Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_rm13

_database_code_CSD	162416

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Abboud, Khalil A.'
'Boncella, James M.'
'Mills, R. C.'

_publ_contact_author_name     	'Prof James M Boncella'  
_publ_contact_author_address 
;
Prof James M Boncella
Department of Chemistry and Center for Catalysis
University of Florida
Gainesville
FL 32611-7200
UNITED STATES OF AMERICA
;

_publ_contact_author_email       'BONCELLA@CHEM.UFL.EDU'

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C22 H31 N3 S Si2 W'
_chemical_formula_weight          609.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C'  'C'   0.0033   0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H'  'H'   0.0000   0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N'  'N'   0.0061   0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Si'  'Si'   0.0817   0.0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'S'  'S'   0.1246   0.1234
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'W'  'W'  -0.8490   6.8722
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1

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

_cell_length_a                    9.4647(4)
_cell_length_b                    11.7141(5)
_cell_length_c                    12.4830(5)
_cell_angle_alpha                 101.246(1)
_cell_angle_beta                  111.655(1)
_cell_angle_gamma                 93.904(1)
_cell_volume                      1246.64(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        blocks
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.624
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              604
_exptl_absorpt_coefficient_mu     4.826
_exptl_absorpt_correction_type    integration
_exptl_absorpt_correction_T_min   0.6137
_exptl_absorpt_correction_T_max   0.8395
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'normal-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'CCD area detector'
_diffrn_measurement_method        'omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             8979
_diffrn_reflns_av_R_equivalents   0.0326
_diffrn_reflns_av_sigmaI/netI     0.0423
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          1.79
_diffrn_reflns_theta_max          27.50
_reflns_number_total              5607
_reflns_number_gt                 5106
_reflns_threshold_expression      >2sigma(I)

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

_refine_special_details
;
Refinement of 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^)+(0.0361P)^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     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5607
_refine_ls_number_parameters      264
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0305
_refine_ls_R_factor_gt            0.0264
_refine_ls_wR_factor_ref          0.0663
_refine_ls_wR_factor_gt           0.0647
_refine_ls_goodness_of_fit_ref    1.024
_refine_ls_restrained_S_all       1.024
_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
W W 0.902740(16) 0.205566(11) 0.280094(12) 0.02218(5) Uani 1 1 d D . .
Si1 Si 0.73511(13) 0.39285(9) 0.10140(9) 0.0281(2) Uani 1 1 d . . .
Si2 Si 1.30132(12) 0.22875(9) 0.38315(10) 0.0283(2) Uani 1 1 d . . .
N1 N 0.8883(4) 0.2828(3) 0.4082(3) 0.0298(7) Uani 1 1 d . A .
N2 N 0.8589(4) 0.2887(3) 0.1468(3) 0.0262(6) Uani 1 1 d . A .
N3 N 1.1127(4) 0.2167(3) 0.2749(3) 0.0249(6) Uani 1 1 d . A .
C1 C 0.8502(4) 0.3122(3) 0.5072(3) 0.0245(7) Uani 1 1 d . . .
C2 C 0.7850(5) 0.2230(3) 0.5423(3) 0.0301(8) Uani 1 1 d . A .
H2A H 0.7716 0.1430 0.5017 0.036 Uiso 1 1 calc R . .
C3 C 0.7403(5) 0.2520(4) 0.6364(4) 0.0368(9) Uani 1 1 d . . .
H3A H 0.6945 0.1915 0.6595 0.044 Uiso 1 1 calc R A .
C4 C 0.7609(5) 0.3676(4) 0.6975(3) 0.0348(9) Uani 1 1 d . A .
H4A H 0.7283 0.3867 0.7614 0.042 Uiso 1 1 calc R . .
C5 C 0.8296(5) 0.4557(3) 0.6649(4) 0.0329(8) Uani 1 1 d . . .
H5A H 0.8469 0.5351 0.7082 0.040 Uiso 1 1 calc R A .
C6 C 0.8731(5) 0.4288(3) 0.5701(4) 0.0308(8) Uani 1 1 d . A .
H6A H 0.9187 0.4898 0.5476 0.037 Uiso 1 1 calc R . .
C7 C 0.9419(4) 0.2360(3) 0.0836(3) 0.0268(7) Uani 1 1 d . . .
C8 C 1.0795(4) 0.1969(3) 0.1536(3) 0.0258(7) Uani 1 1 d . A .
C9 C 1.1697(5) 0.1426(3) 0.0959(4) 0.0342(9) Uani 1 1 d . . .
H9A H 1.2600 0.1148 0.1403 0.041 Uiso 1 1 calc R A .
C10 C 1.1275(5) 0.1298(4) -0.0238(4) 0.0399(10) Uani 1 1 d . A .
H10A H 1.1898 0.0941 -0.0612 0.048 Uiso 1 1 calc R . .
C11 C 0.9942(6) 0.1686(4) -0.0916(4) 0.0409(10) Uani 1 1 d . . .
H11A H 0.9673 0.1595 -0.1743 0.049 Uiso 1 1 calc R A .
C12 C 0.9014(5) 0.2200(4) -0.0391(4) 0.0366(9) Uani 1 1 d . A .
H12A H 0.8099 0.2447 -0.0860 0.044 Uiso 1 1 calc R . .
C13 C 0.8311(5) 0.5027(4) 0.0510(4) 0.0395(10) Uani 1 1 d . A .
H13A H 0.9203 0.5499 0.1187 0.059 Uiso 1 1 calc R . .
H13B H 0.7585 0.5544 0.0171 0.059 Uiso 1 1 calc R . .
H13C H 0.8651 0.4617 -0.0094 0.059 Uiso 1 1 calc R . .
C14 C 0.5491(5) 0.3185(4) -0.0214(5) 0.0491(12) Uani 1 1 d . A .
H14A H 0.5693 0.2748 -0.0883 0.074 Uiso 1 1 calc R . .
H14B H 0.4844 0.3778 -0.0471 0.074 Uiso 1 1 calc R . .
H14C H 0.4959 0.2639 0.0067 0.074 Uiso 1 1 calc R . .
C15 C 0.7006(5) 0.4672(4) 0.2328(4) 0.0395(10) Uani 1 1 d . A .
H15A H 0.6608 0.4081 0.2645 0.059 Uiso 1 1 calc R . .
H15B H 0.6253 0.5206 0.2097 0.059 Uiso 1 1 calc R . .
H15C H 0.7973 0.5124 0.2937 0.059 Uiso 1 1 calc R . .
C16 C 1.4371(5) 0.3203(4) 0.3460(4) 0.0433(10) Uani 1 1 d . A .
H16A H 1.4626 0.2718 0.2842 0.065 Uiso 1 1 calc R . .
H16B H 1.5312 0.3515 0.4170 0.065 Uiso 1 1 calc R . .
H16C H 1.3889 0.3858 0.3171 0.065 Uiso 1 1 calc R . .
C17 C 1.3563(5) 0.0785(4) 0.3873(4) 0.0403(10) Uani 1 1 d . A .
H17A H 1.3215 0.0465 0.4418 0.060 Uiso 1 1 calc R . .
H17B H 1.4683 0.0840 0.4146 0.060 Uiso 1 1 calc R . .
H17C H 1.3077 0.0265 0.3075 0.060 Uiso 1 1 calc R . .
C18 C 1.2988(5) 0.3014(4) 0.5277(4) 0.0389(9) Uani 1 1 d . A .
H18A H 1.2831 0.3833 0.5283 0.058 Uiso 1 1 calc R . .
H18B H 1.3971 0.2997 0.5914 0.058 Uiso 1 1 calc R . .
H18C H 1.2149 0.2597 0.5401 0.058 Uiso 1 1 calc R . .
S1 S 0.6492(3) 0.1087(2) 0.1585(3) 0.0322(7) Uiso 0.546(5) 1 d PD A 1
C19 C 0.5977(15) -0.0102(10) 0.2057(11) 0.041(3) Uiso 0.546(5) 1 d P A 1
H19A H 0.4925 -0.0436 0.1631 0.049 Uiso 0.546(5) 1 calc PR A 1
C20 C 0.6641(14) -0.0602(10) 0.2796(10) 0.038(3) Uiso 0.546(5) 1 d P A 1
H20A H 0.6067 -0.1055 0.3094 0.046 Uiso 0.546(5) 1 calc PR A 1
C21 C 0.8472(12) -0.0532(8) 0.3300(8) 0.032(2) Uiso 0.546(5) 1 d P A 1
H21A H 0.8927 -0.1157 0.3611 0.038 Uiso 0.546(5) 1 calc PR A 1
C22 C 0.9340(13) 0.0360(8) 0.3289(9) 0.035(3) Uiso 0.546(5) 1 d PD A 1
H22A H 1.0390 0.0256 0.3566 0.043 Uiso 0.546(5) 1 calc PR A 1
S1' S 0.9715(4) 0.0299(2) 0.3392(3) 0.0282(8) Uiso 0.454(5) 1 d PD A 2
C19' C 0.8132(14) -0.0582(10) 0.3371(11) 0.034(3) Uiso 0.454(5) 1 d P A 2
H19B H 0.8351 -0.0981 0.3994 0.041 Uiso 0.454(5) 1 calc PR A 2
C20' C 0.6891(16) -0.0750(12) 0.2731(12) 0.037(4) Uiso 0.454(5) 1 d P A 2
H20B H 0.6317 -0.1480 0.2653 0.044 Uiso 0.454(5) 1 calc PR A 2
C21' C 0.5963(17) 0.0103(12) 0.1924(12) 0.037(3) Uiso 0.454(5) 1 d P A 2
H21B H 0.4877 -0.0081 0.1520 0.044 Uiso 0.454(5) 1 calc PR A 2
C22' C 0.6705(13) 0.1052(13) 0.1824(14) 0.050(5) Uiso 0.454(5) 1 d PD A 2
H22B H 0.6096 0.1367 0.1190 0.060 Uiso 0.454(5) 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
W 0.02419(8) 0.02175(8) 0.02226(8) 0.00593(5) 0.01007(6) 0.00649(5)
Si1 0.0295(5) 0.0283(5) 0.0293(5) 0.0107(4) 0.0115(4) 0.0114(4)
Si2 0.0255(5) 0.0288(5) 0.0317(5) 0.0113(4) 0.0096(4) 0.0081(4)
N1 0.0335(18) 0.0282(15) 0.0317(17) 0.0096(13) 0.0156(14) 0.0075(13)
N2 0.0294(16) 0.0281(15) 0.0235(15) 0.0086(12) 0.0109(13) 0.0095(13)
N3 0.0261(15) 0.0262(14) 0.0262(15) 0.0099(12) 0.0115(13) 0.0098(12)
C1 0.0241(17) 0.0261(16) 0.0230(17) 0.0053(14) 0.0088(14) 0.0050(14)
C2 0.039(2) 0.0248(17) 0.0276(19) 0.0065(14) 0.0133(17) 0.0070(16)
C3 0.048(3) 0.035(2) 0.036(2) 0.0158(17) 0.022(2) 0.0063(19)
C4 0.043(2) 0.040(2) 0.0254(19) 0.0074(16) 0.0178(18) 0.0110(18)
C5 0.039(2) 0.0247(17) 0.032(2) 0.0007(15) 0.0134(18) 0.0053(16)
C6 0.032(2) 0.0259(17) 0.036(2) 0.0070(15) 0.0159(17) 0.0023(16)
C7 0.0315(19) 0.0249(16) 0.0271(18) 0.0081(14) 0.0131(16) 0.0089(15)
C8 0.0286(19) 0.0247(16) 0.0262(18) 0.0075(14) 0.0123(15) 0.0052(14)
C9 0.035(2) 0.035(2) 0.041(2) 0.0123(17) 0.0201(18) 0.0183(17)
C10 0.049(3) 0.043(2) 0.039(2) 0.0118(19) 0.027(2) 0.020(2)
C11 0.054(3) 0.043(2) 0.031(2) 0.0080(18) 0.020(2) 0.018(2)
C12 0.043(2) 0.039(2) 0.031(2) 0.0103(17) 0.0138(18) 0.0182(19)
C13 0.045(3) 0.042(2) 0.041(2) 0.0202(19) 0.021(2) 0.014(2)
C14 0.035(2) 0.042(2) 0.055(3) 0.014(2) -0.002(2) 0.010(2)
C15 0.044(2) 0.045(2) 0.041(2) 0.0157(19) 0.025(2) 0.020(2)
C16 0.027(2) 0.049(2) 0.057(3) 0.021(2) 0.017(2) 0.0050(19)
C17 0.037(2) 0.033(2) 0.053(3) 0.0160(19) 0.015(2) 0.0162(18)
C18 0.039(2) 0.042(2) 0.032(2) 0.0086(18) 0.0094(18) 0.0094(19)

_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
W N1 1.734(3) . ?
W N3 2.008(3) . ?
W N2 2.016(3) . ?
W C22' 2.194(10) . ?
W C22 2.196(9) . ?
W S1 2.371(3) . ?
W S1' 2.371(3) . ?
Si1 N2 1.777(3) . ?
Si1 C15 1.853(4) . ?
Si1 C13 1.859(4) . ?
Si1 C14 1.868(5) . ?
Si2 N3 1.773(3) . ?
Si2 C18 1.849(4) . ?
Si2 C16 1.861(4) . ?
Si2 C17 1.873(4) . ?
N1 C1 1.399(4) . ?
N2 C7 1.398(4) . ?
N3 C8 1.396(5) . ?
C1 C6 1.394(5) . ?
C1 C2 1.398(5) . ?
C2 C3 1.380(5) . ?
C3 C4 1.380(6) . ?
C4 C5 1.385(6) . ?
C5 C6 1.379(5) . ?
C7 C12 1.404(5) . ?
C7 C8 1.437(5) . ?
C8 C9 1.415(5) . ?
C9 C10 1.370(6) . ?
C10 C11 1.398(6) . ?
C11 C12 1.381(6) . ?
S1 C19 1.722(12) . ?
C19 C20 1.192(16) . ?
C20 C21 1.600(16) . ?
C21 C22 1.289(14) . ?
S1' C19' 1.750(13) . ?
C19' C20' 1.127(18) . ?
C20' C21' 1.63(2) . ?
C21' C22' 1.325(19) . ?

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
N1 W N3 117.02(14) . . ?
N1 W N2 116.06(13) . . ?
N3 W N2 82.25(12) . . ?
N1 W C22' 101.7(5) . . ?
N3 W C22' 140.7(4) . . ?
N2 W C22' 87.1(5) . . ?
N1 W C22 98.0(3) . . ?
N3 W C22 89.0(3) . . ?
N2 W C22 145.1(3) . . ?
C22' W C22 78.5(5) . . ?
N1 W S1 104.49(13) . . ?
N3 W S1 138.47(11) . . ?
N2 W S1 80.88(11) . . ?
C22' W S1 6.2(5) . . ?
C22 W S1 83.7(3) . . ?
N1 W S1' 99.32(12) . . ?
N3 W S1' 81.79(11) . . ?
N2 W S1' 144.62(11) . . ?
C22' W S1' 85.5(4) . . ?
C22 W S1' 7.6(3) . . ?
S1 W S1' 90.62(10) . . ?
N2 Si1 C15 106.94(17) . . ?
N2 Si1 C13 109.44(18) . . ?
C15 Si1 C13 109.7(2) . . ?
N2 Si1 C14 110.92(18) . . ?
C15 Si1 C14 110.2(2) . . ?
C13 Si1 C14 109.6(2) . . ?
N3 Si2 C18 107.06(18) . . ?
N3 Si2 C16 108.95(18) . . ?
C18 Si2 C16 110.2(2) . . ?
N3 Si2 C17 109.84(18) . . ?
C18 Si2 C17 110.0(2) . . ?
C16 Si2 C17 110.7(2) . . ?
C1 N1 W 162.4(3) . . ?
C7 N2 Si1 124.2(2) . . ?
C7 N2 W 102.9(2) . . ?
Si1 N2 W 132.66(17) . . ?
C8 N3 Si2 123.1(2) . . ?
C8 N3 W 102.7(2) . . ?
Si2 N3 W 133.78(17) . . ?
C6 C1 C2 119.4(3) . . ?
C6 C1 N1 121.3(3) . . ?
C2 C1 N1 119.3(3) . . ?
C3 C2 C1 119.6(3) . . ?
C4 C3 C2 121.0(4) . . ?
C3 C4 C5 119.5(4) . . ?
C6 C5 C4 120.4(3) . . ?
C5 C6 C1 120.1(3) . . ?
N2 C7 C12 125.3(3) . . ?
N2 C7 C8 115.2(3) . . ?
C12 C7 C8 119.4(3) . . ?
N3 C8 C9 125.4(3) . . ?
N3 C8 C7 116.1(3) . . ?
C9 C8 C7 118.6(3) . . ?
C10 C9 C8 120.3(4) . . ?
C9 C10 C11 121.0(4) . . ?
C12 C11 C10 120.5(4) . . ?
C11 C12 C7 120.2(4) . . ?
C19 S1 W 112.4(5) . . ?
C20 C19 S1 134.5(11) . . ?
C19 C20 C21 121.9(11) . . ?
C22 C21 C20 121.0(9) . . ?
C21 C22 W 136.8(9) . . ?
C19' S1' W 111.4(4) . . ?
C20' C19' S1' 129.9(12) . . ?
C19' C20' C21' 128.1(13) . . ?
C22' C21' C20' 120.8(13) . . ?
C21' C22' W 134.1(12) . . ?

_diffrn_measured_fraction_theta_max    0.978
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.978
_refine_diff_density_max    1.568
_refine_diff_density_min   -1.022
_refine_diff_density_rms    0.116