Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002


data_global
#========================================================================
#======
_audit_creation_date             9-04-01

_journal_coden_Cambridge         186

loop_
_publ_author_name
'Lutz Gade'
'Ralf A. Findeis'

_publ_contact_author_name        'Prof Lutz Gade'
_publ_contact_author_address     
;
Laboratoire de Chimie 
Organometallique et de Catalysis 
Institut Le Bel 
Universite Louis Pasteur 
4 rue Blaise Pascal 
67070 Strasbourg, Cedex 
FRANCE 
;

_publ_contact_author_phone       0033-390-241530
_publ_contact_author_fax         0033-390-241531
_publ_contact_author_email       gade@chimie.u-strasbg.fr

_publ_requested_journal          'J. Chem. Soc. Dalton Trans.'

_publ_requested_category         FM
#========================================================================

_publ_section_title              
; 
Tridentate Phosphine Ligands with Novel Linker-Units
;

# 4. TEXT

_publ_section_abstract           
; 
The synthesis of two novel types of tripodal phosphine ligands containing vinyl
and alkynyl linker functions in their ligand backbones are reported. 
Using pentaerythrol (1) as the starting material the functionalized phosphines 
H2C=CH-CH2OCH2C(CH2PPh2)3 (6), Me3SiC*C-CH2OCH2C(CH2PPh2)3 (10) and 
HC*C-CH2OCH2C(CH2PPh2)3 (11) were obtained in good yield in 4-5-step syntheses.
H2C=CH-CH2OCH2C(CH2PPh2)3 (6) and the silyl 
protected alkinyl derivative (CH3)3Si-C*C-CH2OCH2C(CH2PPh2)3 (10) were reacted 
with one molar equivalent of [Mo(CO)3(MeCN)3] to yield the yellow-brown, 
air stable triphosphine-molybdenum complexes 
[{H2C=CH-CH2OCH2C(CH2PPh2)3}Mo(CO)3] (12) and 
[{(CH3)3Si-C*C-CH2OCH2C(CH2PPh2)3}Mo(CO)3] (13) the latter of which was 
characterized by X-ray diffraction.
;

_publ_section_comment            
; 
?
;

_publ_section_exptl_prep         
; 
Crystals grown from dichloromethane/hexane at 293 K
;

_publ_section_exptl_refinement   
; 
?
;

_publ_section_references         
;

Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G.,
Spagna, R. &Viterbo, D. (1989).  SIR.  J. Appl. Cryst. 22, 389-393.

OpenMoleN, Interactive Intelligent Structure  solution (1997)
Nonius B.V., Delft, The Netherlands.

KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands.

Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326.

Walker, N. & Stuart, D. (1983). Acta Cryst.,  A39, 158-166.

;

data_st882
_database_code_CSD               197230

#========================================================================
#======

# 5. CHEMICAL DATA

_chemical_name_systematic        
; 
?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C50 H49 Mo O4 P3 Si'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C50 H49 Mo O4 P3 Si'
_chemical_formula_weight         930.89
_chemical_melting_point          ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1
H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1
Mo ? -1.825 0.688 International_Tables_Vol_IV_Table_2.3.1
O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1
P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1
Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1

#========================================================================
#======

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a                   10.9160(2)
_cell_length_b                   22.8277(4)
_cell_length_c                   17.9896(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.864(5)
_cell_angle_gamma                90
_cell_volume                     4440.6(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    294
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_special_details            
;
Cell parameters refined using Scalepack part of DENZO
Z. Otwinowski, W. Minor, 1997
;

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_method    none

_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_T_max  1.0000

#========================================================================
#======

# 7. EXPERIMENTAL DATA

_diffrn_special_details          
; ?
;

_diffrn_ambient_temperature      294
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           Mo-K\a

_diffrn_source                   xray_tube

_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'

_diffrn_measurement_details      
;
10365 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  1.4 deg 1 scans of   80 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  130 frames
Set 2 Theta =   -6.30 Kappa =  -86.00 Phi   =    0.00   34 frames
Friedel pairs were averaged. Internal R = 0.06
;

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0

_diffrn_reflns_number            10365
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.5
_diffrn_reflns_theta_max         27.47

_reflns_number_total             10365
_reflns_number_gt                6776
_reflns_threshold_expression     >3.0\s(I)

_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_molecular_graphics    ?
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)

#========================================================================
#======

# 8. REFINEMENT DATA

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_expression ?
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_number_reflns         6776
_refine_ls_number_parameters     532
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.090
_refine_ls_R_factor_gt           0.044
_refine_ls_wR_factor_all         0.517
_refine_ls_wR_factor_ref         0.056
_refine_ls_goodness_of_fit_all   11.359
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_shift/su_max          0.005
_refine_ls_shift/esd_mean        0.000
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.170

#========================================================================
#======

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_type_symbol
MO 0.75707(3) 0.22375(1) 0.78761(2) 0.0186(1) Uani ? ? Mo
C1 0.8218(4) 0.1649(2) 0.7227(2) 0.028(2) Uani ? ? C
O1 0.8523(4) 0.1299(1) 0.6828(2) 0.052(2) Uani ? ? O
C2 0.6201(4) 0.1688(2) 0.7923(2) 0.033(2) Uani ? ? C
O2 0.5359(3) 0.1370(2) 0.7892(2) 0.054(2) Uani ? ? O
C3 0.6530(4) 0.2511(2) 0.6978(2) 0.028(2) Uani ? ? C
O3 0.5880(3) 0.2626(1) 0.6423(2) 0.044(2) Uani ? ? O
P1 0.8913(1) 0.18458(4) 0.90340(6) 0.0200(5) Uani ? ? P
C4 1.0093(4) 0.1277(2) 0.8947(2) 0.025(2) Uani ? ? C
C5 1.1014(6) 0.1388(2) 0.8525(3) 0.073(3) Uani ? ? C
C6 1.1961(6) 0.0990(3) 0.8477(4) 0.088(4) Uani ? ? C
C7 1.1967(5) 0.0469(2) 0.8839(3) 0.044(3) Uani ? ? C
C8 1.1074(5) 0.0347(2) 0.9249(3) 0.049(3) Uani ? ? C
C9 1.0141(5) 0.0750(2) 0.9314(3) 0.048(3) Uani ? ? C
C10 0.8093(4) 0.1528(2) 0.9764(2) 0.023(2) Uani ? ? C
C11 0.8320(5) 0.1667(2) 1.0522(2) 0.036(2) Uani ? ? C
C12 0.7607(5) 0.1421(2) 1.1027(3) 0.043(3) Uani ? ? C
C13 0.6670(5) 0.1044(2) 1.0791(3) 0.041(2) Uani ? ? C
C14 0.6448(4) 0.0890(2) 1.0049(3) 0.039(2) Uani ? ? C
C15 0.7160(4) 0.1125(2) 0.9539(2) 0.033(2) Uani ? ? C
C16 0.9932(3) 0.2423(2) 0.9499(2) 0.020(2) Uani ? ? C
C17 0.9428(3) 0.3060(2) 0.9463(2) 0.018(2) Uani ? ? C
C18 0.9693(4) 0.3380(2) 0.8740(2) 0.020(2) Uani ? ? C
P2 0.92563(9) 0.30066(4) 0.78319(5) 0.0194(4) Uani ? ? P
C19 1.0715(4) 0.2743(2) 0.7540(2) 0.022(2) Uani ? ? C
C20 1.0617(4) 0.2423(2) 0.6876(2) 0.029(2) Uani ? ? C
C21 1.1642(4) 0.2180(2) 0.6623(3) 0.039(2) Uani ? ? C
C22 1.2802(4) 0.2248(2) 0.7037(3) 0.040(2) Uani ? ? C
C23 1.2909(4) 0.2567(2) 0.7681(3) 0.042(3) Uani ? ? C
C24 1.1891(4) 0.2818(2) 0.7940(2) 0.032(2) Uani ? ? C
C25 0.8933(4) 0.3627(2) 0.7179(2) 0.025(2) Uani ? ? C
C26 0.8307(4) 0.3514(2) 0.6465(2) 0.030(2) Uani ? ? C
C27 0.8035(5) 0.3962(2) 0.5944(2) 0.039(2) Uani ? ? C
C28 0.8379(5) 0.4524(2) 0.6134(3) 0.044(3) Uani ? ? C
C29 0.9013(5) 0.4647(2) 0.6827(3) 0.042(3) Uani ? ? C
C30 0.9298(4) 0.4203(2) 0.7353(2) 0.033(2) Uani ? ? C
C31 0.8053(3) 0.3096(2) 0.9579(2) 0.019(2) Uani ? ? C
P3 0.68767(9) 0.30045(4) 0.87474(5) 0.0196(5) Uani ? ? P
C32 0.6616(4) 0.3743(2) 0.8349(2) 0.023(2) Uani ? ? C
C33 0.5938(4) 0.3786(2) 0.7634(2) 0.029(2) Uani ? ? C
C34 0.5731(4) 0.4324(2) 0.7283(3) 0.037(2) Uani ? ? C
C35 0.6173(5) 0.4830(2) 0.7638(3) 0.039(2) Uani ? ? C
C36 0.6815(4) 0.4799(2) 0.8354(3) 0.036(2) Uani ? ? C
C37 0.7040(4) 0.4262(2) 0.8705(2) 0.029(2) Uani ? ? C
C38 0.5517(3) 0.2907(2) 0.9235(2) 0.022(2) Uani ? ? C
C39 0.5167(4) 0.2351(2) 0.9411(3) 0.038(2) Uani ? ? C
C40 0.4183(5) 0.2265(2) 0.9815(3) 0.043(3) Uani ? ? C
C41 0.3552(4) 0.2731(2) 1.0044(3) 0.036(2) Uani ? ? C
C42 0.3897(4) 0.3288(2) 0.9882(3) 0.042(3) Uani ? ? C
C43 0.4869(4) 0.3381(2) 0.9473(3) 0.034(2) Uani ? ? C
C44 1.0178(4) 0.3379(2) 1.0128(2) 0.022(2) Uani ? ? C
O4 0.9774(3) 0.3969(1) 1.0152(2) 0.027(1) Uani ? ? O
C45 1.0716(4) 0.4343(2) 1.0511(2) 0.030(2) Uani ? ? C
C46 1.1517(4) 0.4544(2) 0.9965(3) 0.032(2) Uani ? ? C
C47 1.2076(4) 0.4722(2) 0.9477(3) 0.038(2) Uani ? ? C
SI 1.2737(1) 0.50578(6) 0.86985(8) 0.0446(7) Uani ? ? Si
C48 1.2886(5) 0.4483(2) 0.8004(3) 0.054(3) Uani ? ? C
C49 1.4197(6) 0.5412(3) 0.9056(4) 0.087(4) Uani ? ? C
C50 1.1613(7) 0.5622(3) 0.8306(4) 0.083(4) Uani ? ? C
H1 1.1006 0.1746 0.8256 0.0953 Uiso calc C5 H
H2 1.2605 0.1084 0.8192 0.1112 Uiso calc C6 H
H3 1.2604 0.0192 0.8799 0.0605 Uiso calc C7 H
H4 1.1074 -0.0019 0.9501 0.0678 Uiso calc C8 H
H5 0.9523 0.0658 0.9619 0.0635 Uiso calc C9 H
H6 0.8966 0.1932 1.0697 0.0497 Uiso calc C11 H
H7 0.7777 0.1519 1.1544 0.0605 Uiso calc C12 H
H8 0.6173 0.0889 1.1138 0.0535 Uiso calc C13 H
H9 0.5804 0.0621 0.9883 0.0519 Uiso calc C14 H
H10 0.7008 0.1008 0.9027 0.0438 Uiso calc C15 H
H11 1.0670 0.2423 0.9274 0.0269 Uiso calc C16 H
H12 1.0119 0.2320 1.0013 0.0269 Uiso calc C16 H
H13 1.0557 0.3453 0.8791 0.0272 Uiso calc C18 H
H14 0.9261 0.3743 0.8717 0.0272 Uiso calc C18 H
H15 0.9826 0.2371 0.6590 0.0371 Uiso calc C20 H
H16 1.1553 0.1965 0.6166 0.0503 Uiso calc C21 H
H17 1.3510 0.2075 0.6873 0.0517 Uiso calc C22 H
H18 1.3704 0.2620 0.7961 0.0567 Uiso calc C23 H
H19 1.1996 0.3041 0.8390 0.0429 Uiso calc C24 H
H20 0.8062 0.3124 0.6332 0.0412 Uiso calc C26 H
H21 0.7613 0.3877 0.5459 0.0536 Uiso calc C27 H
H22 0.8176 0.4831 0.5782 0.0587 Uiso calc C28 H
H23 0.9259 0.5038 0.6950 0.0596 Uiso calc C29 H
H24 0.9742 0.4292 0.7832 0.0436 Uiso calc C30 H
H25 0.7926 0.3470 0.9787 0.0260 Uiso calc C31 H
H26 0.7913 0.2800 0.9928 0.0260 Uiso calc C31 H
H27 0.5615 0.3441 0.7385 0.0393 Uiso calc C33 H
H28 0.5279 0.4344 0.6793 0.0497 Uiso calc C34 H
H29 0.6038 0.5198 0.7393 0.0523 Uiso calc C35 H
H30 0.7105 0.5148 0.8607 0.0510 Uiso calc C36 H
H31 0.7489 0.4246 0.9196 0.0388 Uiso calc C37 H
H32 0.5602 0.2022 0.9255 0.0488 Uiso calc C39 H
H33 0.3950 0.1879 0.9933 0.0555 Uiso calc C40 H
H34 0.2875 0.2670 1.0315 0.0488 Uiso calc C41 H
H35 0.3467 0.3613 1.0050 0.0549 Uiso calc C42 H
H36 0.5093 0.3769 0.9356 0.0444 Uiso calc C43 H
H37 1.1030 0.3372 1.0070 0.0295 Uiso calc C44 H
H38 1.0064 0.3187 1.0582 0.0295 Uiso calc C44 H
H39 1.1200 0.4135 1.0904 0.0406 Uiso calc C45 H
H40 1.0346 0.4673 1.0714 0.0406 Uiso calc C45 H
H41 1.3228 0.4645 0.7591 0.0696 Uiso calc C48 H
H42 1.3413 0.4182 0.8228 0.0696 Uiso calc C48 H
H43 1.2093 0.4324 0.7832 0.0696 Uiso calc C48 H
H44 1.4541 0.5586 0.8652 0.1097 Uiso calc C49 H
H45 1.4055 0.5705 0.9409 0.1097 Uiso calc C49 H
H46 1.4756 0.5129 0.9294 0.1097 Uiso calc C49 H
H47 1.1912 0.5812 0.7896 0.1070 Uiso calc C50 H
H48 1.0841 0.5442 0.8137 0.1070 Uiso calc C50 H
H49 1.1510 0.5902 0.8682 0.1070 Uiso calc C50 H

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
MO 0.0261(2) 0.0163(1) 0.0151(1) -0.0001(1) -0.0030(1) -0.0016(1) Mo
C1 0.048(2) 0.020(2) 0.024(2) -0.004(2) 0.004(2) -0.002(2) C
O1 0.091(3) 0.031(2) 0.050(2) -0.000(2) 0.027(2) -0.016(2) O
C2 0.037(2) 0.029(2) 0.033(2) -0.004(2) -0.008(2) -0.001(2) C
O2 0.046(2) 0.053(2) 0.064(2) -0.023(2) -0.011(2) 0.007(2) O
C3 0.039(2) 0.024(2) 0.024(2) 0.000(2) -0.002(2) -0.007(2) C
O3 0.060(2) 0.046(2) 0.031(2) 0.007(2) -0.024(2) -0.005(1) O
P1 0.0295(5) 0.0158(4) 0.0173(5) -0.0009(4) -0.0016(4) 0.0002(4) P
C4 0.038(2) 0.020(2) 0.021(2) 0.005(2) -0.000(2) -0.001(2) C
C5 0.112(4) 0.045(3) 0.077(3) 0.050(3) 0.066(3) 0.038(2) C
C6 0.120(4) 0.057(3) 0.097(4) 0.051(3) 0.081(3) 0.034(3) C
C7 0.068(3) 0.029(2) 0.042(3) 0.022(2) 0.007(3) 0.001(2) C
C8 0.057(3) 0.029(2) 0.071(3) 0.015(2) 0.010(3) 0.021(2) C
C9 0.051(3) 0.035(2) 0.063(3) 0.008(2) 0.017(2) 0.021(2) C
C10 0.031(2) 0.017(2) 0.024(2) 0.002(2) -0.000(2) 0.003(2) C
C11 0.057(3) 0.031(2) 0.028(2) -0.012(2) 0.008(2) 0.003(2) C
C12 0.081(3) 0.031(2) 0.030(2) -0.006(3) 0.018(2) 0.001(2) C
C13 0.051(3) 0.028(2) 0.048(3) 0.000(2) 0.022(2) 0.008(2) C
C14 0.037(2) 0.029(2) 0.054(3) -0.003(2) 0.006(2) 0.009(2) C
C15 0.042(2) 0.028(2) 0.030(2) -0.004(2) 0.002(2) 0.005(2) C
C16 0.026(2) 0.018(2) 0.017(2) -0.001(2) -0.002(2) 0.000(1) C
C17 0.022(2) 0.019(2) 0.014(2) -0.002(2) -0.002(1) -0.000(1) C
C18 0.025(2) 0.019(2) 0.018(2) 0.000(2) -0.000(2) -0.002(2) C
P2 0.0261(5) 0.0178(4) 0.0156(4) 0.0020(4) 0.0003(4) 0.0004(4) P
C19 0.026(2) 0.021(2) 0.021(2) 0.004(2) 0.002(2) 0.005(2) C
C20 0.030(2) 0.030(2) 0.027(2) 0.001(2) 0.005(2) -0.002(2) C
C21 0.047(3) 0.032(2) 0.039(2) 0.004(2) 0.014(2) -0.005(2) C
C22 0.035(2) 0.042(2) 0.044(3) 0.014(2) 0.011(2) 0.002(2) C
C23 0.030(2) 0.053(3) 0.046(3) 0.007(2) -0.001(2) 0.007(2) C
C24 0.032(2) 0.038(2) 0.027(2) 0.003(2) -0.002(2) -0.001(2) C
C25 0.030(2) 0.023(2) 0.022(2) 0.006(2) 0.009(2) 0.006(2) C
C26 0.042(2) 0.032(2) 0.021(2) 0.006(2) 0.004(2) 0.004(2) C
C27 0.058(3) 0.043(2) 0.024(2) 0.020(2) 0.007(2) 0.010(2) C
C28 0.064(3) 0.038(2) 0.035(2) 0.020(2) 0.015(2) 0.018(2) C
C29 0.067(3) 0.024(2) 0.049(3) 0.006(2) 0.014(3) 0.010(2) C
C30 0.046(2) 0.027(2) 0.027(2) 0.002(2) 0.008(2) 0.006(2) C
C31 0.021(2) 0.021(2) 0.016(2) -0.000(2) -0.002(2) 0.001(1) C
P3 0.0218(5) 0.0195(4) 0.0176(4) 0.0009(4) -0.0015(4) -0.0001(4) P
C32 0.023(2) 0.022(2) 0.023(2) 0.002(2) 0.003(2) 0.002(2) C
C33 0.037(2) 0.025(2) 0.027(2) 0.005(2) -0.000(2) -0.002(2) C
C34 0.043(2) 0.039(2) 0.031(2) 0.011(2) -0.001(2) 0.007(2) C
C35 0.050(3) 0.026(2) 0.045(3) 0.008(2) 0.006(2) 0.013(2) C
C36 0.042(3) 0.021(2) 0.051(3) -0.001(2) -0.005(2) -0.000(2) C
C37 0.032(2) 0.024(2) 0.030(2) 0.002(2) -0.004(2) -0.002(2) C
C38 0.018(2) 0.030(2) 0.019(2) 0.000(2) -0.003(2) 0.003(2) C
C39 0.045(2) 0.029(2) 0.041(2) 0.006(2) 0.016(2) 0.006(2) C
C40 0.047(3) 0.039(2) 0.045(3) -0.003(2) 0.016(2) 0.012(2) C
C41 0.024(2) 0.054(3) 0.037(2) 0.004(2) 0.010(2) 0.016(2) C
C42 0.034(2) 0.045(3) 0.050(3) 0.009(2) 0.013(2) -0.002(2) C
C43 0.032(2) 0.030(2) 0.041(2) -0.002(2) 0.007(2) -0.003(2) C
C44 0.024(2) 0.021(2) 0.021(2) 0.001(2) -0.003(2) -0.001(2) C
O4 0.031(1) 0.021(1) 0.030(1) 0.000(1) -0.005(1) -0.007(1) O
C45 0.040(2) 0.027(2) 0.026(2) -0.003(2) 0.002(2) -0.005(2) C
C46 0.039(2) 0.025(2) 0.034(2) 0.001(2) 0.002(2) -0.002(2) C
C47 0.043(3) 0.030(2) 0.042(3) 0.000(2) 0.004(2) 0.004(2) C
SI 0.0515(8) 0.0387(7) 0.0445(7) 0.0006(6) 0.0191(6) 0.0035(6) Si
C48 0.059(3) 0.055(3) 0.049(3) 0.004(3) 0.014(3) -0.008(3) C
C49 0.089(4) 0.086(4) 0.086(4) -0.046(3) 0.043(3) -0.031(4) C
C50 0.117(5) 0.075(4) 0.065(3) 0.045(3) 0.048(3) 0.031(3) C

# 10. MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
MO C1 1.973(4) . . ?
MO C2 1.963(5) . . ?
MO C3 1.947(4) . . ?
MO P1 2.540(1) . . ?
MO P2 2.552(1) . . ?
MO P3 2.534(1) . . ?
C1 O1 1.154(5) . . ?
C2 O2 1.166(5) . . ?
C3 O3 1.172(5) . . ?
P1 C4 1.850(4) . . ?
P1 C10 1.836(4) . . ?
P1 C16 1.849(4) . . ?
C4 C5 1.364(7) . . ?
C4 C9 1.369(6) . . ?
C5 C6 1.387(8) . . ?
C6 C7 1.356(7) . . ?
C7 C8 1.330(8) . . ?
C8 C9 1.389(7) . . ?
C10 C11 1.389(6) . . ?
C10 C15 1.392(6) . . ?
C11 C12 1.393(7) . . ?
C12 C13 1.359(7) . . ?
C13 C14 1.370(7) . . ?
C14 C15 1.389(6) . . ?
C16 C17 1.552(5) . . ?
C17 C18 1.554(5) . . ?
C17 C31 1.545(5) . . ?
C17 C44 1.537(5) . . ?
C18 P2 1.847(4) . . ?
P2 C19 1.844(4) . . ?
P2 C25 1.844(4) . . ?
C19 C20 1.392(6) . . ?
C19 C24 1.394(6) . . ?
C20 C21 1.382(6) . . ?
C21 C22 1.387(7) . . ?
C22 C23 1.361(7) . . ?
C23 C24 1.386(7) . . ?
C25 C26 1.394(6) . . ?
C25 C30 1.396(6) . . ?
C26 C27 1.391(6) . . ?
C27 C28 1.367(7) . . ?
C28 C29 1.371(7) . . ?
C29 C30 1.393(6) . . ?
C31 P3 1.845(4) . . ?
P3 C32 1.839(4) . . ?
P3 C38 1.839(4) . . ?
C32 C33 1.397(5) . . ?
C32 C37 1.394(6) . . ?
C33 C34 1.386(6) . . ?
C34 C35 1.374(7) . . ?
C35 C36 1.382(6) . . ?
C36 C37 1.386(6) . . ?
C38 C39 1.376(6) . . ?
C38 C43 1.391(6) . . ?
C39 C40 1.391(7) . . ?
C40 C41 1.361(7) . . ?
C41 C42 1.368(7) . . ?
C42 C43 1.388(7) . . ?
C44 O4 1.420(5) . . ?
O4 C45 1.423(5) . . ?
C45 C46 1.476(7) . . ?
C46 C47 1.205(6) . . ?
C47 SI 1.830(5) . . ?
SI C48 1.835(6) . . ?
SI C49 1.824(7) . . ?
SI C50 1.852(6) . . ?

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 MO C2 85.8(2) . . . ?
C1 MO C3 86.7(2) . . . ?
C1 MO P1 91.9(1) . . . ?
C1 MO P2 97.6(1) . . . ?
C1 MO P3 176.4(1) . . . ?
C2 MO C3 83.1(2) . . . ?
C2 MO P1 95.6(1) . . . ?
C2 MO P2 176.2(1) . . . ?
C2 MO P3 97.0(1) . . . ?
C3 MO P1 178.1(1) . . . ?
C3 MO P2 95.4(1) . . . ?
C3 MO P3 95.9(1) . . . ?
P1 MO P2 85.99(3) . . . ?
P1 MO P3 85.63(3) . . . ?
P2 MO P3 79.73(3) . . . ?
C4 P1 C10 101.3(2) . . . ?
C4 P1 C16 99.0(2) . . . ?
C10 P1 C16 106.3(2) . . . ?
P1 C4 C5 119.4(3) . . . ?
P1 C4 C9 123.9(4) . . . ?
C5 C4 C9 116.6(4) . . . ?
C4 C5 C6 121.7(5) . . . ?
C5 C6 C7 119.9(6) . . . ?
C6 C7 C8 119.6(5) . . . ?
C7 C8 C9 120.6(5) . . . ?
C4 C9 C8 121.5(5) . . . ?
P1 C10 C11 125.0(3) . . . ?
P1 C10 C15 117.5(3) . . . ?
C11 C10 C15 117.5(4) . . . ?
C10 C11 C12 120.5(4) . . . ?
C11 C12 C13 121.0(5) . . . ?
C12 C13 C14 119.5(5) . . . ?
C13 C14 C15 120.3(4) . . . ?
C10 C15 C14 121.1(4) . . . ?
P1 C16 C17 117.4(2) . . . ?
C16 C17 C18 111.7(3) . . . ?
C16 C17 C31 112.9(3) . . . ?
C16 C17 C44 105.2(3) . . . ?
C18 C17 C31 112.5(3) . . . ?
C18 C17 C44 106.7(3) . . . ?
C31 C17 C44 107.1(3) . . . ?
C17 C18 P2 117.9(3) . . . ?
C18 P2 C19 105.9(2) . . . ?
C18 P2 C25 102.3(2) . . . ?
C19 P2 C25 99.6(2) . . . ?
P2 C19 C20 116.6(3) . . . ?
P2 C19 C24 125.7(3) . . . ?
C20 C19 C24 117.6(4) . . . ?
C19 C20 C21 121.6(4) . . . ?
C20 C21 C22 120.0(4) . . . ?
C21 C22 C23 118.9(4) . . . ?
C22 C23 C24 121.9(4) . . . ?
C19 C24 C23 120.0(4) . . . ?
P2 C25 C26 118.1(3) . . . ?
P2 C25 C30 123.8(3) . . . ?
C26 C25 C30 118.1(4) . . . ?
C25 C26 C27 121.0(4) . . . ?
C26 C27 C28 119.8(4) . . . ?
C27 C28 C29 120.4(4) . . . ?
C28 C29 C30 120.5(5) . . . ?
C25 C30 C29 120.1(4) . . . ?
C17 C31 P3 117.8(3) . . . ?
C31 P3 C32 105.4(2) . . . ?
C31 P3 C38 98.3(2) . . . ?
C32 P3 C38 101.8(2) . . . ?
P3 C32 C33 117.2(3) . . . ?
P3 C32 C37 125.2(3) . . . ?
C33 C32 C37 117.7(4) . . . ?
C32 C33 C34 121.0(4) . . . ?
C33 C34 C35 120.5(4) . . . ?
C34 C35 C36 119.4(4) . . . ?
C35 C36 C37 120.4(4) . . . ?
C32 C37 C36 121.0(4) . . . ?
P3 C38 C39 119.2(3) . . . ?
P3 C38 C43 122.1(3) . . . ?
C39 C38 C43 118.6(4) . . . ?
C38 C39 C40 120.5(4) . . . ?
C39 C40 C41 120.5(4) . . . ?
C40 C41 C42 119.7(4) . . . ?
C41 C42 C43 120.6(4) . . . ?
C38 C43 C42 120.1(4) . . . ?
C17 C44 O4 109.8(3) . . . ?
C44 O4 C45 112.0(3) . . . ?
O4 C45 C46 110.0(4) . . . ?
C45 C46 C47 174.2(5) . . . ?
C46 C47 SI 172.0(4) . . . ?
C47 SI C48 107.6(2) . . . ?
C47 SI C49 109.4(3) . . . ?
C47 SI C50 105.9(3) . . . ?
C48 SI C49 113.8(3) . . . ?
C48 SI C50 110.7(3) . . . ?
C49 SI C50 109.1(4) . . . ?