# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Marc Fourmigue'
'Narcis Avarvari'

_publ_contact_author_name        'Dr Marc Fourmigue'
_publ_contact_author_address     
;
CIMMA
Universite d'Angers
UMR 6200 CNRS
UFR Sciences
2 Bd Lavoisier
Angers
49045
FRANCE
;

_publ_contact_author_email       MARC.FOURMIGUE@UNIV-ANGERS.FR

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
First cation radical salt of a tetrathiafulvalene
based phosphine metal complex
;

data_na91merg
_database_code_depnum_ccdc_archive 'CCDC 233488'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            o-Me2-TTF(PPh2)2(Mo(CO)4)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H26 Mo O4 P2 S4'
_chemical_formula_weight         808.69

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'
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'
Mo Mo -1.6832 0.6857 '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                   12.821(1)
_cell_length_b                   18.266(2)
_cell_length_c                   18.629(2)
_cell_angle_alpha                114.96(1)
_cell_angle_beta                 105.50(1)
_cell_angle_gamma                95.50(1)
_cell_volume                     3701.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      52.1

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, Phi. incr. = 1.2'
_diffrn_detector_area_resol_mean 6.66
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38275
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.1024
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         25.99
_reflns_number_total             13477
_reflns_number_gt                7383
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13477
_refine_ls_number_parameters     847
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0623
_refine_ls_wR_factor_gt          0.0548
_refine_ls_goodness_of_fit_ref   0.767
_refine_ls_restrained_S_all      0.767
_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
Mo1 Mo 0.35345(3) 0.78929(2) 0.390247(17) 0.04056(10) Uani 1 1 d . . .
S1 S 0.39310(10) 0.51630(6) 0.16606(5) 0.0547(3) Uani 1 1 d . . .
S2 S 0.36547(10) 0.62853(6) 0.08956(6) 0.0561(3) Uani 1 1 d . . .
S3 S 0.38082(9) 0.36695(6) -0.01563(5) 0.0535(3) Uani 1 1 d . . .
S4 S 0.33068(10) 0.47547(7) -0.09288(6) 0.0598(3) Uani 1 1 d . . .
P1 P 0.33096(8) 0.63522(6) 0.31977(5) 0.0411(3) Uani 1 1 d . . .
P2 P 0.30843(8) 0.75926(6) 0.24056(5) 0.0401(2) Uani 1 1 d . . .
O1 O 0.6128(3) 0.8227(2) 0.4224(2) 0.0884(11) Uani 1 1 d . . .
O2 O 0.4117(3) 0.8114(3) 0.5733(2) 0.1416(19) Uani 1 1 d . . .
O3 O 0.3686(3) 0.9810(2) 0.4585(2) 0.1006(12) Uani 1 1 d . . .
O4 O 0.0982(3) 0.7692(2) 0.3747(2) 0.0972(12) Uani 1 1 d . . .
C1 C 0.3553(3) 0.6085(2) 0.22054(19) 0.0405(9) Uani 1 1 d . . .
C2 C 0.3431(3) 0.6608(2) 0.18619(19) 0.0396(9) Uani 1 1 d . . .
C3 C 0.3707(3) 0.5274(2) 0.0740(2) 0.0465(10) Uani 1 1 d . . .
C4 C 0.3611(3) 0.4651(2) -0.0012(2) 0.0451(10) Uani 1 1 d . . .
C5 C 0.3341(3) 0.3198(2) -0.1262(2) 0.0521(11) Uani 1 1 d . . .
C6 C 0.3113(4) 0.3695(3) -0.1606(2) 0.0565(11) Uani 1 1 d . . .
C7 C 0.3299(4) 0.2287(3) -0.1700(3) 0.0824(15) Uani 1 1 d . . .
H7A H 0.3497 0.2089 -0.1292 0.124 Uiso 1 1 calc R . .
H7B H 0.3814 0.2200 -0.2003 0.124 Uiso 1 1 calc R . .
H7C H 0.2558 0.1989 -0.2088 0.124 Uiso 1 1 calc R . .
C8 C 0.2738(5) 0.3453(3) -0.2530(2) 0.0999(19) Uani 1 1 d . . .
H8A H 0.2644 0.3935 -0.2604 0.150 Uiso 1 1 calc R . .
H8B H 0.2041 0.3044 -0.2815 0.150 Uiso 1 1 calc R . .
H8C H 0.3288 0.3226 -0.2761 0.150 Uiso 1 1 calc R . .
C9 C 0.5184(4) 0.8093(2) 0.4085(2) 0.0572(11) Uani 1 1 d . . .
C10 C 0.3893(4) 0.8018(3) 0.5057(3) 0.0747(15) Uani 1 1 d . . .
C11 C 0.3640(4) 0.9104(3) 0.4329(2) 0.0637(13) Uani 1 1 d . . .
C12 C 0.1898(4) 0.7744(3) 0.3782(2) 0.0605(12) Uani 1 1 d . . .
C13 C 0.4184(3) 0.5793(2) 0.36099(19) 0.0449(10) Uani 1 1 d . . .
C14 C 0.3779(4) 0.5002(3) 0.3501(2) 0.0598(12) Uani 1 1 d . . .
H14 H 0.3023 0.4749 0.3220 0.072 Uiso 1 1 calc R . .
C15 C 0.4479(5) 0.4588(3) 0.3801(3) 0.0691(13) Uani 1 1 d . . .
H15 H 0.4191 0.4062 0.3724 0.083 Uiso 1 1 calc R . .
C16 C 0.5582(5) 0.4944(3) 0.4208(3) 0.0688(13) Uani 1 1 d . . .
H16 H 0.6051 0.4666 0.4413 0.083 Uiso 1 1 calc R . .
C17 C 0.6003(4) 0.5714(4) 0.4315(3) 0.0818(15) Uani 1 1 d . . .
H17 H 0.6763 0.5953 0.4581 0.098 Uiso 1 1 calc R . .
C18 C 0.5316(4) 0.6135(3) 0.4034(3) 0.0713(13) Uani 1 1 d . . .
H18 H 0.5616 0.6666 0.4129 0.086 Uiso 1 1 calc R . .
C19 C 0.1894(3) 0.5760(2) 0.2873(2) 0.0489(10) Uani 1 1 d . . .
C20 C 0.1181(4) 0.5347(3) 0.2050(3) 0.0721(14) Uani 1 1 d . . .
H20 H 0.1453 0.5293 0.1619 0.087 Uiso 1 1 calc R . .
C21 C 0.0072(4) 0.5011(4) 0.1856(4) 0.102(2) Uani 1 1 d . . .
H21 H -0.0395 0.4726 0.1296 0.122 Uiso 1 1 calc R . .
C22 C -0.0344(4) 0.5095(4) 0.2481(4) 0.0967(18) Uani 1 1 d . . .
H22 H -0.1099 0.4888 0.2350 0.116 Uiso 1 1 calc R . .
C23 C 0.0349(5) 0.5481(3) 0.3294(4) 0.0870(16) Uani 1 1 d . . .
H23 H 0.0071 0.5519 0.3718 0.104 Uiso 1 1 calc R . .
C24 C 0.1461(4) 0.5819(3) 0.3498(3) 0.0710(14) Uani 1 1 d . . .
H24 H 0.1924 0.6089 0.4059 0.085 Uiso 1 1 calc R . .
C25 C 0.3810(3) 0.8263(2) 0.2100(2) 0.0430(9) Uani 1 1 d . . .
C26 C 0.4752(3) 0.8881(2) 0.2675(2) 0.0506(10) Uani 1 1 d . . .
H26 H 0.4998 0.8972 0.3230 0.061 Uiso 1 1 calc R . .
C27 C 0.5333(3) 0.9365(3) 0.2441(3) 0.0603(11) Uani 1 1 d . . .
H27 H 0.5964 0.9780 0.2836 0.072 Uiso 1 1 calc R . .
C28 C 0.4981(4) 0.9234(3) 0.1627(3) 0.0592(12) Uani 1 1 d . . .
H28 H 0.5384 0.9553 0.1468 0.071 Uiso 1 1 calc R . .
C29 C 0.4048(4) 0.8642(3) 0.1048(3) 0.0643(12) Uani 1 1 d . . .
H29 H 0.3811 0.8564 0.0498 0.077 Uiso 1 1 calc R . .
C30 C 0.3448(4) 0.8153(2) 0.1272(2) 0.0544(11) Uani 1 1 d . . .
H30 H 0.2806 0.7752 0.0874 0.065 Uiso 1 1 calc R . .
C31 C 0.1628(3) 0.7410(3) 0.1796(2) 0.0483(10) Uani 1 1 d . . .
C32 C 0.1110(4) 0.8055(4) 0.2029(3) 0.0882(16) Uani 1 1 d . . .
H32 H 0.1524 0.8578 0.2459 0.106 Uiso 1 1 calc R . .
C33 C -0.0009(5) 0.7941(5) 0.1637(4) 0.112(2) Uani 1 1 d . . .
H33 H -0.0343 0.8387 0.1798 0.134 Uiso 1 1 calc R . .
C34 C -0.0624(5) 0.7184(5) 0.1020(4) 0.104(2) Uani 1 1 d . . .
H34 H -0.1385 0.7106 0.0768 0.124 Uiso 1 1 calc R . .
C35 C -0.0138(5) 0.6534(5) 0.0764(4) 0.111(2) Uani 1 1 d . . .
H35 H -0.0559 0.6015 0.0332 0.133 Uiso 1 1 calc R . .
C36 C 0.0990(4) 0.6656(3) 0.1154(3) 0.0837(15) Uani 1 1 d . . .
H36 H 0.1325 0.6214 0.0974 0.100 Uiso 1 1 calc R . .
Mo2 Mo -0.04341(3) -0.27124(2) -0.393018(18) 0.04547(10) Uani 1 1 d . . .
S5 S 0.21239(8) 0.01829(6) -0.17266(5) 0.0502(3) Uani 1 1 d . . .
S6 S 0.28059(9) -0.09984(7) -0.11102(6) 0.0592(3) Uani 1 1 d . . .
S7 S 0.35835(10) 0.17283(7) 0.01247(6) 0.0600(3) Uani 1 1 d . . .
S8 S 0.42279(10) 0.05513(7) 0.07338(6) 0.0712(4) Uani 1 1 d . . .
P3 P 0.00822(8) -0.11644(6) -0.32160(5) 0.0411(3) Uani 1 1 d . . .
P4 P 0.07270(8) -0.24324(6) -0.24944(5) 0.0419(3) Uani 1 1 d . . .
O5 O -0.2588(3) -0.2718(2) -0.3398(2) 0.1049(13) Uani 1 1 d . . .
O6 O -0.1758(4) -0.2680(3) -0.5583(2) 0.1471(19) Uani 1 1 d . . .
O7 O -0.1145(4) -0.4663(2) -0.4769(2) 0.1176(14) Uani 1 1 d . . .
O8 O 0.1675(3) -0.2870(3) -0.4512(2) 0.1126(14) Uani 1 1 d . . .
C37 C 0.1281(3) -0.0833(2) -0.22724(18) 0.0389(9) Uani 1 1 d . . .
C38 C 0.1585(3) -0.1378(2) -0.19885(19) 0.0419(9) Uani 1 1 d . . .
C39 C 0.2889(3) 0.0055(2) -0.0871(2) 0.0428(9) Uani 1 1 d . . .
C40 C 0.3484(3) 0.0688(2) -0.0112(2) 0.0451(10) Uani 1 1 d . . .
C41 C 0.4124(4) 0.2118(3) 0.1223(2) 0.0636(13) Uani 1 1 d . . .
C42 C 0.4427(4) 0.1583(3) 0.1497(2) 0.0681(14) Uani 1 1 d . . .
C43 C 0.4180(4) 0.3016(3) 0.1750(3) 0.0952(18) Uani 1 1 d . . .
H43A H 0.3903 0.3257 0.1390 0.143 Uiso 1 1 calc R . .
H43B H 0.4940 0.3304 0.2098 0.143 Uiso 1 1 calc R . .
H43C H 0.3734 0.3063 0.2100 0.143 Uiso 1 1 calc R . .
C44 C 0.4990(5) 0.1784(3) 0.2410(2) 0.118(2) Uani 1 1 d . . .
H44A H 0.5124 0.1286 0.2436 0.178 Uiso 1 1 calc R . .
H44B H 0.4515 0.2007 0.2727 0.178 Uiso 1 1 calc R . .
H44C H 0.5686 0.2186 0.2643 0.178 Uiso 1 1 calc R . .
C45 C -0.1811(4) -0.2697(3) -0.3581(3) 0.0646(12) Uani 1 1 d . . .
C46 C -0.1286(4) -0.2712(3) -0.4984(3) 0.0817(16) Uani 1 1 d . . .
C47 C -0.0858(4) -0.3942(3) -0.4446(3) 0.0765(15) Uani 1 1 d . . .
C48 C 0.0923(5) -0.2794(3) -0.4293(2) 0.0714(14) Uani 1 1 d . . .
C49 C -0.0982(3) -0.0689(2) -0.2837(2) 0.0474(10) Uani 1 1 d . . .
C50 C -0.0866(4) -0.0270(3) -0.2003(3) 0.0777(15) Uani 1 1 d . . .
H50 H -0.0186 -0.0165 -0.1595 0.093 Uiso 1 1 calc R . .
C51 C -0.1747(6) -0.0002(4) -0.1759(4) 0.106(2) Uani 1 1 d . . .
H51 H -0.1654 0.0287 -0.1191 0.127 Uiso 1 1 calc R . .
C52 C -0.2742(5) -0.0160(4) -0.2349(5) 0.0968(18) Uani 1 1 d . . .
H52 H -0.3337 0.0008 -0.2182 0.116 Uiso 1 1 calc R . .
C53 C -0.2879(4) -0.0560(3) -0.3179(4) 0.0883(16) Uani 1 1 d . . .
H53 H -0.3559 -0.0652 -0.3580 0.106 Uiso 1 1 calc R . .
C54 C -0.1999(4) -0.0831(3) -0.3426(3) 0.0680(13) Uani 1 1 d . . .
H54 H -0.2096 -0.1112 -0.3996 0.082 Uiso 1 1 calc R . .
C55 C 0.0582(3) -0.0526(3) -0.3650(2) 0.0488(10) Uani 1 1 d . . .
C56 C 0.0294(4) 0.0205(3) -0.3545(3) 0.0684(13) Uani 1 1 d . . .
H56 H -0.0233 0.0364 -0.3287 0.082 Uiso 1 1 calc R . .
C57 C 0.0767(5) 0.0720(3) -0.3812(3) 0.0872(16) Uani 1 1 d . . .
H57 H 0.0570 0.1220 -0.3724 0.105 Uiso 1 1 calc R . .
C58 C 0.1514(5) 0.0480(4) -0.4202(3) 0.0883(19) Uani 1 1 d . . .
H58 H 0.1821 0.0811 -0.4395 0.106 Uiso 1 1 calc R . .
C59 C 0.1820(5) -0.0238(4) -0.4313(3) 0.100(2) Uani 1 1 d . . .
H59 H 0.2351 -0.0389 -0.4569 0.120 Uiso 1 1 calc R . .
C60 C 0.1351(4) -0.0752(3) -0.4050(3) 0.0811(15) Uani 1 1 d . . .
H60 H 0.1555 -0.1251 -0.4143 0.097 Uiso 1 1 calc R . .
C61 C 0.0009(3) -0.2383(3) -0.1756(2) 0.0505(10) Uani 1 1 d . . .
C62 C -0.0598(4) -0.3111(3) -0.1868(3) 0.0814(15) Uani 1 1 d . . .
H62 H -0.0619 -0.3614 -0.2310 0.098 Uiso 1 1 calc R . .
C63 C -0.1170(5) -0.3111(4) -0.1344(4) 0.109(2) Uani 1 1 d . . .
H63 H -0.1568 -0.3609 -0.1427 0.131 Uiso 1 1 calc R . .
C64 C -0.1156(5) -0.2385(5) -0.0708(4) 0.110(2) Uani 1 1 d . . .
H64 H -0.1536 -0.2386 -0.0348 0.131 Uiso 1 1 calc R . .
C65 C -0.0594(6) -0.1657(5) -0.0590(3) 0.121(2) Uani 1 1 d . . .
H65 H -0.0612 -0.1158 -0.0163 0.146 Uiso 1 1 calc R . .
C66 C 0.0013(5) -0.1652(3) -0.1106(3) 0.0906(17) Uani 1 1 d . . .
H66 H 0.0423 -0.1152 -0.1010 0.109 Uiso 1 1 calc R . .
C67 C 0.1719(3) -0.3038(2) -0.2313(2) 0.0480(10) Uani 1 1 d . . .
C68 C 0.2272(4) -0.2943(3) -0.1513(3) 0.0631(12) Uani 1 1 d . . .
H68 H 0.2137 -0.2552 -0.1051 0.076 Uiso 1 1 calc R . .
C69 C 0.3004(4) -0.3408(4) -0.1392(4) 0.0803(15) Uani 1 1 d . . .
H69 H 0.3374 -0.3323 -0.0850 0.096 Uiso 1 1 calc R . .
C70 C 0.3198(4) -0.3999(4) -0.2062(5) 0.0882(16) Uani 1 1 d . . .
H70 H 0.3698 -0.4315 -0.1977 0.106 Uiso 1 1 calc R . .
C71 C 0.2655(5) -0.4123(3) -0.2857(4) 0.0863(16) Uani 1 1 d . . .
H71 H 0.2783 -0.4529 -0.3313 0.104 Uiso 1 1 calc R . .
C72 C 0.1917(4) -0.3650(3) -0.2989(3) 0.0634(12) Uani 1 1 d . . .
H72 H 0.1552 -0.3742 -0.3534 0.076 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0445(2) 0.0357(2) 0.03202(16) 0.00650(14) 0.01688(15) 0.00275(17)
S1 0.0820(8) 0.0457(6) 0.0410(5) 0.0188(5) 0.0264(5) 0.0263(6)
S2 0.0920(9) 0.0421(6) 0.0446(5) 0.0185(5) 0.0392(6) 0.0235(6)
S3 0.0683(8) 0.0419(6) 0.0419(5) 0.0124(5) 0.0164(5) 0.0187(6)
S4 0.0888(9) 0.0496(7) 0.0390(5) 0.0177(5) 0.0219(5) 0.0220(6)
P1 0.0430(6) 0.0399(6) 0.0341(5) 0.0125(4) 0.0143(4) 0.0022(5)
P2 0.0435(6) 0.0341(6) 0.0395(5) 0.0122(4) 0.0185(4) 0.0072(5)
O1 0.045(2) 0.081(3) 0.133(3) 0.050(2) 0.023(2) 0.005(2)
O2 0.139(4) 0.218(5) 0.0452(19) 0.060(3) 0.019(2) -0.008(3)
O3 0.123(3) 0.043(2) 0.122(3) 0.015(2) 0.061(2) 0.018(2)
O4 0.064(2) 0.105(3) 0.133(3) 0.052(2) 0.054(2) 0.028(2)
C1 0.044(2) 0.034(2) 0.0382(18) 0.0113(16) 0.0164(17) 0.0065(19)
C2 0.043(2) 0.037(2) 0.0357(18) 0.0126(16) 0.0168(16) 0.0077(19)
C3 0.058(3) 0.041(2) 0.0381(19) 0.0143(17) 0.0195(18) 0.015(2)
C4 0.051(2) 0.041(2) 0.0373(19) 0.0114(17) 0.0157(17) 0.014(2)
C5 0.055(3) 0.040(3) 0.045(2) 0.0056(19) 0.0170(19) 0.013(2)
C6 0.070(3) 0.050(3) 0.0330(19) 0.0067(19) 0.0133(19) 0.016(2)
C7 0.108(4) 0.051(3) 0.062(3) 0.004(2) 0.025(3) 0.024(3)
C8 0.149(5) 0.085(4) 0.038(2) 0.012(2) 0.015(3) 0.032(4)
C9 0.065(3) 0.039(3) 0.057(2) 0.017(2) 0.018(2) 0.002(2)
C10 0.073(3) 0.084(4) 0.045(2) 0.016(2) 0.018(2) -0.004(3)
C11 0.069(3) 0.053(3) 0.057(2) 0.008(2) 0.035(2) 0.007(3)
C12 0.072(3) 0.054(3) 0.060(2) 0.022(2) 0.037(2) 0.015(3)
C13 0.055(3) 0.045(2) 0.0325(18) 0.0154(17) 0.0187(18) 0.009(2)
C14 0.062(3) 0.059(3) 0.055(2) 0.028(2) 0.015(2) 0.007(3)
C15 0.098(4) 0.058(3) 0.067(3) 0.038(3) 0.034(3) 0.027(3)
C16 0.080(4) 0.082(4) 0.055(3) 0.038(3) 0.023(3) 0.036(3)
C17 0.061(3) 0.080(4) 0.095(4) 0.043(3) 0.008(3) 0.017(3)
C18 0.053(3) 0.063(3) 0.084(3) 0.035(3) 0.007(3) 0.003(3)
C19 0.051(3) 0.040(2) 0.056(2) 0.0212(19) 0.022(2) 0.010(2)
C20 0.055(3) 0.076(3) 0.072(3) 0.037(3) 0.007(2) -0.012(3)
C21 0.057(4) 0.114(5) 0.107(4) 0.058(4) -0.005(3) -0.024(3)
C22 0.043(3) 0.094(5) 0.149(5) 0.061(4) 0.026(4) -0.001(3)
C23 0.072(4) 0.074(4) 0.128(5) 0.045(3) 0.058(4) 0.011(3)
C24 0.066(3) 0.063(3) 0.073(3) 0.018(2) 0.036(2) -0.002(3)
C25 0.045(2) 0.040(2) 0.050(2) 0.0208(18) 0.0243(19) 0.017(2)
C26 0.047(3) 0.049(3) 0.059(2) 0.026(2) 0.020(2) 0.011(2)
C27 0.047(3) 0.055(3) 0.084(3) 0.039(2) 0.022(2) 0.008(2)
C28 0.053(3) 0.071(3) 0.084(3) 0.054(3) 0.037(3) 0.024(3)
C29 0.080(4) 0.067(3) 0.073(3) 0.046(3) 0.039(3) 0.029(3)
C30 0.067(3) 0.048(3) 0.051(2) 0.024(2) 0.021(2) 0.014(2)
C31 0.046(2) 0.049(3) 0.048(2) 0.023(2) 0.0167(19) 0.007(2)
C32 0.064(4) 0.087(4) 0.081(3) 0.014(3) 0.015(3) 0.027(3)
C33 0.061(4) 0.150(7) 0.106(4) 0.041(4) 0.025(4) 0.052(4)
C34 0.044(4) 0.164(7) 0.097(4) 0.067(5) 0.009(3) 0.012(5)
C35 0.065(4) 0.104(5) 0.125(5) 0.052(4) -0.010(4) -0.007(4)
C36 0.062(4) 0.068(4) 0.092(3) 0.031(3) -0.004(3) 0.001(3)
Mo2 0.0417(2) 0.0457(2) 0.03028(16) 0.00753(15) 0.00383(14) 0.00344(18)
S5 0.0490(6) 0.0446(6) 0.0445(5) 0.0203(5) 0.0018(5) -0.0003(5)
S6 0.0521(7) 0.0430(7) 0.0546(6) 0.0185(5) -0.0127(5) 0.0012(6)
S7 0.0732(8) 0.0447(7) 0.0487(6) 0.0147(5) 0.0146(5) 0.0081(6)
S8 0.0787(9) 0.0607(8) 0.0469(6) 0.0222(5) -0.0088(5) 0.0008(7)
P3 0.0358(6) 0.0490(7) 0.0323(5) 0.0160(5) 0.0079(4) 0.0085(5)
P4 0.0383(6) 0.0396(6) 0.0367(5) 0.0112(4) 0.0089(4) 0.0050(5)
O5 0.057(2) 0.114(3) 0.145(3) 0.059(3) 0.045(2) 0.009(2)
O6 0.169(4) 0.187(5) 0.056(2) 0.059(3) -0.010(2) 0.048(4)
O7 0.126(4) 0.052(2) 0.115(3) 0.011(2) 0.005(2) 0.004(2)
O8 0.123(3) 0.132(3) 0.122(3) 0.058(3) 0.094(3) 0.058(3)
C37 0.031(2) 0.044(2) 0.0331(17) 0.0119(17) 0.0090(15) 0.0053(19)
C38 0.038(2) 0.042(2) 0.0377(18) 0.0148(17) 0.0083(16) 0.010(2)
C39 0.037(2) 0.044(2) 0.0396(19) 0.0177(18) 0.0060(17) 0.0036(19)
C40 0.037(2) 0.047(2) 0.0398(19) 0.0171(18) 0.0054(17) 0.001(2)
C41 0.063(3) 0.055(3) 0.048(2) 0.004(2) 0.020(2) -0.002(3)
C42 0.069(3) 0.069(3) 0.039(2) 0.011(2) 0.009(2) -0.008(3)
C43 0.088(4) 0.062(3) 0.077(3) -0.012(3) 0.022(3) -0.003(3)
C44 0.151(5) 0.110(5) 0.038(2) 0.020(3) -0.006(3) -0.026(4)
C45 0.050(3) 0.061(3) 0.072(3) 0.032(2) 0.007(2) 0.001(3)
C46 0.081(4) 0.087(4) 0.047(2) 0.017(2) 0.004(2) 0.009(3)
C47 0.063(3) 0.069(4) 0.060(3) 0.013(3) -0.003(2) 0.004(3)
C48 0.100(4) 0.064(3) 0.048(2) 0.019(2) 0.033(3) 0.024(3)
C49 0.040(2) 0.049(3) 0.056(2) 0.026(2) 0.0179(19) 0.012(2)
C50 0.072(3) 0.101(4) 0.063(3) 0.030(3) 0.035(3) 0.042(3)
C51 0.097(5) 0.133(6) 0.097(4) 0.041(4) 0.059(4) 0.058(4)
C52 0.075(4) 0.097(5) 0.137(5) 0.050(4) 0.063(4) 0.044(4)
C53 0.049(3) 0.085(4) 0.131(5) 0.054(4) 0.023(3) 0.021(3)
C54 0.041(3) 0.077(4) 0.081(3) 0.037(3) 0.014(2) 0.015(3)
C55 0.043(2) 0.064(3) 0.0348(19) 0.0240(19) 0.0059(17) 0.011(2)
C56 0.066(3) 0.072(4) 0.080(3) 0.042(3) 0.032(3) 0.019(3)
C57 0.096(4) 0.078(4) 0.097(4) 0.055(3) 0.029(3) 0.013(3)
C58 0.097(5) 0.098(5) 0.063(3) 0.047(3) 0.013(3) -0.014(4)
C59 0.106(5) 0.122(5) 0.095(4) 0.058(4) 0.061(3) 0.009(4)
C60 0.096(4) 0.080(4) 0.092(3) 0.046(3) 0.059(3) 0.023(3)
C61 0.048(3) 0.057(3) 0.043(2) 0.020(2) 0.0170(18) 0.013(2)
C62 0.088(4) 0.069(4) 0.102(4) 0.039(3) 0.056(3) 0.017(3)
C63 0.114(5) 0.117(5) 0.153(5) 0.082(5) 0.094(5) 0.036(4)
C64 0.110(5) 0.170(7) 0.105(4) 0.084(5) 0.076(4) 0.063(5)
C65 0.139(6) 0.125(6) 0.094(4) 0.025(4) 0.078(4) 0.027(5)
C66 0.114(5) 0.080(4) 0.076(3) 0.024(3) 0.054(3) 0.019(3)
C67 0.043(2) 0.043(2) 0.053(2) 0.0214(19) 0.0130(19) 0.007(2)
C68 0.061(3) 0.046(3) 0.067(3) 0.023(2) 0.007(2) 0.010(3)
C69 0.061(4) 0.070(4) 0.106(4) 0.053(3) 0.004(3) 0.013(3)
C70 0.060(4) 0.093(5) 0.150(5) 0.082(4) 0.043(4) 0.038(3)
C71 0.087(4) 0.081(4) 0.131(5) 0.059(4) 0.072(4) 0.048(4)
C72 0.066(3) 0.063(3) 0.076(3) 0.035(3) 0.039(2) 0.029(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C10 1.982(4) . ?
Mo1 C11 1.987(5) . ?
Mo1 C9 2.021(5) . ?
Mo1 C12 2.029(5) . ?
Mo1 P2 2.4896(11) . ?
Mo1 P1 2.5002(14) . ?
S1 C1 1.755(4) . ?
S1 C3 1.763(3) . ?
S2 C2 1.756(3) . ?
S2 C3 1.756(4) . ?
S3 C4 1.751(4) . ?
S3 C5 1.757(4) . ?
S4 C4 1.743(3) . ?
S4 C6 1.755(4) . ?
P1 C13 1.820(4) . ?
P1 C19 1.820(4) . ?
P1 C1 1.824(3) . ?
P2 C31 1.820(4) . ?
P2 C2 1.820(4) . ?
P2 C25 1.827(4) . ?
O1 C9 1.146(5) . ?
O2 C10 1.143(4) . ?
O3 C11 1.159(5) . ?
O4 C12 1.150(5) . ?
C1 C2 1.355(5) . ?
C3 C4 1.344(4) . ?
C5 C6 1.328(5) . ?
C5 C7 1.500(6) . ?
C6 C8 1.505(5) . ?
C13 C18 1.385(5) . ?
C13 C14 1.397(5) . ?
C14 C15 1.382(6) . ?
C15 C16 1.354(6) . ?
C16 C17 1.367(6) . ?
C17 C18 1.366(6) . ?
C19 C20 1.378(5) . ?
C19 C24 1.388(5) . ?
C20 C21 1.378(6) . ?
C21 C22 1.364(7) . ?
C22 C23 1.357(7) . ?
C23 C24 1.379(6) . ?
C25 C26 1.381(5) . ?
C25 C30 1.405(5) . ?
C26 C27 1.380(5) . ?
C27 C28 1.366(5) . ?
C28 C29 1.356(6) . ?
C29 C30 1.384(5) . ?
C31 C36 1.366(6) . ?
C31 C32 1.375(6) . ?
C32 C33 1.375(7) . ?
C33 C34 1.349(8) . ?
C34 C35 1.359(8) . ?
C35 C36 1.382(7) . ?
Mo2 C46 1.975(5) . ?
Mo2 C47 1.982(6) . ?
Mo2 C48 2.025(5) . ?
Mo2 C45 2.037(5) . ?
Mo2 P3 2.4899(15) . ?
Mo2 P4 2.4906(14) . ?
S5 C39 1.755(4) . ?
S5 C37 1.755(4) . ?
S6 C38 1.753(4) . ?
S6 C39 1.767(4) . ?
S7 C40 1.743(4) . ?
S7 C41 1.759(4) . ?
S8 C40 1.740(4) . ?
S8 C42 1.757(5) . ?
P3 C37 1.816(3) . ?
P3 C49 1.827(4) . ?
P3 C55 1.831(4) . ?
P4 C67 1.819(4) . ?
P4 C38 1.821(4) . ?
P4 C61 1.826(4) . ?
O5 C45 1.138(5) . ?
O6 C46 1.148(5) . ?
O7 C47 1.162(5) . ?
O8 C48 1.141(5) . ?
C37 C38 1.353(5) . ?
C39 C40 1.340(4) . ?
C41 C42 1.324(6) . ?
C41 C43 1.497(6) . ?
C42 C44 1.522(5) . ?
C49 C50 1.368(5) . ?
C49 C54 1.379(5) . ?
C50 C51 1.384(6) . ?
C51 C52 1.353(7) . ?
C52 C53 1.354(7) . ?
C53 C54 1.386(6) . ?
C55 C56 1.367(6) . ?
C55 C60 1.382(6) . ?
C56 C57 1.396(6) . ?
C57 C58 1.349(7) . ?
C58 C59 1.353(7) . ?
C59 C60 1.386(6) . ?
C61 C66 1.370(6) . ?
C61 C62 1.378(6) . ?
C62 C63 1.369(6) . ?
C63 C64 1.349(8) . ?
C64 C65 1.349(8) . ?
C65 C66 1.391(6) . ?
C67 C72 1.393(5) . ?
C67 C68 1.395(5) . ?
C68 C69 1.363(6) . ?
C69 C70 1.366(7) . ?
C70 C71 1.365(7) . ?
C71 C72 1.383(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 Mo1 C11 91.22(19) . . ?
C10 Mo1 C9 88.54(17) . . ?
C11 Mo1 C9 89.84(18) . . ?
C10 Mo1 C12 89.28(17) . . ?
C11 Mo1 C12 88.02(18) . . ?
C9 Mo1 C12 176.91(16) . . ?
C10 Mo1 P2 174.50(15) . . ?
C11 Mo1 P2 94.27(12) . . ?
C9 Mo1 P2 91.14(11) . . ?
C12 Mo1 P2 91.24(12) . . ?
C10 Mo1 P1 95.33(15) . . ?
C11 Mo1 P1 173.35(12) . . ?
C9 Mo1 P1 91.47(13) . . ?
C12 Mo1 P1 90.91(13) . . ?
P2 Mo1 P1 79.19(5) . . ?
C1 S1 C3 94.01(17) . . ?
C2 S2 C3 94.94(17) . . ?
C4 S3 C5 95.73(19) . . ?
C4 S4 C6 95.18(18) . . ?
C13 P1 C19 104.18(18) . . ?
C13 P1 C1 101.09(17) . . ?
C19 P1 C1 103.72(17) . . ?
C13 P1 Mo1 125.10(13) . . ?
C19 P1 Mo1 113.87(14) . . ?
C1 P1 Mo1 106.31(12) . . ?
C31 P2 C2 103.31(18) . . ?
C31 P2 C25 102.95(17) . . ?
C2 P2 C25 102.00(16) . . ?
C31 P2 Mo1 117.44(12) . . ?
C2 P2 Mo1 106.71(12) . . ?
C25 P2 Mo1 121.96(12) . . ?
C2 C1 S1 117.8(2) . . ?
C2 C1 P1 119.6(3) . . ?
S1 C1 P1 122.5(2) . . ?
C1 C2 S2 116.2(3) . . ?
C1 C2 P2 120.4(2) . . ?
S2 C2 P2 123.4(2) . . ?
C4 C3 S2 122.6(3) . . ?
C4 C3 S1 123.5(3) . . ?
S2 C3 S1 113.84(18) . . ?
C3 C4 S4 122.9(3) . . ?
C3 C4 S3 123.3(3) . . ?
S4 C4 S3 113.84(18) . . ?
C6 C5 C7 127.9(4) . . ?
C6 C5 S3 116.3(3) . . ?
C7 C5 S3 115.8(3) . . ?
C5 C6 C8 126.7(4) . . ?
C5 C6 S4 117.9(3) . . ?
C8 C6 S4 115.3(3) . . ?
O1 C9 Mo1 177.1(4) . . ?
O2 C10 Mo1 177.9(4) . . ?
O3 C11 Mo1 178.7(4) . . ?
O4 C12 Mo1 177.0(4) . . ?
C18 C13 C14 116.5(4) . . ?
C18 C13 P1 120.4(3) . . ?
C14 C13 P1 123.1(3) . . ?
C15 C14 C13 121.3(4) . . ?
C16 C15 C14 120.2(5) . . ?
C15 C16 C17 119.7(5) . . ?
C18 C17 C16 120.6(5) . . ?
C17 C18 C13 121.7(5) . . ?
C20 C19 C24 117.8(4) . . ?
C20 C19 P1 123.7(3) . . ?
C24 C19 P1 117.9(3) . . ?
C19 C20 C21 121.0(4) . . ?
C22 C21 C20 120.3(5) . . ?
C23 C22 C21 119.7(5) . . ?
C22 C23 C24 120.6(5) . . ?
C23 C24 C19 120.6(4) . . ?
C26 C25 C30 117.9(3) . . ?
C26 C25 P2 120.7(3) . . ?
C30 C25 P2 121.4(3) . . ?
C27 C26 C25 121.1(4) . . ?
C28 C27 C26 119.9(4) . . ?
C29 C28 C27 120.6(4) . . ?
C28 C29 C30 120.4(4) . . ?
C29 C30 C25 120.0(4) . . ?
C36 C31 C32 117.4(4) . . ?
C36 C31 P2 124.2(4) . . ?
C32 C31 P2 118.3(3) . . ?
C31 C32 C33 121.2(5) . . ?
C34 C33 C32 120.1(6) . . ?
C33 C34 C35 120.5(6) . . ?
C34 C35 C36 119.1(6) . . ?
C31 C36 C35 121.8(6) . . ?
C46 Mo2 C47 92.6(2) . . ?
C46 Mo2 C48 89.95(19) . . ?
C47 Mo2 C48 89.2(2) . . ?
C46 Mo2 C45 90.86(19) . . ?
C47 Mo2 C45 87.7(2) . . ?
C48 Mo2 C45 176.87(19) . . ?
C46 Mo2 P3 89.54(16) . . ?
C47 Mo2 P3 177.06(13) . . ?
C48 Mo2 P3 92.73(14) . . ?
C45 Mo2 P3 90.30(13) . . ?
C46 Mo2 P4 169.57(15) . . ?
C47 Mo2 P4 97.79(14) . . ?
C48 Mo2 P4 90.23(13) . . ?
C45 Mo2 P4 89.53(12) . . ?
P3 Mo2 P4 80.03(5) . . ?
C39 S5 C37 94.12(17) . . ?
C38 S6 C39 94.47(18) . . ?
C40 S7 C41 95.3(2) . . ?
C40 S8 C42 95.1(2) . . ?
C37 P3 C49 104.88(16) . . ?
C37 P3 C55 99.81(16) . . ?
C49 P3 C55 103.85(19) . . ?
C37 P3 Mo2 106.96(14) . . ?
C49 P3 Mo2 113.79(13) . . ?
C55 P3 Mo2 125.13(14) . . ?
C67 P4 C38 103.74(17) . . ?
C67 P4 C61 101.62(18) . . ?
C38 P4 C61 102.30(17) . . ?
C67 P4 Mo2 122.86(12) . . ?
C38 P4 Mo2 106.34(12) . . ?
C61 P4 Mo2 117.48(13) . . ?
C38 C37 S5 117.6(3) . . ?
C38 C37 P3 120.7(3) . . ?
S5 C37 P3 121.7(2) . . ?
C37 C38 S6 116.3(3) . . ?
C37 C38 P4 120.3(3) . . ?
S6 C38 P4 123.4(2) . . ?
C40 C39 S5 123.7(3) . . ?
C40 C39 S6 123.0(3) . . ?
S5 C39 S6 113.30(19) . . ?
C39 C40 S8 123.2(3) . . ?
C39 C40 S7 123.2(3) . . ?
S8 C40 S7 113.58(19) . . ?
C42 C41 C43 126.9(4) . . ?
C42 C41 S7 116.5(3) . . ?
C43 C41 S7 116.6(4) . . ?
C41 C42 C44 126.2(4) . . ?
C41 C42 S8 117.3(3) . . ?
C44 C42 S8 116.5(4) . . ?
O5 C45 Mo2 177.6(4) . . ?
O6 C46 Mo2 177.2(5) . . ?
O7 C47 Mo2 177.4(5) . . ?
O8 C48 Mo2 177.6(4) . . ?
C50 C49 C54 118.1(4) . . ?
C50 C49 P3 123.7(3) . . ?
C54 C49 P3 117.9(3) . . ?
C49 C50 C51 120.8(5) . . ?
C52 C51 C50 120.0(5) . . ?
C51 C52 C53 120.6(5) . . ?
C52 C53 C54 119.5(5) . . ?
C49 C54 C53 120.9(4) . . ?
C56 C55 C60 117.5(4) . . ?
C56 C55 P3 123.1(3) . . ?
C60 C55 P3 119.2(4) . . ?
C55 C56 C57 122.1(4) . . ?
C58 C57 C56 118.9(6) . . ?
C57 C58 C59 120.6(5) . . ?
C58 C59 C60 120.7(5) . . ?
C55 C60 C59 120.2(5) . . ?
C66 C61 C62 117.9(4) . . ?
C66 C61 P4 123.3(3) . . ?
C62 C61 P4 118.8(3) . . ?
C63 C62 C61 121.4(5) . . ?
C64 C63 C62 119.8(6) . . ?
C65 C64 C63 120.6(5) . . ?
C64 C65 C66 120.0(6) . . ?
C61 C66 C65 120.3(5) . . ?
C72 C67 C68 117.2(4) . . ?
C72 C67 P4 120.2(3) . . ?
C68 C67 P4 122.6(3) . . ?
C69 C68 C67 121.7(4) . . ?
C68 C69 C70 120.3(5) . . ?
C71 C70 C69 119.8(6) . . ?
C70 C71 C72 120.6(5) . . ?
C71 C72 C67 120.4(4) . . ?

_diffrn_measured_fraction_theta_max 0.928
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.928
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.054

#===END

data_nas1merge
_database_code_depnum_ccdc_archive 'CCDC 233489'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '(o-Me2-TTF(PPh2)2(Mo(CO)4)2 Mo6O19'
_chemical_melting_point          ?
_chemical_formula_moiety         '(C36 H26 Mo O4 P2 S4)2, Mo6 O19'
_chemical_formula_sum            'C72 H52 Mo8 O27 P4 S8'
_chemical_formula_weight         2497.02
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'
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   21.602(4)
_cell_length_b                   11.893(2)
_cell_length_c                   17.225(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.68(3)
_cell_angle_gamma                90.00
_cell_volume                     4423.4(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7998
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      52.1

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2448
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3813
_exptl_absorpt_correction_T_max  0.8683
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Rotation, Phi. incr. = 1.1'
_diffrn_detector_area_resol_mean 6.66
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36239
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.86
_reflns_number_total             8433
_reflns_number_gt                6088
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'EXPOSE [STOE-IPDS]'
_computing_cell_refinement       'SELECT, CELL [STOE-IPDS]'
_computing_data_reduction        'INTEGRATE [STOE-IPDS]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8433
_refine_ls_number_parameters     538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0738
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_restrained_S_all      0.913
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.117168(17) 0.51556(3) 0.63392(2) 0.04457(10) Uani 1 1 d . . .
S1 S 0.31953(4) 0.31899(8) 0.71751(6) 0.0361(2) Uani 1 1 d . . .
S2 S 0.31772(4) 0.52797(8) 0.80557(6) 0.0355(2) Uani 1 1 d . . .
S3 S 0.46475(4) 0.29256(7) 0.75507(6) 0.0332(2) Uani 1 1 d . . .
S4 S 0.46225(5) 0.48254(8) 0.85846(6) 0.0401(2) Uani 1 1 d . . .
P1 P 0.18646(5) 0.35290(8) 0.64914(6) 0.0334(2) Uani 1 1 d . . .
P2 P 0.18201(5) 0.58595(8) 0.74506(6) 0.0344(2) Uani 1 1 d . . .
O1 O 0.1927(3) 0.6357(4) 0.5027(3) 0.141(3) Uani 1 1 d . . .
O2 O 0.0439(3) 0.3912(5) 0.5003(4) 0.174(3) Uani 1 1 d . . .
O3 O 0.0340(2) 0.7330(4) 0.6324(3) 0.1048(15) Uani 1 1 d . . .
O4 O 0.0276(2) 0.3963(4) 0.7507(4) 0.121(2) Uani 1 1 d . . .
C1 C 0.25172(16) 0.3969(3) 0.7125(2) 0.0291(8) Uani 1 1 d . . .
C2 C 0.25030(16) 0.4935(3) 0.7526(2) 0.0298(8) Uani 1 1 d . . .
C3 C 0.35985(17) 0.4119(3) 0.7761(2) 0.0313(8) Uani 1 1 d . . .
C4 C 0.42212(17) 0.3966(3) 0.7955(2) 0.0300(8) Uani 1 1 d . . .
C5 C 0.53439(17) 0.3291(3) 0.7995(2) 0.0334(8) Uani 1 1 d . . .
C6 C 0.53335(17) 0.4171(3) 0.8488(2) 0.0364(9) Uani 1 1 d . . .
C7 C 0.58988(18) 0.2626(3) 0.7779(3) 0.0398(9) Uani 1 1 d . . .
H7A H 0.5776 0.2048 0.7417 0.060 Uiso 1 1 calc R . .
H7B H 0.6083 0.2289 0.8236 0.060 Uiso 1 1 calc R . .
H7C H 0.6194 0.3114 0.7545 0.060 Uiso 1 1 calc R . .
C8 C 0.5873(2) 0.4622(4) 0.8945(3) 0.0571(12) Uani 1 1 d . . .
H8A H 0.5743 0.5249 0.9250 0.086 Uiso 1 1 calc R . .
H8B H 0.6186 0.4862 0.8597 0.086 Uiso 1 1 calc R . .
H8C H 0.6038 0.4045 0.9281 0.086 Uiso 1 1 calc R . .
C9 C 0.1668(3) 0.5912(5) 0.5513(3) 0.0818(19) Uani 1 1 d . . .
C10 C 0.0695(3) 0.4402(6) 0.5484(4) 0.095(2) Uani 1 1 d . . .
C11 C 0.0637(3) 0.6537(4) 0.6328(3) 0.0658(14) Uani 1 1 d . . .
C12 C 0.0598(2) 0.4399(4) 0.7101(4) 0.0702(16) Uani 1 1 d . . .
C13 C 0.22905(17) 0.2873(3) 0.5702(2) 0.0350(9) Uani 1 1 d . . .
C14 C 0.2499(2) 0.1781(4) 0.5748(3) 0.0556(12) Uani 1 1 d . . .
H14 H 0.2387 0.1330 0.6162 0.067 Uiso 1 1 calc R . .
C15 C 0.2873(3) 0.1350(4) 0.5183(3) 0.0676(15) Uani 1 1 d . . .
H15 H 0.3006 0.0607 0.5214 0.081 Uiso 1 1 calc R . .
C16 C 0.3048(2) 0.2009(5) 0.4579(3) 0.0662(15) Uani 1 1 d . . .
H16 H 0.3308 0.1721 0.4207 0.079 Uiso 1 1 calc R . .
C17 C 0.2842(3) 0.3085(5) 0.4520(3) 0.0685(15) Uani 1 1 d . . .
H17 H 0.2955 0.3529 0.4103 0.082 Uiso 1 1 calc R . .
C18 C 0.2465(2) 0.3521(4) 0.5079(3) 0.0532(12) Uani 1 1 d . . .
H18 H 0.2327 0.4259 0.5036 0.064 Uiso 1 1 calc R . .
C19 C 0.15554(18) 0.2326(3) 0.7012(3) 0.0392(9) Uani 1 1 d . . .
C20 C 0.1709(2) 0.2076(4) 0.7771(3) 0.0599(13) Uani 1 1 d . . .
H20 H 0.2006 0.2504 0.8036 0.072 Uiso 1 1 calc R . .
C21 C 0.1424(3) 0.1189(5) 0.8150(4) 0.0825(19) Uani 1 1 d . . .
H21 H 0.1535 0.1030 0.8664 0.099 Uiso 1 1 calc R . .
C22 C 0.0990(3) 0.0560(5) 0.7778(4) 0.0851(19) Uani 1 1 d . . .
H22 H 0.0802 -0.0031 0.8035 0.102 Uiso 1 1 calc R . .
C23 C 0.0828(3) 0.0795(5) 0.7023(4) 0.0820(18) Uani 1 1 d . . .
H23 H 0.0530 0.0358 0.6764 0.098 Uiso 1 1 calc R . .
C24 C 0.1104(2) 0.1683(4) 0.6641(3) 0.0617(13) Uani 1 1 d . . .
H24 H 0.0983 0.1846 0.6130 0.074 Uiso 1 1 calc R . .
C25 C 0.1473(2) 0.5772(4) 0.8403(3) 0.0459(10) Uani 1 1 d . . .
C26 C 0.1030(3) 0.6563(5) 0.8584(3) 0.0757(17) Uani 1 1 d . . .
H26 H 0.0935 0.7138 0.8235 0.091 Uiso 1 1 calc R . .
C27 C 0.0730(3) 0.6507(7) 0.9276(4) 0.099(2) Uani 1 1 d . . .
H27 H 0.0430 0.7039 0.9388 0.119 Uiso 1 1 calc R . .
C28 C 0.0870(4) 0.5680(8) 0.9795(4) 0.119(3) Uani 1 1 d . . .
H28 H 0.0668 0.5648 1.0264 0.143 Uiso 1 1 calc R . .
C29 C 0.1300(4) 0.4908(8) 0.9628(5) 0.150(4) Uani 1 1 d . . .
H29 H 0.1393 0.4337 0.9981 0.179 Uiso 1 1 calc R . .
C30 C 0.1606(3) 0.4958(6) 0.8931(4) 0.095(2) Uani 1 1 d . . .
H30 H 0.1908 0.4425 0.8826 0.113 Uiso 1 1 calc R . .
C31 C 0.21625(19) 0.7264(3) 0.7488(3) 0.0415(10) Uani 1 1 d . . .
C32 C 0.2164(3) 0.7911(4) 0.6822(3) 0.0654(14) Uani 1 1 d . . .
H32 H 0.1989 0.7626 0.6362 0.078 Uiso 1 1 calc R . .
C33 C 0.2421(3) 0.8976(5) 0.6829(4) 0.087(2) Uani 1 1 d . . .
H33 H 0.2424 0.9398 0.6375 0.105 Uiso 1 1 calc R . .
C34 C 0.2668(3) 0.9403(4) 0.7494(5) 0.084(2) Uani 1 1 d . . .
H34 H 0.2836 1.0124 0.7497 0.100 Uiso 1 1 calc R . .
C35 C 0.2674(2) 0.8786(5) 0.8164(4) 0.0761(18) Uani 1 1 d . . .
H35 H 0.2849 0.9083 0.8620 0.091 Uiso 1 1 calc R . .
C36 C 0.2417(2) 0.7714(4) 0.8162(3) 0.0583(13) Uani 1 1 d . . .
H36 H 0.2418 0.7297 0.8619 0.070 Uiso 1 1 calc R . .
Mo2 Mo 0.445894(16) 0.47883(3) 0.382600(19) 0.03392(9) Uani 1 1 d . . .
Mo3 Mo 0.592845(16) 0.47536(3) 0.43738(2) 0.03480(9) Uani 1 1 d . . .
Mo4 Mo 0.493901(17) 0.30775(3) 0.52064(2) 0.03499(9) Uani 1 1 d . . .
O5 O 0.52769(12) 0.4614(2) 0.35300(15) 0.0367(6) Uani 1 1 d . . .
O6 O 0.45904(13) 0.6386(2) 0.38984(15) 0.0368(6) Uani 1 1 d . . .
O7 O 0.38057(12) 0.5068(2) 0.45922(15) 0.0368(6) Uani 1 1 d . . .
O8 O 0.44747(12) 0.32831(19) 0.42492(15) 0.0362(6) Uani 1 1 d . . .
O9 O 0.56738(12) 0.32256(19) 0.46238(15) 0.0363(6) Uani 1 1 d . . .
O10 O 0.57857(12) 0.6328(2) 0.42779(15) 0.0363(6) Uani 1 1 d . . .
O11 O 0.40354(14) 0.4625(2) 0.29960(16) 0.0467(7) Uani 1 1 d . . .
O12 O 0.65817(13) 0.4539(2) 0.38859(17) 0.0471(7) Uani 1 1 d . . .
O13 O 0.48896(15) 0.1685(2) 0.53573(17) 0.0485(7) Uani 1 1 d . . .
O14 O 0.5000 0.5000 0.5000 0.0278(8) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.0385(2) 0.0481(2) 0.0465(2) -0.00356(17) -0.01059(17) 0.01215(16)
S1 0.0260(5) 0.0367(5) 0.0454(6) -0.0059(4) -0.0018(4) 0.0014(4)
S2 0.0295(5) 0.0376(5) 0.0392(6) -0.0059(4) -0.0006(4) -0.0015(4)
S3 0.0321(5) 0.0347(4) 0.0330(5) 0.0001(4) 0.0018(4) -0.0003(4)
S4 0.0304(5) 0.0471(5) 0.0424(6) -0.0117(5) -0.0034(4) 0.0029(4)
P1 0.0269(5) 0.0373(5) 0.0358(6) -0.0019(4) -0.0017(4) 0.0005(4)
P2 0.0308(5) 0.0359(5) 0.0367(6) 0.0003(4) 0.0027(5) 0.0035(4)
O1 0.245(7) 0.093(3) 0.089(4) 0.041(3) 0.074(4) 0.037(4)
O2 0.168(6) 0.164(5) 0.183(6) -0.096(5) -0.121(5) 0.053(4)
O3 0.106(4) 0.082(3) 0.126(4) -0.003(3) -0.006(3) 0.049(3)
O4 0.066(3) 0.097(3) 0.203(6) 0.026(3) 0.072(4) 0.006(2)
C1 0.0247(19) 0.0334(18) 0.029(2) 0.0016(15) 0.0018(16) -0.0017(14)
C2 0.0249(18) 0.0354(19) 0.029(2) 0.0041(15) 0.0031(15) -0.0007(14)
C3 0.032(2) 0.0353(19) 0.027(2) 0.0039(15) 0.0025(16) -0.0025(15)
C4 0.030(2) 0.0352(18) 0.025(2) 0.0043(15) 0.0023(16) -0.0020(15)
C5 0.028(2) 0.040(2) 0.031(2) 0.0086(16) -0.0001(17) 0.0009(15)
C6 0.023(2) 0.049(2) 0.037(2) 0.0040(18) -0.0004(17) -0.0009(16)
C7 0.031(2) 0.042(2) 0.046(3) 0.0072(18) 0.0054(19) 0.0045(17)
C8 0.034(2) 0.072(3) 0.066(3) -0.016(3) -0.008(2) 0.004(2)
C9 0.127(6) 0.066(3) 0.053(4) 0.007(3) 0.012(4) 0.034(3)
C10 0.093(5) 0.090(4) 0.098(5) -0.039(4) -0.054(4) 0.036(4)
C11 0.064(3) 0.065(3) 0.067(4) -0.003(3) -0.016(3) 0.024(3)
C12 0.037(3) 0.061(3) 0.114(5) -0.006(3) 0.017(3) 0.013(2)
C13 0.030(2) 0.040(2) 0.035(2) -0.0100(17) -0.0007(17) -0.0026(16)
C14 0.066(3) 0.055(3) 0.047(3) 0.002(2) 0.010(2) 0.017(2)
C15 0.068(4) 0.066(3) 0.069(4) -0.012(3) 0.004(3) 0.024(3)
C16 0.050(3) 0.090(4) 0.060(4) -0.033(3) 0.015(3) -0.010(3)
C17 0.084(4) 0.069(3) 0.053(3) -0.012(3) 0.025(3) -0.023(3)
C18 0.066(3) 0.044(2) 0.050(3) -0.007(2) 0.013(3) -0.005(2)
C19 0.027(2) 0.047(2) 0.044(3) 0.0029(18) 0.0034(18) -0.0003(17)
C20 0.053(3) 0.069(3) 0.057(3) 0.007(2) -0.001(2) -0.020(2)
C21 0.069(4) 0.103(4) 0.075(4) 0.036(3) -0.001(3) -0.032(3)
C22 0.074(4) 0.082(4) 0.100(5) 0.030(4) 0.006(4) -0.029(3)
C23 0.062(4) 0.077(4) 0.107(5) -0.004(4) 0.002(4) -0.041(3)
C24 0.059(3) 0.066(3) 0.060(3) -0.003(2) -0.003(3) -0.020(2)
C25 0.034(2) 0.067(3) 0.037(3) 0.001(2) 0.0057(19) 0.004(2)
C26 0.075(4) 0.084(4) 0.070(4) 0.002(3) 0.030(3) 0.025(3)
C27 0.071(4) 0.138(6) 0.091(5) -0.028(5) 0.034(4) 0.028(4)
C28 0.095(6) 0.206(9) 0.058(4) 0.017(5) 0.037(4) 0.038(6)
C29 0.148(8) 0.215(10) 0.090(6) 0.079(6) 0.073(6) 0.080(7)
C30 0.090(5) 0.121(5) 0.075(4) 0.044(4) 0.044(4) 0.049(4)
C31 0.036(2) 0.0348(19) 0.054(3) -0.0015(19) 0.006(2) 0.0031(16)
C32 0.075(4) 0.047(3) 0.074(4) 0.009(2) -0.006(3) -0.005(2)
C33 0.099(5) 0.054(3) 0.109(6) 0.023(3) -0.001(4) -0.016(3)
C34 0.064(4) 0.041(3) 0.146(7) -0.006(4) 0.008(4) -0.005(2)
C35 0.054(3) 0.063(3) 0.112(5) -0.032(3) 0.004(3) -0.005(3)
C36 0.053(3) 0.056(3) 0.065(3) -0.012(2) 0.002(3) -0.002(2)
Mo2 0.04059(19) 0.03779(16) 0.02327(18) 0.00231(14) -0.00113(14) 0.00195(14)
Mo3 0.03623(19) 0.03977(17) 0.02884(19) 0.00138(15) 0.00845(15) 0.00194(15)
Mo4 0.0473(2) 0.02575(15) 0.0320(2) 0.00581(13) 0.00327(16) 0.00063(14)
O5 0.0446(16) 0.0389(14) 0.0268(14) 0.0032(11) 0.0058(12) 0.0036(12)
O6 0.0503(17) 0.0332(13) 0.0270(15) 0.0076(11) 0.0030(13) 0.0054(12)
O7 0.0371(15) 0.0418(14) 0.0314(15) 0.0020(11) 0.0005(12) 0.0017(11)
O8 0.0441(16) 0.0337(13) 0.0307(15) -0.0004(11) 0.0007(12) -0.0029(11)
O9 0.0413(16) 0.0329(13) 0.0349(16) 0.0005(11) 0.0068(12) 0.0058(11)
O10 0.0426(16) 0.0342(13) 0.0328(15) 0.0038(11) 0.0105(13) -0.0008(11)
O11 0.0545(19) 0.0540(17) 0.0312(16) -0.0004(13) -0.0076(14) 0.0035(14)
O12 0.0422(17) 0.0551(17) 0.0450(18) -0.0020(13) 0.0176(14) 0.0016(13)
O13 0.065(2) 0.0325(14) 0.0484(19) 0.0088(12) 0.0042(16) 0.0011(13)
O14 0.0340(19) 0.0293(17) 0.0202(18) 0.0021(13) 0.0037(15) 0.0039(14)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C10 1.985(6) . ?
Mo1 C11 2.008(5) . ?
Mo1 C9 2.019(7) . ?
Mo1 C12 2.040(6) . ?
Mo1 P1 2.4553(11) . ?
Mo1 P2 2.4840(13) . ?
S1 C3 1.716(4) . ?
S1 C1 1.734(4) . ?
S2 C3 1.738(4) . ?
S2 C2 1.745(4) . ?
S3 C4 1.703(4) . ?
S3 C5 1.723(4) . ?
S4 C4 1.708(4) . ?
S4 C6 1.735(4) . ?
P1 C19 1.826(4) . ?
P1 C1 1.834(4) . ?
P1 C13 1.838(4) . ?
P2 C25 1.826(4) . ?
P2 C31 1.827(4) . ?
P2 C2 1.841(4) . ?
O1 C9 1.148(7) . ?
O2 C10 1.144(7) . ?
O3 C11 1.141(6) . ?
O4 C12 1.127(7) . ?
C1 C2 1.341(5) . ?
C3 C4 1.388(5) . ?
C5 C6 1.348(5) . ?
C5 C7 1.492(5) . ?
C6 C8 1.487(6) . ?
C13 C14 1.376(6) . ?
C13 C18 1.382(6) . ?
C14 C15 1.382(7) . ?
C15 C16 1.365(8) . ?
C16 C17 1.357(8) . ?
C17 C18 1.380(7) . ?
C19 C20 1.371(6) . ?
C19 C24 1.382(6) . ?
C20 C21 1.392(7) . ?
C21 C22 1.346(8) . ?
C22 C23 1.366(9) . ?
C23 C24 1.388(7) . ?
C25 C30 1.353(7) . ?
C25 C26 1.385(6) . ?
C26 C27 1.374(8) . ?
C27 C28 1.357(10) . ?
C28 C29 1.343(10) . ?
C29 C30 1.389(8) . ?
C31 C36 1.378(6) . ?
C31 C32 1.382(6) . ?
C32 C33 1.384(7) . ?
C33 C34 1.349(9) . ?
C34 C35 1.368(9) . ?
C35 C36 1.391(7) . ?
Mo2 O11 1.686(3) . ?
Mo2 O5 1.865(3) . ?
Mo2 O6 1.925(2) . ?
Mo2 O8 1.933(2) . ?
Mo2 O7 1.988(3) . ?
Mo2 O14 2.3195(7) . ?
Mo3 O12 1.683(3) . ?
Mo3 O7 1.867(3) 3_666 ?
Mo3 O10 1.904(2) . ?
Mo3 O9 1.951(2) . ?
Mo3 O5 2.000(3) . ?
Mo3 O14 2.3236(7) . ?
Mo4 O13 1.681(2) . ?
Mo4 O9 1.911(3) . ?
Mo4 O8 1.920(3) . ?
Mo4 O6 1.930(3) 3_666 ?
Mo4 O10 1.955(3) 3_666 ?
Mo4 O14 2.3182(5) . ?
O6 Mo4 1.930(3) 3_666 ?
O7 Mo3 1.867(3) 3_666 ?
O10 Mo4 1.955(3) 3_666 ?
O14 Mo4 2.3182(5) 3_666 ?
O14 Mo2 2.3195(7) 3_666 ?
O14 Mo3 2.3235(7) 3_666 ?
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
C10 Mo1 C11 94.4(2) . . ?
C10 Mo1 C9 87.3(3) . . ?
C11 Mo1 C9 86.9(2) . . ?
C10 Mo1 C12 88.1(3) . . ?
C11 Mo1 C12 90.4(2) . . ?
C9 Mo1 C12 174.5(3) . . ?
C10 Mo1 P1 91.40(17) . . ?
C11 Mo1 P1 173.88(16) . . ?
C9 Mo1 P1 95.24(16) . . ?
C12 Mo1 P1 87.90(14) . . ?
C10 Mo1 P2 172.76(18) . . ?
C11 Mo1 P2 92.44(16) . . ?
C9 Mo1 P2 95.4(2) . . ?
C12 Mo1 P2 89.56(18) . . ?
P1 Mo1 P2 81.67(4) . . ?
C3 S1 C1 95.65(18) . . ?
C3 S2 C2 95.56(17) . . ?
C4 S3 C5 96.36(18) . . ?
C4 S4 C6 95.99(19) . . ?
C19 P1 C1 102.56(18) . . ?
C19 P1 C13 103.22(18) . . ?
C1 P1 C13 99.73(17) . . ?
C19 P1 Mo1 116.06(13) . . ?
C1 P1 Mo1 107.10(12) . . ?
C13 P1 Mo1 124.92(14) . . ?
C25 P2 C31 101.3(2) . . ?
C25 P2 C2 104.56(18) . . ?
C31 P2 C2 102.75(17) . . ?
C25 P2 Mo1 115.86(15) . . ?
C31 P2 Mo1 123.64(15) . . ?
C2 P2 Mo1 106.60(13) . . ?
C2 C1 S1 117.7(3) . . ?
C2 C1 P1 121.5(3) . . ?
S1 C1 P1 120.7(2) . . ?
C1 C2 S2 116.0(3) . . ?
C1 C2 P2 120.4(3) . . ?
S2 C2 P2 123.5(2) . . ?
C4 C3 S1 121.9(3) . . ?
C4 C3 S2 123.1(3) . . ?
S1 C3 S2 115.0(2) . . ?
C3 C4 S3 121.9(3) . . ?
C3 C4 S4 123.0(3) . . ?
S3 C4 S4 115.1(2) . . ?
C6 C5 C7 126.6(4) . . ?
C6 C5 S3 116.4(3) . . ?
C7 C5 S3 116.9(3) . . ?
C5 C6 C8 125.9(4) . . ?
C5 C6 S4 116.1(3) . . ?
C8 C6 S4 118.0(3) . . ?
O1 C9 Mo1 177.0(7) . . ?
O2 C10 Mo1 176.1(6) . . ?
O3 C11 Mo1 179.1(5) . . ?
O4 C12 Mo1 178.3(6) . . ?
C14 C13 C18 118.4(4) . . ?
C14 C13 P1 121.9(3) . . ?
C18 C13 P1 119.4(3) . . ?
C13 C14 C15 120.4(5) . . ?
C16 C15 C14 120.3(5) . . ?
C17 C16 C15 120.0(5) . . ?
C16 C17 C18 120.1(5) . . ?
C17 C18 C13 120.8(4) . . ?
C20 C19 C24 117.9(4) . . ?
C20 C19 P1 123.8(3) . . ?
C24 C19 P1 118.0(4) . . ?
C19 C20 C21 120.9(5) . . ?
C22 C21 C20 120.6(6) . . ?
C21 C22 C23 119.6(5) . . ?
C22 C23 C24 120.3(5) . . ?
C19 C24 C23 120.6(5) . . ?
C30 C25 C26 118.0(5) . . ?
C30 C25 P2 124.1(4) . . ?
C26 C25 P2 117.9(4) . . ?
C27 C26 C25 120.6(6) . . ?
C28 C27 C26 120.3(6) . . ?
C29 C28 C27 119.7(6) . . ?
C28 C29 C30 120.4(7) . . ?
C25 C30 C29 120.9(6) . . ?
C36 C31 C32 118.3(4) . . ?
C36 C31 P2 122.4(4) . . ?
C32 C31 P2 119.3(4) . . ?
C31 C32 C33 120.8(6) . . ?
C34 C33 C32 120.1(6) . . ?
C33 C34 C35 120.5(5) . . ?
C34 C35 C36 119.8(6) . . ?
C31 C36 C35 120.5(5) . . ?
O11 Mo2 O5 104.50(13) . . ?
O11 Mo2 O6 104.12(12) . . ?
O5 Mo2 O6 89.33(11) . . ?
O11 Mo2 O8 102.50(12) . . ?
O5 Mo2 O8 89.64(11) . . ?
O6 Mo2 O8 152.75(11) . . ?
O11 Mo2 O7 101.78(13) . . ?
O5 Mo2 O7 153.73(11) . . ?
O6 Mo2 O7 84.16(10) . . ?
O8 Mo2 O7 84.81(10) . . ?
O11 Mo2 O14 177.33(10) . . ?
O5 Mo2 O14 78.07(9) . . ?
O6 Mo2 O14 76.51(8) . . ?
O8 Mo2 O14 76.63(8) . . ?
O7 Mo2 O14 75.67(8) . . ?
O12 Mo3 O7 104.75(14) . 3_666 ?
O12 Mo3 O10 104.00(12) . . ?
O7 Mo3 O10 90.88(11) 3_666 . ?
O12 Mo3 O9 102.41(12) . . ?
O7 Mo3 O9 88.63(11) 3_666 . ?
O10 Mo3 O9 152.79(11) . . ?
O12 Mo3 O5 101.95(13) . . ?
O7 Mo3 O5 153.20(11) 3_666 . ?
O10 Mo3 O5 84.84(11) . . ?
O9 Mo3 O5 83.46(11) . . ?
O12 Mo3 O14 177.17(11) . . ?
O7 Mo3 O14 77.78(8) 3_666 . ?
O10 Mo3 O14 77.08(8) . . ?
O9 Mo3 O14 76.24(7) . . ?
O5 Mo3 O14 75.48(7) . . ?
O13 Mo4 O9 103.28(13) . . ?
O13 Mo4 O8 102.97(13) . . ?
O9 Mo4 O8 87.61(12) . . ?
O13 Mo4 O6 103.68(13) . 3_666 ?
O9 Mo4 O6 87.88(11) . 3_666 ?
O8 Mo4 O6 153.31(10) . 3_666 ?
O13 Mo4 O10 103.34(13) . 3_666 ?
O9 Mo4 O10 153.38(10) . 3_666 ?
O8 Mo4 O10 86.51(11) . 3_666 ?
O6 Mo4 O10 85.84(11) 3_666 3_666 ?
O13 Mo4 O14 179.61(11) . . ?
O9 Mo4 O14 77.10(7) . . ?
O8 Mo4 O14 76.90(7) . . ?
O6 Mo4 O14 76.44(7) 3_666 . ?
O10 Mo4 O14 76.28(7) 3_666 . ?
Mo2 O5 Mo3 116.38(13) . . ?
Mo2 O6 Mo4 116.82(12) . 3_666 ?
Mo3 O7 Mo2 116.60(14) 3_666 . ?
Mo4 O8 Mo2 116.41(12) . . ?
Mo4 O9 Mo3 116.48(12) . . ?
Mo3 O10 Mo4 116.49(12) . 3_666 ?
Mo4 O14 Mo4 180.0 3_666 . ?
Mo4 O14 Mo2 90.160(12) 3_666 . ?
Mo4 O14 Mo2 89.839(13) . . ?
Mo4 O14 Mo2 89.841(13) 3_666 3_666 ?
Mo4 O14 Mo2 90.160(12) . 3_666 ?
Mo2 O14 Mo2 180.0 . 3_666 ?
Mo4 O14 Mo3 90.030(13) 3_666 3_666 ?
Mo4 O14 Mo3 89.969(13) . 3_666 ?
Mo2 O14 Mo3 89.93(2) . 3_666 ?
Mo2 O14 Mo3 90.07(2) 3_666 3_666 ?
Mo4 O14 Mo3 89.970(13) 3_666 . ?
Mo4 O14 Mo3 90.031(13) . . ?
Mo2 O14 Mo3 90.07(2) . . ?
Mo2 O14 Mo3 89.93(2) 3_666 . ?
Mo3 O14 Mo3 180.000(15) 3_666 . ?
_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.86
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.090