# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_publication_text
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#TrackingRef '- 08147.cif'

_publ_contact_author_name        'Kim M. Baines'
_publ_contact_author_address     
;1151 Richmond St.
Department of Chemistry
University of Western Ontario
London, Ontario, Canada
N6A 5B7
;
_publ_contact_author_email       kbaines2@uwo.ca
_publ_contact_author_phone       1-519-661-2166
_publ_contact_author_fax         1-519-661-3022
loop_
_publ_author_name
_publ_author_address
J.Hardwick
;1151 Richmond St.
Department of Chemistry
University of Western Ontario
London, Ontario, Canada
N6A 5B7
;
L.Pavelka
;1151 Richmond St.
Department of Chemistry
University of Western Ontario
London, Ontario, Canada
N6A 5B7
;
K.Baines ''

data_08147
_database_code_depnum_ccdc_archive 'CCDC 778245'
#TrackingRef '- 08147.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H41 N O2 Si4'
_chemical_melting_point          ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless

_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         391.86

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'
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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_int_tables_number      61
_chemical_absolute_configuration ?

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

_cell_length_a                   9.77160(10)
_cell_length_b                   19.9934(3)
_cell_length_c                   25.5683(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4995.22(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    67810
_cell_measurement_theta_min      2.04
_cell_measurement_theta_max      27.48
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1728
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8870
_exptl_absorpt_correction_T_max  0.9758
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'

_exptl_special_details           
;
?
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10797
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5720
_reflns_number_gt                3407
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC

_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^)+(0.0690P)^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         5720
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1146
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
C1 C -0.0779(2) 0.17862(11) 0.38801(9) 0.0273(5) Uani 1 1 d . . .
H1 H -0.1467 0.1909 0.3607 0.033 Uiso 1 1 calc R . .
Si2 Si 0.03138(6) 0.10738(3) 0.35949(2) 0.02553(16) Uani 1 1 d . . .
N3 N 0.08542(16) 0.14027(8) 0.29761(7) 0.0268(4) Uani 1 1 d . . .
H3 H 0.1733 0.1477 0.2930 0.032 Uiso 1 1 calc R . .
C4 C -0.0002(2) 0.15430(10) 0.25770(8) 0.0276(5) Uani 1 1 d . . .
O5 O -0.12490(14) 0.14350(8) 0.26127(6) 0.0341(4) Uani 1 1 d . . .
C6 C 0.0593(2) 0.18528(12) 0.20931(9) 0.0368(6) Uani 1 1 d . . .
H6A H 0.0253 0.1615 0.1784 0.055 Uiso 1 1 calc R . .
H6B H 0.1593 0.1822 0.2105 0.055 Uiso 1 1 calc R . .
H6C H 0.0320 0.2324 0.2074 0.055 Uiso 1 1 calc R . .
O7 O 0.01522(14) 0.23464(7) 0.39259(6) 0.0322(4) Uani 1 1 d . . .
Si8 Si 0.01464(7) 0.30766(3) 0.36296(3) 0.0396(2) Uani 1 1 d . . .
C9 C 0.1790(3) 0.31844(14) 0.32765(12) 0.0617(8) Uani 1 1 d . . .
H9A H 0.2551 0.3152 0.3525 0.093 Uiso 1 1 calc R . .
H9B H 0.1807 0.3624 0.3107 0.093 Uiso 1 1 calc R . .
H9C H 0.1881 0.2834 0.3010 0.093 Uiso 1 1 calc R . .
C10 C 0.0032(3) 0.37366(13) 0.41408(12) 0.0627(8) Uani 1 1 d . . .
H10A H -0.0869 0.3717 0.4309 0.094 Uiso 1 1 calc R . .
H10B H 0.0157 0.4177 0.3979 0.094 Uiso 1 1 calc R . .
H10C H 0.0747 0.3664 0.4404 0.094 Uiso 1 1 calc R . .
C11 C -0.1305(3) 0.31432(13) 0.31640(10) 0.0502(7) Uani 1 1 d . . .
H11A H -0.1265 0.2772 0.2914 0.075 Uiso 1 1 calc R . .
H11B H -0.1246 0.3569 0.2975 0.075 Uiso 1 1 calc R . .
H11C H -0.2170 0.3124 0.3357 0.075 Uiso 1 1 calc R . .
C12 C -0.1571(2) 0.17022(11) 0.43993(9) 0.0328(5) Uani 1 1 d . . .
C13 C -0.2538(2) 0.11046(12) 0.43484(11) 0.0485(7) Uani 1 1 d . . .
H13A H -0.2001 0.0692 0.4319 0.073 Uiso 1 1 calc R . .
H13B H -0.3106 0.1159 0.4035 0.073 Uiso 1 1 calc R . .
H13C H -0.3126 0.1080 0.4658 0.073 Uiso 1 1 calc R . .
C14 C -0.0608(3) 0.15913(15) 0.48540(10) 0.0564(8) Uani 1 1 d . . .
H14A H -0.1133 0.1575 0.5180 0.085 Uiso 1 1 calc R . .
H14B H 0.0054 0.1959 0.4870 0.085 Uiso 1 1 calc R . .
H14C H -0.0120 0.1167 0.4806 0.085 Uiso 1 1 calc R . .
C15 C -0.2447(2) 0.23210(12) 0.45006(11) 0.0502(7) Uani 1 1 d . . .
H15A H -0.3074 0.2389 0.4206 0.075 Uiso 1 1 calc R . .
H15B H -0.1854 0.2713 0.4538 0.075 Uiso 1 1 calc R . .
H15C H -0.2975 0.2258 0.4823 0.075 Uiso 1 1 calc R . .
Si16 Si -0.07233(7) 0.00306(3) 0.34079(3) 0.03211(18) Uani 1 1 d . . .
C17 C 0.0152(3) -0.03256(13) 0.28215(10) 0.0510(7) Uani 1 1 d . . .
H17A H 0.1138 -0.0355 0.2888 0.077 Uiso 1 1 calc R . .
H17B H -0.0011 -0.0035 0.2519 0.077 Uiso 1 1 calc R . .
H17C H -0.0211 -0.0773 0.2749 0.077 Uiso 1 1 calc R . .
C18 C -0.2584(3) 0.00629(13) 0.32555(12) 0.0535(8) Uani 1 1 d . . .
H18A H -0.2769 0.0444 0.3025 0.080 Uiso 1 1 calc R . .
H18B H -0.3105 0.0113 0.3581 0.080 Uiso 1 1 calc R . .
H18C H -0.2858 -0.0352 0.3080 0.080 Uiso 1 1 calc R . .
C19 C -0.0436(3) -0.05738(14) 0.39573(11) 0.0545(7) Uani 1 1 d . . .
H19A H -0.0868 -0.1003 0.3872 0.082 Uiso 1 1 calc R . .
H19B H -0.0838 -0.0394 0.4279 0.082 Uiso 1 1 calc R . .
H19C H 0.0549 -0.0640 0.4008 0.082 Uiso 1 1 calc R . .
Si20 Si 0.24462(6) 0.09121(3) 0.40104(3) 0.03438(19) Uani 1 1 d . . .
C21 C 0.3304(2) 0.17314(13) 0.41409(11) 0.0524(7) Uani 1 1 d . . .
H21A H 0.4218 0.1652 0.4285 0.079 Uiso 1 1 calc R . .
H21B H 0.2759 0.1989 0.4392 0.079 Uiso 1 1 calc R . .
H21C H 0.3383 0.1983 0.3814 0.079 Uiso 1 1 calc R . .
C22 C 0.3480(2) 0.04146(12) 0.35357(10) 0.0436(7) Uani 1 1 d . . .
H22A H 0.3469 0.0636 0.3194 0.065 Uiso 1 1 calc R . .
H22B H 0.3089 -0.0035 0.3503 0.065 Uiso 1 1 calc R . .
H22C H 0.4425 0.0381 0.3661 0.065 Uiso 1 1 calc R . .
C23 C 0.2402(3) 0.04312(16) 0.46417(10) 0.0645(9) Uani 1 1 d . . .
H23A H 0.1830 0.0032 0.4599 0.097 Uiso 1 1 calc R . .
H23B H 0.2019 0.0714 0.4918 0.097 Uiso 1 1 calc R . .
H23C H 0.3333 0.0296 0.4737 0.097 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
C1 0.0287(11) 0.0287(12) 0.0246(13) 0.0008(10) -0.0001(9) -0.0014(9)
Si2 0.0257(3) 0.0287(3) 0.0222(4) 0.0020(3) 0.0003(2) 0.0005(3)
N3 0.0218(8) 0.0348(10) 0.0240(10) 0.0018(8) -0.0010(8) -0.0026(8)
C4 0.0295(12) 0.0304(12) 0.0229(13) -0.0033(10) 0.0002(10) 0.0015(10)
O5 0.0242(8) 0.0473(9) 0.0307(10) 0.0003(7) -0.0015(7) -0.0011(7)
C6 0.0347(13) 0.0484(15) 0.0273(14) 0.0086(12) -0.0004(10) -0.0005(11)
O7 0.0345(8) 0.0270(8) 0.0350(10) -0.0008(7) -0.0011(7) -0.0060(7)
Si8 0.0510(4) 0.0284(4) 0.0394(4) 0.0008(3) 0.0014(3) -0.0071(3)
C9 0.0663(19) 0.0502(17) 0.069(2) 0.0102(16) 0.0104(16) -0.0164(15)
C10 0.098(2) 0.0354(16) 0.055(2) -0.0057(14) 0.0022(18) -0.0133(16)
C11 0.0678(18) 0.0346(14) 0.0483(18) 0.0092(13) -0.0048(15) 0.0022(13)
C12 0.0357(13) 0.0344(13) 0.0284(13) -0.0018(11) 0.0048(10) 0.0025(11)
C13 0.0520(15) 0.0477(15) 0.0457(18) -0.0018(13) 0.0218(13) -0.0067(13)
C14 0.0551(17) 0.086(2) 0.0287(16) 0.0054(15) 0.0048(13) 0.0080(15)
C15 0.0585(17) 0.0457(15) 0.0463(17) -0.0047(14) 0.0164(14) 0.0093(13)
Si16 0.0403(4) 0.0275(3) 0.0285(4) 0.0000(3) 0.0025(3) -0.0008(3)
C17 0.0687(17) 0.0427(15) 0.0416(17) -0.0073(13) 0.0066(14) 0.0044(14)
C18 0.0490(16) 0.0422(15) 0.069(2) -0.0058(14) -0.0053(14) -0.0124(12)
C19 0.078(2) 0.0405(15) 0.0453(18) 0.0092(13) 0.0010(15) -0.0015(15)
Si20 0.0284(3) 0.0479(4) 0.0268(4) 0.0051(3) -0.0010(3) 0.0046(3)
C21 0.0346(14) 0.0707(19) 0.0518(18) -0.0164(15) -0.0035(12) 0.0004(13)
C22 0.0359(13) 0.0416(15) 0.0534(18) 0.0079(13) 0.0026(12) 0.0101(12)
C23 0.0488(16) 0.106(2) 0.0385(18) 0.0254(17) -0.0027(13) 0.0125(16)

_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
C1 O7 1.448(2) . ?
C1 C12 1.546(3) . ?
C1 Si2 1.924(2) . ?
Si2 N3 1.7928(18) . ?
Si2 Si20 2.3612(8) . ?
Si2 Si16 2.3678(9) . ?
N3 C4 1.349(3) . ?
C4 O5 1.241(2) . ?
C4 C6 1.501(3) . ?
O7 Si8 1.6449(16) . ?
Si8 C9 1.855(3) . ?
Si8 C11 1.856(3) . ?
Si8 C10 1.861(3) . ?
C12 C14 1.512(3) . ?
C12 C15 1.526(3) . ?
C12 C13 1.528(3) . ?
Si16 C18 1.861(3) . ?
Si16 C17 1.867(3) . ?
Si16 C19 1.874(3) . ?
Si20 C22 1.866(2) . ?
Si20 C21 1.870(3) . ?
Si20 C23 1.879(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 C1 C12 109.22(17) . . ?
O7 C1 Si2 104.76(13) . . ?
C12 C1 Si2 121.54(15) . . ?
N3 Si2 C1 103.08(9) . . ?
N3 Si2 Si20 100.80(6) . . ?
C1 Si2 Si20 114.87(7) . . ?
N3 Si2 Si16 105.72(6) . . ?
C1 Si2 Si16 119.43(7) . . ?
Si20 Si2 Si16 110.36(3) . . ?
C4 N3 Si2 124.14(14) . . ?
O5 C4 N3 121.1(2) . . ?
O5 C4 C6 120.84(19) . . ?
N3 C4 C6 118.00(18) . . ?
C1 O7 Si8 130.33(14) . . ?
O7 Si8 C9 108.92(11) . . ?
O7 Si8 C11 111.20(10) . . ?
C9 Si8 C11 109.94(13) . . ?
O7 Si8 C10 107.82(11) . . ?
C9 Si8 C10 108.16(13) . . ?
C11 Si8 C10 110.71(13) . . ?
C14 C12 C15 109.7(2) . . ?
C14 C12 C13 109.6(2) . . ?
C15 C12 C13 107.6(2) . . ?
C14 C12 C1 111.36(19) . . ?
C15 C12 C1 109.79(19) . . ?
C13 C12 C1 108.74(19) . . ?
C18 Si16 C17 107.03(13) . . ?
C18 Si16 C19 109.02(13) . . ?
C17 Si16 C19 106.70(12) . . ?
C18 Si16 Si2 115.46(9) . . ?
C17 Si16 Si2 107.58(9) . . ?
C19 Si16 Si2 110.63(9) . . ?
C22 Si20 C21 109.90(12) . . ?
C22 Si20 C23 107.37(12) . . ?
C21 Si20 C23 107.77(14) . . ?
C22 Si20 Si2 104.95(8) . . ?
C21 Si20 Si2 110.84(9) . . ?
C23 Si20 Si2 115.86(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.065