 
data_2008src1017
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C10 H22 N2 O2 Si2'
_chemical_formula_weight          258.48
 
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            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    10.6069(12)
_cell_length_b                    10.7107(13)
_cell_length_c                    10.7782(15)
_cell_angle_alpha                 83.058(7)
_cell_angle_beta                  64.192(6)
_cell_angle_gamma                 88.751(9)
_cell_volume                      1093.6(2)
_cell_formula_units_Z             3
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     48165
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        fragment
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.177
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              420
_exptl_absorpt_coefficient_mu     0.234
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9680
_exptl_absorpt_correction_T_max   0.9953
_exptl_absorpt_process_details    'SADABS 2007/2 (Sheldrick, G.M., 2007)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             15672
_diffrn_reflns_av_R_equivalents   0.1521
_diffrn_reflns_av_sigmaI/netI     0.1966
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.92
_diffrn_reflns_theta_max          27.48
_reflns_number_total              4889
_reflns_number_gt                 2657
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0000P)²+8.6698P] where P=(Fo²+2Fc²)/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          4889
_refine_ls_number_parameters      226
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2538
_refine_ls_R_factor_gt            0.1451
_refine_ls_wR_factor_ref          0.2719
_refine_ls_wR_factor_gt           0.2243
_refine_ls_goodness_of_fit_ref    1.176
_refine_ls_restrained_S_all       1.176
_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 0.1623(2) 0.3279(2) 0.3377(2) 0.0266(5) Uani 1 1 d . . .
Si2 Si 0.1592(2) 0.7702(2) 0.9444(2) 0.0279(5) Uani 1 1 d . . .
Si3 Si 0.4588(2) 0.8287(2) 0.3186(2) 0.0264(5) Uani 1 1 d . . .
O5 O 0.3528(6) 0.6215(5) 0.5466(5) 0.0318(13) Uani 1 1 d . . .
O22 O -0.1336(6) 0.7024(5) 1.1118(6) 0.0345(14) Uani 1 1 d . . .
O2 O 0.3243(6) 0.5109(5) 0.1001(5) 0.0322(13) Uani 1 1 d . . .
N21 N 0.0708(7) 0.6214(6) 0.9737(6) 0.0234(14) Uani 1 1 d . . .
N1 N 0.2932(7) 0.4407(6) 0.3193(6) 0.0260(15) Uani 1 1 d . . .
C2 C 0.3561(7) 0.5166(7) 0.1962(7) 0.0229(16) Uani 1 1 d . . .
N4 N 0.4287(7) 0.6661(6) 0.3139(6) 0.0270(15) Uani 1 1 d . . .
C6 C 0.3479(8) 0.4520(7) 0.4221(8) 0.0280(18) Uani 1 1 d . . .
H6A H 0.4359 0.4058 0.3959 0.034 Uiso 1 1 calc R . .
H6B H 0.2793 0.4117 0.5141 0.034 Uiso 1 1 calc R . .
C5 C 0.3762(8) 0.5870(7) 0.4338(8) 0.0263(18) Uani 1 1 d . . .
C22 C -0.0676(8) 0.6118(8) 1.0587(8) 0.0277(18) Uani 1 1 d . . .
C26 C 0.1484(8) 0.5112(7) 0.9139(8) 0.0271(18) Uani 1 1 d . . .
H26A H 0.2208 0.4958 0.9483 0.033 Uiso 1 1 calc R . .
H26B H 0.1982 0.5339 0.8120 0.033 Uiso 1 1 calc R . .
C3 C 0.4693(8) 0.6086(8) 0.1826(8) 0.0283(18) Uani 1 1 d . . .
H3A H 0.5580 0.5642 0.1606 0.034 Uiso 1 1 calc R . .
H3B H 0.4854 0.6758 0.1052 0.034 Uiso 1 1 calc R . .
C12 C 0.5871(8) 0.8484(7) 0.3886(8) 0.0299(18) Uani 1 1 d . . .
H12A H 0.5465 0.8142 0.4870 0.045 Uiso 1 1 calc R . .
H12B H 0.6111 0.9381 0.3787 0.045 Uiso 1 1 calc R . .
H12C H 0.6720 0.8035 0.3372 0.045 Uiso 1 1 calc R . .
C28 C 0.3456(9) 0.7451(8) 0.8259(8) 0.035(2) Uani 1 1 d . . .
H28A H 0.3841 0.6820 0.8725 0.052 Uiso 1 1 calc R . .
H28B H 0.3998 0.8245 0.8015 0.052 Uiso 1 1 calc R . .
H28C H 0.3508 0.7154 0.7413 0.052 Uiso 1 1 calc R . .
C8 C 0.1062(8) 0.2373(8) 0.5134(8) 0.034(2) Uani 1 1 d . . .
H8A H 0.1882 0.2006 0.5214 0.050 Uiso 1 1 calc R . .
H8B H 0.0390 0.1699 0.5264 0.050 Uiso 1 1 calc R . .
H8C H 0.0621 0.2938 0.5845 0.050 Uiso 1 1 calc R . .
C27 C 0.1475(9) 0.8154(8) 1.1102(8) 0.038(2) Uani 1 1 d . . .
H27A H 0.0493 0.8280 1.1725 0.057 Uiso 1 1 calc R . .
H27B H 0.2024 0.8937 1.0913 0.057 Uiso 1 1 calc R . .
H27C H 0.1845 0.7484 1.1541 0.057 Uiso 1 1 calc R . .
C11 C 0.2869(9) 0.8951(8) 0.4209(9) 0.040(2) Uani 1 1 d . . .
H11A H 0.2247 0.8855 0.3767 0.061 Uiso 1 1 calc R . .
H11B H 0.2999 0.9847 0.4247 0.061 Uiso 1 1 calc R . .
H11C H 0.2450 0.8504 0.5153 0.061 Uiso 1 1 calc R . .
C29 C 0.0844(10) 0.8922(8) 0.8586(9) 0.039(2) Uani 1 1 d . . .
H29A H 0.1014 0.8704 0.7670 0.058 Uiso 1 1 calc R . .
H29B H 0.1292 0.9744 0.8478 0.058 Uiso 1 1 calc R . .
H29C H -0.0167 0.8959 0.9159 0.058 Uiso 1 1 calc R . .
C7 C 0.2389(9) 0.2196(8) 0.2020(8) 0.035(2) Uani 1 1 d . . .
H7A H 0.2471 0.2622 0.1129 0.052 Uiso 1 1 calc R . .
H7B H 0.1780 0.1440 0.2288 0.052 Uiso 1 1 calc R . .
H7C H 0.3320 0.1956 0.1929 0.052 Uiso 1 1 calc R . .
C10 C 0.5335(11) 0.9028(9) 0.1356(8) 0.048(3) Uani 1 1 d . . .
H10A H 0.6233 0.8655 0.0822 0.072 Uiso 1 1 calc R . .
H10B H 0.5480 0.9935 0.1322 0.072 Uiso 1 1 calc R . .
H10C H 0.4685 0.8887 0.0957 0.072 Uiso 1 1 calc R . .
C9 C 0.0121(8) 0.4147(8) 0.3285(9) 0.038(2) Uani 1 1 d . . .
H9A H -0.0345 0.4583 0.4110 0.058 Uiso 1 1 calc R . .
H9B H -0.0546 0.3551 0.3248 0.058 Uiso 1 1 calc R . .
H9C H 0.0464 0.4763 0.2450 0.058 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 1.790(6) . ?
Si1 C9 1.860(9) . ?
Si1 C8 1.865(8) . ?
Si1 C7 1.866(8) . ?
Si2 N21 1.790(6) . ?
Si2 C27 1.859(8) . ?
Si2 C28 1.863(9) . ?
Si2 C29 1.870(8) . ?
Si3 N4 1.787(7) . ?
Si3 C12 1.847(8) . ?
Si3 C11 1.852(9) . ?
Si3 C10 1.854(8) . ?
O5 C5 1.232(8) . ?
O22 C22 1.230(9) . ?
O2 C2 1.229(8) . ?
N21 C22 1.348(9) . ?
N21 C26 1.472(10) . ?
N1 C2 1.363(9) . ?
N1 C6 1.474(9) . ?
C2 C3 1.516(10) . ?
N4 C5 1.352(9) . ?
N4 C3 1.496(9) . ?
C6 C5 1.515(11) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C22 C26 1.515(11) 2_567 ?
C26 C22 1.515(11) 2_567 ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
 
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 Si1 C9 108.2(4) . . ?
N1 Si1 C8 106.1(3) . . ?
C9 Si1 C8 110.0(4) . . ?
N1 Si1 C7 109.9(3) . . ?
C9 Si1 C7 112.8(4) . . ?
C8 Si1 C7 109.7(4) . . ?
N21 Si2 C27 110.5(3) . . ?
N21 Si2 C28 105.0(3) . . ?
C27 Si2 C28 109.6(4) . . ?
N21 Si2 C29 109.8(3) . . ?
C27 Si2 C29 111.4(4) . . ?
C28 Si2 C29 110.2(4) . . ?
N4 Si3 C12 111.1(3) . . ?
N4 Si3 C11 107.5(4) . . ?
C12 Si3 C11 113.1(4) . . ?
N4 Si3 C10 105.8(4) . . ?
C12 Si3 C10 108.7(4) . . ?
C11 Si3 C10 110.3(4) . . ?
C22 N21 C26 121.1(6) . . ?
C22 N21 Si2 117.8(5) . . ?
C26 N21 Si2 121.0(5) . . ?
C2 N1 C6 116.5(6) . . ?
C2 N1 Si1 117.9(5) . . ?
C6 N1 Si1 125.4(5) . . ?
O2 C2 N1 122.3(7) . . ?
O2 C2 C3 121.2(6) . . ?
N1 C2 C3 116.5(6) . . ?
C5 N4 C3 116.8(6) . . ?
C5 N4 Si3 119.3(5) . . ?
C3 N4 Si3 123.7(5) . . ?
N1 C6 C5 113.2(6) . . ?
N1 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
N1 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.8 . . ?
O5 C5 N4 122.5(7) . . ?
O5 C5 C6 121.3(7) . . ?
N4 C5 C6 116.1(6) . . ?
O22 C22 N21 122.0(7) . . ?
O22 C22 C26 117.7(7) . 2_567 ?
N21 C22 C26 120.3(7) . 2_567 ?
N21 C26 C22 118.5(6) . 2_567 ?
N21 C26 H26A 107.7 . . ?
C22 C26 H26A 107.7 2_567 . ?
N21 C26 H26B 107.7 . . ?
C22 C26 H26B 107.7 2_567 . ?
H26A C26 H26B 107.1 . . ?
N4 C3 C2 111.0(6) . . ?
N4 C3 H3A 109.4 . . ?
C2 C3 H3A 109.4 . . ?
N4 C3 H3B 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C29 H29A 109.5 . . ?
Si2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.976
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.976
_refine_diff_density_max    0.562
_refine_diff_density_min   -0.493
_refine_diff_density_rms    0.121
