data_12kaw3h2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 N4 O8 Si2' _chemical_formula_weight 596.83 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 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.418(6) _cell_length_b 7.6590(19) _cell_length_c 18.298(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.870(4) _cell_angle_gamma 90.00 _cell_volume 3085.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5762 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 22.30 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9125 _exptl_absorpt_correction_T_max 0.9934 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31572 _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_sigmaI/netI 0.2135 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 21.99 _reflns_number_total 3768 _reflns_number_gt 1719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0380P)^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 3768 _refine_ls_number_parameters 369 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.1617 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2357 _refine_ls_wR_factor_gt 0.2181 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.049 _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 0.19893(14) 0.0843(4) 0.01901(17) 0.0573(9) Uani 1 1 d . . . Si2 Si 0.14161(14) -0.0737(4) 0.15085(18) 0.0607(10) Uani 1 1 d . . . O1 O 0.1554(3) 0.0300(9) 0.0770(4) 0.065(2) Uani 1 1 d U . . O2 O 0.2688(3) 0.1143(8) 0.0626(3) 0.0474(18) Uani 1 1 d . . . O3 O 0.2040(3) -0.0894(9) 0.2117(4) 0.0532(19) Uani 1 1 d U . . O4 O 0.3688(3) 0.1996(8) 0.1848(3) 0.0435(17) Uani 1 1 d . . . O5 O 0.5348(3) 0.6373(8) 0.0054(3) 0.0369(16) Uani 1 1 d . . . O6 O 0.6163(3) 0.7916(8) 0.0067(3) 0.0516(19) Uani 1 1 d U . . O7 O 0.6323(3) 1.3722(8) 0.0976(4) 0.055(2) Uani 1 1 d U . . O8 O 0.5695(3) 1.4662(8) 0.1642(4) 0.0461(18) Uani 1 1 d . . . N1 N 0.4199(3) 0.6859(10) 0.1443(4) 0.035(2) Uani 1 1 d . . . N2 N 0.4636(3) 0.7125(9) 0.1000(4) 0.0316(19) Uani 1 1 d . . . H2N H 0.4692 0.6347 0.0666 0.038 Uiso 1 1 calc R . . N3 N 0.5669(4) 0.7657(11) 0.0257(4) 0.037(2) Uani 1 1 d . . . N4 N 0.5898(4) 1.3512(10) 0.1292(5) 0.046(2) Uani 1 1 d . . . C1 C 0.3032(4) -0.0081(13) 0.1095(6) 0.050(3) Uani 1 1 d . . . H1A H 0.3398 -0.0400 0.0893 0.060 Uiso 1 1 calc R . . H1B H 0.2790 -0.1152 0.1119 0.060 Uiso 1 1 calc R . . C2 C 0.3225(4) 0.0696(13) 0.1881(5) 0.043(3) Uani 1 1 d . . . H2 H 0.3406 -0.0255 0.2227 0.051 Uiso 1 1 calc R . . C3 C 0.2743(4) 0.1592(12) 0.2207(5) 0.041(3) Uani 1 1 d U . . H3 H 0.2467 0.2225 0.1799 0.049 Uiso 1 1 calc R . . C4 C 0.2356(5) 0.0363(14) 0.2591(6) 0.060(3) Uani 1 1 d U . . H4A H 0.2625 -0.0236 0.3007 0.072 Uiso 1 1 calc R . . H4B H 0.2061 0.1069 0.2805 0.072 Uiso 1 1 calc R . . C5 C 0.3100(4) 0.2912(12) 0.2710(5) 0.043(3) Uani 1 1 d U . . H5A H 0.3276 0.2387 0.3197 0.052 Uiso 1 1 calc R . . H5B H 0.2841 0.3914 0.2791 0.052 Uiso 1 1 calc R . . C6 C 0.3599(4) 0.3482(12) 0.2296(5) 0.040(3) Uani 1 1 d U . . H6 H 0.3981 0.3733 0.2661 0.049 Uiso 1 1 calc R . . C7 C 0.1764(5) 0.2999(17) -0.0182(7) 0.090(4) Uani 1 1 d DU . . H7 H 0.1725 0.3612 0.0290 0.109 Uiso 1 1 calc R . . C8 C 0.1132(5) 0.3218(19) -0.0606(8) 0.120(4) Uani 1 1 d DU . . H8A H 0.1067 0.4438 -0.0761 0.179 Uiso 1 1 calc R . . H8B H 0.0843 0.2895 -0.0289 0.179 Uiso 1 1 calc R . . H8C H 0.1071 0.2464 -0.1047 0.179 Uiso 1 1 calc R . . C9 C 0.2266(6) 0.4099(18) -0.0410(7) 0.105(5) Uani 1 1 d U . . H9A H 0.2435 0.3479 -0.0793 0.157 Uiso 1 1 calc R . . H9B H 0.2587 0.4306 0.0024 0.157 Uiso 1 1 calc R . . H9C H 0.2097 0.5220 -0.0610 0.157 Uiso 1 1 calc R . . C10 C 0.1976(5) -0.0965(16) -0.0467(6) 0.072(3) Uani 1 1 d . . . H10 H 0.2142 -0.2009 -0.0168 0.087 Uiso 1 1 calc R . . C11 C 0.1337(5) -0.1491(16) -0.0910(6) 0.088(4) Uani 1 1 d U . . H11A H 0.1185 -0.0576 -0.1272 0.131 Uiso 1 1 calc R . . H11B H 0.1055 -0.1633 -0.0564 0.131 Uiso 1 1 calc R . . H11C H 0.1368 -0.2594 -0.1171 0.131 Uiso 1 1 calc R . . C12 C 0.2369(5) -0.0695(16) -0.1043(6) 0.081(4) Uani 1 1 d U . . H12A H 0.2390 -0.1785 -0.1318 0.121 Uiso 1 1 calc R . . H12B H 0.2778 -0.0349 -0.0796 0.121 Uiso 1 1 calc R . . H12C H 0.2192 0.0225 -0.1390 0.121 Uiso 1 1 calc R . . C13 C 0.1219(6) -0.3044(16) 0.1225(7) 0.087(4) Uani 1 1 d U . . H13 H 0.1485 -0.3323 0.0859 0.104 Uiso 1 1 calc R . . C14 C 0.0562(5) -0.3306(17) 0.0780(7) 0.098(4) Uani 1 1 d U . . H14A H 0.0544 -0.4375 0.0482 0.147 Uiso 1 1 calc R . . H14B H 0.0447 -0.2304 0.0451 0.147 Uiso 1 1 calc R . . H14C H 0.0280 -0.3406 0.1128 0.147 Uiso 1 1 calc R . . C15 C 0.1382(6) -0.4418(17) 0.1831(7) 0.106(5) Uani 1 1 d U . . H15A H 0.1149 -0.4206 0.2225 0.159 Uiso 1 1 calc R . . H15B H 0.1817 -0.4352 0.2040 0.159 Uiso 1 1 calc R . . H15C H 0.1284 -0.5580 0.1618 0.159 Uiso 1 1 calc R . . C16 C 0.0859(6) 0.0657(18) 0.1865(7) 0.097(4) Uani 1 1 d U . . H16 H 0.1081 0.1706 0.2102 0.116 Uiso 1 1 calc R . . C17 C 0.0342(5) 0.1301(17) 0.1258(7) 0.095(4) Uani 1 1 d U . . H17A H 0.0061 0.0335 0.1095 0.143 Uiso 1 1 calc R . . H17B H 0.0508 0.1735 0.0835 0.143 Uiso 1 1 calc R . . H17C H 0.0123 0.2245 0.1456 0.143 Uiso 1 1 calc R . . C18 C 0.0586(6) -0.030(2) 0.2466(8) 0.115(4) Uani 1 1 d U . . H18A H 0.0165 0.0083 0.2441 0.173 Uiso 1 1 calc R . . H18B H 0.0825 -0.0028 0.2959 0.173 Uiso 1 1 calc R . . H18C H 0.0593 -0.1562 0.2381 0.173 Uiso 1 1 calc R . . C19 C 0.3434(4) 0.5039(11) 0.1786(5) 0.040(3) Uani 1 1 d . . . H19A H 0.3045 0.4801 0.1443 0.048 Uiso 1 1 calc R . . H19B H 0.3375 0.6075 0.2088 0.048 Uiso 1 1 calc R . . C20 C 0.3908(4) 0.5426(12) 0.1344(5) 0.036(2) Uani 1 1 d . . . H20 H 0.3994 0.4606 0.0989 0.043 Uiso 1 1 calc R . . C21 C 0.4971(4) 0.8612(11) 0.1098(4) 0.026(2) Uani 1 1 d . . . C22 C 0.5461(4) 0.8930(11) 0.0730(4) 0.026(2) Uani 1 1 d . . . C23 C 0.5774(4) 1.0541(13) 0.0818(5) 0.038(2) Uani 1 1 d . . . H23 H 0.6108 1.0749 0.0577 0.045 Uiso 1 1 calc R . . C24 C 0.5588(4) 1.1781(12) 0.1252(5) 0.031(2) Uani 1 1 d . . . C25 C 0.5117(4) 1.1507(12) 0.1625(5) 0.035(2) Uani 1 1 d . . . H25 H 0.4999 1.2404 0.1927 0.042 Uiso 1 1 calc R . . C26 C 0.4824(4) 0.9953(12) 0.1561(5) 0.032(2) Uani 1 1 d . . . H26 H 0.4510 0.9762 0.1836 0.039 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 0.053(2) 0.062(2) 0.060(2) 0.0016(18) 0.0184(17) 0.0004(17) Si2 0.045(2) 0.070(2) 0.067(2) 0.0164(19) 0.0104(17) -0.0064(17) O1 0.056(4) 0.081(4) 0.061(4) 0.007(3) 0.015(3) -0.006(3) O2 0.040(4) 0.047(4) 0.056(5) 0.005(4) 0.012(4) 0.002(4) O3 0.051(4) 0.052(4) 0.057(4) 0.007(3) 0.013(3) -0.012(3) O4 0.042(4) 0.027(4) 0.065(5) -0.004(3) 0.019(4) 0.001(3) O5 0.049(4) 0.025(4) 0.040(4) -0.003(3) 0.017(3) -0.006(3) O6 0.054(4) 0.047(4) 0.062(4) -0.012(3) 0.032(4) -0.010(3) O7 0.058(4) 0.034(4) 0.076(4) 0.003(3) 0.024(4) -0.004(3) O8 0.057(5) 0.025(4) 0.056(5) -0.007(4) 0.011(4) 0.001(3) N1 0.043(5) 0.029(5) 0.035(5) -0.005(4) 0.014(4) 0.011(4) N2 0.037(5) 0.029(5) 0.034(5) 0.000(4) 0.017(4) 0.011(4) N3 0.046(6) 0.037(6) 0.032(5) 0.001(4) 0.017(4) 0.002(5) N4 0.050(6) 0.026(6) 0.059(6) -0.006(5) 0.002(5) 0.004(5) C1 0.042(7) 0.038(7) 0.072(8) -0.008(6) 0.013(6) 0.011(5) C2 0.037(6) 0.036(6) 0.056(7) -0.003(6) 0.012(5) -0.002(5) C3 0.045(6) 0.035(6) 0.044(6) 0.004(5) 0.011(5) -0.003(5) C4 0.058(5) 0.062(5) 0.063(5) 0.007(4) 0.019(4) -0.003(4) C5 0.045(4) 0.044(4) 0.044(4) 0.004(4) 0.015(4) 0.002(4) C6 0.045(4) 0.037(4) 0.040(4) -0.003(4) 0.010(4) 0.005(4) C7 0.084(5) 0.089(5) 0.097(5) 0.014(4) 0.014(4) 0.004(4) C8 0.106(7) 0.111(7) 0.134(7) 0.022(6) 0.003(6) -0.003(6) C9 0.103(8) 0.102(8) 0.114(8) 0.024(7) 0.030(7) -0.004(7) C10 0.061(8) 0.075(9) 0.085(9) -0.003(7) 0.023(7) -0.009(7) C11 0.096(8) 0.096(8) 0.075(7) -0.010(6) 0.027(6) -0.028(6) C12 0.089(7) 0.080(7) 0.081(7) -0.020(6) 0.038(6) -0.012(6) C13 0.085(6) 0.080(6) 0.091(6) 0.008(4) 0.005(4) -0.009(4) C14 0.082(8) 0.098(8) 0.108(8) 0.004(7) 0.001(7) -0.022(6) C15 0.128(9) 0.088(8) 0.096(8) 0.009(7) 0.001(7) -0.016(7) C16 0.097(5) 0.101(6) 0.095(5) 0.012(4) 0.026(4) 0.008(4) C17 0.081(7) 0.100(8) 0.106(8) 0.015(7) 0.018(7) 0.012(6) C18 0.117(7) 0.125(7) 0.114(7) 0.010(6) 0.046(6) 0.015(6) C19 0.057(7) 0.029(6) 0.042(6) -0.008(5) 0.031(6) -0.002(5) C20 0.056(7) 0.022(6) 0.034(6) -0.007(5) 0.021(5) -0.004(5) C21 0.031(5) 0.021(6) 0.024(5) 0.006(5) 0.003(5) 0.001(5) C22 0.035(5) 0.027(6) 0.020(5) 0.001(4) 0.016(4) 0.006(5) C23 0.030(6) 0.045(7) 0.037(6) 0.005(5) 0.003(5) -0.002(5) C24 0.032(6) 0.022(6) 0.037(6) 0.001(5) 0.000(5) -0.001(5) C25 0.035(6) 0.029(6) 0.044(6) -0.011(5) 0.011(5) 0.010(5) C26 0.037(6) 0.026(6) 0.039(6) -0.005(5) 0.018(5) 0.004(5) _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 O1 1.626(7) . ? Si1 O2 1.634(7) . ? Si1 C7 1.821(13) . ? Si1 C10 1.830(12) . ? Si2 O3 1.620(7) . ? Si2 O1 1.646(7) . ? Si2 C16 1.851(13) . ? Si2 C13 1.871(12) . ? O2 C1 1.400(11) . ? O3 C4 1.396(11) . ? O4 C6 1.439(10) . ? O4 C2 1.448(10) . ? O5 N3 1.234(9) . ? O6 N3 1.236(8) . ? O7 N4 1.214(9) . ? O8 N4 1.227(9) . ? N1 C20 1.273(10) . ? N1 N2 1.399(9) . ? N2 C21 1.357(10) . ? N2 H2N 0.8800 . ? N3 C22 1.439(10) . ? N4 C24 1.493(11) . ? C1 C2 1.542(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.496(11) . ? C2 H2 1.0000 . ? C3 C5 1.493(12) . ? C3 C4 1.536(12) . ? C3 H3 1.0000 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C19 1.517(12) . ? C6 H6 1.0000 . ? C7 C8 1.492(9) . ? C7 C9 1.525(15) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.510(13) . ? C10 C11 1.561(15) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.522(15) . ? C13 C14 1.556(16) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.528(16) . ? C16 C18 1.543(16) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.481(11) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20 0.9500 . ? C21 C26 1.410(11) . ? C21 C22 1.414(11) . ? C22 C23 1.413(12) . ? C23 C24 1.355(11) . ? C23 H23 0.9500 . ? C24 C25 1.376(11) . ? C25 C26 1.354(11) . ? C25 H25 0.9500 . ? C26 H26 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 O1 Si1 O2 110.8(4) . . ? O1 Si1 C7 108.5(5) . . ? O2 Si1 C7 103.2(5) . . ? O1 Si1 C10 107.3(4) . . ? O2 Si1 C10 108.8(4) . . ? C7 Si1 C10 118.2(6) . . ? O3 Si2 O1 109.2(4) . . ? O3 Si2 C16 110.7(5) . . ? O1 Si2 C16 104.7(5) . . ? O3 Si2 C13 104.4(5) . . ? O1 Si2 C13 107.4(5) . . ? C16 Si2 C13 120.2(6) . . ? Si1 O1 Si2 152.6(5) . . ? C1 O2 Si1 124.9(6) . . ? C4 O3 Si2 130.4(7) . . ? C6 O4 C2 110.0(6) . . ? C20 N1 N2 116.1(7) . . ? C21 N2 N1 118.4(7) . . ? C21 N2 H2N 120.8 . . ? N1 N2 H2N 120.8 . . ? O5 N3 O6 123.1(8) . . ? O5 N3 C22 119.0(8) . . ? O6 N3 C22 117.9(8) . . ? O7 N4 O8 123.8(8) . . ? O7 N4 C24 119.6(8) . . ? O8 N4 C24 116.5(8) . . ? O2 C1 C2 109.7(8) . . ? O2 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O2 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O4 C2 C3 106.2(7) . . ? O4 C2 C1 107.6(7) . . ? C3 C2 C1 117.0(8) . . ? O4 C2 H2 108.6 . . ? C3 C2 H2 108.6 . . ? C1 C2 H2 108.6 . . ? C5 C3 C2 102.3(7) . . ? C5 C3 C4 114.6(8) . . ? C2 C3 C4 114.4(8) . . ? C5 C3 H3 108.4 . . ? C2 C3 H3 108.4 . . ? C4 C3 H3 108.4 . . ? O3 C4 C3 113.8(8) . . ? O3 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? O3 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C3 C5 C6 104.3(7) . . ? C3 C5 H5A 110.9 . . ? C6 C5 H5A 110.9 . . ? C3 C5 H5B 110.9 . . ? C6 C5 H5B 110.9 . . ? H5A C5 H5B 108.9 . . ? O4 C6 C19 108.3(7) . . ? O4 C6 C5 104.5(7) . . ? C19 C6 C5 114.4(8) . . ? O4 C6 H6 109.8 . . ? C19 C6 H6 109.8 . . ? C5 C6 H6 109.8 . . ? C8 C7 C9 118.2(11) . . ? C8 C7 Si1 117.7(10) . . ? C9 C7 Si1 115.9(9) . . ? C8 C7 H7 99.6 . . ? C9 C7 H7 99.6 . . ? Si1 C7 H7 99.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C11 105.8(9) . . ? C12 C10 Si1 114.6(8) . . ? C11 C10 Si1 115.8(8) . . ? C12 C10 H10 106.7 . . ? C11 C10 H10 106.7 . . ? Si1 C10 H10 106.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 111.4(11) . . ? C15 C13 Si2 116.0(9) . . ? C14 C13 Si2 114.7(9) . . ? C15 C13 H13 104.4 . . ? C14 C13 H13 104.4 . . ? Si2 C13 H13 104.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 108.8(11) . . ? C17 C16 Si2 113.6(9) . . ? C18 C16 Si2 111.3(10) . . ? C17 C16 H16 107.7 . . ? C18 C16 H16 107.7 . . ? Si2 C16 H16 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C6 112.1(8) . . ? C20 C19 H19A 109.2 . . ? C6 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C6 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N1 C20 C19 119.8(8) . . ? N1 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? N2 C21 C26 120.3(8) . . ? N2 C21 C22 122.9(8) . . ? C26 C21 C22 116.8(8) . . ? C23 C22 C21 120.7(8) . . ? C23 C22 N3 116.7(8) . . ? C21 C22 N3 122.6(8) . . ? C24 C23 C22 118.5(8) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 122.3(8) . . ? C23 C24 N4 117.3(8) . . ? C25 C24 N4 120.4(9) . . ? C26 C25 C24 119.8(8) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 121.8(8) . . ? C25 C26 H26 119.1 . . ? C21 C26 H26 119.1 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.527 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.071 _vrf_THETM01_12kaw3h2 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5268 RESPONSE: The crystal does not diffract well in the higer two-theta angle even with 60 seconds per frame, which can be explained by the molecular dynamic disorder. ; _vrf_PLAT220_12kaw3h2 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.6 Ratio RESPONSE: It is due to the dynamic disorder. ; _vrf_PLAT340_12kaw3h2 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0148 Ang RESPONSE: It is due to the dynamic disorder. ; _vrf_PLAT430_12kaw3h2 ; PROBLEM: Short Inter D...A Contact O5 .. O5 .. 2.60 Ang. RESPONSE: This intermolecular distance is really short, which may be explained by the cooperative intramolecular and intermolecular hydrogen bonds from the NO2 and NH groups. ;