data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Jing Zhi Sun' _publ_contact_author_email sunjz@zju.edu.cn _publ_section_title ; ; loop_ _publ_author_name 'Ju Mei' 'Jian Wang' 'Anjun Qin' 'Hui Zhao' 'Wangzhang Yuan' 'Zujin Zhao' 'Herman Sung' 'Chunmei Dneg' 'Shuang Zhang' I.Williams 'Jing Zhi Sun' 'Ben Tang' # Attachment 'c O.cif' data_crystal_O _database_code_depnum_ccdc_archive 'CCDC 829494' #TrackingRef 'c O.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 N4 Si' _chemical_formula_weight 652.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.7917(4) _cell_length_b 10.23740(10) _cell_length_c 11.7082(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.4810(10) _cell_angle_gamma 90.00 _cell_volume 3690.61(9) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 4698 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 71.43 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.175 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.828 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6043 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 67.49 _reflns_number_total 3269 _reflns_number_gt 2964 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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 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^)+(0.0680P)^2^+1.3862P] 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 3269 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.5000 0.55696(4) 0.2500 0.02399(15) Uani 1 2 d S . . N29 N 0.23114(4) 0.38946(12) 0.34883(10) 0.0362(3) Uani 1 1 d . . . N30 N 0.17120(4) 0.65023(12) 0.09860(11) 0.0378(3) Uani 1 1 d . . . C1 C 0.51704(5) 0.65940(15) 0.12659(14) 0.0408(3) Uani 1 1 d . . . H1A H 0.5454 0.6987 0.1432 0.061 Uiso 1 1 calc R . . H1B H 0.4956 0.7286 0.1135 0.061 Uiso 1 1 calc R . . H1C H 0.5191 0.6047 0.0581 0.061 Uiso 1 1 calc R . . C10 C 0.47607(4) 0.31018(11) 0.23509(9) 0.0223(3) Uani 1 1 d . . . C11 C 0.45224(4) 0.18378(11) 0.22841(10) 0.0229(3) Uani 1 1 d . . . C12 C 0.45202(4) 0.09824(12) 0.32117(11) 0.0271(3) Uani 1 1 d . . . H12A H 0.4678 0.1199 0.3887 0.033 Uiso 1 1 calc R . . C13 C 0.42898(4) -0.01830(13) 0.31562(12) 0.0326(3) Uani 1 1 d . . . H13A H 0.4289 -0.0756 0.3795 0.039 Uiso 1 1 calc R . . C14 C 0.40615(5) -0.05138(13) 0.21761(13) 0.0365(3) Uani 1 1 d . . . H14A H 0.3905 -0.1312 0.2141 0.044 Uiso 1 1 calc R . . C15 C 0.40620(5) 0.03199(14) 0.12492(12) 0.0360(3) Uani 1 1 d . . . H15A H 0.3906 0.0094 0.0575 0.043 Uiso 1 1 calc R . . C16 C 0.42911(4) 0.14903(12) 0.13007(11) 0.0284(3) Uani 1 1 d . . . H16A H 0.4290 0.2059 0.0659 0.034 Uiso 1 1 calc R . . C20 C 0.45791(4) 0.42961(11) 0.21801(10) 0.0239(3) Uani 1 1 d . . . C21 C 0.41170(4) 0.45965(11) 0.19545(10) 0.0234(3) Uani 1 1 d . . . C22 C 0.37766(4) 0.39717(11) 0.25308(10) 0.0242(3) Uani 1 1 d . . . H22A H 0.3842 0.3294 0.3059 0.029 Uiso 1 1 calc R . . C23 C 0.33499(4) 0.43254(11) 0.23421(10) 0.0242(3) Uani 1 1 d . . . H23A H 0.3126 0.3896 0.2750 0.029 Uiso 1 1 calc R . . C24 C 0.32411(4) 0.53133(12) 0.15534(10) 0.0236(3) Uani 1 1 d . . . C25 C 0.35807(4) 0.59387(12) 0.09729(11) 0.0275(3) Uani 1 1 d . . . H25A H 0.3516 0.6604 0.0432 0.033 Uiso 1 1 calc R . . C26 C 0.40088(4) 0.55946(12) 0.11820(11) 0.0281(3) Uani 1 1 d . . . H26A H 0.4234 0.6044 0.0795 0.034 Uiso 1 1 calc R . . C27 C 0.28030(4) 0.57503(12) 0.12816(10) 0.0250(3) Uani 1 1 d . . . H27A H 0.2783 0.6352 0.0666 0.030 Uiso 1 1 calc R . . C28 C 0.24182(4) 0.54388(11) 0.17641(11) 0.0252(3) Uani 1 1 d . . . C29 C 0.23608(4) 0.45750(12) 0.27197(11) 0.0273(3) Uani 1 1 d . . . C30 C 0.20246(4) 0.60309(12) 0.13303(11) 0.0287(3) Uani 1 1 d . . . C1S C 0.22568(4) 0.26202(13) -0.00821(11) 0.0321(3) Uani 1 1 d . . . H1SA H 0.2199 0.3570 -0.0036 0.038 Uiso 1 1 calc R . . H1SB H 0.2168 0.2321 -0.0854 0.038 Uiso 1 1 calc R . . C2S C 0.19834(5) 0.19194(13) 0.08022(12) 0.0341(3) Uani 1 1 d . . . H2SA H 0.2084 0.2183 0.1574 0.041 Uiso 1 1 calc R . . H2SB H 0.2030 0.0967 0.0728 0.041 Uiso 1 1 calc R . . C3S C 0.14997(5) 0.22028(15) 0.06916(13) 0.0399(3) Uani 1 1 d . . . H3SA H 0.1342 0.1724 0.1283 0.060 Uiso 1 1 calc R . . H3SB H 0.1396 0.1925 -0.0064 0.060 Uiso 1 1 calc R . . H3SC H 0.1449 0.3142 0.0784 0.060 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 0.0222(2) 0.0193(2) 0.0303(3) 0.000 -0.00178(18) 0.000 N29 0.0336(6) 0.0348(6) 0.0403(7) 0.0034(5) 0.0032(5) -0.0018(5) N30 0.0291(6) 0.0428(7) 0.0414(7) 0.0026(5) -0.0006(5) 0.0096(5) C1 0.0376(7) 0.0367(7) 0.0481(8) 0.0142(6) -0.0051(6) -0.0116(6) C10 0.0219(6) 0.0241(6) 0.0210(5) 0.0009(4) 0.0001(4) -0.0005(5) C11 0.0210(5) 0.0210(6) 0.0267(6) 0.0006(5) 0.0022(4) 0.0011(4) C12 0.0275(6) 0.0260(6) 0.0279(6) 0.0023(5) 0.0005(5) 0.0009(5) C13 0.0379(7) 0.0250(6) 0.0348(7) 0.0063(5) 0.0074(5) -0.0009(5) C14 0.0430(8) 0.0244(6) 0.0422(8) -0.0016(5) 0.0067(6) -0.0104(6) C15 0.0418(8) 0.0335(7) 0.0329(7) -0.0037(6) -0.0022(6) -0.0110(6) C16 0.0323(6) 0.0266(6) 0.0262(6) 0.0028(5) -0.0006(5) -0.0044(5) C20 0.0228(6) 0.0235(6) 0.0254(6) 0.0016(4) 0.0003(4) -0.0013(5) C21 0.0228(6) 0.0208(6) 0.0265(6) -0.0014(4) -0.0020(5) -0.0001(4) C22 0.0261(6) 0.0218(6) 0.0247(6) 0.0020(4) -0.0015(4) 0.0009(4) C23 0.0235(6) 0.0241(6) 0.0252(6) -0.0003(4) 0.0010(4) -0.0003(4) C24 0.0235(6) 0.0224(6) 0.0249(6) -0.0032(5) -0.0020(5) 0.0018(4) C25 0.0295(6) 0.0235(6) 0.0296(6) 0.0053(5) -0.0022(5) 0.0014(5) C26 0.0251(6) 0.0261(6) 0.0332(7) 0.0061(5) 0.0015(5) -0.0017(5) C27 0.0282(6) 0.0223(6) 0.0245(6) -0.0029(4) -0.0033(5) 0.0039(5) C28 0.0252(6) 0.0234(6) 0.0269(6) -0.0046(5) -0.0043(5) 0.0034(5) C29 0.0225(6) 0.0262(6) 0.0331(7) -0.0056(5) -0.0014(5) 0.0009(5) C30 0.0269(7) 0.0284(6) 0.0307(6) -0.0033(5) 0.0004(5) 0.0040(5) C1S 0.0360(8) 0.0287(6) 0.0314(7) -0.0033(5) -0.0060(5) -0.0001(5) C2S 0.0375(7) 0.0334(7) 0.0312(7) -0.0001(5) -0.0054(5) 0.0024(6) C3S 0.0365(8) 0.0429(8) 0.0403(8) -0.0005(6) 0.0008(6) 0.0053(6) _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 C1 1.8642(14) 2_655 ? Si1 C1 1.8642(14) . ? Si1 C20 1.8739(12) . ? Si1 C20 1.8739(12) 2_655 ? N29 C29 1.1491(18) . ? N30 C30 1.1468(17) . ? C10 C20 1.3585(17) . ? C10 C11 1.4892(16) . ? C10 C10 1.512(2) 2_655 ? C11 C16 1.3949(18) . ? C11 C12 1.3953(17) . ? C12 C13 1.3894(18) . ? C13 C14 1.383(2) . ? C14 C15 1.381(2) . ? C15 C16 1.3914(18) . ? C20 C21 1.4774(16) . ? C21 C26 1.4029(17) . ? C21 C22 1.4054(17) . ? C22 C23 1.3789(17) . ? C23 C24 1.4081(17) . ? C24 C25 1.4061(17) . ? C24 C27 1.4539(16) . ? C25 C26 1.3843(18) . ? C27 C28 1.3550(18) . ? C28 C29 1.4382(18) . ? C28 C30 1.4436(17) . ? C1S C2S 1.5198(19) . ? C1S C1S 1.528(3) 7 ? C2S C3S 1.5220(19) . ? 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 C1 Si1 C1 111.54(11) 2_655 . ? C1 Si1 C20 110.34(6) 2_655 . ? C1 Si1 C20 115.79(6) . . ? C1 Si1 C20 115.79(6) 2_655 2_655 ? C1 Si1 C20 110.34(6) . 2_655 ? C20 Si1 C20 91.83(8) . 2_655 ? C20 C10 C11 124.91(10) . . ? C20 C10 C10 115.67(7) . 2_655 ? C11 C10 C10 119.41(6) . 2_655 ? C16 C11 C12 118.47(11) . . ? C16 C11 C10 120.86(11) . . ? C12 C11 C10 120.67(11) . . ? C13 C12 C11 120.55(12) . . ? C14 C13 C12 120.33(12) . . ? C15 C14 C13 119.80(12) . . ? C14 C15 C16 120.15(13) . . ? C15 C16 C11 120.70(12) . . ? C10 C20 C21 127.46(11) . . ? C10 C20 Si1 108.28(9) . . ? C21 C20 Si1 123.66(9) . . ? C26 C21 C22 117.84(11) . . ? C26 C21 C20 119.35(11) . . ? C22 C21 C20 122.72(11) . . ? C23 C22 C21 121.14(11) . . ? C22 C23 C24 120.99(11) . . ? C25 C24 C23 118.05(11) . . ? C25 C24 C27 116.52(11) . . ? C23 C24 C27 125.43(11) . . ? C26 C25 C24 120.64(11) . . ? C25 C26 C21 121.33(11) . . ? C28 C27 C24 130.49(12) . . ? C27 C28 C29 125.64(11) . . ? C27 C28 C30 119.27(12) . . ? C29 C28 C30 115.06(11) . . ? N29 C29 C28 179.21(14) . . ? N30 C30 C28 179.94(18) . . ? C2S C1S C1S 112.71(14) . 7 ? C1S C2S C3S 113.54(11) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.371 _refine_diff_density_min -0.194 _refine_diff_density_rms 0.039 # Attachment 'c R.cif' data_crystal_R _database_code_depnum_ccdc_archive 'CCDC 829495' #TrackingRef 'c R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H32 N4 O Si' _chemical_formula_weight 624.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.268(3) _cell_length_b 10.287(2) _cell_length_c 13.771(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.39(3) _cell_angle_gamma 90.00 _cell_volume 1725.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1347 _cell_measurement_theta_min 9.48 _cell_measurement_theta_max 71.36 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; 'The six largest residual electrons in the cavity was refined as a acetone molecule disordered in two positions. In order to have a reasonable thermal U(eq)s, overlapping of oxygen and carbon as two pairs, O(1S), C(1SA) and O(1SA), C(1S), which bear partial occupancies were adopted with restrains EADP and EXYZ applied. The overall occupancy for this acetone molecule is 0.5 per asymmetric unit.' ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5512 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 10.08 _diffrn_reflns_theta_max 67.50 _reflns_number_total 3033 _reflns_number_gt 1810 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _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 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^)+(0.0320P)^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 3033 _refine_ls_number_parameters 208 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.016 _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 0.0000 0.54209(11) 0.2500 0.0390(3) Uani 1 2 d S . . N1 N 0.6881(2) 0.2603(3) 0.4500(2) 0.0655(8) Uani 1 1 d . . . N2 N 0.8301(2) 0.6527(3) 0.4748(2) 0.0693(8) Uani 1 1 d . . . C1 C 0.1077(2) 0.4145(3) 0.2659(2) 0.0376(6) Uani 1 1 d . . . C2 C 0.05860(19) 0.2964(3) 0.2551(2) 0.0395(6) Uani 1 1 d . . . C10 C 0.0302(2) 0.6436(3) 0.3700(2) 0.0520(7) Uani 1 1 d . . . H10A H 0.0405 0.5873 0.4306 0.078 Uiso 1 1 calc R . . H10B H -0.0312 0.7030 0.3584 0.078 Uiso 1 1 calc R . . H10C H 0.0973 0.6940 0.3843 0.078 Uiso 1 1 calc R . . C11 C 0.22447(19) 0.4433(3) 0.2918(2) 0.0379(6) Uani 1 1 d . . . C12 C 0.3100(2) 0.3512(3) 0.3203(2) 0.0452(7) Uani 1 1 d . . . H12A H 0.2924 0.2614 0.3175 0.054 Uiso 1 1 calc R . . C13 C 0.4175(2) 0.3873(3) 0.3519(2) 0.0447(7) Uani 1 1 d . . . H13A H 0.4725 0.3219 0.3703 0.054 Uiso 1 1 calc R . . C14 C 0.4484(2) 0.5172(3) 0.3577(2) 0.0415(6) Uani 1 1 d . . . C15 C 0.3648(2) 0.6109(3) 0.3277(2) 0.0465(7) Uani 1 1 d . . . H15A H 0.3828 0.7005 0.3289 0.056 Uiso 1 1 calc R . . C16 C 0.2560(2) 0.5732(3) 0.2962(2) 0.0438(6) Uani 1 1 d . . . H16A H 0.2008 0.6385 0.2769 0.053 Uiso 1 1 calc R . . C17 C 0.5595(2) 0.5683(3) 0.3912(2) 0.0453(7) Uani 1 1 d . . . H17A H 0.5636 0.6603 0.3879 0.054 Uiso 1 1 calc R . . C18 C 0.6576(2) 0.5071(3) 0.4261(2) 0.0464(7) Uani 1 1 d . . . C19 C 0.6740(2) 0.3702(4) 0.4392(2) 0.0499(7) Uani 1 1 d . . . C20 C 0.7545(2) 0.5863(3) 0.4535(2) 0.0518(8) Uani 1 1 d . . . C21 C 0.1083(2) 0.1690(2) 0.2464(2) 0.0406(6) Uani 1 1 d . . . C22 C 0.1175(3) 0.1398(3) 0.1518(3) 0.0563(8) Uani 1 1 d . . . H22A H 0.0927 0.2007 0.0953 0.068 Uiso 1 1 calc R . . C23 C 0.1623(3) 0.0231(4) 0.1390(3) 0.0728(10) Uani 1 1 d . . . H23A H 0.1668 0.0036 0.0734 0.087 Uiso 1 1 calc R . . C24 C 0.2003(3) -0.0646(3) 0.2204(4) 0.0751(11) Uani 1 1 d . . . H24A H 0.2320 -0.1442 0.2118 0.090 Uiso 1 1 calc R . . C25 C 0.1921(3) -0.0362(3) 0.3157(3) 0.0691(10) Uani 1 1 d . . . H25A H 0.2188 -0.0964 0.3726 0.083 Uiso 1 1 calc R . . C26 C 0.1451(2) 0.0802(3) 0.3278(3) 0.0545(8) Uani 1 1 d . . . H26A H 0.1382 0.0985 0.3925 0.065 Uiso 1 1 calc R . . O1S O 0.5000 0.8412(5) 0.2500 0.1096(14) Uiso 0.64 2 d SP . . C1SA C 0.5000 0.8412(5) 0.2500 0.1096(14) Uiso 0.64 2 d SPD . . H1SA H 0.4978 0.8464 0.3180 0.164 Uiso 0.32 1 d PR . . H1SB H 0.4425 0.7727 0.2100 0.164 Uiso 0.32 1 d PR . . H1SC H 0.5698 0.7953 0.2592 0.164 Uiso 0.32 1 d PR . . C1S C 0.5000 1.0664(10) 0.2500 0.143(3) Uiso 0.36 2 d SPD . . H1SD H 0.5032 1.0542 0.3203 0.214 Uiso 0.18 1 d PR . . H1SE H 0.5671 1.1055 0.2537 0.214 Uiso 0.18 1 d PR . . H1SF H 0.4393 1.1221 0.2110 0.214 Uiso 0.18 1 d PR . . O1SA O 0.5000 1.0664(10) 0.2500 0.143(3) Uiso 0.36 2 d SP . . C2S C 0.4870(6) 0.9558(8) 0.1986(6) 0.0750(19) Uiso 0.50 1 d PD . . C3S C 0.4829(9) 0.9783(11) 0.0992(9) 0.122(3) Uiso 0.50 1 d PD . . H3SA H 0.4735 0.9003 0.0582 0.183 Uiso 0.50 1 d PR . . H3SB H 0.4226 1.0361 0.0641 0.183 Uiso 0.50 1 d PR . . H3SC H 0.5504 1.0198 0.1067 0.183 Uiso 0.50 1 d PR . . 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 0.0270(4) 0.0363(6) 0.0537(6) 0.000 0.0161(4) 0.000 N1 0.0455(15) 0.0644(19) 0.081(2) -0.0087(17) 0.0185(14) 0.0026(14) N2 0.0448(15) 0.098(2) 0.0653(17) -0.0030(17) 0.0220(13) -0.0152(16) C1 0.0327(12) 0.0369(14) 0.0451(15) -0.0001(12) 0.0176(11) 0.0037(11) C2 0.0336(13) 0.0439(16) 0.0417(14) 0.0019(12) 0.0159(11) 0.0024(12) C10 0.0331(13) 0.0536(18) 0.0688(19) -0.0126(16) 0.0197(13) -0.0048(13) C11 0.0316(12) 0.0409(15) 0.0417(13) -0.0006(13) 0.0149(10) 0.0015(12) C12 0.0363(13) 0.0385(16) 0.0588(17) -0.0019(13) 0.0168(12) 0.0011(12) C13 0.0328(13) 0.0431(16) 0.0582(17) 0.0014(14) 0.0180(12) 0.0074(12) C14 0.0316(13) 0.0495(17) 0.0445(14) 0.0025(13) 0.0164(11) 0.0003(12) C15 0.0377(14) 0.0456(17) 0.0585(17) 0.0055(14) 0.0216(13) 0.0009(13) C16 0.0340(13) 0.0406(16) 0.0576(17) 0.0066(14) 0.0190(12) 0.0034(12) C17 0.0369(13) 0.0549(19) 0.0465(14) 0.0021(14) 0.0193(12) -0.0039(13) C18 0.0341(14) 0.064(2) 0.0424(15) 0.0002(14) 0.0169(11) -0.0019(13) C19 0.0291(13) 0.070(2) 0.0494(17) -0.0084(17) 0.0142(12) -0.0002(14) C20 0.0335(14) 0.075(2) 0.0474(15) 0.0010(16) 0.0169(12) -0.0037(15) C21 0.0300(12) 0.0352(15) 0.0574(16) -0.0007(13) 0.0183(12) -0.0011(11) C22 0.0575(18) 0.0525(19) 0.0631(18) -0.0018(16) 0.0283(15) 0.0082(15) C23 0.085(3) 0.061(2) 0.084(3) -0.018(2) 0.046(2) 0.001(2) C24 0.068(2) 0.042(2) 0.130(4) -0.005(2) 0.055(2) 0.0054(17) C25 0.0546(17) 0.052(2) 0.099(3) 0.023(2) 0.0285(18) 0.0090(17) C26 0.0485(15) 0.0456(17) 0.070(2) 0.0097(16) 0.0245(15) 0.0023(14) _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 C10 1.859(3) . ? Si1 C10 1.859(3) 2 ? Si1 C1 1.888(3) 2 ? Si1 C1 1.888(3) . ? N1 C19 1.146(4) . ? N2 C20 1.151(4) . ? C1 C2 1.359(4) . ? C1 C11 1.475(3) . ? C2 C21 1.493(4) . ? C2 C2 1.505(5) 2 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.394(4) . ? C11 C12 1.409(4) . ? C12 C13 1.367(4) . ? C12 H12A 0.9500 . ? C13 C14 1.391(4) . ? C13 H13A 0.9500 . ? C14 C15 1.402(4) . ? C14 C17 1.456(4) . ? C15 C16 1.389(4) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.352(4) . ? C17 H17A 0.9500 . ? C18 C19 1.425(5) . ? C18 C20 1.440(4) . ? C21 C26 1.377(4) . ? C21 C22 1.388(4) . ? C22 C23 1.382(4) . ? C22 H22A 0.9500 . ? C23 C24 1.369(5) . ? C23 H23A 0.9500 . ? C24 C25 1.389(5) . ? C24 H24A 0.9500 . ? C25 C26 1.391(4) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? O1S C2S 1.350(8) . ? O1S C2S 1.350(8) 2_655 ? O1S H1SA 0.9497 . ? O1S H1SB 1.0236 . ? O1S H1SC 1.0016 . ? C1S C2S 1.315(9) . ? C1S C2S 1.315(9) 2_655 ? C1S H1SD 0.9600 . ? C1S H1SE 0.9599 . ? C1S H1SF 0.9600 . ? C2S C2S 1.318(15) 2_655 ? C2S C3S 1.368(11) . ? C3S H3SA 0.9600 . ? C3S H3SB 0.9600 . ? C3S H3SC 0.9600 . ? 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 C10 Si1 C10 111.6(2) . 2 ? C10 Si1 C1 112.32(11) . 2 ? C10 Si1 C1 113.65(12) 2 2 ? C10 Si1 C1 113.65(12) . . ? C10 Si1 C1 112.32(11) 2 . ? C1 Si1 C1 91.93(16) 2 . ? C2 C1 C11 128.2(2) . . ? C2 C1 Si1 107.50(17) . . ? C11 C1 Si1 124.2(2) . . ? C1 C2 C21 125.8(2) . . ? C1 C2 C2 116.31(14) . 2 ? C21 C2 C2 117.75(13) . 2 ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 116.0(2) . . ? C16 C11 C1 118.1(2) . . ? C12 C11 C1 125.8(2) . . ? C13 C12 C11 121.9(3) . . ? C13 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? C12 C13 C14 121.7(3) . . ? C12 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? C13 C14 C15 117.6(2) . . ? C13 C14 C17 127.1(3) . . ? C15 C14 C17 115.3(3) . . ? C16 C15 C14 120.2(3) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C11 122.5(3) . . ? C15 C16 H16A 118.7 . . ? C11 C16 H16A 118.7 . . ? C18 C17 C14 131.0(3) . . ? C18 C17 H17A 114.5 . . ? C14 C17 H17A 114.5 . . ? C17 C18 C19 125.6(3) . . ? C17 C18 C20 117.6(3) . . ? C19 C18 C20 116.8(3) . . ? N1 C19 C18 179.4(3) . . ? N2 C20 C18 178.1(4) . . ? C26 C21 C22 119.1(3) . . ? C26 C21 C2 122.8(3) . . ? C22 C21 C2 118.1(3) . . ? C23 C22 C21 120.7(3) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C21 C26 C25 120.3(3) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C2S O1S C2S 58.4(7) . 2_655 ? C2S O1S H1SA 114.8 . . ? C2S O1S H1SA 58.7 2_655 . ? C2S O1S H1SB 113.9 . . ? C2S O1S H1SB 142.7 2_655 . ? H1SA O1S H1SB 105.1 . . ? C2S O1S H1SC 113.4 . . ? C2S O1S H1SC 115.2 2_655 . ? H1SA O1S H1SC 106.9 . . ? H1SB O1S H1SC 101.4 . . ? C2S C1S C2S 60.1(8) . 2_655 ? C2S C1S H1SD 111.9 . . ? C2S C1S H1SD 53.1 2_655 . ? C2S C1S H1SE 108.2 . . ? C2S C1S H1SE 114.5 2_655 . ? H1SD C1S H1SE 109.5 . . ? C2S C1S H1SF 108.3 . . ? C2S C1S H1SF 136.0 2_655 . ? H1SD C1S H1SF 109.5 . . ? H1SE C1S H1SF 109.5 . . ? C1S C2S C2S 59.9(4) . 2_655 ? C1S C2S O1S 120.7(7) . . ? C2S C2S O1S 60.8(4) 2_655 . ? C1S C2S C3S 109.7(7) . . ? C2S C2S C3S 164.8(9) 2_655 . ? O1S C2S C3S 128.2(8) . . ? C2S C3S H3SA 113.1 . . ? C2S C3S H3SB 107.6 . . ? H3SA C3S H3SB 109.5 . . ? C2S C3S H3SC 107.7 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Si1 C1 C2 117.5(2) . . . . ? C10 Si1 C1 C2 -114.5(2) 2 . . . ? C1 Si1 C1 C2 2.09(13) 2 . . . ? C10 Si1 C1 C11 -59.1(3) . . . . ? C10 Si1 C1 C11 68.8(2) 2 . . . ? C1 Si1 C1 C11 -174.5(3) 2 . . . ? C11 C1 C2 C21 -12.9(5) . . . . ? Si1 C1 C2 C21 170.7(2) . . . . ? C11 C1 C2 C2 170.8(3) . . . 2 ? Si1 C1 C2 C2 -5.6(4) . . . 2 ? C2 C1 C11 C16 178.4(3) . . . . ? Si1 C1 C11 C16 -5.7(3) . . . . ? C2 C1 C11 C12 -6.4(4) . . . . ? Si1 C1 C11 C12 169.6(2) . . . . ? C16 C11 C12 C13 1.0(4) . . . . ? C1 C11 C12 C13 -174.3(3) . . . . ? C11 C12 C13 C14 0.1(4) . . . . ? C12 C13 C14 C15 -1.4(4) . . . . ? C12 C13 C14 C17 179.2(3) . . . . ? C13 C14 C15 C16 1.7(4) . . . . ? C17 C14 C15 C16 -178.8(3) . . . . ? C14 C15 C16 C11 -0.6(5) . . . . ? C12 C11 C16 C15 -0.7(4) . . . . ? C1 C11 C16 C15 175.0(3) . . . . ? C13 C14 C17 C18 -1.6(5) . . . . ? C15 C14 C17 C18 178.9(3) . . . . ? C14 C17 C18 C19 -0.7(5) . . . . ? C14 C17 C18 C20 180.0(3) . . . . ? C17 C18 C19 N1 175(100) . . . . ? C20 C18 C19 N1 -6(32) . . . . ? C17 C18 C20 N2 2(10) . . . . ? C19 C18 C20 N2 -177(100) . . . . ? C1 C2 C21 C26 106.0(3) . . . . ? C2 C2 C21 C26 -77.8(4) 2 . . . ? C1 C2 C21 C22 -74.0(4) . . . . ? C2 C2 C21 C22 102.2(3) 2 . . . ? C26 C21 C22 C23 0.3(4) . . . . ? C2 C21 C22 C23 -179.7(3) . . . . ? C21 C22 C23 C24 -1.2(5) . . . . ? C22 C23 C24 C25 0.9(6) . . . . ? C23 C24 C25 C26 0.4(5) . . . . ? C22 C21 C26 C25 0.9(4) . . . . ? C2 C21 C26 C25 -179.1(3) . . . . ? C24 C25 C26 C21 -1.3(5) . . . . ? C2S C1S C2S O1S 0.000(3) 2_655 . . . ? C2S C1S C2S C3S -167.7(11) 2_655 . . . ? C2S O1S C2S C1S 0.000(3) 2_655 . . . ? C2S O1S C2S C3S 165.2(14) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.472 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.043