data_01sot104
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C27 H36 N2 O6 Si'
_chemical_formula_weight          512.67
 
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                    7.9703(16)
_cell_length_b                    12.128(2)
_cell_length_c                    14.121(3)
_cell_angle_alpha                 79.14(3)
_cell_angle_beta                  83.06(3)
_cell_angle_gamma                 77.29(3)
_cell_volume                      1303.2(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     9132
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.38
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.307
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              548
_exptl_absorpt_coefficient_mu     0.135
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9506
_exptl_absorpt_correction_T_max   0.9920
_exptl_absorpt_process_details    'SORTAV Blessing (1997)'
 
_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   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD'
_diffrn_measurement_method        'Φ & ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             19904
_diffrn_reflns_av_R_equivalents   0.0503
_diffrn_reflns_av_sigmaI/netI     0.0432
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.95
_diffrn_reflns_theta_max          27.47
_reflns_number_total              5893
_reflns_number_gt                 4879
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_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 > 2sigma(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)+(0.0702P)²+0.5256P] 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      SHELXL
_refine_ls_extinction_coef        0.008(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          5893
_refine_ls_number_parameters      332
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0576
_refine_ls_R_factor_gt            0.0450
_refine_ls_wR_factor_ref          0.1278
_refine_ls_wR_factor_gt           0.1196
_refine_ls_goodness_of_fit_ref    1.020
_refine_ls_restrained_S_all       1.020
_refine_ls_shift/su_max           0.023
_refine_ls_shift/su_mean          0.002
 
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 0.19127(18) 0.81773(12) 0.24030(10) 0.0169(3) Uani 1 1 d . . .
C2 C 0.31726(19) 0.70920(12) 0.28815(11) 0.0186(3) Uani 1 1 d . . .
H2 H 0.4103 0.7328 0.3165 0.022 Uiso 1 1 calc R . .
C3 C 0.04386(19) 0.67705(13) 0.33902(11) 0.0202(3) Uani 1 1 d . . .
H3 H 0.0284 0.6360 0.2865 0.024 Uiso 1 1 calc R . .
C4 C 0.01894(18) 0.80596(12) 0.30108(11) 0.0190(3) Uani 1 1 d . . .
H4A H -0.0001 0.8502 0.3550 0.023 Uiso 1 1 calc R . .
H4B H -0.0799 0.8326 0.2605 0.023 Uiso 1 1 calc R . .
C5 C 0.34403(19) 0.69788(13) 0.12162(11) 0.0199(3) Uani 1 1 d . . .
H5 H 0.4407 0.7335 0.0864 0.024 Uiso 1 1 calc R . .
C6 C 0.18500(19) 0.79205(12) 0.13737(11) 0.0184(3) Uani 1 1 d . . .
H6A H 0.0779 0.7654 0.1329 0.022 Uiso 1 1 calc R . .
H6B H 0.1891 0.8616 0.0883 0.022 Uiso 1 1 calc R . .
C7 C -0.0787(2) 0.65004(13) 0.42593(11) 0.0217(3) Uani 1 1 d . . .
C8 C -0.0426(2) 0.65256(13) 0.51978(12) 0.0246(3) Uani 1 1 d . . .
H8 H 0.0686 0.6608 0.5314 0.029 Uiso 1 1 calc R . .
C9 C -0.1684(2) 0.64306(13) 0.59587(12) 0.0261(4) Uani 1 1 d . . .
H9 H -0.1450 0.6453 0.6598 0.031 Uiso 1 1 calc R . .
C10 C -0.3293(2) 0.63023(13) 0.57713(12) 0.0246(3) Uani 1 1 d . . .
C11 C -0.3662(2) 0.62176(14) 0.48604(12) 0.0261(3) Uani 1 1 d . . .
H11 H -0.4757 0.6096 0.4754 0.031 Uiso 1 1 calc R . .
C12 C -0.2393(2) 0.63155(14) 0.41051(12) 0.0245(3) Uani 1 1 d . . .
H12 H -0.2618 0.6256 0.3473 0.029 Uiso 1 1 calc R . .
C13 C 0.30829(18) 0.61183(13) 0.06597(11) 0.0179(3) Uani 1 1 d . . .
C14 C 0.33627(18) 0.62753(13) -0.03453(11) 0.0197(3) Uani 1 1 d . . .
H14 H 0.3850 0.6903 -0.0678 0.024 Uiso 1 1 calc R . .
C15 C 0.29371(19) 0.55254(14) -0.08670(11) 0.0210(3) Uani 1 1 d . . .
H15 H 0.3106 0.5638 -0.1553 0.025 Uiso 1 1 calc R . .
C16 C 0.22599(18) 0.46094(13) -0.03533(11) 0.0201(3) Uani 1 1 d . . .
C17 C 0.19931(19) 0.44168(13) 0.06449(11) 0.0209(3) Uani 1 1 d . . .
H17 H 0.1542 0.3773 0.0976 0.025 Uiso 1 1 calc R . .
C18 C 0.23984(19) 0.51823(13) 0.11482(11) 0.0194(3) Uani 1 1 d . . .
H18 H 0.2209 0.5071 0.1834 0.023 Uiso 1 1 calc R . .
C19 C 0.4367(2) 0.97993(13) 0.14535(12) 0.0224(3) Uani 1 1 d . . .
H19 H 0.4038 0.9572 0.0867 0.027 Uiso 1 1 calc R . .
C20 C 0.6085(2) 0.90035(16) 0.17067(15) 0.0341(4) Uani 1 1 d . . .
H20A H 0.6937 0.9067 0.1148 0.051 Uiso 1 1 calc R . .
H20B H 0.5922 0.8210 0.1877 0.051 Uiso 1 1 calc R . .
H20C H 0.6497 0.9223 0.2257 0.051 Uiso 1 1 calc R . .
C21 C 0.4645(2) 1.10360(15) 0.11479(14) 0.0308(4) Uani 1 1 d . . .
H21A H 0.4881 1.1320 0.1713 0.046 Uiso 1 1 calc R . .
H21B H 0.3605 1.1525 0.0876 0.046 Uiso 1 1 calc R . .
H21C H 0.5627 1.1051 0.0659 0.046 Uiso 1 1 calc R . .
C22 C 0.0700(2) 1.08596(14) 0.21359(13) 0.0273(4) Uani 1 1 d . . .
H22 H 0.1213 1.1559 0.2038 0.033 Uiso 1 1 calc R . .
C23 C 0.0003(2) 1.08686(15) 0.11646(14) 0.0332(4) Uani 1 1 d . . .
H23A H -0.0558 1.0214 0.1220 0.050 Uiso 1 1 calc R . .
H23B H 0.0960 1.0815 0.0659 0.050 Uiso 1 1 calc R . .
H23C H -0.0837 1.1583 0.0996 0.050 Uiso 1 1 calc R . .
C24 C -0.0799(3) 1.10447(17) 0.29217(16) 0.0442(5) Uani 1 1 d . . .
H24A H -0.1589 1.1773 0.2721 0.066 Uiso 1 1 calc R . .
H24B H -0.0342 1.1065 0.3531 0.066 Uiso 1 1 calc R . .
H24C H -0.1421 1.0415 0.3014 0.066 Uiso 1 1 calc R . .
C25 C 0.3409(3) 0.95501(15) 0.36494(13) 0.0329(4) Uani 1 1 d . . .
H25 H 0.4612 0.9087 0.3614 0.040 Uiso 1 1 calc R . .
C26 C 0.3579(4) 1.07440(17) 0.37917(15) 0.0501(6) Uani 1 1 d . . .
H26A H 0.2453 1.1268 0.3745 0.075 Uiso 1 1 calc R . .
H26B H 0.4411 1.1033 0.3290 0.075 Uiso 1 1 calc R . .
H26C H 0.3981 1.0693 0.4431 0.075 Uiso 1 1 calc R . .
C27 C 0.2487(3) 0.89806(18) 0.45464(13) 0.0397(5) Uani 1 1 d . . .
H27A H 0.3084 0.8976 0.5115 0.060 Uiso 1 1 calc R . .
H27B H 0.2483 0.8191 0.4482 0.060 Uiso 1 1 calc R . .
H27C H 0.1295 0.9406 0.4624 0.060 Uiso 1 1 calc R . .
N1 N -0.4682(2) 0.62935(12) 0.65594(10) 0.0301(3) Uani 1 1 d . . .
N2 N 0.17936(17) 0.38074(12) -0.08868(11) 0.0269(3) Uani 1 1 d . . .
O1 O 0.22103(14) 0.64699(9) 0.36191(8) 0.0238(3) Uani 1 1 d . . .
O2 O 0.39047(14) 0.64166(10) 0.21635(8) 0.0250(3) Uani 1 1 d . . .
O3 O -0.44662(18) 0.65988(11) 0.73097(9) 0.0369(3) Uani 1 1 d . . .
O4 O -0.60067(18) 0.60044(14) 0.64261(10) 0.0456(4) Uani 1 1 d . . .
O5 O 0.17938(17) 0.40609(13) -0.17666(10) 0.0384(3) Uani 1 1 d . . .
O6 O 0.14076(17) 0.29202(11) -0.04211(11) 0.0383(3) Uani 1 1 d . . .
Si1 Si 0.25547(5) 0.96039(3) 0.24340(3) 0.01786(13) Uani 1 1 d . . .
 
 
_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 C4 1.549(2) . ?
C1 C6 1.551(2) . ?
C1 C2 1.564(2) . ?
C1 Si1 1.9186(15) . ?
C2 O2 1.4138(19) . ?
C2 O1 1.4169(19) . ?
C2 H2 1.0000 . ?
C3 O1 1.4391(18) . ?
C3 C7 1.506(2) . ?
C3 C4 1.531(2) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O2 1.4339(19) . ?
C5 C13 1.510(2) . ?
C5 C6 1.533(2) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.397(2) . ?
C7 C12 1.395(2) . ?
C8 C9 1.385(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(2) . ?
C10 N1 1.472(2) . ?
C11 C12 1.386(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.393(2) . ?
C13 C18 1.396(2) . ?
C14 C15 1.391(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.383(2) . ?
C16 N2 1.468(2) . ?
C17 C18 1.381(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.530(2) . ?
C19 C21 1.538(2) . ?
C19 Si1 1.8980(17) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.537(3) . ?
C22 C23 1.538(3) . ?
C22 Si1 1.8975(18) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.513(3) . ?
C25 C26 1.536(2) . ?
C25 Si1 1.9061(18) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N1 O3 1.229(2) . ?
N1 O4 1.228(2) . ?
N2 O5 1.222(2) . ?
N2 O6 1.231(2) . ?
 
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
C4 C1 C6 109.80(12) . . ?
C4 C1 C2 101.54(12) . . ?
C6 C1 C2 102.77(12) . . ?
C4 C1 Si1 112.28(10) . . ?
C6 C1 Si1 114.81(10) . . ?
C2 C1 Si1 114.49(10) . . ?
O2 C2 O1 110.25(12) . . ?
O2 C2 C1 108.49(12) . . ?
O1 C2 C1 108.19(12) . . ?
O2 C2 H2 110.0 . . ?
O1 C2 H2 110.0 . . ?
C1 C2 H2 110.0 . . ?
O1 C3 C7 112.24(13) . . ?
O1 C3 C4 102.82(12) . . ?
C7 C3 C4 112.14(13) . . ?
O1 C3 H3 109.8 . . ?
C7 C3 H3 109.8 . . ?
C4 C3 H3 109.8 . . ?
C3 C4 C1 103.18(12) . . ?
C3 C4 H4A 111.1 . . ?
C1 C4 H4A 111.1 . . ?
C3 C4 H4B 111.1 . . ?
C1 C4 H4B 111.1 . . ?
H4A C4 H4B 109.1 . . ?
O2 C5 C13 109.71(12) . . ?
O2 C5 C6 105.91(12) . . ?
C13 C5 C6 112.50(12) . . ?
O2 C5 H5 109.5 . . ?
C13 C5 H5 109.5 . . ?
C6 C5 H5 109.5 . . ?
C5 C6 C1 105.75(12) . . ?
C5 C6 H6A 110.6 . . ?
C1 C6 H6A 110.6 . . ?
C5 C6 H6B 110.6 . . ?
C1 C6 H6B 110.6 . . ?
H6A C6 H6B 108.7 . . ?
C8 C7 C12 119.40(15) . . ?
C8 C7 C3 122.13(14) . . ?
C12 C7 C3 118.25(14) . . ?
C9 C8 C7 120.13(15) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 118.84(15) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C11 C10 C9 122.36(15) . . ?
C11 C10 N1 118.33(15) . . ?
C9 C10 N1 119.28(15) . . ?
C10 C11 C12 118.17(15) . . ?
C10 C11 H11 120.9 . . ?
C12 C11 H11 120.9 . . ?
C11 C12 C7 120.95(15) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
C14 C13 C18 119.40(14) . . ?
C14 C13 C5 120.52(13) . . ?
C18 C13 C5 120.02(13) . . ?
C15 C14 C13 120.84(14) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C16 C15 C14 117.81(14) . . ?
C16 C15 H15 121.1 . . ?
C14 C15 H15 121.1 . . ?
C15 C16 C17 122.86(14) . . ?
C15 C16 N2 118.90(14) . . ?
C17 C16 N2 118.24(14) . . ?
C18 C17 C16 118.40(14) . . ?
C18 C17 H17 120.8 . . ?
C16 C17 H17 120.8 . . ?
C17 C18 C13 120.67(14) . . ?
C17 C18 H18 119.7 . . ?
C13 C18 H18 119.7 . . ?
C20 C19 C21 109.23(13) . . ?
C20 C19 Si1 112.69(12) . . ?
C21 C19 Si1 115.11(12) . . ?
C20 C19 H19 106.4 . . ?
C21 C19 H19 106.4 . . ?
Si1 C19 H19 106.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C23 110.25(16) . . ?
C24 C22 Si1 117.14(13) . . ?
C23 C22 Si1 112.24(12) . . ?
C24 C22 H22 105.4 . . ?
C23 C22 H22 105.4 . . ?
Si1 C22 H22 105.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C27 C25 C26 109.54(17) . . ?
C27 C25 Si1 117.65(13) . . ?
C26 C25 Si1 111.40(13) . . ?
C27 C25 H25 105.8 . . ?
C26 C25 H25 105.8 . . ?
Si1 C25 H25 105.8 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O3 N1 O4 123.48(15) . . ?
O3 N1 C10 118.06(15) . . ?
O4 N1 C10 118.44(15) . . ?
O5 N2 O6 123.60(15) . . ?
O5 N2 C16 118.33(14) . . ?
O6 N2 C16 118.07(14) . . ?
C2 O1 C3 107.52(11) . . ?
C2 O2 C5 112.11(11) . . ?
C19 Si1 C22 106.57(8) . . ?
C19 Si1 C25 107.94(8) . . ?
C22 Si1 C25 113.16(9) . . ?
C19 Si1 C1 108.20(7) . . ?
C22 Si1 C1 111.10(7) . . ?
C25 Si1 C1 109.67(7) . . ?
 
_diffrn_measured_fraction_theta_max    0.989
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.989
_refine_diff_density_max    0.666
_refine_diff_density_min   -0.374
_refine_diff_density_rms    0.057
