(4) . . ?
C62 C61 C66 119.4(5) . . ?
C62 C61 P2 127.0(5) . . ?
C66 C61 P2 113.6(4) . . ?
C81 C94 C90 119.8(6) . . ?
C81 C94 P3 120.6(4) . . ?
C90 C94 P3 119.6(4) . . ?
C52 C51 C56 119.9(5) . . ?
C52 C51 P2 130.2(5) . . ?
C56 C51 P2 109.9(4) . . ?
C91 C93 C77 119.3(6) . . ?
C91 C93 P3 120.7(5) . . ?
C77 C93 P3 120.0(5) . . ?
C45 C46 C41 117.0(5) . . ?
C45 C46 S4 121.1(5) . . ?
C41 C46 S4 121.9(4) . . ?
C31 C36 C35 118.6(6) . . ?
C31 C36 S3 122.5(4) . . ?
C35 C36 S3 118.8(5) . . ?
C34 C33 C32 120.5(6) . . ?
C36 C31 C32 120.5(5) . . ?
C36 C31 P1 113.2(4) . . ?
C32 C31 P1 125.9(5) . . ?
C61 C66 C65 118.2(6) . . ?
C61 C66 S6 121.2(4) . . ?
C65 C66 S6 120.5(5) . . ?
C103 C108 C102 119.5(6) . . ?
C103 C108 P4 117.4(5) . . ?
C102 C108 P4 122.7(5) . . ?
C25 C26 C21 119.7(6) . . ?
C25 C26 S2 120.9(5) . . ?
C21 C26 S2 119.3(5) . . ?
C85 C92 C78 116.9(6) . . ?
C85 C92 P3 121.3(5) . . ?
C78 C92 P3 121.8(5) . . ?
C116 C107 C115 118.9(7) . . ?
C116 C107 P4 118.7(5) . . ?
C115 C107 P4 121.9(6) . . ?
C93 C91 C86 120.4(6) . . ?
C13 C12 C11 119.6(6) . . ?
C63 C62 C61 121.4(7) . . ?
C55 C56 C51 117.9(6) . . ?
C55 C56 S5 122.8(5) . . ?
C51 C56 S5 119.3(4) . . ?
C74 C90 C94 120.3(6) . . ?
C41 C42 C43 121.4(6) . . ?
C33 C32 C31 119.6(7) . . ?
C44 C45 C46 121.7(6) . . ?
C75 C89 C73 118.8(6) . . ?
C75 C89 P3 121.2(5) . . ?
C73 C89 P3 120.0(5) . . ?
C14 C15 C16 120.8(6) . . ?
C44 C43 C42 118.0(6) . . ?
C21 C22 C23 119.8(6) . . ?
C15 C14 C13 121.0(6) . . ?
C34 C35 C36 120.4(7) . . ?
C80 C88 C75 119.2(8) . . ?
C53 C52 C51 121.3(6) . . ?
C14 C13 C12 119.3(6) . . ?
C79 C87 C84 119.9(7) . . ?
C64 C63 C62 119.0(7) . . ?
C63 C64 C65 121.8(6) . . ?
C24 C25 C26 118.2(7) . . ?
C82 C86 C91 120.0(6) . . ?
C117 C106 C118 119.2(7) . . ?
C117 C106 P4 123.3(5) . . ?
C118 C106 P4 117.5(6) . . ?
C92 C85 C79 120.5(7) . . ?
C35 C34 C33 120.3(6) . . ?
C64 C65 C66 120.0(6) . . ?
C97 C105 C104 119.7(7) . . ?
C97 C105 P4 121.2(5) . . ?
C104 C105 P4 119.0(6) . . ?
C87 C84 C78 120.2(7) . . ?
C98 C104 C105 120.5(8) . . ?
C76 C83 C74 120.8(7) . . ?
C108 C103 C101 121.2(7) . . ?
C72 C82 C86 119.5(6) . . ?
C108 C102 C100 118.4(6) . . ?
C24 C23 C22 119.4(7) . . ?
C99 C101 C103 119.7(7) . . ?
C56 C55 C54 120.7(6) . . ?
C99 C100 C102 121.2(6) . . ?
C94 C81 C76 120.2(6) . . ?
C88 C80 C71 120.3(7) . . ?
C87 C79 C85 121.0(7) . . ?
C84 C78 C92 121.4(7) . . ?
C45 C44 C43 121.4(6) . . ?
C72 C77 C93 119.6(7) . . ?
C100 C99 C101 119.9(6) . . ?
C83 C76 C81 119.3(6) . . ?
C89 C75 C88 121.4(7) . . ?
C83 C74 C90 119.6(6) . . ?
C89 C73 C71 119.2(7) . . ?
C95 C98 C104 120.1(9) . . ?
C54 C53 C52 119.6(7) . . ?
C82 C72 C77 121.3(7) . . ?
C105 C97 C96 117.3(8) . . ?
C23 C24 C25 122.3(7) . . ?
C80 C71 C73 121.2(8) . . ?
C95 C96 C97 121.5(10) . . ?
C98 C95 C96 120.9(9) . . ?
C114 C118 C106 120.3(8) . . ?
C106 C117 C113 121.7(8) . . ?
C53 C54 C55 120.4(6) . . ?
C112 C116 C107 118.9(8) . . ?
C109 C115 C107 119.9(9) . . ?
C111 C114 C118 118.7(8) . . ?
C117 C113 C111 118.7(9) . . ?
C110 C112 C116 122.1(9) . . ?
C114 C111 C113 121.3(9) . . ?
C109 C110 C112 118.6(8) . . ?
C110 C109 C115 121.4(9) . . ?
N3 C128 C129 176.6(14) . . ?
C126 O1 C126 107(2) 2 . ?
C127 C126 O1 107.3(18) . . ?
C126 C127 C127 109.3(14) . 2 ?
N1 C122 C121 178.6(12) . . ?
N2 C124 C125 178.7(15) . . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        28.49
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 990545'
_audit_update_record             
;
2014-03-07 deposited with the CCDC.
2015-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ?
;
_chemical_name_common            '[V2(PS3)2(mu-S2)(mu-S)]'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44.40 H35 N2 O P2 S9 V2'
_chemical_formula_weight         1064.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
V V 0.3005 0.5294 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   18.842(2)
_cell_length_b                   12.4528(14)
_cell_length_c                   20.766(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.691(2)
_cell_angle_gamma                90.00
_cell_volume                     4713.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9965
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      28.27

_exptl_crystal_description       block
_exptl_crystal_colour            reddish-purple
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.37
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2174
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5248
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35059
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         28.31
_reflns_number_total             11648
_reflns_number_gt                9228
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of 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)+(0.0653P)²+4.7886P] 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         11648
_refine_ls_number_parameters     543
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1287
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
S7 S 0.30652(5) 0.89911(6) 0.03741(4) 0.02957(16) Uani 0.95 1 d P . .
V1 V 0.37191(2) 0.74732(3) 0.01799(2) 0.02843(11) Uani 1 1 d . . .
V2 V 0.36129(2) 0.82800(3) 0.14628(2) 0.02836(11) Uani 1 1 d . . .
P2 P 0.30441(4) 0.96112(5) 0.19920(3) 0.02770(14) Uani 1 1 d . . .
S3 S 0.40648(4) 0.93821(5) 0.00731(3) 0.03223(14) Uani 1 1 d . . .
S6 S 0.44329(4) 0.97736(6) 0.16446(4) 0.03352(15) Uani 1 1 d . . .
P1 P 0.32414(4) 0.77509(5) -0.09939(3) 0.02884(14) Uani 1 1 d . . .
S8 S 0.38303(4) 0.64600(5) 0.11688(4) 0.03524(15) Uani 1 1 d . . .
S1 S 0.46413(4) 0.66142(6) -0.01917(4) 0.03815(16) Uani 1 1 d . . .
S9 S 0.46642(4) 0.74856(6) 0.12106(4) 0.03568(16) Uani 1 1 d . . .
S5 S 0.23436(4) 0.77478(6) 0.10843(4) 0.03592(16) Uani 1 1 d . . .
S4 S 0.39081(4) 0.75866(5) 0.25405(4) 0.03397(15) Uani 1 1 d . . .
S2 S 0.27237(4) 0.62928(5) -0.01123(4) 0.03414(15) Uani 1 1 d . . .
C37 C 0.32277(15) 1.0937(2) 0.17353(13) 0.0299(5) Uani 1 1 d . . .
C36 C 0.37543(14) 0.9788(2) -0.07742(14) 0.0318(5) Uani 1 1 d . . .
C35 C 0.36672(15) 0.6792(2) -0.14298(14) 0.0333(6) Uani 1 1 d . . .
C34 C 0.34057(18) 0.6533(2) -0.20999(16) 0.0409(7) Uani 1 1 d . . .
H34A H 0.2982 0.6880 -0.2364 0.049 Uiso 1 1 calc R . .
C33 C 0.42936(15) 0.6301(2) -0.10385(15) 0.0342(6) Uani 1 1 d . . .
C32 C 0.17859(15) 0.8555(2) 0.14496(15) 0.0352(6) Uani 1 1 d . . .
C31 C 0.37762(15) 0.8574(2) 0.31050(14) 0.0340(6) Uani 1 1 d . . .
C30 C 0.20751(14) 0.9409(2) 0.18665(14) 0.0326(5) Uani 1 1 d . . .
C29 C 0.16192(18) 1.0008(2) 0.21600(18) 0.0446(7) Uani 1 1 d . . .
H29A H 0.1815 1.0580 0.2454 0.053 Uiso 1 1 calc R . .
C28 C 0.28042(17) 1.1856(2) 0.16997(15) 0.0374(6) Uani 1 1 d . . .
H28A H 0.2341 1.1829 0.1802 0.045 Uiso 1 1 calc R . .
C27 C 0.34273(16) 0.9541(2) 0.28779(13) 0.0344(6) Uani 1 1 d . . .
C26 C 0.20705(15) 0.6743(2) -0.08280(14) 0.0340(6) Uani 1 1 d . . .
C25 C 0.46493(17) 0.5524(2) -0.13298(18) 0.0440(7) Uani 1 1 d . . .
H25A H 0.5074 0.5173 -0.1071 0.053 Uiso 1 1 calc R . .
C24 C 0.41611(17) 1.1930(2) 0.13815(16) 0.0415(7) Uani 1 1 d . . .
H24A H 0.4618 1.1963 0.1268 0.050 Uiso 1 1 calc R . .
C23 C 0.22708(14) 0.7491(2) -0.12496(14) 0.0316(5) Uani 1 1 d . . .
C22 C 0.38905(16) 1.0847(2) -0.09242(16) 0.0381(6) Uani 1 1 d . . .
H22A H 0.4119 1.1334 -0.0582 0.046 Uiso 1 1 calc R . .
C21 C 0.32291(16) 0.9413(2) -0.19318(15) 0.0395(6) Uani 1 1 d . . .
H21A H 0.3009 0.8926 -0.2277 0.047 Uiso 1 1 calc R . .
C20 C 0.39071(15) 1.0962(2) 0.15737(13) 0.0315(5) Uani 1 1 d . . .
C19 C 0.34189(14) 0.9075(2) -0.12682(14) 0.0323(5) Uani 1 1 d . . .
C18 C 0.33654(17) 1.0464(3) -0.20796(16) 0.0430(7) Uani 1 1 d . . .
H18A H 0.3236 1.0700 -0.2529 0.052 Uiso 1 1 calc R . .
C17 C 0.33415(19) 1.0329(3) 0.33247(16) 0.0452(7) Uani 1 1 d . . .
H17A H 0.3105 1.0987 0.3167 0.054 Uiso 1 1 calc R . .
C16 C 0.40300(18) 0.8406(3) 0.37903(15) 0.0451(7) Uani 1 1 d . . .
H16A H 0.4263 0.7748 0.3953 0.054 Uiso 1 1 calc R . .
C15 C 0.10375(17) 0.8312(3) 0.13214(19) 0.0490(8) Uani 1 1 d . . .
H15A H 0.0838 0.7730 0.1038 0.059 Uiso 1 1 calc R . .
C14 C 0.30672(19) 1.2820(2) 0.15118(17) 0.0458(7) Uani 1 1 d . . .
H14A H 0.2786 1.3458 0.1490 0.055 Uiso 1 1 calc R . .
C13 C 0.3769(2) 0.5764(3) -0.23804(18) 0.0497(8) Uani 1 1 d . . .
H13A H 0.3595 0.5582 -0.2838 0.060 Uiso 1 1 calc R . .
C12 C 0.36872(16) 1.1172(2) -0.15798(16) 0.0425(7) Uani 1 1 d . . .
H12A H 0.3770 1.1894 -0.1689 0.051 Uiso 1 1 calc R . .
C11 C 0.05928(18) 0.8925(3) 0.1610(2) 0.0569(9) Uani 1 1 d . . .
H11A H 0.0085 0.8762 0.1523 0.068 Uiso 1 1 calc R . .
C10 C 0.3943(2) 0.9190(3) 0.42286(16) 0.0561(9) Uani 1 1 d . . .
H10A H 0.4119 0.9072 0.4694 0.067 Uiso 1 1 calc R . .
C9 C 0.17541(17) 0.7886(3) -0.17988(15) 0.0416(7) Uani 1 1 d . . .
H9A H 0.1889 0.8407 -0.2080 0.050 Uiso 1 1 calc R . .
C8 C 0.13538(17) 0.6357(3) -0.09748(16) 0.0453(7) Uani 1 1 d . . .
H8A H 0.1216 0.5831 -0.0698 0.054 Uiso 1 1 calc R . .
C7 C 0.08759(19) 0.9768(3) 0.2021(2) 0.0558(9) Uani 1 1 d . . .
H7A H 0.0562 1.0190 0.2212 0.067 Uiso 1 1 calc R . .
C6 C 0.3603(2) 1.0149(3) 0.40012(17) 0.0572(9) Uani 1 1 d . . .
H6A H 0.3549 1.0686 0.4310 0.069 Uiso 1 1 calc R . .
C5 C 0.37354(19) 1.2846(3) 0.13580(18) 0.0485(8) Uani 1 1 d . . .
H5A H 0.3910 1.3510 0.1232 0.058 Uiso 1 1 calc R . .
C3 C 0.08443(17) 0.6747(3) -0.15283(19) 0.0541(9) Uani 1 1 d . . .
H3A H 0.0355 0.6485 -0.1630 0.065 Uiso 1 1 calc R . .
C2 C 0.10367(18) 0.7508(3) -0.19317(18) 0.0496(8) Uani 1 1 d . . .
H2A H 0.0678 0.7778 -0.2304 0.059 Uiso 1 1 calc R . .
C1 C 0.4381(2) 0.5267(3) -0.19946(19) 0.0523(9) Uani 1 1 d . . .
H1A H 0.4624 0.4737 -0.2188 0.063 Uiso 1 1 calc R . .
C40 C 0.9517(3) 0.6439(4) 0.1375(2) 0.0740(12) Uani 1 1 d . . .
N2 N 0.9564(4) 0.6426(6) 0.0857(3) 0.146(3) Uani 1 1 d . . .
C41 C 0.9485(4) 0.6505(6) 0.2043(3) 0.122(2) Uani 1 1 d . . .
H41A H 0.9248 0.5859 0.2160 0.183 Uiso 1 1 calc R . .
H41B H 0.9201 0.7140 0.2102 0.183 Uiso 1 1 calc R . .
H41C H 0.9983 0.6562 0.2332 0.183 Uiso 1 1 calc R . .
O1 O 0.3769(3) 0.5493(8) -0.4031(3) 0.184(3) Uani 1 1 d . . .
C44 C 0.3181(5) 0.6084(9) -0.4246(5) 0.164(4) Uani 1 1 d . . .
H44A H 0.3186 0.6745 -0.3980 0.197 Uiso 1 1 calc R . .
H44B H 0.2720 0.5680 -0.4282 0.197 Uiso 1 1 calc R . .
C46 C 0.3919(7) 0.5557(9) -0.5055(5) 0.181(5) Uani 1 1 d D . .
H46A H 0.4394 0.5929 -0.5008 0.217 Uiso 1 1 calc R . .
H46B H 0.3770 0.5212 -0.5499 0.217 Uiso 1 1 calc R . .
C47 C 0.3958(5) 0.4739(7) -0.4493(6) 0.173(5) Uani 1 1 d . . .
H47A H 0.3593 0.4155 -0.4622 0.208 Uiso 1 1 calc R . .
H47B H 0.4455 0.4432 -0.4323 0.208 Uiso 1 1 calc R . .
C45 C 0.3340(7) 0.6308(8) -0.4944(4) 0.241(8) Uani 1 1 d D . .
H45A H 0.2884 0.6211 -0.5301 0.289 Uiso 1 1 calc R . .
H45B H 0.3506 0.7060 -0.4961 0.289 Uiso 1 1 calc R . .
N1 N 0.2423(3) 0.8427(5) -0.3412(2) 0.124(2) Uani 1 1 d . . .
C50 C 0.1661(4) 0.8666(5) -0.4585(3) 0.1049(18) Uiso 1 1 d . . .
C51 C 0.2049(4) 0.8731(6) -0.3889(4) 0.113(2) Uiso 1 1 d . . .
C52 C 0.2678(9) 0.7624(13) -0.3925(8) 0.044(3) Uiso 0.20 1 d P . .
C53 C 0.2258(10) 0.8183(15) -0.4606(9) 0.054(4) Uiso 0.20 1 d P . .
S7' S 0.2856(8) 0.8830(12) 0.0449(7) 0.017(3) Uiso 0.05 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
S7 S7' 0.500(13) . ?
S7 V2 2.4036(9) . ?
V1 S1 2.3321(8) . ?
V1 S2 2.3386(8) . ?
V1 S8 2.3739(9) . ?
V1 P1 2.3996(9) . ?
V1 S9 2.4124(9) . ?
V1 S3 2.4895(8) . ?
V1 S7' 2.505(14) . ?
V1 V2 2.9014(7) . ?
V2 S7' 2.327(14) . ?
V2 S4 2.3305(8) . ?
V2 S6 2.3861(8) . ?
V2 P2 2.3879(8) . ?
V2 S9 2.3881(8) . ?
V2 S8 2.4091(8) . ?
V2 S5 2.4133(8) . ?
P2 C37 1.795(3) . ?
P2 C30 1.795(3) . ?
P2 C27 1.800(3) . ?
S3 C36 1.781(3) . ?
S6 C20 1.766(3) . ?
P1 C23 1.800(3) . ?
P1 C19 1.804(3) . ?
P1 C35 1.805(3) . ?
S8 S9 2.0095(11) . ?
S1 C33 1.758(3) . ?
S5 C32 1.759(3) . ?
S5 S7' 2.267(14) . ?
S4 C31 1.760(3) . ?
S2 C26 1.764(3) . ?
C37 C28 1.387(4) . ?
C37 C20 1.404(4) . ?
C36 C19 1.382(4) . ?
C36 C22 1.393(4) . ?
C35 C34 1.391(4) . ?
C35 C33 1.393(4) . ?
C34 C13 1.388(4) . ?
C33 C25 1.399(4) . ?
C32 C30 1.391(4) . ?
C32 C15 1.400(4) . ?
C31 C27 1.395(4) . ?
C31 C16 1.397(4) . ?
C30 C29 1.390(4) . ?
C29 C7 1.389(4) . ?
C28 C14 1.391(4) . ?
C27 C17 1.388(4) . ?
C26 C8 1.392(4) . ?
C26 C23 1.394(4) . ?
C25 C1 1.382(5) . ?
C24 C5 1.388(5) . ?
C24 C20 1.392(4) . ?
C23 C9 1.388(4) . ?
C22 C12 1.378(4) . ?
C21 C18 1.383(4) . ?
C21 C19 1.398(4) . ?
C18 C12 1.380(5) . ?
C17 C6 1.384(5) . ?
C16 C10 1.373(5) . ?
C15 C11 1.378(5) . ?
C14 C5 1.376(5) . ?
C13 C1 1.373(5) . ?
C11 C7 1.373(5) . ?
C10 C6 1.380(5) . ?
C9 C2 1.391(4) . ?
C8 C3 1.385(5) . ?
C3 C2 1.373(5) . ?
C40 N2 1.100(7) . ?
C40 C41 1.407(7) . ?
O1 C44 1.311(10) . ?
O1 C47 1.450(12) . ?
C44 C45 1.577(12) . ?
C46 C45 1.4994(10) . ?
C46 C47 1.538(13) . ?
N1 C51 1.125(8) . ?
N1 C52 1.620(17) . ?
C50 C53 1.285(19) . ?
C50 C51 1.447(9) . ?
C51 C53 1.77(2) . ?
C51 C52 1.831(18) . ?
C52 C53 1.60(2) . ?

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
S7' S7 V2 75.2(17) . . ?
S1 V1 S2 103.99(3) . . ?
S1 V1 S8 97.63(3) . . ?
S2 V1 S8 77.25(3) . . ?
S1 V1 P1 81.32(3) . . ?
S2 V1 P1 75.97(3) . . ?
S8 V1 P1 152.06(3) . . ?
S1 V1 S9 81.50(3) . . ?
S2 V1 S9 126.67(3) . . ?
S8 V1 S9 49.64(3) . . ?
P1 V1 S9 154.51(3) . . ?
S1 V1 S3 100.07(3) . . ?
S2 V1 S3 141.98(3) . . ?
S8 V1 S3 128.09(3) . . ?
P1 V1 S3 79.11(3) . . ?
S9 V1 S3 85.52(3) . . ?
S1 V1 S7' 164.5(3) . . ?
S2 V1 S7' 87.6(3) . . ?
S8 V1 S7' 94.9(3) . . ?
P1 V1 S7' 91.8(3) . . ?
S9 V1 S7' 99.9(3) . . ?
S3 V1 S7' 64.8(3) . . ?
S1 V1 V2 133.89(3) . . ?
S2 V1 V2 102.61(2) . . ?
S8 V1 V2 53.21(2) . . ?
P1 V1 V2 141.94(3) . . ?
S9 V1 V2 52.43(2) . . ?
S3 V1 V2 80.31(2) . . ?
S7' V1 V2 50.3(3) . . ?
S7' V2 S4 157.0(3) . . ?
S7' V2 S6 97.9(4) . . ?
S4 V2 S6 98.61(3) . . ?
S7' V2 P2 88.2(3) . . ?
S4 V2 P2 80.85(3) . . ?
S6 V2 P2 74.59(3) . . ?
S7' V2 S9 106.0(3) . . ?
S4 V2 S9 92.75(3) . . ?
S6 V2 S9 79.50(3) . . ?
P2 V2 S9 151.96(3) . . ?
S7' V2 S7 12.0(3) . . ?
S4 V2 S7 168.72(4) . . ?
S6 V2 S7 88.16(3) . . ?
P2 V2 S7 92.37(3) . . ?
S9 V2 S7 97.38(3) . . ?
S7' V2 S8 98.8(4) . . ?
S4 V2 S8 83.13(3) . . ?
S6 V2 S8 128.94(3) . . ?
P2 V2 S8 153.48(3) . . ?
S9 V2 S8 49.53(3) . . ?
S7 V2 S8 99.69(3) . . ?
S7' V2 S5 57.1(3) . . ?
S4 V2 S5 100.75(3) . . ?
S6 V2 S5 144.49(3) . . ?
P2 V2 S5 79.46(3) . . ?
S9 V2 S5 128.57(3) . . ?
S7 V2 S5 68.97(3) . . ?
S8 V2 S5 82.95(3) . . ?
S7' V2 V1 56.0(3) . . ?
S4 V2 V1 134.28(3) . . ?
S6 V2 V1 102.85(2) . . ?
P2 V2 V1 143.76(3) . . ?
S9 V2 V1 53.20(2) . . ?
S7 V2 V1 51.47(2) . . ?
S8 V2 V1 52.10(2) . . ?
S5 V2 V1 84.22(2) . . ?
C37 P2 C30 110.58(13) . . ?
C37 P2 C27 106.90(13) . . ?
C30 P2 C27 105.73(13) . . ?
C37 P2 V2 111.03(9) . . ?
C30 P2 V2 113.22(9) . . ?
C27 P2 V2 109.02(10) . . ?
C36 S3 V1 109.33(9) . . ?
C20 S6 V2 108.24(9) . . ?
C23 P1 C19 109.10(13) . . ?
C23 P1 C35 106.30(12) . . ?
C19 P1 C35 107.77(12) . . ?
C23 P1 V1 111.41(9) . . ?
C19 P1 V1 113.62(10) . . ?
C35 P1 V1 108.30(10) . . ?
S9 S8 V1 66.17(3) . . ?
S9 S8 V2 64.69(3) . . ?
V1 S8 V2 74.69(3) . . ?
C33 S1 V1 108.22(9) . . ?
S8 S9 V2 65.78(3) . . ?
S8 S9 V1 64.18(3) . . ?
V2 S9 V1 74.37(3) . . ?
C32 S5 S7' 107.5(4) . . ?
C32 S5 V2 110.71(10) . . ?
S7' S5 V2 59.5(4) . . ?
C31 S4 V2 109.94(10) . . ?
C26 S2 V1 111.18(10) . . ?
C28 C37 C20 121.0(2) . . ?
C28 C37 P2 128.6(2) . . ?
C20 C37 P2 110.37(19) . . ?
C19 C36 C22 121.1(3) . . ?
C19 C36 S3 121.7(2) . . ?
C22 C36 S3 117.1(2) . . ?
C34 C35 C33 121.0(3) . . ?
C34 C35 P1 124.4(2) . . ?
C33 C35 P1 114.6(2) . . ?
C13 C34 C35 119.5(3) . . ?
C35 C33 C25 118.6(3) . . ?
C35 C33 S1 122.2(2) . . ?
C25 C33 S1 119.2(2) . . ?
C30 C32 C15 120.0(3) . . ?
C30 C32 S5 121.5(2) . . ?
C15 C32 S5 118.5(2) . . ?
C27 C31 C16 118.9(3) . . ?
C27 C31 S4 120.8(2) . . ?
C16 C31 S4 120.3(2) . . ?
C29 C30 C32 119.7(3) . . ?
C29 C30 P2 125.4(2) . . ?
C32 C30 P2 114.9(2) . . ?
C7 C29 C30 119.7(3) . . ?
C37 C28 C14 119.1(3) . . ?
C17 C27 C31 120.6(3) . . ?
C17 C27 P2 124.3(2) . . ?
C31 C27 P2 114.8(2) . . ?
C8 C26 C23 119.7(3) . . ?
C8 C26 S2 120.4(2) . . ?
C23 C26 S2 119.9(2) . . ?
C1 C25 C33 119.8(3) . . ?
C5 C24 C20 118.9(3) . . ?
C9 C23 C26 120.5(3) . . ?
C9 C23 P1 128.8(2) . . ?
C26 C23 P1 110.6(2) . . ?
C12 C22 C36 118.6(3) . . ?
C18 C21 C19 119.2(3) . . ?
C24 C20 C37 119.3(3) . . ?
C24 C20 S6 121.5(2) . . ?
C37 C20 S6 119.2(2) . . ?
C36 C19 C21 119.6(3) . . ?
C36 C19 P1 116.1(2) . . ?
C21 C19 P1 124.4(2) . . ?
C12 C18 C21 120.6(3) . . ?
C6 C17 C27 119.4(3) . . ?
C10 C16 C31 120.0(3) . . ?
C11 C15 C32 119.5(3) . . ?
C5 C14 C28 119.9(3) . . ?
C1 C13 C34 119.7(3) . . ?
C22 C12 C18 120.9(3) . . ?
C7 C11 C15 120.7(3) . . ?
C16 C10 C6 120.8(3) . . ?
C23 C9 C2 119.2(3) . . ?
C3 C8 C26 119.4(3) . . ?
C11 C7 C29 120.4(3) . . ?
C10 C6 C17 120.2(3) . . ?
C14 C5 C24 121.8(3) . . ?
C2 C3 C8 120.9(3) . . ?
C3 C2 C9 120.4(3) . . ?
C13 C1 C25 121.3(3) . . ?
N2 C40 C41 176.8(7) . . ?
C44 O1 C47 117.8(7) . . ?
O1 C44 C45 94.1(8) . . ?
C45 C46 C47 101.1(9) . . ?
O1 C47 C46 95.8(7) . . ?
C46 C45 C44 110.3(9) . . ?
C51 N1 C52 81.6(8) . . ?
C53 C50 C51 80.6(10) . . ?
N1 C51 C50 154.8(8) . . ?
N1 C51 C53 112.8(9) . . ?
C50 C51 C53 45.7(7) . . ?
N1 C51 C52 61.0(7) . . ?
C50 C51 C52 94.9(7) . . ?
C53 C51 C52 52.6(8) . . ?
C53 C52 N1 98.6(11) . . ?
C53 C52 C51 61.8(9) . . ?
N1 C52 C51 37.4(4) . . ?
C50 C53 C52 114.5(14) . . ?
C50 C53 C51 53.7(8) . . ?
C52 C53 C51 65.7(10) . . ?
S7 S7' S5 155(2) . . ?
S7 S7' V2 92.8(17) . . ?
S5 S7' V2 63.4(4) . . ?
S7 S7' V1 66.1(16) . . ?
S5 S7' V1 97.2(5) . . ?
V2 S7' V1 73.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.083
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 990546'
_audit_update_record             
;
2014-03-07 deposited with the CCDC.
2015-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[V2(PS3")2(mu-Se2)(mu-Se)]'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C57.40 H72 O0.85 P2 S6 Se3 Si6 V2'
_chemical_formula_weight         1537.15

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'
Si Si 0.0817 0.0704 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   15.430(2)
_cell_length_b                   15.527(2)
_cell_length_c                   17.671(2)
_cell_angle_alpha                80.054(2)
_cell_angle_beta                 69.489(2)
_cell_angle_gamma                77.016(2)
_cell_volume                     3843.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4427
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      21.73

_exptl_crystal_description       block
_exptl_crystal_colour            bluish-purple
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1562
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45695
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_sigmaI/netI    0.1539
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         28.04
_reflns_number_total             18526
_reflns_number_gt                8406
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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)+(0.0929P)²+0.0000P] 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         18526
_refine_ls_number_parameters     678
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1733
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.2082
_refine_ls_wR_factor_gt          0.1654
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_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
Se1 Se 0.44043(5) 0.69850(5) 0.22028(4) 0.04118(19) Uani 1 1 d . . .
Se3 Se 0.54937(5) 0.88296(5) 0.25066(5) 0.0467(2) Uani 1 1 d . . .
Se2 Se 0.58956(5) 0.76005(5) 0.32956(4) 0.0478(2) Uani 1 1 d . . .
V2 V 0.41997(8) 0.79499(7) 0.32792(7) 0.0358(3) Uani 1 1 d . . .
V1 V 0.60051(8) 0.73473(7) 0.18901(7) 0.0358(3) Uani 1 1 d . . .
P1 P 0.66114(13) 0.64459(11) 0.07983(11) 0.0385(4) Uani 1 1 d . . .
S3 S 0.49879(13) 0.80497(11) 0.10252(10) 0.0392(4) Uani 1 1 d . . .
P2 P 0.25691(13) 0.78859(12) 0.38242(11) 0.0403(4) Uani 1 1 d . . .
S1 S 0.73150(13) 0.79883(12) 0.11235(11) 0.0442(5) Uani 1 1 d . . .
S5 S 0.42112(13) 0.63062(12) 0.36309(11) 0.0431(4) Uani 1 1 d . . .
S4 S 0.39101(13) 0.83263(13) 0.45750(11) 0.0457(5) Uani 1 1 d . . .
S2 S 0.67242(14) 0.59684(12) 0.24168(11) 0.0481(5) Uani 1 1 d . . .
S6 S 0.34467(13) 0.92894(12) 0.27261(12) 0.0478(5) Uani 1 1 d . . .
Si2 Si 0.37242(16) 0.86699(14) -0.02696(13) 0.0490(5) Uani 1 1 d . . .
Si3 Si 0.77798(18) 0.38869(16) 0.29320(15) 0.0642(7) Uani 1 1 d . . .
Si4 Si 0.31549(18) 0.96139(19) 0.61296(16) 0.0712(8) Uani 1 1 d . . .
Si1 Si 0.95433(17) 0.83229(18) 0.02282(17) 0.0696(8) Uani 1 1 d . . .
Si5 Si 0.20237(19) 1.11391(16) 0.22407(17) 0.0692(7) Uani 1 1 d . . .
Si6 Si 0.3839(2) 0.41565(16) 0.39776(18) 0.0738(8) Uani 1 1 d . . .
C41 C 0.2067(5) 0.8520(5) 0.4693(4) 0.0443(18) Uani 1 1 d . . .
C42 C 0.2677(5) 0.8712(5) 0.5030(4) 0.0428(17) Uani 1 1 d . . .
C11 C 0.7845(5) 0.6501(5) 0.0317(4) 0.0440(18) Uani 1 1 d . . .
C12 C 0.8138(5) 0.7227(5) 0.0453(4) 0.0402(17) Uani 1 1 d . . .
C1 C 0.6056(5) 0.6763(4) 0.0032(4) 0.0422(17) Uani 1 1 d . . .
C52 C 0.3051(5) 0.6082(5) 0.3992(4) 0.0430(17) Uani 1 1 d . . .
C31 C 0.1916(5) 0.8478(5) 0.3163(4) 0.0416(17) Uani 1 1 d . . .
C2 C 0.5292(5) 0.7456(4) 0.0156(4) 0.0370(16) Uani 1 1 d . . .
C16 C 0.8504(6) 0.5864(5) -0.0158(4) 0.052(2) Uani 1 1 d . . .
H16A H 0.8306 0.5366 -0.0250 0.063 Uiso 1 1 calc R . .
C13 C 0.9080(5) 0.7333(5) 0.0110(4) 0.0482(19) Uani 1 1 d . . .
C43 C 0.2376(5) 0.9217(5) 0.5682(4) 0.051(2) Uani 1 1 d . . .
C32 C 0.2290(5) 0.9248(5) 0.2793(4) 0.0429(17) Uani 1 1 d . . .
C3 C 0.4769(5) 0.7739(5) -0.0389(4) 0.0421(17) Uani 1 1 d . . .
C33 C 0.1756(5) 0.9977(5) 0.2457(4) 0.0494(19) Uani 1 1 d . . .
C22 C 0.6896(5) 0.5085(4) 0.1833(4) 0.0421(17) Uani 1 1 d . . .
C23 C 0.7261(5) 0.4205(4) 0.2076(5) 0.0482(19) Uani 1 1 d . . .
C56 C 0.1362(6) 0.6620(6) 0.4544(5) 0.064(2) Uani 1 1 d . . .
H56A H 0.0845 0.7098 0.4663 0.077 Uiso 1 1 calc R . .
C21 C 0.6664(5) 0.5279(4) 0.1122(4) 0.0430(17) Uani 1 1 d . . .
C51 C 0.2289(6) 0.6789(5) 0.4156(5) 0.053(2) Uani 1 1 d . . .
C26 C 0.6639(6) 0.4611(5) 0.0707(5) 0.056(2) Uani 1 1 d . . .
H26A H 0.6428 0.4754 0.0249 0.067 Uiso 1 1 calc R . .
C4 C 0.5085(6) 0.7293(5) -0.1077(5) 0.060(2) Uani 1 1 d . . .
H4A H 0.4755 0.7460 -0.1459 0.072 Uiso 1 1 calc R . .
C46 C 0.1106(5) 0.8841(5) 0.5008(4) 0.0496(19) Uani 1 1 d . . .
H46A H 0.0688 0.8723 0.4768 0.060 Uiso 1 1 calc R . .
C15 C 0.9413(6) 0.5945(5) -0.0486(5) 0.061(2) Uani 1 1 d . . .
H15A H 0.9855 0.5504 -0.0803 0.073 Uiso 1 1 calc R . .
C34 C 0.0930(6) 0.9813(6) 0.2424(5) 0.056(2) Uani 1 1 d . . .
H34A H 0.0549 1.0282 0.2200 0.067 Uiso 1 1 calc R . .
C6 C 0.6355(6) 0.6340(5) -0.0689(5) 0.059(2) Uani 1 1 d . . .
H6A H 0.6886 0.5873 -0.0796 0.070 Uiso 1 1 calc R . .
C35 C 0.0618(6) 0.9015(6) 0.2694(5) 0.061(2) Uani 1 1 d . . .
H35A H 0.0077 0.8922 0.2600 0.073 Uiso 1 1 calc R . .
C24 C 0.7252(6) 0.3548(5) 0.1626(5) 0.065(2) Uani 1 1 d . . .
H24A H 0.7481 0.2947 0.1782 0.078 Uiso 1 1 calc R . .
C25 C 0.6926(7) 0.3728(5) 0.0966(5) 0.066(2) Uani 1 1 d . . .
H25A H 0.6899 0.3260 0.0698 0.079 Uiso 1 1 calc R . .
C45 C 0.0760(6) 0.9329(6) 0.5666(5) 0.059(2) Uani 1 1 d . . .
H45A H 0.0103 0.9533 0.5894 0.071 Uiso 1 1 calc R . .
C44 C 0.1393(6) 0.9516(6) 0.5992(5) 0.063(2) Uani 1 1 d . . .
H44A H 0.1154 0.9859 0.6441 0.076 Uiso 1 1 calc R . .
C36 C 0.1093(5) 0.8356(5) 0.3099(4) 0.051(2) Uani 1 1 d . . .
H36A H 0.0856 0.7822 0.3331 0.062 Uiso 1 1 calc R . .
C53 C 0.2903(6) 0.5187(5) 0.4181(5) 0.057(2) Uani 1 1 d . . .
C54 C 0.1955(7) 0.5068(6) 0.4546(6) 0.075(3) Uani 1 1 d . . .
H54A H 0.1821 0.4482 0.4659 0.090 Uiso 1 1 calc R . .
C48 C 0.4052(6) 0.8703(8) 0.6403(6) 0.095(4) Uani 1 1 d . . .
H48A H 0.4428 0.8951 0.6628 0.142 Uiso 1 1 calc R . .
H48B H 0.4464 0.8420 0.5915 0.142 Uiso 1 1 calc R . .
H48C H 0.3734 0.8260 0.6807 0.142 Uiso 1 1 calc R . .
C59 C 0.4735(7) 0.4284(7) 0.2965(6) 0.093(3) Uani 1 1 d . . .
H59A H 0.5058 0.4770 0.2941 0.140 Uiso 1 1 calc R . .
H59B H 0.4429 0.4421 0.2546 0.140 Uiso 1 1 calc R . .
H59C H 0.5193 0.3731 0.2871 0.140 Uiso 1 1 calc R . .
C55 C 0.1220(6) 0.5774(6) 0.4743(6) 0.076(3) Uani 1 1 d . . .
H55A H 0.0601 0.5660 0.5024 0.092 Uiso 1 1 calc R . .
C47 C 0.2386(7) 1.0113(8) 0.7086(6) 0.105(4) Uani 1 1 d . . .
H47A H 0.2773 1.0319 0.7330 0.157 Uiso 1 1 calc R . .
H47B H 0.2052 0.9664 0.7469 0.157 Uiso 1 1 calc R . .
H47C H 0.1928 1.0617 0.6961 0.157 Uiso 1 1 calc R . .
C14 C 0.9706(5) 0.6678(5) -0.0359(5) 0.058(2) Uani 1 1 d . . .
H14A H 1.0349 0.6732 -0.0597 0.070 Uiso 1 1 calc R . .
C5 C 0.5865(6) 0.6613(6) -0.1234(5) 0.067(3) Uani 1 1 d . . .
H5A H 0.6061 0.6335 -0.1720 0.081 Uiso 1 1 calc R . .
C9 C 0.4072(8) 0.9734(6) -0.0278(8) 0.108(4) Uani 1 1 d . . .
H9A H 0.3525 1.0213 -0.0218 0.162 Uiso 1 1 calc R . .
H9B H 0.4564 0.9856 -0.0793 0.162 Uiso 1 1 calc R . .
H9C H 0.4313 0.9698 0.0174 0.162 Uiso 1 1 calc R . .
C18 C 0.8872(7) 0.9377(6) -0.0096(7) 0.097(4) Uani 1 1 d . . .
H18A H 0.9120 0.9877 -0.0029 0.146 Uiso 1 1 calc R . .
H18B H 0.8208 0.9425 0.0237 0.146 Uiso 1 1 calc R . .
H18C H 0.8932 0.9388 -0.0668 0.146 Uiso 1 1 calc R . .
C8 C 0.3320(6) 0.8754(6) -0.1160(5) 0.069(3) Uani 1 1 d . . .
H8A H 0.2775 0.9234 -0.1114 0.104 Uiso 1 1 calc R . .
H8B H 0.3141 0.8191 -0.1175 0.104 Uiso 1 1 calc R . .
H8C H 0.3829 0.8880 -0.1661 0.104 Uiso 1 1 calc R . .
C17 C 0.9498(9) 0.8323(10) 0.1259(7) 0.139(5) Uani 1 1 d . . .
H17A H 0.9738 0.8839 0.1302 0.208 Uiso 1 1 calc R . .
H17B H 0.9885 0.7777 0.1416 0.208 Uiso 1 1 calc R . .
H17C H 0.8846 0.8352 0.1619 0.208 Uiso 1 1 calc R . .
C28 C 0.8323(8) 0.2689(6) 0.2922(7) 0.109(4) Uani 1 1 d . . .
H28A H 0.8599 0.2509 0.3359 0.164 Uiso 1 1 calc R . .
H28B H 0.8815 0.2592 0.2398 0.164 Uiso 1 1 calc R . .
H28C H 0.7841 0.2334 0.3002 0.164 Uiso 1 1 calc R . .
C7 C 0.2767(6) 0.8386(7) 0.0656(5) 0.087(3) Uani 1 1 d . . .
H7A H 0.2220 0.8866 0.0720 0.131 Uiso 1 1 calc R . .
H7B H 0.2979 0.8310 0.1129 0.131 Uiso 1 1 calc R . .
H7C H 0.2595 0.7832 0.0609 0.131 Uiso 1 1 calc R . .
C58 C 0.3220(10) 0.3241(7) 0.3965(10) 0.173(7) Uani 1 1 d . . .
H58A H 0.2736 0.3154 0.4493 0.259 Uiso 1 1 calc R . .
H58B H 0.3677 0.2689 0.3857 0.259 Uiso 1 1 calc R . .
H58C H 0.2926 0.3406 0.3538 0.259 Uiso 1 1 calc R . .
C57 C 0.4334(8) 0.3928(7) 0.4826(6) 0.120(5) Uani 1 1 d . . .
H57A H 0.3826 0.3870 0.5344 0.180 Uiso 1 1 calc R . .
H57B H 0.4641 0.4419 0.4817 0.180 Uiso 1 1 calc R . .
H57C H 0.4795 0.3375 0.4763 0.180 Uiso 1 1 calc R . .
C27 C 0.8699(8) 0.4524(8) 0.2770(7) 0.123(5) Uani 1 1 d . . .
H27A H 0.8962 0.4355 0.3216 0.185 Uiso 1 1 calc R . .
H27B H 0.8432 0.5160 0.2751 0.185 Uiso 1 1 calc R . .
H27C H 0.9197 0.4400 0.2255 0.185 Uiso 1 1 calc R . .
C19 C 1.0812(7) 0.8211(8) -0.0416(8) 0.133(6) Uani 1 1 d . . .
H19A H 1.1068 0.8715 -0.0367 0.200 Uiso 1 1 calc R . .
H19B H 1.0867 0.8204 -0.0984 0.200 Uiso 1 1 calc R . .
H19C H 1.1165 0.7656 -0.0233 0.200 Uiso 1 1 calc R . .
C29 C 0.6867(8) 0.4018(8) 0.3940(5) 0.114(4) Uani 1 1 d . . .
H29A H 0.7164 0.3851 0.4365 0.171 Uiso 1 1 calc R . .
H29B H 0.6410 0.3634 0.4026 0.171 Uiso 1 1 calc R . .
H29C H 0.6546 0.4639 0.3962 0.171 Uiso 1 1 calc R . .
C49 C 0.3741(8) 1.0472(7) 0.5379(7) 0.109(4) Uani 1 1 d . . .
H49A H 0.4150 1.0687 0.5594 0.163 Uiso 1 1 calc R . .
H49B H 0.3264 1.0970 0.5276 0.163 Uiso 1 1 calc R . .
H49C H 0.4118 1.0214 0.4870 0.163 Uiso 1 1 calc R . .
C39 C 0.2187(10) 1.1427(7) 0.3138(8) 0.140(6) Uani 1 1 d . . .
H39A H 0.2329 1.2029 0.3032 0.209 Uiso 1 1 calc R . .
H39B H 0.2709 1.1005 0.3260 0.209 Uiso 1 1 calc R . .
H39C H 0.1610 1.1401 0.3603 0.209 Uiso 1 1 calc R . .
C38 C 0.1005(8) 1.1914(7) 0.2075(7) 0.120(4) Uani 1 1 d . . .
H38A H 0.1136 1.2520 0.1960 0.180 Uiso 1 1 calc R . .
H38B H 0.0454 1.1876 0.2563 0.180 Uiso 1 1 calc R . .
H38C H 0.0880 1.1759 0.1613 0.180 Uiso 1 1 calc R . .
C37 C 0.3041(8) 1.1266(8) 0.1336(7) 0.132(5) Uani 1 1 d . . .
H37A H 0.3152 1.1878 0.1250 0.199 Uiso 1 1 calc R . .
H37B H 0.2921 1.1133 0.0863 0.199 Uiso 1 1 calc R . .
H37C H 0.3596 1.0855 0.1409 0.199 Uiso 1 1 calc R . .
O1A O 0.7586 0.4195 -0.1922 0.132 Uiso 0.30 1 d P . .
O1B O 0.8050 0.4531 -0.1349 0.089 Uiso 0.30 1 d P . .
C61 C 0.8573 0.5132 -0.2443 0.177 Uiso 0.60 1 d P . .
C62 C 0.9012 0.4334 -0.2158 0.191 Uiso 0.60 1 d P . .
C60 C 0.7774 0.4947 -0.2241 0.144 Uiso 0.60 1 d P . .
C63 C 0.8224 0.3891 -0.1674 0.220 Uiso 0.60 1 d P . .
O2 O 0.082(3) 0.316(3) 0.559(3) 0.152(14) Uiso 0.25 1 d P . .
C68 C 0.081(5) 0.338(4) 0.621(4) 0.14(2) Uiso 0.25 1 d P . .
C65 C 0.119(4) 0.227(4) 0.565(4) 0.14(2) Uiso 0.25 1 d P . .
C67 C 0.154(4) 0.322(4) 0.646(3) 0.110(16) Uiso 0.25 1 d P . .
C66 C 0.152(5) 0.259(5) 0.629(4) 0.16(3) Uiso 0.25 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
Se1 S3 2.4579(19) . ?
Se1 S5 2.503(2) . ?
Se1 V1 2.5067(14) . ?
Se1 V2 2.5127(13) . ?
Se3 Se2 2.2640(11) . ?
Se3 V2 2.5273(14) . ?
Se3 V1 2.5602(13) . ?
Se2 V1 2.5229(13) . ?
Se2 V2 2.5598(14) . ?
V2 S4 2.326(2) . ?
V2 S6 2.375(2) . ?
V2 P2 2.377(2) . ?
V2 S5 2.518(2) . ?
V2 V1 3.0808(15) . ?
V1 S1 2.330(2) . ?
V1 P1 2.3740(19) . ?
V1 S2 2.377(2) . ?
V1 S3 2.515(2) . ?
P1 C1 1.790(7) . ?
P1 C21 1.795(7) . ?
P1 C11 1.808(8) . ?
S3 C2 1.794(6) . ?
P2 C51 1.799(8) . ?
P2 C31 1.806(7) . ?
P2 C41 1.809(7) . ?
S1 C12 1.780(6) . ?
S5 C52 1.770(7) . ?
S4 C42 1.791(7) . ?
S2 C22 1.775(7) . ?
S6 C32 1.762(7) . ?
Si2 C7 1.844(9) . ?
Si2 C9 1.845(9) . ?
Si2 C8 1.861(8) . ?
Si2 C3 1.886(7) . ?
Si3 C27 1.822(12) . ?
Si3 C29 1.854(9) . ?
Si3 C28 1.861(9) . ?
Si3 C23 1.894(8) . ?
Si4 C49 1.856(11) . ?
Si4 C47 1.871(9) . ?
Si4 C48 1.872(10) . ?
Si4 C43 1.901(8) . ?
Si1 C17 1.797(12) . ?
Si1 C18 1.846(10) . ?
Si1 C19 1.874(10) . ?
Si1 C13 1.904(8) . ?
Si5 C37 1.825(11) . ?
Si5 C38 1.832(10) . ?
Si5 C39 1.832(11) . ?
Si5 C33 1.886(9) . ?
Si6 C59 1.850(10) . ?
Si6 C57 1.858(10) . ?
Si6 C58 1.889(12) . ?
Si6 C53 1.890(8) . ?
C41 C42 1.381(10) . ?
C41 C46 1.394(9) . ?
C42 C43 1.391(9) . ?
C11 C12 1.390(9) . ?
C11 C16 1.398(9) . ?
C12 C13 1.400(10) . ?
C1 C2 1.388(9) . ?
C1 C6 1.417(9) . ?
C52 C51 1.401(10) . ?
C52 C53 1.423(10) . ?
C31 C36 1.371(10) . ?
C31 C32 1.402(10) . ?
C2 C3 1.418(9) . ?
C16 C15 1.343(11) . ?
C13 C14 1.394(9) . ?
C43 C44 1.416(10) . ?
C32 C33 1.416(9) . ?
C3 C4 1.385(9) . ?
C33 C34 1.378(11) . ?
C22 C21 1.391(9) . ?
C22 C23 1.410(9) . ?
C23 C24 1.403(10) . ?
C56 C55 1.346(11) . ?
C56 C51 1.417(11) . ?
C21 C26 1.384(9) . ?
C26 C25 1.392(10) . ?
C4 C5 1.391(11) . ?
C46 C45 1.378(10) . ?
C15 C14 1.393(11) . ?
C34 C35 1.378(12) . ?
C6 C5 1.381(11) . ?
C35 C36 1.369(11) . ?
C24 C25 1.387(11) . ?
C45 C44 1.397(11) . ?
C53 C54 1.417(12) . ?
C54 C55 1.380(12) . ?
O1A C63 1.1874 . ?
O1A C60 1.2541 . ?
O1A O1B 1.6341 . ?
O1B C63 1.1649 . ?
O1B C62 1.6740 . ?
O1B C60 1.7545 . ?
C61 C60 1.2431 . ?
C61 C62 1.3764 . ?
C62 C63 1.4583 . ?
C62 C60 1.9771 . ?
C60 C63 1.8930 . ?
O2 C68 1.20(6) . ?
O2 C65 1.38(6) . ?
O2 C66 1.90(8) . ?
C68 C67 1.30(7) . ?
C68 C66 1.47(9) . ?
C68 C65 2.01(9) . ?
C65 C66 1.58(8) . ?
C67 C66 1.08(8) . ?

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
S3 Se1 S5 152.84(7) . . ?
S3 Se1 V1 60.86(5) . . ?
S5 Se1 V1 96.94(6) . . ?
S3 Se1 V2 96.93(5) . . ?
S5 Se1 V2 60.27(5) . . ?
V1 Se1 V2 75.73(4) . . ?
Se2 Se3 V2 64.31(4) . . ?
Se2 Se3 V1 62.71(4) . . ?
V2 Se3 V1 74.54(4) . . ?
Se3 Se2 V1 64.40(4) . . ?
Se3 Se2 V2 62.84(4) . . ?
V1 Se2 V2 74.62(4) . . ?
S4 V2 S6 99.59(8) . . ?
S4 V2 P2 81.27(7) . . ?
S6 V2 P2 75.03(7) . . ?
S4 V2 Se1 157.84(7) . . ?
S6 V2 Se1 98.18(6) . . ?
P2 V2 Se1 90.67(6) . . ?
S4 V2 S5 98.32(8) . . ?
S6 V2 S5 144.48(8) . . ?
P2 V2 S5 77.72(7) . . ?
Se1 V2 S5 59.67(5) . . ?
S4 V2 Se3 98.58(7) . . ?
S6 V2 Se3 74.71(6) . . ?
P2 V2 Se3 149.26(7) . . ?
Se1 V2 Se3 98.80(4) . . ?
S5 V2 Se3 132.07(6) . . ?
S4 V2 Se2 81.69(6) . . ?
S6 V2 Se2 126.77(7) . . ?
P2 V2 Se2 154.41(7) . . ?
Se1 V2 Se2 98.09(4) . . ?
S5 V2 Se2 86.04(6) . . ?
Se3 V2 Se2 52.85(3) . . ?
S4 V2 V1 133.69(7) . . ?
S6 V2 V1 105.18(6) . . ?
P2 V2 V1 142.67(6) . . ?
Se1 V2 V1 52.05(3) . . ?
S5 V2 V1 83.46(5) . . ?
Se3 V2 V1 53.22(3) . . ?
Se2 V2 V1 52.14(3) . . ?
S1 V1 P1 80.95(7) . . ?
S1 V1 S2 101.24(8) . . ?
P1 V1 S2 74.76(7) . . ?
S1 V1 Se1 155.57(7) . . ?
P1 V1 Se1 90.25(6) . . ?
S2 V1 Se1 98.30(7) . . ?
S1 V1 S3 97.13(8) . . ?
P1 V1 S3 77.99(7) . . ?
S2 V1 S3 144.03(8) . . ?
Se1 V1 S3 58.61(5) . . ?
S1 V1 Se2 99.79(6) . . ?
P1 V1 Se2 149.63(7) . . ?
S2 V1 Se2 75.34(6) . . ?
Se1 V1 Se2 99.23(5) . . ?
S3 V1 Se2 131.37(6) . . ?
S1 V1 Se3 81.48(6) . . ?
P1 V1 Se3 154.14(7) . . ?
S2 V1 Se3 127.48(7) . . ?
Se1 V1 Se3 98.09(4) . . ?
S3 V1 Se3 85.55(5) . . ?
Se2 V1 Se3 52.89(3) . . ?
S1 V1 V2 133.69(6) . . ?
P1 V1 V2 142.42(7) . . ?
S2 V1 V2 105.43(6) . . ?
Se1 V1 V2 52.22(3) . . ?
S3 V1 V2 82.69(5) . . ?
Se2 V1 V2 53.24(3) . . ?
Se3 V1 V2 52.24(3) . . ?
C1 P1 C21 110.3(3) . . ?
C1 P1 C11 107.7(3) . . ?
C21 P1 C11 101.2(3) . . ?
C1 P1 V1 115.0(2) . . ?
C21 P1 V1 113.5(2) . . ?
C11 P1 V1 108.1(2) . . ?
C2 S3 Se1 105.1(2) . . ?
C2 S3 V1 110.7(2) . . ?
Se1 S3 V1 60.53(5) . . ?
C51 P2 C31 110.0(4) . . ?
C51 P2 C41 107.6(3) . . ?
C31 P2 C41 101.8(3) . . ?
C51 P2 V2 115.4(3) . . ?
C31 P2 V2 113.1(2) . . ?
C41 P2 V2 107.8(3) . . ?
C12 S1 V1 109.3(3) . . ?
C52 S5 Se1 103.6(2) . . ?
C52 S5 V2 110.7(2) . . ?
Se1 S5 V2 60.06(5) . . ?
C42 S4 V2 109.6(2) . . ?
C22 S2 V1 113.0(2) . . ?
C32 S6 V2 112.8(2) . . ?
C7 Si2 C9 113.6(5) . . ?
C7 Si2 C8 108.3(4) . . ?
C9 Si2 C8 107.9(5) . . ?
C7 Si2 C3 108.9(4) . . ?
C9 Si2 C3 110.2(4) . . ?
C8 Si2 C3 107.7(3) . . ?
C27 Si3 C29 111.4(6) . . ?
C27 Si3 C28 108.2(6) . . ?
C29 Si3 C28 107.0(5) . . ?
C27 Si3 C23 110.1(4) . . ?
C29 Si3 C23 112.0(4) . . ?
C28 Si3 C23 108.0(4) . . ?
C49 Si4 C47 109.9(5) . . ?
C49 Si4 C48 110.3(5) . . ?
C47 Si4 C48 107.2(5) . . ?
C49 Si4 C43 107.8(4) . . ?
C47 Si4 C43 108.0(4) . . ?
C48 Si4 C43 113.6(4) . . ?
C17 Si1 C18 109.9(6) . . ?
C17 Si1 C19 107.0(6) . . ?
C18 Si1 C19 110.0(6) . . ?
C17 Si1 C13 111.2(5) . . ?
C18 Si1 C13 110.8(4) . . ?
C19 Si1 C13 107.9(4) . . ?
C37 Si5 C38 107.9(6) . . ?
C37 Si5 C39 111.4(7) . . ?
C38 Si5 C39 107.4(6) . . ?
C37 Si5 C33 112.5(5) . . ?
C38 Si5 C33 108.7(5) . . ?
C39 Si5 C33 108.7(5) . . ?
C59 Si6 C57 113.4(5) . . ?
C59 Si6 C58 107.0(6) . . ?
C57 Si6 C58 111.8(7) . . ?
C59 Si6 C53 111.7(4) . . ?
C57 Si6 C53 106.7(4) . . ?
C58 Si6 C53 106.1(5) . . ?
C42 C41 C46 119.8(6) . . ?
C42 C41 P2 117.7(5) . . ?
C46 C41 P2 122.5(6) . . ?
C41 C42 C43 122.9(7) . . ?
C41 C42 S4 118.1(5) . . ?
C43 C42 S4 119.0(6) . . ?
C12 C11 C16 119.3(7) . . ?
C12 C11 P1 116.2(5) . . ?
C16 C11 P1 124.5(6) . . ?
C11 C12 C13 120.8(6) . . ?
C11 C12 S1 119.1(5) . . ?
C13 C12 S1 120.0(5) . . ?
C2 C1 C6 118.7(6) . . ?
C2 C1 P1 117.9(5) . . ?
C6 C1 P1 123.3(5) . . ?
C51 C52 C53 120.7(7) . . ?
C51 C52 S5 119.4(6) . . ?
C53 C52 S5 119.7(6) . . ?
C36 C31 C32 120.8(7) . . ?
C36 C31 P2 130.2(6) . . ?
C32 C31 P2 108.0(5) . . ?
C1 C2 C3 123.1(6) . . ?
C1 C2 S3 118.2(5) . . ?
C3 C2 S3 118.7(5) . . ?
C15 C16 C11 121.0(7) . . ?
C14 C13 C12 117.4(7) . . ?
C14 C13 Si1 118.5(6) . . ?
C12 C13 Si1 124.1(5) . . ?
C42 C43 C44 115.5(7) . . ?
C42 C43 Si4 126.5(6) . . ?
C44 C43 Si4 117.8(6) . . ?
C31 C32 C33 120.6(7) . . ?
C31 C32 S6 119.2(5) . . ?
C33 C32 S6 120.1(6) . . ?
C4 C3 C2 115.6(7) . . ?
C4 C3 Si2 118.3(5) . . ?
C2 C3 Si2 126.0(5) . . ?
C34 C33 C32 114.7(7) . . ?
C34 C33 Si5 121.1(6) . . ?
C32 C33 Si5 123.3(6) . . ?
C21 C22 C23 120.3(6) . . ?
C21 C22 S2 118.3(5) . . ?
C23 C22 S2 121.4(5) . . ?
C24 C23 C22 116.1(7) . . ?
C24 C23 Si3 119.8(6) . . ?
C22 C23 Si3 124.0(6) . . ?
C55 C56 C51 119.4(8) . . ?
C26 C21 C22 121.2(7) . . ?
C26 C21 P1 128.7(6) . . ?
C22 C21 P1 109.4(5) . . ?
C52 C51 C56 120.2(7) . . ?
C52 C51 P2 116.1(6) . . ?
C56 C51 P2 123.7(6) . . ?
C21 C26 C25 119.6(8) . . ?
C3 C4 C5 122.9(7) . . ?
C45 C46 C41 120.3(7) . . ?
C16 C15 C14 119.8(7) . . ?
C33 C34 C35 124.4(8) . . ?
C5 C6 C1 119.2(7) . . ?
C36 C35 C34 119.4(8) . . ?
C25 C24 C23 123.6(7) . . ?
C24 C25 C26 118.4(7) . . ?
C46 C45 C44 118.7(7) . . ?
C45 C44 C43 122.9(7) . . ?
C35 C36 C31 119.0(8) . . ?
C54 C53 C52 116.0(7) . . ?
C54 C53 Si6 117.5(6) . . ?
C52 C53 Si6 126.4(6) . . ?
C55 C54 C53 122.3(8) . . ?
C56 C55 C54 121.4(9) . . ?
C15 C14 C13 121.7(8) . . ?
C6 C5 C4 120.5(7) . . ?
C63 O1A C60 101.6 . . ?
C63 O1A O1B 45.4 . . ?
C60 O1A O1B 73.5 . . ?
C63 O1B O1A 46.6 . . ?
C63 O1B C62 58.6 . . ?
O1A O1B C62 80.8 . . ?
C63 O1B C60 78.0 . . ?
O1A O1B C60 43.3 . . ?
C62 O1B C60 70.4 . . ?
C60 C61 C62 97.9 . . ?
C61 C62 C63 102.6 . . ?
C61 C62 O1B 79.8 . . ?
C63 C62 O1B 43.0 . . ?
C61 C62 C60 38.5 . . ?
C63 C62 C60 64.8 . . ?
O1B C62 C60 56.7 . . ?
C61 C60 O1A 123.3 . . ?
C61 C60 O1B 80.2 . . ?
O1A C60 O1B 63.3 . . ?
C61 C60 C63 87.2 . . ?
O1A C60 C63 37.9 . . ?
O1B C60 C63 37.0 . . ?
C61 C60 C62 43.6 . . ?
O1A C60 C62 79.8 . . ?
O1B C60 C62 52.9 . . ?
C63 C60 C62 44.2 . . ?
O1B C63 O1A 88.0 . . ?
O1B C63 C62 78.4 . . ?
O1A C63 C62 107.9 . . ?
O1B C63 C60 65.0 . . ?
O1A C63 C60 40.5 . . ?
C62 C63 C60 71.0 . . ?
C68 O2 C65 103(5) . . ?
C68 O2 C66 51(4) . . ?
C65 O2 C66 55(3) . . ?
O2 C68 C67 124(6) . . ?
O2 C68 C66 90(6) . . ?
C67 C68 C66 45(4) . . ?
O2 C68 C65 42(3) . . ?
C67 C68 C65 94(5) . . ?
C66 C68 C65 51(4) . . ?
O2 C65 C66 79(4) . . ?
O2 C65 C68 35(3) . . ?
C66 C65 C68 46(3) . . ?
C66 C67 C68 76(6) . . ?
C67 C66 C68 59(5) . . ?
C67 C66 C65 137(8) . . ?
C68 C66 C65 82(5) . . ?
C67 C66 O2 92(6) . . ?
C68 C66 O2 39(3) . . ?
C65 C66 O2 46(3) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.04
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.109
####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 990547'
_audit_update_record             
;
2014-03-07 deposited with the CCDC.
2015-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[V2(PS3")2(mu-S2)(mu-S)]'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63.50 H95 O4 P2 S9 Si6 V2'
_chemical_formula_weight         1543.30

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   14.3175(5)
_cell_length_b                   16.3327(6)
_cell_length_c                   19.5112(7)
_cell_angle_alpha                81.827(2)
_cell_angle_beta                 88.006(2)
_cell_angle_gamma                64.137(2)
_cell_volume                     4062.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    45567
_cell_measurement_theta_min      1.05
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            dark-brown
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1624
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45567
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             14146
_reflns_number_gt                9894
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of 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 isotropic restraints 
 are used to the C16, O1, C44 and C55 atoms. To avoid the short inter H...H 
 contact, the distance of H60B-H44F was restrained to 2.20 %A. 
;

_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)+(0.1015P)²+5.9310P] 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         14146
_refine_ls_number_parameters     790
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1962
_refine_ls_wR_factor_gt          0.1731
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.008
_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
V1 V 0.25297(6) 0.31922(6) 0.83776(4) 0.0293(2) Uani 1 1 d . . .
V2 V 0.45806(6) 0.32940(6) 0.82111(4) 0.0298(2) Uani 1 1 d . . .
S1 S 0.16820(9) 0.30073(9) 0.93791(6) 0.0333(3) Uani 1 1 d . . .
S2 S 0.12797(10) 0.44887(9) 0.76867(7) 0.0363(3) Uani 1 1 d . . .
S7 S 0.38283(10) 0.25585(9) 0.75539(7) 0.0347(3) Uani 1 1 d . . .
S3 S 0.37702(10) 0.15571(9) 0.83478(7) 0.0369(3) Uani 1 1 d . . .
S4 S 0.51954(10) 0.42625(9) 0.85841(7) 0.0354(3) Uani 1 1 d . . .
S5 S 0.41095(10) 0.41180(9) 0.70134(7) 0.0385(3) Uani 1 1 d . . .
S6 S 0.56760(10) 0.19319(9) 0.89237(7) 0.0391(3) Uani 1 1 d . . .
S8 S 0.29043(9) 0.44277(9) 0.85389(7) 0.0337(3) Uani 1 1 d . . .
S9 S 0.36367(9) 0.33022(9) 0.92386(6) 0.0332(3) Uani 1 1 d . . .
P1 P 0.14333(10) 0.26205(9) 0.79164(7) 0.0330(3) Uani 1 1 d . . .
P2 P 0.61448(10) 0.28172(9) 0.75837(7) 0.0331(3) Uani 1 1 d . . .
Si1 Si 0.00264(11) 0.29763(11) 1.06539(7) 0.0382(4) Uani 1 1 d . . .
Si2 Si -0.03474(12) 0.61530(12) 0.64958(8) 0.0474(4) Uani 1 1 d . . .
Si3 Si 0.5243(10) -0.0545(9) 0.7829(5) 0.0466(16) Uani 0.542(9) 1 d P A 1
Si3' Si 0.5305(13) -0.0668(11) 0.8081(5) 0.0466(16) Uani 0.458(9) 1 d P A 2
Si4 Si 0.64431(12) 0.54674(11) 0.89975(8) 0.0399(4) Uani 1 1 d . . .
Si5 Si 0.3408(10) 0.4575(7) 0.5323(6) 0.051(2) Uani 0.542(9) 1 d P A 1
Si5' Si 0.3474(12) 0.4232(9) 0.5269(8) 0.051(2) Uani 0.458(9) 1 d P A 2
Si6 Si 0.75567(12) 0.04150(10) 1.00261(9) 0.0452(4) Uani 1 1 d . . .
C1 C 0.0418(4) 0.2695(3) 0.8527(3) 0.0325(11) Uani 1 1 d . . .
C2 C 0.0593(4) 0.2825(3) 0.9193(3) 0.0324(11) Uani 1 1 d . . .
C3 C -0.0113(4) 0.2819(3) 0.9726(3) 0.0348(12) Uani 1 1 d . . .
C4 C -0.0963(4) 0.2688(4) 0.9532(3) 0.0386(12) Uani 1 1 d . . .
H4 H -0.1444 0.2672 0.9876 0.046 Uiso 1 1 calc R . .
C5 C -0.1142(4) 0.2579(4) 0.8868(3) 0.0398(13) Uani 1 1 d . . .
H5 H -0.1740 0.2502 0.8763 0.048 Uiso 1 1 calc R . .
C6 C -0.0455(4) 0.2583(3) 0.8356(3) 0.0355(12) Uani 1 1 d . . .
H6 H -0.0572 0.2511 0.7896 0.043 Uiso 1 1 calc R . .
C7 C -0.0198(5) 0.4180(4) 1.0690(3) 0.0486(14) Uani 1 1 d . . .
H7A H -0.0196 0.4276 1.1174 0.073 Uiso 1 1 calc R . .
H7B H -0.0872 0.4605 1.0466 0.073 Uiso 1 1 calc R . .
H7C H 0.0354 0.4294 1.0448 0.073 Uiso 1 1 calc R . .
C8 C 0.1316(4) 0.2131(4) 1.1054(3) 0.0442(14) Uani 1 1 d . . .
H8A H 0.1867 0.2252 1.0816 0.066 Uiso 1 1 calc R . .
H8B H 0.1422 0.1506 1.1009 0.066 Uiso 1 1 calc R . .
H8C H 0.1335 0.2191 1.1545 0.066 Uiso 1 1 calc R . .
C9 C -0.0983(5) 0.2748(5) 1.1172(3) 0.0595(17) Uani 1 1 d . . .
H9A H -0.0894 0.2786 1.1660 0.089 Uiso 1 1 calc R . .
H9B H -0.0906 0.2132 1.1127 0.089 Uiso 1 1 calc R . .
H9C H -0.1675 0.3206 1.1000 0.089 Uiso 1 1 calc R . .
C10 C 0.2112(4) 0.1417(4) 0.7788(3) 0.0390(12) Uani 1 1 d . . .
C11 C 0.3179(4) 0.0976(4) 0.7924(3) 0.0396(13) Uani 1 1 d . A .
C12 C 0.3798(4) 0.0078(4) 0.7803(3) 0.0500(15) Uani 1 1 d . . .
C13 C 0.3276(5) -0.0377(4) 0.7565(4) 0.0563(16) Uani 1 1 d . A .
H13 H 0.3666 -0.0990 0.7474 0.068 Uiso 1 1 calc R . .
C14 C 0.2201(5) 0.0031(4) 0.7455(3) 0.0534(16) Uani 1 1 d . . .
H14 H 0.1865 -0.0309 0.7312 0.064 Uiso 1 1 calc R A .
C15 C 0.1629(4) 0.0936(4) 0.7557(3) 0.0466(14) Uani 1 1 d . A .
H15 H 0.0900 0.1228 0.7466 0.056 Uiso 1 1 calc R . .
C16 C 0.5919(14) 0.0190(12) 0.7517(9) 0.065(3) Uani 0.542(9) 1 d PU A 1
H16A H 0.5709 0.0697 0.7791 0.097 Uiso 0.542(9) 1 calc PR A 1
H16B H 0.5728 0.0440 0.7028 0.097 Uiso 0.542(9) 1 calc PR A 1
H16C H 0.6672 -0.0182 0.7567 0.097 Uiso 0.542(9) 1 calc PR A 1
C17 C 0.566(3) -0.148(2) 0.7277(9) 0.056(4) Uani 0.542(9) 1 d P A 1
H17A H 0.5282 -0.1858 0.7406 0.084 Uiso 0.542(9) 1 calc PR A 1
H17B H 0.6407 -0.1873 0.7347 0.084 Uiso 0.542(9) 1 calc PR A 1
H17C H 0.5505 -0.1216 0.6789 0.084 Uiso 0.542(9) 1 calc PR A 1
C18 C 0.557(5) -0.102(3) 0.878(3) 0.080(9) Uani 0.542(9) 1 d P A 1
H18A H 0.5193 -0.1384 0.8934 0.121 Uiso 0.542(9) 1 calc PR A 1
H18B H 0.5365 -0.0508 0.9048 0.121 Uiso 0.542(9) 1 calc PR A 1
H18C H 0.6318 -0.1405 0.8840 0.121 Uiso 0.542(9) 1 calc PR A 1
C16' C 0.6044(16) 0.0046(14) 0.7893(10) 0.065(3) Uani 0.458(9) 1 d P A 2
H16D H 0.6774 -0.0328 0.8038 0.097 Uiso 0.458(9) 1 calc PR A 2
H16E H 0.5746 0.0574 0.8148 0.097 Uiso 0.458(9) 1 calc PR A 2
H16F H 0.5997 0.0264 0.7395 0.097 Uiso 0.458(9) 1 calc PR A 2
C17' C 0.575(3) -0.160(3) 0.7564(11) 0.056(4) Uani 0.458(9) 1 d P A 2
H17D H 0.6486 -0.2000 0.7671 0.084 Uiso 0.458(9) 1 calc PR A 2
H17E H 0.5655 -0.1345 0.7071 0.084 Uiso 0.458(9) 1 calc PR A 2
H17F H 0.5346 -0.1953 0.7669 0.084 Uiso 0.458(9) 1 calc PR A 2
C18' C 0.556(6) -0.125(4) 0.897(4) 0.080(9) Uani 0.458(9) 1 d P A 2
H18D H 0.6307 -0.1600 0.9057 0.121 Uiso 0.458(9) 1 calc PR A 2
H18E H 0.5231 -0.1676 0.9036 0.121 Uiso 0.458(9) 1 calc PR A 2
H18F H 0.5265 -0.0798 0.9288 0.121 Uiso 0.458(9) 1 calc PR A 2
C19 C 0.0790(4) 0.3292(4) 0.7106(3) 0.0349(12) Uani 1 1 d . . .
C20 C 0.0640(4) 0.4202(4) 0.7067(2) 0.0364(12) Uani 1 1 d . . .
C21 C 0.0031(4) 0.4891(4) 0.6525(3) 0.0400(13) Uani 1 1 d . . .
C22 C -0.0327(4) 0.4574(4) 0.6007(3) 0.0463(15) Uani 1 1 d . . .
H22 H -0.0728 0.5008 0.5629 0.056 Uiso 1 1 calc R . .
C23 C -0.0130(4) 0.3667(5) 0.6017(3) 0.0489(15) Uani 1 1 d . . .
H23 H -0.0366 0.3486 0.5642 0.059 Uiso 1 1 calc R . .
C24 C 0.0417(4) 0.3014(4) 0.6579(3) 0.0443(14) Uani 1 1 d . . .
H24 H 0.0531 0.2393 0.6600 0.053 Uiso 1 1 calc R . .
C25 C -0.1087(6) 0.6555(5) 0.7278(3) 0.0649(18) Uani 1 1 d . . .
H25A H -0.0640 0.6238 0.7693 0.097 Uiso 1 1 calc R . .
H25B H -0.1691 0.6419 0.7302 0.097 Uiso 1 1 calc R . .
H25C H -0.1321 0.7219 0.7252 0.097 Uiso 1 1 calc R . .
C26 C 0.0779(5) 0.6424(5) 0.6405(5) 0.085(3) Uani 1 1 d . . .
H26A H 0.0540 0.7089 0.6378 0.128 Uiso 1 1 calc R . .
H26B H 0.1142 0.6217 0.5982 0.128 Uiso 1 1 calc R . .
H26C H 0.1255 0.6109 0.6807 0.128 Uiso 1 1 calc R . .
C27 C -0.1239(6) 0.6789(5) 0.5726(3) 0.073(2) Uani 1 1 d . . .
H27A H -0.1444 0.7449 0.5703 0.110 Uiso 1 1 calc R . .
H27B H -0.1859 0.6677 0.5769 0.110 Uiso 1 1 calc R . .
H27C H -0.0881 0.6575 0.5304 0.110 Uiso 1 1 calc R . .
C28 C 0.6627(4) 0.3680(3) 0.7578(2) 0.0326(11) Uani 1 1 d . . .
C29 C 0.6273(4) 0.4246(3) 0.8100(3) 0.0328(11) Uani 1 1 d . . .
C30 C 0.6729(4) 0.4815(3) 0.8230(3) 0.0343(12) Uani 1 1 d . . .
C31 C 0.7510(4) 0.4826(4) 0.7782(3) 0.0394(13) Uani 1 1 d . . .
H31 H 0.7839 0.5203 0.7854 0.047 Uiso 1 1 calc R . .
C32 C 0.7823(4) 0.4317(4) 0.7241(3) 0.0435(14) Uani 1 1 d . . .
H32 H 0.8332 0.4373 0.6937 0.052 Uiso 1 1 calc R . .
C33 C 0.7400(4) 0.3721(4) 0.7137(3) 0.0395(13) Uani 1 1 d . . .
H33 H 0.7630 0.3352 0.6776 0.047 Uiso 1 1 calc R . .
C34 C 0.6605(5) 0.4670(4) 0.9812(3) 0.0488(14) Uani 1 1 d . . .
H34A H 0.6122 0.5002 1.0154 0.073 Uiso 1 1 calc R . .
H34B H 0.7319 0.4425 0.9995 0.073 Uiso 1 1 calc R . .
H34C H 0.6460 0.4163 0.9718 0.073 Uiso 1 1 calc R . .
C35 C 0.5116(5) 0.6433(4) 0.8941(3) 0.0557(16) Uani 1 1 d . . .
H35A H 0.4602 0.6196 0.8903 0.084 Uiso 1 1 calc R . .
H35B H 0.5053 0.6881 0.8533 0.084 Uiso 1 1 calc R . .
H35C H 0.4995 0.6732 0.9359 0.084 Uiso 1 1 calc R . .
C36 C 0.7404(6) 0.5954(5) 0.9001(4) 0.0661(19) Uani 1 1 d . . .
H36A H 0.7283 0.6411 0.8588 0.099 Uiso 1 1 calc R . .
H36B H 0.8109 0.5460 0.8998 0.099 Uiso 1 1 calc R . .
H36C H 0.7324 0.6248 0.9417 0.099 Uiso 1 1 calc R . .
C37 C 0.5947(4) 0.2738(4) 0.6691(3) 0.0409(13) Uani 1 1 d . . .
C38 C 0.4972(4) 0.3412(4) 0.6430(3) 0.0432(13) Uani 1 1 d . A .
C39 C 0.4702(4) 0.3518(5) 0.5724(3) 0.0568(18) Uani 1 1 d . . .
C40 C 0.5427(5) 0.2873(6) 0.5334(3) 0.075(2) Uani 1 1 d . A .
H40 H 0.5268 0.2927 0.4857 0.090 Uiso 1 1 calc R . .
C41 C 0.6359(5) 0.2166(6) 0.5604(4) 0.079(2) Uani 1 1 d . . .
H41 H 0.6805 0.1732 0.5323 0.095 Uiso 1 1 calc R A .
C42 C 0.6625(5) 0.2105(5) 0.6290(3) 0.0567(17) Uani 1 1 d . A .
H42 H 0.7265 0.1634 0.6485 0.068 Uiso 1 1 calc R . .
C43 C 0.328(3) 0.5760(13) 0.543(2) 0.070(6) Uani 0.542(9) 1 d P A 1
H43A H 0.2619 0.6231 0.5213 0.105 Uiso 0.542(9) 1 calc PR A 1
H43B H 0.3855 0.5851 0.5200 0.105 Uiso 0.542(9) 1 calc PR A 1
H43C H 0.3298 0.5809 0.5920 0.105 Uiso 0.542(9) 1 calc PR A 1
C44 C 0.3425(14) 0.4511(12) 0.4372(8) 0.069(4) Uani 0.542(9) 1 d PU A 1
H44A H 0.2796 0.5014 0.4145 0.103 Uiso 0.542(9) 1 calc PR A 1
H44B H 0.3449 0.3921 0.4298 0.103 Uiso 0.542(9) 1 calc PR A 1
H44C H 0.4038 0.4565 0.4175 0.103 Uiso 0.542(9) 1 calc PR A 1
C45 C 0.232(3) 0.4381(18) 0.568(2) 0.050(5) Uani 0.542(9) 1 d P A 1
H45A H 0.1663 0.4889 0.5490 0.074 Uiso 0.542(9) 1 calc PR A 1
H45B H 0.2334 0.4348 0.6187 0.074 Uiso 0.542(9) 1 calc PR A 1
H45C H 0.2363 0.3802 0.5561 0.074 Uiso 0.542(9) 1 calc PR A 1
C43' C 0.334(3) 0.5413(16) 0.534(2) 0.070(6) Uani 0.458(9) 1 d P A 2
H43D H 0.3933 0.5488 0.5116 0.105 Uiso 0.458(9) 1 calc PR A 2
H43E H 0.3335 0.5493 0.5824 0.105 Uiso 0.458(9) 1 calc PR A 2
H43F H 0.2695 0.5875 0.5101 0.105 Uiso 0.458(9) 1 calc PR A 2
C44' C 0.3521(18) 0.4041(13) 0.4324(10) 0.069(4) Uani 0.458(9) 1 d P A 2
H44D H 0.4097 0.4135 0.4102 0.103 Uiso 0.458(9) 1 calc PR A 2
H44E H 0.2866 0.4477 0.4083 0.103 Uiso 0.458(9) 1 calc PR A 2
H44F H 0.3623 0.3412 0.4302 0.103 Uiso 0.458(9) 1 calc PRD A 2
C45' C 0.236(4) 0.405(2) 0.571(3) 0.050(5) Uani 0.458(9) 1 d P A 2
H45D H 0.2316 0.4193 0.6182 0.074 Uiso 0.458(9) 1 calc PR A 2
H45E H 0.2482 0.3415 0.5712 0.074 Uiso 0.458(9) 1 calc PR A 2
H45F H 0.1710 0.4465 0.5450 0.074 Uiso 0.458(9) 1 calc PR A 2
C46 C 0.7198(4) 0.1764(3) 0.7981(3) 0.0371(12) Uani 1 1 d . . .
C47 C 0.6966(4) 0.1437(3) 0.8628(3) 0.0369(12) Uani 1 1 d . . .
C48 C 0.7748(4) 0.0731(3) 0.9074(3) 0.0405(13) Uani 1 1 d . . .
C49 C 0.8737(4) 0.0328(4) 0.8792(3) 0.0468(14) Uani 1 1 d . . .
H49 H 0.9276 -0.0170 0.9068 0.056 Uiso 1 1 calc R . .
C50 C 0.8960(4) 0.0615(4) 0.8142(3) 0.0471(14) Uani 1 1 d . . .
H50 H 0.9635 0.0306 0.7970 0.057 Uiso 1 1 calc R . .
C51 C 0.8203(4) 0.1354(4) 0.7736(3) 0.0413(13) Uani 1 1 d . . .
H51 H 0.8365 0.1582 0.7295 0.050 Uiso 1 1 calc R . .
C52 C 0.7055(5) 0.1467(4) 1.0469(3) 0.0604(17) Uani 1 1 d . . .
H52A H 0.6363 0.1899 1.0277 0.091 Uiso 1 1 calc R . .
H52B H 0.7526 0.1760 1.0393 0.091 Uiso 1 1 calc R . .
H52C H 0.7013 0.1293 1.0966 0.091 Uiso 1 1 calc R . .
C53 C 0.8849(5) -0.0375(4) 1.0447(4) 0.0641(18) Uani 1 1 d . . .
H53A H 0.8758 -0.0562 1.0935 0.096 Uiso 1 1 calc R . .
H53B H 0.9296 -0.0057 1.0416 0.096 Uiso 1 1 calc R . .
H53C H 0.9171 -0.0920 1.0211 0.096 Uiso 1 1 calc R . .
C54 C 0.6705(5) -0.0184(4) 1.0134(4) 0.0583(17) Uani 1 1 d . . .
H54A H 0.7050 -0.0774 0.9956 0.087 Uiso 1 1 calc R . .
H54B H 0.6047 0.0197 0.9876 0.087 Uiso 1 1 calc R . .
H54C H 0.6569 -0.0291 1.0626 0.087 Uiso 1 1 calc R . .
O1 O 0.3063(6) 0.7945(4) 0.6928(3) 0.125(2) Uani 1 1 d U . .
C55 C 0.3889(8) 0.7276(6) 0.6583(5) 0.101(3) Uani 1 1 d U . .
H55A H 0.4462 0.7456 0.6494 0.121 Uiso 1 1 calc R . .
H55B H 0.3632 0.7220 0.6136 0.121 Uiso 1 1 calc R . .
C56 C 0.4245(7) 0.6407(6) 0.7048(5) 0.093(3) Uani 1 1 d . . .
H56A H 0.4812 0.6327 0.7365 0.111 Uiso 1 1 calc R . .
H56B H 0.4489 0.5879 0.6784 0.111 Uiso 1 1 calc R . .
C57 C 0.3276(6) 0.6504(5) 0.7443(4) 0.070(2) Uani 1 1 d . . .
H57A H 0.2836 0.6314 0.7186 0.084 Uiso 1 1 calc R . .
H57B H 0.3457 0.6135 0.7908 0.084 Uiso 1 1 calc R . .
C58 C 0.2751(7) 0.7500(5) 0.7490(4) 0.078(2) Uani 1 1 d . . .
H58A H 0.1988 0.7722 0.7471 0.094 Uiso 1 1 calc R . .
H58B H 0.2952 0.7623 0.7931 0.094 Uiso 1 1 calc R . .
O2 O 0.3006(13) 0.1387(11) 0.5817(8) 0.264(6) Uiso 1 1 d . . .
C59 C 0.4090(18) 0.1284(16) 0.5891(12) 0.252(9) Uiso 1 1 d . . .
H59A H 0.4592 0.0655 0.6086 0.303 Uiso 1 1 calc R . .
H59B H 0.4138 0.1746 0.6147 0.303 Uiso 1 1 calc R . .
C60 C 0.414(2) 0.1491(14) 0.5123(12) 0.289(12) Uiso 1 1 d . . .
H60A H 0.4873 0.1249 0.4975 0.347 Uiso 1 1 calc R . .
H60B H 0.3789 0.2160 0.4964 0.347 Uiso 1 1 calc RD . .
C61 C 0.356(2) 0.0979(18) 0.4836(13) 0.293(12) Uiso 1 1 d . . .
H61A H 0.3041 0.1402 0.4476 0.352 Uiso 1 1 calc R . .
H61B H 0.4068 0.0450 0.4623 0.352 Uiso 1 1 calc R . .
C62 C 0.302(2) 0.0635(18) 0.5440(13) 0.296(12) Uiso 1 1 d . . .
H62A H 0.2318 0.0710 0.5313 0.356 Uiso 1 1 calc R . .
H62B H 0.3450 0.0005 0.5674 0.356 Uiso 1 1 calc R . .
O3 O 0.9706(6) 0.1320(6) 0.6297(4) 0.130(3) Uani 1 1 d . . .
H3 H 0.9910 0.0748 0.6351 0.195 Uiso 1 1 d R . .
C63 C 0.9316(9) 0.1696(9) 0.5620(6) 0.133(4) Uani 1 1 d . . .
H63A H 0.9057 0.1304 0.5437 0.200 Uiso 1 1 calc R . .
H63B H 0.9870 0.1737 0.5329 0.200 Uiso 1 1 calc R . .
H63C H 0.8747 0.2312 0.5621 0.200 Uiso 1 1 calc R . .
O4 O -0.0674(16) -0.0926(14) 0.6133(11) 0.182(7) Uiso 0.50 1 d P B 1
H4A H -0.0547 -0.0486 0.6058 0.273 Uiso 0.50 1 d PR B 1
C64 C -0.1218(19) -0.0802(17) 0.6765(13) 0.142(8) Uiso 0.50 1 d P B 1
H64A H -0.0739 -0.1183 0.7153 0.213 Uiso 0.50 1 calc PR B 1
H64B H -0.1784 -0.0983 0.6746 0.213 Uiso 0.50 1 calc PR B 1
H64C H -0.1505 -0.0154 0.6831 0.213 Uiso 0.50 1 calc PR B 1
O5 O 0.1108(13) -0.0680(11) 0.6074(8) 0.142(5) Uiso 0.50 1 d P C 2
H5A H 0.0750 -0.0739 0.6381 0.212 Uiso 0.50 1 d PR C 2
H5B H 0.1690 -0.1087 0.6082 0.212 Uiso 0.50 1 d PR C 2


_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
V1 S1 2.3173(15) . ?
V1 S2 2.3567(15) . ?
V1 S8 2.3653(15) . ?
V1 S7 2.3868(15) . ?
V1 P1 2.4004(15) . ?
V1 S9 2.4260(14) . ?
V1 S3 2.4877(15) . ?
V1 V2 3.0165(11) . ?
V2 S4 2.3223(15) . ?
V2 S6 2.3601(15) . ?
V2 S9 2.3767(15) . ?
V2 P2 2.3831(15) . ?
V2 S7 2.4312(15) . ?
V2 S8 2.4394(15) . ?
V2 S5 2.4801(15) . ?
S1 C2 1.768(5) . ?
S2 C20 1.770(5) . ?
S7 S3 2.1144(18) . ?
S3 C11 1.809(5) . ?
S4 C29 1.773(5) . ?
S5 C38 1.785(6) . ?
S6 C47 1.776(5) . ?
S8 S9 2.0116(17) . ?
P1 C19 1.811(5) . ?
P1 C1 1.820(5) . ?
P1 C10 1.825(6) . ?
P2 C37 1.806(5) . ?
P2 C46 1.809(5) . ?
P2 C28 1.819(5) . ?
Si1 C7 1.860(6) . ?
Si1 C8 1.869(5) . ?
Si1 C9 1.873(6) . ?
Si1 C3 1.893(5) . ?
Si2 C26 1.846(7) . ?
Si2 C25 1.857(7) . ?
Si2 C27 1.870(6) . ?
Si2 C21 1.881(6) . ?
Si3 C12 1.864(14) . ?
Si3 C18 1.89(5) . ?
Si3 C16 1.87(2) . ?
Si3 C17 1.87(3) . ?
Si3' C17' 1.81(4) . ?
Si3' C18' 1.82(6) . ?
Si3' C16' 1.88(3) . ?
Si3' C12 2.008(16) . ?
Si4 C34 1.857(6) . ?
Si4 C35 1.860(6) . ?
Si4 C36 1.866(6) . ?
Si4 C30 1.890(5) . ?
Si5 C45 1.82(4) . ?
Si5 C43 1.903(19) . ?
Si5 C44 1.871(19) . ?
Si5 C39 1.988(13) . ?
Si5' C39 1.807(16) . ?
Si5' C44' 1.91(2) . ?
Si5' C43' 1.88(2) . ?
Si5' C45' 1.89(5) . ?
Si6 C54 1.858(6) . ?
Si6 C53 1.867(6) . ?
Si6 C52 1.875(6) . ?
Si6 C48 1.899(6) . ?
C1 C2 1.395(7) . ?
C1 C6 1.398(7) . ?
C2 C3 1.426(7) . ?
C3 C4 1.399(7) . ?
C4 C5 1.380(7) . ?
C5 C6 1.380(7) . ?
C10 C15 1.376(8) . ?
C10 C11 1.391(7) . ?
C11 C12 1.394(8) . ?
C12 C13 1.390(8) . ?
C13 C14 1.395(8) . ?
C14 C15 1.382(8) . ?
C19 C24 1.390(7) . ?
C19 C20 1.398(7) . ?
C20 C21 1.419(7) . ?
C21 C22 1.404(8) . ?
C22 C23 1.379(8) . ?
C23 C24 1.396(8) . ?
C28 C33 1.397(7) . ?
C28 C29 1.402(7) . ?
C29 C30 1.401(7) . ?
C30 C31 1.400(7) . ?
C31 C32 1.377(8) . ?
C32 C33 1.391(8) . ?
C37 C42 1.387(8) . ?
C37 C38 1.403(8) . ?
C38 C39 1.409(8) . ?
C39 C40 1.408(9) . ?
C40 C41 1.387(10) . ?
C41 C42 1.383(9) . ?
C46 C47 1.386(7) . ?
C46 C51 1.397(7) . ?
C47 C48 1.414(7) . ?
C48 C49 1.405(8) . ?
C49 C50 1.365(8) . ?
C50 C51 1.380(8) . ?
O1 C58 1.397(8) . ?
O1 C55 1.439(10) . ?
C55 C56 1.459(11) . ?
C56 C57 1.521(10) . ?
C57 C58 1.480(10) . ?
O2 C59 1.50(2) . ?
O2 C62 1.51(2) . ?
C59 C60 1.50(2) . ?
C60 C61 1.57(3) . ?
C61 C62 1.57(3) . ?
O3 C63 1.398(12) . ?
O4 C64 1.43(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 V1 S2 104.91(5) . . ?
S1 V1 S8 102.80(5) . . ?
S2 V1 S8 74.69(5) . . ?
S1 V1 S7 150.32(6) . . ?
S2 V1 S7 101.28(5) . . ?
S8 V1 S7 97.33(5) . . ?
S1 V1 P1 81.30(5) . . ?
S2 V1 P1 76.07(5) . . ?
S8 V1 P1 150.54(6) . . ?
S7 V1 P1 91.80(5) . . ?
S1 V1 S9 79.59(5) . . ?
S2 V1 S9 122.89(6) . . ?
S8 V1 S9 49.63(4) . . ?
S7 V1 S9 97.71(5) . . ?
P1 V1 S9 156.08(6) . . ?
S1 V1 S3 98.97(5) . . ?
S2 V1 S3 141.93(6) . . ?
S8 V1 S3 128.14(5) . . ?
S7 V1 S3 51.36(5) . . ?
P1 V1 S3 78.80(5) . . ?
S9 V1 S3 90.08(5) . . ?
S1 V1 V2 129.54(5) . . ?
S2 V1 V2 107.44(4) . . ?
S8 V1 V2 52.21(4) . . ?
S7 V1 V2 51.90(4) . . ?
P1 V1 V2 143.69(5) . . ?
S9 V1 V2 50.37(4) . . ?
S3 V1 V2 77.74(4) . . ?
S4 V2 S6 97.70(5) . . ?
S4 V2 S9 91.63(5) . . ?
S6 V2 S9 75.85(5) . . ?
S4 V2 P2 82.13(5) . . ?
S6 V2 P2 78.60(5) . . ?
S9 V2 P2 152.62(6) . . ?
S4 V2 S7 165.46(6) . . ?
S6 V2 S7 95.30(5) . . ?
S9 V2 S7 97.85(5) . . ?
P2 V2 S7 94.13(5) . . ?
S4 V2 S8 83.61(5) . . ?
S6 V2 S8 125.17(6) . . ?
S9 V2 S8 49.35(5) . . ?
P2 V2 S8 153.81(6) . . ?
S7 V2 S8 94.21(5) . . ?
S4 V2 S5 95.87(5) . . ?
S6 V2 S5 146.49(6) . . ?
S9 V2 S5 134.21(5) . . ?
P2 V2 S5 73.11(5) . . ?
S7 V2 S5 69.63(5) . . ?
S8 V2 S5 86.68(5) . . ?
S4 V2 V1 132.24(5) . . ?
S6 V2 V1 100.59(4) . . ?
S9 V2 V1 51.82(4) . . ?
P2 V2 V1 144.68(5) . . ?
S7 V2 V1 50.58(4) . . ?
S8 V2 V1 50.02(4) . . ?
S5 V2 V1 92.51(4) . . ?
C2 S1 V1 111.18(17) . . ?
C20 S2 V1 113.19(19) . . ?
S3 S7 V1 66.78(5) . . ?
S3 S7 V2 99.62(6) . . ?
V1 S7 V2 77.52(5) . . ?
C11 S3 S7 103.92(19) . . ?
C11 S3 V1 110.84(18) . . ?
S7 S3 V1 61.86(5) . . ?
C29 S4 V2 111.01(18) . . ?
C38 S5 V2 108.90(19) . . ?
C47 S6 V2 112.84(18) . . ?
S9 S8 V1 66.76(5) . . ?
S9 S8 V2 63.70(5) . . ?
V1 S8 V2 77.76(5) . . ?
S8 S9 V2 66.94(6) . . ?
S8 S9 V1 63.62(5) . . ?
V2 S9 V1 77.81(5) . . ?
C19 P1 C1 106.9(2) . . ?
C19 P1 C10 108.4(2) . . ?
C1 P1 C10 106.4(2) . . ?
C19 P1 V1 112.36(17) . . ?
C1 P1 V1 108.85(16) . . ?
C10 P1 V1 113.60(17) . . ?
C37 P2 C46 110.0(3) . . ?
C37 P2 C28 107.1(2) . . ?
C46 P2 C28 104.2(2) . . ?
C37 P2 V2 112.68(17) . . ?
C46 P2 V2 114.44(18) . . ?
C28 P2 V2 107.85(17) . . ?
C7 Si1 C8 111.6(3) . . ?
C7 Si1 C9 108.8(3) . . ?
C8 Si1 C9 106.7(3) . . ?
C7 Si1 C3 109.8(2) . . ?
C8 Si1 C3 111.7(2) . . ?
C9 Si1 C3 108.2(3) . . ?
C26 Si2 C25 111.6(4) . . ?
C26 Si2 C27 107.6(4) . . ?
C25 Si2 C27 107.3(3) . . ?
C26 Si2 C21 112.6(3) . . ?
C25 Si2 C21 109.2(3) . . ?
C27 Si2 C21 108.4(3) . . ?
C12 Si3 C18 103(2) . . ?
C12 Si3 C16 114.7(8) . . ?
C18 Si3 C16 111(2) . . ?
C12 Si3 C17 109.3(13) . . ?
C18 Si3 C17 112(2) . . ?
C16 Si3 C17 107.4(13) . . ?
C17' Si3' C18' 104(3) . . ?
C17' Si3' C16' 111.4(16) . . ?
C18' Si3' C16' 111(3) . . ?
C17' Si3' C12 104.4(14) . . ?
C18' Si3' C12 115(3) . . ?
C16' Si3' C12 110.8(9) . . ?
C34 Si4 C35 109.6(3) . . ?
C34 Si4 C36 109.4(3) . . ?
C35 Si4 C36 108.3(3) . . ?
C34 Si4 C30 109.8(2) . . ?
C35 Si4 C30 112.6(3) . . ?
C36 Si4 C30 107.0(3) . . ?
C45 Si5 C43 112.2(15) . . ?
C45 Si5 C44 108.1(15) . . ?
C43 Si5 C44 107.2(13) . . ?
C45 Si5 C39 107.4(12) . . ?
C43 Si5 C39 115.8(11) . . ?
C44 Si5 C39 105.7(7) . . ?
C39 Si5' C44' 111.7(10) . . ?
C39 Si5' C43' 101.3(14) . . ?
C44' Si5' C43' 110.8(17) . . ?
C39 Si5' C45' 112.2(18) . . ?
C44' Si5' C45' 110.0(18) . . ?
C43' Si5' C45' 110.6(18) . . ?
C54 Si6 C53 108.5(3) . . ?
C54 Si6 C52 112.7(3) . . ?
C53 Si6 C52 106.1(3) . . ?
C54 Si6 C48 111.0(3) . . ?
C53 Si6 C48 108.6(3) . . ?
C52 Si6 C48 109.8(3) . . ?
C2 C1 C6 121.7(5) . . ?
C2 C1 P1 115.5(4) . . ?
C6 C1 P1 122.7(4) . . ?
C1 C2 C3 120.0(4) . . ?
C1 C2 S1 120.2(4) . . ?
C3 C2 S1 119.8(4) . . ?
C4 C3 C2 116.0(5) . . ?
C4 C3 Si1 119.1(4) . . ?
C2 C3 Si1 124.9(4) . . ?
C5 C4 C3 123.6(5) . . ?
C4 C5 C6 120.1(5) . . ?
C5 C6 C1 118.5(5) . . ?
C15 C10 C11 119.1(5) . . ?
C15 C10 P1 123.6(4) . . ?
C11 C10 P1 117.3(4) . . ?
C10 C11 C12 123.0(5) . . ?
C10 C11 S3 118.5(4) . . ?
C12 C11 S3 118.3(4) . . ?
C13 C12 C11 115.7(5) . . ?
C13 C12 Si3 115.8(6) . . ?
C11 C12 Si3 128.1(6) . . ?
C13 C12 Si3' 117.4(6) . . ?
C11 C12 Si3' 126.1(6) . . ?
Si3 C12 Si3' 14.2(5) . . ?
C12 C13 C14 122.7(6) . . ?
C15 C14 C13 119.2(5) . . ?
C10 C15 C14 120.3(5) . . ?
C24 C19 C20 120.6(5) . . ?
C24 C19 P1 128.1(4) . . ?
C20 C19 P1 111.2(4) . . ?
C19 C20 C21 121.8(5) . . ?
C19 C20 S2 118.9(4) . . ?
C21 C20 S2 119.2(4) . . ?
C22 C21 C20 115.0(5) . . ?
C22 C21 Si2 120.6(4) . . ?
C20 C21 Si2 124.3(4) . . ?
C23 C22 C21 123.6(5) . . ?
C22 C23 C24 120.0(5) . . ?
C19 C24 C23 118.7(6) . . ?
C33 C28 C29 120.5(5) . . ?
C33 C28 P2 122.7(4) . . ?
C29 C28 P2 116.4(4) . . ?
C30 C29 C28 121.6(4) . . ?
C30 C29 S4 119.6(4) . . ?
C28 C29 S4 118.8(4) . . ?
C31 C30 C29 115.9(5) . . ?
C31 C30 Si4 119.1(4) . . ?
C29 C30 Si4 124.7(4) . . ?
C32 C31 C30 123.1(5) . . ?
C31 C32 C33 120.4(5) . . ?
C32 C33 C28 118.3(5) . . ?
C42 C37 C38 121.8(5) . . ?
C42 C37 P2 127.1(4) . . ?
C38 C37 P2 111.1(4) . . ?
C37 C38 C39 119.9(5) . . ?
C37 C38 S5 118.1(4) . . ?
C39 C38 S5 122.0(5) . . ?
C40 C39 C38 116.0(6) . . ?
C40 C39 Si5' 113.7(6) . . ?
C38 C39 Si5' 129.5(7) . . ?
C40 C39 Si5 123.9(6) . . ?
C38 C39 Si5 120.1(6) . . ?
Si5' C39 Si5 15.7(5) . . ?
C41 C40 C39 124.1(6) . . ?
C42 C41 C40 118.6(6) . . ?
C41 C42 C37 119.3(6) . . ?
C47 C46 C51 120.3(5) . . ?
C47 C46 P2 113.1(4) . . ?
C51 C46 P2 126.1(4) . . ?
C46 C47 C48 121.2(5) . . ?
C46 C47 S6 120.2(4) . . ?
C48 C47 S6 118.6(4) . . ?
C49 C48 C47 115.7(5) . . ?
C49 C48 Si6 120.3(4) . . ?
C47 C48 Si6 123.6(4) . . ?
C50 C49 C48 123.2(5) . . ?
C49 C50 C51 120.0(5) . . ?
C50 C51 C46 119.3(5) . . ?
C58 O1 C55 109.7(6) . . ?
O1 C55 C56 106.3(7) . . ?
C55 C56 C57 102.9(7) . . ?
C58 C57 C56 102.6(6) . . ?
O1 C58 C57 107.2(6) . . ?
C59 O2 C62 109.5(18) . . ?
O2 C59 C60 90.8(18) . . ?
C59 C60 C61 103.1(18) . . ?
C62 C61 C60 110(2) . . ?
O2 C62 C61 87.5(18) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.146
