# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_SPM-269 _audit_creation_date 2012-03-01 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C94 H134 N4 Si6, 2(C H Cl3)' _chemical_formula_sum 'C96 H136 Cl6 N4 Si6' _chemical_formula_weight 1727.6 _chemical_melting_point ? 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' 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.7982(12) _cell_length_b 14.7823(10) _cell_length_c 19.3641(14) _cell_angle_alpha 90.00 _cell_angle_beta 105.335(4) _cell_angle_gamma 90.00 _cell_volume 4913.3(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9783 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.998 _cell_measurement_theta_min 2.373 _exptl_absorpt_coefficient_mu 0.293 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.7190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.1315 before and 0.0475 after correction. The Ratio of minimum to maximum transmission is 0.9637. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1689 _exptl_crystal_preparation perfluoroetheroil _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 83646 _diffrn_reflns_theta_full 24.72 _diffrn_reflns_theta_max 24.72 _diffrn_reflns_theta_min 1.82 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART APEX-II CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'double mirrors' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'ImuS microsource' _diffrn_source_current 0.6 _diffrn_source_power 0.03 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _reflns_number_gt 7027 _reflns_number_total 8382 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 1.281 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.084 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 523 _refine_ls_number_reflns 8382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0639 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+8.8878P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1738 _refine_ls_wR_factor_ref 0.1875 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.18643(5) 0.65902(6) 0.24903(5) 0.0239(2) Uani 1 1 d . . . Si2 Si 0.08883(5) 0.75770(6) -0.11002(5) 0.0246(2) Uani 1 1 d . . . Si3 Si 0.73021(5) 0.18213(6) 0.35355(5) 0.0283(2) Uani 1 1 d . . . Cl1 Cl 0.12197(11) 0.33478(9) 0.43078(7) 0.0809(5) Uani 1 1 d . . . Cl3 Cl 0.02410(7) 0.31115(10) 0.52546(10) 0.0821(5) Uani 1 1 d . . . Cl2 Cl 0.12094(11) 0.47011(8) 0.53653(7) 0.0804(5) Uani 1 1 d . . . N1 N 0.55101(13) 0.41017(16) 0.19583(13) 0.0215(5) Uani 1 1 d . . . N2 N 0.41495(13) 0.51678(15) 0.16481(13) 0.0198(5) Uani 1 1 d . . . C10 C 0.46415(16) 0.52614(18) -0.00823(16) 0.0197(6) Uani 1 1 d . . . C8 C 0.52299(16) 0.44780(18) 0.13170(16) 0.0196(6) Uani 1 1 d . . . C7 C 0.45310(15) 0.50084(18) 0.11582(16) 0.0197(6) Uani 1 1 d . . . C9 C 0.42279(16) 0.53882(18) 0.04399(16) 0.0191(6) Uani 1 1 d . . . C3 C 0.40551(16) 0.49807(19) 0.28557(16) 0.0225(6) Uani 1 1 d . . . C28 C 0.60882(19) 0.32380(19) 0.33098(16) 0.0261(7) Uani 1 1 d . . . C14 C 0.35296(16) 0.58763(19) 0.02684(16) 0.0201(6) Uani 1 1 d . . . H14 H 0.3255 0.5966 0.0622 0.024 Uiso 1 1 calc R . . C15 C 0.24883(17) 0.6685(2) -0.06030(17) 0.0244(7) Uani 1 1 d . . . C4 C 0.51199(16) 0.42507(19) 0.24593(16) 0.0219(6) Uani 1 1 d . . . C6 C 0.53918(17) 0.3847(2) 0.31567(17) 0.0254(7) Uani 1 1 d . . . C12 C 0.36518(16) 0.61303(19) -0.09286(16) 0.0211(6) Uani 1 1 d . . . H12 H 0.3458 0.6392 -0.1390 0.025 Uiso 1 1 calc R . . C37 C 0.33710(18) 0.5549(2) 0.27225(16) 0.0231(6) Uani 1 1 d . . . C2 C 0.43494(17) 0.4596(2) 0.35213(17) 0.0263(7) Uani 1 1 d . . . H2 H 0.4102 0.4718 0.3890 0.032 Uiso 1 1 calc R . . C5 C 0.44392(16) 0.48043(19) 0.23073(16) 0.0215(6) Uani 1 1 d . . . C11 C 0.43494(16) 0.56497(18) -0.07712(16) 0.0194(6) Uani 1 1 d . . . C17 C 0.11833(18) 0.5917(2) 0.17609(18) 0.0312(7) Uani 1 1 d . . . H17 H 0.1082 0.5337 0.1987 0.037 Uiso 1 1 calc R . . C13 C 0.32332(16) 0.62322(18) -0.04165(16) 0.0215(6) Uani 1 1 d . . . C1 C 0.50028(18) 0.4030(2) 0.36678(17) 0.0272(7) Uani 1 1 d . . . H1 H 0.5182 0.3767 0.4130 0.033 Uiso 1 1 calc R . . C24 C 0.02634(18) 0.7229(2) -0.04979(17) 0.0296(7) Uani 1 1 d . . . H24 H 0.0591 0.7301 0.0005 0.035 Uiso 1 1 calc R . . C23 C 0.05120(19) 0.7223(3) -0.20661(18) 0.0338(8) Uani 1 1 d . . . H23 H 0.0884 0.7485 -0.2319 0.041 Uiso 1 1 calc R . . C27 C 0.6560(2) 0.2722(3) 0.3481(2) 0.0363(8) Uani 1 1 d . . . C18 C 0.1531(2) 0.5650(3) 0.11408(19) 0.0377(8) Uani 1 1 d . . . H18A H 0.1598 0.6193 0.0873 0.057 Uiso 1 1 calc R . . H18B H 0.1178 0.5228 0.0821 0.057 Uiso 1 1 calc R . . H18C H 0.2038 0.5359 0.1334 0.057 Uiso 1 1 calc R . . C26 C -0.04594(19) 0.7827(3) -0.05710(19) 0.0391(9) Uani 1 1 d . . . H26A H -0.0297 0.8459 -0.0476 0.059 Uiso 1 1 calc R . . H26B H -0.0741 0.7630 -0.0226 0.059 Uiso 1 1 calc R . . H26C H -0.0800 0.7775 -0.1058 0.059 Uiso 1 1 calc R . . C21 C 0.10564(18) 0.8833(2) -0.10323(18) 0.0311(7) Uani 1 1 d . . . H21 H 0.0538 0.9134 -0.1215 0.037 Uiso 1 1 calc R . . C16 C 0.18555(18) 0.7036(2) -0.07735(17) 0.0264(7) Uani 1 1 d . . . C29 C 0.74967(18) 0.1187(2) 0.44019(17) 0.0283(7) Uani 1 1 d . . . H29 H 0.7889 0.0709 0.4385 0.034 Uiso 1 1 calc R . . C36 C 0.28072(18) 0.5995(2) 0.26575(17) 0.0270(7) Uani 1 1 d . . . C46 C 0.8932(2) 0.1762(3) 0.3653(2) 0.0444(9) Uani 1 1 d . . . H46A H 0.9030 0.1623 0.4164 0.067 Uiso 1 1 calc R . . H46B H 0.9386 0.2072 0.3568 0.067 Uiso 1 1 calc R . . H46C H 0.8840 0.1199 0.3377 0.067 Uiso 1 1 calc R . . C34 C -0.0280(2) 0.7648(3) -0.24218(19) 0.0409(9) Uani 1 1 d . . . H34A H -0.0676 0.7395 -0.2209 0.061 Uiso 1 1 calc R . . H34B H -0.0421 0.7517 -0.2936 0.061 Uiso 1 1 calc R . . H34C H -0.0250 0.8305 -0.2348 0.061 Uiso 1 1 calc R . . C25 C 0.0020(2) 0.6234(3) -0.0587(2) 0.0434(9) Uani 1 1 d . . . H25A H -0.0323 0.6137 -0.1068 0.065 Uiso 1 1 calc R . . H25B H -0.0258 0.6074 -0.0229 0.065 Uiso 1 1 calc R . . H25C H 0.0484 0.5853 -0.0520 0.065 Uiso 1 1 calc R . . C38 C 0.1546(2) 0.6568(3) 0.3340(2) 0.0432(9) Uani 1 1 d . . . H38 H 0.2005 0.6762 0.3734 0.052 Uiso 1 1 calc R . . C35 C 0.2559(2) 0.8299(3) 0.2878(2) 0.0445(9) Uani 1 1 d . . . H35A H 0.2336 0.8289 0.3290 0.067 Uiso 1 1 calc R . . H35B H 0.2619 0.8927 0.2740 0.067 Uiso 1 1 calc R . . H35C H 0.3070 0.8003 0.3008 0.067 Uiso 1 1 calc R . . C19 C 0.0389(2) 0.6369(3) 0.1472(2) 0.0469(10) Uani 1 1 d . . . H19A H 0.0151 0.6476 0.1867 0.070 Uiso 1 1 calc R . . H19B H 0.0051 0.5974 0.1116 0.070 Uiso 1 1 calc R . . H19C H 0.0457 0.6948 0.1249 0.070 Uiso 1 1 calc R . . C22 C 0.1576(2) 0.9156(3) -0.1497(2) 0.0435(9) Uani 1 1 d . . . H22A H 0.2069 0.8821 -0.1368 0.065 Uiso 1 1 calc R . . H22B H 0.1681 0.9804 -0.1418 0.065 Uiso 1 1 calc R . . H22C H 0.1312 0.9050 -0.2002 0.065 Uiso 1 1 calc R . . C30 C 0.8209(2) 0.2379(3) 0.3418(2) 0.0405(9) Uani 1 1 d . . . H30 H 0.8122 0.2487 0.2893 0.049 Uiso 1 1 calc R . . C32 C 0.7845(3) 0.1765(3) 0.5059(2) 0.0480(10) Uani 1 1 d . . . H32A H 0.8346 0.2012 0.5028 0.072 Uiso 1 1 calc R . . H32B H 0.7925 0.1392 0.5491 0.072 Uiso 1 1 calc R . . H32C H 0.7488 0.2262 0.5082 0.072 Uiso 1 1 calc R . . C33 C 0.6773(2) 0.0703(3) 0.4492(2) 0.0465(10) Uani 1 1 d . . . H33A H 0.6382 0.1151 0.4535 0.070 Uiso 1 1 calc R . . H33B H 0.6912 0.0329 0.4924 0.070 Uiso 1 1 calc R . . H33C H 0.6559 0.0319 0.4074 0.070 Uiso 1 1 calc R . . C20 C 0.1113(3) 0.3546(3) 0.5151(2) 0.0543(11) Uani 1 1 d . . . H20 H 0.1545 0.3222 0.5498 0.065 Uiso 1 1 calc R . . C41 C 0.20130(19) 0.7793(2) 0.22443(19) 0.0339(8) Uani 1 1 d . . . H41 H 0.1494 0.8099 0.2138 0.041 Uiso 1 1 calc R . . C43 C 0.1391(2) 0.9138(3) -0.0255(2) 0.0432(9) Uani 1 1 d . . . H43A H 0.1033 0.8965 0.0029 0.065 Uiso 1 1 calc R . . H43B H 0.1457 0.9796 -0.0240 0.065 Uiso 1 1 calc R . . H43C H 0.1897 0.8847 -0.0057 0.065 Uiso 1 1 calc R . . C47 C 0.7298(3) 0.0185(3) 0.2749(2) 0.0517(11) Uani 1 1 d . . . H47A H 0.7819 0.0351 0.2712 0.078 Uiso 1 1 calc R . . H47B H 0.7035 -0.0179 0.2332 0.078 Uiso 1 1 calc R . . H47C H 0.7344 -0.0168 0.3187 0.078 Uiso 1 1 calc R . . C48 C 0.6822(3) 0.1050(3) 0.2774(2) 0.0638(14) Uani 1 1 d . . . H48 H 0.6354 0.0821 0.2914 0.077 Uiso 1 1 calc R . . C45 C 0.8371(2) 0.3301(3) 0.3781(3) 0.0593(13) Uani 1 1 d . . . H45A H 0.7920 0.3697 0.3603 0.089 Uiso 1 1 calc R . . H45B H 0.8830 0.3571 0.3673 0.089 Uiso 1 1 calc R . . H45C H 0.8469 0.3227 0.4300 0.089 Uiso 1 1 calc R . . C42 C 0.2311(3) 0.7887(3) 0.1587(2) 0.0550(11) Uani 1 1 d . . . H42A H 0.2784 0.7523 0.1646 0.083 Uiso 1 1 calc R . . H42B H 0.2431 0.8524 0.1522 0.083 Uiso 1 1 calc R . . H42C H 0.1912 0.7676 0.1166 0.083 Uiso 1 1 calc R . . C40 C 0.0880(2) 0.7238(3) 0.3338(2) 0.0554(12) Uani 1 1 d . . . H40A H 0.1042 0.7852 0.3253 0.083 Uiso 1 1 calc R . . H40B H 0.0757 0.7215 0.3802 0.083 Uiso 1 1 calc R . . H40C H 0.0417 0.7071 0.2958 0.083 Uiso 1 1 calc R . . C44 C 0.0499(3) 0.6206(3) -0.2211(2) 0.0629(14) Uani 1 1 d . . . H44A H 0.1019 0.5953 -0.2004 0.094 Uiso 1 1 calc R . . H44B H 0.0345 0.6099 -0.2729 0.094 Uiso 1 1 calc R . . H44C H 0.0125 0.5914 -0.1992 0.094 Uiso 1 1 calc R . . C49 C 0.6493(4) 0.1493(5) 0.2098(3) 0.106(3) Uani 1 1 d . . . H49A H 0.6165 0.1999 0.2169 0.159 Uiso 1 1 calc R . . H49B H 0.6177 0.1060 0.1760 0.159 Uiso 1 1 calc R . . H49C H 0.6914 0.1722 0.1906 0.159 Uiso 1 1 calc R . . C39 C 0.1328(5) 0.5624(4) 0.3527(3) 0.095(2) Uani 1 1 d . . . H39A H 0.0893 0.5398 0.3142 0.142 Uiso 1 1 calc R . . H39B H 0.1172 0.5645 0.3976 0.142 Uiso 1 1 calc R . . H39C H 0.1777 0.5221 0.3583 0.142 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 0.0203(4) 0.0247(4) 0.0273(5) 0.0002(3) 0.0074(3) 0.0026(3) Si2 0.0166(4) 0.0323(5) 0.0241(4) 0.0040(3) 0.0039(3) 0.0122(3) Si3 0.0272(5) 0.0251(5) 0.0279(5) 0.0060(4) -0.0009(4) 0.0069(4) Cl1 0.1462(14) 0.0540(7) 0.0499(7) -0.0041(5) 0.0389(8) -0.0013(8) Cl3 0.0505(7) 0.0702(8) 0.1279(13) 0.0212(8) 0.0277(7) 0.0062(6) Cl2 0.1501(14) 0.0386(6) 0.0584(7) -0.0017(5) 0.0378(8) -0.0039(7) N1 0.0161(12) 0.0151(11) 0.0289(14) 0.0010(10) -0.0019(10) 0.0002(9) N2 0.0143(11) 0.0158(12) 0.0253(13) -0.0008(10) -0.0017(10) -0.0006(9) C10 0.0138(13) 0.0112(12) 0.0289(16) -0.0045(11) -0.0035(11) 0.0001(11) C8 0.0125(13) 0.0125(13) 0.0291(16) -0.0010(11) -0.0029(11) -0.0005(10) C7 0.0130(13) 0.0121(13) 0.0295(16) -0.0012(11) -0.0025(12) -0.0004(10) C9 0.0138(13) 0.0118(13) 0.0277(15) -0.0028(11) -0.0013(11) 0.0000(10) C3 0.0163(14) 0.0180(14) 0.0304(16) 0.0009(12) 0.0009(12) -0.0026(11) C28 0.0357(18) 0.0139(14) 0.0188(15) 0.0105(12) -0.0099(13) -0.0031(14) C14 0.0130(13) 0.0154(13) 0.0289(16) -0.0025(12) 0.0006(11) 0.0030(11) C15 0.0199(15) 0.0242(15) 0.0273(16) 0.0018(12) 0.0032(12) 0.0052(12) C4 0.0159(14) 0.0168(14) 0.0287(16) 0.0016(12) -0.0016(12) -0.0006(11) C6 0.0194(15) 0.0187(14) 0.0322(17) 0.0035(13) -0.0035(13) -0.0005(12) C12 0.0149(14) 0.0156(14) 0.0280(16) 0.0001(12) -0.0026(12) 0.0032(11) C37 0.0248(16) 0.0206(15) 0.0240(15) -0.0014(12) 0.0066(12) -0.0064(13) C2 0.0203(15) 0.0251(16) 0.0322(17) 0.0029(13) 0.0049(13) -0.0046(12) C5 0.0170(14) 0.0141(13) 0.0298(16) -0.0002(12) -0.0002(12) -0.0037(11) C11 0.0138(13) 0.0128(13) 0.0267(15) -0.0031(11) -0.0035(11) -0.0007(10) C17 0.0218(16) 0.0356(18) 0.0355(18) -0.0028(15) 0.0062(14) -0.0009(14) C13 0.0144(14) 0.0137(13) 0.0320(16) -0.0010(12) -0.0016(12) 0.0030(11) C1 0.0243(16) 0.0241(16) 0.0291(17) 0.0060(13) -0.0003(13) -0.0033(13) C24 0.0238(16) 0.0396(19) 0.0250(16) 0.0011(14) 0.0058(13) 0.0051(14) C23 0.0251(17) 0.048(2) 0.0273(17) 0.0015(15) 0.0052(13) 0.0157(15) C27 0.0311(19) 0.037(2) 0.037(2) -0.0022(16) 0.0032(15) -0.0065(17) C18 0.0311(18) 0.046(2) 0.0328(19) -0.0095(16) 0.0030(15) 0.0039(16) C26 0.0242(17) 0.062(2) 0.0330(19) -0.0051(17) 0.0111(14) 0.0072(16) C21 0.0223(16) 0.0328(18) 0.0376(19) 0.0068(14) 0.0070(14) 0.0111(13) C16 0.0221(16) 0.0304(16) 0.0255(16) 0.0036(13) 0.0044(12) 0.0078(13) C29 0.0217(15) 0.0290(17) 0.0327(17) 0.0091(14) 0.0045(13) 0.0047(13) C36 0.0263(17) 0.0265(16) 0.0258(16) 0.0000(13) 0.0025(13) -0.0017(14) C46 0.036(2) 0.050(2) 0.048(2) 0.0165(18) 0.0144(17) 0.0131(17) C34 0.0282(18) 0.059(2) 0.0315(19) 0.0032(17) 0.0001(15) 0.0170(17) C25 0.039(2) 0.047(2) 0.044(2) 0.0024(18) 0.0107(17) -0.0010(17) C38 0.052(2) 0.047(2) 0.035(2) -0.0040(17) 0.0190(17) -0.0003(18) C35 0.038(2) 0.0326(19) 0.059(3) -0.0056(17) 0.0061(18) -0.0040(16) C19 0.0218(17) 0.074(3) 0.041(2) -0.014(2) 0.0026(15) 0.0085(18) C22 0.034(2) 0.045(2) 0.053(2) 0.0147(18) 0.0149(17) 0.0079(17) C30 0.0345(19) 0.043(2) 0.047(2) 0.0253(17) 0.0166(16) 0.0136(16) C32 0.056(2) 0.056(2) 0.0297(19) 0.0018(17) 0.0060(17) 0.000(2) C33 0.0315(19) 0.048(2) 0.063(3) 0.017(2) 0.0183(18) 0.0013(17) C20 0.069(3) 0.042(2) 0.051(3) -0.0008(19) 0.014(2) 0.002(2) C41 0.0251(17) 0.0278(17) 0.045(2) 0.0053(15) 0.0017(15) 0.0020(13) C43 0.045(2) 0.038(2) 0.046(2) -0.0054(17) 0.0102(18) 0.0023(17) C47 0.075(3) 0.036(2) 0.037(2) -0.0044(17) 0.003(2) 0.003(2) C48 0.080(3) 0.040(2) 0.046(2) -0.0077(19) -0.029(2) 0.016(2) C45 0.035(2) 0.031(2) 0.111(4) 0.026(2) 0.018(2) 0.0023(16) C42 0.064(3) 0.049(2) 0.046(2) 0.016(2) 0.004(2) -0.018(2) C40 0.038(2) 0.082(3) 0.051(3) -0.021(2) 0.0217(19) 0.001(2) C44 0.076(3) 0.063(3) 0.041(2) -0.011(2) -0.001(2) 0.033(2) C49 0.119(5) 0.115(5) 0.056(3) -0.031(3) -0.024(3) 0.065(4) C39 0.178(7) 0.062(3) 0.073(4) 0.015(3) 0.086(4) -0.007(4) _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 C17 1.884(3) . ? Si1 C36 1.846(3) . ? Si1 C38 1.877(4) . ? Si1 C41 1.877(3) . ? Si2 C24 1.884(3) . ? Si2 C23 1.886(3) . ? Si2 C21 1.880(4) . ? Si2 C16 1.851(3) . ? Si3 C27 1.859(4) . ? Si3 C29 1.873(3) . ? Si3 C30 1.879(4) . ? Si3 C48 1.880(4) . ? Cl1 C20 1.719(5) . ? Cl3 C20 1.738(5) . ? Cl2 C20 1.755(4) . ? N1 C8 1.331(4) . ? N1 C4 1.352(4) . ? N2 C7 1.326(4) . ? N2 C5 1.355(4) . ? C10 C10 1.453(5) 3_665 ? C10 C9 1.412(4) . ? C10 C11 1.419(4) . ? C8 C7 1.433(4) . ? C8 C11 1.460(4) 3_665 ? C7 C9 1.464(4) . ? C9 C14 1.399(4) . ? C3 C37 1.445(4) . ? C3 C2 1.379(4) . ? C3 C5 1.431(4) . ? C28 C6 1.496(4) . ? C28 C27 1.118(5) . ? C14 H14 0.9500 . ? C14 C13 1.394(4) . ? C15 C13 1.443(4) . ? C15 C16 1.204(4) . ? C4 C6 1.439(4) . ? C4 C5 1.427(4) . ? C6 C1 1.376(5) . ? C12 H12 0.9500 . ? C12 C11 1.393(4) . ? C12 C13 1.397(4) . ? C37 C36 1.179(4) . ? C2 H2 0.9500 . ? C2 C1 1.399(4) . ? C11 C8 1.460(4) 3_665 ? C17 H17 1.0000 . ? C17 C18 1.541(5) . ? C17 C19 1.529(5) . ? C1 H1 0.9500 . ? C24 H24 1.0000 . ? C24 C26 1.537(5) . ? C24 C25 1.530(5) . ? C23 H23 1.0000 . ? C23 C34 1.531(4) . ? C23 C44 1.529(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C21 H21 1.0000 . ? C21 C22 1.527(5) . ? C21 C43 1.532(5) . ? C29 H29 1.0000 . ? C29 C32 1.522(5) . ? C29 C33 1.523(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C46 C30 1.546(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C38 H38 1.0000 . ? C38 C40 1.544(6) . ? C38 C39 1.518(6) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35 C41 1.543(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C30 H30 1.0000 . ? C30 C45 1.525(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C20 H20 1.0000 . ? C41 H41 1.0000 . ? C41 C42 1.509(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C47 C48 1.542(6) . ? C48 H48 1.0000 . ? C48 C49 1.443(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? 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 C36 Si1 C17 104.73(14) . . ? C36 Si1 C38 108.00(17) . . ? C36 Si1 C41 108.26(15) . . ? C38 Si1 C17 111.39(17) . . ? C38 Si1 C41 109.53(17) . . ? C41 Si1 C17 114.59(16) . . ? C24 Si2 C23 115.16(16) . . ? C21 Si2 C24 109.63(15) . . ? C21 Si2 C23 110.58(16) . . ? C16 Si2 C24 108.55(14) . . ? C16 Si2 C23 105.86(14) . . ? C16 Si2 C21 106.64(15) . . ? C27 Si3 C29 111.72(16) . . ? C27 Si3 C30 107.36(16) . . ? C27 Si3 C48 102.78(18) . . ? C29 Si3 C30 111.53(15) . . ? C29 Si3 C48 109.67(19) . . ? C30 Si3 C48 113.5(2) . . ? C8 N1 C4 117.7(2) . . ? C7 N2 C5 117.7(2) . . ? C9 C10 C10 120.5(3) . 3_665 ? C9 C10 C11 119.3(2) . . ? C11 C10 C10 120.2(4) . 3_665 ? N1 C8 C7 121.2(3) . . ? N1 C8 C11 118.9(2) . 3_665 ? C7 C8 C11 119.8(3) . 3_665 ? N2 C7 C8 121.6(3) . . ? N2 C7 C9 118.8(2) . . ? C8 C7 C9 119.6(3) . . ? C10 C9 C7 119.9(2) . . ? C14 C9 C10 119.8(3) . . ? C14 C9 C7 120.3(3) . . ? C2 C3 C37 120.0(3) . . ? C2 C3 C5 118.7(3) . . ? C5 C3 C37 121.3(3) . . ? C27 C28 C6 170.7(4) . . ? C9 C14 H14 119.7 . . ? C13 C14 C9 120.6(3) . . ? C13 C14 H14 119.7 . . ? C16 C15 C13 177.7(3) . . ? N1 C4 C6 119.8(3) . . ? N1 C4 C5 121.0(3) . . ? C5 C4 C6 119.2(3) . . ? C4 C6 C28 119.4(3) . . ? C1 C6 C28 121.6(3) . . ? C1 C6 C4 119.0(3) . . ? C11 C12 H12 119.6 . . ? C11 C12 C13 120.8(3) . . ? C13 C12 H12 119.6 . . ? C36 C37 C3 175.5(3) . . ? C3 C2 H2 119.1 . . ? C3 C2 C1 121.7(3) . . ? C1 C2 H2 119.1 . . ? N2 C5 C3 119.3(3) . . ? N2 C5 C4 120.8(3) . . ? C4 C5 C3 119.9(3) . . ? C10 C11 C8 119.9(2) . 3_665 ? C12 C11 C10 119.7(3) . . ? C12 C11 C8 120.4(3) . 3_665 ? Si1 C17 H17 106.2 . . ? C18 C17 Si1 114.1(2) . . ? C18 C17 H17 106.2 . . ? C19 C17 Si1 113.1(2) . . ? C19 C17 H17 106.2 . . ? C19 C17 C18 110.5(3) . . ? C14 C13 C15 120.3(3) . . ? C14 C13 C12 119.7(3) . . ? C12 C13 C15 120.0(3) . . ? C6 C1 C2 121.4(3) . . ? C6 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? Si2 C24 H24 106.7 . . ? C26 C24 Si2 113.7(2) . . ? C26 C24 H24 106.7 . . ? C25 C24 Si2 112.9(2) . . ? C25 C24 H24 106.7 . . ? C25 C24 C26 109.7(3) . . ? Si2 C23 H23 105.7 . . ? C34 C23 Si2 112.1(2) . . ? C34 C23 H23 105.7 . . ? C44 C23 Si2 116.0(3) . . ? C44 C23 H23 105.7 . . ? C44 C23 C34 110.7(3) . . ? C28 C27 Si3 166.5(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C21 H21 107.4 . . ? C22 C21 Si2 112.2(3) . . ? C22 C21 H21 107.4 . . ? C22 C21 C43 110.3(3) . . ? C43 C21 Si2 111.9(2) . . ? C43 C21 H21 107.4 . . ? C15 C16 Si2 176.0(3) . . ? Si3 C29 H29 106.9 . . ? C32 C29 Si3 114.0(2) . . ? C32 C29 H29 106.9 . . ? C32 C29 C33 109.7(3) . . ? C33 C29 Si3 112.1(2) . . ? C33 C29 H29 106.9 . . ? C37 C36 Si1 173.5(3) . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C30 C46 H46A 109.5 . . ? C30 C46 H46B 109.5 . . ? C30 C46 H46C 109.5 . . ? C23 C34 H34A 109.5 . . ? C23 C34 H34B 109.5 . . ? C23 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C38 H38 106.8 . . ? C40 C38 Si1 113.4(3) . . ? C40 C38 H38 106.8 . . ? C39 C38 Si1 112.4(3) . . ? C39 C38 H38 106.8 . . ? C39 C38 C40 110.2(4) . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C35 H35A 109.5 . . ? C41 C35 H35B 109.5 . . ? C41 C35 H35C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C30 H30 106.6 . . ? C46 C30 Si3 112.4(3) . . ? C46 C30 H30 106.6 . . ? C45 C30 Si3 113.7(3) . . ? C45 C30 C46 110.5(3) . . ? C45 C30 H30 106.6 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Cl1 C20 Cl3 111.9(3) . . ? Cl1 C20 Cl2 111.2(3) . . ? Cl1 C20 H20 107.3 . . ? Cl3 C20 Cl2 111.5(3) . . ? Cl3 C20 H20 107.3 . . ? Cl2 C20 H20 107.3 . . ? Si1 C41 H41 107.3 . . ? C35 C41 Si1 111.0(2) . . ? C35 C41 H41 107.3 . . ? C42 C41 Si1 114.0(3) . . ? C42 C41 C35 109.8(3) . . ? C42 C41 H41 107.3 . . ? C21 C43 H43A 109.5 . . ? C21 C43 H43B 109.5 . . ? C21 C43 H43C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? Si3 C48 H48 103.4 . . ? C47 C48 Si3 112.8(3) . . ? C47 C48 H48 103.4 . . ? C49 C48 Si3 115.3(4) . . ? C49 C48 C47 116.2(4) . . ? C49 C48 H48 103.4 . . ? C30 C45 H45A 109.5 . . ? C30 C45 H45B 109.5 . . ? C30 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C23 C44 H44A 109.5 . . ? C23 C44 H44B 109.5 . . ? C23 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 972121' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_SPM336_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C112 H170 N4 Si6)' _chemical_formula_sum 'C112 H170 N4 Si6' _chemical_formula_weight 1741.06 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 8.7047(3) _cell_length_b 22.2249(7) _cell_length_c 28.1465(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.745(2) _cell_angle_gamma 90.00 _cell_volume 5382.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9382 _cell_measurement_theta_min 2.3448 _cell_measurement_theta_max 24.3031 _exptl_crystal_description needle _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7002 _exptl_absorpt_correction_T_max 0.7409 _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.1374 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.440766550523. The \l/2 correction factor is 0.0015 ; _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 SMART APEX-II CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8 _diffrn_reflns_number 57575 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.1335 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8262 _reflns_number_gt 4794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _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^)+(0.0600P)^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 8262 _refine_ls_number_parameters 625 _refine_ls_number_restraints 439 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.002 _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 0.45921(10) 0.73310(4) 0.35432(3) 0.0228(2) Uani 1 1 d D . . Si2 Si -0.42205(11) 0.18926(4) 0.45745(3) 0.0267(2) Uani 1 1 d D . . Si3 Si 0.33405(10) 0.49846(4) 0.25913(3) 0.0251(2) Uani 1 1 d D . . N1 N 0.0785(3) 0.42653(10) 0.38087(8) 0.0187(6) Uani 1 1 d . B . N2 N -0.0898(3) 0.34895(10) 0.43297(8) 0.0185(6) Uani 1 1 d . . . C1 C 0.3583(4) 0.67754(14) 0.38747(10) 0.0247(7) Uani 1 1 d . . . C2 C -0.2755(4) 0.21206(14) 0.41997(12) 0.0308(8) Uani 1 1 d . A . C3 C 0.2318(4) 0.43102(14) 0.27598(11) 0.0255(7) Uani 1 1 d . B . C11 C 0.2932(3) 0.64057(13) 0.40821(10) 0.0203(7) Uani 1 1 d . . . C22 C -0.1898(4) 0.23714(13) 0.39752(11) 0.0256(7) Uani 1 1 d . . . C33 C 0.1644(4) 0.39248(13) 0.29423(10) 0.0221(7) Uani 1 1 d . . . C40 C 0.0359(3) 0.29439(13) 0.30342(10) 0.0232(7) Uani 1 1 d . . . H40 H 0.0655 0.2807 0.2741 0.028 Uiso 1 1 calc R B . C41 C -0.0496(4) 0.25601(14) 0.32912(10) 0.0257(7) Uani 1 1 d . A . H41 H -0.0772 0.2171 0.3167 0.031 Uiso 1 1 calc R . . C42 C 0.0783(3) 0.35164(13) 0.31957(10) 0.0206(7) Uani 1 1 d . B . C43 C -0.0942(4) 0.27345(13) 0.37176(10) 0.0225(7) Uani 1 1 d . A . C44 C 0.0354(3) 0.37117(12) 0.36418(10) 0.0182(6) Uani 1 1 d . . . C45 C -0.0498(3) 0.33204(13) 0.39033(10) 0.0190(7) Uani 1 1 d . A . C46 C 0.0382(3) 0.44273(12) 0.42257(9) 0.0176(7) Uani 1 1 d . . . C47 C -0.0475(3) 0.40352(13) 0.44907(9) 0.0172(6) Uani 1 1 d . . . C48 C 0.1677(3) 0.54140(12) 0.41667(10) 0.0183(7) Uani 1 1 d . . . H48 H 0.1953 0.5290 0.3868 0.022 Uiso 1 1 calc R B . C49 C 0.0845(3) 0.50224(12) 0.44203(10) 0.0170(6) Uani 1 1 d . B . C50 C 0.2111(3) 0.59854(12) 0.43463(9) 0.0171(6) Uani 1 1 d . B . C51 C 0.0435(3) 0.51980(12) 0.48668(9) 0.0163(6) Uani 1 1 d . . . C52 C 0.1723(3) 0.61582(13) 0.47908(9) 0.0176(6) Uani 1 1 d . . . H52 H 0.2030 0.6543 0.4918 0.021 Uiso 1 1 calc R B . C53 C 0.0890(3) 0.57737(12) 0.50492(9) 0.0177(6) Uani 1 1 d . . . C111 C 0.3516(3) 0.80621(13) 0.34752(11) 0.0237(7) Uani 1 1 d D . . H11A H 0.3356 0.8189 0.3801 0.028 Uiso 1 1 calc R . . H11B H 0.4222 0.8362 0.3363 0.028 Uiso 1 1 calc R . . C112 C 0.1952(3) 0.81212(13) 0.31506(11) 0.0272(7) Uani 1 1 d D . . H112 H 0.2009 0.7894 0.2847 0.033 Uiso 1 1 calc R . . C113 C 0.0644(4) 0.78553(16) 0.33851(13) 0.0400(9) Uani 1 1 d D . . H11C H -0.0341 0.7896 0.3167 0.060 Uiso 1 1 calc R . . H11D H 0.0575 0.8070 0.3685 0.060 Uiso 1 1 calc R . . H11E H 0.0853 0.7428 0.3454 0.060 Uiso 1 1 calc R . . C114 C 0.1607(4) 0.87780(15) 0.30196(12) 0.0381(9) Uani 1 1 d D . . H11F H 0.0603 0.8807 0.2810 0.057 Uiso 1 1 calc R . . H11G H 0.2426 0.8938 0.2852 0.057 Uiso 1 1 calc R . . H11H H 0.1570 0.9011 0.3313 0.057 Uiso 1 1 calc R . . C121 C 0.6509(3) 0.75276(13) 0.39105(11) 0.0259(7) Uani 1 1 d D . . H12A H 0.7182 0.7693 0.3688 0.031 Uiso 1 1 calc R . . H12B H 0.6321 0.7857 0.4131 0.031 Uiso 1 1 calc R . . C122 C 0.7441(4) 0.70371(13) 0.42136(11) 0.0281(8) Uani 1 1 d D . . H122 H 0.6732 0.6842 0.4416 0.034 Uiso 1 1 calc R . . C123 C 0.8806(4) 0.73171(15) 0.45555(11) 0.0347(8) Uani 1 1 d D . . H12C H 0.9383 0.6999 0.4747 0.052 Uiso 1 1 calc R . . H12D H 0.8403 0.7604 0.4770 0.052 Uiso 1 1 calc R . . H12E H 0.9501 0.7526 0.4367 0.052 Uiso 1 1 calc R . . C124 C 0.8019(4) 0.65529(14) 0.39076(12) 0.0363(9) Uani 1 1 d D . . H12F H 0.8592 0.6249 0.4116 0.054 Uiso 1 1 calc R . . H12G H 0.8709 0.6733 0.3702 0.054 Uiso 1 1 calc R . . H12H H 0.7132 0.6364 0.3707 0.054 Uiso 1 1 calc R . . C131 C 0.4724(4) 0.69588(13) 0.29490(10) 0.0253(7) Uani 1 1 d D . . H13A H 0.5013 0.6533 0.3016 0.030 Uiso 1 1 calc R . . H13B H 0.3667 0.6959 0.2760 0.030 Uiso 1 1 calc R . . C132 C 0.5834(4) 0.72126(14) 0.26261(11) 0.0294(8) Uani 1 1 d D . . H132 H 0.6895 0.7238 0.2820 0.035 Uiso 1 1 calc R . . C133 C 0.5369(5) 0.78396(15) 0.24400(13) 0.0442(10) Uani 1 1 d D . . H13C H 0.6123 0.7986 0.2241 0.066 Uiso 1 1 calc R . . H13D H 0.5351 0.8113 0.2712 0.066 Uiso 1 1 calc R . . H13E H 0.4334 0.7824 0.2246 0.066 Uiso 1 1 calc R . . C134 C 0.5915(4) 0.67913(16) 0.22023(11) 0.0388(9) Uani 1 1 d D . . H13F H 0.6633 0.6957 0.2000 0.058 Uiso 1 1 calc R . . H13G H 0.4878 0.6751 0.2013 0.058 Uiso 1 1 calc R . . H13H H 0.6285 0.6395 0.2322 0.058 Uiso 1 1 calc R . . C211 C -0.5710(4) 0.14266(15) 0.41846(12) 0.0337(8) Uani 1 1 d D A . H21A H -0.5815 0.1589 0.3854 0.040 Uiso 1 1 calc R . . H21B H -0.5296 0.1013 0.4175 0.040 Uiso 1 1 calc R . . C212 C -0.7340(4) 0.13861(16) 0.43249(12) 0.0404(9) Uani 1 1 d D . . H212 H -0.7730 0.1805 0.4356 0.048 Uiso 1 1 calc R A . C213 C -0.8456(5) 0.10670(18) 0.39301(13) 0.0530(11) Uani 1 1 d D A . H21C H -0.9495 0.1050 0.4023 0.080 Uiso 1 1 calc R . . H21D H -0.8083 0.0658 0.3887 0.080 Uiso 1 1 calc R . . H21E H -0.8503 0.1290 0.3628 0.080 Uiso 1 1 calc R . . C214 C -0.7273(5) 0.10744(19) 0.48155(12) 0.0560(12) Uani 1 1 d D A . H21F H -0.8320 0.1056 0.4903 0.084 Uiso 1 1 calc R . . H21G H -0.6590 0.1303 0.5060 0.084 Uiso 1 1 calc R . . H21H H -0.6867 0.0665 0.4797 0.084 Uiso 1 1 calc R . . C221 C -0.5041(4) 0.26090(13) 0.47877(10) 0.0262(7) Uani 1 1 d D A . H22A H -0.6090 0.2519 0.4864 0.031 Uiso 1 1 calc R . . H22B H -0.4386 0.2728 0.5092 0.031 Uiso 1 1 calc R . . C222 C -0.5181(4) 0.31574(14) 0.44483(10) 0.0283(8) Uani 1 1 d D . . H222 H -0.4104 0.3277 0.4405 0.034 Uiso 1 1 calc R A . C223 C -0.6077(4) 0.30131(14) 0.39494(10) 0.0320(8) Uani 1 1 d D A . H22C H -0.5592 0.2669 0.3813 0.048 Uiso 1 1 calc R . . H22D H -0.6054 0.3363 0.3739 0.048 Uiso 1 1 calc R . . H22E H -0.7157 0.2915 0.3977 0.048 Uiso 1 1 calc R . . C224 C -0.5913(4) 0.36956(14) 0.46719(11) 0.0305(8) Uani 1 1 d D A . H22F H -0.5991 0.4037 0.4449 0.046 Uiso 1 1 calc R . . H22G H -0.5263 0.3808 0.4974 0.046 Uiso 1 1 calc R . . H22H H -0.6953 0.3586 0.4735 0.046 Uiso 1 1 calc R . . C231 C -0.3181(11) 0.1487(4) 0.5116(2) 0.016(3) Uani 0.653(11) 1 d PD A 1 H23A H -0.2229 0.1718 0.5236 0.020 Uiso 0.653(11) 1 calc PR A 1 H23B H -0.3855 0.1503 0.5369 0.020 Uiso 0.653(11) 1 calc PR A 1 C232 C -0.2700(8) 0.0826(3) 0.50642(19) 0.0341(18) Uani 0.653(11) 1 d PD A 1 H232 H -0.3589 0.0539 0.5056 0.041 Uiso 0.653(11) 1 calc PR A 1 C233 C -0.1334(13) 0.0735(5) 0.5553(3) 0.071(3) Uani 0.653(11) 1 d PDU A 1 H23C H -0.1819 0.0770 0.5844 0.106 Uiso 0.653(11) 1 calc PR A 1 H23D H -0.0535 0.1046 0.5556 0.106 Uiso 0.653(11) 1 calc PR A 1 H23E H -0.0858 0.0337 0.5543 0.106 Uiso 0.653(11) 1 calc PR A 1 C234 C -0.1762(12) 0.0722(6) 0.4666(4) 0.046(3) Uani 0.653(11) 1 d PD A 1 H23F H -0.1502 0.0294 0.4652 0.069 Uiso 0.653(11) 1 calc PR A 1 H23G H -0.0804 0.0959 0.4726 0.069 Uiso 0.653(11) 1 calc PR A 1 H23H H -0.2370 0.0845 0.4359 0.069 Uiso 0.653(11) 1 calc PR A 1 C531 C -0.327(3) 0.1471(12) 0.5113(6) 0.074(12) Uani 0.347(11) 1 d PDU A 2 H53A H -0.2959 0.1770 0.5371 0.089 Uiso 0.347(11) 1 calc PR A 2 H53B H -0.4068 0.1210 0.5222 0.089 Uiso 0.347(11) 1 calc PR A 2 C532 C -0.1833(15) 0.1074(5) 0.5079(3) 0.034(4) Uani 0.347(11) 1 d PD A 2 H532 H -0.0828 0.1292 0.5081 0.040 Uiso 0.347(11) 1 calc PR A 2 C533 C -0.227(2) 0.0622(10) 0.4666(7) 0.044(6) Uani 0.347(11) 1 d PDU A 2 H53C H -0.1408 0.0342 0.4655 0.065 Uiso 0.347(11) 1 calc PR A 2 H53D H -0.2493 0.0839 0.4360 0.065 Uiso 0.347(11) 1 calc PR A 2 H53E H -0.3197 0.0395 0.4720 0.065 Uiso 0.347(11) 1 calc PR A 2 C534 C -0.1903(17) 0.0600(7) 0.5532(6) 0.033(4) Uani 0.347(11) 1 d PDU A 2 H53F H -0.1053 0.0308 0.5546 0.049 Uiso 0.347(11) 1 calc PR A 2 H53G H -0.2900 0.0387 0.5483 0.049 Uiso 0.347(11) 1 calc PR A 2 H53H H -0.1797 0.0825 0.5835 0.049 Uiso 0.347(11) 1 calc PR A 2 C311 C 0.4459(4) 0.48221(14) 0.20869(11) 0.0309(8) Uani 1 1 d D B . H31A H 0.5287 0.5129 0.2098 0.037 Uiso 1 1 calc R . . H31B H 0.4980 0.4428 0.2153 0.037 Uiso 1 1 calc R . . C312 C 0.3588(4) 0.48042(16) 0.15755(12) 0.0398(9) Uani 1 1 d D . . H312 H 0.3060 0.5201 0.1507 0.048 Uiso 1 1 calc R B . C313 C 0.4698(5) 0.47148(18) 0.12134(13) 0.0551(11) Uani 1 1 d D B . H31C H 0.4108 0.4708 0.0888 0.083 Uiso 1 1 calc R . . H31D H 0.5252 0.4333 0.1278 0.083 Uiso 1 1 calc R . . H31E H 0.5449 0.5046 0.1241 0.083 Uiso 1 1 calc R . . C314 C 0.2350(5) 0.43195(19) 0.15134(14) 0.0577(12) Uani 1 1 d D B . H31F H 0.1798 0.4328 0.1183 0.087 Uiso 1 1 calc R . . H31G H 0.1612 0.4392 0.1738 0.087 Uiso 1 1 calc R . . H31H H 0.2839 0.3925 0.1580 0.087 Uiso 1 1 calc R . . C321 C 0.1878(12) 0.5603(6) 0.2419(6) 0.024(4) Uani 0.73(2) 1 d PD B 1 H32A H 0.2456 0.5955 0.2323 0.029 Uiso 0.73(2) 1 calc PR B 1 H32B H 0.1180 0.5466 0.2128 0.029 Uiso 0.73(2) 1 calc PR B 1 C322 C 0.0838(12) 0.5828(5) 0.2778(4) 0.027(2) Uani 0.73(2) 1 d PD B 1 H322 H 0.1513 0.5877 0.3097 0.032 Uiso 0.73(2) 1 calc PR B 1 C323 C -0.0444(8) 0.5377(3) 0.2846(4) 0.038(2) Uani 0.73(2) 1 d PD B 1 H32C H -0.0978 0.5510 0.3109 0.056 Uiso 0.73(2) 1 calc PR B 1 H32D H 0.0019 0.4980 0.2922 0.056 Uiso 0.73(2) 1 calc PR B 1 H32E H -0.1192 0.5352 0.2549 0.056 Uiso 0.73(2) 1 calc PR B 1 C324 C 0.0115(19) 0.6439(5) 0.2638(7) 0.042(4) Uani 0.73(2) 1 d PDU B 1 H32F H -0.0400 0.6592 0.2900 0.062 Uiso 0.73(2) 1 calc PR B 1 H32G H -0.0651 0.6396 0.2346 0.062 Uiso 0.73(2) 1 calc PR B 1 H32H H 0.0929 0.6721 0.2577 0.062 Uiso 0.73(2) 1 calc PR B 1 C621 C 0.190(4) 0.5588(17) 0.2368(18) 0.033(13) Uani 0.27(2) 1 d PDU B 2 H62A H 0.2474 0.5965 0.2328 0.039 Uiso 0.27(2) 1 calc PR B 2 H62B H 0.1349 0.5469 0.2048 0.039 Uiso 0.27(2) 1 calc PR B 2 C622 C 0.070(3) 0.5709(12) 0.2705(12) 0.022(7) Uani 0.27(2) 1 d PDU B 2 H622 H 0.1158 0.5624 0.3046 0.027 Uiso 0.27(2) 1 calc PR B 2 C623 C -0.0756(19) 0.5316(7) 0.2555(12) 0.045(5) Uani 0.27(2) 1 d PDU B 2 H62C H -0.1535 0.5409 0.2762 0.067 Uiso 0.27(2) 1 calc PR B 2 H62D H -0.0469 0.4890 0.2589 0.067 Uiso 0.27(2) 1 calc PR B 2 H62E H -0.1188 0.5401 0.2220 0.067 Uiso 0.27(2) 1 calc PR B 2 C624 C 0.016(4) 0.6368(11) 0.2651(15) 0.020(8) Uani 0.27(2) 1 d PDU B 2 H62F H -0.0583 0.6449 0.2873 0.030 Uiso 0.27(2) 1 calc PR B 2 H62G H -0.0347 0.6439 0.2320 0.030 Uiso 0.27(2) 1 calc PR B 2 H62H H 0.1056 0.6635 0.2726 0.030 Uiso 0.27(2) 1 calc PR B 2 C331 C 0.4684(4) 0.52145(13) 0.31498(10) 0.0259(7) Uani 1 1 d D B . H33A H 0.5617 0.5401 0.3049 0.031 Uiso 1 1 calc R . . H33B H 0.4156 0.5531 0.3313 0.031 Uiso 1 1 calc R . . C332 C 0.5236(4) 0.47248(14) 0.35216(11) 0.0301(8) Uani 1 1 d D . . H332 H 0.4293 0.4523 0.3610 0.036 Uiso 1 1 calc R B . C333 C 0.6211(4) 0.42450(14) 0.33192(13) 0.0380(9) Uani 1 1 d D B . H33C H 0.6522 0.3938 0.3565 0.057 Uiso 1 1 calc R . . H33D H 0.7140 0.4432 0.3226 0.057 Uiso 1 1 calc R . . H33E H 0.5597 0.4058 0.3037 0.057 Uiso 1 1 calc R . . C334 C 0.6144(4) 0.49971(15) 0.39813(12) 0.0407(9) Uani 1 1 d D B . H33F H 0.5504 0.5302 0.4109 0.061 Uiso 1 1 calc R . . H33G H 0.7100 0.5184 0.3907 0.061 Uiso 1 1 calc R . . H33H H 0.6408 0.4679 0.4221 0.061 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 0.0253(5) 0.0213(5) 0.0226(4) 0.0046(4) 0.0066(4) -0.0026(4) Si2 0.0297(5) 0.0263(5) 0.0256(5) 0.0027(4) 0.0086(4) -0.0016(4) Si3 0.0242(5) 0.0232(5) 0.0290(5) 0.0035(4) 0.0073(4) 0.0000(4) N1 0.0187(13) 0.0200(14) 0.0174(13) -0.0001(10) 0.0030(11) 0.0011(11) N2 0.0197(14) 0.0169(13) 0.0186(13) 0.0020(10) 0.0025(11) 0.0013(11) C1 0.0276(18) 0.0255(18) 0.0216(16) 0.0010(14) 0.0052(15) -0.0021(15) C2 0.035(2) 0.0260(18) 0.0313(18) -0.0006(15) 0.0042(17) 0.0020(16) C3 0.0240(18) 0.0281(18) 0.0244(17) -0.0014(14) 0.0034(14) 0.0002(15) C11 0.0225(17) 0.0210(16) 0.0179(15) -0.0029(13) 0.0042(13) 0.0010(14) C22 0.0310(19) 0.0209(17) 0.0260(17) -0.0057(14) 0.0079(16) 0.0021(15) C33 0.0247(18) 0.0232(17) 0.0182(15) -0.0041(13) 0.0029(14) 0.0005(14) C40 0.0282(18) 0.0243(17) 0.0190(15) -0.0059(13) 0.0102(14) -0.0021(14) C41 0.0306(19) 0.0223(17) 0.0254(17) -0.0073(13) 0.0084(15) -0.0056(14) C42 0.0199(16) 0.0239(17) 0.0188(15) 0.0034(13) 0.0051(13) 0.0013(13) C43 0.0238(17) 0.0196(16) 0.0252(16) 0.0019(13) 0.0069(14) 0.0011(14) C44 0.0178(16) 0.0178(16) 0.0188(15) 0.0022(12) 0.0023(13) 0.0026(13) C45 0.0215(17) 0.0193(16) 0.0166(15) 0.0004(12) 0.0044(13) 0.0018(13) C46 0.0161(16) 0.0199(16) 0.0165(15) 0.0020(12) 0.0015(13) 0.0029(13) C47 0.0147(15) 0.0207(16) 0.0163(14) 0.0020(12) 0.0025(12) 0.0022(13) C48 0.0207(16) 0.0216(16) 0.0131(14) 0.0026(12) 0.0041(13) 0.0041(13) C49 0.0170(16) 0.0171(15) 0.0167(15) 0.0022(12) 0.0018(13) 0.0013(13) C50 0.0183(16) 0.0177(15) 0.0161(15) 0.0033(12) 0.0047(13) 0.0008(13) C51 0.0165(16) 0.0167(15) 0.0158(14) 0.0024(11) 0.0024(12) 0.0007(12) C52 0.0171(16) 0.0168(15) 0.0191(15) 0.0022(12) 0.0031(13) -0.0006(13) C53 0.0148(16) 0.0209(16) 0.0169(15) 0.0032(12) 0.0011(13) 0.0025(13) C111 0.0227(17) 0.0242(17) 0.0247(16) 0.0010(13) 0.0060(14) -0.0056(14) C112 0.0240(18) 0.0301(18) 0.0280(17) 0.0002(14) 0.0060(15) -0.0007(15) C113 0.030(2) 0.047(2) 0.044(2) 0.0053(18) 0.0071(17) -0.0055(17) C114 0.031(2) 0.045(2) 0.0374(19) 0.0057(17) 0.0013(16) 0.0049(17) C121 0.0284(19) 0.0263(17) 0.0237(17) 0.0065(13) 0.0063(15) 0.0002(15) C122 0.0258(18) 0.0311(19) 0.0280(17) 0.0069(14) 0.0063(15) 0.0027(15) C123 0.0287(19) 0.041(2) 0.0342(19) 0.0067(16) 0.0045(16) 0.0089(16) C124 0.035(2) 0.031(2) 0.041(2) 0.0006(16) 0.0006(17) 0.0051(16) C131 0.0298(18) 0.0230(17) 0.0237(16) 0.0046(13) 0.0059(15) -0.0020(14) C132 0.0308(19) 0.0343(19) 0.0253(17) 0.0017(14) 0.0109(15) -0.0012(15) C133 0.067(3) 0.033(2) 0.040(2) 0.0095(17) 0.030(2) 0.0001(19) C134 0.041(2) 0.046(2) 0.0316(19) -0.0010(16) 0.0124(17) 0.0008(18) C211 0.038(2) 0.0299(19) 0.0330(19) 0.0046(15) 0.0027(17) -0.0032(16) C212 0.034(2) 0.046(2) 0.040(2) 0.0051(17) 0.0006(17) -0.0070(18) C213 0.042(2) 0.065(3) 0.049(2) 0.007(2) -0.002(2) -0.016(2) C214 0.045(2) 0.082(3) 0.042(2) 0.019(2) 0.010(2) -0.016(2) C221 0.0281(18) 0.0272(18) 0.0248(17) 0.0019(13) 0.0084(15) 0.0005(15) C222 0.0291(19) 0.0318(19) 0.0239(17) 0.0043(14) 0.0036(15) 0.0007(15) C223 0.034(2) 0.0343(19) 0.0266(17) 0.0062(14) 0.0004(16) 0.0014(16) C224 0.0284(19) 0.0337(19) 0.0298(17) 0.0075(14) 0.0060(15) 0.0025(15) C231 0.019(4) 0.017(4) 0.014(4) 0.002(3) 0.006(3) -0.001(3) C232 0.029(4) 0.038(4) 0.035(3) -0.001(3) 0.001(3) -0.001(3) C233 0.098(8) 0.071(6) 0.039(4) -0.004(4) -0.006(5) 0.060(6) C234 0.033(6) 0.064(7) 0.040(4) -0.006(4) 0.001(4) 0.012(5) C531 0.070(15) 0.072(15) 0.080(15) 0.003(10) 0.011(10) -0.001(10) C532 0.025(7) 0.037(7) 0.036(6) -0.005(5) -0.004(5) 0.013(6) C533 0.042(10) 0.035(7) 0.051(8) -0.013(6) -0.004(7) 0.007(7) C534 0.019(6) 0.036(6) 0.037(6) 0.001(5) -0.018(5) -0.009(5) C311 0.0307(19) 0.0268(18) 0.0371(19) 0.0069(15) 0.0114(16) 0.0019(15) C312 0.046(2) 0.044(2) 0.033(2) 0.0045(16) 0.0162(18) 0.0111(18) C313 0.072(3) 0.052(3) 0.049(2) 0.017(2) 0.033(2) 0.018(2) C314 0.053(3) 0.082(3) 0.039(2) -0.014(2) 0.008(2) -0.016(2) C321 0.025(6) 0.023(5) 0.023(5) 0.005(4) 0.003(3) -0.003(3) C322 0.029(4) 0.030(5) 0.023(4) 0.004(4) 0.010(3) 0.003(3) C323 0.035(4) 0.028(3) 0.053(5) 0.009(3) 0.017(4) 0.004(2) C324 0.041(6) 0.034(5) 0.052(6) 0.008(4) 0.013(4) 0.007(4) C621 0.034(16) 0.036(15) 0.030(14) -0.006(8) 0.014(9) -0.001(9) C622 0.023(10) 0.019(10) 0.022(10) -0.003(7) -0.008(7) 0.008(7) C623 0.030(8) 0.036(7) 0.071(11) 0.004(8) 0.018(8) -0.006(6) C624 0.013(11) 0.020(10) 0.030(11) -0.012(8) 0.011(8) -0.005(7) C331 0.0235(18) 0.0210(17) 0.0334(18) 0.0033(13) 0.0048(15) -0.0012(14) C332 0.0263(19) 0.0268(18) 0.0361(19) 0.0049(15) 0.0010(16) -0.0011(15) C333 0.029(2) 0.0280(19) 0.056(2) 0.0036(17) 0.0017(18) 0.0054(16) C334 0.036(2) 0.033(2) 0.048(2) 0.0061(17) -0.0099(18) -0.0025(17) _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 1.848(3) . ? Si1 C111 1.871(3) . ? Si1 C121 1.876(3) . ? Si1 C131 1.885(3) . ? Si2 C2 1.845(4) . ? Si2 C531 1.866(13) . ? Si2 C211 1.877(3) . ? Si2 C221 1.880(3) . ? Si2 C231 1.881(5) . ? Si3 C3 1.842(3) . ? Si3 C311 1.874(3) . ? Si3 C621 1.876(15) . ? Si3 C331 1.882(3) . ? Si3 C321 1.885(6) . ? N1 C46 1.325(4) . ? N1 C44 1.350(3) . ? N2 C47 1.327(3) . ? N2 C45 1.353(4) . ? C1 C11 1.199(4) . ? C2 C22 1.187(4) . ? C3 C33 1.197(4) . ? C11 C50 1.448(4) . ? C22 C43 1.433(4) . ? C33 C42 1.434(4) . ? C40 C42 1.382(4) . ? C40 C41 1.403(4) . ? C40 H40 0.9500 . ? C41 C43 1.372(4) . ? C41 H41 0.9500 . ? C42 C44 1.431(4) . ? C43 C45 1.434(4) . ? C44 C45 1.419(4) . ? C46 C47 1.429(4) . ? C46 C49 1.464(4) . ? C47 C53 1.459(4) 3_566 ? C48 C49 1.396(4) . ? C48 C50 1.397(4) . ? C48 H48 0.9500 . ? C49 C51 1.413(4) . ? C50 C52 1.398(4) . ? C51 C53 1.413(4) . ? C51 C51 1.443(5) 3_566 ? C52 C53 1.395(4) . ? C52 H52 0.9500 . ? C53 C47 1.459(4) 3_566 ? C111 C112 1.526(4) . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C112 C113 1.520(4) . ? C112 C114 1.524(4) . ? C112 H112 1.0000 . ? C113 H11C 0.9800 . ? C113 H11D 0.9800 . ? C113 H11E 0.9800 . ? C114 H11F 0.9800 . ? C114 H11G 0.9800 . ? C114 H11H 0.9800 . ? C121 C122 1.537(4) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 C124 1.512(4) . ? C122 C123 1.542(4) . ? C122 H122 1.0000 . ? C123 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C124 H12F 0.9800 . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C131 C132 1.531(4) . ? C131 H13A 0.9900 . ? C131 H13B 0.9900 . ? C132 C133 1.522(4) . ? C132 C134 1.527(4) . ? C132 H132 1.0000 . ? C133 H13C 0.9800 . ? C133 H13D 0.9800 . ? C133 H13E 0.9800 . ? C134 H13F 0.9800 . ? C134 H13G 0.9800 . ? C134 H13H 0.9800 . ? C211 C212 1.532(5) . ? C211 H21A 0.9900 . ? C211 H21B 0.9900 . ? C212 C213 1.534(4) . ? C212 C214 1.538(5) . ? C212 H212 1.0000 . ? C213 H21C 0.9800 . ? C213 H21D 0.9800 . ? C213 H21E 0.9800 . ? C214 H21F 0.9800 . ? C214 H21G 0.9800 . ? C214 H21H 0.9800 . ? C221 C222 1.542(4) . ? C221 H22A 0.9900 . ? C221 H22B 0.9900 . ? C222 C223 1.533(4) . ? C222 C224 1.535(4) . ? C222 H222 1.0000 . ? C223 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C224 H22F 0.9800 . ? C224 H22G 0.9800 . ? C224 H22H 0.9800 . ? C231 C232 1.541(8) . ? C231 H23A 0.9900 . ? C231 H23B 0.9900 . ? C232 C234 1.502(10) . ? C232 C233 1.688(9) . ? C232 H232 1.0000 . ? C233 H23C 0.9800 . ? C233 H23D 0.9800 . ? C233 H23E 0.9800 . ? C234 H23F 0.9800 . ? C234 H23G 0.9800 . ? C234 H23H 0.9800 . ? C531 C532 1.544(14) . ? C531 H53A 0.9900 . ? C531 H53B 0.9900 . ? C532 C533 1.540(14) . ? C532 C534 1.663(13) . ? C532 H532 1.0000 . ? C533 H53C 0.9800 . ? C533 H53D 0.9800 . ? C533 H53E 0.9800 . ? C534 H53F 0.9800 . ? C534 H53G 0.9800 . ? C534 H53H 0.9800 . ? C311 C312 1.522(4) . ? C311 H31A 0.9900 . ? C311 H31B 0.9900 . ? C312 C314 1.515(5) . ? C312 C313 1.520(5) . ? C312 H312 1.0000 . ? C313 H31C 0.9800 . ? C313 H31D 0.9800 . ? C313 H31E 0.9800 . ? C314 H31F 0.9800 . ? C314 H31G 0.9800 . ? C314 H31H 0.9800 . ? C321 C322 1.541(9) . ? C321 H32A 0.9900 . ? C321 H32B 0.9900 . ? C322 C324 1.522(9) . ? C322 C323 1.534(8) . ? C322 H322 1.0000 . ? C323 H32C 0.9800 . ? C323 H32D 0.9800 . ? C323 H32E 0.9800 . ? C324 H32F 0.9800 . ? C324 H32G 0.9800 . ? C324 H32H 0.9800 . ? C621 C622 1.540(15) . ? C621 H62A 0.9900 . ? C621 H62B 0.9900 . ? C622 C624 1.539(14) . ? C622 C623 1.543(15) . ? C622 H622 1.0000 . ? C623 H62C 0.9800 . ? C623 H62D 0.9800 . ? C623 H62E 0.9800 . ? C624 H62F 0.9800 . ? C624 H62G 0.9800 . ? C624 H62H 0.9800 . ? C331 C332 1.535(4) . ? C331 H33A 0.9900 . ? C331 H33B 0.9900 . ? C332 C333 1.526(4) . ? C332 C334 1.534(4) . ? C332 H332 1.0000 . ? C333 H33C 0.9800 . ? C333 H33D 0.9800 . ? C333 H33E 0.9800 . ? C334 H33F 0.9800 . ? C334 H33G 0.9800 . ? C334 H33H 0.9800 . ? 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 C111 111.29(14) . . ? C1 Si1 C121 109.19(13) . . ? C111 Si1 C121 104.11(13) . . ? C1 Si1 C131 104.61(13) . . ? C111 Si1 C131 112.79(14) . . ? C121 Si1 C131 114.96(15) . . ? C2 Si2 C531 110.0(8) . . ? C2 Si2 C211 107.04(15) . . ? C531 Si2 C211 112.4(10) . . ? C2 Si2 C221 106.20(14) . . ? C531 Si2 C221 108.0(6) . . ? C211 Si2 C221 113.07(15) . . ? C2 Si2 C231 107.8(3) . . ? C531 Si2 C231 2.5(13) . . ? C211 Si2 C231 114.4(3) . . ? C221 Si2 C231 107.8(2) . . ? C3 Si3 C311 111.43(14) . . ? C3 Si3 C621 110.1(12) . . ? C311 Si3 C621 106.3(12) . . ? C3 Si3 C331 105.61(13) . . ? C311 Si3 C331 110.89(15) . . ? C621 Si3 C331 112.6(19) . . ? C3 Si3 C321 109.0(4) . . ? C311 Si3 C321 110.7(4) . . ? C621 Si3 C321 5(2) . . ? C331 Si3 C321 109.1(6) . . ? C46 N1 C44 117.3(2) . . ? C47 N2 C45 117.5(2) . . ? C11 C1 Si1 178.6(3) . . ? C22 C2 Si2 167.9(3) . . ? C33 C3 Si3 168.6(3) . . ? C1 C11 C50 176.9(3) . . ? C2 C22 C43 173.7(3) . . ? C3 C33 C42 173.4(3) . . ? C42 C40 C41 121.7(3) . . ? C42 C40 H40 119.1 . . ? C41 C40 H40 119.1 . . ? C43 C41 C40 121.5(3) . . ? C43 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C40 C42 C44 118.4(3) . . ? C40 C42 C33 123.5(3) . . ? C44 C42 C33 118.0(3) . . ? C41 C43 C22 123.2(3) . . ? C41 C43 C45 118.6(3) . . ? C22 C43 C45 118.2(3) . . ? N1 C44 C45 121.2(3) . . ? N1 C44 C42 119.1(3) . . ? C45 C44 C42 119.7(3) . . ? N2 C45 C44 121.0(3) . . ? N2 C45 C43 118.9(3) . . ? C44 C45 C43 120.0(3) . . ? N1 C46 C47 121.8(3) . . ? N1 C46 C49 118.8(2) . . ? C47 C46 C49 119.4(3) . . ? N2 C47 C46 121.3(3) . . ? N2 C47 C53 118.4(2) . 3_566 ? C46 C47 C53 120.3(3) . 3_566 ? C49 C48 C50 121.0(3) . . ? C49 C48 H48 119.5 . . ? C50 C48 H48 119.5 . . ? C48 C49 C51 120.2(3) . . ? C48 C49 C46 120.4(3) . . ? C51 C49 C46 119.3(2) . . ? C48 C50 C52 119.0(3) . . ? C48 C50 C11 121.9(3) . . ? C52 C50 C11 119.2(2) . . ? C49 C51 C53 118.6(3) . . ? C49 C51 C51 121.1(3) . 3_566 ? C53 C51 C51 120.3(3) . 3_566 ? C53 C52 C50 120.9(3) . . ? C53 C52 H52 119.5 . . ? C50 C52 H52 119.5 . . ? C52 C53 C51 120.3(3) . . ? C52 C53 C47 120.2(3) . 3_566 ? C51 C53 C47 119.5(3) . 3_566 ? C112 C111 Si1 121.6(2) . . ? C112 C111 H11A 106.9 . . ? Si1 C111 H11A 106.9 . . ? C112 C111 H11B 106.9 . . ? Si1 C111 H11B 106.9 . . ? H11A C111 H11B 106.7 . . ? C113 C112 C114 110.1(3) . . ? C113 C112 C111 111.5(2) . . ? C114 C112 C111 110.6(3) . . ? C113 C112 H112 108.2 . . ? C114 C112 H112 108.2 . . ? C111 C112 H112 108.2 . . ? C112 C113 H11C 109.5 . . ? C112 C113 H11D 109.5 . . ? H11C C113 H11D 109.5 . . ? C112 C113 H11E 109.5 . . ? H11C C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? C112 C114 H11F 109.5 . . ? C112 C114 H11G 109.5 . . ? H11F C114 H11G 109.5 . . ? C112 C114 H11H 109.5 . . ? H11F C114 H11H 109.5 . . ? H11G C114 H11H 109.5 . . ? C122 C121 Si1 119.4(2) . . ? C122 C121 H12A 107.5 . . ? Si1 C121 H12A 107.5 . . ? C122 C121 H12B 107.5 . . ? Si1 C121 H12B 107.5 . . ? H12A C121 H12B 107.0 . . ? C124 C122 C121 112.5(3) . . ? C124 C122 C123 110.6(3) . . ? C121 C122 C123 110.6(2) . . ? C124 C122 H122 107.7 . . ? C121 C122 H122 107.7 . . ? C123 C122 H122 107.7 . . ? C122 C123 H12C 109.5 . . ? C122 C123 H12D 109.5 . . ? H12C C123 H12D 109.5 . . ? C122 C123 H12E 109.5 . . ? H12C C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C122 C124 H12F 109.5 . . ? C122 C124 H12G 109.5 . . ? H12F C124 H12G 109.5 . . ? C122 C124 H12H 109.5 . . ? H12F C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? C132 C131 Si1 119.6(2) . . ? C132 C131 H13A 107.4 . . ? Si1 C131 H13A 107.4 . . ? C132 C131 H13B 107.4 . . ? Si1 C131 H13B 107.4 . . ? H13A C131 H13B 107.0 . . ? C133 C132 C134 109.5(3) . . ? C133 C132 C131 112.5(3) . . ? C134 C132 C131 110.2(3) . . ? C133 C132 H132 108.1 . . ? C134 C132 H132 108.1 . . ? C131 C132 H132 108.1 . . ? C132 C133 H13C 109.5 . . ? C132 C133 H13D 109.5 . . ? H13C C133 H13D 109.5 . . ? C132 C133 H13E 109.5 . . ? H13C C133 H13E 109.5 . . ? H13D C133 H13E 109.5 . . ? C132 C134 H13F 109.5 . . ? C132 C134 H13G 109.5 . . ? H13F C134 H13G 109.5 . . ? C132 C134 H13H 109.5 . . ? H13F C134 H13H 109.5 . . ? H13G C134 H13H 109.5 . . ? C212 C211 Si2 117.8(2) . . ? C212 C211 H21A 107.9 . . ? Si2 C211 H21A 107.9 . . ? C212 C211 H21B 107.9 . . ? Si2 C211 H21B 107.9 . . ? H21A C211 H21B 107.2 . . ? C211 C212 C213 110.5(3) . . ? C211 C212 C214 110.4(3) . . ? C213 C212 C214 112.0(3) . . ? C211 C212 H212 107.9 . . ? C213 C212 H212 107.9 . . ? C214 C212 H212 107.9 . . ? C212 C213 H21C 109.5 . . ? C212 C213 H21D 109.5 . . ? H21C C213 H21D 109.5 . . ? C212 C213 H21E 109.5 . . ? H21C C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? C212 C214 H21F 109.5 . . ? C212 C214 H21G 109.5 . . ? H21F C214 H21G 109.5 . . ? C212 C214 H21H 109.5 . . ? H21F C214 H21H 109.5 . . ? H21G C214 H21H 109.5 . . ? C222 C221 Si2 118.0(2) . . ? C222 C221 H22A 107.8 . . ? Si2 C221 H22A 107.8 . . ? C222 C221 H22B 107.8 . . ? Si2 C221 H22B 107.8 . . ? H22A C221 H22B 107.1 . . ? C223 C222 C224 110.7(3) . . ? C223 C222 C221 112.6(2) . . ? C224 C222 C221 111.2(2) . . ? C223 C222 H222 107.4 . . ? C224 C222 H222 107.4 . . ? C221 C222 H222 107.4 . . ? C222 C223 H22C 109.5 . . ? C222 C223 H22D 109.5 . . ? H22C C223 H22D 109.5 . . ? C222 C223 H22E 109.5 . . ? H22C C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C222 C224 H22F 109.5 . . ? C222 C224 H22G 109.5 . . ? H22F C224 H22G 109.5 . . ? C222 C224 H22H 109.5 . . ? H22F C224 H22H 109.5 . . ? H22G C224 H22H 109.5 . . ? C232 C231 Si2 119.0(5) . . ? C232 C231 H23A 107.6 . . ? Si2 C231 H23A 107.6 . . ? C232 C231 H23B 107.6 . . ? Si2 C231 H23B 107.6 . . ? H23A C231 H23B 107.0 . . ? C234 C232 C231 113.8(8) . . ? C234 C232 C233 101.2(7) . . ? C231 C232 C233 101.8(6) . . ? C234 C232 H232 113.0 . . ? C231 C232 H232 113.0 . . ? C233 C232 H232 113.0 . . ? C232 C233 H23C 109.5 . . ? C232 C233 H23D 109.5 . . ? H23C C233 H23D 109.5 . . ? C232 C233 H23E 109.5 . . ? H23C C233 H23E 109.5 . . ? H23D C233 H23E 109.5 . . ? C232 C234 H23F 109.5 . . ? C232 C234 H23G 109.5 . . ? H23F C234 H23G 109.5 . . ? C232 C234 H23H 109.5 . . ? H23F C234 H23H 109.5 . . ? H23G C234 H23H 109.5 . . ? C532 C531 Si2 120.0(12) . . ? C532 C531 H53A 107.3 . . ? Si2 C531 H53A 107.3 . . ? C532 C531 H53B 107.3 . . ? Si2 C531 H53B 107.3 . . ? H53A C531 H53B 106.9 . . ? C533 C532 C531 108.1(14) . . ? C533 C532 C534 97.6(12) . . ? C531 C532 C534 101.0(11) . . ? C533 C532 H532 115.9 . . ? C531 C532 H532 115.9 . . ? C534 C532 H532 115.9 . . ? C532 C533 H53C 109.5 . . ? C532 C533 H53D 109.5 . . ? H53C C533 H53D 109.5 . . ? C532 C533 H53E 109.5 . . ? H53C C533 H53E 109.5 . . ? H53D C533 H53E 109.5 . . ? C532 C534 H53F 109.5 . . ? C532 C534 H53G 109.5 . . ? H53F C534 H53G 109.5 . . ? C532 C534 H53H 109.5 . . ? H53F C534 H53H 109.5 . . ? H53G C534 H53H 109.5 . . ? C312 C311 Si3 118.7(2) . . ? C312 C311 H31A 107.6 . . ? Si3 C311 H31A 107.6 . . ? C312 C311 H31B 107.6 . . ? Si3 C311 H31B 107.6 . . ? H31A C311 H31B 107.1 . . ? C314 C312 C313 110.1(3) . . ? C314 C312 C311 111.8(3) . . ? C313 C312 C311 111.2(3) . . ? C314 C312 H312 107.9 . . ? C313 C312 H312 107.9 . . ? C311 C312 H312 107.9 . . ? C312 C313 H31C 109.5 . . ? C312 C313 H31D 109.5 . . ? H31C C313 H31D 109.5 . . ? C312 C313 H31E 109.5 . . ? H31C C313 H31E 109.5 . . ? H31D C313 H31E 109.5 . . ? C312 C314 H31F 109.5 . . ? C312 C314 H31G 109.5 . . ? H31F C314 H31G 109.5 . . ? C312 C314 H31H 109.5 . . ? H31F C314 H31H 109.5 . . ? H31G C314 H31H 109.5 . . ? C322 C321 Si3 120.6(8) . . ? C322 C321 H32A 107.2 . . ? Si3 C321 H32A 107.2 . . ? C322 C321 H32B 107.2 . . ? Si3 C321 H32B 107.2 . . ? H32A C321 H32B 106.8 . . ? C324 C322 C323 109.6(8) . . ? C324 C322 C321 112.4(8) . . ? C323 C322 C321 112.3(8) . . ? C324 C322 H322 107.4 . . ? C323 C322 H322 107.4 . . ? C321 C322 H322 107.4 . . ? C322 C323 H32C 109.5 . . ? C322 C323 H32D 109.5 . . ? H32C C323 H32D 109.5 . . ? C322 C323 H32E 109.5 . . ? H32C C323 H32E 109.5 . . ? H32D C323 H32E 109.5 . . ? C322 C324 H32F 109.5 . . ? C322 C324 H32G 109.5 . . ? H32F C324 H32G 109.5 . . ? C322 C324 H32H 109.5 . . ? H32F C324 H32H 109.5 . . ? H32G C324 H32H 109.5 . . ? C622 C621 Si3 114(2) . . ? C622 C621 H62A 108.8 . . ? Si3 C621 H62A 108.8 . . ? C622 C621 H62B 108.8 . . ? Si3 C621 H62B 108.8 . . ? H62A C621 H62B 107.7 . . ? C624 C622 C621 109.5(18) . . ? C624 C622 C623 106.5(17) . . ? C621 C622 C623 110(2) . . ? C624 C622 H622 110.3 . . ? C621 C622 H622 110.3 . . ? C623 C622 H622 110.3 . . ? C622 C623 H62C 109.5 . . ? C622 C623 H62D 109.5 . . ? H62C C623 H62D 109.5 . . ? C622 C623 H62E 109.5 . . ? H62C C623 H62E 109.5 . . ? H62D C623 H62E 109.5 . . ? C622 C624 H62F 109.5 . . ? C622 C624 H62G 109.5 . . ? H62F C624 H62G 109.5 . . ? C622 C624 H62H 109.5 . . ? H62F C624 H62H 109.5 . . ? H62G C624 H62H 109.5 . . ? C332 C331 Si3 117.8(2) . . ? C332 C331 H33A 107.8 . . ? Si3 C331 H33A 107.8 . . ? C332 C331 H33B 107.8 . . ? Si3 C331 H33B 107.8 . . ? H33A C331 H33B 107.2 . . ? C333 C332 C334 110.2(3) . . ? C333 C332 C331 112.0(3) . . ? C334 C332 C331 111.3(3) . . ? C333 C332 H332 107.7 . . ? C334 C332 H332 107.7 . . ? C331 C332 H332 107.7 . . ? C332 C333 H33C 109.5 . . ? C332 C333 H33D 109.5 . . ? H33C C333 H33D 109.5 . . ? C332 C333 H33E 109.5 . . ? H33C C333 H33E 109.5 . . ? H33D C333 H33E 109.5 . . ? C332 C334 H33F 109.5 . . ? C332 C334 H33G 109.5 . . ? H33F C334 H33G 109.5 . . ? C332 C334 H33H 109.5 . . ? H33F C334 H33H 109.5 . . ? H33G C334 H33H 109.5 . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.867 _refine_diff_density_max 0.290 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.060 _database_code_depnum_ccdc_archive 'CCDC 972122' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_spm369 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C148 H98 N4 Si6' _chemical_formula_weight 2100.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 '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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/a 1' _space_group_name_Hall '-P 2yab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.4521(4) _cell_length_b 19.5717(5) _cell_length_c 20.2714(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.5443(16) _cell_angle_gamma 90.00 _cell_volume 6784.0(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5839 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 23.236 _cell_measurement_theta_min 2.300 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. R(int) was 0.1407 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.8994. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1098 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _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 ? _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 11305 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 24.53 _reflns_number_total 11305 _reflns_number_gt 7708 _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^)+(0.1061P)^2^+0.7623P] 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 11305 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _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 0.36120(5) 0.76414(4) 0.90772(4) 0.0271(2) Uani 1 1 d . . . Si2 Si 0.18766(5) 0.65525(4) 1.17294(4) 0.0284(2) Uani 1 1 d . . . Si3 Si -0.14563(5) 1.07878(5) 0.57484(4) 0.0337(2) Uani 1 1 d . . . N1 N 0.00994(12) 1.00065(11) 0.81080(10) 0.0181(5) Uani 1 1 d . . . N2 N 0.11346(12) 0.90323(11) 0.88289(10) 0.0179(5) Uani 1 1 d . . . C1 C 0.27798(18) 0.80741(15) 0.85440(15) 0.0282(7) Uani 1 1 d . . . C2 C 0.22476(17) 0.83886(15) 0.82143(14) 0.0250(7) Uani 1 1 d . . . C3 C 0.16280(16) 0.87837(15) 0.78325(14) 0.0244(7) Uani 1 1 d . . . C4 C 0.15406(18) 0.88574(17) 0.71454(15) 0.0356(8) Uani 1 1 d . . . H4A H 0.1900 0.8637 0.6920 0.043 Uiso 1 1 calc R . . C5 C 0.09364(18) 0.92489(17) 0.67732(15) 0.0356(8) Uani 1 1 d . . . H5A H 0.0876 0.9265 0.6297 0.043 Uiso 1 1 calc R . . C6 C 0.04272(16) 0.96106(15) 0.70754(14) 0.0249(7) Uani 1 1 d . . . C7 C -0.02016(17) 0.99940(15) 0.66837(14) 0.0259(7) Uani 1 1 d . . . C8 C -0.07229(19) 1.02861(17) 0.63229(15) 0.0342(8) Uani 1 1 d . . . C9 C 0.05343(15) 0.95926(14) 0.77944(13) 0.0198(6) Uani 1 1 d . . . C10 C 0.10977(15) 0.91409(13) 0.81669(13) 0.0185(6) Uani 1 1 d . . . C11 C 0.06630(14) 0.94090(13) 0.91259(13) 0.0166(6) Uani 1 1 d . . . C12 C 0.01972(15) 0.99377(13) 0.87739(13) 0.0173(6) Uani 1 1 d . . . C13 C 0.09862(15) 0.86902(13) 1.01500(13) 0.0189(6) Uani 1 1 d . . . H13A H 0.1263 0.8389 0.9913 0.023 Uiso 1 1 calc R . . C14 C 0.06309(15) 0.92630(13) 0.98265(13) 0.0166(6) Uani 1 1 d . . . C15 C 0.02038(14) 0.97098(13) 1.01706(12) 0.0158(6) Uani 1 1 d . . . C16 C 0.09480(15) 0.85434(13) 1.08158(13) 0.0184(6) Uani 1 1 d . . . C17 C 0.12761(16) 0.79160(14) 1.11254(13) 0.0204(6) Uani 1 1 d . . . C18 C 0.15480(16) 0.73858(15) 1.13592(14) 0.0243(7) Uani 1 1 d . . . C19 C 0.05751(15) 0.90055(13) 1.11722(13) 0.0185(6) Uani 1 1 d . . . H19A H 0.0574 0.8925 1.1634 0.022 Uiso 1 1 calc R . . C20 C 0.02043(14) 0.95833(13) 1.08567(13) 0.0162(6) Uani 1 1 d . . . C111 C 0.34436(13) 0.66973(9) 0.90088(12) 0.0368(8) Uani 1 1 d G . . C112 C 0.35040(14) 0.63483(12) 0.84242(11) 0.0516(10) Uani 1 1 d G . . H11A H 0.3697 0.6576 0.8077 0.062 Uiso 1 1 calc R . . C113 C 0.32823(16) 0.56662(12) 0.83478(14) 0.0728(14) Uani 1 1 d G . . H11B H 0.3324 0.5428 0.7948 0.087 Uiso 1 1 calc R . . C114 C 0.30002(15) 0.53330(9) 0.88561(19) 0.0792(17) Uani 1 1 d G . . H11C H 0.2849 0.4867 0.8804 0.095 Uiso 1 1 calc R . . C115 C 0.29397(15) 0.56819(14) 0.94407(16) 0.0805(16) Uani 1 1 d G . . H11D H 0.2747 0.5454 0.9788 0.097 Uiso 1 1 calc R . . C116 C 0.31614(15) 0.63641(13) 0.95171(11) 0.0562(11) Uani 1 1 d G . . H11E H 0.3120 0.6603 0.9917 0.067 Uiso 1 1 calc R . . C121 C 0.45168(9) 0.79298(10) 0.87840(12) 0.0299(7) Uani 1 1 d G . . C122 C 0.45600(11) 0.85942(10) 0.85518(14) 0.0512(10) Uani 1 1 d G . . H12B H 0.4115 0.8884 0.8496 0.061 Uiso 1 1 calc R . . C123 C 0.52547(13) 0.88349(9) 0.84015(15) 0.0646(12) Uani 1 1 d G . . H12C H 0.5284 0.9289 0.8243 0.077 Uiso 1 1 calc R . . C124 C 0.59061(10) 0.84113(11) 0.84836(14) 0.0554(11) Uani 1 1 d G . . H12D H 0.6381 0.8576 0.8381 0.066 Uiso 1 1 calc R . . C125 C 0.58630(9) 0.77469(10) 0.87158(13) 0.0449(9) Uani 1 1 d G . . H12E H 0.6308 0.7457 0.8772 0.054 Uiso 1 1 calc R . . C126 C 0.51683(11) 0.75062(8) 0.88661(11) 0.0348(8) Uani 1 1 d G . . H12F H 0.5139 0.7052 0.9025 0.042 Uiso 1 1 calc R . . C131 C 0.36609(11) 0.79399(11) 0.99685(8) 0.0303(7) Uani 1 1 d G . . C132 C 0.43794(9) 0.79391(12) 1.04129(10) 0.0407(8) Uani 1 1 d G . . H13B H 0.4828 0.7757 1.0276 0.049 Uiso 1 1 calc R . . C133 C 0.44420(9) 0.82044(13) 1.10576(9) 0.0478(9) Uani 1 1 d G . . H13C H 0.4933 0.8204 1.1361 0.057 Uiso 1 1 calc R . . C134 C 0.37861(12) 0.84705(13) 1.12578(8) 0.0493(10) Uani 1 1 d G . . H13D H 0.3829 0.8652 1.1698 0.059 Uiso 1 1 calc R . . C135 C 0.30676(10) 0.84713(12) 1.08133(10) 0.0412(9) Uani 1 1 d G . . H13E H 0.2619 0.8653 1.0950 0.049 Uiso 1 1 calc R . . C136 C 0.30050(8) 0.82060(12) 1.01686(9) 0.0346(8) Uani 1 1 d G . . H13F H 0.2514 0.8207 0.9865 0.041 Uiso 1 1 calc R . . C211 C -0.09141(14) 1.14762(12) 0.53717(12) 0.0418(9) Uani 1 1 d G . . C212 C -0.11303(16) 1.21601(14) 0.53664(15) 0.0763(14) Uani 1 1 d G . . H21A H -0.1569 1.2293 0.5548 0.092 Uiso 1 1 calc R . . C213 C -0.0704(2) 1.26490(11) 0.50959(17) 0.0986(18) Uani 1 1 d G . . H21B H -0.0852 1.3116 0.5092 0.118 Uiso 1 1 calc R . . C214 C -0.0062(2) 1.24540(16) 0.48307(16) 0.0898(17) Uani 1 1 d G . . H21C H 0.0229 1.2788 0.4646 0.108 Uiso 1 1 calc R . . C215 C 0.01542(15) 1.17701(18) 0.48360(14) 0.0774(14) Uani 1 1 d G . . H21D H 0.0593 1.1637 0.4655 0.093 Uiso 1 1 calc R . . C216 C -0.02718(15) 1.12812(13) 0.51065(13) 0.0598(11) Uani 1 1 d G . . H21E H -0.0124 1.0814 0.5110 0.072 Uiso 1 1 calc R . . C221 C -0.19745(13) 1.02031(12) 0.50710(10) 0.0387(8) Uani 1 1 d G . . C222 C -0.20452(17) 0.95119(13) 0.52048(11) 0.0711(13) Uani 1 1 d G . . H22A H -0.1797 0.9329 0.5628 0.085 Uiso 1 1 calc R . . C223 C -0.2478(2) 0.90877(11) 0.47191(15) 0.0890(16) Uani 1 1 d G . . H22B H -0.2527 0.8615 0.4811 0.107 Uiso 1 1 calc R . . C224 C -0.28408(16) 0.93547(15) 0.40997(13) 0.0706(13) Uani 1 1 d G . . H22C H -0.3137 0.9065 0.3768 0.085 Uiso 1 1 calc R . . C225 C -0.27701(16) 1.00459(16) 0.39659(10) 0.0758(14) Uani 1 1 d G . . H22D H -0.3018 1.0228 0.3543 0.091 Uiso 1 1 calc R . . C226 C -0.23370(16) 1.04702(12) 0.44516(12) 0.0621(12) Uani 1 1 d G . . H22E H -0.2289 1.0943 0.4360 0.074 Uiso 1 1 calc R . . C231 C -0.21486(11) 1.11930(12) 0.62408(9) 0.0364(8) Uani 1 1 d G . . C232 C -0.28005(13) 1.15475(13) 0.59034(8) 0.0543(10) Uani 1 1 d G . . H23A H -0.2902 1.1578 0.5426 0.065 Uiso 1 1 calc R . . C233 C -0.33040(12) 1.18572(13) 0.62644(12) 0.0630(12) Uani 1 1 d G . . H23B H -0.3750 1.2099 0.6034 0.076 Uiso 1 1 calc R . . C234 C -0.31554(13) 1.18124(13) 0.69628(12) 0.0541(10) Uani 1 1 d G . . H23C H -0.3500 1.2024 0.7210 0.065 Uiso 1 1 calc R . . C235 C -0.25035(14) 1.14580(13) 0.73001(8) 0.0515(10) Uani 1 1 d G . . H23D H -0.2402 1.1427 0.7777 0.062 Uiso 1 1 calc R . . C236 C -0.20001(11) 1.11483(12) 0.69391(9) 0.0383(8) Uani 1 1 d G . . H23E H -0.1554 1.0906 0.7170 0.046 Uiso 1 1 calc R . . C311 C 0.29326(9) 0.65809(11) 1.21533(10) 0.0316(7) Uani 1 1 d G . . C312 C 0.31629(11) 0.63475(12) 1.28107(10) 0.0459(9) Uani 1 1 d G . . H31A H 0.2784 0.6177 1.3046 0.055 Uiso 1 1 calc R . . C313 C 0.39478(12) 0.63633(13) 1.31238(9) 0.0556(11) Uani 1 1 d G . . H31B H 0.4105 0.6204 1.3573 0.067 Uiso 1 1 calc R . . C314 C 0.45023(9) 0.66127(13) 1.27794(11) 0.0491(10) Uani 1 1 d G . . H31C H 0.5039 0.6623 1.2993 0.059 Uiso 1 1 calc R . . C315 C 0.42719(10) 0.68461(12) 1.21220(11) 0.0462(9) Uani 1 1 d G . . H31D H 0.4651 0.7017 1.1887 0.055 Uiso 1 1 calc R . . C316 C 0.34870(11) 0.68303(11) 1.18090(8) 0.0366(8) Uani 1 1 d G . . H31E H 0.3330 0.6990 1.1360 0.044 Uiso 1 1 calc R . . C321 C 0.17141(12) 0.58955(9) 1.10396(10) 0.0321(7) Uani 1 1 d G . . C322 C 0.21340(11) 0.52876(10) 1.11294(9) 0.0381(8) Uani 1 1 d G . . H32A H 0.2553 0.5234 1.1505 0.046 Uiso 1 1 calc R . . C323 C 0.19407(13) 0.47576(8) 1.06697(12) 0.0452(9) Uani 1 1 d G . . H32B H 0.2228 0.4342 1.0731 0.054 Uiso 1 1 calc R . . C324 C 0.13273(14) 0.48355(10) 1.01204(11) 0.0517(10) Uani 1 1 d G . . H32C H 0.1195 0.4473 0.9806 0.062 Uiso 1 1 calc R . . C325 C 0.09074(12) 0.54433(12) 1.00307(10) 0.0610(11) Uani 1 1 d G . . H32D H 0.0488 0.5497 0.9655 0.073 Uiso 1 1 calc R . . C326 C 0.11007(12) 0.59733(10) 1.04903(11) 0.0499(10) Uani 1 1 d G . . H32E H 0.0814 0.6389 1.0429 0.060 Uiso 1 1 calc R . . C331 C 0.12134(12) 0.63496(11) 1.23319(10) 0.0347(8) Uani 1 1 d G . . C332 C 0.08983(14) 0.56984(10) 1.23427(11) 0.0482(10) Uani 1 1 d G . . H33A H 0.1046 0.5347 1.2070 0.058 Uiso 1 1 calc R . . C333 C 0.03668(14) 0.55612(12) 1.27528(13) 0.0643(12) Uani 1 1 d G . . H33B H 0.0151 0.5116 1.2760 0.077 Uiso 1 1 calc R . . C335 C 0.01504(13) 0.60752(15) 1.31521(12) 0.0634(12) Uani 1 1 d G . . H33C H -0.0213 0.5981 1.3432 0.076 Uiso 1 1 calc R . . C334 C 0.04656(15) 0.67264(13) 1.31414(11) 0.0623(12) Uani 1 1 d G . . H33D H 0.0318 0.7078 1.3414 0.075 Uiso 1 1 calc R . . C336 C 0.09971(14) 0.68636(9) 1.27313(12) 0.0470(9) Uani 1 1 d G . . H33E H 0.1212 0.7309 1.2724 0.056 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 0.0185(4) 0.0278(5) 0.0331(5) 0.0073(4) 0.0010(4) 0.0044(3) Si2 0.0262(5) 0.0217(5) 0.0342(5) 0.0118(4) -0.0016(4) 0.0056(3) Si3 0.0281(5) 0.0492(6) 0.0194(4) 0.0007(4) -0.0059(4) 0.0054(4) N1 0.0174(12) 0.0195(12) 0.0155(12) 0.0007(9) -0.0012(9) 0.0009(10) N2 0.0166(12) 0.0182(12) 0.0167(12) 0.0005(9) -0.0016(10) 0.0001(9) C1 0.0253(17) 0.0279(17) 0.0323(17) 0.0023(14) 0.0078(15) 0.0064(14) C2 0.0253(17) 0.0297(17) 0.0214(15) -0.0011(13) 0.0082(14) 0.0032(14) C3 0.0193(15) 0.0292(17) 0.0221(15) -0.0017(12) -0.0018(13) 0.0043(13) C4 0.0329(19) 0.051(2) 0.0236(17) -0.0002(15) 0.0067(14) 0.0143(16) C5 0.0387(19) 0.051(2) 0.0160(15) 0.0014(14) 0.0027(14) 0.0132(16) C6 0.0254(16) 0.0255(17) 0.0210(15) 0.0003(12) -0.0024(13) 0.0056(13) C7 0.0272(17) 0.0339(18) 0.0139(14) -0.0032(13) -0.0022(13) 0.0020(14) C8 0.0304(18) 0.044(2) 0.0237(16) -0.0014(15) -0.0044(15) -0.0005(16) C9 0.0174(14) 0.0203(15) 0.0201(15) -0.0003(12) -0.0002(12) -0.0015(12) C10 0.0189(15) 0.0149(14) 0.0198(14) -0.0025(11) -0.0005(12) -0.0025(11) C11 0.0123(14) 0.0145(14) 0.0199(14) -0.0023(11) -0.0042(11) -0.0042(11) C12 0.0139(14) 0.0165(15) 0.0194(14) 0.0005(11) -0.0020(11) -0.0019(11) C13 0.0148(14) 0.0174(15) 0.0220(15) -0.0003(11) -0.0022(12) 0.0017(11) C14 0.0152(14) 0.0142(14) 0.0178(14) 0.0019(11) -0.0029(11) -0.0016(11) C15 0.0128(14) 0.0151(14) 0.0163(14) 0.0004(10) -0.0048(11) -0.0031(10) C16 0.0159(14) 0.0146(14) 0.0222(15) 0.0036(11) -0.0022(12) -0.0007(11) C17 0.0187(15) 0.0226(16) 0.0176(14) -0.0002(12) -0.0015(12) -0.0006(12) C18 0.0191(15) 0.0242(17) 0.0276(16) 0.0060(13) -0.0004(13) 0.0014(13) C19 0.0178(14) 0.0186(15) 0.0157(14) 0.0040(11) -0.0050(12) -0.0016(11) C20 0.0129(13) 0.0159(14) 0.0171(14) -0.0002(11) -0.0036(11) -0.0009(11) C111 0.0184(16) 0.0337(19) 0.053(2) 0.0139(16) -0.0052(15) 0.0061(14) C112 0.046(2) 0.036(2) 0.069(3) -0.0005(19) 0.002(2) 0.0054(17) C113 0.046(3) 0.041(3) 0.122(4) -0.014(3) -0.007(3) 0.007(2) C114 0.033(2) 0.029(2) 0.168(5) 0.027(3) -0.001(3) 0.0013(18) C115 0.056(3) 0.050(3) 0.136(5) 0.043(3) 0.022(3) 0.005(2) C116 0.047(2) 0.045(2) 0.079(3) 0.026(2) 0.016(2) 0.0028(18) C121 0.0240(17) 0.0275(17) 0.0374(18) 0.0063(14) 0.0042(14) 0.0046(13) C122 0.030(2) 0.039(2) 0.088(3) 0.021(2) 0.022(2) 0.0090(16) C123 0.053(3) 0.040(2) 0.107(4) 0.025(2) 0.029(2) 0.0045(19) C124 0.031(2) 0.062(3) 0.080(3) 0.008(2) 0.027(2) -0.0054(18) C125 0.0281(19) 0.047(2) 0.061(2) -0.0006(18) 0.0113(17) 0.0087(16) C126 0.0272(18) 0.0331(19) 0.0435(19) 0.0054(15) 0.0058(15) 0.0045(14) C131 0.0213(17) 0.0353(18) 0.0325(17) 0.0082(14) 0.0007(14) -0.0005(13) C132 0.0238(18) 0.054(2) 0.041(2) 0.0079(17) -0.0016(16) 0.0018(16) C133 0.030(2) 0.069(3) 0.039(2) 0.0040(18) -0.0047(17) -0.0091(18) C134 0.044(2) 0.071(3) 0.0319(19) -0.0012(18) 0.0032(18) -0.0112(19) C135 0.0261(19) 0.057(2) 0.040(2) -0.0019(17) 0.0043(16) -0.0074(16) C136 0.0191(16) 0.045(2) 0.0371(19) 0.0011(15) 0.0001(14) -0.0029(14) C211 0.046(2) 0.054(2) 0.0208(17) 0.0059(15) -0.0057(16) 0.0046(17) C212 0.091(4) 0.063(3) 0.082(3) 0.020(3) 0.034(3) 0.008(3) C213 0.128(5) 0.080(4) 0.100(4) 0.030(3) 0.052(4) -0.004(3) C214 0.110(4) 0.101(4) 0.058(3) 0.013(3) 0.017(3) -0.041(4) C215 0.077(3) 0.100(4) 0.059(3) 0.009(3) 0.023(3) -0.017(3) C216 0.056(3) 0.079(3) 0.044(2) 0.006(2) 0.010(2) -0.005(2) C221 0.0274(18) 0.059(2) 0.0264(18) -0.0086(16) -0.0014(14) 0.0012(16) C222 0.079(3) 0.075(3) 0.047(2) -0.011(2) -0.015(2) -0.008(3) C223 0.111(4) 0.073(3) 0.074(3) -0.017(3) -0.003(3) -0.021(3) C224 0.056(3) 0.105(4) 0.048(3) -0.034(3) 0.005(2) -0.019(3) C225 0.075(3) 0.104(4) 0.040(2) -0.011(3) -0.009(2) -0.012(3) C226 0.070(3) 0.076(3) 0.032(2) -0.0042(19) -0.012(2) -0.005(2) C231 0.0308(18) 0.043(2) 0.0326(18) -0.0031(15) -0.0016(15) 0.0022(15) C232 0.045(2) 0.075(3) 0.038(2) 0.0007(19) -0.0022(18) 0.021(2) C233 0.053(3) 0.072(3) 0.062(3) 0.000(2) 0.006(2) 0.028(2) C234 0.044(2) 0.056(3) 0.065(3) -0.023(2) 0.017(2) -0.0033(19) C235 0.041(2) 0.078(3) 0.035(2) -0.0150(19) 0.0079(18) -0.009(2) C236 0.0310(19) 0.048(2) 0.0313(18) -0.0056(15) -0.0041(15) 0.0007(15) C311 0.0285(18) 0.0244(17) 0.0388(18) 0.0107(14) -0.0005(15) 0.0064(13) C312 0.038(2) 0.053(2) 0.043(2) 0.0138(17) 0.0010(17) 0.0083(17) C313 0.047(2) 0.067(3) 0.045(2) 0.0151(19) -0.0084(19) 0.016(2) C314 0.033(2) 0.045(2) 0.065(3) 0.0099(19) -0.0017(19) 0.0153(17) C315 0.036(2) 0.043(2) 0.059(2) 0.0023(18) 0.0072(18) 0.0099(16) C316 0.0334(19) 0.038(2) 0.0357(19) 0.0016(15) 0.0002(16) 0.0088(15) C321 0.0270(17) 0.0253(17) 0.0419(19) 0.0097(14) 0.0020(15) 0.0035(13) C322 0.039(2) 0.0259(18) 0.044(2) 0.0062(15) -0.0043(16) 0.0055(15) C323 0.043(2) 0.0276(19) 0.060(2) 0.0037(17) -0.0023(19) 0.0046(16) C324 0.042(2) 0.040(2) 0.067(3) -0.0114(19) -0.003(2) 0.0027(17) C325 0.046(2) 0.061(3) 0.064(3) -0.015(2) -0.018(2) 0.017(2) C326 0.041(2) 0.048(2) 0.052(2) -0.0021(18) -0.0098(19) 0.0201(18) C331 0.0301(18) 0.037(2) 0.0330(18) 0.0172(15) -0.0036(15) 0.0089(15) C332 0.046(2) 0.056(2) 0.039(2) 0.0146(17) 0.0003(17) -0.0146(18) C333 0.059(3) 0.082(3) 0.049(2) 0.016(2) 0.003(2) -0.022(2) C335 0.043(2) 0.091(4) 0.057(3) 0.036(3) 0.012(2) 0.009(2) C334 0.062(3) 0.078(3) 0.051(2) 0.022(2) 0.020(2) 0.031(2) C336 0.052(2) 0.046(2) 0.046(2) 0.0192(17) 0.0152(19) 0.0138(17) _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 1.835(3) . ? Si1 C111 1.8718(19) . ? Si1 C121 1.8818(16) . ? Si1 C131 1.8843(17) . ? Si2 C18 1.838(3) . ? Si2 C311 1.8719(17) . ? Si2 C321 1.8789(18) . ? Si2 C331 1.8853(18) . ? Si3 C8 1.834(3) . ? Si3 C221 1.875(2) . ? Si3 C231 1.8887(17) . ? Si3 C211 1.893(2) . ? N1 C12 1.333(3) . ? N1 C9 1.352(3) . ? N2 C11 1.335(3) . ? N2 C10 1.347(3) . ? C1 C2 1.200(4) . ? C2 C3 1.425(4) . ? C3 C4 1.378(4) . ? C3 C10 1.434(4) . ? C4 C5 1.396(4) . ? C5 C6 1.372(4) . ? C6 C7 1.431(4) . ? C6 C9 1.432(4) . ? C7 C8 1.193(4) . ? C9 C10 1.422(4) . ? C11 C12 1.417(4) . ? C11 C14 1.461(4) . ? C12 C20 1.463(4) 3_577 ? C13 C14 1.382(4) . ? C13 C16 1.394(4) . ? C14 C15 1.419(4) . ? C15 C20 1.412(4) . ? C15 C15 1.441(5) 3_577 ? C16 C19 1.397(4) . ? C16 C17 1.444(4) . ? C17 C18 1.199(4) . ? C19 C20 1.393(4) . ? C20 C12 1.463(4) 3_577 ? C111 C112 1.3900 . ? C111 C116 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C115 C116 1.3900 . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C124 C125 1.3900 . ? C125 C126 1.3900 . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C135 C136 1.3900 . ? C211 C212 1.3900 . ? C211 C216 1.3900 . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C214 C215 1.3900 . ? C215 C216 1.3900 . ? C221 C222 1.3900 . ? C221 C226 1.3900 . ? C222 C223 1.3900 . ? C223 C224 1.3900 . ? C224 C225 1.3900 . ? C225 C226 1.3900 . ? C231 C232 1.3900 . ? C231 C236 1.3900 . ? C232 C233 1.3900 . ? C233 C234 1.3900 . ? C234 C235 1.3900 . ? C235 C236 1.3900 . ? C311 C312 1.3900 . ? C311 C316 1.3900 . ? C312 C313 1.3900 . ? C313 C314 1.3900 . ? C314 C315 1.3900 . ? C315 C316 1.3900 . ? C321 C322 1.3900 . ? C321 C326 1.3900 . ? C322 C323 1.3900 . ? C323 C324 1.3900 . ? C324 C325 1.3900 . ? C325 C326 1.3900 . ? C331 C332 1.3900 . ? C331 C336 1.3900 . ? C332 C333 1.3900 . ? C333 C335 1.3900 . ? C335 C334 1.3900 . ? C334 C336 1.3900 . ? 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 C111 108.53(13) . . ? C1 Si1 C121 106.91(12) . . ? C111 Si1 C121 113.70(10) . . ? C1 Si1 C131 107.49(11) . . ? C111 Si1 C131 110.69(11) . . ? C121 Si1 C131 109.26(10) . . ? C18 Si2 C311 111.04(12) . . ? C18 Si2 C321 108.35(11) . . ? C311 Si2 C321 110.50(10) . . ? C18 Si2 C331 105.63(11) . . ? C311 Si2 C331 112.61(10) . . ? C321 Si2 C331 108.49(11) . . ? C8 Si3 C221 108.15(14) . . ? C8 Si3 C231 109.16(12) . . ? C221 Si3 C231 112.18(11) . . ? C8 Si3 C211 107.19(13) . . ? C221 Si3 C211 110.23(12) . . ? C231 Si3 C211 109.79(12) . . ? C12 N1 C9 116.4(2) . . ? C11 N2 C10 116.8(2) . . ? C2 C1 Si1 176.5(3) . . ? C1 C2 C3 178.0(3) . . ? C4 C3 C2 121.6(3) . . ? C4 C3 C10 118.4(3) . . ? C2 C3 C10 119.9(2) . . ? C3 C4 C5 121.5(3) . . ? C6 C5 C4 121.9(3) . . ? C5 C6 C7 121.0(3) . . ? C5 C6 C9 118.5(3) . . ? C7 C6 C9 120.5(2) . . ? C8 C7 C6 175.7(3) . . ? C7 C8 Si3 174.7(3) . . ? N1 C9 C10 121.1(2) . . ? N1 C9 C6 119.5(2) . . ? C10 C9 C6 119.4(2) . . ? N2 C10 C9 121.1(2) . . ? N2 C10 C3 119.2(2) . . ? C9 C10 C3 119.7(2) . . ? N2 C11 C12 121.3(2) . . ? N2 C11 C14 118.5(2) . . ? C12 C11 C14 120.2(2) . . ? N1 C12 C11 121.9(2) . . ? N1 C12 C20 118.4(2) . 3_577 ? C11 C12 C20 119.7(2) . 3_577 ? C14 C13 C16 121.5(2) . . ? C13 C14 C15 119.8(2) . . ? C13 C14 C11 121.3(2) . . ? C15 C14 C11 118.9(2) . . ? C20 C15 C14 118.6(2) . . ? C20 C15 C15 120.9(3) . 3_577 ? C14 C15 C15 120.5(3) . 3_577 ? C13 C16 C19 119.0(2) . . ? C13 C16 C17 120.3(2) . . ? C19 C16 C17 120.7(2) . . ? C18 C17 C16 177.6(3) . . ? C17 C18 Si2 174.8(3) . . ? C20 C19 C16 120.6(2) . . ? C19 C20 C15 120.2(2) . . ? C19 C20 C12 120.7(2) . 3_577 ? C15 C20 C12 119.1(2) . 3_577 ? C112 C111 C116 120.0 . . ? C112 C111 Si1 120.70(14) . . ? C116 C111 Si1 118.81(14) . . ? C111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C113 C114 C115 120.0 . . ? C116 C115 C114 120.0 . . ? C115 C116 C111 120.0 . . ? C122 C121 C126 120.0 . . ? C122 C121 Si1 119.56(11) . . ? C126 C121 Si1 120.09(11) . . ? C123 C122 C121 120.0 . . ? C122 C123 C124 120.0 . . ? C123 C124 C125 120.0 . . ? C124 C125 C126 120.0 . . ? C125 C126 C121 120.0 . . ? C132 C131 C136 120.0 . . ? C132 C131 Si1 118.89(11) . . ? C136 C131 Si1 120.93(11) . . ? C131 C132 C133 120.0 . . ? C134 C133 C132 120.0 . . ? C133 C134 C135 120.0 . . ? C136 C135 C134 120.0 . . ? C135 C136 C131 120.0 . . ? C212 C211 C216 120.0 . . ? C212 C211 Si3 122.12(15) . . ? C216 C211 Si3 117.87(15) . . ? C213 C212 C211 120.0 . . ? C212 C213 C214 120.0 . . ? C215 C214 C213 120.0 . . ? C216 C215 C214 120.0 . . ? C215 C216 C211 120.0 . . ? C222 C221 C226 120.0 . . ? C222 C221 Si3 119.98(14) . . ? C226 C221 Si3 119.85(14) . . ? C221 C222 C223 120.0 . . ? C222 C223 C224 120.0 . . ? C225 C224 C223 120.0 . . ? C226 C225 C224 120.0 . . ? C225 C226 C221 120.0 . . ? C232 C231 C236 120.0 . . ? C232 C231 Si3 119.78(12) . . ? C236 C231 Si3 120.21(12) . . ? C231 C232 C233 120.0 . . ? C234 C233 C232 120.0 . . ? C235 C234 C233 120.0 . . ? C236 C235 C234 120.0 . . ? C235 C236 C231 120.0 . . ? C312 C311 C316 120.0 . . ? C312 C311 Si2 119.98(11) . . ? C316 C311 Si2 120.02(11) . . ? C311 C312 C313 120.0 . . ? C312 C313 C314 120.0 . . ? C315 C314 C313 120.0 . . ? C316 C315 C314 120.0 . . ? C315 C316 C311 120.0 . . ? C322 C321 C326 120.0 . . ? C322 C321 Si2 119.42(11) . . ? C326 C321 Si2 119.91(11) . . ? C323 C322 C321 120.0 . . ? C322 C323 C324 120.0 . . ? C325 C324 C323 120.0 . . ? C326 C325 C324 120.0 . . ? C325 C326 C321 120.0 . . ? C332 C331 C336 120.0 . . ? C332 C331 Si2 119.96(12) . . ? C336 C331 Si2 119.89(12) . . ? C331 C332 C333 120.0 . . ? C335 C333 C332 120.0 . . ? C333 C335 C334 120.0 . . ? C336 C334 C335 120.0 . . ? C334 C336 C331 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.405 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.061 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.135 0.303 0.500 1400 271 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL CELL 0.71073 17.4522 19.5708 20.2712 90 101.54 90 ZERR 1 0.0004 0.0004 0.0005 0 0.0015 0 LATT 1 SYMM 0.5-X,0.5+Y,-Z SFAC Si N C H Cl UNIT 6 4 148 98 1 L.S. 4 PLAN 20 TEMP -173.15 ACTA FMAP 2 SHEL 999 0.7 REM WGHT 0.106100 0.762300 FVAR 1.04028 SI1 1 0.361197 0.764145 0.907724 11.00000 0.01854 0.02777 = 0.03311 0.00732 0.00096 0.00445 SI2 1 0.187662 0.655247 1.172944 11.00000 0.02623 0.02167 = 0.03423 0.01185 -0.00160 0.00556 SI3 1 -0.145634 1.078782 0.574836 11.00000 0.02809 0.04920 = 0.01945 0.00066 -0.00594 0.00543 N1 2 0.009940 1.000652 0.810797 11.00000 0.01736 0.01950 = 0.01547 0.00071 -0.00121 0.00086 N2 2 0.113462 0.903231 0.882893 11.00000 0.01661 0.01825 = 0.01673 0.00055 -0.00157 0.00011 C1 3 0.277979 0.807409 0.854397 11.00000 0.02530 0.02788 = 0.03231 0.00229 0.00783 0.00639 C2 3 0.224759 0.838857 0.821433 11.00000 0.02533 0.02967 = 0.02140 -0.00111 0.00817 0.00320 C3 3 0.162805 0.878373 0.783249 11.00000 0.01925 0.02925 = 0.02210 -0.00174 -0.00181 0.00425 C4 3 0.154059 0.885738 0.714544 11.00000 0.03285 0.05073 = 0.02360 -0.00022 0.00668 0.01426 AFIX 43 H4A 4 0.189952 0.863680 0.691984 11.00000 -1.20000 AFIX 0 C5 3 0.093636 0.924889 0.677324 11.00000 0.03872 0.05103 = 0.01601 0.00138 0.00272 0.01322 AFIX 43 H5A 4 0.087601 0.926536 0.629724 11.00000 -1.20000 AFIX 0 C6 3 0.042720 0.961057 0.707541 11.00000 0.02536 0.02553 = 0.02101 0.00026 -0.00242 0.00562 C7 3 -0.020155 0.999396 0.668366 11.00000 0.02721 0.03390 = 0.01391 -0.00324 -0.00220 0.00203 C8 3 -0.072295 1.028610 0.632288 11.00000 0.03043 0.04442 = 0.02374 -0.00140 -0.00437 -0.00050 C9 3 0.053427 0.959256 0.779445 11.00000 0.01737 0.02032 = 0.02014 -0.00034 -0.00018 -0.00152 C10 3 0.109772 0.914087 0.816693 11.00000 0.01893 0.01491 = 0.01976 -0.00249 -0.00049 -0.00252 C11 3 0.066304 0.940905 0.912587 11.00000 0.01231 0.01447 = 0.01992 -0.00228 -0.00422 -0.00417 C12 3 0.019723 0.993768 0.877394 11.00000 0.01386 0.01653 = 0.01936 0.00052 -0.00195 -0.00187 C13 3 0.098618 0.869016 1.015005 11.00000 0.01476 0.01742 = 0.02198 -0.00026 -0.00215 0.00170 AFIX 43 H13A 4 0.126287 0.838930 0.991348 11.00000 -1.20000 AFIX 0 C14 3 0.063094 0.926300 0.982645 11.00000 0.01521 0.01418 = 0.01779 0.00186 -0.00294 -0.00155 C15 3 0.020383 0.970977 1.017056 11.00000 0.01283 0.01511 = 0.01628 0.00040 -0.00485 -0.00307 C16 3 0.094804 0.854336 1.081582 11.00000 0.01588 0.01459 = 0.02215 0.00358 -0.00217 -0.00067 C17 3 0.127607 0.791603 1.112538 11.00000 0.01870 0.02262 = 0.01762 -0.00020 -0.00147 -0.00059 C18 3 0.154799 0.738580 1.135917 11.00000 0.01913 0.02419 = 0.02756 0.00597 -0.00039 0.00142 C19 3 0.057506 0.900551 1.117223 11.00000 0.01782 0.01859 = 0.01568 0.00403 -0.00496 -0.00161 AFIX 43 H19A 4 0.057423 0.892497 1.163423 11.00000 -1.20000 AFIX 0 C20 3 0.020432 0.958335 1.085667 11.00000 0.01286 0.01585 = 0.01711 -0.00021 -0.00361 -0.00085 AFIX 66 C111 3 0.344355 0.669731 0.900885 11.00000 0.01842 0.03366 = 0.05315 0.01390 -0.00523 0.00609 C112 3 0.350401 0.634834 0.842422 11.00000 0.04630 0.03607 = 0.06861 -0.00050 0.00223 0.00539 AFIX 43 H11A 4 0.369684 0.657607 0.807687 11.00000 -1.20000 AFIX 65 C113 3 0.328232 0.566617 0.834782 11.00000 0.04584 0.04074 = 0.12186 -0.01373 -0.00717 0.00705 AFIX 43 H11B 4 0.332364 0.542767 0.794825 11.00000 -1.20000 AFIX 65 C114 3 0.300018 0.533297 0.885605 11.00000 0.03257 0.02860 = 0.16752 0.02676 -0.00111 0.00132 AFIX 43 H11C 4 0.284867 0.486673 0.880383 11.00000 -1.20000 AFIX 65 C115 3 0.293972 0.568193 0.944068 11.00000 0.05640 0.04964 = 0.13643 0.04292 0.02168 0.00484 AFIX 43 H11D 4 0.274688 0.545419 0.978803 11.00000 -1.20000 AFIX 65 C116 3 0.316140 0.636410 0.951709 11.00000 0.04652 0.04487 = 0.07866 0.02592 0.01630 0.00279 AFIX 43 H11E 4 0.312008 0.660260 0.991666 11.00000 -1.20000 AFIX 66 C121 3 0.451683 0.792984 0.878402 11.00000 0.02404 0.02751 = 0.03745 0.00626 0.00415 0.00458 C122 3 0.456000 0.859420 0.855177 11.00000 0.03009 0.03921 = 0.08848 0.02069 0.02166 0.00900 AFIX 43 H12B 4 0.411475 0.888374 0.849570 11.00000 -1.20000 AFIX 65 C123 3 0.525465 0.883493 0.840155 11.00000 0.05256 0.03958 = 0.10716 0.02452 0.02946 0.00450 AFIX 43 H12C 4 0.528416 0.928899 0.824281 11.00000 -1.20000 AFIX 65 C124 3 0.590613 0.841130 0.848359 11.00000 0.03121 0.06174 = 0.07978 0.00849 0.02711 -0.00543 AFIX 43 H12D 4 0.638089 0.857583 0.838092 11.00000 -1.20000 AFIX 65 C125 3 0.586296 0.774693 0.871584 11.00000 0.02814 0.04650 = 0.06103 -0.00061 0.01133 0.00871 AFIX 43 H12E 4 0.630822 0.745740 0.877191 11.00000 -1.20000 AFIX 65 C126 3 0.516832 0.750620 0.886606 11.00000 0.02724 0.03308 = 0.04350 0.00536 0.00583 0.00451 AFIX 43 H12F 4 0.513882 0.705213 0.902480 11.00000 -1.20000 AFIX 66 C131 3 0.366091 0.793988 0.996846 11.00000 0.02127 0.03526 = 0.03255 0.00817 0.00069 -0.00047 C132 3 0.437940 0.793909 1.041293 11.00000 0.02382 0.05381 = 0.04117 0.00793 -0.00162 0.00179 AFIX 43 H13B 4 0.482769 0.775724 1.027611 11.00000 -1.20000 AFIX 65 C133 3 0.444197 0.820439 1.105758 11.00000 0.03032 0.06913 = 0.03898 0.00404 -0.00467 -0.00914 AFIX 43 H13C 4 0.493303 0.820385 1.136135 11.00000 -1.20000 AFIX 65 C134 3 0.378606 0.847047 1.125777 11.00000 0.04354 0.07053 = 0.03193 -0.00121 0.00325 -0.01124 AFIX 43 H13D 4 0.382883 0.865178 1.169836 11.00000 -1.20000 AFIX 65 C135 3 0.306757 0.847126 1.081330 11.00000 0.02606 0.05713 = 0.03954 -0.00191 0.00434 -0.00743 AFIX 43 H13E 4 0.261928 0.865312 1.095012 11.00000 -1.20000 AFIX 65 C136 3 0.300498 0.820597 1.016865 11.00000 0.01915 0.04518 = 0.03706 0.00113 0.00007 -0.00292 AFIX 43 H13F 4 0.251392 0.820651 0.986488 11.00000 -1.20000 AFIX 66 C211 3 -0.091411 1.147623 0.537170 11.00000 0.04574 0.05372 = 0.02084 0.00595 -0.00565 0.00464 C212 3 -0.113030 1.216009 0.536641 11.00000 0.09082 0.06297 = 0.08206 0.02029 0.03378 0.00792 AFIX 43 H21A 4 -0.156925 1.229336 0.554765 11.00000 -1.20000 AFIX 65 C213 3 -0.070422 1.264897 0.509593 11.00000 0.12771 0.08012 = 0.09992 0.03018 0.05166 -0.00392 AFIX 43 H21B 4 -0.085198 1.311636 0.509231 11.00000 -1.20000 AFIX 65 C214 3 -0.006196 1.245398 0.483073 11.00000 0.11047 0.10074 = 0.05842 0.01293 0.01711 -0.04063 AFIX 43 H21C 4 0.022924 1.278811 0.464587 11.00000 -1.20000 AFIX 65 C215 3 0.015423 1.177013 0.483602 11.00000 0.07713 0.09958 = 0.05916 0.00925 0.02267 -0.01704 AFIX 43 H21D 4 0.059319 1.163687 0.465477 11.00000 -1.20000 AFIX 65 C216 3 -0.027183 1.128124 0.510650 11.00000 0.05578 0.07944 = 0.04420 0.00600 0.01021 -0.00453 AFIX 43 H21E 4 -0.012407 1.081386 0.511011 11.00000 -1.20000 AFIX 66 C221 3 -0.197452 1.020314 0.507101 11.00000 0.02738 0.05937 = 0.02645 -0.00859 -0.00138 0.00118 C222 3 -0.204518 0.951192 0.520477 11.00000 0.07939 0.07544 = 0.04707 -0.01057 -0.01467 -0.00768 AFIX 43 H22A 4 -0.179745 0.932943 0.562812 11.00000 -1.20000 AFIX 65 C223 3 -0.247830 0.908772 0.471911 11.00000 0.11118 0.07303 = 0.07386 -0.01662 -0.00261 -0.02079 AFIX 43 H22B 4 -0.252659 0.861531 0.481054 11.00000 -1.20000 AFIX 65 C224 3 -0.284077 0.935473 0.409968 11.00000 0.05647 0.10464 = 0.04832 -0.03443 0.00465 -0.01850 AFIX 43 H22C 4 -0.313679 0.906480 0.376776 11.00000 -1.20000 AFIX 65 C225 3 -0.277011 1.004594 0.396591 11.00000 0.07468 0.10370 = 0.04040 -0.01124 -0.00883 -0.01204 AFIX 43 H22D 4 -0.301785 1.022843 0.354256 11.00000 -1.20000 AFIX 65 C226 3 -0.233699 1.047016 0.445157 11.00000 0.06973 0.07565 = 0.03173 -0.00416 -0.01164 -0.00541 AFIX 43 H22E 4 -0.228870 1.094257 0.436014 11.00000 -1.20000 AFIX 66 C231 3 -0.214857 1.119303 0.624078 11.00000 0.03082 0.04261 = 0.03258 -0.00310 -0.00157 0.00220 C232 3 -0.280052 1.154747 0.590343 11.00000 0.04504 0.07542 = 0.03814 0.00069 -0.00218 0.02148 AFIX 43 H23A 4 -0.290202 1.157804 0.542614 11.00000 -1.20000 AFIX 65 C233 3 -0.330396 1.185716 0.626443 11.00000 0.05312 0.07167 = 0.06161 0.00024 0.00558 0.02835 AFIX 43 H23B 4 -0.374954 1.209940 0.603386 11.00000 -1.20000 AFIX 65 C234 3 -0.315545 1.181242 0.696278 11.00000 0.04428 0.05561 = 0.06512 -0.02279 0.01727 -0.00334 AFIX 43 H23C 4 -0.349953 1.202409 0.720950 11.00000 -1.20000 AFIX 65 C235 3 -0.250350 1.145799 0.730014 11.00000 0.04126 0.07828 = 0.03521 -0.01504 0.00789 -0.00944 AFIX 43 H23D 4 -0.240201 1.142742 0.777743 11.00000 -1.20000 AFIX 65 C236 3 -0.200005 1.114829 0.693915 11.00000 0.03104 0.04828 = 0.03126 -0.00556 -0.00412 0.00072 AFIX 43 H23E 4 -0.155448 1.090605 0.716971 11.00000 -1.20000 AFIX 66 C311 3 0.293256 0.658094 1.215332 11.00000 0.02849 0.02443 = 0.03876 0.01068 -0.00053 0.00636 C312 3 0.316294 0.634746 1.281074 11.00000 0.03819 0.05332 = 0.04333 0.01383 0.00099 0.00829 AFIX 43 H31A 4 0.278398 0.617704 1.304609 11.00000 -1.20000 AFIX 65 C313 3 0.394779 0.636331 1.312380 11.00000 0.04704 0.06684 = 0.04547 0.01508 -0.00838 0.01595 AFIX 43 H31B 4 0.410524 0.620374 1.357312 11.00000 -1.20000 AFIX 65 C314 3 0.450227 0.661266 1.277945 11.00000 0.03274 0.04498 = 0.06481 0.00994 -0.00167 0.01532 AFIX 43 H31C 4 0.503867 0.662349 1.299342 11.00000 -1.20000 AFIX 65 C315 3 0.427190 0.684614 1.212203 11.00000 0.03555 0.04266 = 0.05932 0.00230 0.00722 0.00989 AFIX 43 H31D 4 0.465086 0.701655 1.188668 11.00000 -1.20000 AFIX 65 C316 3 0.348705 0.683029 1.180895 11.00000 0.03342 0.03784 = 0.03568 0.00163 0.00023 0.00878 AFIX 43 H31E 4 0.332960 0.698987 1.135964 11.00000 -1.20000 AFIX 66 C321 3 0.171408 0.589550 1.103964 11.00000 0.02700 0.02529 = 0.04194 0.00971 0.00200 0.00354 C322 3 0.213403 0.528765 1.112935 11.00000 0.03908 0.02592 = 0.04393 0.00623 -0.00428 0.00552 AFIX 43 H32A 4 0.255321 0.523444 1.150480 11.00000 -1.20000 AFIX 65 C323 3 0.194065 0.475764 1.066973 11.00000 0.04291 0.02758 = 0.05976 0.00370 -0.00233 0.00464 AFIX 43 H32B 4 0.222767 0.434220 1.073105 11.00000 -1.20000 AFIX 65 C324 3 0.132733 0.483549 1.012039 11.00000 0.04249 0.04016 = 0.06669 -0.01143 -0.00256 0.00269 AFIX 43 H32C 4 0.119517 0.447325 0.980626 11.00000 -1.20000 AFIX 65 C325 3 0.090737 0.544334 1.003067 11.00000 0.04562 0.06104 = 0.06421 -0.01475 -0.01813 0.01721 AFIX 43 H32D 4 0.048819 0.549654 0.965522 11.00000 -1.20000 AFIX 65 C326 3 0.110074 0.597335 1.049029 11.00000 0.04145 0.04838 = 0.05183 -0.00212 -0.00981 0.02008 AFIX 43 H32E 4 0.081372 0.638879 1.042897 11.00000 -1.20000 AFIX 66 C331 3 0.121342 0.634963 1.233194 11.00000 0.03011 0.03677 = 0.03301 0.01718 -0.00355 0.00887 C332 3 0.089828 0.569841 1.234268 11.00000 0.04625 0.05610 = 0.03875 0.01457 0.00029 -0.01464 AFIX 43 H33A 4 0.104614 0.534711 1.206975 11.00000 -1.20000 AFIX 65 C333 3 0.036679 0.556118 1.275278 11.00000 0.05862 0.08184 = 0.04929 0.01584 0.00345 -0.02241 AFIX 43 H33B 4 0.015141 0.511610 1.276012 11.00000 -1.20000 AFIX 65 C335 3 0.015045 0.607517 1.315213 11.00000 0.04342 0.09083 = 0.05664 0.03563 0.01182 0.00862 AFIX 43 H33C 4 -0.021280 0.598138 1.343241 11.00000 -1.20000 AFIX 65 C334 3 0.046559 0.672640 1.314139 11.00000 0.06175 0.07825 = 0.05054 0.02197 0.02027 0.03148 AFIX 43 H33D 4 0.031772 0.707769 1.341433 11.00000 -1.20000 AFIX 65 C336 3 0.099707 0.686363 1.273130 11.00000 0.05167 0.04559 = 0.04594 0.01916 0.01523 0.01375 AFIX 43 H33E 4 0.121246 0.730871 1.272396 11.00000 -1.20000 HKLF 4 REM REM R1 = 0.0647 for 7708 Fo > 4sig(Fo) and 0.0978 for all 11305 data REM 604 parameters refined using 0 restraints END WGHT 0.1061 0.7623 REM Highest difference peak 0.405, deepest hole -0.348, 1-sigma level 0.061 Q1 1 0.1748 0.6087 1.1367 11.00000 0.05 0.41 Q2 1 -0.1445 1.0300 0.5691 11.00000 0.05 0.39 Q3 1 0.2952 0.5535 0.9017 11.00000 0.05 0.36 Q4 1 0.3522 0.6397 1.2221 11.00000 0.05 0.36 Q5 1 -0.1872 0.9369 0.4094 11.00000 0.05 0.35 Q6 1 0.3701 0.7953 0.9505 11.00000 0.05 0.35 Q7 1 -0.3168 0.9434 0.4602 11.00000 0.05 0.35 Q8 1 0.4292 0.7821 0.8838 11.00000 0.05 0.34 Q9 1 -0.1442 1.1315 0.5411 11.00000 0.05 0.32 Q10 1 0.4379 0.7652 1.1148 11.00000 0.05 0.32 Q11 1 0.2990 0.7078 1.2946 11.00000 0.05 0.31 Q12 1 -0.1473 0.9818 0.4663 11.00000 0.05 0.30 Q13 1 -0.2736 0.9875 0.5066 11.00000 0.05 0.30 Q14 1 0.1741 0.6965 1.1532 11.00000 0.05 0.28 Q15 1 0.4298 0.6829 1.3184 11.00000 0.05 0.28 Q16 1 0.3840 0.7915 1.1403 11.00000 0.05 0.27 Q17 1 -0.2058 1.0615 0.6407 11.00000 0.05 0.27 Q18 1 0.4198 0.6484 1.2549 11.00000 0.05 0.27 Q19 1 0.1235 0.5864 1.0396 11.00000 0.05 0.26 Q20 1 0.1682 0.6667 1.2107 11.00000 0.05 0.26 ; _database_code_depnum_ccdc_archive 'CCDC 972123'