Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_publ_contact_author_name        'Dr. Lisa Rosenberg'
_publ_contact_author_address     
; Department of Chemistry
University of Victoria
P.O. Box 3065
Victoria, British Columbia V8W 3V6
Canada
;
_publ_contact_author_email       lisarose@uvic.ca
_publ_contact_author_fax         1(250)7217147
_publ_contact_author_phone       1(250)7217173
_publ_contact_letter             
; To: Cambridge Crystallographic Data Centre
Please accept the following CIF data for a structure to be
published in Dalton Transactions. Please forward any questions
concerning this CIF to Bob McDonald (Bob.McDonald@ualberta.ca).
;
_publ_section_title              
; Structure and molybdenum coordination chemistry of tripodal
tris(phosphine) ligands with dimethylsilyl "elbow" groups'
;
loop_
_publ_author_name
_publ_author_footnote
_publ_author_address
D.M.Friesen .
; Department of Chemistry
University of Victoria
P.O. Box 3065
Victoria, British Columbia V8W 3V6
Canada
;
O.Bowles .
; Department of Chemistry
University of Victoria
P.O. Box 3065
Victoria, British Columbia V8W 3V6
Canada
;
R.McDonald .
; X-ray Crystallography Laboratory
Department of Chemistry
University of Alberta
Edmonton, Alberta T6G 2G2
Canada
;
L.Rosenberg .
; Department of Chemistry
University of Victoria
P.O. Box 3065
Victoria, British Columbia V8W 3V6
Canada
;

# Attachment 'lr051026.cif'

data_3b
_database_code_depnum_ccdc_archive 'CCDC 289572'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_formula_moiety         'C44 H51 P3 Si3'
_chemical_formula_sum            'C44 H51 P3 Si3'
_chemical_formula_weight         757.03

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   12.2968(11)
_cell_length_b                   13.0128(12)
_cell_length_c                   13.7299(12)
_cell_angle_alpha                104.2431(15)
_cell_angle_beta                 100.4996(14)
_cell_angle_gamma                95.9048(14)
_cell_volume                     2068.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    6375
_cell_measurement_theta_min      2.523
_cell_measurement_theta_max      26.348

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             804
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.8982
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(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 PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            10365
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         26.39
_reflns_number_total             8299
_reflns_number_gt                5997
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'

_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^)+(0.0731P)^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         8299
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1260
_refine_ls_wR_factor_gt          0.1149
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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
P1 P 0.17943(5) 0.21433(5) 0.31371(5) 0.02901(15) Uani 1 1 d . . .
P2 P 0.26916(5) 0.31584(5) 0.84358(5) 0.02812(15) Uani 1 1 d . . .
P3 P 0.32258(5) 0.08331(5) 0.68689(5) 0.03067(16) Uani 1 1 d . . .
Si1 Si 0.22292(5) 0.34434(5) 0.46994(5) 0.02633(16) Uani 1 1 d . . .
Si2 Si 0.20495(5) 0.37071(5) 0.69990(5) 0.02619(16) Uani 1 1 d . . .
Si3 Si 0.35334(5) 0.20772(5) 0.59690(5) 0.02575(16) Uani 1 1 d . . .
C1 C 0.22067(17) 0.27232(18) 0.57642(16) 0.0238(5) Uani 1 1 d . . .
C2 C 0.11629(18) 0.18162(19) 0.53802(17) 0.0292(5) Uani 1 1 d . . .
H2A H 0.1123 0.1430 0.5905 0.035 Uiso 1 1 calc R . .
H2B H 0.1232 0.1315 0.4741 0.035 Uiso 1 1 calc R . .
H2C H 0.0481 0.2136 0.5254 0.035 Uiso 1 1 calc R . .
C3 C 0.3619(2) 0.4257(2) 0.48155(19) 0.0358(6) Uani 1 1 d . . .
H3A H 0.4203 0.3800 0.4840 0.043 Uiso 1 1 calc R . .
H3B H 0.3785 0.4848 0.5447 0.043 Uiso 1 1 calc R . .
H3C H 0.3595 0.4550 0.4220 0.043 Uiso 1 1 calc R . .
C4 C 0.1161(2) 0.4366(2) 0.46675(19) 0.0400(6) Uani 1 1 d . . .
H4A H 0.0420 0.3968 0.4608 0.048 Uiso 1 1 calc R . .
H4B H 0.1153 0.4661 0.4075 0.048 Uiso 1 1 calc R . .
H4C H 0.1349 0.4954 0.5302 0.048 Uiso 1 1 calc R . .
C5 C 0.2963(2) 0.5029(2) 0.72781(19) 0.0346(6) Uani 1 1 d . . .
H5A H 0.3743 0.4917 0.7306 0.042 Uiso 1 1 calc R . .
H5B H 0.2898 0.5488 0.7941 0.042 Uiso 1 1 calc R . .
H5C H 0.2727 0.5376 0.6734 0.042 Uiso 1 1 calc R . .
C6 C 0.0583(2) 0.4017(2) 0.69620(19) 0.0387(6) Uani 1 1 d . . .
H6A H 0.0063 0.3348 0.6818 0.046 Uiso 1 1 calc R . .
H6B H 0.0376 0.4375 0.6420 0.046 Uiso 1 1 calc R . .
H6C H 0.0547 0.4489 0.7628 0.046 Uiso 1 1 calc R . .
C7 C 0.3881(2) 0.1390(2) 0.47235(18) 0.0344(6) Uani 1 1 d . . .
H7A H 0.3237 0.0863 0.4299 0.041 Uiso 1 1 calc R . .
H7B H 0.4527 0.1025 0.4861 0.041 Uiso 1 1 calc R . .
H7C H 0.4060 0.1923 0.4358 0.041 Uiso 1 1 calc R . .
C8 C 0.47828(19) 0.3081(2) 0.67434(18) 0.0337(6) Uani 1 1 d . . .
H8A H 0.4624 0.3454 0.7402 0.040 Uiso 1 1 calc R . .
H8B H 0.4951 0.3603 0.6364 0.040 Uiso 1 1 calc R . .
H8C H 0.5428 0.2711 0.6869 0.040 Uiso 1 1 calc R . .
C11 C 0.28558(19) 0.2589(2) 0.24802(17) 0.0288(5) Uani 1 1 d . . .
C12 C 0.3553(2) 0.1860(2) 0.21601(18) 0.0363(6) Uani 1 1 d . . .
H12 H 0.3454 0.1172 0.2281 0.044 Uiso 1 1 calc R . .
C13 C 0.4388(2) 0.2112(2) 0.1670(2) 0.0438(7) Uani 1 1 d . . .
H13 H 0.4861 0.1603 0.1466 0.053 Uiso 1 1 calc R . .
C14 C 0.4536(2) 0.3096(2) 0.1475(2) 0.0427(7) Uani 1 1 d . . .
H14 H 0.5101 0.3265 0.1127 0.051 Uiso 1 1 calc R . .
C15 C 0.3860(2) 0.3837(2) 0.17883(18) 0.0395(6) Uani 1 1 d . . .
H15 H 0.3966 0.4522 0.1661 0.047 Uiso 1 1 calc R . .
C16 C 0.3025(2) 0.3590(2) 0.22891(17) 0.0334(6) Uani 1 1 d . . .
H16 H 0.2566 0.4108 0.2504 0.040 Uiso 1 1 calc R . .
C21 C 0.0476(2) 0.2448(2) 0.24754(18) 0.0324(6) Uani 1 1 d . . .
C22 C 0.0346(2) 0.2753(2) 0.15684(19) 0.0407(6) Uani 1 1 d . . .
H22 H 0.0985 0.2890 0.1294 0.049 Uiso 1 1 calc R . .
C23 C -0.0697(2) 0.2860(3) 0.1052(2) 0.0506(8) Uani 1 1 d . . .
H23 H -0.0768 0.3063 0.0428 0.061 Uiso 1 1 calc R . .
C24 C -0.1627(2) 0.2674(3) 0.1442(2) 0.0511(8) Uani 1 1 d . . .
H24 H -0.2340 0.2764 0.1098 0.061 Uiso 1 1 calc R . .
C25 C -0.1520(2) 0.2357(3) 0.2335(2) 0.0573(9) Uani 1 1 d . . .
H25 H -0.2163 0.2217 0.2602 0.069 Uiso 1 1 calc R . .
C26 C -0.0478(2) 0.2239(3) 0.2848(2) 0.0479(7) Uani 1 1 d . . .
H26 H -0.0416 0.2014 0.3461 0.058 Uiso 1 1 calc R . .
C31 C 0.1643(2) 0.21182(19) 0.85659(17) 0.0301(5) Uani 1 1 d . . .
C32 C 0.1947(2) 0.1691(2) 0.9394(2) 0.0409(6) Uani 1 1 d . . .
H32 H 0.2625 0.1997 0.9884 0.049 Uiso 1 1 calc R . .
C33 C 0.1282(3) 0.0833(3) 0.9515(2) 0.0570(8) Uani 1 1 d . . .
H33 H 0.1498 0.0559 1.0090 0.068 Uiso 1 1 calc R . .
C34 C 0.0305(3) 0.0372(3) 0.8804(3) 0.0613(9) Uani 1 1 d . . .
H34 H -0.0144 -0.0233 0.8876 0.074 Uiso 1 1 calc R . .
C35 C -0.0020(3) 0.0791(3) 0.7988(2) 0.0545(8) Uani 1 1 d . . .
H35 H -0.0702 0.0484 0.7503 0.065 Uiso 1 1 calc R . .
C36 C 0.0646(2) 0.1661(2) 0.7870(2) 0.0410(6) Uani 1 1 d . . .
H36 H 0.0414 0.1946 0.7305 0.049 Uiso 1 1 calc R . .
C41 C 0.2524(2) 0.4330(2) 0.94325(17) 0.0299(5) Uani 1 1 d . . .
C42 C 0.1599(2) 0.4387(2) 0.98895(18) 0.0347(6) Uani 1 1 d . . .
H42 H 0.0987 0.3815 0.9651 0.042 Uiso 1 1 calc R . .
C43 C 0.1562(3) 0.5269(2) 1.0690(2) 0.0485(7) Uani 1 1 d . . .
H43 H 0.0932 0.5289 1.1001 0.058 Uiso 1 1 calc R . .
C44 C 0.2428(3) 0.6110(2) 1.1032(2) 0.0551(8) Uani 1 1 d . . .
H44 H 0.2396 0.6710 1.1578 0.066 Uiso 1 1 calc R . .
C45 C 0.3339(3) 0.6088(2) 1.0589(2) 0.0517(8) Uani 1 1 d . . .
H45 H 0.3929 0.6681 1.0815 0.062 Uiso 1 1 calc R . .
C46 C 0.3404(2) 0.5193(2) 0.98017(19) 0.0413(7) Uani 1 1 d . . .
H46 H 0.4051 0.5172 0.9515 0.050 Uiso 1 1 calc R . .
C51 C 0.4638(2) 0.0910(2) 0.76431(18) 0.0327(6) Uani 1 1 d . . .
C52 C 0.5606(2) 0.0893(2) 0.72432(19) 0.0354(6) Uani 1 1 d . . .
H52 H 0.5554 0.0839 0.6533 0.043 Uiso 1 1 calc R . .
C53 C 0.6639(2) 0.0953(2) 0.7872(2) 0.0427(7) Uani 1 1 d . . .
H53 H 0.7290 0.0952 0.7592 0.051 Uiso 1 1 calc R . .
C54 C 0.6733(2) 0.1016(2) 0.8900(2) 0.0481(7) Uani 1 1 d . . .
H54 H 0.7445 0.1054 0.9327 0.058 Uiso 1 1 calc R . .
C55 C 0.5788(3) 0.1023(2) 0.9305(2) 0.0479(7) Uani 1 1 d . . .
H55 H 0.5847 0.1060 1.0013 0.057 Uiso 1 1 calc R . .
C56 C 0.4749(2) 0.0977(2) 0.86850(19) 0.0423(7) Uani 1 1 d . . .
H56 H 0.4105 0.0991 0.8975 0.051 Uiso 1 1 calc R . .
C61 C 0.30498(19) -0.0491(2) 0.59412(19) 0.0316(5) Uani 1 1 d . . .
C62 C 0.2273(2) -0.0772(2) 0.5005(2) 0.0463(7) Uani 1 1 d . . .
H62 H 0.1877 -0.0240 0.4811 0.056 Uiso 1 1 calc R . .
C63 C 0.2061(3) -0.1796(3) 0.4354(3) 0.0555(8) Uani 1 1 d . . .
H63 H 0.1542 -0.1953 0.3714 0.067 Uiso 1 1 calc R . .
C64 C 0.2604(3) -0.2596(2) 0.4630(3) 0.0554(8) Uani 1 1 d . . .
H64 H 0.2455 -0.3305 0.4187 0.066 Uiso 1 1 calc R . .
C65 C 0.3361(2) -0.2349(2) 0.5556(3) 0.0554(8) Uani 1 1 d . . .
H65 H 0.3736 -0.2891 0.5757 0.066 Uiso 1 1 calc R . .
C66 C 0.3579(2) -0.1315(2) 0.6197(2) 0.0413(6) Uani 1 1 d . . .
H66 H 0.4106 -0.1162 0.6832 0.050 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
P1 0.0328(3) 0.0294(4) 0.0249(3) 0.0097(3) 0.0043(2) 0.0029(3)
P2 0.0272(3) 0.0327(4) 0.0264(3) 0.0117(3) 0.0054(2) 0.0048(3)
P3 0.0329(3) 0.0328(4) 0.0307(3) 0.0123(3) 0.0089(3) 0.0120(3)
Si1 0.0291(3) 0.0268(4) 0.0240(3) 0.0098(3) 0.0036(3) 0.0048(3)
Si2 0.0274(3) 0.0287(4) 0.0239(3) 0.0086(3) 0.0060(3) 0.0068(3)
Si3 0.0256(3) 0.0281(4) 0.0238(3) 0.0075(3) 0.0040(2) 0.0069(3)
C1 0.0241(11) 0.0259(12) 0.0214(11) 0.0065(9) 0.0035(9) 0.0057(9)
C2 0.0285(12) 0.0323(14) 0.0283(12) 0.0109(10) 0.0063(10) 0.0043(10)
C3 0.0413(14) 0.0352(15) 0.0284(13) 0.0105(11) 0.0037(11) -0.0026(11)
C4 0.0482(16) 0.0424(17) 0.0331(14) 0.0141(12) 0.0057(12) 0.0203(13)
C5 0.0455(15) 0.0290(14) 0.0291(13) 0.0078(10) 0.0077(11) 0.0056(11)
C6 0.0358(14) 0.0476(17) 0.0354(14) 0.0119(12) 0.0077(11) 0.0168(12)
C7 0.0370(13) 0.0393(15) 0.0285(12) 0.0066(11) 0.0102(10) 0.0133(12)
C8 0.0277(12) 0.0381(15) 0.0330(13) 0.0083(11) 0.0022(10) 0.0056(11)
C11 0.0335(12) 0.0307(14) 0.0209(11) 0.0077(10) 0.0021(9) 0.0039(10)
C12 0.0495(16) 0.0339(15) 0.0293(13) 0.0128(11) 0.0088(11) 0.0130(12)
C13 0.0447(16) 0.0564(19) 0.0374(15) 0.0166(13) 0.0147(12) 0.0194(14)
C14 0.0381(14) 0.059(2) 0.0318(14) 0.0146(13) 0.0105(11) -0.0015(13)
C15 0.0480(16) 0.0377(16) 0.0283(13) 0.0131(11) -0.0010(11) -0.0070(13)
C16 0.0409(14) 0.0321(14) 0.0266(12) 0.0101(10) 0.0015(10) 0.0081(11)
C21 0.0324(13) 0.0352(15) 0.0256(12) 0.0049(10) 0.0019(10) 0.0031(11)
C22 0.0377(14) 0.0503(18) 0.0336(14) 0.0145(12) 0.0024(11) 0.0062(13)
C23 0.0514(18) 0.058(2) 0.0371(15) 0.0151(14) -0.0071(13) 0.0085(15)
C24 0.0390(16) 0.059(2) 0.0426(16) -0.0006(14) -0.0072(13) 0.0160(14)
C25 0.0329(15) 0.084(3) 0.0467(18) 0.0038(16) 0.0071(13) 0.0072(15)
C26 0.0382(15) 0.070(2) 0.0331(14) 0.0151(14) 0.0045(12) 0.0024(14)
C31 0.0352(13) 0.0269(13) 0.0288(12) 0.0048(10) 0.0129(10) 0.0044(10)
C32 0.0535(17) 0.0385(16) 0.0318(13) 0.0117(12) 0.0103(12) 0.0048(13)
C33 0.082(2) 0.0457(19) 0.0519(18) 0.0243(15) 0.0242(17) 0.0044(17)
C34 0.085(2) 0.0382(18) 0.061(2) 0.0082(15) 0.0348(19) -0.0113(17)
C35 0.0529(18) 0.052(2) 0.0497(18) 0.0025(15) 0.0169(14) -0.0140(15)
C36 0.0384(14) 0.0465(17) 0.0363(14) 0.0100(12) 0.0090(11) -0.0004(12)
C41 0.0364(13) 0.0292(14) 0.0228(11) 0.0123(10) -0.0026(10) 0.0030(10)
C42 0.0397(14) 0.0323(15) 0.0301(13) 0.0068(11) 0.0036(11) 0.0076(11)
C43 0.067(2) 0.0450(18) 0.0347(15) 0.0098(13) 0.0088(14) 0.0229(16)
C44 0.089(2) 0.0358(17) 0.0326(15) 0.0054(12) -0.0038(16) 0.0158(17)
C45 0.076(2) 0.0297(16) 0.0346(15) 0.0115(12) -0.0178(15) -0.0114(14)
C46 0.0449(15) 0.0427(17) 0.0325(14) 0.0180(12) -0.0061(11) -0.0045(13)
C51 0.0374(13) 0.0273(14) 0.0337(13) 0.0095(10) 0.0031(11) 0.0114(11)
C52 0.0397(14) 0.0325(15) 0.0351(14) 0.0096(11) 0.0063(11) 0.0122(11)
C53 0.0398(15) 0.0348(16) 0.0497(17) 0.0072(12) 0.0034(12) 0.0112(12)
C54 0.0496(17) 0.0371(17) 0.0480(17) 0.0054(13) -0.0095(14) 0.0138(13)
C55 0.0637(19) 0.0461(18) 0.0286(14) 0.0084(12) -0.0039(13) 0.0142(15)
C56 0.0543(17) 0.0413(17) 0.0327(14) 0.0099(12) 0.0086(12) 0.0161(13)
C61 0.0292(12) 0.0316(14) 0.0378(13) 0.0129(11) 0.0115(10) 0.0053(10)
C62 0.0447(16) 0.0361(16) 0.0532(17) 0.0102(13) 0.0005(13) 0.0065(13)
C63 0.0520(18) 0.0415(19) 0.061(2) 0.0053(15) 0.0001(15) -0.0062(15)
C64 0.0499(18) 0.0320(17) 0.077(2) -0.0003(15) 0.0212(16) -0.0029(14)
C65 0.0458(17) 0.0345(17) 0.088(2) 0.0172(16) 0.0175(17) 0.0111(14)
C66 0.0389(14) 0.0353(16) 0.0525(16) 0.0157(13) 0.0101(12) 0.0087(12)

_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
P1 C21 1.840(2) . ?
P1 C11 1.840(2) . ?
P1 Si1 2.3151(9) . ?
P2 C31 1.836(2) . ?
P2 C41 1.839(2) . ?
P2 Si2 2.2948(9) . ?
P3 C61 1.839(3) . ?
P3 C51 1.842(2) . ?
P3 Si3 2.3063(9) . ?
Si1 C4 1.871(3) . ?
Si1 C3 1.874(3) . ?
Si1 C1 1.923(2) . ?
Si2 C5 1.868(3) . ?
Si2 C6 1.882(2) . ?
Si2 C1 1.911(2) . ?
Si3 C7 1.870(2) . ?
Si3 C8 1.872(2) . ?
Si3 C1 1.918(2) . ?
C1 C2 1.567(3) . ?
C11 C12 1.389(3) . ?
C11 C16 1.393(3) . ?
C12 C13 1.380(4) . ?
C13 C14 1.372(4) . ?
C14 C15 1.377(4) . ?
C15 C16 1.389(4) . ?
C21 C22 1.384(3) . ?
C21 C26 1.391(4) . ?
C22 C23 1.387(4) . ?
C23 C24 1.373(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.388(4) . ?
C31 C36 1.384(3) . ?
C31 C32 1.393(4) . ?
C32 C33 1.377(4) . ?
C33 C34 1.376(5) . ?
C34 C35 1.377(5) . ?
C35 C36 1.387(4) . ?
C41 C42 1.395(3) . ?
C41 C46 1.399(3) . ?
C42 C43 1.392(4) . ?
C43 C44 1.370(4) . ?
C44 C45 1.369(5) . ?
C45 C46 1.400(4) . ?
C51 C56 1.392(3) . ?
C51 C52 1.399(3) . ?
C52 C53 1.382(4) . ?
C53 C54 1.376(4) . ?
C54 C55 1.377(4) . ?
C55 C56 1.386(4) . ?
C61 C66 1.394(4) . ?
C61 C62 1.395(4) . ?
C62 C63 1.378(4) . ?
C63 C64 1.385(5) . ?
C64 C65 1.376(5) . ?
C65 C66 1.383(4) . ?

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
C21 P1 C11 104.64(11) . . ?
C21 P1 Si1 103.48(8) . . ?
C11 P1 Si1 101.75(8) . . ?
C31 P2 C41 101.34(11) . . ?
C31 P2 Si2 110.01(8) . . ?
C41 P2 Si2 99.37(8) . . ?
C61 P3 C51 101.32(11) . . ?
C61 P3 Si3 106.05(8) . . ?
C51 P3 Si3 101.72(9) . . ?
C4 Si1 C3 107.11(13) . . ?
C4 Si1 C1 112.36(11) . . ?
C3 Si1 C1 113.51(11) . . ?
C4 Si1 P1 107.47(9) . . ?
C3 Si1 P1 108.59(8) . . ?
C1 Si1 P1 107.60(7) . . ?
C5 Si2 C6 105.82(12) . . ?
C5 Si2 C1 112.21(11) . . ?
C6 Si2 C1 113.37(10) . . ?
C5 Si2 P2 101.70(8) . . ?
C6 Si2 P2 110.69(9) . . ?
C1 Si2 P2 112.26(7) . . ?
C7 Si3 C8 107.72(11) . . ?
C7 Si3 C1 112.09(10) . . ?
C8 Si3 C1 112.19(11) . . ?
C7 Si3 P3 109.15(9) . . ?
C8 Si3 P3 107.82(9) . . ?
C1 Si3 P3 107.77(7) . . ?
C2 C1 Si2 109.00(14) . . ?
C2 C1 Si3 108.79(15) . . ?
Si2 C1 Si3 112.09(11) . . ?
C2 C1 Si1 107.10(14) . . ?
Si2 C1 Si1 110.03(11) . . ?
Si3 C1 Si1 109.69(11) . . ?
C12 C11 C16 117.7(2) . . ?
C12 C11 P1 116.46(19) . . ?
C16 C11 P1 125.84(19) . . ?
C13 C12 C11 121.5(3) . . ?
C14 C13 C12 120.2(3) . . ?
C13 C14 C15 119.6(2) . . ?
C14 C15 C16 120.4(3) . . ?
C15 C16 C11 120.6(2) . . ?
C22 C21 C26 117.9(2) . . ?
C22 C21 P1 124.31(19) . . ?
C26 C21 P1 117.4(2) . . ?
C21 C22 C23 121.3(3) . . ?
C24 C23 C22 120.2(3) . . ?
C23 C24 C25 119.5(3) . . ?
C24 C25 C26 120.5(3) . . ?
C25 C26 C21 120.7(3) . . ?
C36 C31 C32 118.1(2) . . ?
C36 C31 P2 125.9(2) . . ?
C32 C31 P2 115.70(19) . . ?
C33 C32 C31 121.2(3) . . ?
C34 C33 C32 120.1(3) . . ?
C33 C34 C35 119.7(3) . . ?
C34 C35 C36 120.2(3) . . ?
C31 C36 C35 120.7(3) . . ?
C42 C41 C46 117.7(2) . . ?
C42 C41 P2 123.91(19) . . ?
C46 C41 P2 118.3(2) . . ?
C43 C42 C41 120.9(3) . . ?
C44 C43 C42 120.4(3) . . ?
C45 C44 C43 120.2(3) . . ?
C44 C45 C46 120.1(3) . . ?
C41 C46 C45 120.7(3) . . ?
C56 C51 C52 117.9(2) . . ?
C56 C51 P3 118.2(2) . . ?
C52 C51 P3 123.86(19) . . ?
C53 C52 C51 120.6(2) . . ?
C54 C53 C52 120.7(3) . . ?
C53 C54 C55 119.5(3) . . ?
C54 C55 C56 120.3(3) . . ?
C55 C56 C51 120.9(3) . . ?
C66 C61 C62 116.1(2) . . ?
C66 C61 P3 121.2(2) . . ?
C62 C61 P3 122.1(2) . . ?
C63 C62 C61 122.3(3) . . ?
C62 C63 C64 120.2(3) . . ?
C65 C64 C63 119.0(3) . . ?
C64 C65 C66 120.4(3) . . ?
C65 C66 C61 122.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 P1 Si1 C4 -4.27(13) . . . . ?
C11 P1 Si1 C4 104.11(12) . . . . ?
C21 P1 Si1 C3 -119.81(12) . . . . ?
C11 P1 Si1 C3 -11.44(12) . . . . ?
C21 P1 Si1 C1 116.95(11) . . . . ?
C11 P1 Si1 C1 -134.68(10) . . . . ?
C31 P2 Si2 C5 160.82(11) . . . . ?
C41 P2 Si2 C5 55.03(12) . . . . ?
C31 P2 Si2 C6 48.75(13) . . . . ?
C41 P2 Si2 C6 -57.05(12) . . . . ?
C31 P2 Si2 C1 -79.04(11) . . . . ?
C41 P2 Si2 C1 175.16(11) . . . . ?
C61 P3 Si3 C7 -14.73(12) . . . . ?
C51 P3 Si3 C7 90.83(12) . . . . ?
C61 P3 Si3 C8 -131.47(11) . . . . ?
C51 P3 Si3 C8 -25.91(12) . . . . ?
C61 P3 Si3 C1 107.22(11) . . . . ?
C51 P3 Si3 C1 -147.21(10) . . . . ?
C5 Si2 C1 C2 -160.77(15) . . . . ?
C6 Si2 C1 C2 -40.95(19) . . . . ?
P2 Si2 C1 C2 85.41(15) . . . . ?
C5 Si2 C1 Si3 78.74(14) . . . . ?
C6 Si2 C1 Si3 -161.43(12) . . . . ?
P2 Si2 C1 Si3 -35.08(13) . . . . ?
C5 Si2 C1 Si1 -43.60(14) . . . . ?
C6 Si2 C1 Si1 76.22(14) . . . . ?
P2 Si2 C1 Si1 -157.42(7) . . . . ?
C7 Si3 C1 C2 73.61(17) . . . . ?
C8 Si3 C1 C2 -165.04(14) . . . . ?
P3 Si3 C1 C2 -46.50(15) . . . . ?
C7 Si3 C1 Si2 -165.78(12) . . . . ?
C8 Si3 C1 Si2 -44.43(15) . . . . ?
P3 Si3 C1 Si2 74.11(11) . . . . ?
C7 Si3 C1 Si1 -43.24(15) . . . . ?
C8 Si3 C1 Si1 78.11(13) . . . . ?
P3 Si3 C1 Si1 -163.36(8) . . . . ?
C4 Si1 C1 C2 76.03(17) . . . . ?
C3 Si1 C1 C2 -162.24(15) . . . . ?
P1 Si1 C1 C2 -42.07(15) . . . . ?
C4 Si1 C1 Si2 -42.32(15) . . . . ?
C3 Si1 C1 Si2 79.41(14) . . . . ?
P1 Si1 C1 Si2 -160.41(8) . . . . ?
C4 Si1 C1 Si3 -166.07(12) . . . . ?
C3 Si1 C1 Si3 -44.34(15) . . . . ?
P1 Si1 C1 Si3 75.84(10) . . . . ?
C21 P1 C11 C12 -130.27(19) . . . . ?
Si1 P1 C11 C12 122.24(17) . . . . ?
C21 P1 C11 C16 50.5(2) . . . . ?
Si1 P1 C11 C16 -57.0(2) . . . . ?
C16 C11 C12 C13 0.0(4) . . . . ?
P1 C11 C12 C13 -179.3(2) . . . . ?
C11 C12 C13 C14 -0.8(4) . . . . ?
C12 C13 C14 C15 1.1(4) . . . . ?
C13 C14 C15 C16 -0.6(4) . . . . ?
C14 C15 C16 C11 -0.2(4) . . . . ?
C12 C11 C16 C15 0.5(3) . . . . ?
P1 C11 C16 C15 179.71(18) . . . . ?
C11 P1 C21 C22 10.8(3) . . . . ?
Si1 P1 C21 C22 117.0(2) . . . . ?
C11 P1 C21 C26 -177.0(2) . . . . ?
Si1 P1 C21 C26 -70.8(2) . . . . ?
C26 C21 C22 C23 0.8(4) . . . . ?
P1 C21 C22 C23 173.1(2) . . . . ?
C21 C22 C23 C24 0.6(5) . . . . ?
C22 C23 C24 C25 -1.5(5) . . . . ?
C23 C24 C25 C26 0.9(5) . . . . ?
C24 C25 C26 C21 0.5(5) . . . . ?
C22 C21 C26 C25 -1.4(4) . . . . ?
P1 C21 C26 C25 -174.2(2) . . . . ?
C41 P2 C31 C36 109.1(2) . . . . ?
Si2 P2 C31 C36 4.6(2) . . . . ?
C41 P2 C31 C32 -77.5(2) . . . . ?
Si2 P2 C31 C32 178.03(17) . . . . ?
C36 C31 C32 C33 0.5(4) . . . . ?
P2 C31 C32 C33 -173.4(2) . . . . ?
C31 C32 C33 C34 0.9(5) . . . . ?
C32 C33 C34 C35 -1.8(5) . . . . ?
C33 C34 C35 C36 1.3(5) . . . . ?
C32 C31 C36 C35 -1.0(4) . . . . ?
P2 C31 C36 C35 172.2(2) . . . . ?
C34 C35 C36 C31 0.1(4) . . . . ?
C31 P2 C41 C42 -16.2(2) . . . . ?
Si2 P2 C41 C42 96.6(2) . . . . ?
C31 P2 C41 C46 159.82(19) . . . . ?
Si2 P2 C41 C46 -87.42(18) . . . . ?
C46 C41 C42 C43 -0.5(4) . . . . ?
P2 C41 C42 C43 175.5(2) . . . . ?
C41 C42 C43 C44 1.2(4) . . . . ?
C42 C43 C44 C45 -0.1(4) . . . . ?
C43 C44 C45 C46 -1.7(4) . . . . ?
C42 C41 C46 C45 -1.3(4) . . . . ?
P2 C41 C46 C45 -177.5(2) . . . . ?
C44 C45 C46 C41 2.4(4) . . . . ?
C61 P3 C51 C56 -117.3(2) . . . . ?
Si3 P3 C51 C56 133.43(19) . . . . ?
C61 P3 C51 C52 61.9(2) . . . . ?
Si3 P3 C51 C52 -47.4(2) . . . . ?
C56 C51 C52 C53 -0.8(4) . . . . ?
P3 C51 C52 C53 -180.0(2) . . . . ?
C51 C52 C53 C54 1.0(4) . . . . ?
C52 C53 C54 C55 -0.3(4) . . . . ?
C53 C54 C55 C56 -0.5(4) . . . . ?
C54 C55 C56 C51 0.7(4) . . . . ?
C52 C51 C56 C55 -0.1(4) . . . . ?
P3 C51 C56 C55 179.2(2) . . . . ?
C51 P3 C61 C66 29.3(2) . . . . ?
Si3 P3 C61 C66 135.18(19) . . . . ?
C51 P3 C61 C62 -159.4(2) . . . . ?
Si3 P3 C61 C62 -53.6(2) . . . . ?
C66 C61 C62 C63 -1.8(4) . . . . ?
P3 C61 C62 C63 -173.5(2) . . . . ?
C61 C62 C63 C64 1.8(5) . . . . ?
C62 C63 C64 C65 -0.6(5) . . . . ?
C63 C64 C65 C66 -0.3(5) . . . . ?
C64 C65 C66 C61 0.1(5) . . . . ?
C62 C61 C66 C65 0.9(4) . . . . ?
P3 C61 C66 C65 172.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        26.39
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.061

#===END

data_6b
_database_code_depnum_ccdc_archive 'CCDC 289573'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_formula_moiety         'C8 H21 Br3 Si3'
_chemical_formula_sum            'C8 H21 Br3 Si3'
_chemical_formula_weight         441.25

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

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

_cell_length_a                   9.3209(9)
_cell_length_b                   9.3209(9)
_cell_length_c                   11.143(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     838.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    1506
_cell_measurement_theta_min      2.523
_cell_measurement_theta_max      25.992

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.88
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             432
_exptl_absorpt_coefficient_mu    7.404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0591
_exptl_absorpt_correction_T_max  0.3838
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(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 PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3156
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         26.36
_reflns_number_total             608
_reflns_number_gt                519
_reflns_threshold_expression     I>2\s(I)

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

_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^)+(0.0174P)^2^+0.5075P] 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     SHELXL
_refine_ls_extinction_coef       0.0155(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         608
_refine_ls_number_parameters     38
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0575
_refine_ls_wR_factor_gt          0.0544
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_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
Br Br 0.38480(5) 0.45728(5) 0.2500 0.0659(2) Uani 1 2 d S . .
Si Si 0.44495(11) 0.24979(11) 0.2500 0.0381(3) Uani 1 2 d S . .
C1 C 0.6667 0.3333 0.3039(7) 0.0278(15) Uani 0.50 3 d SP . .
C2 C 0.6667 0.3333 0.4454(7) 0.051(2) Uani 0.50 3 d SP . .
H2 H 0.5961 0.2200 0.4747 0.061 Uiso 0.50 1 calc PR . .
C3 C 0.2905(8) 0.0944(7) 0.3595(7) 0.0642(18) Uani 0.50 1 d P . .
H3A H 0.3201 0.1382 0.4413 0.077 Uiso 0.50 1 calc PR . .
H3B H 0.2921 -0.0097 0.3537 0.077 Uiso 0.50 1 calc PR . .
H3C H 0.1793 0.0742 0.3403 0.077 Uiso 0.50 1 calc PR . .
C4 C 0.4019(9) 0.1787(9) 0.0957(6) 0.0649(17) Uani 0.50 1 d P . .
H4A H 0.4854 0.2634 0.0429 0.078 Uiso 0.50 1 calc PR . .
H4B H 0.2918 0.1585 0.0730 0.078 Uiso 0.50 1 calc PR . .
H4C H 0.4054 0.0758 0.0878 0.078 Uiso 0.50 1 calc PR . .

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
Br 0.0459(3) 0.0515(3) 0.1131(5) 0.000 0.000 0.0340(2)
Si 0.0286(5) 0.0345(5) 0.0499(6) 0.000 0.000 0.0148(4)
C1 0.028(2) 0.028(2) 0.028(3) 0.000 0.000 0.0138(10)
C2 0.060(4) 0.060(4) 0.031(4) 0.000 0.000 0.0301(18)
C3 0.041(3) 0.041(3) 0.102(5) 0.009(3) 0.025(4) 0.014(3)
C4 0.060(4) 0.067(4) 0.069(4) -0.023(4) -0.034(3) 0.034(4)

_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
Br Si 2.2670(10) . ?
Si C4 1.814(7) . ?
Si C3 1.890(6) . ?
Si C1 1.905(2) . ?
C1 C2 1.577(11) . ?
C1 Si 1.905(2) 3_655 ?
C1 Si 1.905(2) 5_665 ?

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
C4 Si C3 112.8(4) . . ?
C4 Si C1 116.4(3) . . ?
C3 Si C1 111.4(3) . . ?
C4 Si Br 102.0(2) . . ?
C3 Si Br 103.60(18) . . ?
C1 Si Br 109.38(5) . . ?
C2 C1 Si 108.4(2) . 3_655 ?
C2 C1 Si 108.4(2) . 5_665 ?
Si C1 Si 110.6(2) 3_655 5_665 ?
C2 C1 Si 108.4(2) . . ?
Si C1 Si 110.6(2) 3_655 . ?
Si C1 Si 110.6(2) 5_665 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 Si C1 C2 -161.8(3) . . . . ?
C3 Si C1 C2 -30.6(2) . . . . ?
Br Si C1 C2 83.29(8) . . . . ?
C4 Si C1 Si -43.2(4) . . . 3_655 ?
C3 Si C1 Si 88.0(4) . . . 3_655 ?
Br Si C1 Si -158.08(19) . . . 3_655 ?
C4 Si C1 Si 79.5(4) . . . 5_665 ?
C3 Si C1 Si -149.3(3) . . . 5_665 ?
Br Si C1 Si -35.3(3) . . . 5_665 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.058

#===END

data_8a
_database_code_depnum_ccdc_archive 'CCDC 289574'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_formula_moiety         'C47 H49 Mo O4 P3 Si3, C7 H8'
_chemical_formula_sum            'C54 H57 Mo O4 P3 Si3'
_chemical_formula_weight         1043.12

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'
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   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   14.8482(8)
_cell_length_b                   14.8803(8)
_cell_length_c                   23.9239(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4133(10)
_cell_angle_gamma                90.00
_cell_volume                     5270.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    6857
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      26.37

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2168
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7549
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(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 PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            40529
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         26.39
_reflns_number_total             10791
_reflns_number_gt                9105
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'

_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^)+(0.0427P)^2^+2.3909P] 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         10791
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.321458(11) -0.182573(11) 0.224033(7) 0.02334(6) Uani 1 1 d . . .
P1 P 0.28684(3) -0.02839(3) 0.26338(2) 0.02326(11) Uani 1 1 d . . .
P2 P 0.26750(3) -0.13210(3) 0.12524(2) 0.02297(11) Uani 1 1 d . . .
P3 P 0.16209(4) 0.30503(4) 0.13567(2) 0.02817(12) Uani 1 1 d . . .
Si1 Si 0.32455(4) 0.09811(4) 0.21493(2) 0.02616(12) Uani 1 1 d . . .
Si2 Si 0.28684(4) 0.01115(4) 0.09088(2) 0.02418(12) Uani 1 1 d . . .
Si3 Si 0.28043(4) 0.22121(4) 0.11002(2) 0.02731(12) Uani 1 1 d . . .
O1 O 0.35477(14) -0.37679(12) 0.17900(8) 0.0569(5) Uani 1 1 d . . .
O2 O 0.37829(12) -0.25110(12) 0.34519(6) 0.0472(4) Uani 1 1 d . . .
O3 O 0.12193(12) -0.24977(13) 0.23924(7) 0.0547(5) Uani 1 1 d . . .
O4 O 0.52946(11) -0.14288(14) 0.21366(8) 0.0537(5) Uani 1 1 d . . .
C1 C 0.34350(16) -0.30485(15) 0.19477(9) 0.0345(5) Uani 1 1 d . . .
C2 C 0.35705(14) -0.22511(14) 0.30068(9) 0.0308(4) Uani 1 1 d . . .
C3 C 0.19279(16) -0.22288(15) 0.23361(8) 0.0335(5) Uani 1 1 d . . .
C4 C 0.45355(15) -0.15358(15) 0.21617(9) 0.0335(5) Uani 1 1 d . . .
C10 C 0.26557(13) 0.10443(12) 0.14178(8) 0.0235(4) Uani 1 1 d . . .
H10 H 0.1997 0.1002 0.1476 0.028 Uiso 1 1 calc R . .
C11 C 0.34959(14) -0.00034(13) 0.33111(8) 0.0292(4) Uani 1 1 d . . .
C12 C 0.43996(16) -0.02452(15) 0.34035(10) 0.0389(5) Uani 1 1 d . . .
H12 H 0.4683 -0.0572 0.3124 0.047 Uiso 1 1 calc R . .
C13 C 0.48935(19) -0.00138(17) 0.39000(11) 0.0522(7) Uani 1 1 d . . .
H13 H 0.5515 -0.0168 0.3954 0.063 Uiso 1 1 calc R . .
C14 C 0.4485(2) 0.04378(17) 0.43125(11) 0.0560(8) Uani 1 1 d . . .
H14 H 0.4821 0.0589 0.4653 0.067 Uiso 1 1 calc R . .
C15 C 0.3592(2) 0.06696(19) 0.42309(11) 0.0561(7) Uani 1 1 d . . .
H15 H 0.3309 0.0975 0.4519 0.067 Uiso 1 1 calc R . .
C16 C 0.30971(18) 0.04635(16) 0.37323(10) 0.0426(6) Uani 1 1 d . . .
H16 H 0.2482 0.0642 0.3678 0.051 Uiso 1 1 calc R . .
C17 C 0.44969(14) 0.08868(16) 0.21368(10) 0.0394(5) Uani 1 1 d . . .
H17A H 0.4773 0.0863 0.2522 0.047 Uiso 1 1 calc R . .
H17B H 0.4728 0.1410 0.1945 0.047 Uiso 1 1 calc R . .
H17C H 0.4646 0.0338 0.1937 0.047 Uiso 1 1 calc R . .
C18 C 0.29490(18) 0.19643(15) 0.25886(10) 0.0407(5) Uani 1 1 d . . .
H18A H 0.3264 0.1912 0.2962 0.049 Uiso 1 1 calc R . .
H18B H 0.2295 0.1973 0.2622 0.049 Uiso 1 1 calc R . .
H18C H 0.3132 0.2522 0.2411 0.049 Uiso 1 1 calc R . .
C21 C 0.17080(13) -0.01405(14) 0.28341(8) 0.0282(4) Uani 1 1 d . . .
C22 C 0.14164(15) -0.07127(15) 0.32461(9) 0.0351(5) Uani 1 1 d . . .
H22 H 0.1792 -0.1196 0.3380 0.042 Uiso 1 1 calc R . .
C23 C 0.05881(16) -0.05855(16) 0.34614(10) 0.0417(6) Uani 1 1 d . . .
H23 H 0.0403 -0.0974 0.3746 0.050 Uiso 1 1 calc R . .
C24 C 0.00316(16) 0.01010(19) 0.32653(11) 0.0489(6) Uani 1 1 d . . .
H24 H -0.0534 0.0193 0.3418 0.059 Uiso 1 1 calc R . .
C25 C 0.02955(17) 0.0655(2) 0.28478(12) 0.0520(7) Uani 1 1 d . . .
H25 H -0.0093 0.1124 0.2707 0.062 Uiso 1 1 calc R . .
C26 C 0.11291(15) 0.05326(16) 0.26302(10) 0.0393(5) Uani 1 1 d . . .
H26 H 0.1303 0.0915 0.2339 0.047 Uiso 1 1 calc R . .
C27 C 0.40676(14) 0.01258(16) 0.07267(10) 0.0369(5) Uani 1 1 d . . .
H27A H 0.4469 0.0106 0.1071 0.044 Uiso 1 1 calc R . .
H27B H 0.4182 0.0677 0.0519 0.044 Uiso 1 1 calc R . .
H27C H 0.4182 -0.0398 0.0494 0.044 Uiso 1 1 calc R . .
C28 C 0.20760(15) 0.01645(15) 0.02624(9) 0.0328(5) Uani 1 1 d . . .
H28A H 0.1452 0.0137 0.0368 0.039 Uiso 1 1 calc R . .
H28B H 0.2191 -0.0344 0.0018 0.039 Uiso 1 1 calc R . .
H28C H 0.2170 0.0728 0.0063 0.039 Uiso 1 1 calc R . .
C31 C 0.31931(14) -0.19113(13) 0.06803(8) 0.0271(4) Uani 1 1 d . . .
C32 C 0.41039(15) -0.21353(15) 0.07504(9) 0.0337(5) Uani 1 1 d . . .
H32 H 0.4431 -0.2032 0.1101 0.040 Uiso 1 1 calc R . .
C33 C 0.45416(17) -0.25107(16) 0.03107(10) 0.0430(6) Uani 1 1 d . . .
H33 H 0.5168 -0.2647 0.0361 0.052 Uiso 1 1 calc R . .
C34 C 0.40692(18) -0.26847(17) -0.01955(10) 0.0460(6) Uani 1 1 d . . .
H34 H 0.4366 -0.2949 -0.0492 0.055 Uiso 1 1 calc R . .
C35 C 0.31633(17) -0.24740(16) -0.02704(9) 0.0423(6) Uani 1 1 d . . .
H35 H 0.2838 -0.2593 -0.0620 0.051 Uiso 1 1 calc R . .
C36 C 0.27230(15) -0.20889(14) 0.01619(8) 0.0331(5) Uani 1 1 d . . .
H36 H 0.2099 -0.1945 0.0106 0.040 Uiso 1 1 calc R . .
C37 C 0.38605(15) 0.28039(16) 0.13710(12) 0.0452(6) Uani 1 1 d . . .
H37A H 0.3907 0.2794 0.1782 0.054 Uiso 1 1 calc R . .
H37B H 0.3842 0.3428 0.1240 0.054 Uiso 1 1 calc R . .
H37C H 0.4385 0.2500 0.1233 0.054 Uiso 1 1 calc R . .
C38 C 0.28801(17) 0.22735(16) 0.03209(9) 0.0409(5) Uani 1 1 d . . .
H38A H 0.2364 0.1959 0.0131 0.049 Uiso 1 1 calc R . .
H38B H 0.3442 0.1989 0.0223 0.049 Uiso 1 1 calc R . .
H38C H 0.2874 0.2904 0.0203 0.049 Uiso 1 1 calc R . .
C41 C 0.14672(13) -0.15694(14) 0.11204(8) 0.0273(4) Uani 1 1 d . . .
C42 C 0.11901(15) -0.24447(15) 0.09956(9) 0.0346(5) Uani 1 1 d . . .
H42 H 0.1630 -0.2896 0.0947 0.042 Uiso 1 1 calc R . .
C43 C 0.02823(17) -0.26678(18) 0.09408(10) 0.0466(6) Uani 1 1 d . . .
H43 H 0.0104 -0.3266 0.0849 0.056 Uiso 1 1 calc R . .
C44 C -0.03635(17) -0.2024(2) 0.10190(12) 0.0557(7) Uani 1 1 d . . .
H44 H -0.0986 -0.2177 0.0981 0.067 Uiso 1 1 calc R . .
C45 C -0.01022(16) -0.11600(19) 0.11526(12) 0.0543(7) Uani 1 1 d . . .
H45 H -0.0546 -0.0717 0.1211 0.065 Uiso 1 1 calc R . .
C46 C 0.08095(15) -0.09287(16) 0.12028(10) 0.0383(5) Uani 1 1 d . . .
H46 H 0.0983 -0.0329 0.1294 0.046 Uiso 1 1 calc R . .
C51 C 0.16507(14) 0.39536(14) 0.08323(9) 0.0319(5) Uani 1 1 d . . .
C52 C 0.10826(16) 0.40298(16) 0.03482(10) 0.0420(5) Uani 1 1 d . . .
H52 H 0.0625 0.3593 0.0267 0.050 Uiso 1 1 calc R . .
C53 C 0.1176(2) 0.47421(19) -0.00217(12) 0.0542(7) Uani 1 1 d . . .
H53 H 0.0783 0.4786 -0.0353 0.065 Uiso 1 1 calc R . .
C54 C 0.1833(2) 0.53792(17) 0.00900(12) 0.0531(7) Uani 1 1 d . . .
H54 H 0.1904 0.5855 -0.0168 0.064 Uiso 1 1 calc R . .
C55 C 0.23875(18) 0.53275(16) 0.05750(12) 0.0474(6) Uani 1 1 d . . .
H55 H 0.2838 0.5773 0.0655 0.057 Uiso 1 1 calc R . .
C56 C 0.22931(16) 0.46301(14) 0.09479(10) 0.0385(5) Uani 1 1 d . . .
H56 H 0.2670 0.4610 0.1287 0.046 Uiso 1 1 calc R . .
C61 C 0.06509(13) 0.23327(13) 0.11299(9) 0.0284(4) Uani 1 1 d . . .
C62 C 0.04873(15) 0.19326(15) 0.06042(9) 0.0363(5) Uani 1 1 d . . .
H62 H 0.0895 0.2035 0.0324 0.044 Uiso 1 1 calc R . .
C63 C -0.02585(16) 0.13888(17) 0.04844(10) 0.0415(5) Uani 1 1 d . . .
H63 H -0.0360 0.1124 0.0124 0.050 Uiso 1 1 calc R . .
C64 C -0.08539(16) 0.12312(17) 0.08869(10) 0.0435(6) Uani 1 1 d . . .
H64 H -0.1366 0.0858 0.0805 0.052 Uiso 1 1 calc R . .
C65 C -0.07025(17) 0.16174(18) 0.14094(10) 0.0466(6) Uani 1 1 d . . .
H65 H -0.1111 0.1509 0.1688 0.056 Uiso 1 1 calc R . .
C66 C 0.00403(15) 0.21615(16) 0.15294(9) 0.0363(5) Uani 1 1 d . . .
H66 H 0.0136 0.2424 0.1891 0.044 Uiso 1 1 calc R . .
C10S C 0.8131(3) -0.0162(3) 0.23331(17) 0.1079(15) Uani 1 1 d . . .
H10A H 0.7922 -0.0518 0.2643 0.129 Uiso 1 1 calc R . .
H10B H 0.8114 0.0477 0.2429 0.129 Uiso 1 1 calc R . .
H10C H 0.8751 -0.0336 0.2268 0.129 Uiso 1 1 calc R . .
C11S C 0.7540(2) -0.0329(2) 0.18231(13) 0.0623(8) Uani 1 1 d . . .
C12S C 0.7030(2) 0.0344(2) 0.15605(15) 0.0657(8) Uani 1 1 d . . .
H12S H 0.7062 0.0934 0.1711 0.079 Uiso 1 1 calc R . .
C13S C 0.64808(19) 0.0179(2) 0.10884(15) 0.0676(9) Uani 1 1 d . . .
H13S H 0.6144 0.0656 0.0910 0.081 Uiso 1 1 calc R . .
C14S C 0.6411(2) -0.0675(3) 0.08684(14) 0.0680(9) Uani 1 1 d . . .
H14S H 0.6018 -0.0789 0.0544 0.082 Uiso 1 1 calc R . .
C15S C 0.6907(2) -0.1353(2) 0.11182(13) 0.0652(8) Uani 1 1 d . . .
H15S H 0.6858 -0.1946 0.0971 0.078 Uiso 1 1 calc R . .
C16S C 0.7478(2) -0.1177(2) 0.15836(13) 0.0619(8) Uani 1 1 d . . .
H16S H 0.7841 -0.1649 0.1746 0.074 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
Mo 0.02780(10) 0.02227(9) 0.01998(9) -0.00006(6) 0.00192(6) 0.00162(6)
P1 0.0250(2) 0.0231(2) 0.0216(2) -0.00128(19) 0.00148(19) -0.00063(19)
P2 0.0252(2) 0.0226(2) 0.0211(2) -0.00109(19) 0.00167(19) 0.00145(19)
P3 0.0301(3) 0.0256(3) 0.0287(3) -0.0012(2) 0.0018(2) 0.0007(2)
Si1 0.0281(3) 0.0227(3) 0.0272(3) 0.0000(2) -0.0009(2) -0.0035(2)
Si2 0.0245(3) 0.0240(3) 0.0241(3) 0.0011(2) 0.0022(2) 0.0000(2)
Si3 0.0266(3) 0.0233(3) 0.0324(3) 0.0049(2) 0.0044(2) -0.0009(2)
O1 0.0793(14) 0.0337(10) 0.0569(11) -0.0127(8) 0.0012(10) 0.0127(9)
O2 0.0619(11) 0.0517(10) 0.0271(8) 0.0088(7) -0.0020(8) -0.0028(8)
O3 0.0505(11) 0.0709(13) 0.0441(10) -0.0051(9) 0.0123(8) -0.0286(9)
O4 0.0292(9) 0.0767(13) 0.0557(11) 0.0016(10) 0.0056(8) 0.0031(8)
C1 0.0449(13) 0.0307(12) 0.0276(11) -0.0009(9) 0.0010(9) 0.0063(9)
C2 0.0363(11) 0.0293(11) 0.0268(11) -0.0002(9) 0.0029(9) -0.0018(9)
C3 0.0451(13) 0.0329(11) 0.0232(10) -0.0030(9) 0.0065(9) -0.0067(10)
C4 0.0367(12) 0.0375(12) 0.0262(10) 0.0014(9) 0.0018(9) 0.0065(9)
C10 0.0225(9) 0.0216(9) 0.0263(10) 0.0010(7) 0.0011(7) -0.0015(7)
C11 0.0389(11) 0.0239(10) 0.0241(10) -0.0001(8) -0.0028(8) -0.0044(8)
C12 0.0430(13) 0.0330(12) 0.0389(12) -0.0037(9) -0.0095(10) 0.0015(10)
C13 0.0600(16) 0.0364(13) 0.0551(16) -0.0024(12) -0.0285(13) 0.0017(12)
C14 0.087(2) 0.0365(14) 0.0390(14) -0.0011(11) -0.0283(14) -0.0057(14)
C15 0.087(2) 0.0489(15) 0.0318(13) -0.0135(11) 0.0008(13) -0.0075(15)
C16 0.0515(14) 0.0432(14) 0.0329(12) -0.0095(10) 0.0015(10) -0.0028(11)
C17 0.0281(11) 0.0423(13) 0.0465(13) 0.0122(11) -0.0057(10) -0.0085(10)
C18 0.0577(15) 0.0283(11) 0.0356(12) -0.0066(9) 0.0013(11) -0.0068(10)
C21 0.0287(10) 0.0286(10) 0.0276(10) -0.0077(8) 0.0042(8) -0.0014(8)
C22 0.0378(12) 0.0295(11) 0.0390(12) -0.0018(9) 0.0099(10) -0.0028(9)
C23 0.0446(13) 0.0419(13) 0.0406(13) -0.0067(10) 0.0170(11) -0.0115(11)
C24 0.0337(12) 0.0605(16) 0.0550(15) -0.0097(13) 0.0186(11) -0.0011(12)
C25 0.0394(14) 0.0597(17) 0.0580(16) 0.0056(13) 0.0110(12) 0.0147(12)
C26 0.0349(12) 0.0441(13) 0.0397(12) 0.0044(10) 0.0076(10) 0.0062(10)
C27 0.0322(11) 0.0355(12) 0.0442(13) 0.0025(10) 0.0106(10) 0.0013(9)
C28 0.0384(12) 0.0303(11) 0.0289(11) 0.0019(9) -0.0023(9) 0.0008(9)
C31 0.0361(11) 0.0232(10) 0.0225(9) 0.0007(8) 0.0052(8) 0.0032(8)
C32 0.0388(12) 0.0346(11) 0.0280(11) -0.0003(9) 0.0038(9) 0.0080(9)
C33 0.0457(13) 0.0446(14) 0.0402(13) 0.0022(11) 0.0121(11) 0.0146(11)
C34 0.0646(16) 0.0444(14) 0.0313(12) -0.0035(10) 0.0176(11) 0.0130(12)
C35 0.0606(16) 0.0445(14) 0.0220(11) -0.0045(9) 0.0044(10) 0.0029(12)
C36 0.0419(12) 0.0310(11) 0.0263(10) -0.0003(9) 0.0018(9) 0.0022(9)
C37 0.0314(12) 0.0340(12) 0.0694(17) 0.0141(12) -0.0001(11) -0.0079(10)
C38 0.0512(14) 0.0339(12) 0.0398(13) 0.0098(10) 0.0177(11) 0.0057(10)
C41 0.0273(10) 0.0312(10) 0.0233(10) 0.0020(8) 0.0006(8) -0.0019(8)
C42 0.0390(12) 0.0317(11) 0.0328(11) -0.0012(9) 0.0003(9) -0.0046(9)
C43 0.0489(14) 0.0445(14) 0.0458(14) -0.0009(11) -0.0006(11) -0.0203(12)
C44 0.0315(13) 0.0690(19) 0.0660(18) 0.0069(15) -0.0001(12) -0.0152(13)
C45 0.0315(13) 0.0563(17) 0.0763(19) 0.0050(14) 0.0109(12) 0.0032(12)
C46 0.0322(11) 0.0343(12) 0.0486(14) -0.0005(10) 0.0053(10) 0.0001(9)
C51 0.0334(11) 0.0250(10) 0.0377(12) -0.0003(9) 0.0060(9) 0.0057(8)
C52 0.0426(13) 0.0374(13) 0.0451(13) 0.0085(10) -0.0023(10) -0.0002(10)
C53 0.0603(17) 0.0529(16) 0.0478(15) 0.0174(12) -0.0064(13) 0.0030(13)
C54 0.0634(17) 0.0391(14) 0.0573(17) 0.0174(12) 0.0084(14) 0.0026(12)
C55 0.0505(15) 0.0293(12) 0.0633(17) 0.0035(11) 0.0102(13) -0.0029(10)
C56 0.0423(13) 0.0277(11) 0.0451(13) -0.0008(9) 0.0010(10) 0.0018(9)
C61 0.0284(10) 0.0244(10) 0.0322(11) 0.0018(8) 0.0003(8) 0.0038(8)
C62 0.0333(11) 0.0415(13) 0.0344(12) -0.0035(10) 0.0043(9) 0.0000(9)
C63 0.0385(12) 0.0482(14) 0.0368(12) -0.0077(11) -0.0041(10) -0.0031(11)
C64 0.0342(12) 0.0470(14) 0.0481(14) 0.0023(11) -0.0045(10) -0.0092(10)
C65 0.0413(13) 0.0589(16) 0.0403(13) 0.0035(12) 0.0076(11) -0.0121(12)
C66 0.0387(12) 0.0398(12) 0.0305(11) -0.0003(9) 0.0033(9) -0.0028(10)
C10S 0.129(4) 0.103(3) 0.087(3) 0.022(2) -0.023(3) -0.038(3)
C11S 0.0575(17) 0.065(2) 0.0651(19) 0.0165(15) 0.0091(15) -0.0120(15)
C12S 0.0529(17) 0.0499(17) 0.095(3) 0.0073(16) 0.0116(17) -0.0012(13)
C13S 0.0410(15) 0.069(2) 0.094(3) 0.0212(19) 0.0116(16) 0.0073(14)
C14S 0.0564(18) 0.090(3) 0.0594(19) 0.0048(18) 0.0145(15) -0.0009(17)
C15S 0.072(2) 0.066(2) 0.0602(19) -0.0016(15) 0.0217(16) 0.0013(16)
C16S 0.0615(18) 0.0549(18) 0.072(2) 0.0242(15) 0.0215(16) 0.0055(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
Mo C2 1.973(2) . ?
Mo C1 1.986(2) . ?
Mo C4 2.031(2) . ?
Mo C3 2.032(2) . ?
Mo P1 2.5473(5) . ?
Mo P2 2.5497(5) . ?
P1 C21 1.836(2) . ?
P1 C11 1.853(2) . ?
P1 Si1 2.3022(7) . ?
P2 C41 1.835(2) . ?
P2 C31 1.843(2) . ?
P2 Si2 2.3103(7) . ?
P3 C61 1.841(2) . ?
P3 C51 1.842(2) . ?
P3 Si3 2.2772(8) . ?
Si1 C17 1.866(2) . ?
Si1 C18 1.874(2) . ?
Si1 C10 1.8981(19) . ?
Si2 C27 1.865(2) . ?
Si2 C28 1.871(2) . ?
Si2 C10 1.8890(19) . ?
Si3 C37 1.870(2) . ?
Si3 C38 1.879(2) . ?
Si3 C10 1.9162(19) . ?
O1 C1 1.151(3) . ?
O2 C2 1.154(2) . ?
O3 C3 1.143(3) . ?
O4 C4 1.144(3) . ?
C11 C12 1.390(3) . ?
C11 C16 1.393(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.373(4) . ?
C14 C15 1.370(4) . ?
C15 C16 1.386(3) . ?
C21 C26 1.384(3) . ?
C21 C22 1.396(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.374(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.391(3) . ?
C31 C32 1.390(3) . ?
C31 C36 1.401(3) . ?
C32 C33 1.395(3) . ?
C33 C34 1.377(3) . ?
C34 C35 1.379(3) . ?
C35 C36 1.389(3) . ?
C41 C46 1.390(3) . ?
C41 C42 1.391(3) . ?
C42 C43 1.385(3) . ?
C43 C44 1.378(4) . ?
C44 C45 1.374(4) . ?
C45 C46 1.393(3) . ?
C51 C52 1.384(3) . ?
C51 C56 1.400(3) . ?
C52 C53 1.395(3) . ?
C53 C54 1.372(4) . ?
C54 C55 1.372(4) . ?
C55 C56 1.383(3) . ?
C61 C66 1.391(3) . ?
C61 C62 1.396(3) . ?
C62 C63 1.384(3) . ?
C63 C64 1.377(3) . ?
C64 C65 1.378(3) . ?
C65 C66 1.380(3) . ?
C10S C11S 1.468(5) . ?
C11S C12S 1.377(4) . ?
C11S C16S 1.386(4) . ?
C12S C13S 1.364(5) . ?
C13S C14S 1.375(5) . ?
C14S C15S 1.361(5) . ?
C15S C16S 1.372(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Mo C1 89.66(9) . . ?
C2 Mo C4 87.86(8) . . ?
C1 Mo C4 88.59(9) . . ?
C2 Mo C3 89.28(9) . . ?
C1 Mo C3 87.20(9) . . ?
C4 Mo C3 174.93(9) . . ?
C2 Mo P1 89.58(6) . . ?
C1 Mo P1 177.44(7) . . ?
C4 Mo P1 93.83(6) . . ?
C3 Mo P1 90.34(6) . . ?
C2 Mo P2 176.93(6) . . ?
C1 Mo P2 89.52(6) . . ?
C4 Mo P2 95.07(6) . . ?
C3 Mo P2 87.73(6) . . ?
P1 Mo P2 91.109(16) . . ?
C21 P1 C11 99.47(9) . . ?
C21 P1 Si1 107.81(7) . . ?
C11 P1 Si1 97.50(7) . . ?
C21 P1 Mo 114.91(7) . . ?
C11 P1 Mo 115.07(7) . . ?
Si1 P1 Mo 119.11(2) . . ?
C41 P2 C31 103.56(9) . . ?
C41 P2 Si2 105.74(7) . . ?
C31 P2 Si2 96.04(6) . . ?
C41 P2 Mo 109.48(6) . . ?
C31 P2 Mo 115.37(7) . . ?
Si2 P2 Mo 124.24(2) . . ?
C61 P3 C51 106.37(10) . . ?
C61 P3 Si3 101.85(7) . . ?
C51 P3 Si3 99.01(7) . . ?
C17 Si1 C18 110.18(11) . . ?
C17 Si1 C10 112.23(10) . . ?
C18 Si1 C10 111.52(10) . . ?
C17 Si1 P1 103.16(7) . . ?
C18 Si1 P1 106.22(8) . . ?
C10 Si1 P1 113.07(6) . . ?
C27 Si2 C28 110.93(10) . . ?
C27 Si2 C10 110.62(10) . . ?
C28 Si2 C10 112.08(9) . . ?
C27 Si2 P2 103.93(8) . . ?
C28 Si2 P2 104.21(7) . . ?
C10 Si2 P2 114.65(6) . . ?
C37 Si3 C38 102.02(12) . . ?
C37 Si3 C10 114.12(10) . . ?
C38 Si3 C10 117.07(10) . . ?
C37 Si3 P3 107.01(9) . . ?
C38 Si3 P3 110.32(8) . . ?
C10 Si3 P3 105.96(6) . . ?
O1 C1 Mo 178.0(2) . . ?
O2 C2 Mo 179.0(2) . . ?
O3 C3 Mo 176.7(2) . . ?
O4 C4 Mo 175.1(2) . . ?
Si2 C10 Si1 118.02(10) . . ?
Si2 C10 Si3 112.38(10) . . ?
Si1 C10 Si3 110.58(9) . . ?
C12 C11 C16 118.2(2) . . ?
C12 C11 P1 119.66(16) . . ?
C16 C11 P1 122.11(17) . . ?
C13 C12 C11 120.7(2) . . ?
C14 C13 C12 120.1(3) . . ?
C15 C14 C13 119.8(2) . . ?
C14 C15 C16 120.7(3) . . ?
C15 C16 C11 120.4(2) . . ?
C26 C21 C22 118.17(19) . . ?
C26 C21 P1 124.20(16) . . ?
C22 C21 P1 117.48(16) . . ?
C23 C22 C21 120.8(2) . . ?
C24 C23 C22 120.2(2) . . ?
C23 C24 C25 119.8(2) . . ?
C24 C25 C26 120.3(2) . . ?
C21 C26 C25 120.6(2) . . ?
C32 C31 C36 118.37(19) . . ?
C32 C31 P2 118.84(15) . . ?
C36 C31 P2 122.64(16) . . ?
C31 C32 C33 120.7(2) . . ?
C34 C33 C32 120.2(2) . . ?
C33 C34 C35 119.8(2) . . ?
C34 C35 C36 120.5(2) . . ?
C35 C36 C31 120.4(2) . . ?
C46 C41 C42 118.24(19) . . ?
C46 C41 P2 121.72(16) . . ?
C42 C41 P2 119.64(16) . . ?
C43 C42 C41 121.0(2) . . ?
C44 C43 C42 120.2(2) . . ?
C45 C44 C43 119.7(2) . . ?
C44 C45 C46 120.4(2) . . ?
C41 C46 C45 120.5(2) . . ?
C52 C51 C56 117.9(2) . . ?
C52 C51 P3 125.79(17) . . ?
C56 C51 P3 116.24(17) . . ?
C51 C52 C53 120.6(2) . . ?
C54 C53 C52 120.4(2) . . ?
C53 C54 C55 119.8(2) . . ?
C54 C55 C56 120.2(2) . . ?
C55 C56 C51 120.9(2) . . ?
C66 C61 C62 117.6(2) . . ?
C66 C61 P3 116.12(16) . . ?
C62 C61 P3 126.23(16) . . ?
C63 C62 C61 121.1(2) . . ?
C64 C63 C62 120.1(2) . . ?
C63 C64 C65 119.7(2) . . ?
C64 C65 C66 120.3(2) . . ?
C65 C66 C61 121.1(2) . . ?
C12S C11S C16S 117.1(3) . . ?
C12S C11S C10S 121.9(3) . . ?
C16S C11S C10S 120.9(3) . . ?
C13S C12S C11S 121.3(3) . . ?
C12S C13S C14S 120.4(3) . . ?
C15S C14S C13S 119.6(3) . . ?
C14S C15S C16S 119.6(3) . . ?
C15S C16S C11S 121.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Mo P1 C21 -89.21(10) . . . . ?
C1 Mo P1 C21 -16.4(15) . . . . ?
C4 Mo P1 C21 -177.04(9) . . . . ?
C3 Mo P1 C21 0.07(9) . . . . ?
P2 Mo P1 C21 87.80(7) . . . . ?
C2 Mo P1 C11 25.47(10) . . . . ?
C1 Mo P1 C11 98.3(15) . . . . ?
C4 Mo P1 C11 -62.36(9) . . . . ?
C3 Mo P1 C11 114.75(9) . . . . ?
P2 Mo P1 C11 -157.52(7) . . . . ?
C2 Mo P1 Si1 140.65(7) . . . . ?
C1 Mo P1 Si1 -146.5(14) . . . . ?
C4 Mo P1 Si1 52.82(6) . . . . ?
C3 Mo P1 Si1 -130.07(6) . . . . ?
P2 Mo P1 Si1 -42.33(3) . . . . ?
C2 Mo P2 C41 12.0(12) . . . . ?
C1 Mo P2 C41 86.53(10) . . . . ?
C4 Mo P2 C41 175.07(9) . . . . ?
C3 Mo P2 C41 -0.69(9) . . . . ?
P1 Mo P2 C41 -90.98(7) . . . . ?
C2 Mo P2 C31 -104.3(12) . . . . ?
C1 Mo P2 C31 -29.77(10) . . . . ?
C4 Mo P2 C31 58.78(10) . . . . ?
C3 Mo P2 C31 -116.99(10) . . . . ?
P1 Mo P2 C31 152.72(7) . . . . ?
C2 Mo P2 Si2 138.1(12) . . . . ?
C1 Mo P2 Si2 -147.39(7) . . . . ?
C4 Mo P2 Si2 -58.85(7) . . . . ?
C3 Mo P2 Si2 125.39(7) . . . . ?
P1 Mo P2 Si2 35.09(3) . . . . ?
C21 P1 Si1 C17 165.86(10) . . . . ?
C11 P1 Si1 C17 63.35(11) . . . . ?
Mo P1 Si1 C17 -60.88(9) . . . . ?
C21 P1 Si1 C18 49.95(11) . . . . ?
C11 P1 Si1 C18 -52.56(11) . . . . ?
Mo P1 Si1 C18 -176.79(8) . . . . ?
C21 P1 Si1 C10 -72.68(9) . . . . ?
C11 P1 Si1 C10 -175.19(9) . . . . ?
Mo P1 Si1 C10 60.58(7) . . . . ?
C41 P2 Si2 C27 -153.33(10) . . . . ?
C31 P2 Si2 C27 -47.38(10) . . . . ?
Mo P2 Si2 C27 79.01(8) . . . . ?
C41 P2 Si2 C28 -37.07(10) . . . . ?
C31 P2 Si2 C28 68.88(10) . . . . ?
Mo P2 Si2 C28 -164.73(7) . . . . ?
C41 P2 Si2 C10 85.81(9) . . . . ?
C31 P2 Si2 C10 -168.24(9) . . . . ?
Mo P2 Si2 C10 -41.85(7) . . . . ?
C61 P3 Si3 C37 -174.33(11) . . . . ?
C51 P3 Si3 C37 76.72(11) . . . . ?
C61 P3 Si3 C38 75.46(11) . . . . ?
C51 P3 Si3 C38 -33.49(11) . . . . ?
C61 P3 Si3 C10 -52.18(9) . . . . ?
C51 P3 Si3 C10 -161.14(9) . . . . ?
C2 Mo C1 O1 49(6) . . . . ?
C4 Mo C1 O1 137(6) . . . . ?
C3 Mo C1 O1 -40(6) . . . . ?
P1 Mo C1 O1 -24(8) . . . . ?
P2 Mo C1 O1 -128(6) . . . . ?
C1 Mo C2 O2 10(12) . . . . ?
C4 Mo C2 O2 -79(12) . . . . ?
C3 Mo C2 O2 97(12) . . . . ?
P1 Mo C2 O2 -172(100) . . . . ?
P2 Mo C2 O2 85(12) . . . . ?
C2 Mo C3 O3 -63(3) . . . . ?
C1 Mo C3 O3 26(3) . . . . ?
C4 Mo C3 O3 -8(4) . . . . ?
P1 Mo C3 O3 -153(3) . . . . ?
P2 Mo C3 O3 116(3) . . . . ?
C2 Mo C4 O4 41(2) . . . . ?
C1 Mo C4 O4 -49(2) . . . . ?
C3 Mo C4 O4 -15(3) . . . . ?
P1 Mo C4 O4 131(2) . . . . ?
P2 Mo C4 O4 -138(2) . . . . ?
C27 Si2 C10 Si1 -66.43(13) . . . . ?
C28 Si2 C10 Si1 169.20(10) . . . . ?
P2 Si2 C10 Si1 50.67(12) . . . . ?
C27 Si2 C10 Si3 64.09(13) . . . . ?
C28 Si2 C10 Si3 -60.28(13) . . . . ?
P2 Si2 C10 Si3 -178.81(6) . . . . ?
C17 Si1 C10 Si2 55.79(14) . . . . ?
C18 Si1 C10 Si2 179.97(11) . . . . ?
P1 Si1 C10 Si2 -60.40(11) . . . . ?
C17 Si1 C10 Si3 -75.54(12) . . . . ?
C18 Si1 C10 Si3 48.63(13) . . . . ?
P1 Si1 C10 Si3 168.26(6) . . . . ?
C37 Si3 C10 Si2 -106.26(13) . . . . ?
C38 Si3 C10 Si2 12.76(14) . . . . ?
P3 Si3 C10 Si2 136.25(8) . . . . ?
C37 Si3 C10 Si1 27.94(15) . . . . ?
C38 Si3 C10 Si1 146.96(11) . . . . ?
P3 Si3 C10 Si1 -89.54(9) . . . . ?
C21 P1 C11 C12 163.24(18) . . . . ?
Si1 P1 C11 C12 -87.20(17) . . . . ?
Mo P1 C11 C12 39.91(19) . . . . ?
C21 P1 C11 C16 -18.2(2) . . . . ?
Si1 P1 C11 C16 91.40(18) . . . . ?
Mo P1 C11 C16 -141.49(16) . . . . ?
C16 C11 C12 C13 -1.0(3) . . . . ?
P1 C11 C12 C13 177.66(19) . . . . ?
C11 C12 C13 C14 1.7(4) . . . . ?
C12 C13 C14 C15 -0.8(4) . . . . ?
C13 C14 C15 C16 -0.8(4) . . . . ?
C14 C15 C16 C11 1.6(4) . . . . ?
C12 C11 C16 C15 -0.6(3) . . . . ?
P1 C11 C16 C15 -179.27(19) . . . . ?
C11 P1 C21 C26 112.28(19) . . . . ?
Si1 P1 C21 C26 11.2(2) . . . . ?
Mo P1 C21 C26 -124.27(18) . . . . ?
C11 P1 C21 C22 -63.28(18) . . . . ?
Si1 P1 C21 C22 -164.39(15) . . . . ?
Mo P1 C21 C22 60.16(17) . . . . ?
C26 C21 C22 C23 -2.7(3) . . . . ?
P1 C21 C22 C23 173.10(17) . . . . ?
C21 C22 C23 C24 1.0(4) . . . . ?
C22 C23 C24 C25 0.9(4) . . . . ?
C23 C24 C25 C26 -1.1(4) . . . . ?
C22 C21 C26 C25 2.6(3) . . . . ?
P1 C21 C26 C25 -173.0(2) . . . . ?
C24 C25 C26 C21 -0.7(4) . . . . ?
C41 P2 C31 C32 -157.76(17) . . . . ?
Si2 P2 C31 C32 94.41(16) . . . . ?
Mo P2 C31 C32 -38.16(18) . . . . ?
C41 P2 C31 C36 26.80(19) . . . . ?
Si2 P2 C31 C36 -81.03(17) . . . . ?
Mo P2 C31 C36 146.40(15) . . . . ?
C36 C31 C32 C33 1.3(3) . . . . ?
P2 C31 C32 C33 -174.34(18) . . . . ?
C31 C32 C33 C34 -1.6(4) . . . . ?
C32 C33 C34 C35 1.0(4) . . . . ?
C33 C34 C35 C36 -0.1(4) . . . . ?
C34 C35 C36 C31 -0.2(3) . . . . ?
C32 C31 C36 C35 -0.4(3) . . . . ?
P2 C31 C36 C35 175.04(17) . . . . ?
C31 P2 C41 C46 -141.46(18) . . . . ?
Si2 P2 C41 C46 -41.07(18) . . . . ?
Mo P2 C41 C46 94.97(17) . . . . ?
C31 P2 C41 C42 45.91(18) . . . . ?
Si2 P2 C41 C42 146.30(15) . . . . ?
Mo P2 C41 C42 -77.66(17) . . . . ?
C46 C41 C42 C43 1.6(3) . . . . ?
P2 C41 C42 C43 174.49(17) . . . . ?
C41 C42 C43 C44 -1.1(4) . . . . ?
C42 C43 C44 C45 -0.1(4) . . . . ?
C43 C44 C45 C46 0.8(4) . . . . ?
C42 C41 C46 C45 -0.9(3) . . . . ?
P2 C41 C46 C45 -173.67(19) . . . . ?
C44 C45 C46 C41 -0.2(4) . . . . ?
C61 P3 C51 C52 -3.7(2) . . . . ?
Si3 P3 C51 C52 101.6(2) . . . . ?
C61 P3 C51 C56 174.51(16) . . . . ?
Si3 P3 C51 C56 -80.22(16) . . . . ?
C56 C51 C52 C53 2.5(4) . . . . ?
P3 C51 C52 C53 -179.3(2) . . . . ?
C51 C52 C53 C54 -0.1(4) . . . . ?
C52 C53 C54 C55 -1.6(4) . . . . ?
C53 C54 C55 C56 0.8(4) . . . . ?
C54 C55 C56 C51 1.7(4) . . . . ?
C52 C51 C56 C55 -3.3(3) . . . . ?
P3 C51 C56 C55 178.37(18) . . . . ?
C51 P3 C61 C66 -127.89(17) . . . . ?
Si3 P3 C61 C66 128.90(15) . . . . ?
C51 P3 C61 C62 53.8(2) . . . . ?
Si3 P3 C61 C62 -49.43(19) . . . . ?
C66 C61 C62 C63 0.3(3) . . . . ?
P3 C61 C62 C63 178.64(18) . . . . ?
C61 C62 C63 C64 -0.2(4) . . . . ?
C62 C63 C64 C65 0.0(4) . . . . ?
C63 C64 C65 C66 0.2(4) . . . . ?
C64 C65 C66 C61 0.0(4) . . . . ?
C62 C61 C66 C65 -0.2(3) . . . . ?
P3 C61 C66 C65 -178.69(19) . . . . ?
C16S C11S C12S C13S 0.7(5) . . . . ?
C10S C11S C12S C13S -179.7(3) . . . . ?
C11S C12S C13S C14S 1.2(5) . . . . ?
C12S C13S C14S C15S -1.3(5) . . . . ?
C13S C14S C15S C16S -0.6(5) . . . . ?
C14S C15S C16S C11S 2.6(5) . . . . ?
C12S C11S C16S C15S -2.6(4) . . . . ?
C10S C11S C16S C15S 177.8(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.39
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.062

#===END

data_10a
_database_code_depnum_ccdc_archive 'CCDC 289575'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_formula_moiety         'C22 H49 Mo O3 P3 Si3'
_chemical_formula_sum            'C22 H49 Mo O3 P3 Si3'
_chemical_formula_weight         634.73

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R 3'
_symmetry_space_group_name_Hall  'R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   17.1523(3)
_cell_length_b                   17.1523(3)
_cell_length_c                   9.2856(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2365.84(12)
_cell_formula_units_Z            3
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    5701
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      26.35

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1002
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7664
_exptl_absorpt_correction_T_max  0.8551
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(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 PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5046
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.59
_diffrn_reflns_theta_max         26.35
_reflns_number_total             2083
_reflns_number_gt                2080
_reflns_threshold_expression     I>2\s(I)

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

_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^)+(0.0243P)^2^+0.8197P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         2083
_refine_ls_number_parameters     105
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0178
_refine_ls_wR_factor_ref         0.0445
_refine_ls_wR_factor_gt          0.0445
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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
Mo Mo 0.0000 0.0000 0.015517(8) 0.02337(7) Uani 1 3 d S . .
P P 0.14090(3) 0.06403(4) 0.17350(5) 0.03045(12) Uani 1 1 d . . .
SiA Si 0.11779(4) 0.02589(4) 0.41617(6) 0.02700(13) Uani 0.83 1 d P A 1
SiB Si 0.11746(17) 0.09139(18) 0.4048(3) 0.0242(6) Uiso 0.17 1 d P A 2
O O -0.16057(12) -0.08568(13) -0.2001(2) 0.0561(5) Uani 1 1 d . A .
C1 C -0.10379(14) -0.05422(14) -0.1139(2) 0.0360(4) Uani 1 1 d . . .
C10 C 0.0000 0.0000 0.4625(3) 0.0258(6) Uani 1 3 d S . .
H10 H 0.0000 0.0000 0.5702 0.031 Uiso 1 3 calc SR A 1
C11 C 0.21307(13) 0.01686(14) 0.1230(2) 0.0378(4) Uani 1 1 d . A .
H11A H 0.1790 -0.0487 0.1420 0.045 Uiso 1 1 calc R . .
H11B H 0.2239 0.0249 0.0179 0.045 Uiso 1 1 calc R . .
C12 C 0.30408(14) 0.05573(18) 0.1979(3) 0.0504(6) Uani 1 1 d . . .
H12A H 0.3361 0.0258 0.1616 0.060 Uiso 1 1 calc R A .
H12B H 0.2949 0.0460 0.3020 0.060 Uiso 1 1 calc R . .
H12C H 0.3398 0.1204 0.1783 0.060 Uiso 1 1 calc R . .
C13 C 0.22216(15) 0.18591(14) 0.1620(3) 0.0491(6) Uani 1 1 d . A .
H13A H 0.1902 0.2194 0.1819 0.059 Uiso 1 1 calc R . .
H13B H 0.2684 0.2021 0.2376 0.059 Uiso 1 1 calc R . .
C14 C 0.26917(19) 0.21601(19) 0.0157(3) 0.0651(8) Uani 1 1 d . . .
H14A H 0.3101 0.2813 0.0166 0.078 Uiso 1 1 calc R A .
H14B H 0.2240 0.2006 -0.0600 0.078 Uiso 1 1 calc R . .
H14C H 0.3035 0.1855 -0.0030 0.078 Uiso 1 1 calc R . .
C15 C 0.20560(15) 0.11304(18) 0.5332(3) 0.0460(5) Uani 1 1 d . . .
H15A H 0.2648 0.1229 0.5044 0.055 Uiso 0.83 1 calc PR A 1
H15B H 0.1939 0.0929 0.6337 0.055 Uiso 0.83 1 calc PR A 1
H15C H 0.2045 0.1694 0.5236 0.055 Uiso 0.83 1 calc PR A 1
H15D H 0.1880 0.1235 0.6286 0.055 Uiso 0.17 1 d PR A 2
H15E H 0.2618 0.1663 0.5034 0.055 Uiso 0.17 1 d PR A 2
H15F H 0.2145 0.0609 0.5374 0.055 Uiso 0.17 1 d PR A 2
C16A C 0.13132(17) -0.07504(17) 0.4465(3) 0.0374(5) Uani 0.83 1 d P A 1
H16A H 0.0873 -0.1254 0.3878 0.045 Uiso 0.83 1 calc PR A 1
H16B H 0.1214 -0.0919 0.5485 0.045 Uiso 0.83 1 calc PR A 1
H16C H 0.1923 -0.0604 0.4190 0.045 Uiso 0.83 1 calc PR A 1
C16B C 0.1344(9) 0.2074(8) 0.4328(15) 0.039(3) Uiso 0.17 1 d P A 2
H16D H 0.1229 0.2147 0.5339 0.046 Uiso 0.17 1 calc PR A 2
H16E H 0.0927 0.2156 0.3711 0.046 Uiso 0.17 1 calc PR A 2
H16F H 0.1965 0.2524 0.4080 0.046 Uiso 0.17 1 calc PR A 2

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
Mo 0.02406(8) 0.02406(8) 0.02198(12) 0.000 0.000 0.01203(4)
P 0.0230(2) 0.0360(3) 0.0275(3) -0.0068(2) 0.00107(19) 0.0111(2)
SiA 0.0259(3) 0.0302(3) 0.0251(3) -0.0031(2) -0.0031(2) 0.0141(2)
O 0.0476(9) 0.0636(11) 0.0425(10) 0.0016(8) -0.0174(8) 0.0168(8)
C1 0.0356(11) 0.0390(11) 0.0297(10) 0.0040(8) 0.0007(8) 0.0159(9)
C10 0.0268(8) 0.0268(8) 0.0238(13) 0.000 0.000 0.0134(4)
C11 0.0293(10) 0.0453(11) 0.0401(12) -0.0087(9) -0.0037(8) 0.0196(9)
C12 0.0313(10) 0.0639(15) 0.0573(15) -0.0093(11) -0.0094(10) 0.0248(10)
C13 0.0334(10) 0.0345(10) 0.0703(17) -0.0091(10) 0.0013(10) 0.0100(8)
C14 0.0459(14) 0.0506(14) 0.083(2) 0.0202(14) 0.0087(13) 0.0121(11)
C15 0.0348(11) 0.0618(15) 0.0357(12) -0.0094(10) -0.0094(9) 0.0198(10)
C16A 0.0372(13) 0.0425(13) 0.0399(14) 0.0024(11) -0.0024(10) 0.0255(11)

_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
Mo C1 1.955(2) 2 ?
Mo C1 1.955(2) . ?
Mo C1 1.955(2) 3 ?
Mo P 2.5582(5) . ?
Mo P 2.5582(5) 2 ?
Mo P 2.5582(5) 3 ?
P C11 1.846(2) . ?
P C13 1.847(2) . ?
P SiB 2.277(3) . ?
P SiA 2.3245(8) . ?
SiA C15 1.853(2) . ?
SiA C16A 1.879(3) . ?
SiA C10 1.8886(9) . ?
SiB C15 1.812(3) . ?
SiB C16B 1.880(13) . ?
SiB C10 1.909(3) . ?
O C1 1.164(3) . ?
C10 SiA 1.8886(9) 3 ?
C10 SiA 1.8887(9) 2 ?
C10 SiB 1.909(3) 3 ?
C10 SiB 1.909(3) 2 ?
C11 C12 1.524(3) . ?
C13 C14 1.531(4) . ?

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
C1 Mo C1 86.18(9) 2 . ?
C1 Mo C1 86.18(9) 2 3 ?
C1 Mo C1 86.18(9) . 3 ?
C1 Mo P 89.22(6) 2 . ?
C1 Mo P 175.35(7) . . ?
C1 Mo P 94.25(7) 3 . ?
C1 Mo P 175.34(7) 2 2 ?
C1 Mo P 94.25(7) . 2 ?
C1 Mo P 89.22(6) 3 2 ?
P Mo P 90.388(15) . 2 ?
C1 Mo P 94.25(7) 2 3 ?
C1 Mo P 89.22(6) . 3 ?
C1 Mo P 175.35(7) 3 3 ?
P Mo P 90.388(15) . 3 ?
P Mo P 90.388(15) 2 3 ?
C11 P C13 100.92(10) . . ?
C11 P SiB 123.78(10) . . ?
C13 P SiB 86.13(11) . . ?
C11 P SiA 100.37(7) . . ?
C13 P SiA 107.51(9) . . ?
C11 P Mo 111.27(7) . . ?
C13 P Mo 117.97(9) . . ?
SiB P Mo 113.77(7) . . ?
SiA P Mo 116.33(2) . . ?
C15 SiA C16A 103.32(12) . . ?
C15 SiA C10 113.49(11) . . ?
C16A SiA C10 111.08(9) . . ?
C15 SiA P 112.72(9) . . ?
C16A SiA P 108.79(9) . . ?
C10 SiA P 107.38(9) . . ?
C15 SiB C16B 91.2(4) . . ?
C15 SiB C10 114.41(19) . . ?
C16B SiB C10 111.8(4) . . ?
C15 SiB P 116.60(15) . . ?
C16B SiB P 113.5(4) . . ?
C10 SiB P 108.55(15) . . ?
O C1 Mo 174.2(2) . . ?
SiA C10 SiA 114.98(7) 3 . ?
SiA C10 SiA 114.97(7) 3 2 ?
SiA C10 SiA 114.98(7) . 2 ?
SiB C10 SiB 112.45(11) . 3 ?
SiB C10 SiB 112.45(11) . 2 ?
SiB C10 SiB 112.45(11) 3 2 ?
C12 C11 P 117.19(15) . . ?
C14 C13 P 113.91(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Mo P C11 -12.22(10) 2 . . . ?
C1 Mo P C11 -3.2(8) . . . . ?
C1 Mo P C11 -98.33(10) 3 . . . ?
P Mo P C11 172.42(8) 2 . . . ?
P Mo P C11 82.03(8) 3 . . . ?
C1 Mo P C13 103.69(11) 2 . . . ?
C1 Mo P C13 112.7(8) . . . . ?
C1 Mo P C13 17.58(11) 3 . . . ?
P Mo P C13 -71.67(9) 2 . . . ?
P Mo P C13 -162.06(9) 3 . . . ?
C1 Mo P SiB -157.65(10) 2 . . . ?
C1 Mo P SiB -148.6(8) . . . . ?
C1 Mo P SiB 116.23(10) 3 . . . ?
P Mo P SiB 26.98(8) 2 . . . ?
P Mo P SiB -63.41(8) 3 . . . ?
C1 Mo P SiA -126.31(7) 2 . . . ?
C1 Mo P SiA -117.3(8) . . . . ?
C1 Mo P SiA 147.58(7) 3 . . . ?
P Mo P SiA 58.33(2) 2 . . . ?
P Mo P SiA -32.06(2) 3 . . . ?
C11 P SiA C15 88.75(11) . . . . ?
C13 P SiA C15 -16.30(12) . . . . ?
Mo P SiA C15 -151.11(9) . . . . ?
C11 P SiA C16A -25.22(11) . . . . ?
C13 P SiA C16A -130.27(12) . . . . ?
Mo P SiA C16A 94.92(9) . . . . ?
C11 P SiA C10 -145.52(7) . . . . ?
C13 P SiA C10 109.43(9) . . . . ?
Mo P SiA C10 -25.38(5) . . . . ?
C11 P SiB C15 26.4(2) . . . . ?
C13 P SiB C15 -74.15(19) . . . . ?
Mo P SiB C15 166.91(14) . . . . ?
C11 P SiB C16B 130.5(4) . . . . ?
C13 P SiB C16B 29.9(5) . . . . ?
Mo P SiB C16B -89.0(4) . . . . ?
C11 P SiB C10 -104.56(14) . . . . ?
C13 P SiB C10 154.89(14) . . . . ?
Mo P SiB C10 35.95(14) . . . . ?
C1 Mo C1 O -28(2) 2 . . . ?
C1 Mo C1 O 58.5(19) 3 . . . ?
P Mo C1 O -37(3) . . . . ?
P Mo C1 O 147(2) 2 . . . ?
P Mo C1 O -122(2) 3 . . . ?
C15 SiA C10 SiA -152.18(15) . . . 3 ?
C16A SiA C10 SiA -36.3(2) . . . 3 ?
P SiA C10 SiA 82.55(13) . . . 3 ?
C15 SiA C10 SiA 70.87(19) . . . 2 ?
C16A SiA C10 SiA -173.24(14) . . . 2 ?
P SiA C10 SiA -54.40(15) . . . 2 ?
C15 SiB C10 SiB -88.2(3) . . . 3 ?
C16B SiB C10 SiB 169.9(5) . . . 3 ?
P SiB C10 SiB 43.9(2) . . . 3 ?
C15 SiB C10 SiB 143.6(2) . . . 2 ?
C16B SiB C10 SiB 41.7(5) . . . 2 ?
P SiB C10 SiB -84.26(15) . . . 2 ?
C13 P C11 C12 48.1(2) . . . . ?
SiB P C11 C12 -44.6(2) . . . . ?
SiA P C11 C12 -62.20(18) . . . . ?
Mo P C11 C12 174.08(16) . . . . ?
C11 P C13 C14 55.4(2) . . . . ?
SiB P C13 C14 179.1(2) . . . . ?
SiA P C13 C14 160.07(18) . . . . ?
Mo P C13 C14 -66.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.35
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.043

#===END

data_10b
_database_code_depnum_ccdc_archive 'CCDC 289576'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_formula_moiety         'C23 H51 Mo O3 P3 Si3'
_chemical_formula_sum            'C23 H51 Mo O3 P3 Si3'
_chemical_formula_weight         648.76

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'
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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   11.5080(5)
_cell_length_b                   17.2076(7)
_cell_length_c                   16.6511(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3365(7)
_cell_angle_gamma                90.00
_cell_volume                     3297.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    6208
_cell_measurement_theta_min      2.157
_cell_measurement_theta_max      26.368

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7559
_exptl_absorpt_correction_T_max  0.8496
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(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 PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21617
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         26.39
_reflns_number_total             6733
_reflns_number_gt                6370
_reflns_threshold_expression     I>2\s(I)

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

_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^)+(0.0306P)^2^+1.4152P] 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     SHELXL
_refine_ls_extinction_coef       0.0090(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6733
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0587
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo 0.156802(10) 0.259032(7) 0.199130(7) 0.01938(5) Uani 1 1 d . . .
P1 P 0.23824(3) 0.21836(2) 0.33606(2) 0.02163(8) Uani 1 1 d . . .
P2 P 0.00681(3) 0.34851(2) 0.26377(2) 0.02090(8) Uani 1 1 d . . .
P3 P 0.00966(3) 0.14801(2) 0.20437(2) 0.02324(9) Uani 1 1 d . . .
Si1 Si 0.10871(4) 0.17286(2) 0.42917(2) 0.02510(9) Uani 1 1 d . . .
Si2 Si -0.06113(3) 0.31225(2) 0.38736(2) 0.02393(9) Uani 1 1 d . . .
Si3 Si -0.10956(4) 0.14475(2) 0.31455(3) 0.02768(10) Uani 1 1 d . . .
O1 O 0.08688(12) 0.28355(9) 0.01967(7) 0.0472(3) Uani 1 1 d . . .
O2 O 0.36230(12) 0.16785(9) 0.12324(8) 0.0517(4) Uani 1 1 d . . .
O3 O 0.31960(13) 0.40233(8) 0.17517(10) 0.0553(4) Uani 1 1 d . . .
C1 C 0.10773(13) 0.27690(10) 0.08771(9) 0.0290(3) Uani 1 1 d . . .
C2 C 0.28336(14) 0.19847(10) 0.15255(9) 0.0303(3) Uani 1 1 d . . .
C3 C 0.25972(14) 0.34944(10) 0.18740(10) 0.0318(3) Uani 1 1 d . . .
C4 C -0.04572(13) 0.20258(9) 0.40165(9) 0.0253(3) Uani 1 1 d . . .
C5 C -0.12124(16) 0.18111(10) 0.47750(10) 0.0375(4) Uani 1 1 d . . .
H5A H -0.1166 0.1250 0.4873 0.045 Uiso 1 1 calc R . .
H5B H -0.2023 0.1958 0.4677 0.045 Uiso 1 1 calc R . .
H5C H -0.0916 0.2092 0.5246 0.045 Uiso 1 1 calc R . .
C11 C 0.34211(15) 0.13660(10) 0.32687(10) 0.0325(3) Uani 1 1 d . . .
H11A H 0.2984 0.0907 0.3075 0.039 Uiso 1 1 calc R . .
H11B H 0.3989 0.1503 0.2847 0.039 Uiso 1 1 calc R . .
C12 C 0.41028(17) 0.11236(12) 0.40174(11) 0.0447(4) Uani 1 1 d . . .
H12A H 0.4647 0.0707 0.3879 0.054 Uiso 1 1 calc R . .
H12B H 0.3563 0.0937 0.4427 0.054 Uiso 1 1 calc R . .
H12C H 0.4536 0.1571 0.4226 0.054 Uiso 1 1 calc R . .
C13 C 0.32790(14) 0.29099(10) 0.39119(10) 0.0328(3) Uani 1 1 d . . .
H13A H 0.2818 0.3391 0.3980 0.039 Uiso 1 1 calc R . .
H13B H 0.3459 0.2704 0.4454 0.039 Uiso 1 1 calc R . .
C14 C 0.44160(15) 0.31135(12) 0.34940(13) 0.0449(4) Uani 1 1 d . . .
H14A H 0.4837 0.3503 0.3811 0.054 Uiso 1 1 calc R . .
H14B H 0.4247 0.3323 0.2959 0.054 Uiso 1 1 calc R . .
H14C H 0.4894 0.2645 0.3444 0.054 Uiso 1 1 calc R . .
C15 C 0.12006(17) 0.06415(10) 0.43291(11) 0.0404(4) Uani 1 1 d . . .
H15A H 0.0650 0.0438 0.4724 0.048 Uiso 1 1 calc R . .
H15B H 0.1993 0.0493 0.4485 0.048 Uiso 1 1 calc R . .
H15C H 0.1018 0.0426 0.3798 0.048 Uiso 1 1 calc R . .
C16 C 0.14958(18) 0.20410(11) 0.53389(10) 0.0410(4) Uani 1 1 d . . .
H16A H 0.0925 0.1839 0.5720 0.049 Uiso 1 1 calc R . .
H16B H 0.1508 0.2610 0.5367 0.049 Uiso 1 1 calc R . .
H16C H 0.2267 0.1837 0.5475 0.049 Uiso 1 1 calc R . .
C21 C -0.12487(13) 0.37022(9) 0.20281(10) 0.0294(3) Uani 1 1 d . . .
H21A H -0.1628 0.3207 0.1874 0.035 Uiso 1 1 calc R . .
H21B H -0.1803 0.4001 0.2360 0.035 Uiso 1 1 calc R . .
C22 C -0.09801(16) 0.41637(11) 0.12711(10) 0.0389(4) Uani 1 1 d . . .
H22A H -0.1703 0.4264 0.0975 0.047 Uiso 1 1 calc R . .
H22B H -0.0449 0.3865 0.0932 0.047 Uiso 1 1 calc R . .
H22C H -0.0616 0.4659 0.1419 0.047 Uiso 1 1 calc R . .
C23 C 0.06225(14) 0.44798(8) 0.28350(10) 0.0284(3) Uani 1 1 d . . .
H23A H 0.1232 0.4443 0.3255 0.034 Uiso 1 1 calc R . .
H23B H 0.1001 0.4669 0.2340 0.034 Uiso 1 1 calc R . .
C24 C -0.02567(16) 0.50933(9) 0.30995(11) 0.0373(4) Uani 1 1 d . . .
H24A H 0.0148 0.5583 0.3209 0.045 Uiso 1 1 calc R . .
H24B H -0.0649 0.4916 0.3587 0.045 Uiso 1 1 calc R . .
H24C H -0.0832 0.5173 0.2671 0.045 Uiso 1 1 calc R . .
C25 C -0.21445(14) 0.34624(10) 0.40422(11) 0.0380(4) Uani 1 1 d . . .
H25A H -0.2400 0.3299 0.4577 0.046 Uiso 1 1 calc R . .
H25B H -0.2657 0.3235 0.3633 0.046 Uiso 1 1 calc R . .
H25C H -0.2175 0.4030 0.4005 0.046 Uiso 1 1 calc R . .
C26 C 0.02838(15) 0.36760(9) 0.46273(9) 0.0320(3) Uani 1 1 d . . .
H26A H 0.0031 0.3542 0.5171 0.038 Uiso 1 1 calc R . .
H26B H 0.0183 0.4235 0.4539 0.038 Uiso 1 1 calc R . .
H26C H 0.1105 0.3539 0.4565 0.038 Uiso 1 1 calc R . .
C31 C 0.06833(16) 0.04771(9) 0.19750(10) 0.0350(4) Uani 1 1 d . . .
H31A H 0.1245 0.0393 0.2419 0.042 Uiso 1 1 calc R . .
H31B H 0.0039 0.0102 0.2043 0.042 Uiso 1 1 calc R . .
C32 C 0.1288(2) 0.03138(11) 0.11757(13) 0.0508(5) Uani 1 1 d . . .
H32A H 0.1612 -0.0213 0.1183 0.061 Uiso 1 1 calc R . .
H32B H 0.1915 0.0691 0.1097 0.061 Uiso 1 1 calc R . .
H32C H 0.0724 0.0359 0.0735 0.061 Uiso 1 1 calc R . .
C33 C -0.09411(15) 0.14864(10) 0.11836(10) 0.0351(4) Uani 1 1 d . . .
H33A H -0.1442 0.1951 0.1237 0.042 Uiso 1 1 calc R . .
H33B H -0.0487 0.1551 0.0685 0.042 Uiso 1 1 calc R . .
C34 C -0.17339(18) 0.07772(13) 0.10756(12) 0.0499(5) Uani 1 1 d . . .
H34A H -0.2243 0.0857 0.0609 0.060 Uiso 1 1 calc R . .
H34B H -0.2208 0.0709 0.1557 0.060 Uiso 1 1 calc R . .
H34C H -0.1258 0.0312 0.0992 0.060 Uiso 1 1 calc R . .
C35 C -0.14092(19) 0.04094(11) 0.34286(12) 0.0458(5) Uani 1 1 d . . .
H35A H -0.1908 0.0399 0.3904 0.055 Uiso 1 1 calc R . .
H35B H -0.0678 0.0140 0.3548 0.055 Uiso 1 1 calc R . .
H35C H -0.1805 0.0149 0.2981 0.055 Uiso 1 1 calc R . .
C36 C -0.25632(14) 0.18474(12) 0.28645(12) 0.0428(4) Uani 1 1 d . . .
H36A H -0.3071 0.1837 0.3335 0.051 Uiso 1 1 calc R . .
H36B H -0.2905 0.1530 0.2436 0.051 Uiso 1 1 calc R . .
H36C H -0.2478 0.2384 0.2677 0.051 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
Mo 0.01914(8) 0.01867(8) 0.02035(8) 0.00251(4) 0.00254(5) 0.00104(4)
P1 0.02189(18) 0.02090(18) 0.02210(17) -0.00059(14) -0.00017(13) 0.00249(14)
P2 0.02047(17) 0.01745(17) 0.02479(18) 0.00028(13) 0.00124(13) 0.00013(13)
P3 0.02604(18) 0.01969(18) 0.02399(18) -0.00064(13) -0.00056(14) -0.00210(14)
Si1 0.0329(2) 0.0215(2) 0.02092(19) 0.00204(14) 0.00195(16) 0.00035(16)
Si2 0.02291(19) 0.0223(2) 0.0267(2) -0.00213(15) 0.00619(15) -0.00035(15)
Si3 0.0263(2) 0.0246(2) 0.0322(2) -0.00060(16) 0.00469(16) -0.00824(16)
O1 0.0458(7) 0.0698(9) 0.0261(6) 0.0080(6) -0.0005(5) 0.0136(7)
O2 0.0509(8) 0.0641(9) 0.0403(7) 0.0125(6) 0.0208(6) 0.0311(7)
O3 0.0537(8) 0.0422(8) 0.0702(10) 0.0111(7) 0.0088(7) -0.0217(7)
C1 0.0258(7) 0.0324(8) 0.0287(8) 0.0047(6) 0.0034(6) 0.0051(6)
C2 0.0337(8) 0.0334(8) 0.0238(7) 0.0069(6) 0.0053(6) 0.0076(7)
C3 0.0301(8) 0.0301(8) 0.0351(8) 0.0042(6) 0.0043(6) -0.0011(6)
C4 0.0273(7) 0.0236(7) 0.0252(7) 0.0007(6) 0.0079(6) -0.0030(6)
C5 0.0428(9) 0.0345(9) 0.0355(9) 0.0017(7) 0.0175(7) -0.0063(7)
C11 0.0352(8) 0.0334(8) 0.0287(8) -0.0040(6) -0.0038(6) 0.0142(7)
C12 0.0486(11) 0.0468(11) 0.0385(9) -0.0017(8) -0.0111(8) 0.0211(9)
C13 0.0284(8) 0.0335(9) 0.0366(8) -0.0082(7) -0.0021(6) -0.0030(7)
C14 0.0265(8) 0.0497(11) 0.0585(12) -0.0027(9) -0.0029(8) -0.0070(8)
C15 0.0536(11) 0.0246(8) 0.0430(9) 0.0091(7) -0.0004(8) 0.0013(7)
C16 0.0540(11) 0.0449(10) 0.0239(7) -0.0002(7) -0.0019(7) 0.0058(8)
C21 0.0253(7) 0.0258(7) 0.0370(8) -0.0002(6) -0.0043(6) 0.0026(6)
C22 0.0412(9) 0.0406(10) 0.0348(9) 0.0046(7) -0.0067(7) 0.0097(8)
C23 0.0298(8) 0.0203(7) 0.0352(8) -0.0013(6) 0.0017(6) -0.0040(6)
C24 0.0438(10) 0.0214(8) 0.0468(10) -0.0046(7) 0.0019(8) 0.0010(7)
C25 0.0291(8) 0.0367(9) 0.0485(10) -0.0021(8) 0.0126(7) 0.0040(7)
C26 0.0385(9) 0.0293(8) 0.0283(7) -0.0051(6) 0.0034(6) -0.0007(7)
C31 0.0442(9) 0.0210(7) 0.0397(9) -0.0021(6) -0.0013(7) 0.0020(7)
C32 0.0621(13) 0.0330(10) 0.0574(12) -0.0134(9) 0.0131(10) 0.0056(9)
C33 0.0375(9) 0.0353(9) 0.0323(8) -0.0006(7) -0.0095(7) -0.0052(7)
C34 0.0490(11) 0.0510(12) 0.0494(11) -0.0070(9) -0.0146(9) -0.0170(9)
C35 0.0573(12) 0.0327(9) 0.0474(10) 0.0022(8) 0.0066(9) -0.0208(8)
C36 0.0257(8) 0.0453(10) 0.0575(11) -0.0076(9) 0.0014(8) -0.0078(7)

_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
Mo C2 1.9550(16) . ?
Mo C1 1.9604(16) . ?
Mo C3 1.9657(16) . ?
Mo P3 2.5547(4) . ?
Mo P2 2.5554(4) . ?
Mo P1 2.5577(4) . ?
P1 C11 1.8530(16) . ?
P1 C13 1.8597(16) . ?
P1 Si1 2.2947(5) . ?
P2 C23 1.8554(15) . ?
P2 C21 1.8569(15) . ?
P2 Si2 2.2923(5) . ?
P3 C31 1.8571(16) . ?
P3 C33 1.8594(16) . ?
P3 Si3 2.2979(6) . ?
Si1 C15 1.8762(17) . ?
Si1 C16 1.8818(17) . ?
Si1 C4 1.9028(16) . ?
Si2 C26 1.8782(16) . ?
Si2 C25 1.8814(17) . ?
Si2 C4 1.9103(16) . ?
Si3 C36 1.8803(19) . ?
Si3 C35 1.8829(18) . ?
Si3 C4 1.9028(16) . ?
O1 C1 1.162(2) . ?
O2 C2 1.160(2) . ?
O3 C3 1.160(2) . ?
C4 C5 1.581(2) . ?
C11 C12 1.527(2) . ?
C13 C14 1.526(2) . ?
C21 C22 1.523(2) . ?
C23 C24 1.529(2) . ?
C31 C32 1.531(3) . ?
C33 C34 1.534(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
C2 Mo C1 85.37(6) . . ?
C2 Mo C3 86.09(7) . . ?
C1 Mo C3 87.26(7) . . ?
C2 Mo P3 96.34(5) . . ?
C1 Mo P3 87.84(5) . . ?
C3 Mo P3 174.34(5) . . ?
C2 Mo P2 174.20(5) . . ?
C1 Mo P2 96.46(5) . . ?
C3 Mo P2 88.50(5) . . ?
P3 Mo P2 89.236(12) . . ?
C2 Mo P1 86.44(4) . . ?
C1 Mo P1 171.33(5) . . ?
C3 Mo P1 95.01(5) . . ?
P3 Mo P1 90.251(12) . . ?
P2 Mo P1 91.964(12) . . ?
C11 P1 C13 101.23(8) . . ?
C11 P1 Si1 102.63(6) . . ?
C13 P1 Si1 104.87(6) . . ?
C11 P1 Mo 111.55(5) . . ?
C13 P1 Mo 117.10(6) . . ?
Si1 P1 Mo 117.360(18) . . ?
C23 P2 C21 100.94(7) . . ?
C23 P2 Si2 102.17(5) . . ?
C21 P2 Si2 105.31(5) . . ?
C23 P2 Mo 113.45(5) . . ?
C21 P2 Mo 116.23(5) . . ?
Si2 P2 Mo 116.676(18) . . ?
C31 P3 C33 100.96(8) . . ?
C31 P3 Si3 104.22(6) . . ?
C33 P3 Si3 103.37(6) . . ?
C31 P3 Mo 116.85(6) . . ?
C33 P3 Mo 113.09(6) . . ?
Si3 P3 Mo 116.390(18) . . ?
C15 Si1 C16 103.72(8) . . ?
C15 Si1 C4 109.92(8) . . ?
C16 Si1 C4 111.98(8) . . ?
C15 Si1 P1 108.50(6) . . ?
C16 Si1 P1 111.64(7) . . ?
C4 Si1 P1 110.80(5) . . ?
C26 Si2 C25 104.70(8) . . ?
C26 Si2 C4 111.57(7) . . ?
C25 Si2 C4 112.02(7) . . ?
C26 Si2 P2 105.85(5) . . ?
C25 Si2 P2 111.99(6) . . ?
C4 Si2 P2 110.41(5) . . ?
C36 Si3 C35 103.67(9) . . ?
C36 Si3 C4 109.91(8) . . ?
C35 Si3 C4 112.27(8) . . ?
C36 Si3 P3 109.39(7) . . ?
C35 Si3 P3 109.83(7) . . ?
C4 Si3 P3 111.48(5) . . ?
O1 C1 Mo 174.02(14) . . ?
O2 C2 Mo 174.79(15) . . ?
O3 C3 Mo 175.59(15) . . ?
C5 C4 Si1 105.18(11) . . ?
C5 C4 Si3 105.97(11) . . ?
Si1 C4 Si3 113.51(8) . . ?
C5 C4 Si2 106.22(10) . . ?
Si1 C4 Si2 112.42(7) . . ?
Si3 C4 Si2 112.74(8) . . ?
C12 C11 P1 117.94(12) . . ?
C14 C13 P1 113.82(12) . . ?
C22 C21 P2 112.86(11) . . ?
C24 C23 P2 117.42(11) . . ?
C32 C31 P3 113.04(12) . . ?
C34 C33 P3 117.68(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Mo P1 C11 -14.90(8) . . . . ?
C1 Mo P1 C11 4.2(3) . . . . ?
C3 Mo P1 C11 -100.65(8) . . . . ?
P3 Mo P1 C11 81.44(6) . . . . ?
P2 Mo P1 C11 170.68(6) . . . . ?
C2 Mo P1 C13 101.03(8) . . . . ?
C1 Mo P1 C13 120.1(3) . . . . ?
C3 Mo P1 C13 15.28(8) . . . . ?
P3 Mo P1 C13 -162.64(6) . . . . ?
P2 Mo P1 C13 -73.39(6) . . . . ?
C2 Mo P1 Si1 -132.87(5) . . . . ?
C1 Mo P1 Si1 -113.8(3) . . . . ?
C3 Mo P1 Si1 141.38(5) . . . . ?
P3 Mo P1 Si1 -36.54(2) . . . . ?
P2 Mo P1 Si1 52.71(2) . . . . ?
C2 Mo P2 C23 13.4(4) . . . . ?
C1 Mo P2 C23 -94.72(7) . . . . ?
C3 Mo P2 C23 -7.64(7) . . . . ?
P3 Mo P2 C23 177.54(6) . . . . ?
P1 Mo P2 C23 87.32(6) . . . . ?
C2 Mo P2 C21 129.8(4) . . . . ?
C1 Mo P2 C21 21.68(8) . . . . ?
C3 Mo P2 C21 108.75(8) . . . . ?
P3 Mo P2 C21 -66.06(6) . . . . ?
P1 Mo P2 C21 -156.29(6) . . . . ?
C2 Mo P2 Si2 -104.9(4) . . . . ?
C1 Mo P2 Si2 146.91(5) . . . . ?
C3 Mo P2 Si2 -126.01(5) . . . . ?
P3 Mo P2 Si2 59.17(2) . . . . ?
P1 Mo P2 Si2 -31.05(2) . . . . ?
C2 Mo P3 C31 18.34(8) . . . . ?
C1 Mo P3 C31 103.44(8) . . . . ?
C3 Mo P3 C31 133.5(5) . . . . ?
P2 Mo P3 C31 -160.06(6) . . . . ?
P1 Mo P3 C31 -68.10(6) . . . . ?
C2 Mo P3 C33 -98.23(8) . . . . ?
C1 Mo P3 C33 -13.13(8) . . . . ?
C3 Mo P3 C33 16.9(5) . . . . ?
P2 Mo P3 C33 83.37(6) . . . . ?
P1 Mo P3 C33 175.33(6) . . . . ?
C2 Mo P3 Si3 142.29(5) . . . . ?
C1 Mo P3 Si3 -132.62(5) . . . . ?
C3 Mo P3 Si3 -102.6(5) . . . . ?
P2 Mo P3 Si3 -36.12(2) . . . . ?
P1 Mo P3 Si3 55.84(2) . . . . ?
C11 P1 Si1 C15 -20.21(8) . . . . ?
C13 P1 Si1 C15 -125.63(9) . . . . ?
Mo P1 Si1 C15 102.46(7) . . . . ?
C11 P1 Si1 C16 93.48(8) . . . . ?
C13 P1 Si1 C16 -11.95(9) . . . . ?
Mo P1 Si1 C16 -143.86(7) . . . . ?
C11 P1 Si1 C4 -140.97(7) . . . . ?
C13 P1 Si1 C4 113.61(8) . . . . ?
Mo P1 Si1 C4 -18.30(6) . . . . ?
C23 P2 Si2 C26 -27.98(8) . . . . ?
C21 P2 Si2 C26 -133.08(8) . . . . ?
Mo P2 Si2 C26 96.35(6) . . . . ?
C23 P2 Si2 C25 85.55(8) . . . . ?
C21 P2 Si2 C25 -19.55(8) . . . . ?
Mo P2 Si2 C25 -150.12(6) . . . . ?
C23 P2 Si2 C4 -148.88(7) . . . . ?
C21 P2 Si2 C4 106.03(7) . . . . ?
Mo P2 Si2 C4 -24.54(6) . . . . ?
C31 P3 Si3 C36 -128.53(9) . . . . ?
C33 P3 Si3 C36 -23.36(9) . . . . ?
Mo P3 Si3 C36 101.25(7) . . . . ?
C31 P3 Si3 C35 -15.38(9) . . . . ?
C33 P3 Si3 C35 89.80(9) . . . . ?
Mo P3 Si3 C35 -145.60(7) . . . . ?
C31 P3 Si3 C4 109.71(8) . . . . ?
C33 P3 Si3 C4 -145.12(8) . . . . ?
Mo P3 Si3 C4 -20.51(6) . . . . ?
C2 Mo C1 O1 0.3(15) . . . . ?
C3 Mo C1 O1 86.6(15) . . . . ?
P3 Mo C1 O1 -96.3(15) . . . . ?
P2 Mo C1 O1 174.8(15) . . . . ?
P1 Mo C1 O1 -18.9(18) . . . . ?
C1 Mo C2 O2 74.3(16) . . . . ?
C3 Mo C2 O2 -13.3(16) . . . . ?
P3 Mo C2 O2 161.6(16) . . . . ?
P2 Mo C2 O2 -34.4(19) . . . . ?
P1 Mo C2 O2 -108.6(16) . . . . ?
C2 Mo C3 O3 69(2) . . . . ?
C1 Mo C3 O3 -17(2) . . . . ?
P3 Mo C3 O3 -47(2) . . . . ?
P2 Mo C3 O3 -114(2) . . . . ?
P1 Mo C3 O3 155(2) . . . . ?
C15 Si1 C4 C5 70.01(12) . . . . ?
C16 Si1 C4 C5 -44.72(13) . . . . ?
P1 Si1 C4 C5 -170.08(9) . . . . ?
C15 Si1 C4 Si3 -45.39(10) . . . . ?
C16 Si1 C4 Si3 -160.12(8) . . . . ?
P1 Si1 C4 Si3 74.52(8) . . . . ?
C15 Si1 C4 Si2 -174.84(8) . . . . ?
C16 Si1 C4 Si2 70.43(10) . . . . ?
P1 Si1 C4 Si2 -54.93(8) . . . . ?
C36 Si3 C4 C5 70.18(13) . . . . ?
C35 Si3 C4 C5 -44.64(14) . . . . ?
P3 Si3 C4 C5 -168.36(9) . . . . ?
C36 Si3 C4 Si1 -174.89(8) . . . . ?
C35 Si3 C4 Si1 70.28(10) . . . . ?
P3 Si3 C4 Si1 -53.43(8) . . . . ?
C36 Si3 C4 Si2 -45.60(10) . . . . ?
C35 Si3 C4 Si2 -160.43(9) . . . . ?
P3 Si3 C4 Si2 75.86(7) . . . . ?
C26 Si2 C4 C5 76.00(12) . . . . ?
C25 Si2 C4 C5 -41.02(13) . . . . ?
P2 Si2 C4 C5 -166.58(10) . . . . ?
C26 Si2 C4 Si1 -38.52(10) . . . . ?
C25 Si2 C4 Si1 -155.54(8) . . . . ?
P2 Si2 C4 Si1 78.91(7) . . . . ?
C26 Si2 C4 Si3 -168.37(7) . . . . ?
C25 Si2 C4 Si3 74.61(10) . . . . ?
P2 Si2 C4 Si3 -50.94(8) . . . . ?
C13 P1 C11 C12 46.95(16) . . . . ?
Si1 P1 C11 C12 -61.26(15) . . . . ?
Mo P1 C11 C12 172.24(13) . . . . ?
C11 P1 C13 C14 56.35(15) . . . . ?
Si1 P1 C13 C14 162.81(12) . . . . ?
Mo P1 C13 C14 -65.13(14) . . . . ?
C23 P2 C21 C22 57.99(13) . . . . ?
Si2 P2 C21 C22 163.99(11) . . . . ?
Mo P2 C21 C22 -65.19(13) . . . . ?
C21 P2 C23 C24 45.74(14) . . . . ?
Si2 P2 C23 C24 -62.73(13) . . . . ?
Mo P2 C23 C24 170.81(11) . . . . ?
C33 P3 C31 C32 60.16(15) . . . . ?
Si3 P3 C31 C32 167.14(13) . . . . ?
Mo P3 C31 C32 -62.91(15) . . . . ?
C31 P3 C33 C34 44.62(16) . . . . ?
Si3 P3 C33 C34 -63.03(15) . . . . ?
Mo P3 C33 C34 170.25(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.39
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.062

#===END