# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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data_h11kcm23
_database_code_depnum_ccdc_archive 'CCDC 921374'
#TrackingRef 'web_deposit_cif_file_0_ManchalChaudhary_1358921721.h11kcm23 CIF-corr.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H72 O4 Si8'
_chemical_formula_sum            'C44 H72 O4 Si8'
_chemical_formula_weight         889.74
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'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
_cell_length_a                   19.8932(7)
_cell_length_b                   19.8932(7)
_cell_length_c                   6.6091(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2615.48(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    65182
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      25.028
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9532
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(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  'Nonius Kappa CCD'
_diffrn_measurement_method       '448 1.6 degree images with \f and \w scans'
_diffrn_standards_number         0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27924
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         4.10
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2300
_reflns_number_gt                2052
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
;
DENZO-SCALEPACK Z. Otwinowski and W. Minor, "
Processing of X-ray Diffraction Data Collected in Oscillation Mode ",
Methods in Enzymology, Volume 276: Macromolecular Crystallography,
part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_structure_solution    
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119
;
_computing_structure_refinement  
;
SHELXL97 -Program for Crystal Structure Analysis (Release 97-2).
Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at,
Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material  
;
'WinGX publication routines, Farrugia,
L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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^)+(0.1061P)^2^+1.2699P] 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   0.5(2)
_refine_ls_number_reflns         2300
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1505
_refine_ls_wR_factor_gt          0.1435
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_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
Si1 Si 0.46975(5) 0.39734(4) 0.06364(18) 0.0488(3) Uani 1 1 d . . .
Si2 Si 0.44998(5) 0.17911(5) -0.13822(16) 0.0457(3) Uani 1 1 d . . .
O O 0.54163(12) 0.41690(12) -0.0314(6) 0.0678(9) Uani 1 1 d . . .
C1 C 0.4797(3) 0.3825(3) 0.3374(9) 0.0831(15) Uani 1 1 d . . .
H1A H 0.5151 0.3490 0.3596 0.125 Uiso 1 1 calc R . .
H1B H 0.4373 0.3658 0.3935 0.125 Uiso 1 1 calc R . .
H1C H 0.4920 0.4246 0.4044 0.125 Uiso 1 1 calc R . .
C2 C 0.43919(17) 0.32141(17) -0.0647(6) 0.0449(8) Uani 1 1 d . . .
H2A H 0.3916 0.3141 -0.0274 0.054 Uiso 1 1 calc R . .
H2B H 0.4411 0.3287 -0.2128 0.054 Uiso 1 1 calc R . .
C3 C 0.47989(18) 0.25765(17) -0.0117(5) 0.0441(8) Uani 1 1 d . . .
H3A H 0.4782 0.2509 0.1366 0.053 Uiso 1 1 calc R . .
H3B H 0.5274 0.2652 -0.0494 0.053 Uiso 1 1 calc R . .
C4 C 0.4975(2) 0.1062(2) -0.0276(9) 0.0718(14) Uani 1 1 d . . .
H4A H 0.4820 0.0644 -0.0904 0.108 Uiso 1 1 calc R . .
H4B H 0.4895 0.1043 0.1186 0.108 Uiso 1 1 calc R . .
H4C H 0.5456 0.1120 -0.0534 0.108 Uiso 1 1 calc R . .
C5 C 0.4649(3) 0.1867(2) -0.4163(6) 0.0671(11) Uani 1 1 d . . .
H5A H 0.4538 0.1440 -0.4824 0.101 Uiso 1 1 calc R . .
H5B H 0.5123 0.1975 -0.4408 0.101 Uiso 1 1 calc R . .
H5C H 0.4365 0.2224 -0.4716 0.101 Uiso 1 1 calc R . .
C6 C 0.35776(19) 0.16854(17) -0.0848(6) 0.0474(8) Uani 1 1 d . . .
C7 C 0.3096(2) 0.1771(3) -0.2291(9) 0.0731(13) Uani 1 1 d . . .
H7 H 0.3226 0.1880 -0.3634 0.088 Uiso 1 1 calc R . .
C8 C 0.2417(3) 0.1702(4) -0.1840(11) 0.0960(19) Uani 1 1 d . . .
H8 H 0.2091 0.1761 -0.2875 0.115 Uiso 1 1 calc R . .
C9 C 0.2212(3) 0.1545(3) 0.0113(11) 0.0859(17) Uani 1 1 d . . .
H9 H 0.1747 0.1501 0.0423 0.103 Uiso 1 1 calc R . .
C10 C 0.2676(3) 0.1458(3) 0.1546(12) 0.0915(17) Uani 1 1 d . . .
H10 H 0.2543 0.1351 0.2888 0.110 Uiso 1 1 calc R . .
C11 C 0.3364(2) 0.1526(3) 0.1077(8) 0.0712(12) Uani 1 1 d . . .
H11 H 0.3688 0.1460 0.2114 0.085 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
Si1 0.0322(5) 0.0281(5) 0.0861(8) 0.0012(4) -0.0005(5) -0.0002(4)
Si2 0.0433(5) 0.0367(5) 0.0569(5) -0.0046(4) 0.0009(4) -0.0011(4)
O 0.0327(13) 0.0347(13) 0.136(3) -0.0008(15) 0.0113(16) -0.0049(10)
C1 0.099(4) 0.067(3) 0.084(3) -0.021(3) -0.015(3) 0.000(3)
C2 0.0402(17) 0.0381(18) 0.0562(19) 0.0044(15) -0.0096(16) -0.0016(14)
C3 0.0386(17) 0.0345(17) 0.059(2) -0.0008(15) -0.0028(15) 0.0000(14)
C4 0.056(2) 0.046(2) 0.114(4) -0.016(2) -0.009(2) 0.0123(19)
C5 0.073(3) 0.069(3) 0.059(2) -0.010(2) 0.009(2) -0.019(2)
C6 0.0488(19) 0.0321(16) 0.061(2) -0.0034(15) 0.0002(17) -0.0034(14)
C7 0.052(2) 0.086(3) 0.082(3) 0.008(3) -0.009(2) 0.009(2)
C8 0.053(3) 0.121(5) 0.114(5) 0.001(4) -0.018(3) 0.012(3)
C9 0.044(3) 0.079(3) 0.135(5) -0.022(3) 0.015(3) -0.009(2)
C10 0.078(4) 0.088(4) 0.109(4) 0.001(3) 0.031(4) -0.019(3)
C11 0.066(3) 0.082(3) 0.066(3) 0.000(2) 0.005(2) -0.004(2)
_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
Si1 O 1.610(3) . ?
Si1 O 1.620(2) 2_565 ?
Si1 C2 1.836(4) . ?
Si1 C1 1.844(6) . ?
Si2 C5 1.868(4) . ?
Si2 C3 1.869(3) . ?
Si2 C4 1.878(5) . ?
Si2 C6 1.880(4) . ?
O Si1 1.620(2) 4_655 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.545(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.363(6) . ?
C6 C11 1.379(6) . ?
C7 C8 1.389(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.389(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.335(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.409(7) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
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
O Si1 O 110.14(18) . 2_565 ?
O Si1 C2 108.22(17) . . ?
O Si1 C2 109.93(16) 2_565 . ?
O Si1 C1 109.1(2) . . ?
O Si1 C1 108.6(2) 2_565 . ?
C2 Si1 C1 110.9(2) . . ?
C5 Si2 C3 108.80(18) . . ?
C5 Si2 C4 111.4(2) . . ?
C3 Si2 C4 108.12(19) . . ?
C5 Si2 C6 110.4(2) . . ?
C3 Si2 C6 108.67(16) . . ?
C4 Si2 C6 109.4(2) . . ?
Si1 O Si1 150.9(2) . 4_655 ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 Si1 113.4(2) . . ?
C3 C2 H2A 108.9 . . ?
Si1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
Si1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C2 C3 Si2 114.7(2) . . ?
C2 C3 H3A 108.6 . . ?
Si2 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
Si2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 117.2(4) . . ?
C7 C6 Si2 122.8(3) . . ?
C11 C6 Si2 120.0(3) . . ?
C6 C7 C8 121.4(5) . . ?
C6 C7 H7 119.3 . . ?
C8 C7 H7 119.3 . . ?
C7 C8 C9 120.5(6) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 119.0(5) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 120.3(6) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C6 C11 C10 121.6(5) . . ?
C6 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.065