 
data_01sot096
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
;
Lee Patient - Kilburn

; 
_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            Orthorhombic
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, -z' 
 '-x, y+1/2, -z+1/2' 
 '-x+1/2, -y, z+1/2' 
 
_cell_length_a                    11.4829(3) 
_cell_length_b                    14.5419(3) 
_cell_length_c                    15.7595(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2631.57(11) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     2624 
_cell_measurement_theta_min       2.94 
_cell_measurement_theta_max       25.02 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.294 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1096 
_exptl_absorpt_coefficient_mu     0.133 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_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             2624 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0463 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.94 
_diffrn_reflns_theta_max          25.02 
_reflns_number_total              2624 
_reflns_number_gt                 2328 
_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)+(0.0435P)²+0.0000P] 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        0.0051(9) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.52(15) 
_refine_ls_number_reflns          2624 
_refine_ls_number_parameters      327 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0363 
_refine_ls_R_factor_gt            0.0307 
_refine_ls_wR_factor_ref          0.0738 
_refine_ls_wR_factor_gt           0.0722 
_refine_ls_goodness_of_fit_ref    1.005 
_refine_ls_restrained_S_all       1.005 
_refine_ls_shift/su_max           0.003 
_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 0.2460(2) 0.30747(15) 0.55008(15) 0.0178(5) Uani 1 1 d . . . 
C2 C 0.3168(2) 0.37223(16) 0.58729(15) 0.0209(6) Uani 1 1 d . . . 
H2 H 0.3840 0.3542 0.6182 0.025 Uiso 1 1 calc R . . 
C3 C 0.2878(2) 0.46470(16) 0.57872(15) 0.0203(6) Uani 1 1 d . . . 
H3 H 0.3357 0.5104 0.6040 0.024 Uiso 1 1 calc R . . 
C4 C 0.1888(2) 0.49063(15) 0.53331(14) 0.0171(5) Uani 1 1 d . . . 
C5 C 0.1188(2) 0.42277(16) 0.49706(14) 0.0205(5) Uani 1 1 d . . . 
H5 H 0.0511 0.4400 0.4663 0.025 Uiso 1 1 calc R . . 
C6 C 0.1469(2) 0.33031(16) 0.50542(15) 0.0206(6) Uani 1 1 d . . . 
H6 H 0.0991 0.2840 0.4810 0.025 Uiso 1 1 calc R . . 
C7 C 0.1563(2) 0.59052(15) 0.52227(14) 0.0165(5) Uani 1 1 d . . . 
H7 H 0.1385 0.6027 0.4612 0.020 Uiso 1 1 calc R . . 
C8 C 0.0539(2) 0.62350(15) 0.57728(14) 0.0171(5) Uani 1 1 d . . . 
H8A H 0.0492 0.5874 0.6304 0.020 Uiso 1 1 calc R . . 
H8B H -0.0206 0.6171 0.5462 0.020 Uiso 1 1 calc R . . 
C9 C 0.07978(19) 0.72631(15) 0.59681(14) 0.0159(5) Uani 1 1 d . . . 
C10 C 0.0163(2) 0.79099(16) 0.53388(14) 0.0183(5) Uani 1 1 d . . . 
H10A H -0.0604 0.7656 0.5175 0.022 Uiso 1 1 calc R . . 
H10B H 0.0051 0.8529 0.5588 0.022 Uiso 1 1 calc R . . 
C11 C 0.0981(2) 0.79479(16) 0.45808(15) 0.0173(5) Uani 1 1 d . . . 
H11 H 0.0887 0.7376 0.4235 0.021 Uiso 1 1 calc R . . 
C12 C 0.2091(2) 0.73604(16) 0.56853(14) 0.0171(5) Uani 1 1 d . . . 
H12 H 0.2561 0.7633 0.6156 0.020 Uiso 1 1 calc R . . 
C13 C 0.0841(2) 0.87788(15) 0.40152(14) 0.0163(5) Uani 1 1 d . . . 
C14 C 0.1228(2) 0.96459(16) 0.42589(15) 0.0209(6) Uani 1 1 d . . . 
H14 H 0.1595 0.9726 0.4794 0.025 Uiso 1 1 calc R . . 
C15 C 0.1080(2) 1.03916(16) 0.37237(17) 0.0240(6) Uani 1 1 d . . . 
H15 H 0.1339 1.0987 0.3887 0.029 Uiso 1 1 calc R . . 
C16 C 0.0549(2) 1.02526(16) 0.29490(15) 0.0217(6) Uani 1 1 d . . . 
C17 C 0.0148(2) 0.94039(15) 0.26914(15) 0.0211(6) Uani 1 1 d . . . 
H17 H -0.0215 0.9325 0.2155 0.025 Uiso 1 1 calc R . . 
C18 C 0.0292(2) 0.86713(16) 0.32403(15) 0.0207(6) Uani 1 1 d . . . 
H18 H 0.0008 0.8082 0.3082 0.025 Uiso 1 1 calc R . . 
C19 C 0.0972(2) 0.66032(16) 0.78274(15) 0.0213(6) Uani 1 1 d . . . 
H19 H 0.0536 0.6055 0.7614 0.026 Uiso 1 1 calc R . . 
C20 C 0.0649(3) 0.6703(2) 0.87682(16) 0.0347(7) Uani 1 1 d . . . 
H20A H -0.0180 0.6855 0.8818 0.052 Uiso 1 1 calc R . . 
H20B H 0.1115 0.7195 0.9024 0.052 Uiso 1 1 calc R . . 
H20C H 0.0805 0.6123 0.9064 0.052 Uiso 1 1 calc R . . 
C21 C 0.2267(2) 0.63656(18) 0.77502(17) 0.0266(6) Uani 1 1 d . . . 
H21A H 0.2470 0.6289 0.7150 0.040 Uiso 1 1 calc R . . 
H21B H 0.2426 0.5792 0.8056 0.040 Uiso 1 1 calc R . . 
H21C H 0.2734 0.6863 0.7995 0.040 Uiso 1 1 calc R . . 
C22 C -0.1077(2) 0.78269(16) 0.73428(15) 0.0217(6) Uani 1 1 d . . . 
H22 H -0.1125 0.7978 0.7961 0.026 Uiso 1 1 calc R . . 
C23 C -0.1818(2) 0.69634(18) 0.72308(17) 0.0302(6) Uani 1 1 d . . . 
H23A H -0.1444 0.6446 0.7522 0.045 Uiso 1 1 calc R . . 
H23B H -0.1891 0.6822 0.6625 0.045 Uiso 1 1 calc R . . 
H23C H -0.2593 0.7068 0.7473 0.045 Uiso 1 1 calc R . . 
C24 C -0.1647(2) 0.86469(19) 0.68863(17) 0.0314(7) Uani 1 1 d . . . 
H24A H -0.1165 0.9197 0.6965 0.047 Uiso 1 1 calc R . . 
H24B H -0.2423 0.8756 0.7124 0.047 Uiso 1 1 calc R . . 
H24C H -0.1714 0.8510 0.6279 0.047 Uiso 1 1 calc R . . 
C25 C 0.1407(2) 0.86618(16) 0.74326(15) 0.0210(6) Uani 1 1 d . . . 
H25 H 0.2196 0.8429 0.7595 0.025 Uiso 1 1 calc R . . 
C26 C 0.0914(2) 0.91351(18) 0.82277(16) 0.0322(7) Uani 1 1 d . . . 
H26A H 0.0785 0.8675 0.8672 0.048 Uiso 1 1 calc R . . 
H26B H 0.0174 0.9434 0.8087 0.048 Uiso 1 1 calc R . . 
H26C H 0.1469 0.9597 0.8431 0.048 Uiso 1 1 calc R . . 
C27 C 0.1612(2) 0.93938(16) 0.67442(17) 0.0273(6) Uani 1 1 d . . . 
H27A H 0.1932 0.9100 0.6235 0.041 Uiso 1 1 calc R . . 
H27B H 0.2163 0.9855 0.6955 0.041 Uiso 1 1 calc R . . 
H27C H 0.0872 0.9693 0.6604 0.041 Uiso 1 1 calc R . . 
N1 N 0.2808(2) 0.20975(14) 0.55615(13) 0.0238(5) Uani 1 1 d . . . 
N2 N 0.04043(19) 1.10405(15) 0.23782(16) 0.0306(6) Uani 1 1 d . . . 
O1 O 0.37434(17) 0.19132(12) 0.58972(13) 0.0352(5) Uani 1 1 d . . . 
O2 O 0.21475(17) 0.15145(12) 0.52698(13) 0.0375(5) Uani 1 1 d . . . 
O3 O 0.05984(18) 1.18117(12) 0.26648(14) 0.0452(6) Uani 1 1 d . . . 
O4 O 0.00969(19) 1.08988(14) 0.16448(13) 0.0470(6) Uani 1 1 d . . . 
O5 O 0.25199(14) 0.64726(10) 0.54850(10) 0.0178(4) Uani 1 1 d . . . 
O6 O 0.21196(13) 0.79532(10) 0.49653(10) 0.0176(4) Uani 1 1 d . . . 
Si1 Si 0.05191(6) 0.76047(4) 0.71302(4) 0.01664(17) 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 C2 1.375(3) . ? 
C1 C6 1.378(4) . ? 
C1 N1 1.480(3) . ? 
C2 C3 1.392(3) . ? 
C3 C4 1.395(3) . ? 
C4 C5 1.395(3) . ? 
C4 C7 1.510(3) . ? 
C5 C6 1.389(3) . ? 
C7 O5 1.435(3) . ? 
C7 C8 1.538(3) . ? 
C8 C9 1.555(3) . ? 
C9 C10 1.549(3) . ? 
C9 C12 1.557(3) . ? 
C9 Si1 1.924(2) . ? 
C10 C11 1.520(3) . ? 
C11 O6 1.441(3) . ? 
C11 C13 1.510(3) . ? 
C12 O5 1.417(3) . ? 
C12 O6 1.425(3) . ? 
C13 C18 1.383(3) . ? 
C13 C14 1.391(3) . ? 
C14 C15 1.384(3) . ? 
C15 C16 1.379(4) . ? 
C16 C17 1.379(3) . ? 
C16 N2 1.466(3) . ? 
C17 C18 1.382(3) . ? 
C19 C21 1.531(4) . ? 
C19 C20 1.536(3) . ? 
C19 Si1 1.897(2) . ? 
C22 C23 1.527(3) . ? 
C22 C24 1.538(3) . ? 
C22 Si1 1.891(2) . ? 
C25 C26 1.538(3) . ? 
C25 C27 1.538(3) . ? 
C25 Si1 1.905(2) . ? 
N1 O1 1.226(3) . ? 
N1 O2 1.227(3) . ? 
N2 O4 1.226(3) . ? 
N2 O3 1.229(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 
C2 C1 C6 122.7(2) . . ? 
C2 C1 N1 118.0(2) . . ? 
C6 C1 N1 119.2(2) . . ? 
C1 C2 C3 118.6(2) . . ? 
C2 C3 C4 120.4(2) . . ? 
C3 C4 C5 119.2(2) . . ? 
C3 C4 C7 121.4(2) . . ? 
C5 C4 C7 119.4(2) . . ? 
C6 C5 C4 120.8(2) . . ? 
C1 C6 C5 118.2(2) . . ? 
O5 C7 C4 109.29(18) . . ? 
O5 C7 C8 104.12(17) . . ? 
C4 C7 C8 115.11(19) . . ? 
C7 C8 C9 105.37(18) . . ? 
C10 C9 C8 111.54(19) . . ? 
C10 C9 C12 102.12(18) . . ? 
C8 C9 C12 102.31(18) . . ? 
C10 C9 Si1 111.99(15) . . ? 
C8 C9 Si1 113.88(15) . . ? 
C12 C9 Si1 114.06(15) . . ? 
C11 C10 C9 103.59(18) . . ? 
O6 C11 C13 109.91(19) . . ? 
O6 C11 C10 103.29(18) . . ? 
C13 C11 C10 115.28(19) . . ? 
O5 C12 O6 111.45(18) . . ? 
O5 C12 C9 108.21(18) . . ? 
O6 C12 C9 107.76(18) . . ? 
C18 C13 C14 119.5(2) . . ? 
C18 C13 C11 118.6(2) . . ? 
C14 C13 C11 121.9(2) . . ? 
C15 C14 C13 120.2(2) . . ? 
C16 C15 C14 118.6(2) . . ? 
C17 C16 C15 122.7(2) . . ? 
C17 C16 N2 118.7(2) . . ? 
C15 C16 N2 118.6(2) . . ? 
C16 C17 C18 117.8(2) . . ? 
C17 C18 C13 121.3(2) . . ? 
C21 C19 C20 109.5(2) . . ? 
C21 C19 Si1 113.18(18) . . ? 
C20 C19 Si1 114.84(18) . . ? 
C23 C22 C24 110.3(2) . . ? 
C23 C22 Si1 112.25(16) . . ? 
C24 C22 Si1 117.47(17) . . ? 
C26 C25 C27 108.7(2) . . ? 
C26 C25 Si1 111.59(17) . . ? 
C27 C25 Si1 117.64(17) . . ? 
O1 N1 O2 123.5(2) . . ? 
O1 N1 C1 118.3(2) . . ? 
O2 N1 C1 118.2(2) . . ? 
O4 N2 O3 123.5(2) . . ? 
O4 N2 C16 118.7(2) . . ? 
O3 N2 C16 117.8(2) . . ? 
C12 O5 C7 108.76(17) . . ? 
C12 O6 C11 108.09(16) . . ? 
C22 Si1 C19 107.13(11) . . ? 
C22 Si1 C25 109.67(10) . . ? 
C19 Si1 C25 109.12(11) . . ? 
C22 Si1 C9 111.96(10) . . ? 
C19 Si1 C9 107.90(10) . . ? 
C25 Si1 C9 110.94(10) . . ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              25.02 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.287 
_refine_diff_density_min   -0.201 
_refine_diff_density_rms    0.038 
