# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Daofeng Sun' _publ_contact_author_email DFSUN@SDU.EDU.CN _publ_section_title ; A 3D Porous Metal-Organic Framework Constructed of 1D Zigzag and Helical Chains Exhibiting Selective Anion Exchange ; loop_ _publ_author_name 'Daofeng Sun' 'Xiaohui Chen' 'Shengyu Feng' 'Haiyan He' 'Yuzhong Niu' ; Dengxu Wang ; # Attachment '1.cif' data_ag _database_code_depnum_ccdc_archive 'CCDC 734767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H60 Ag2.50 Cl2.50 N10 O15 Si2.50' _chemical_formula_weight 1469.60 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 24.328(5) _cell_length_b 31.067(6) _cell_length_c 16.658(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12590(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3503 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 15.71 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5960 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8257 _exptl_absorpt_correction_T_max 0.9070 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _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 40172 _diffrn_reflns_av_R_equivalents 0.0930 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 20.86 _reflns_number_total 6620 _reflns_number_gt 3291 _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^)+(0.1371P)^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 6620 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1376 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.2443 _refine_ls_wR_factor_gt 0.2095 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.067 _refine_ls_shift/su_mean 0.003 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 O1 O 0.1802(7) 0.3192(4) 0.4567(15) 0.284(11) Uani 1 1 d . . . O01 O 0.1315(15) 0.3658(12) 0.245(2) 0.130(12) Uiso 0.25 1 d P . . O2 O 0.1564(14) 0.2766(10) 0.5519(18) 0.35(2) Uani 1 1 d . . . O3 O 0.2336(7) 0.2655(5) 0.5087(14) 0.274(11) Uani 1 1 d . . . O4 O 0.1559(7) 0.2493(4) 0.4367(10) 0.227(7) Uani 1 1 d . . . O5 O 0.0603(15) 0.5146(11) 0.7016(14) 0.43(2) Uani 1 1 d . . . O6 O -0.0017(6) 0.5656(5) 0.7097(12) 0.242(8) Uani 1 1 d . . . O7 O -0.0110(13) 0.4990(10) 0.7690(19) 0.41(2) Uani 1 1 d . . . O8 O 0.0451(9) 0.5438(6) 0.8199(11) 0.287(11) Uani 1 1 d . . . O9 O 0.2172(11) 0.4758(6) 0.7314(16) 0.326(13) Uani 1 1 d . . . O10 O 0.2191(10) 0.5274(6) 0.8243(14) 0.331(13) Uani 1 1 d . . . Ag1 Ag 0.17233(4) 0.38233(3) 0.61738(7) 0.1121(5) Uani 1 1 d . . . Ag2 Ag -0.25524(5) 0.56943(5) 0.00443(10) 0.1510(7) Uani 1 1 d . . . Ag3 Ag 0.2500 0.5000 0.54854(12) 0.1218(7) Uani 1 2 d S . . Si1 Si 0.02034(17) 0.65969(12) 0.4128(3) 0.1063(13) Uani 1 1 d . . . Si2 Si -0.5595(3) 0.36118(18) 0.0725(4) 0.163(2) Uani 1 1 d . . . Si3 Si 0.0286(2) 0.7500 0.7500 0.120(2) Uani 1 2 d S . . N1 N 0.1324(4) 0.4215(4) 0.5356(8) 0.101(3) Uani 1 1 d . . . N2 N 0.1008(4) 0.4783(4) 0.4738(8) 0.094(3) Uani 1 1 d . . . N3 N -0.1315(5) 0.6364(4) 0.1288(8) 0.091(3) Uani 1 1 d . . . N4 N -0.1926(5) 0.6105(5) 0.0450(10) 0.115(4) Uani 1 1 d . . . N5 N -0.3154(7) 0.5294(5) -0.0416(15) 0.171(8) Uani 1 1 d . . . N6 N -0.3821(7) 0.4834(5) -0.0401(12) 0.130(4) Uani 1 1 d . . . N7 N -0.7255(4) 0.3394(4) -0.1923(7) 0.078(3) Uani 1 1 d . . . N8 N -0.7792(4) 0.3519(4) -0.2935(7) 0.087(3) Uani 1 1 d . . . N9 N 0.2139(6) 0.5609(4) 0.5431(11) 0.109(4) Uani 1 1 d . . . N10 N 0.1716(5) 0.6220(4) 0.5733(8) 0.092(3) Uani 1 1 d . . . C1 C 0.1166(5) 0.4617(5) 0.5427(9) 0.095(4) Uani 1 1 d . . . H1 H 0.1165 0.4768 0.5909 0.114 Uiso 1 1 calc R . . C2 C 0.1278(5) 0.4123(5) 0.4531(14) 0.117(5) Uani 1 1 d . . . H2 H 0.1363 0.3861 0.4289 0.141 Uiso 1 1 calc R . . C3 C 0.1091(6) 0.4477(6) 0.4151(10) 0.116(5) Uani 1 1 d . . . H3 H 0.1030 0.4509 0.3603 0.139 Uiso 1 1 calc R . . C4 C 0.0814(6) 0.5216(5) 0.4656(10) 0.082(4) Uani 1 1 d . . . C5 C 0.0457(6) 0.5399(5) 0.5169(8) 0.089(4) Uani 1 1 d . . . H5 H 0.0322 0.5245 0.5605 0.107 Uiso 1 1 calc R . . C6 C 0.0298(5) 0.5812(5) 0.5039(9) 0.094(4) Uani 1 1 d . . . H6 H 0.0067 0.5942 0.5412 0.113 Uiso 1 1 calc R . . C7 C 0.0463(6) 0.6046(4) 0.4381(9) 0.087(4) Uani 1 1 d . . . C8 C 0.0838(6) 0.5853(5) 0.3869(9) 0.114(5) Uani 1 1 d . . . H8 H 0.0973 0.6004 0.3431 0.136 Uiso 1 1 calc R . . C9 C 0.1015(6) 0.5428(5) 0.4009(10) 0.122(5) Uani 1 1 d . . . H9 H 0.1264 0.5295 0.3665 0.146 Uiso 1 1 calc R . . C10 C 0.0759(6) 0.6950(4) 0.3804(10) 0.146(6) Uani 1 1 d . . . H10A H 0.0947 0.6822 0.3358 0.219 Uiso 1 1 calc R . . H10B H 0.1012 0.6992 0.4239 0.219 Uiso 1 1 calc R . . H10C H 0.0609 0.7223 0.3644 0.219 Uiso 1 1 calc R . . C11 C -0.0146(7) 0.6849(5) 0.4965(8) 0.136(6) Uani 1 1 d . . . H11A H 0.0107 0.6885 0.5402 0.203 Uiso 1 1 calc R . . H11B H -0.0447 0.6671 0.5133 0.203 Uiso 1 1 calc R . . H11C H -0.0284 0.7125 0.4802 0.203 Uiso 1 1 calc R . . C12 C -0.0281(5) 0.6528(5) 0.3285(8) 0.087(4) Uani 1 1 d . . . C13 C -0.0523(5) 0.6856(4) 0.2891(10) 0.098(4) Uani 1 1 d . . . H13 H -0.0451 0.7132 0.3079 0.117 Uiso 1 1 calc R . . C14 C -0.0853(6) 0.6822(4) 0.2259(9) 0.090(4) Uani 1 1 d . . . H14 H -0.0999 0.7065 0.2011 0.108 Uiso 1 1 calc R . . C15 C -0.0971(5) 0.6412(5) 0.1984(8) 0.084(4) Uani 1 1 d . . . C16 C -0.0740(5) 0.6068(4) 0.2352(10) 0.090(4) Uani 1 1 d . . . H16 H -0.0814 0.5792 0.2165 0.108 Uiso 1 1 calc R . . C17 C -0.0395(6) 0.6124(4) 0.3002(9) 0.096(4) Uani 1 1 d . . . H17 H -0.0238 0.5885 0.3250 0.115 Uiso 1 1 calc R . . C18 C -0.1655(7) 0.6041(5) 0.1094(11) 0.097(4) Uani 1 1 d . . . H18 H -0.1689 0.5792 0.1401 0.116 Uiso 1 1 calc R . . C19 C -0.1400(6) 0.6658(5) 0.0680(13) 0.113(5) Uani 1 1 d . . . H19 H -0.1233 0.6926 0.0639 0.136 Uiso 1 1 calc R . . C20 C -0.1766(7) 0.6494(6) 0.0153(12) 0.124(6) Uani 1 1 d . . . H20 H -0.1885 0.6621 -0.0321 0.149 Uiso 1 1 calc R . . C21 C -0.3483(9) 0.5093(6) 0.0007(11) 0.132(6) Uani 1 1 d . . . H21 H -0.3495 0.5120 0.0563 0.158 Uiso 1 1 calc R . . C22 C -0.3275(12) 0.5136(10) -0.1170(13) 0.213(12) Uani 1 1 d . . . H22 H -0.3092 0.5218 -0.1635 0.255 Uiso 1 1 calc R . . C23 C -0.3681(10) 0.4855(8) -0.1158(18) 0.205(11) Uani 1 1 d . . . H23 H -0.3832 0.4705 -0.1588 0.246 Uiso 1 1 calc R . . C24 C -0.4261(10) 0.4571(6) -0.0112(15) 0.127(7) Uani 1 1 d . . . C25 C -0.4318(8) 0.4187(9) -0.0513(12) 0.151(7) Uani 1 1 d . . . H25 H -0.4095 0.4116 -0.0946 0.182 Uiso 1 1 calc R . . C26 C -0.4732(10) 0.3905(6) -0.0236(15) 0.136(6) Uani 1 1 d . . . H26 H -0.4783 0.3647 -0.0507 0.163 Uiso 1 1 calc R . . C27 C -0.5065(7) 0.3993(7) 0.0416(13) 0.122(6) Uani 1 1 d . . . C28 C -0.4986(7) 0.4387(6) 0.0745(11) 0.125(6) Uani 1 1 d . . . H28 H -0.5215 0.4468 0.1166 0.150 Uiso 1 1 calc R . . C29 C -0.4600(9) 0.4667(6) 0.0504(12) 0.124(6) Uani 1 1 d . . . H29 H -0.4565 0.4930 0.0764 0.149 Uiso 1 1 calc R . . C30 C -0.5891(11) 0.3772(9) 0.1638(12) 0.299(19) Uani 1 1 d . . . H30A H -0.6169 0.3568 0.1792 0.449 Uiso 1 1 calc R . . H30B H -0.6055 0.4051 0.1577 0.449 Uiso 1 1 calc R . . H30C H -0.5613 0.3784 0.2046 0.449 Uiso 1 1 calc R . . C31 C -0.5252(9) 0.3055(6) 0.0824(15) 0.238(13) Uani 1 1 d . . . H31A H -0.5089 0.2976 0.0321 0.357 Uiso 1 1 calc R . . H31B H -0.5523 0.2845 0.0971 0.357 Uiso 1 1 calc R . . H31C H -0.4972 0.3066 0.1231 0.357 Uiso 1 1 calc R . . C32 C -0.6124(6) 0.3582(5) -0.0085(10) 0.112(4) Uani 1 1 d . . . C33 C -0.6133(7) 0.3827(4) -0.0791(11) 0.116(5) Uani 1 1 d . . . H33 H -0.5865 0.4038 -0.0861 0.139 Uiso 1 1 calc R . . C34 C -0.6507(6) 0.3773(4) -0.1368(9) 0.095(4) Uani 1 1 d . . . H34 H -0.6510 0.3953 -0.1814 0.114 Uiso 1 1 calc R . . C35 C -0.6881(5) 0.3457(4) -0.1298(8) 0.081(3) Uani 1 1 d . . . C36 C -0.6904(5) 0.3198(4) -0.0618(9) 0.089(4) Uani 1 1 d . . . H36 H -0.7173 0.2988 -0.0561 0.106 Uiso 1 1 calc R . . C37 C -0.6529(6) 0.3262(5) -0.0053(9) 0.118(5) Uani 1 1 d . . . H37 H -0.6535 0.3083 0.0394 0.142 Uiso 1 1 calc R . . C38 C -0.7451(5) 0.3683(5) -0.2436(9) 0.083(4) Uani 1 1 d . . . H38 H -0.7351 0.3972 -0.2433 0.099 Uiso 1 1 calc R . . C39 C -0.7809(6) 0.3083(5) -0.2765(10) 0.107(4) Uani 1 1 d . . . H39 H -0.8012 0.2874 -0.3034 0.129 Uiso 1 1 calc R . . C40 C -0.7465(6) 0.3018(5) -0.2120(9) 0.100(4) Uani 1 1 d . . . H40 H -0.7394 0.2756 -0.1870 0.120 Uiso 1 1 calc R . . C41 C 0.1798(6) 0.5817(7) 0.5917(10) 0.105(5) Uani 1 1 d . . . H41 H 0.1630 0.5686 0.6355 0.126 Uiso 1 1 calc R . . C42 C 0.2270(6) 0.5896(8) 0.4893(13) 0.132(6) Uani 1 1 d . . . H42 H 0.2495 0.5843 0.4453 0.159 Uiso 1 1 calc R . . C43 C 0.2026(7) 0.6294(5) 0.5066(12) 0.106(4) Uani 1 1 d . . . H43 H 0.2067 0.6552 0.4787 0.127 Uiso 1 1 calc R . . C44 C 0.1385(6) 0.6521(5) 0.6160(9) 0.089(4) Uani 1 1 d . . . C45 C 0.1518(6) 0.6946(6) 0.6107(9) 0.106(5) Uani 1 1 d . . . H45 H 0.1821 0.7036 0.5811 0.127 Uiso 1 1 calc R . . C46 C 0.1215(6) 0.7221(5) 0.6475(10) 0.109(5) Uani 1 1 d . . . H46 H 0.1301 0.7511 0.6422 0.131 Uiso 1 1 calc R . . C47 C 0.0764(7) 0.7112(5) 0.6950(9) 0.108(5) Uani 1 1 d . . . C48 C 0.0646(5) 0.6659(6) 0.7009(8) 0.104(4) Uani 1 1 d . . . H48 H 0.0356 0.6561 0.7324 0.125 Uiso 1 1 calc R . . C49 C 0.0967(7) 0.6375(4) 0.6594(9) 0.098(4) Uani 1 1 d . . . H49 H 0.0893 0.6081 0.6616 0.118 Uiso 1 1 calc R . . C50 C -0.0142(7) 0.7224(5) 0.8310(12) 0.176(8) Uani 1 1 d . . . H50A H -0.0393 0.7025 0.8063 0.265 Uiso 1 1 calc R . . H50B H -0.0346 0.7436 0.8604 0.265 Uiso 1 1 calc R . . H50C H 0.0096 0.7071 0.8670 0.265 Uiso 1 1 calc R . . Cl1 Cl 0.1824(3) 0.2771(2) 0.4860(5) 0.180(3) Uani 1 1 d . . . Cl2 Cl 0.0233(3) 0.53124(19) 0.7505(3) 0.1543(18) Uani 1 1 d . . . Cl3 Cl 0.2500 0.5000 0.7785(5) 0.155(3) Uani 1 2 d S . . 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 O1 0.263(17) 0.084(9) 0.51(3) 0.066(13) -0.121(19) 0.028(9) O2 0.38(4) 0.34(3) 0.32(3) -0.15(3) -0.17(3) 0.05(3) O3 0.190(13) 0.162(12) 0.47(3) -0.003(14) -0.135(17) 0.075(11) O4 0.292(17) 0.160(11) 0.228(16) -0.039(11) -0.122(14) -0.048(11) O5 0.60(5) 0.50(4) 0.20(2) 0.04(2) 0.12(3) 0.30(4) O6 0.212(15) 0.192(14) 0.32(2) 0.078(14) -0.075(14) 0.009(11) O7 0.43(4) 0.38(3) 0.43(4) 0.08(3) -0.08(3) -0.25(3) O8 0.46(3) 0.245(17) 0.158(14) -0.033(13) -0.122(17) -0.038(17) O9 0.39(3) 0.203(18) 0.39(3) -0.009(18) -0.15(2) -0.057(17) O10 0.40(3) 0.239(18) 0.35(3) -0.134(18) 0.20(2) 0.010(17) Ag1 0.0986(8) 0.1181(9) 0.1194(10) 0.0323(7) -0.0124(7) 0.0176(6) Ag2 0.1294(11) 0.1685(13) 0.1550(14) -0.0234(10) -0.0289(9) -0.0262(9) Ag3 0.1073(12) 0.1010(12) 0.1571(17) 0.000 0.000 0.0191(9) Si1 0.128(3) 0.080(2) 0.110(3) -0.012(2) -0.026(3) 0.011(2) Si2 0.202(5) 0.160(4) 0.127(5) 0.057(4) -0.068(4) -0.056(4) Si3 0.101(4) 0.114(4) 0.147(6) -0.040(4) 0.000 0.000 N1 0.099(8) 0.114(11) 0.091(10) 0.006(8) -0.016(7) 0.013(7) N2 0.096(8) 0.103(9) 0.084(9) 0.018(8) -0.018(7) 0.030(7) N3 0.097(9) 0.078(8) 0.099(10) 0.006(8) 0.024(8) 0.009(8) N4 0.089(8) 0.168(15) 0.088(10) -0.013(9) -0.016(8) 0.002(8) N5 0.150(13) 0.145(13) 0.22(2) 0.025(14) 0.010(14) -0.050(10) N6 0.145(13) 0.142(12) 0.104(13) 0.010(10) -0.013(11) -0.024(11) N7 0.095(7) 0.056(7) 0.082(8) 0.014(7) 0.002(7) -0.007(6) N8 0.071(7) 0.088(9) 0.101(9) 0.014(7) 0.006(7) 0.011(6) N9 0.120(11) 0.088(9) 0.118(12) 0.008(9) -0.026(9) 0.005(8) N10 0.091(8) 0.075(10) 0.112(11) 0.010(8) -0.024(8) 0.003(7) C1 0.106(10) 0.078(10) 0.102(13) 0.013(9) -0.021(9) 0.013(8) C2 0.096(10) 0.076(10) 0.18(2) 0.025(12) -0.014(11) 0.022(8) C3 0.140(13) 0.116(12) 0.092(12) -0.018(11) -0.012(10) 0.021(10) C4 0.090(9) 0.089(11) 0.068(10) 0.002(9) -0.029(8) -0.002(9) C5 0.113(11) 0.088(11) 0.065(9) 0.000(8) 0.008(8) 0.005(8) C6 0.107(10) 0.097(12) 0.078(11) -0.009(9) -0.012(8) 0.009(9) C7 0.102(10) 0.080(9) 0.080(10) -0.002(9) -0.018(8) 0.019(8) C8 0.129(12) 0.106(12) 0.107(12) 0.021(10) 0.003(10) 0.027(9) C9 0.146(13) 0.121(13) 0.099(13) 0.012(11) 0.012(11) 0.056(10) C10 0.150(14) 0.111(11) 0.177(17) 0.018(11) -0.016(12) -0.011(10) C11 0.196(16) 0.109(11) 0.102(12) -0.026(9) -0.031(11) 0.026(10) C12 0.102(9) 0.067(9) 0.092(10) 0.009(8) -0.003(8) 0.010(8) C13 0.097(10) 0.072(10) 0.125(13) -0.016(9) -0.035(9) 0.016(8) C14 0.103(10) 0.058(9) 0.111(12) -0.011(8) -0.006(9) 0.019(7) C15 0.064(8) 0.121(13) 0.066(10) -0.011(9) -0.006(7) -0.004(8) C16 0.088(9) 0.072(9) 0.108(12) 0.002(9) 0.004(9) 0.024(7) C17 0.119(11) 0.081(11) 0.088(11) 0.006(8) -0.015(9) 0.002(8) C18 0.097(11) 0.088(11) 0.105(14) -0.012(9) 0.013(10) 0.003(9) C19 0.086(11) 0.116(13) 0.137(15) -0.016(13) -0.004(10) -0.003(9) C20 0.103(12) 0.121(13) 0.149(17) 0.038(13) 0.002(12) -0.005(10) C21 0.156(16) 0.135(14) 0.105(14) -0.025(12) -0.075(14) -0.040(12) C22 0.21(2) 0.35(4) 0.085(15) -0.067(19) 0.025(16) -0.07(2) C23 0.168(19) 0.31(3) 0.14(2) -0.016(19) -0.034(17) -0.139(19) C24 0.17(2) 0.081(12) 0.128(18) -0.023(12) -0.070(16) -0.017(12) C25 0.108(14) 0.21(2) 0.133(16) 0.014(18) -0.040(12) -0.007(15) C26 0.125(16) 0.111(14) 0.17(2) -0.010(13) -0.037(14) 0.007(13) C27 0.104(13) 0.129(16) 0.133(16) 0.031(12) -0.049(12) -0.037(11) C28 0.126(13) 0.100(13) 0.148(16) 0.008(12) -0.024(12) -0.037(10) C29 0.153(16) 0.128(17) 0.091(14) -0.022(12) -0.031(12) 0.041(15) C30 0.38(4) 0.44(4) 0.080(15) 0.059(19) -0.042(19) -0.27(3) C31 0.22(2) 0.179(18) 0.32(3) 0.14(2) -0.13(2) -0.043(16) C32 0.110(11) 0.112(10) 0.115(13) 0.020(10) -0.017(9) -0.039(9) C33 0.137(14) 0.102(11) 0.108(13) 0.038(10) 0.001(11) -0.028(9) C34 0.084(9) 0.095(10) 0.106(13) 0.022(8) -0.015(9) -0.018(8) C35 0.082(9) 0.095(10) 0.066(10) 0.002(8) -0.021(8) -0.002(8) C36 0.092(9) 0.101(10) 0.073(10) 0.020(9) -0.015(8) -0.009(7) C37 0.111(11) 0.157(14) 0.086(11) 0.061(10) -0.019(10) -0.019(11) C38 0.072(8) 0.091(10) 0.085(10) 0.005(9) -0.013(7) -0.018(8) C39 0.113(11) 0.077(11) 0.133(14) 0.001(9) -0.010(10) -0.026(8) C40 0.106(10) 0.088(12) 0.105(12) 0.016(9) -0.036(9) 0.011(9) C41 0.089(10) 0.114(14) 0.111(13) -0.022(12) -0.013(9) 0.003(9) C42 0.084(10) 0.155(17) 0.158(19) -0.042(16) -0.024(11) 0.037(12) C43 0.091(10) 0.103(13) 0.124(14) 0.017(10) -0.005(10) 0.003(9) C44 0.059(9) 0.091(12) 0.119(12) -0.045(10) -0.018(8) 0.005(9) C45 0.077(9) 0.102(13) 0.138(13) -0.047(10) 0.011(8) 0.005(9) C46 0.088(10) 0.117(13) 0.122(13) -0.002(10) 0.021(10) -0.035(10) C47 0.126(13) 0.086(11) 0.111(13) -0.026(9) -0.036(11) 0.021(9) C48 0.090(9) 0.131(14) 0.092(11) -0.010(10) 0.017(8) 0.004(10) C49 0.090(10) 0.089(10) 0.116(12) -0.020(9) 0.001(9) -0.010(9) C50 0.151(14) 0.162(15) 0.22(2) -0.055(14) 0.066(14) -0.038(11) Cl1 0.203(7) 0.107(4) 0.230(8) -0.013(5) -0.101(6) 0.032(4) Cl2 0.224(6) 0.132(4) 0.107(4) 0.003(3) 0.008(4) -0.039(4) Cl3 0.216(8) 0.106(5) 0.144(7) 0.000 0.000 -0.006(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 O1 Cl1 1.396(15) . ? O2 Cl1 1.27(3) . ? O3 Cl1 1.350(16) . ? O4 Cl1 1.356(13) . ? O5 Cl2 1.32(2) . ? O6 Cl2 1.402(14) . ? O7 Cl2 1.34(2) . ? O8 Cl2 1.330(15) . ? O9 Cl3 1.35(2) . ? O10 Cl3 1.368(15) . ? Ag1 N1 2.069(12) . ? Ag1 N8 2.118(10) 1_656 ? Ag2 N5 2.067(18) . ? Ag2 N4 2.098(13) . ? Ag3 N9 2.088(13) . ? Ag3 N9 2.088(13) 2_565 ? Si1 C11 1.811(14) . ? Si1 C10 1.823(15) . ? Si1 C12 1.845(13) . ? Si1 C7 1.871(13) . ? Si2 C30 1.76(3) . ? Si2 C27 1.825(17) . ? Si2 C32 1.868(15) . ? Si2 C31 1.93(2) . ? Si3 C47 1.909(15) 4_566 ? Si3 C47 1.909(15) . ? Si3 C50 1.909(17) 4_566 ? Si3 C50 1.909(17) . ? N1 C1 1.314(14) . ? N1 C2 1.408(18) . ? N2 C1 1.314(15) . ? N2 C3 1.378(16) . ? N2 C4 1.434(16) . ? N3 C18 1.340(16) . ? N3 C19 1.379(18) . ? N3 C15 1.438(15) . ? N4 C18 1.275(16) . ? N4 C20 1.363(17) . ? N5 C21 1.24(2) . ? N5 C22 1.38(2) . ? N6 C23 1.31(2) . ? N6 C21 1.336(19) . ? N6 C24 1.43(2) . ? N7 C40 1.316(15) . ? N7 C38 1.328(14) . ? N7 C35 1.397(14) . ? N8 C38 1.281(13) . ? N8 C39 1.386(14) . ? N8 Ag1 2.118(10) 1_454 ? N9 C42 1.30(2) . ? N9 C41 1.328(17) . ? N10 C41 1.304(18) . ? N10 C43 1.362(17) . ? N10 C44 1.423(16) . ? C2 C3 1.348(17) . ? C4 C5 1.344(16) . ? C4 C9 1.354(17) . ? C5 C6 1.356(16) . ? C6 C7 1.377(16) . ? C7 C8 1.386(17) . ? C8 C9 1.408(17) . ? C12 C13 1.347(15) . ? C12 C17 1.370(15) . ? C13 C14 1.329(16) . ? C14 C15 1.383(16) . ? C15 C16 1.355(16) . ? C16 C17 1.381(17) . ? C19 C20 1.349(19) . ? C21 C22 2.03(3) . ? C22 C23 1.32(3) . ? C24 C29 1.35(2) . ? C24 C25 1.37(2) . ? C25 C26 1.41(2) . ? C26 C27 1.38(2) . ? C27 C28 1.35(2) . ? C28 C29 1.34(2) . ? C32 C37 1.399(17) . ? C32 C33 1.402(18) . ? C33 C34 1.334(17) . ? C34 C35 1.343(16) . ? C35 C36 1.391(16) . ? C36 C37 1.326(16) . ? C39 C40 1.376(17) . ? C42 C43 1.403(19) . ? C44 C49 1.329(17) . ? C44 C45 1.363(17) . ? C45 C46 1.283(17) . ? C46 C47 1.392(18) . ? C47 C48 1.440(18) . ? C48 C49 1.365(16) . ? Cl3 O9 1.35(2) 2_565 ? Cl3 O10 1.368(15) 2_565 ? 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 Ag1 N8 170.2(5) . 1_656 ? N5 Ag2 N4 177.0(8) . . ? N9 Ag3 N9 175.0(10) . 2_565 ? C11 Si1 C10 108.4(8) . . ? C11 Si1 C12 109.6(7) . . ? C10 Si1 C12 108.5(7) . . ? C11 Si1 C7 112.4(7) . . ? C10 Si1 C7 111.6(7) . . ? C12 Si1 C7 106.3(6) . . ? C30 Si2 C27 110.6(11) . . ? C30 Si2 C32 111.0(10) . . ? C27 Si2 C32 108.4(7) . . ? C30 Si2 C31 111.0(12) . . ? C27 Si2 C31 107.4(10) . . ? C32 Si2 C31 108.4(8) . . ? C47 Si3 C47 105.0(10) 4_566 . ? C47 Si3 C50 112.8(8) 4_566 4_566 ? C47 Si3 C50 106.1(7) . 4_566 ? C47 Si3 C50 106.1(7) 4_566 . ? C47 Si3 C50 112.8(8) . . ? C50 Si3 C50 113.8(13) 4_566 . ? C1 N1 C2 105.0(12) . . ? C1 N1 Ag1 129.6(12) . . ? C2 N1 Ag1 124.1(11) . . ? C1 N2 C3 107.9(12) . . ? C1 N2 C4 123.1(14) . . ? C3 N2 C4 128.9(14) . . ? C18 N3 C19 103.1(13) . . ? C18 N3 C15 129.1(15) . . ? C19 N3 C15 127.6(15) . . ? C18 N4 C20 107.1(14) . . ? C18 N4 Ag2 123.5(16) . . ? C20 N4 Ag2 129.1(15) . . ? C21 N5 C22 101.5(19) . . ? C21 N5 Ag2 123.5(19) . . ? C22 N5 Ag2 135(2) . . ? C23 N6 C21 107.5(18) . . ? C23 N6 C24 123(2) . . ? C21 N6 C24 129(2) . . ? C40 N7 C38 107.5(12) . . ? C40 N7 C35 124.3(12) . . ? C38 N7 C35 128.2(12) . . ? C38 N8 C39 106.0(12) . . ? C38 N8 Ag1 129.7(11) . 1_454 ? C39 N8 Ag1 124.3(12) . 1_454 ? C42 N9 C41 103.8(14) . . ? C42 N9 Ag3 123.1(16) . . ? C41 N9 Ag3 132.7(16) . . ? C41 N10 C43 105.7(13) . . ? C41 N10 C44 126.7(17) . . ? C43 N10 C44 127.6(15) . . ? N1 C1 N2 112.2(13) . . ? C3 C2 N1 108.5(14) . . ? C2 C3 N2 106.2(15) . . ? C5 C4 C9 122.3(14) . . ? C5 C4 N2 123.4(15) . . ? C9 C4 N2 114.4(15) . . ? C4 C5 C6 118.9(13) . . ? C5 C6 C7 122.9(13) . . ? C6 C7 C8 116.9(12) . . ? C6 C7 Si1 124.4(12) . . ? C8 C7 Si1 118.7(12) . . ? C7 C8 C9 120.5(14) . . ? C4 C9 C8 118.4(14) . . ? C13 C12 C17 115.9(12) . . ? C13 C12 Si1 124.2(12) . . ? C17 C12 Si1 119.8(11) . . ? C14 C13 C12 126.3(12) . . ? C13 C14 C15 117.4(12) . . ? C16 C15 C14 119.4(12) . . ? C16 C15 N3 121.6(15) . . ? C14 C15 N3 118.9(15) . . ? C15 C16 C17 120.6(12) . . ? C12 C17 C16 120.5(12) . . ? N4 C18 N3 113.9(14) . . ? C20 C19 N3 109.0(15) . . ? C19 C20 N4 106.8(16) . . ? N5 C21 N6 114.3(19) . . ? N5 C21 C22 41.8(14) . . ? N6 C21 C22 72.5(12) . . ? C23 C22 N5 112(2) . . ? C23 C22 C21 75.8(16) . . ? N5 C22 C21 36.6(9) . . ? N6 C23 C22 104(2) . . ? C29 C24 C25 120(2) . . ? C29 C24 N6 126.0(19) . . ? C25 C24 N6 114(2) . . ? C24 C25 C26 117(2) . . ? C27 C26 C25 123.6(18) . . ? C28 C27 C26 114.4(16) . . ? C28 C27 Si2 125(2) . . ? C26 C27 Si2 121(2) . . ? C29 C28 C27 124.3(19) . . ? C28 C29 C24 120.8(19) . . ? C37 C32 C33 114.1(13) . . ? C37 C32 Si2 119.5(12) . . ? C33 C32 Si2 126.1(12) . . ? C34 C33 C32 123.1(13) . . ? C33 C34 C35 119.5(13) . . ? C34 C35 C36 121.4(12) . . ? C34 C35 N7 118.7(14) . . ? C36 C35 N7 120.0(13) . . ? C37 C36 C35 117.6(12) . . ? C36 C37 C32 124.2(13) . . ? N8 C38 N7 112.4(12) . . ? C40 C39 N8 106.5(12) . . ? N7 C40 C39 107.5(12) . . ? N10 C41 N9 114.8(16) . . ? N9 C42 C43 111.0(17) . . ? N10 C43 C42 104.6(15) . . ? C49 C44 C45 123.1(13) . . ? C49 C44 N10 118.8(15) . . ? C45 C44 N10 118.0(16) . . ? C46 C45 C44 118.5(14) . . ? C45 C46 C47 124.2(14) . . ? C46 C47 C48 115.7(12) . . ? C46 C47 Si3 126.8(14) . . ? C48 C47 Si3 117.6(14) . . ? C49 C48 C47 118.9(13) . . ? C44 C49 C48 119.5(13) . . ? O2 Cl1 O3 102.5(18) . . ? O2 Cl1 O4 106.2(18) . . ? O3 Cl1 O4 115.9(11) . . ? O2 Cl1 O1 107.1(17) . . ? O3 Cl1 O1 112.6(11) . . ? O4 Cl1 O1 111.6(12) . . ? O5 Cl2 O8 112(2) . . ? O5 Cl2 O7 106(2) . . ? O8 Cl2 O7 105.5(16) . . ? O5 Cl2 O6 107.1(14) . . ? O8 Cl2 O6 111.8(12) . . ? O7 Cl2 O6 114.3(17) . . ? O9 Cl3 O9 109(2) 2_565 . ? O9 Cl3 O10 107.6(13) 2_565 . ? O9 Cl3 O10 110.3(18) . . ? O9 Cl3 O10 110.3(18) 2_565 2_565 ? O9 Cl3 O10 107.6(13) . 2_565 ? O10 Cl3 O10 112(2) . 2_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 20.86 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.767 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.095 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.250 0.212 0.250 858.4 53.9 2 0.637 0.484 0.191 12.9 0.1 3 0.863 0.515 0.191 12.9 0.2 4 0.637 0.015 0.309 12.9 0.3 5 0.863 0.984 0.309 12.9 0.1 6 0.750 0.151 0.750 858.5 53.9 7 0.137 0.015 0.691 12.9 0.3 8 0.363 -0.015 0.691 12.9 0.0 9 0.137 0.484 0.809 12.9 0.1 10 0.363 0.515 0.809 12.8 0.4 _platon_squeeze_details ; ; # Attachment '1-final.cif' data_d:\bips\bips _database_code_depnum_ccdc_archive 'CCDC 734768' #TrackingRef '1-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H21.52 N4 O1.52 Si' _chemical_formula_weight 371.97 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 5.772(2) _cell_length_b 19.128(7) _cell_length_c 17.295(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1909.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3503 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 15.71 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9790 _exptl_absorpt_correction_T_max 0.9929 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _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 10565 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.65 _reflns_number_total 2263 _reflns_number_gt 1236 _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^)+(0.1138P)^2^+0.3779P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.001(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2263 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1319 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2222 _refine_ls_wR_factor_gt 0.1862 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.0733(2) 0.7500 0.42035(7) 0.0453(4) Uani 1 2 d S . . N1 N 0.7037(5) 0.49770(13) 0.37601(15) 0.0509(8) Uani 1 1 d . . . N2 N 1.0169(7) 0.4325(2) 0.3818(2) 0.0928(13) Uani 1 1 d . . . C1 C 0.2590(5) 0.67064(16) 0.40730(17) 0.0427(8) Uani 1 1 d . . . C2 C 0.4003(6) 0.64591(17) 0.46662(19) 0.0502(8) Uani 1 1 d . . . H2A H 0.3970 0.6684 0.5143 0.060 Uiso 1 1 calc R . . C3 C 0.5451(6) 0.58909(17) 0.45703(19) 0.0497(8) Uani 1 1 d . . . H3A H 0.6372 0.5737 0.4978 0.060 Uiso 1 1 calc R . . C4 C 0.5522(5) 0.55547(17) 0.38699(18) 0.0460(8) Uani 1 1 d . . . C5 C 0.4151(6) 0.57785(16) 0.32695(18) 0.0492(8) Uani 1 1 d . . . H5A H 0.4192 0.5549 0.2796 0.059 Uiso 1 1 calc R . . C6 C 0.2710(6) 0.63481(16) 0.33753(18) 0.0473(8) Uani 1 1 d . . . H6A H 0.1791 0.6497 0.2965 0.057 Uiso 1 1 calc R . . C7 C 0.6579(8) 0.4370(2) 0.3372(2) 0.0689(11) Uani 1 1 d . . . C8 C 0.8433(9) 0.3974(2) 0.3406(2) 0.0760(13) Uani 1 1 d . . . H8 H 0.8574 0.3531 0.3190 0.091 Uiso 1 1 calc R . . C9 C 0.9254(7) 0.4924(2) 0.4016(2) 0.0636(10) Uani 1 1 d . . . C10 C -0.0465(9) 0.7500 0.5204(3) 0.0621(14) Uani 1 2 d S . . H10A H -0.1419 0.7906 0.5276 0.093 Uiso 0.50 1 calc PR . . H10B H 0.0785 0.7507 0.5570 0.093 Uiso 1 2 calc SR . . H10C H -0.1379 0.7087 0.5281 0.093 Uiso 0.50 1 calc PR . . C11 C -0.1555(8) 0.7500 0.3465(3) 0.0572(13) Uani 1 2 d S . . H11A H -0.0863 0.7500 0.2960 0.086 Uiso 1 2 calc SR . . H11B H -0.2499 0.7910 0.3524 0.086 Uiso 0.50 1 calc PR . . H11C H -0.2499 0.7090 0.3524 0.086 Uiso 0.50 1 calc PR . . H9 H 0.9956 0.5316 0.4304 0.085(13) Uiso 1 1 d R . . H7 H 0.5077 0.4277 0.3058 0.116(16) Uiso 1 1 d R . . O01 O 0.899(5) 0.2500 0.2152(15) 0.64(4) Uiso 1.51(13) 2 d SP . . 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 0.0426(7) 0.0437(7) 0.0495(8) 0.000 -0.0004(6) 0.000 N1 0.0525(18) 0.0453(16) 0.0549(17) 0.0030(13) 0.0038(13) 0.0061(13) N2 0.086(3) 0.082(3) 0.110(3) 0.021(2) 0.025(3) 0.026(2) C1 0.0423(17) 0.0400(16) 0.0458(17) 0.0044(14) -0.0005(14) -0.0075(13) C2 0.054(2) 0.0507(19) 0.0458(18) -0.0034(14) 0.0013(15) -0.0008(16) C3 0.052(2) 0.0508(19) 0.0463(18) 0.0065(15) -0.0041(15) 0.0028(15) C4 0.0456(19) 0.0427(17) 0.0497(19) 0.0042(14) 0.0051(15) -0.0002(14) C5 0.056(2) 0.0503(18) 0.0412(17) 0.0010(14) 0.0016(15) -0.0003(16) C6 0.0484(19) 0.0477(18) 0.0457(18) 0.0023(14) -0.0049(15) -0.0018(15) C7 0.087(3) 0.057(2) 0.063(2) -0.0060(19) -0.004(2) 0.013(2) C8 0.116(4) 0.049(2) 0.063(2) 0.0016(19) 0.015(3) 0.024(2) C9 0.054(2) 0.057(2) 0.080(3) 0.008(2) 0.003(2) 0.0077(18) C10 0.058(3) 0.063(3) 0.065(3) 0.000 0.008(3) 0.000 C11 0.049(3) 0.063(3) 0.060(3) 0.000 -0.002(2) 0.000 _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 C11 1.838(5) . ? Si1 C10 1.863(5) . ? Si1 C1 1.872(3) 8_575 ? Si1 C1 1.872(3) . ? N1 C9 1.358(5) . ? N1 C7 1.367(4) . ? N1 C4 1.422(4) . ? N2 C9 1.306(5) . ? N2 C8 1.401(6) . ? C1 C6 1.390(4) . ? C1 C2 1.394(4) . ? C2 C3 1.381(5) . ? C2 H2A 0.9300 . ? C3 C4 1.372(4) . ? C3 H3A 0.9300 . ? C4 C5 1.374(4) . ? C5 C6 1.383(4) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.312(5) . ? C7 H7 1.0390 . ? C8 H8 0.9300 . ? C9 H9 0.9873 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 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 C11 Si1 C10 112.3(2) . . ? C11 Si1 C1 109.12(13) . 8_575 ? C10 Si1 C1 108.94(13) . 8_575 ? C11 Si1 C1 109.12(13) . . ? C10 Si1 C1 108.94(13) . . ? C1 Si1 C1 108.38(19) 8_575 . ? C9 N1 C7 106.2(3) . . ? C9 N1 C4 126.4(3) . . ? C7 N1 C4 127.4(3) . . ? C9 N2 C8 105.3(4) . . ? C6 C1 C2 116.3(3) . . ? C6 C1 Si1 122.2(2) . . ? C2 C1 Si1 121.4(2) . . ? C3 C2 C1 122.2(3) . . ? C3 C2 H2A 118.9 . . ? C1 C2 H2A 118.9 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 120.3(3) . . ? C5 C4 N1 119.7(3) . . ? C3 C4 N1 120.0(3) . . ? C4 C5 C6 119.5(3) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C5 C6 C1 122.2(3) . . ? C5 C6 H6A 118.9 . . ? C1 C6 H6A 118.9 . . ? C8 C7 N1 108.1(4) . . ? C8 C7 H7 127.2 . . ? N1 C7 H7 124.3 . . ? C7 C8 N2 109.2(4) . . ? C7 C8 H8 125.4 . . ? N2 C8 H8 125.4 . . ? N2 C9 N1 111.2(4) . . ? N2 C9 H9 129.2 . . ? N1 C9 H9 119.6 . . ? 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 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 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 C11 Si1 C1 C6 21.7(3) . . . . ? C10 Si1 C1 C6 144.6(3) . . . . ? C1 Si1 C1 C6 -97.0(3) 8_575 . . . ? C11 Si1 C1 C2 -160.9(3) . . . . ? C10 Si1 C1 C2 -38.0(3) . . . . ? C1 Si1 C1 C2 80.4(3) 8_575 . . . ? C6 C1 C2 C3 0.1(5) . . . . ? Si1 C1 C2 C3 -177.4(3) . . . . ? C1 C2 C3 C4 0.2(5) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C2 C3 C4 N1 178.9(3) . . . . ? C9 N1 C4 C5 137.8(4) . . . . ? C7 N1 C4 C5 -41.4(5) . . . . ? C9 N1 C4 C3 -41.5(5) . . . . ? C7 N1 C4 C3 139.3(4) . . . . ? C3 C4 C5 C6 0.4(5) . . . . ? N1 C4 C5 C6 -178.9(3) . . . . ? C4 C5 C6 C1 -0.1(5) . . . . ? C2 C1 C6 C5 -0.1(5) . . . . ? Si1 C1 C6 C5 177.4(2) . . . . ? C9 N1 C7 C8 0.7(4) . . . . ? C4 N1 C7 C8 -180.0(3) . . . . ? N1 C7 C8 N2 -0.5(5) . . . . ? C9 N2 C8 C7 0.0(5) . . . . ? C8 N2 C9 N1 0.4(5) . . . . ? C7 N1 C9 N2 -0.7(4) . . . . ? C4 N1 C9 N2 180.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.571 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.055