#------------------------------------------------------------------------------ #$Date: 2025-01-11 10:06:07 +0200 (Sat, 11 Jan 2025) $ #$Revision: 297289 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/77/7127763.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7127763 loop_ _publ_author_name 'Espinosa-Jalapa, Noel Angel' 'Berg, Nele' 'Seidl, Michael' 'Shenderovich, Ilya G.' 'Gschwind, Ruth M.' 'Bauer, Jonathan O.' _publ_section_title ; Complexation behaviour of LiCl and LiPF6- model studies in the solid-state and in solution using a bidentate picolyl-based ligand. ; _journal_issue 87 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 13335 _journal_page_last 13338 _journal_paper_doi 10.1039/d0cc05682k _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C26 H26 N2 Si' _chemical_formula_sum 'C26 H26 N2 Si' _chemical_formula_weight 394.57 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-06-24 _audit_creation_method ; Olex2 1.3-alpha (compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115) ; _audit_update_record ; 2020-07-22 deposited with the CCDC. 2020-10-15 downloaded from the CCDC. ; _cell_angle_alpha 100.776(2) _cell_angle_beta 93.428(2) _cell_angle_gamma 109.092(2) _cell_formula_units_Z 4 _cell_length_a 10.2134(2) _cell_length_b 14.0734(3) _cell_length_c 16.2616(3) _cell_measurement_reflns_used 10888 _cell_measurement_temperature 123(1) _cell_measurement_theta_max 71.3130 _cell_measurement_theta_min 3.8940 _cell_volume 2151.38(8) _computing_cell_refinement 'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 123(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2548 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -98.00 -22.00 1.00 2.00 -- -39.78 125.00-180.00 76 2 \w 1.00 87.00 1.00 2.00 -- 39.78-125.00 90.00 86 3 \w -43.00 27.00 1.00 2.00 -- 39.78 -19.00-120.00 70 4 \w -43.00 27.00 1.00 2.00 -- 39.78 -19.00-180.00 70 5 \w -43.00 27.00 1.00 2.00 -- 39.78 -19.00 120.00 70 6 \w 25.00 84.00 1.00 12.00 -- 104.85-111.00 -30.00 59 7 \w 80.00 178.00 1.00 12.00 -- 104.85 77.00 150.00 98 8 \w 76.00 178.00 1.00 12.00 -- 104.85 45.00-150.00 102 9 \w 71.00 178.00 1.00 12.00 -- 104.85 30.00 -90.00 107 10 \w 17.00 143.00 1.00 12.00 -- 104.85 -88.00 -14.16 126 11 \w 17.00 143.00 1.00 12.00 -- 104.85 -88.00 62.17 126 12 \w 76.00 178.00 1.00 12.00 -- 104.85 45.00 120.00 102 13 \w 17.00 143.00 1.00 12.00 -- 104.85 -88.00 146.09 126 14 \w 29.00 71.00 1.00 12.00 -- 104.85 -61.00-120.00 42 15 \w 18.00 143.00 1.00 12.00 -- 104.85 -87.00-133.63 125 16 \w 6.00 97.00 1.00 2.00 -- 39.78 73.00-160.13 91 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, AtlasS2, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0196191000 _diffrn_orient_matrix_UB_12 0.0709602000 _diffrn_orient_matrix_UB_13 -0.0632536000 _diffrn_orient_matrix_UB_21 -0.0315275000 _diffrn_orient_matrix_UB_22 -0.0941030000 _diffrn_orient_matrix_UB_23 -0.0736346000 _diffrn_orient_matrix_UB_31 -0.1566478000 _diffrn_orient_matrix_UB_32 -0.0142605000 _diffrn_orient_matrix_UB_33 -0.0061264000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 17359 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.963 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.507 _diffrn_reflns_theta_min 3.406 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.257 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.218 _exptl_crystal_description block _exptl_crystal_F_000 840 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Hexane' _exptl_crystal_size_max 0.756 _exptl_crystal_size_mid 0.616 _exptl_crystal_size_min 0.216 _refine_diff_density_max 0.361 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 527 _refine_ls_number_reflns 8084 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0359 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.6022P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0937 _refine_ls_wR_factor_ref 0.0969 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7390 _reflns_number_total 8084 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc05682k2.cif _cod_data_source_block ph2silut2_ap_abs_gaus _cod_depositor_comments ; 2025-01-11 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C52 H52 N4 Si2' _cod_original_formula_weight 789.15 _cod_original_formula_moiety '2(C26 H26 N2 Si)' _cod_original_formula_units_Z 2 _cod_database_code 7127763 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C52H52N4Si2 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 98.62 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C1(H1A,H1B), C27(H27A,H27B), C34(H34A,H34B) 2.b Aromatic/amide H refined with riding coordinates: C26(H26), C20(H20), C22(H22), C16(H16), C12(H12), C10(H10), C29(H29), C52(H52), C42(H42), C46(H46), C11(H11), C36(H36), C18(H18), C48(H48), C19(H19), C51(H51), C49(H49), C17(H17), C31(H31), C43(H43), C50(H50), C30(H30), C38(H38), C23(H23), C3(H3), C25(H25), C37(H37), C5(H5), C44(H44), C24(H24), C45(H45), C4(H4) 2.c Idealised Me refined as rotating group: C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C14(H14A,H14B,H14C), C7(H7A,H7B,H7C) ; _shelx_res_file ; TITL ph2silut2_ap_a.res in P-1 ph2silut2_ap_abs_gaus.res created by SHELXL-2018/3 at 13:59:50 on 24-Jun-2020 REM Old TITL Ph2SiLut2_aP in P-1 REM SHELXT solution in P-1: R1 0.099, Rweak 0.005, Alpha 0.028 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C52 N4 Si2 CELL 1.54184 10.2134 14.0734 16.2616 100.776 93.428 109.092 ZERR 2 0.0002 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N Si UNIT 104 104 8 4 L.S. 10 PLAN 10 TEMP -150 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.051900 0.602200 FVAR 5.65866 SI1 4 0.326412 0.254028 0.882395 11.00000 0.01920 0.02046 = 0.01928 0.00337 0.00123 0.00836 SI2 4 0.786342 0.239574 0.491047 11.00000 0.02202 0.02079 = 0.01873 0.00363 0.00404 0.00797 N4 3 0.532678 0.232796 0.312129 11.00000 0.02156 0.02610 = 0.02301 0.00357 0.00266 0.00600 N3 3 0.719559 0.427526 0.650748 11.00000 0.02499 0.02175 = 0.02762 0.00615 0.00546 0.00972 N2 3 0.250176 0.459549 0.820735 11.00000 0.02255 0.02351 = 0.02500 0.00498 0.00247 0.00879 N1 3 0.091948 0.208998 1.042008 11.00000 0.02083 0.02643 = 0.02852 0.00678 0.00132 0.00645 C9 1 0.224338 0.421647 0.890526 11.00000 0.02377 0.01703 = 0.02182 -0.00072 0.00103 0.00834 C21 1 0.313808 0.221979 0.764211 11.00000 0.02431 0.01988 = 0.02132 0.00274 0.00195 0.00807 C41 1 0.774785 0.181986 0.587130 11.00000 0.01948 0.02376 = 0.02249 0.00493 0.00524 0.00990 C8 1 0.336407 0.390154 0.929524 11.00000 0.02460 0.02221 = 0.02051 0.00175 0.00130 0.01014 AFIX 23 H8A 2 0.330103 0.396836 0.990725 11.00000 -1.20000 H8B 2 0.428714 0.438376 0.923094 11.00000 -1.20000 AFIX 0 C28 1 0.689703 0.400572 0.566233 11.00000 0.03038 0.01929 = 0.02871 0.00747 0.00679 0.01110 C15 1 0.485650 0.233170 0.927865 11.00000 0.02278 0.02516 = 0.01866 0.00551 0.00249 0.01016 C35 1 0.606500 0.173726 0.329304 11.00000 0.02105 0.02344 = 0.02259 0.00324 0.00155 0.00292 C2 1 0.144304 0.145691 0.992725 11.00000 0.01842 0.02497 = 0.02640 0.00643 0.00064 0.00428 C26 1 0.416333 0.193746 0.722914 11.00000 0.02755 0.02682 = 0.02558 0.00571 0.00330 0.01196 AFIX 43 H26 2 0.498949 0.196863 0.755118 11.00000 -1.20000 AFIX 0 C47 1 0.943317 0.229000 0.440936 11.00000 0.02457 0.02676 = 0.01647 0.00302 0.00249 0.00975 C13 1 0.150271 0.484847 0.782356 11.00000 0.02446 0.02182 = 0.02793 0.00450 0.00030 0.00779 C32 1 0.617835 0.439416 0.696309 11.00000 0.02622 0.02122 = 0.02749 0.00557 0.00584 0.00966 C20 1 0.492507 0.133794 0.911234 11.00000 0.02570 0.02679 = 0.02633 0.00207 -0.00019 0.01069 AFIX 43 H20 2 0.413288 0.077823 0.881530 11.00000 -1.20000 AFIX 0 C22 1 0.193527 0.216189 0.714382 11.00000 0.02643 0.02871 = 0.02691 0.00285 0.00047 0.01196 AFIX 43 H22 2 0.122248 0.234666 0.740863 11.00000 -1.20000 AFIX 0 C16 1 0.603780 0.313000 0.972351 11.00000 0.02779 0.02571 = 0.02402 0.00694 0.00117 0.00903 AFIX 43 H16 2 0.601957 0.381190 0.985539 11.00000 -1.20000 AFIX 0 C1 1 0.159406 0.159257 0.904270 11.00000 0.02171 0.02682 = 0.02709 0.00637 0.00061 0.00523 AFIX 23 H1A 2 0.081085 0.179861 0.884788 11.00000 -1.20000 H1B 2 0.146831 0.090953 0.868500 11.00000 -1.20000 AFIX 0 C12 1 0.023565 0.475853 0.812931 11.00000 0.02418 0.02426 = 0.03196 0.00225 -0.00076 0.01125 AFIX 43 H12 2 -0.044611 0.495110 0.784589 11.00000 -1.20000 AFIX 0 C10 1 0.099709 0.409877 0.924869 11.00000 0.02870 0.02760 = 0.02409 0.00384 0.00637 0.01168 AFIX 43 H10 2 0.084283 0.382955 0.974231 11.00000 -1.20000 AFIX 0 C39 1 0.514131 0.243216 0.232060 11.00000 0.02244 0.02422 = 0.02686 0.00540 0.00167 0.00384 C29 1 0.560583 0.388886 0.524389 11.00000 0.03759 0.02936 = 0.02645 0.00516 0.00070 0.01652 AFIX 43 H29 2 0.543025 0.371033 0.464479 11.00000 -1.20000 AFIX 0 C52 1 0.957160 0.131889 0.416986 11.00000 0.02676 0.02596 = 0.02474 0.00404 0.00443 0.00808 AFIX 43 H52 2 0.884164 0.072221 0.423214 11.00000 -1.20000 AFIX 0 C42 1 0.714744 0.075422 0.579425 11.00000 0.02713 0.02450 = 0.02557 0.00343 0.00135 0.00919 AFIX 43 H42 2 0.681491 0.032029 0.524810 11.00000 -1.20000 AFIX 0 C27 1 0.802892 0.380005 0.518252 11.00000 0.03210 0.02270 = 0.02787 0.00660 0.00908 0.01142 AFIX 23 H27A 2 0.894641 0.420142 0.552427 11.00000 -1.20000 H27B 2 0.801246 0.405001 0.465327 11.00000 -1.20000 AFIX 0 C34 1 0.619358 0.159856 0.418411 11.00000 0.02466 0.03020 = 0.02243 0.00651 0.00272 0.00725 AFIX 23 H34A 2 0.605667 0.086356 0.415897 11.00000 -1.20000 H34B 2 0.541116 0.174111 0.445039 11.00000 -1.20000 AFIX 0 C46 1 0.823934 0.242557 0.668412 11.00000 0.03372 0.02549 = 0.02664 0.00221 -0.00177 0.01298 AFIX 43 H46 2 0.867934 0.314944 0.675792 11.00000 -1.20000 AFIX 0 C11 1 -0.001426 0.438335 0.885405 11.00000 0.02486 0.03159 = 0.03368 0.00260 0.00752 0.01337 AFIX 43 H11 2 -0.086822 0.432117 0.907909 11.00000 -1.20000 AFIX 0 C36 1 0.666394 0.125085 0.267453 11.00000 0.03312 0.02862 = 0.02648 0.00426 0.00415 0.01364 AFIX 43 H36 2 0.719747 0.084883 0.281310 11.00000 -1.20000 AFIX 0 C18 1 0.729202 0.195800 0.979409 11.00000 0.02431 0.04544 = 0.02422 0.01120 0.00295 0.01841 AFIX 43 H18 2 0.812090 0.183537 0.995701 11.00000 -1.20000 AFIX 0 C48 1 1.051988 0.314587 0.429568 11.00000 0.02880 0.02651 = 0.02406 0.00434 0.00413 0.00917 AFIX 43 H48 2 1.044817 0.381104 0.444447 11.00000 -1.20000 AFIX 0 C6 1 0.068307 0.193963 1.119736 11.00000 0.02169 0.03308 = 0.02670 0.00293 0.00014 0.00410 C19 1 0.611818 0.114751 0.936930 11.00000 0.03375 0.03273 = 0.02693 0.00506 0.00467 0.02004 AFIX 43 H19 2 0.613162 0.046386 0.925474 11.00000 -1.20000 AFIX 0 C51 1 1.075299 0.121513 0.384451 11.00000 0.03443 0.03277 = 0.02395 0.00267 0.00457 0.01730 AFIX 43 H51 2 1.082585 0.055138 0.368520 11.00000 -1.20000 AFIX 0 C49 1 1.170893 0.304140 0.396750 11.00000 0.02568 0.03513 = 0.02622 0.00711 0.00489 0.00587 AFIX 43 H49 2 1.243587 0.363253 0.389290 11.00000 -1.20000 AFIX 0 C17 1 0.724493 0.294696 0.997846 11.00000 0.02338 0.03517 = 0.02611 0.00885 -0.00088 0.00604 AFIX 43 H17 2 0.803795 0.350263 1.027972 11.00000 -1.20000 AFIX 0 C31 1 0.486260 0.428339 0.659167 11.00000 0.02638 0.02718 = 0.03428 0.00507 0.00571 0.01320 AFIX 43 H31 2 0.416733 0.437401 0.692976 11.00000 -1.20000 AFIX 0 C43 1 0.702554 0.031553 0.649499 11.00000 0.02503 0.02852 = 0.03857 0.01377 0.00343 0.00937 AFIX 43 H43 2 0.662743 -0.041077 0.642606 11.00000 -1.20000 AFIX 0 C50 1 1.183114 0.208006 0.375086 11.00000 0.02690 0.04462 = 0.02254 0.00704 0.00688 0.01640 AFIX 43 H50 2 1.264940 0.201055 0.353859 11.00000 -1.20000 AFIX 0 C30 1 0.458229 0.403905 0.572175 11.00000 0.02895 0.03211 = 0.03685 0.00473 -0.00254 0.01544 AFIX 43 H30 2 0.369599 0.397446 0.545315 11.00000 -1.20000 AFIX 0 C38 1 0.567942 0.195042 0.166944 11.00000 0.03452 0.02916 = 0.02166 0.00592 0.00388 0.00801 AFIX 43 H38 2 0.550988 0.202190 0.110733 11.00000 -1.20000 AFIX 0 C23 1 0.176317 0.183983 0.627036 11.00000 0.03638 0.03365 = 0.02718 0.00205 -0.00688 0.01483 AFIX 43 H23 2 0.094229 0.180922 0.594306 11.00000 -1.20000 AFIX 0 C3 1 0.178678 0.068306 1.021113 11.00000 0.02881 0.03107 = 0.03412 0.00924 0.00332 0.01270 AFIX 43 H3 2 0.220365 0.027234 0.986352 11.00000 -1.20000 AFIX 0 C25 1 0.399111 0.161167 0.635377 11.00000 0.04097 0.03123 = 0.02778 0.00365 0.00957 0.01878 AFIX 43 H25 2 0.469695 0.142279 0.608391 11.00000 -1.20000 AFIX 0 C33 1 0.652415 0.463032 0.790697 11.00000 0.02923 0.03863 = 0.02723 0.00630 0.00579 0.01375 AFIX 137 H33A 2 0.570854 0.468945 0.817130 11.00000 -1.50000 H33B 2 0.730963 0.528138 0.809028 11.00000 -1.50000 H33C 2 0.677976 0.407412 0.807480 11.00000 -1.50000 AFIX 0 C37 1 0.646454 0.136618 0.185314 11.00000 0.03725 0.02903 = 0.02475 0.00084 0.00772 0.01160 AFIX 43 H37 2 0.686520 0.104558 0.142050 11.00000 -1.20000 AFIX 0 C5 1 0.093913 0.114627 1.150226 11.00000 0.03206 0.03872 = 0.02527 0.01074 -0.00055 0.00564 AFIX 43 H5 2 0.072184 0.103719 1.204464 11.00000 -1.20000 AFIX 0 C44 1 0.748617 0.094025 0.729429 11.00000 0.03731 0.04501 = 0.02863 0.01801 0.00745 0.02194 AFIX 43 H44 2 0.738114 0.064599 0.777727 11.00000 -1.20000 AFIX 0 C24 1 0.279587 0.156297 0.587797 11.00000 0.04967 0.03088 = 0.02088 0.00053 0.00069 0.01739 AFIX 43 H24 2 0.267982 0.133969 0.528117 11.00000 -1.20000 AFIX 0 C45 1 0.809749 0.199002 0.738825 11.00000 0.05111 0.03999 = 0.02104 0.00210 -0.00192 0.02372 AFIX 43 H45 2 0.842377 0.241850 0.793690 11.00000 -1.20000 AFIX 0 C40 1 0.434684 0.311991 0.215169 11.00000 0.03222 0.03732 = 0.03640 0.00973 0.00075 0.01461 AFIX 137 H40A 2 0.381334 0.322784 0.261999 11.00000 -1.50000 H40B 2 0.370444 0.279552 0.162613 11.00000 -1.50000 H40C 2 0.500452 0.378498 0.209877 11.00000 -1.50000 AFIX 0 C4 1 0.151407 0.052191 1.100203 11.00000 0.03472 0.03515 = 0.03598 0.01601 -0.00117 0.01198 AFIX 43 H4 2 0.171918 -0.001308 1.120161 11.00000 -1.20000 AFIX 0 C14 1 0.178608 0.521963 0.701819 11.00000 0.03095 0.05264 = 0.04136 0.02512 0.00398 0.01540 AFIX 137 H14A 2 0.173283 0.463778 0.656321 11.00000 -1.50000 H14B 2 0.272132 0.574298 0.710055 11.00000 -1.50000 H14C 2 0.108825 0.551933 0.686743 11.00000 -1.50000 AFIX 0 C7 1 0.014131 0.267948 1.173765 11.00000 0.03488 0.04543 = 0.03631 0.00018 0.00640 0.01337 AFIX 137 H7A 2 -0.040423 0.233813 1.214199 11.00000 -1.50000 H7B 2 -0.045455 0.290288 1.137913 11.00000 -1.50000 H7C 2 0.092917 0.328023 1.204441 11.00000 -1.50000 AFIX 0 HKLF 4 REM ph2silut2_ap_a.res in P-1 REM wR2 = 0.0969, GooF = S = 1.025, Restrained GooF = 1.025 for all data REM R1 = 0.0359 for 7390 Fo > 4sig(Fo) and 0.0394 for all 8084 data REM 527 parameters refined using 0 restraints END WGHT 0.0518 0.5956 REM Highest difference peak 0.361, deepest hole -0.238, 1-sigma level 0.041 Q1 1 0.8037 0.3157 0.5062 11.00000 0.05 0.36 Q2 1 0.4252 0.2399 0.9032 11.00000 0.05 0.34 Q3 1 0.3364 0.3293 0.9061 11.00000 0.05 0.33 Q4 1 0.3148 0.2430 0.8151 11.00000 0.05 0.32 Q5 1 0.7957 0.2187 0.5453 11.00000 0.05 0.31 Q6 1 0.8765 0.2365 0.4658 11.00000 0.05 0.27 Q7 1 0.2386 0.1992 0.8979 11.00000 0.05 0.25 Q8 1 0.6791 0.1835 0.4514 11.00000 0.05 0.25 Q9 1 0.6176 0.1663 0.3772 11.00000 0.05 0.24 Q10 1 0.7449 0.3916 0.5392 11.00000 0.05 0.23 ; _shelx_res_checksum 323 _shelx_hkl_file ; 0 0 -2 19110.0 562.735 16 0 0 2 19254.7 557.147 4 0 0 -3 6412.83 343.615 16 0 0 3 6619.46 342.967 4 0 0 -4 31925.8 1025.36 16 0 0 4 31353.5 994.645 4 0 0 -5 3010.19 319.907 16 0 0 5 3213.63 310.170 4 0 0 -6 10726.2 681.191 16 0 0 6 10531.6 646.188 4 0 0 -7 937.768 237.906 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11057.0 997.178 4 0 8 -11 11082.5 464.585 8 0 8 -11 11248.3 458.065 7 0 8 -11 10035.3 414.078 12 0 8 -10 71.9534 56.7355 7 0 -8 10 213.221 128.798 4 0 -8 10 107.314 179.668 5 0 8 -10 14.9242 44.6399 12 0 -8 9 25567.1 1404.10 5 0 8 -9 24478.3 706.608 7 0 8 -9 23533.9 674.787 12 0 -8 8 11356.4 869.324 5 0 8 -8 10997.4 408.817 7 0 -8 7 21999.4 1198.61 5 0 -8 6 8074.30 682.023 5 0 -8 5 29441.0 1349.63 5 0 -8 4 191.446 112.846 5 0 -8 3 382746. 8210.62 5 0 -8 2 26441.7 1246.28 5 0 -8 1 1635.96 306.494 5 0 -8 0 61.4516 126.397 5 0 8 0 105.893 96.0936 3 0 8 1 1993.47 318.584 3 0 8 2 566.798 195.284 3 0 8 3 244.777 99.0735 3 0 8 4 31952.3 1514.44 3 0 -8 -4 32126.8 843.997 9 0 -8 -4 30616.5 858.575 8 0 8 4 32173.4 802.299 12 0 -8 -4 32142.0 838.681 10 0 8 5 24377.8 1343.42 3 0 -8 -5 23526.5 713.940 8 0 -8 -5 23171.2 687.516 9 0 8 5 23514.7 654.374 12 0 8 6 1086.19 278.888 3 0 -8 -6 1211.22 139.132 9 0 -8 -6 1089.00 147.123 8 0 8 6 1287.72 129.710 12 0 -8 -7 11369.3 454.291 9 0 -8 -7 11059.3 471.110 8 0 8 7 11492.4 421.026 12 0 -8 -8 1289.14 148.135 9 0 -8 -8 1212.08 162.313 8 0 8 8 1338.27 135.119 12 0 -8 -9 402.961 90.4796 9 0 -8 -9 376.918 102.552 8 0 8 9 343.625 79.9417 12 0 -8 -10 2870.85 214.926 9 0 -8 -10 2870.67 228.697 8 0 8 10 2734.76 189.324 12 0 -8 -11 1083.06 137.930 8 0 -8 -11 1049.50 127.467 9 0 8 11 1198.01 121.207 12 0 -8 -12 505.311 88.3560 9 0 -8 -12 586.521 109.831 8 0 8 12 383.461 68.5102 12 0 -8 -13 288.252 62.7314 9 0 -8 -13 256.453 70.0703 8 0 9 -17 12.2036 38.9077 7 0 9 -16 299.014 124.807 7 0 9 -16 235.451 71.9948 8 0 9 -15 3449.03 233.179 8 0 9 -15 3723.15 250.440 7 0 9 -14 116.178 58.7707 7 0 9 -14 137.307 68.4107 8 0 9 -13 1230.57 155.344 7 0 9 -13 1143.32 147.561 8 0 9 -12 1480.99 160.819 7 0 9 -12 1436.33 162.058 8 0 9 -12 1406.02 151.888 12 0 9 -11 11813.3 478.740 8 0 9 -11 11659.1 474.026 7 0 9 -11 10957.5 432.510 12 0 9 -10 13690.1 501.771 7 0 9 -10 12634.6 463.950 12 0 9 -9 7766.18 358.313 7 0 9 -9 8047.53 342.632 12 0 -9 8 13283.2 982.555 5 0 9 -8 12712.1 450.978 7 0 9 -8 11419.0 419.999 12 0 -9 7 779.752 271.215 5 0 9 -7 1136.13 120.878 7 0 9 -7 760.642 95.3186 12 0 -9 6 1227.08 302.031 5 0 -9 6 989.037 112.935 9 0 9 -6 1159.02 115.703 7 0 9 -6 1256.39 118.183 12 0 -9 5 1553.59 330.119 5 0 -9 4 13722.7 944.329 5 0 -9 3 2315.57 398.177 5 0 -9 2 135726. 3760.59 5 0 -9 1 1233.07 304.175 5 0 9 0 3908.36 468.275 3 0 -9 0 3937.91 512.954 5 0 9 0 3901.11 200.991 12 0 9 1 88.7012 101.602 3 0 -9 -1 93.7242 128.207 5 0 -9 -1-5.47402 44.9575 9 0 9 1 26.4464 43.0953 12 0 9 2 2646.39 409.368 3 0 -9 -2 2746.77 190.356 9 0 9 2 2833.46 177.018 12 0 9 3 4605.19 552.687 3 0 -9 -3 4840.08 257.020 9 0 9 3 4708.48 239.944 12 0 9 4 2699.08 440.871 3 0 -9 -4 2921.77 206.440 9 0 9 4 2827.34 185.361 12 0 9 5 39798.2 1878.83 3 0 -9 -5 42961.5 1084.43 9 0 9 5 42451.8 1036.36 12 0 -9 -6 7546.58 356.184 9 0 -9 -6 7061.33 361.539 8 0 9 6 7379.46 324.157 12 0 -9 -7 1604.88 177.176 8 0 -9 -7 1891.74 177.340 9 0 9 7 1796.57 156.034 12 0 -9 -8 5915.30 315.468 9 0 -9 -8 5163.22 316.080 8 0 9 8 5828.85 285.671 12 0 -9 -9 4507.44 281.039 8 0 -9 -9 4911.51 277.721 9 0 9 9 4989.18 256.343 12 0 -9 -10 478.415 99.1257 9 0 9 10 424.124 70.1336 12 0 -9 -11 202.592 76.7757 9 0 9 11 185.807 56.3494 12 0 -9 -12 1745.12 138.079 9 0 -9 -13 439.233 65.8727 9 0 10 -17 223.940 51.9784 7 0 10 -16 4907.56 258.070 7 0 10 -15 2481.30 184.152 8 0 10 -15 2652.12 203.824 7 0 10 -14 144.703 70.0097 7 0 10 -14 179.012 75.4385 8 0 10 -13 4323.49 263.094 8 0 10 -13 4018.12 267.052 7 0 10 -12 8701.81 388.161 8 0 10 -12 7962.44 388.264 7 0 10 -12 8047.92 355.735 12 0 10 -11 16393.8 575.037 7 0 10 -11 15225.5 557.036 8 0 10 -11 15474.1 529.787 12 0 10 -10 31121.3 883.182 7 0 10 -10 31476.2 849.718 12 0 10 -9 13000.3 487.865 7 0 10 -9 12839.3 462.764 12 0 10 -8 30.7509 54.8675 7 0 -10 8 49.2090 138.977 5 0 10 -8 256.322 71.5971 12 0 -10 7 4064.32 559.153 5 0 10 -7 4012.64 235.237 7 0 10 -7 3569.36 216.712 12 0 -10 6 5839.97 653.922 5 0 10 -6 5120.92 262.576 7 0 -10 6 5042.94 263.726 9 0 10 -6 5134.85 258.634 12 0 -10 5 45148.7 1921.97 5 0 -10 5 43155.8 1052.83 9 0 10 -5 42168.5 1025.01 7 0 10 -5 43250.8 1030.03 12 0 -10 4 23876.0 1341.95 5 0 -10 4 21849.0 637.006 9 0 10 -4 21955.5 622.387 12 0 -10 3 10078.3 852.584 5 0 -10 3 8938.00 357.834 9 0 10 -3 9142.91 347.626 12 0 -10 2 969.846 270.253 5 0 -10 2 1295.28 132.377 9 0 10 -2 1085.04 115.516 12 0 -10 1 1516.05 360.556 5 0 -10 1 1771.67 152.391 9 0 10 -1 1817.79 149.790 12 0 -10 0 1554.55 334.329 5 0 -10 0 1360.75 136.192 9 0 10 0 1388.90 128.202 12 0 -10 -1 1475.76 382.735 5 0 10 1 1337.83 314.560 3 0 -10 -1 1192.08 131.595 9 0 10 1 1065.41 111.293 12 0 -10 -2 2032.36 172.558 9 0 10 2 2408.86 174.368 12 0 10 3 3546.13 526.954 3 0 -10 -3 4288.17 252.232 9 0 10 3 4206.61 237.679 12 0 -10 -4 86043.6 1890.47 9 0 10 4 84750.6 1834.09 12 0 -10 -5 2249.40 189.912 9 0 10 5 2231.26 174.145 12 0 -10 -6 9155.07 401.702 9 0 10 6 9167.85 372.501 12 0 -10 -7 7531.58 356.911 9 0 10 7 7632.48 329.944 12 0 -10 -8 8682.44 376.203 9 0 10 8 9079.94 357.624 12 0 -10 -9 5132.46 266.158 9 0 10 9 4702.36 238.958 12 0 -10 -10 3733.00 212.502 9 0 10 10 3865.29 199.542 12 0 -10 -11 577.761 80.2782 9 0 -10 -12 145.826 42.6699 9 0 11 -17 657.979 73.9518 7 0 11 -16 1932.20 146.121 7 0 11 -15 1890.76 160.681 7 0 11 -14 5768.07 302.636 7 0 11 -13 5204.42 268.321 8 0 11 -13 5066.41 289.242 7 0 11 -12 347.276 95.3958 7 0 11 -12 257.620 80.5440 8 0 11 -12 269.361 70.8343 12 0 11 -11 2614.94 209.959 8 0 11 -11 2975.11 220.238 7 0 11 -10 4749.71 278.479 7 0 11 -10 4457.65 253.644 12 0 11 -9 3657.54 240.011 7 0 11 -9 3612.30 224.354 12 0 11 -8 2874.37 214.808 7 0 11 -8 3273.48 207.350 12 0 11 -7 3389.94 218.228 7 0 11 -7 3021.85 204.881 12 0 11 -6 32.2097 51.5406 7 0 -11 6 69.9402 60.1453 9 0 11 -6 0.13570 47.9870 12 0 -11 5 30190.3 829.091 9 0 11 -5 30324.2 806.894 7 0 11 -5 31062.9 809.667 12 0 11 -4 108.753 50.9766 7 0 -11 4 68.9214 60.8635 9 0 11 -4 28.5347 52.3367 12 0 -11 3 16124.0 535.339 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58.3470 49.7537 12 0 12 -9 12331.2 465.328 7 0 12 -9 12282.7 443.695 12 0 12 -8 822.182 124.792 7 0 12 -8 735.964 108.684 12 0 12 -7 246.237 74.2106 7 0 12 -7 374.451 88.0307 12 0 12 -6 1537.70 149.724 7 0 12 -6 1529.59 144.153 12 0 12 -5 7706.94 332.717 7 0 -12 5 7106.28 335.697 9 0 12 -5 7152.71 319.251 12 0 12 -4 18088.9 553.632 7 0 -12 4 16423.4 568.006 9 0 12 -4 17610.9 556.276 12 0 12 -3 429.031 80.0330 7 0 -12 3 488.075 104.085 9 0 12 -3 477.322 91.2183 12 0 -12 2 20845.2 663.114 9 0 12 -2 22722.2 646.255 12 0 -12 1 9208.37 402.898 9 0 12 -1 9870.77 381.500 12 0 -12 0 1370.17 146.238 9 0 12 0 1302.75 131.357 12 0 -12 -1 601.579 110.478 9 0 12 1 498.303 90.0094 12 0 -12 -2 1951.50 177.196 9 0 12 2 2137.33 172.594 12 0 -12 -3 754.903 122.937 9 0 12 3 737.833 103.226 12 0 -12 -4 1715.26 161.114 9 0 12 4 1649.89 146.541 12 0 -12 -5 9851.93 392.719 9 0 12 5 10017.6 376.345 12 0 -12 -6 3326.40 211.436 9 0 12 6 3578.77 200.467 12 0 -12 -7 1654.47 142.391 9 0 12 7 1760.64 135.410 12 0 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192.238 7 -2 4 -14 1876.80 200.207 8 -2 4 -15 23105.3 789.186 7 -2 4 -15 25852.1 813.994 8 -2 4 -16 193.377 80.4490 7 -2 4 -16 104.133 72.3040 8 -2 4 -17 1426.32 149.564 8 -2 4 -18 17315.1 544.719 8 -2 4 -19 258.888 93.2606 11 2 -3 -18 6957.83 277.320 9 2 -3 -18 6975.18 284.432 8 2 -3 -17 1443.58 144.126 9 2 -3 -17 1192.64 135.547 8 2 -3 -16 930.977 135.049 8 2 -3 -16 975.685 131.470 9 2 -3 -15 6893.87 365.663 9 2 -3 -15 6635.05 373.228 8 2 -3 -14 19806.1 702.845 9 2 -3 -14 20186.8 720.710 8 2 -3 -13 15949.6 602.658 9 2 -3 -13 15074.9 598.301 8 2 -3 -12 644.041 115.908 8 2 -3 -12 675.559 119.136 9 -2 3 12 512.356 211.579 3 -2 3 12 796.636 348.782 4 2 -3 -11 4692.83 292.687 9 2 -3 -11 4679.11 286.500 8 -2 3 11 5457.22 735.817 3 -2 3 11 5538.64 749.404 4 2 -3 -10 53472.8 1318.26 9 -2 3 10 58112.9 2456.33 3 -2 3 10 59070.5 2484.54 4 -2 3 9 4714.45 610.374 3 -2 3 9 5162.78 631.951 4 -2 3 8 694.435 210.610 4 -2 3 8 378.491 185.587 3 2 -3 -7 333.413 131.062 16 -2 3 7 419.077 194.312 3 -2 3 7 384.276 155.463 4 2 -3 -6 36850.3 1412.44 16 -2 3 6 37388.1 1467.27 3 -2 3 6 37213.1 1494.99 4 2 -3 -5 2985.27 321.830 16 -2 3 5 2948.76 346.797 3 -2 3 5 3325.25 375.867 4 2 -3 -4 68561.5 1827.99 16 -2 3 4 72555.4 1964.11 3 -2 3 4 71090.8 1995.47 4 2 -3 -3 63414.0 1580.79 16 -2 3 3 65005.2 1719.24 3 2 -3 -2 10070.0 396.831 16 -2 3 2 10123.9 494.484 3 2 -3 -1 841.695 76.2351 16 -2 3 1 855.760 135.272 1 -2 3 1 964.155 131.960 3 -2 3 0 312321. 6169.14 3 -2 3 0 317850. 6162.17 1 -2 3 0 322253. 6295.40 2 -2 3 -1 15997.5 569.386 1 -2 3 -1 15296.2 637.628 2 -2 3 -1 15783.7 582.784 3 2 -3 2 185654. 3799.64 5 -2 3 -2 191920. 3910.77 1 -2 3 -3 19579.4 837.639 2 2 -3 3 18304.6 626.783 5 -2 3 -4 715.112 169.547 2 2 -3 4 737.139 124.748 5 2 -3 5 2699.14 275.215 5 -2 3 -5 2671.25 344.329 2 -2 3 -6 14191.1 896.306 2 2 -3 6 15173.6 764.858 4 -2 3 -7 73.9549 147.848 2 2 -3 7 75.5655 105.204 4 -2 3 -8 33803.6 1683.50 2 2 -3 8 33599.4 1430.44 4 -2 3 -9 39959.7 1980.85 2 2 -3 9 44369.5 1803.67 4 2 -3 10 14118.0 1038.21 4 -2 3 -10 12719.9 1131.10 2 2 -3 11 14243.4 1115.57 4 -2 3 -11 13311.1 1247.39 2 -2 3 -11 14890.4 555.546 8 -2 3 -11 15355.9 570.108 7 -2 3 -12 346.571 274.495 2 2 -3 12 130.045 193.688 4 -2 3 -12 66.3059 73.1469 8 -2 3 -12 145.098 71.7914 7 -2 3 -13 4500.19 302.234 8 -2 3 -13 4008.76 290.140 7 -2 3 -14 7986.36 417.835 8 -2 3 -14 8182.08 420.884 7 -2 3 -15 6202.79 353.714 7 -2 3 -15 6241.24 366.649 8 -2 3 -16 205.042 89.0632 8 -2 3 -17 384.336 98.1432 8 -2 3 -18 2977.10 196.246 8 -2 3 -18 2759.63 230.203 11 -2 3 -19 88.0919 64.4294 11 2 -2 -18 152.678 48.6466 8 2 -2 -18 268.565 71.7190 9 2 -2 -17 286.168 82.3383 8 2 -2 -17 457.934 102.665 9 2 -2 -16 11477.2 480.132 9 2 -2 -16 11171.0 486.072 8 2 -2 -15 14718.8 587.335 9 2 -2 -15 15552.5 616.349 8 2 -2 -14 7481.96 400.962 9 2 -2 -14 6826.58 391.777 8 2 -2 -13 3817.39 281.233 8 2 -2 -13 4247.97 288.060 9 2 -2 -12 6944.65 371.451 9 2 -2 -12 6564.15 359.108 8 -2 2 12 7261.03 886.583 3 -2 2 12 7792.38 915.825 4 2 -2 -11 2006.37 192.463 8 2 -2 -11 2172.01 198.630 9 -2 2 11 1522.09 409.676 3 -2 2 11 2377.76 494.089 4 -2 2 10 2122.96 441.991 4 2 -2 -9 216.277 175.482 16 -2 2 9 66.9403 109.864 4 2 -2 -8 22467.1 1230.48 16 -2 2 8 22613.9 1258.79 4 2 -2 -7 3846.48 450.659 16 -2 2 7 4498.34 490.447 4 2 -2 -6 16784.9 858.912 16 -2 2 6 16361.5 895.123 4 2 -2 -5 1682.22 231.336 16 -2 2 5 1818.74 260.888 4 2 -2 -4 599.684 126.233 16 -2 2 4 491.037 128.343 4 -2 2 4 528.323 118.239 3 2 -2 -3 10322.7 465.334 16 -2 2 3 10716.8 516.162 3 -2 2 3 10229.9 528.284 4 2 -2 -2 374736. 7264.29 16 -2 2 2 391356. 7386.12 3 -2 2 2 387339. 7444.72 4 2 -2 -1 302359. 5649.04 16 -2 2 1 300592. 6020.07 2 -2 2 1 289187. 5755.58 3 -2 2 1 306762. 5954.70 1 -2 2 0 89109.7 1859.82 3 -2 2 0 87522.9 1991.39 1 -2 2 0 82444.9 2052.66 2 2 -2 1 653109. 12016.0 5 -2 2 -1 650059. 12347.4 1 -2 2 -1 661195. 12454.3 2 -2 2 -2 2581.81 239.705 1 2 -2 2 2497.13 150.074 5 -2 2 -2 2610.10 263.291 2 -2 2 -3 14875.4 717.864 2 -2 2 -4 9126.35 593.619 2 -2 2 -5 23414.5 1100.65 2 2 -2 5 24812.6 911.726 4 2 -2 6 6089.26 464.893 4 -2 2 -6 5905.61 560.311 2 -2 2 -7 8551.80 764.056 2 2 -2 7 8983.89 630.160 4 -2 2 -8 176426. 4880.78 2 2 -2 8 182784. 4445.22 4 2 -2 9 24316.8 1281.22 4 -2 2 -9 23335.0 1490.36 2 -2 2 -10 107565. 3819.61 2 2 -2 10 106732. 3363.06 4 2 -2 11 617.047 273.808 4 -2 2 -11 892.640 309.789 2 -2 2 -11 1054.17 138.860 7 -2 2 -11 738.260 120.902 8 -2 2 -12-27.7464 228.452 2 -2 2 -12 56.8162 57.0239 8 -2 2 -12 49.5939 61.7760 7 -2 2 -13 1918.03 204.039 7 -2 2 -13 1879.32 195.422 8 -2 2 -14 17470.0 665.437 8 -2 2 -14 17370.3 646.946 7 -2 2 -15 179.026 86.5815 8 -2 2 -16 575.347 116.702 8 -2 2 -17 1490.77 160.894 8 -2 2 -17 1436.85 191.796 11 -2 2 -18 11578.3 423.884 8 -2 2 -19 166.763 74.6863 11 2 -1 -19 319.196 60.5387 8 2 -1 -19 385.158 61.3184 9 2 -1 -18 5286.68 260.706 9 2 -1 -18 5417.69 276.766 8 2 -1 -17 97.9196 76.0596 8 2 -1 -17 35.7238 55.4405 9 2 -1 -16 1553.08 181.687 8 2 -1 -16 1638.13 167.281 9 2 -1 -15 782.849 143.645 8 2 -1 -15 725.295 144.820 9 2 -1 -14 1115.84 160.771 8 2 -1 -14 1359.23 169.557 9 2 -1 -13 22067.5 748.485 9 2 -1 -13 20409.2 734.792 8 2 -1 -12 6171.37 346.607 8 -2 1 12 6967.43 888.784 4 2 -1 -11 31857.2 915.306 8 2 -1 -11 32759.9 1888.19 16 -2 1 11 33595.7 1873.53 4 2 -1 -10 33510.0 1770.93 16 -2 1 10 35312.3 1813.51 4 2 -1 -9 5698.42 635.859 16 -2 1 9 6560.14 691.339 4 2 -1 -8 46221.3 1818.20 16 -2 1 8 46342.2 1869.30 4 2 -1 -7 5840.65 535.074 16 -2 1 7 6582.43 587.946 4 2 -1 -6 44650.4 1509.00 16 -2 1 6 44072.7 1567.17 4 2 -1 -5 13960.1 686.642 16 -2 1 5 13925.8 727.630 4 2 -1 -4 62.4058 46.9964 16 -2 1 4 43.1104 70.0301 4 2 -1 -3 174.694 72.6516 16 -2 1 3 99.1992 71.2569 4 2 -1 -2 58130.5 1386.87 16 -2 1 2 57083.1 1328.90 3 -2 1 2 57318.8 1393.88 4 2 -1 -1 41391.1 1057.75 16 -2 1 1 44443.0 972.646 3 -2 1 1 43818.1 1285.10 2 -2 1 1 42480.8 1015.53 4 -2 1 0 69079.8 1748.75 2 -2 1 -1 139986. 3099.55 2 -2 1 -2 138.673 92.5559 2 2 -1 2 160.748 44.2870 4 -2 1 -3 121301. 2891.11 2 2 -1 3 119867. 2502.10 4 -2 1 -4 129751. 3157.67 2 2 -1 4 126471. 2777.97 4 2 -1 5 59157.0 1628.95 4 -2 1 -5 60097.5 1940.39 2 -2 1 -6 564.604 200.036 2 2 -1 6 2420.04 288.202 4 2 -1 7 1513.89 263.665 4 -2 1 -7 1746.66 336.321 2 2 -1 8 4433.54 483.044 4 -2 1 -8 4273.74 581.331 2 -2 1 -9 16751.6 1261.88 2 2 -1 9 18440.0 1096.95 4 2 -1 10 46772.1 2001.01 4 -2 1 -10 46553.4 2361.99 2 -2 1 -11 4528.26 748.133 2 2 -1 11 4746.23 637.448 4 -2 1 -11 4914.43 298.611 8 -2 1 -11 5320.55 304.432 7 -2 1 -12 904.491 145.001 7 -2 1 -12 917.844 135.655 8 -2 1 -13 20277.3 698.728 7 -2 1 -13 19846.4 719.756 8 -2 1 -14 2622.69 244.334 8 -2 1 -15 10894.5 505.109 8 -2 1 -16 5400.40 326.433 8 -2 1 -17 2401.29 198.856 8 -2 1 -17 2183.66 224.756 11 -2 1 -18 3839.28 223.430 8 2 0 -19 1502.75 117.076 9 2 0 -19 1316.46 118.400 8 2 0 -18 348.040 87.4306 8 2 0 -18 276.808 75.3108 9 2 0 -17 4369.41 279.317 8 2 0 -17 4245.11 264.101 9 2 0 -16 165.432 87.1570 8 2 0 -16 174.630 73.3452 9 2 0 -15 21382.8 758.326 8 2 0 -15 22368.1 753.354 9 -2 0 15 19642.7 701.475 15 2 0 -14 14111.9 591.457 8 2 0 -13 50587.6 1352.13 8 -2 0 13 52415.7 2632.08 4 2 0 -12 49.8983 73.5745 8 2 0 -12-155.357 172.859 16 -2 0 12 60.1327 144.380 4 2 0 -11 4203.63 629.405 16 -2 0 11 3704.07 596.989 4 2 0 -10 14822.4 1121.95 16 -2 0 10 15482.5 1146.56 4 2 0 -9 22229.1 1279.31 16 -2 0 9 22083.5 1289.79 4 2 0 -8 45542.2 1796.52 16 -2 0 8 49128.3 1888.08 4 2 0 -7 47137.9 1689.01 16 -2 0 7 49377.5 1769.33 4 2 0 -6 54286.9 1715.37 16 -2 0 6 54967.1 1771.07 4 2 0 -5 34060.2 1172.60 16 -2 0 5 33748.3 1200.15 4 2 0 -4 54744.0 1509.07 16 -2 0 4 53656.0 1520.49 4 2 0 -3 24.3034 58.1611 16 -2 0 3 133.747 74.2094 4 -2 0 2 15363.1 549.895 5 -2 0 2 14471.9 518.870 4 -2 0 1 233134. 4468.62 5 -2 0 1 233097. 4851.10 2 -2 0 1 231736. 4418.40 4 -2 0 0 120470. 2329.79 5 -2 0 0 117579. 2722.48 2 -2 0 -1 14212.9 636.563 2 -2 0 -2 16194.2 711.824 2 2 0 2 15186.3 425.845 4 2 0 3 140546. 2902.30 4 -2 0 -3 145371. 3331.74 2 -2 0 -4 26299.4 1100.49 2 2 0 4 27527.6 876.486 4 -2 0 -5 38228.7 1474.86 2 2 0 5 38786.5 1219.55 4 2 0 6 679.291 157.203 4 -2 0 -6 682.563 214.363 2 2 0 7 24828.7 1097.79 4 -2 0 -7 21815.0 1257.63 2 -2 0 -8 171394. 4890.86 2 2 0 8 187723. 4485.14 4 2 0 9-87.8224 128.589 4 -2 0 -9 23.5688 110.409 2 -2 0 -10 29045.9 1857.77 2 2 0 10 33427.0 1636.30 4 -2 0 -11 425.905 273.458 2 -2 0 -11 552.798 108.081 8 -2 0 -11 594.858 107.857 7 -2 0 -12 4901.79 859.332 2 -2 0 -12 5427.47 331.978 8 -2 0 -13 3902.69 290.367 8 -2 0 -14 2497.95 237.798 8 -2 0 -15 12940.0 551.627 8 -2 0 -15 11675.4 575.124 11 -2 0 -16 60.4394 74.8270 8 -2 0 -16 211.869 125.957 11 -2 0 -17-14.9759 61.7435 8 -2 0 -17-7.79079 73.8840 11 -2 0 -18 1356.06 126.195 8 -2 0 -18 1412.27 148.815 11 2 1 -19 542.286 80.8389 8 2 1 -19 580.358 78.7520 9 2 1 -18 4136.22 237.845 9 2 1 -18 4215.48 254.351 8 2 1 -17 63.7772 68.0668 8 2 1 -17 73.2594 60.6551 9 -2 -1 17 116.428 55.7350 15 2 1 -16 208.204 81.6852 8 2 1 -16 206.301 97.2157 9 -2 -1 16 120.326 67.7430 15 2 1 -15 4171.48 304.046 8 2 1 -14 6628.36 386.451 8 2 1 -13 32.1459 76.5152 8 2 1 -13 301.307 210.905 16 -2 -1 13-21.8590 188.839 4 2 1 -12 7192.77 376.410 8 2 1 -12 6497.81 842.700 16 -2 -1 12 7686.63 910.557 4 2 1 -11 554.419 283.612 16 -2 -1 11 109.180 203.648 4 2 1 -10 80113.6 2848.08 16 -2 -1 10 79641.3 2881.86 4 2 1 -9 129.528 163.624 16 -2 -1 9 25.7863 112.581 4 2 1 -8 27948.2 1310.51 16 -2 -1 8 28515.8 1365.78 4 2 1 -7 21209.3 1033.15 16 -2 -1 7 19687.1 1027.19 4 2 1 -6 4339.66 415.469 16 -2 -1 6 4043.11 410.402 4 2 1 -5 79200.2 2149.84 16 -2 -1 5 84294.5 2186.21 4 2 1 -4 47621.3 1409.36 16 -2 -1 4 47810.1 1423.32 5 -2 -1 4 48105.1 1393.65 4 2 1 -3 184445. 3946.41 16 -2 -1 3 190378. 4140.15 1 -2 -1 3 187526. 3928.29 5 -2 -1 3 187764. 3880.49 4 2 1 -2 13183.2 567.269 16 -2 -1 2 13995.6 539.022 5 -2 -1 2 14359.6 665.280 1 -2 -1 2 13954.4 500.672 4 -2 -1 1 593401. 11298.3 1 -2 -1 1 569944. 11365.0 2 -2 -1 1 594233. 11021.9 5 2 1 0 263015. 4780.72 3 -2 -1 0 250078. 4971.81 5 -2 -1 0 248390. 5293.45 2 -2 -1 0 251517. 5272.63 1 -2 -1 -1 994530. 18048.4 1 -2 -1 -1 999999. 18027.5 2 -2 -1 -2 31364.7 1093.98 2 -2 -1 -3 25767.1 1020.66 2 2 1 4 40112.7 1156.71 4 -2 -1 -4 38100.1 1398.98 2 2 1 5 51157.6 1500.48 4 -2 -1 -5 49694.0 1754.70 2 -2 -1 -6 163.944 110.143 2 2 1 6 300.426 143.755 4 2 1 7 22380.8 1058.25 4 -2 -1 -7 20514.0 1215.00 2 -2 -1 -8 1435.41 363.583 2 2 1 8 2011.15 331.724 4 -2 -1 -9 7478.41 860.664 2 2 1 9 7897.54 709.125 4 -2 -1 -10 51170.1 2519.49 2 -2 -1 -10 51648.6 1291.09 8 -2 -1 -11 7728.89 998.221 2 -2 -1 -11 9285.02 429.753 8 -2 -1 -12 10994.6 495.936 8 -2 -1 -13-7.00786 81.9662 8 -2 -1 -14 79.8569 86.6978 8 -2 -1 -14-38.5015 100.504 11 -2 -1 -15 2341.57 219.110 8 -2 -1 -15 2331.57 239.156 11 -2 -1 -16 8100.00 394.559 8 -2 -1 -16 6458.04 369.369 11 -2 -1 -17 6926.00 325.914 8 -2 -1 -17 6440.18 326.689 11 -2 -1 -18 1629.49 128.332 8 2 2 -19 5684.12 265.686 8 2 2 -19 5537.27 245.576 9 2 2 -18 1478.16 146.706 9 2 2 -18 1350.95 146.627 8 -2 -2 18 1200.68 133.894 15 2 2 -17 75.7375 82.4164 8 2 2 -17 83.2315 67.3355 9 -2 -2 17 66.5024 60.1337 15 2 2 -16 4246.18 302.782 8 2 2 -15 12275.5 542.006 8 2 2 -14 2094.23 209.786 8 2 2 -13 136.116 78.2844 8 2 2 -13 103.027 227.182 16 -2 -2 13 50.0190 252.801 4 2 2 -12 256.009 97.1710 8 2 2 -12 79.6210 222.107 16 -2 -2 12 367.294 252.081 4 2 2 -11 6154.01 322.058 8 2 2 -11 5642.76 719.543 16 -2 -2 11 6718.79 778.396 4 2 2 -10 16860.3 1149.79 16 -2 -2 10 16064.8 1150.66 4 2 2 -9 1489.53 325.754 16 -2 -2 9 1889.96 370.617 4 2 2 -8 236439. 5609.12 16 -2 -2 8 244821. 5698.55 4 2 2 -7 3097.51 378.604 16 -2 -2 7 3672.83 435.816 4 2 2 -6 800.952 207.843 16 -2 -2 6 815.635 201.443 5 -2 -2 6 853.836 200.592 4 2 2 -5 9534.93 594.810 16 -2 -2 5 9990.82 586.044 4 -2 -2 5 10514.1 620.433 5 2 2 -4 1417.16 215.387 16 -2 -2 4 1750.10 258.631 1 -2 -2 4 1402.02 213.785 5 -2 -2 4 1523.81 197.736 4 2 2 -3 15361.3 678.594 16 -2 -2 3 15185.7 651.569 5 -2 -2 3 16074.4 764.029 1 2 2 -2 447.474 109.880 16 -2 -2 2 552.051 116.607 5 -2 -2 2 517.690 132.818 1 -2 -2 1 444401. 8681.18 1 -2 -2 1 441152. 8476.53 5 -2 -2 1 436991. 8720.82 2 2 2 0 174655. 3425.28 3 -2 -2 0 177783. 3866.61 2 -2 -2 0 177837. 3646.82 5 -2 -2 0 177645. 3859.65 1 -2 -2 -1 59.6425 64.7735 1 2 2 1 102.801 43.9534 3 -2 -2 -1 175.949 75.7577 2 2 2 2 109381. 2416.47 3 -2 -2 -2 109858. 2686.51 2 -2 -2 -3 10122.3 614.062 2 2 2 3 10019.3 523.481 3 2 2 4 55090.8 1607.95 3 -2 -2 -4 53367.4 1757.11 2 2 2 5 27461.9 1126.71 3 -2 -2 -5 26923.6 1228.01 2 -2 -2 -6 1477.33 300.154 2 2 2 7 81.1595 80.9900 3 -2 -2 -7 431.967 195.047 2 2 2 8 2927.39 440.328 3 -2 -2 -8 2261.81 436.416 2 -2 -2 -9 1901.77 400.620 2 2 2 9 2291.67 427.469 3 2 2 10 13073.6 1103.07 3 -2 -2 -10 13494.3 1212.78 2 -2 -2 -10 13817.5 533.450 8 2 2 11 2783.15 563.018 3 -2 -2 -11 2441.24 567.888 2 -2 -2 -11 3290.14 252.756 8 -2 -2 -11 3424.58 277.709 11 -2 -2 -12 56.2693 71.6997 8 -2 -2 -12 73.5737 93.7848 11 -2 -2 -13 21129.7 745.147 8 -2 -2 -13 20642.1 756.889 11 -2 -2 -14 730.719 142.534 8 -2 -2 -14 686.020 147.803 11 -2 -2 -15 4629.57 308.006 8 -2 -2 -15 4525.94 298.902 11 -2 -2 -16 196.925 87.1400 8 -2 -2 -16 180.844 87.3811 11 -2 -2 -17 91.0581 52.5425 8 2 3 -19 94.7516 56.4952 8 -2 -3 19 52.2308 38.3533 15 2 3 -18 12699.6 478.923 8 2 3 -18 13139.0 463.637 9 -2 -3 18 12684.3 463.938 15 2 3 -17 1513.46 176.649 8 2 3 -17 1337.45 157.135 9 2 3 -16 4192.20 295.524 8 2 3 -15 7026.34 393.399 8 2 3 -14 2117.16 214.097 8 2 3 -13 290.571 96.3669 8 2 3 -13 386.410 254.998 16 2 3 -12 10534.0 461.781 8 -2 -3 12 10093.4 1007.99 4 2 3 -12 10114.6 1023.62 16 2 3 -11 837.642 115.404 8 -2 -3 11 748.506 278.760 4 2 3 -11 921.018 294.650 16 -2 -3 11 467.646 108.561 11 -2 -3 10 41460.5 1896.34 4 2 3 -10 39743.5 1868.60 16 -2 -3 9 71942.8 2481.70 4 2 3 -9 69559.0 2456.64 16 -2 -3 8 32616.8 1457.72 4 2 3 -8 34075.3 1489.84 16 -2 -3 7 371.829 115.886 5 -2 -3 7 455.603 169.968 4 2 3 -7 318.440 150.471 16 -2 -3 6 1025.27 216.412 5 -2 -3 6 975.569 194.866 4 2 3 -6 1144.48 235.108 16 -2 -3 5 73404.0 2222.48 1 -2 -3 5 74620.0 2087.96 5 2 3 -5 74762.4 2106.89 16 -2 -3 4 4196.61 366.166 5 -2 -3 4 4442.50 405.546 1 2 3 -4 4010.74 367.968 16 -2 -3 3 61535.6 1701.11 5 -2 -3 3 64030.4 1799.56 1 2 3 -3 60830.2 1732.31 16 -2 -3 2 19055.8 766.582 5 -2 -3 2 19575.3 824.444 1 -2 -3 1 248541. 5223.30 1 -2 -3 1 248174. 5106.26 5 2 3 0 143114. 2986.91 3 -2 -3 0 147282. 3231.96 5 -2 -3 0 144491. 3367.19 2 -2 -3 0 150034. 3364.83 1 2 3 1 15508.5 569.086 3 -2 -3 -1 14510.0 707.720 2 2 3 2 1712.27 194.827 3 -2 -3 -2 1528.13 229.614 2 -2 -3 -3 976.628 208.006 2 2 3 3 805.123 158.831 3 -2 -3 -4 42638.7 1554.42 2 2 3 4 43334.9 1424.24 3 2 3 5 18496.2 922.485 3 -2 -3 -5 17180.1 972.766 2 2 3 6 3180.05 396.222 3 -2 -3 -6 3575.84 457.999 2 2 3 7 9014.10 750.629 3 -2 -3 -7 8461.61 775.316 2 -2 -3 -8 361.546 192.571 2 2 3 8 225.172 117.328 3 2 3 9 909.842 269.570 3 -2 -3 -9 912.388 290.602 2 -2 -3 -9 1045.86 140.672 8 -2 -3 -9 892.648 138.974 11 2 3 10 12738.9 1097.94 3 -2 -3 -10 12305.2 512.855 8 -2 -3 -10 13151.4 538.713 11 -2 -3 -11 1516.44 181.356 8 -2 -3 -11 2009.80 202.166 11 -2 -3 -12 4045.86 294.763 8 -2 -3 -12 4498.11 308.441 11 -2 -3 -13 3216.18 264.906 8 -2 -3 -13 3467.62 272.984 11 -2 -3 -14 272.561 101.439 8 -2 -3 -15 20097.5 672.223 8 -2 -3 -16 1977.57 170.371 8 -2 -3 -17 2675.36 168.164 8 2 4 -19 8545.24 327.735 8 2 4 -19 7939.92 299.998 9 -2 -4 19 8392.35 317.578 15 2 4 -18 133.254 80.1218 8 2 4 -18 83.7173 64.5382 9 -2 -4 18 95.8120 67.6691 15 2 4 -17 310.670 95.1798 8 2 4 -16 177.857 81.8089 8 2 4 -15 1881.55 197.758 8 2 4 -14 8311.44 427.196 8 2 4 -13 874.732 133.757 8 2 4 -12 3068.81 234.959 8 -2 -4 12 2861.24 526.283 4 2 4 -12 2901.95 543.958 16 2 4 -11 646.148 110.584 8 -2 -4 11 572.771 267.140 4 2 4 -11 460.788 230.424 16 -2 -4 11 330.054 95.5127 11 2 4 -10 113.396 167.272 16 -2 -4 10 291.142 175.885 4 2 4 -9 2579.26 431.099 16 -2 -4 9 1729.70 353.996 4 2 4 -8 129575. 3607.51 16 -2 -4 8 139124. 3704.66 5 -2 -4 8 129596. 3562.19 4 2 4 -7 12783.2 836.093 16 -2 -4 7 14679.5 890.788 5 -2 -4 7 14565.5 892.223 1 -2 -4 7 13553.0 826.802 4 2 4 -6 13468.5 806.488 16 -2 -4 6 14627.3 834.310 5 -2 -4 6 14987.7 874.130 1 2 4 -5 1218.72 234.566 16 -2 -4 5 1724.40 294.279 1 -2 -4 5 1728.99 275.978 5 2 4 -4 14715.7 767.699 16 -2 -4 4 15737.8 778.397 5 -2 -4 4 16700.7 828.160 1 2 4 -3 4897.39 426.804 16 -2 -4 3 5788.20 443.821 1 -2 -4 3 5000.87 415.347 5 -2 -4 2 13513.5 684.415 5 -2 -4 2 13688.0 686.424 1 -2 -4 1 3296.10 321.709 5 -2 -4 1 3710.16 340.031 1 -2 -4 0 1538.32 231.857 1 -2 -4 0 1239.54 203.478 2 -2 -4 0 1291.32 217.019 5 -2 -4 -1 69817.0 1947.35 2 2 4 1 68079.7 1720.86 3 -2 -4 -2 98696.5 2565.09 2 2 4 2 99932.5 2399.33 3 2 4 3 7247.10 487.505 3 -2 -4 -3 6571.48 520.147 2 -2 -4 -4 30940.7 1303.60 2 2 4 4 31264.2 1218.43 3 2 4 5 4711.07 463.104 3 -2 -4 -5 4543.20 510.825 2 2 4 6 7164.22 628.685 3 2 4 7 5743.89 606.841 3 -2 -4 -8 7011.16 354.423 8 2 4 8 6636.90 706.157 3 -2 -4 -9 1449.47 165.991 8 2 4 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3270.05 1 -7 2 1 1414.72 406.489 1 -7 2 0 27791.5 1807.72 2 -7 2 0 28668.3 1770.93 1 -7 2 -1 39656.5 2249.99 2 -7 2 -1 39284.5 2124.38 1 -7 2 -1 41888.9 1134.38 6 -7 2 -2 1033.91 371.362 2 -7 2 -2 1115.52 331.166 1 -7 2 -2 1283.09 140.177 10 -7 2 -2 1190.23 157.134 11 -7 2 -3 53667.6 2699.56 2 -7 2 -3 52570.4 1298.40 10 -7 2 -4 14.9371 212.933 2 -7 2 -4 198.841 66.1450 10 -7 2 -4 130.774 106.045 11 -7 2 -5 40024.7 2401.53 2 -7 2 -5 38047.5 1129.30 11 -7 2 -5 41157.8 1091.01 10 -7 2 -6 3461.71 282.791 11 -7 2 -6 3539.74 255.805 10 -7 2 -7 6971.52 409.757 11 -7 2 -7 6472.40 358.181 10 -7 2 -8 1522.94 177.310 10 -7 2 -8 1907.42 227.723 11 -7 2 -9 3721.78 321.629 11 -7 2 -9 3439.62 255.103 10 -7 2 -10 1757.43 171.741 10 -7 2 -10 2083.96 235.288 11 -7 2 -11 22272.7 812.199 11 -7 2 -11 22502.8 676.929 10 -7 2 -12 259.896 64.9714 10 -7 2 -12 371.409 131.122 11 -7 2 -13 4470.34 310.657 11 -7 2 -14 17.6199 84.5677 11 -7 2 -15 480.831 92.6710 11 7 -1 -16 1919.22 140.917 9 -7 1 16 2080.72 155.766 15 7 -1 -15 667.339 96.4634 9 -7 1 15 568.076 101.935 15 7 -1 -14 2.24529 49.0019 9 -7 1 14 100.555 70.8059 15 7 -1 -13-73.1048 64.0956 9 -7 1 13 0.22152 72.3417 15 -7 1 13 168.549 66.4434 13 7 -1 -12 1263.00 148.587 9 -7 1 12 1593.77 163.811 13 -7 1 12 1302.89 176.511 15 -7 1 11 6575.42 352.764 13 -7 1 11 6056.43 375.948 15 -7 1 10 32447.3 949.385 13 -7 1 10 31186.0 983.630 15 -7 1 9 32505.4 969.219 13 -7 1 9 31945.4 982.898 15 -7 1 9 31353.5 858.013 11 -7 1 8 4237.68 743.668 1 -7 1 8 4300.90 301.585 13 -7 1 8 4203.00 297.292 15 -7 1 8 4101.09 251.790 11 -7 1 7 8574.37 1045.63 1 -7 1 7 9103.16 451.099 13 -7 1 7 9098.81 435.833 15 7 -1 -7 8299.39 804.563 16 -7 1 7 8966.03 380.585 11 -7 1 6 3214.84 648.458 1 7 -1 -6 3356.30 476.988 16 -7 1 6 3742.14 286.552 13 -7 1 6 3840.11 266.914 15 -7 1 6 3754.24 280.858 11 -7 1 5 73.2842 164.385 1 -7 1 5 269.972 82.8557 15 7 -1 -5 275.854 151.390 16 -7 1 5 236.330 90.4770 11 -7 1 5 143.062 77.1903 13 -7 1 4 9215.73 1028.79 1 7 -1 -4 6836.81 687.678 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2026.18 145.420 13 -10 4 10 224.486 81.8840 13 -10 4 10 25.6444 54.7199 15 -10 4 9 12878.3 481.160 15 -10 4 9 13971.2 489.251 13 -10 4 8 9080.12 402.903 13 -10 4 8 8926.59 389.441 15 -10 4 7 1644.48 178.965 13 -10 4 7 1630.30 160.894 15 -10 4 6 14768.8 557.712 13 -10 4 6 13800.0 522.492 15 -10 4 5 4348.60 284.901 13 -10 4 5 4253.45 268.056 15 -10 4 4 1529.97 175.527 13 -10 4 4 1633.87 165.955 15 -10 4 3 6103.06 341.791 13 -10 4 3 6448.46 328.469 15 -10 4 2 1111.25 142.847 13 -10 4 2 1231.50 141.891 15 -10 4 1 4862.55 288.482 13 -10 4 1 5332.67 283.094 15 -10 4 0 3169.27 210.605 15 -10 4 0 2606.40 198.339 10 -10 4 -1 12.9498 64.4606 10 -10 4 -1 155.118 65.0332 15 -10 4 -2 8387.34 371.448 10 -10 4 -3 363.432 97.0397 10 -10 4 -4 290.275 103.229 10 -10 4 -4 376.218 113.777 11 -10 4 -5 1849.04 187.439 11 -10 4 -5 2325.41 193.567 10 -10 4 -6 12627.1 474.489 10 -10 4 -7 8135.19 357.682 10 -10 4 -8 837.452 112.026 10 -10 4 -9 11.1006 50.2495 10 -10 4 -10 446.196 64.2510 10 -10 3 13 231.819 47.5945 15 -10 3 12 2006.90 140.304 15 -10 3 12 1942.37 128.974 13 -10 3 11 1739.34 144.483 15 -10 3 11 1778.75 136.889 13 -10 3 10 82.0454 59.7998 13 -10 3 10 44.3309 45.7512 15 -10 3 9 370.634 88.6731 13 -10 3 9 298.383 78.3549 15 -10 3 8 8010.19 377.058 13 -10 3 8 7440.40 354.015 15 -10 3 7 2434.37 220.685 13 -10 3 7 2299.40 195.185 15 -10 3 6 6585.99 356.757 13 -10 3 6 6233.61 324.934 15 -10 3 5 135.718 75.6805 13 -10 3 5 191.891 79.4780 15 -10 3 4 4817.19 310.166 13 -10 3 4 4909.39 282.270 15 -10 3 3 1333.65 153.852 15 -10 3 3 1273.27 165.424 13 -10 3 2 10921.9 475.366 13 -10 3 2 12196.8 458.009 15 -10 3 1 239.545 73.7380 15 -10 3 1 247.401 93.6899 13 -10 3 0 1631.72 172.372 11 -10 3 0 1813.44 161.117 10 -10 3 -1 1002.16 125.590 10 -10 3 -1 778.450 132.783 11 -10 3 -2-42.8170 62.2691 10 -10 3 -2 89.1612 81.9702 11 -10 3 -3 2022.11 176.443 10 -10 3 -3 2152.36 211.737 11 -10 3 -4 533.378 104.353 10 -10 3 -4 454.428 119.798 11 -10 3 -5 3766.06 238.446 10 -10 3 -5 3117.18 249.887 11 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5044.13 267.090 10 -10 2 -1 4827.58 302.669 11 -10 2 -2 367.497 88.3317 10 -10 2 -2 508.790 128.550 11 -10 2 -3 345.710 86.8519 10 -10 2 -3 324.956 100.906 11 -10 2 -4 1000.69 125.713 10 -10 2 -4 874.850 154.369 11 -10 2 -5 754.677 109.647 10 -10 2 -5 523.942 135.371 11 -10 2 -6 1441.29 145.838 10 -10 2 -6 1432.60 170.666 11 -10 2 -7 19103.4 554.567 10 -10 2 -7 16661.7 581.425 11 -10 2 -8 1778.41 141.858 10 -10 2 -8 1800.55 164.414 11 -10 2 -9 1208.17 105.632 10 -10 2 -9 1323.28 130.820 11 -10 1 12 7.86951 33.5126 13 -10 1 12 25.2239 35.5055 15 -10 1 11 2556.93 167.190 15 -10 1 11 2525.21 164.594 13 -10 1 10 1378.24 134.556 13 -10 1 10 1417.49 131.615 15 -10 1 9 1656.72 157.080 13 -10 1 9 1662.11 152.387 15 -10 1 8 4074.04 259.147 13 -10 1 8 4125.44 245.244 15 -10 1 7 515.710 91.2018 15 -10 1 7 373.313 111.805 13 -10 1 6 219.524 106.788 13 -10 1 6 290.625 76.7038 15 -10 1 6 258.662 79.4721 11 -10 1 5 1435.10 175.210 13 -10 1 4 439.450 99.7560 13 -10 1 4 502.423 114.936 11 -10 1 3 2152.54 206.125 13 -10 1 3 2162.22 183.799 11 -10 1 2 12959.6 526.077 13 -10 1 2 12223.0 482.212 11 -10 1 1 16463.7 595.474 13 -10 1 1 16193.9 580.978 11 -10 1 0 2106.56 198.449 11 -10 1 0 2172.53 167.657 10 -10 1 -1 1597.99 183.896 11 -10 1 -1 1757.16 156.453 10 -10 1 -2 6658.04 311.586 10 -10 1 -3 311.766 78.3280 10 -10 1 -3 159.785 113.274 11 -10 1 -4-20.6114 73.6801 10 -10 1 -4 17.5588 82.2431 11 -10 1 -5 978.227 121.282 10 -10 1 -5 827.350 133.147 11 -10 1 -6 525.963 100.060 10 -10 1 -6 290.078 86.5638 11 -10 1 -7 2545.04 168.686 10 -10 1 -7 2611.72 194.026 11 -10 1 -8 319.938 66.4064 10 -10 1 -8 293.127 84.9981 11 -10 1 -9 26587.3 638.813 10 -10 1 -9 29356.2 708.324 11 -10 0 12 392.206 56.4573 13 -10 0 11 17720.5 503.476 13 -10 0 10 1602.21 139.861 13 -10 0 9 32139.4 856.219 13 -10 0 8 1477.37 154.810 13 -10 0 7 1584.25 173.909 13 -10 0 7 1658.33 149.824 11 -10 0 6 4038.39 277.560 13 -10 0 6 4048.12 233.932 11 -10 0 5 3765.89 275.279 13 -10 0 5 3386.24 223.246 11 -10 0 4 1398.12 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142.045 11 -10 -2 4 5414.15 304.215 13 -10 -2 4 5332.04 269.820 11 -10 -2 3 5503.53 306.790 13 -10 -2 3 5151.25 272.672 11 -10 -2 2 2019.51 186.706 13 -10 -2 2 2118.50 177.223 11 -10 -2 1 667.970 123.617 11 -10 -2 1 860.508 121.632 13 -10 -2 0 37.3846 74.5014 11 -10 -2 -1 871.533 121.226 11 -10 -2 -2 94.0018 56.2944 10 -10 -2 -2 209.810 83.5604 11 -10 -2 -3 18.5141 47.0231 10 -10 -2 -3-2.33887 63.8279 11 -10 -2 -4 17276.7 483.189 10 -10 -2 -4 18839.5 542.439 11 -10 -2 -5 81.6412 43.3860 10 -10 -2 -5 27.7397 61.2548 11 -10 -2 -6 1385.58 99.6001 10 -10 -2 -6 1440.28 117.632 11 -10 -3 10 287.195 53.6420 13 -10 -3 10 423.516 61.9203 11 -10 -3 9 24425.7 642.822 13 -10 -3 9 25568.4 611.598 11 -10 -3 8 5049.62 246.267 13 -10 -3 8 4772.50 212.453 11 -10 -3 7 11116.5 404.738 13 -10 -3 7 10532.6 355.552 11 -10 -3 6 354.496 86.6461 13 -10 -3 6 424.970 87.4942 11 -10 -3 5 6781.37 323.056 13 -10 -3 5 6511.44 284.523 11 -10 -3 4 586.809 102.529 11 -10 -3 4 383.365 92.5018 13 -10 -3 3 12387.6 463.752 13 -10 -3 3 12127.9 420.653 11 -10 -3 2 32.5204 65.4701 11 -10 -3 2-57.5840 67.6203 13 -10 -3 1 7616.60 319.189 11 -10 -3 0 412.709 89.7010 11 -10 -3 -1 3785.08 214.302 11 -10 -3 -2 4985.08 205.386 10 -10 -3 -2 5754.47 255.466 11 -10 -3 -3 4748.89 195.610 10 -10 -3 -3 5226.60 236.938 11 -10 -3 -4 1043.39 91.8296 10 -10 -3 -4 1000.26 104.562 11 -10 -4 9 2352.72 139.969 13 -10 -4 9 2786.76 138.648 11 -10 -4 8 4375.53 206.393 13 -10 -4 8 4476.95 187.599 11 -10 -4 7-25.9929 46.7336 13 -10 -4 7 43.1215 46.5329 11 -10 -4 6 6.46078 45.6735 13 -10 -4 6-0.35753 48.7272 11 -10 -4 5 585.026 86.0076 11 -10 -4 5 533.533 91.2829 13 -10 -4 4 15731.6 500.902 13 -10 -4 4 15748.7 461.041 11 -10 -4 3 706.715 85.5267 11 -10 -4 3 663.049 96.7287 13 -10 -4 2 1799.18 146.350 13 -10 -4 2 1902.97 139.461 11 -10 -4 1 623.574 94.2639 11 -10 -4 0 155.336 62.3997 11 -10 -4 -1 139.890 56.1209 11 -10 -4 -2 22.3244 42.4383 11 -10 -5 6 4213.20 197.250 13 -10 -5 6 4360.02 182.453 11 -10 -5 5 2192.42 144.265 13 -10 -5 5 2249.39 131.274 11 -10 -5 4 146.117 51.6262 11 -10 -5 4 37.6288 41.9977 13 -10 -5 3 667.815 78.9808 11 -10 -5 3 575.349 79.7997 13 -10 -5 2 42.1602 51.0126 11 -10 -5 1 2493.50 133.593 11 -11 12 3 15.9563 34.2334 6 -11 12 2 2833.68 165.453 6 -11 12 2 2516.50 126.055 15 -11 12 1 1858.65 139.277 6 -11 12 1 1620.44 103.015 15 -11 12 0 4435.68 217.736 6 -11 12 0 4042.01 171.845 15 -11 12 -1 439.151 58.0709 15 -11 12 -2 1576.40 103.941 15 -11 12 -3 86.9150 37.9161 15 -11 12 -4-20.8709 33.3132 15 -11 12 -5 3878.69 154.370 15 -11 11 4 4501.69 214.231 6 -11 11 4 4154.41 174.633 15 -11 11 3 2016.96 150.290 6 -11 11 3 1855.64 116.625 15 -11 11 2 9514.06 361.280 6 -11 11 2 9132.13 301.626 15 -11 11 1 336.168 77.8836 6 -11 11 1 349.497 63.8590 15 -11 11 0 8164.73 339.397 6 -11 11 0 8276.45 287.455 15 -11 11 -1 387.942 63.0668 15 -11 11 -2 618.065 74.7585 15 -11 11 -3 13420.8 386.432 15 -11 11 -4 3403.04 161.841 15 -11 11 -4 3727.41 187.654 10 -11 11 -5 668.567 80.5639 10 -11 11 -5 669.015 70.7026 15 -11 11 -6 4035.23 161.953 15 -11 11 -6 4363.92 193.801 10 -11 10 6 1885.67 111.470 15 -11 10 5 96.4744 40.3053 15 -11 10 4 1637.56 115.860 15 -11 10 4 1719.34 140.362 6 -11 10 3 76.2850 43.4556 15 -11 10 3 42.3178 43.0815 6 -11 10 2 29.9655 38.5540 15 -11 10 2-2.86283 48.4869 6 -11 10 1 3293.28 178.882 15 -11 10 1 3197.32 218.306 6 -11 10 0 9347.38 328.104 15 -11 10 0 9280.12 391.557 6 -11 10 -1 3789.29 192.319 15 -11 10 -2 13798.4 416.775 15 -11 10 -3-22.2271 46.3896 15 -11 10 -4 503.066 81.8731 10 -11 10 -4 518.202 71.6765 15 -11 10 -5 10802.8 326.618 15 -11 10 -5 10709.0 370.673 10 -11 10 -6 1810.09 108.559 15 -11 10 -6 1881.59 134.539 10 -11 10 -7 13.1446 34.7576 10 -11 9 7 4296.99 182.797 15 -11 9 7 4423.77 201.026 13 -11 9 6-25.5748 41.7280 15 -11 9 6 6.13830 44.2436 13 -11 9 5 4140.13 200.622 15 -11 9 4 8890.79 358.448 6 -11 9 4 9209.98 330.904 15 -11 9 3 2151.07 175.331 6 -11 9 3 2159.45 150.474 15 -11 9 2 20595.4 655.325 6 -11 9 2 21314.8 585.323 15 -11 9 1 49.0652 60.7179 6 -11 9 1 165.893 52.6755 15 -11 9 0 530.843 79.1865 15 -11 9 -1 7248.91 287.571 15 -11 9 -2 245.141 64.5424 15 -11 9 -3 5493.57 235.132 15 -11 9 -3 5576.08 262.674 10 -11 9 -4 973.112 112.567 10 -11 9 -4 980.128 94.2977 15 -11 9 -5 511.898 88.8131 10 -11 9 -5 553.922 71.4774 15 -11 9 -6 2156.87 151.103 10 -11 9 -7 270.666 65.6369 10 -11 9 -8 9900.09 312.486 10 -11 8 8 7161.10 256.862 15 -11 8 8 7572.31 277.081 13 -11 8 7 1196.42 111.529 13 -11 8 7 1288.12 107.709 15 -11 8 6 6782.94 273.215 15 -11 8 6 6887.20 283.355 13 -11 8 5 64.8499 49.9836 13 -11 8 5 97.7594 49.2753 15 -11 8 4 2134.34 170.513 6 -11 8 4 2267.33 158.080 15 -11 8 3 22.3646 48.1044 6 -11 8 3 51.1646 51.7423 15 -11 8 2 39.4272 55.5309 15 -11 8 1 2326.44 162.104 15 -11 8 0 16793.4 508.609 15 -11 8 -1 8730.73 328.489 15 -11 8 -2 7379.08 292.689 15 -11 8 -3 1979.59 136.393 15 -11 8 -3 1752.35 146.769 10 -11 8 -4 200.601 60.3169 10 -11 8 -4 246.452 55.1586 15 -11 8 -5 111.009 59.2717 10 -11 8 -6 1335.94 122.669 10 -11 8 -7 548.511 81.0171 10 -11 8 -8 2093.16 132.027 10 -11 7 9 726.207 84.4034 13 -11 7 9 704.219 71.6361 15 -11 7 8 39.7608 52.5154 13 -11 7 8 131.510 46.4743 15 -11 7 7 7309.58 289.576 15 -11 7 7 7732.40 304.978 13 -11 7 6 1997.42 147.621 15 -11 7 6 1984.68 150.239 13 -11 7 5 5523.51 259.502 15 -11 7 5 5538.91 267.692 13 -11 7 4 6842.08 295.976 15 -11 7 4 6880.03 300.823 13 -11 7 3 13644.6 454.283 15 -11 7 2 25338.3 693.401 15 -11 7 1 150.387 60.6044 15 -11 7 0 1511.05 131.745 15 -11 7 -1 6248.27 272.147 15 -11 7 -2 12279.9 399.028 15 -11 7 -2 11891.5 417.982 10 -11 7 -3 15488.4 499.932 10 -11 7 -4 1851.98 154.753 10 -11 7 -5 1983.48 160.925 10 -11 7 -6 5145.31 250.635 10 -11 7 -7 1899.99 140.486 10 -11 7 -8 1583.11 119.157 10 -11 6 10 3379.67 157.789 15 -11 6 10 3146.19 154.906 13 -11 6 9 2364.20 144.844 15 -11 6 9 2251.91 145.548 13 -11 6 8-101.263 57.2819 13 -11 6 8-21.9740 38.0763 15 -11 6 7 2266.04 157.643 15 -11 6 7 2320.13 166.354 13 -11 6 6 1384.08 130.271 15 -11 6 6 1477.81 142.809 13 -11 6 5 132.700 66.0997 13 -11 6 5 171.005 57.3276 15 -11 6 4 261.786 71.8736 13 -11 6 4 440.885 86.2935 15 -11 6 3 11064.6 403.344 15 -11 6 2 2735.88 182.497 15 -11 6 1 1266.15 125.972 15 -11 6 0 161.038 53.9884 15 -11 6 -1 805.160 95.6154 15 -11 6 -2 158.532 61.1030 10 -11 6 -3 316.054 80.2956 10 -11 6 -4 2215.83 169.026 10 -11 6 -5 285.770 70.2667 10 -11 6 -6 469.805 86.7416 10 -11 6 -7 712.752 91.7376 10 -11 6 -8 5472.86 226.198 10 -11 5 10 14191.5 410.156 15 -11 5 10 14757.4 415.091 13 -11 5 9 150.480 54.7664 13 -11 5 9 184.841 58.1787 15 -11 5 8 3966.85 209.735 15 -11 5 8 4253.57 220.559 13 -11 5 7 130.880 60.9456 13 -11 5 7 129.152 49.3065 15 -11 5 6 630.257 102.601 13 -11 5 6 239.419 63.6438 15 -11 5 5 3604.82 212.718 15 -11 5 5 3621.43 222.578 13 -11 5 4 4387.23 236.106 15 -11 5 4 4576.63 252.210 13 -11 5 3 3752.64 217.685 15 -11 5 3 3586.75 223.294 13 -11 5 2 865.028 105.197 15 -11 5 1 1128.90 116.301 15 -11 5 -2 6543.32 287.422 10 -11 5 -3 7101.02 307.548 10 -11 5 -4 1320.61 128.605 10 -11 5 -5 2050.23 158.432 10 -11 5 -6 8118.66 321.157 10 -11 5 -7 248.857 63.4523 10 -11 5 -8 3046.66 159.971 10 -11 4 10 1775.23 121.181 15 -11 4 10 1824.10 125.233 13 -11 4 9 1242.53 109.619 15 -11 4 9 1295.32 117.612 13 -11 4 8 298.365 74.4676 13 -11 4 8 520.385 78.2040 15 -11 4 7 26.7593 52.9970 13 -11 4 7 11.1815 43.7597 15 -11 4 6 66.7565 57.3571 13 -11 4 6 28.2763 42.7055 15 -11 4 5 3679.16 230.456 13 -11 4 5 3618.13 209.710 15 -11 4 4 642.966 108.076 13 -11 4 4 752.193 100.747 15 -11 4 3 19614.7 603.241 13 -11 4 3 19554.6 573.976 15 -11 4 -2 204.713 64.5543 10 -11 4 -3 7368.42 304.566 10 -11 4 -4 2741.56 179.793 10 -11 4 -5 221.823 67.6747 10 -11 4 -6 2140.25 152.206 10 -11 4 -7 10998.4 357.363 10 -11 4 -8 2233.70 130.824 10 -11 3 10 10161.9 329.407 15 -11 3 10 11023.2 343.111 13 -11 3 9 878.113 97.2541 13 -11 3 9 684.216 81.4765 15 -11 3 8 8075.31 312.046 15 -11 3 8 8414.88 331.734 13 -11 3 7 6482.00 300.861 13 -11 3 7 6217.83 273.282 15 -11 3 6-1.75328 63.9925 13 -11 3 6 45.1143 39.7226 15 -11 3 5 7071.58 327.016 13 -11 3 4 9465.17 393.404 13 -11 3 3 134.279 71.1201 13 -11 3 -2-89.0725 55.2414 10 -11 3 -3 16057.0 485.912 10 -11 3 -4 1307.36 118.756 10 -11 3 -5 242.934 64.9099 10 -11 3 -6 339.233 64.4019 10 -11 3 -7 300.987 67.9422 10 -11 2 10 887.877 86.9986 13 -11 2 9 532.984 78.4059 13 -11 2 8 60.5124 57.5043 13 -11 2 7 970.383 121.322 13 -11 2 6 1162.51 130.265 13 -11 2 5 975.059 123.940 13 -11 2 4 2219.06 183.092 13 -11 2 3 17645.5 564.186 13 -11 2 -3 1521.38 127.141 10 -11 2 -4 301.826 70.4982 10 -11 2 -5 4149.81 196.283 10 -11 2 -6 450.252 64.4115 10 -11 1 10 10565.9 325.968 13 -11 1 9 1000.71 100.719 13 -11 1 8 9682.41 351.511 13 -11 1 7 6705.71 295.975 13 -11 1 6 63.4301 70.0646 13 -11 1 5 14442.5 496.131 13 -11 1 4 2282.44 183.995 13 -11 1 3 1237.69 127.124 13 -11 1 1 276.813 71.8579 11 -11 1 0 16137.9 509.018 11 -11 1 -1 6468.31 290.086 11 -11 1 -2 440.474 94.8996 11 -11 1 -3 1285.58 106.077 10 -11 1 -3 1424.65 132.190 11 -11 1 -4 1672.54 118.414 10 -11 1 -5 1375.92 102.709 10 -11 1 -5 1540.32 125.500 11 -11 0 9 2663.71 151.404 13 -11 0 8-38.7982 49.1442 13 -11 0 7 882.310 104.956 13 -11 0 6 2602.80 183.334 13 -11 0 5 1953.19 160.257 13 -11 0 4 63.1363 61.7811 13 -11 0 3 9330.61 364.853 13 -11 0 3 8558.19 323.862 11 -11 0 2 1163.26 121.473 11 -11 0 1 96.2050 62.5185 11 -11 0 0 121.412 60.2842 11 -11 0 -1-59.9595 55.8364 11 -11 0 -2 3780.39 201.281 11 -11 0 -3 3414.63 191.225 11 -11 0 -4-29.6301 32.7225 10 -11 0 -4-50.9810 54.8872 11 -11 -1 8 4199.61 195.916 13 -11 -1 7 1578.62 128.551 13 -11 -1 6 2268.47 159.727 13 -11 -1 5 1767.82 143.483 13 -11 -1 5 1618.51 118.637 11 -11 -1 4 25.7125 55.8602 13 -11 -1 4 107.407 60.0005 11 -11 -1 3-56.2896 58.6361 13 -11 -1 3 129.996 64.3875 11 -11 -1 2 12786.9 403.681 11 -11 -1 1 584.912 89.5798 11 -11 -1 0 6060.95 254.336 11 -11 -1 -1 1143.90 104.164 11 -11 -1 -2 266.875 68.9074 11 -11 -1 -3 1951.12 128.793 11 -11 -2 7 484.137 65.6060 13 -11 -2 6 89.4823 48.2802 13 -11 -2 6 59.7197 38.4456 11 -11 -2 5 2129.31 148.106 13 -11 -2 5 2299.94 131.385 11 -11 -2 4 195.958 55.8694 13 -11 -2 4 227.664 55.3923 11 -11 -2 3 2069.41 130.976 11 -11 -2 2 43.8681 46.6198 11 -11 -2 1 407.680 67.8706 11 -11 -2 0 3027.47 159.292 11 -11 -2 -1 3103.21 155.848 11 -12 10 1 18176.0 447.757 15 -12 10 0 239.957 41.6376 15 -12 9 4 1162.90 82.5070 15 -12 9 3 4053.66 167.919 15 -12 9 2 129.423 38.8076 15 -12 9 1 509.615 62.6546 15 -12 9 0 950.007 80.3655 15 -12 9 -1 7210.60 236.942 15 -12 8 5 1490.71 96.5444 15 -12 8 4 1507.61 100.561 15 -12 8 3 4481.76 186.314 15 -12 8 2 170.662 42.8607 15 -12 8 1 1510.19 103.861 15 -12 8 0 522.264 63.8187 15 -12 7 6 397.357 50.6794 15 -12 7 5 9483.51 293.125 15 -12 7 4 7334.03 254.554 15 -12 7 3 4253.85 183.860 15 -12 7 2 138.926 50.7496 15 -12 6 6 4849.60 189.562 15 -12 6 5 868.947 79.8478 15 -12 6 4 9159.77 293.589 15 -12 4 6 185.364 51.5565 13 -12 3 6 10.2633 35.4969 13 0 0 0 0.00 0.00 0 TITL Ph2SiLut2_aP_abs_gaus in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 10.213430 14.073351 16.261619 100.7756 93.4285 109.0919 ZERR 2.00 0.000187 0.000289 0.000329 0.0017 0.0016 0.0018 LATT 1 SFAC C H N Si UNIT 104.00 104.00 8.00 4.00 SIZE 0.22 0.62 0.76 TREF HKLF 4 END ; _shelx_hkl_checksum 10040 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.588 _oxdiff_exptl_absorpt_empirical_full_min 0.728 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.32641(3) 0.25403(2) 0.88240(2) 0.01945(9) Uani 1 1 d . . . . . Si2 Si 0.78634(4) 0.23957(3) 0.49105(2) 0.02040(9) Uani 1 1 d . . . . . N4 N 0.53268(12) 0.23280(9) 0.31213(7) 0.0244(2) Uani 1 1 d . . . . . N3 N 0.71956(12) 0.42753(8) 0.65075(7) 0.0242(2) Uani 1 1 d . . . . . N2 N 0.25018(12) 0.45955(8) 0.82074(7) 0.0235(2) Uani 1 1 d . . . . . N1 N 0.09195(12) 0.20900(9) 1.04201(7) 0.0257(2) Uani 1 1 d . . . . . C9 C 0.22434(13) 0.42165(9) 0.89053(8) 0.0213(3) Uani 1 1 d . . . . . C21 C 0.31381(14) 0.22198(9) 0.76421(8) 0.0220(3) Uani 1 1 d . . . . . C41 C 0.77479(13) 0.18199(10) 0.58713(8) 0.0212(3) Uani 1 1 d . . . . . C8 C 0.33641(14) 0.39015(10) 0.92952(8) 0.0224(3) Uani 1 1 d . . . . . H8A H 0.330103 0.396836 0.990725 0.027 Uiso 1 1 calc R U . . . H8B H 0.428714 0.438376 0.923094 0.027 Uiso 1 1 calc R U . . . C28 C 0.68970(15) 0.40057(10) 0.56623(9) 0.0251(3) Uani 1 1 d . . . . . C15 C 0.48565(13) 0.23317(10) 0.92787(8) 0.0216(3) Uani 1 1 d . . . . . C35 C 0.60650(14) 0.17373(10) 0.32930(8) 0.0239(3) Uani 1 1 d . . . . . C2 C 0.14430(13) 0.14569(10) 0.99273(9) 0.0241(3) Uani 1 1 d . . . . . C26 C 0.41633(15) 0.19375(10) 0.72291(9) 0.0260(3) Uani 1 1 d . . . . . H26 H 0.498949 0.196863 0.755118 0.031 Uiso 1 1 calc R U . . . C47 C 0.94332(14) 0.22900(10) 0.44094(8) 0.0226(3) Uani 1 1 d . . . . . C13 C 0.15027(14) 0.48485(10) 0.78236(9) 0.0250(3) Uani 1 1 d . . . . . C32 C 0.61783(14) 0.43942(10) 0.69631(9) 0.0245(3) Uani 1 1 d . . . . . C20 C 0.49251(15) 0.13379(11) 0.91123(9) 0.0265(3) Uani 1 1 d . . . . . H20 H 0.413288 0.077823 0.881530 0.032 Uiso 1 1 calc R U . . . C22 C 0.19353(15) 0.21619(11) 0.71438(9) 0.0273(3) Uani 1 1 d . . . . . H22 H 0.122248 0.234666 0.740863 0.033 Uiso 1 1 calc R U . . . C16 C 0.60378(14) 0.31300(10) 0.97235(9) 0.0258(3) Uani 1 1 d . . . . . H16 H 0.601957 0.381190 0.985539 0.031 Uiso 1 1 calc R U . . . C1 C 0.15941(14) 0.15926(10) 0.90427(9) 0.0260(3) Uani 1 1 d . . . . . H1A H 0.081085 0.179861 0.884788 0.031 Uiso 1 1 calc R U . . . H1B H 0.146831 0.090953 0.868500 0.031 Uiso 1 1 calc R U . . . C12 C 0.02357(14) 0.47585(10) 0.81293(9) 0.0268(3) Uani 1 1 d . . . . . H12 H -0.044611 0.495110 0.784589 0.032 Uiso 1 1 calc R U . . . C10 C 0.09971(15) 0.40988(10) 0.92487(9) 0.0264(3) Uani 1 1 d . . . . . H10 H 0.084283 0.382955 0.974231 0.032 Uiso 1 1 calc R U . . . C39 C 0.51413(14) 0.24322(10) 0.23206(9) 0.0257(3) Uani 1 1 d . . . . . C29 C 0.56058(16) 0.38889(11) 0.52439(9) 0.0302(3) Uani 1 1 d . . . . . H29 H 0.543025 0.371033 0.464479 0.036 Uiso 1 1 calc R U . . . C52 C 0.95716(15) 0.13189(10) 0.41699(9) 0.0262(3) Uani 1 1 d . . . . . H52 H 0.884164 0.072221 0.423214 0.031 Uiso 1 1 calc R U . . . C42 C 0.71474(14) 0.07542(10) 0.57943(9) 0.0260(3) Uani 1 1 d . . . . . H42 H 0.681491 0.032029 0.524810 0.031 Uiso 1 1 calc R U . . . C27 C 0.80289(15) 0.38001(10) 0.51825(9) 0.0267(3) Uani 1 1 d . . . . . H27A H 0.894641 0.420142 0.552427 0.032 Uiso 1 1 calc R U . . . H27B H 0.801246 0.405001 0.465327 0.032 Uiso 1 1 calc R U . . . C34 C 0.61936(14) 0.15986(11) 0.41841(9) 0.0262(3) Uani 1 1 d . . . . . H34A H 0.605667 0.086356 0.415897 0.031 Uiso 1 1 calc R U . . . H34B H 0.541116 0.174111 0.445039 0.031 Uiso 1 1 calc R U . . . C46 C 0.82393(15) 0.24256(11) 0.66841(9) 0.0287(3) Uani 1 1 d . . . . . H46 H 0.867934 0.314944 0.675792 0.034 Uiso 1 1 calc R U . . . C11 C -0.00143(15) 0.43834(11) 0.88540(9) 0.0296(3) Uani 1 1 d . . . . . H11 H -0.086822 0.432117 0.907909 0.036 Uiso 1 1 calc R U . . . C36 C 0.66639(15) 0.12508(11) 0.26745(9) 0.0289(3) Uani 1 1 d . . . . . H36 H 0.719747 0.084883 0.281310 0.035 Uiso 1 1 calc R U . . . C18 C 0.72920(15) 0.19580(12) 0.97941(9) 0.0292(3) Uani 1 1 d . . . . . H18 H 0.812090 0.183537 0.995701 0.035 Uiso 1 1 calc R U . . . C48 C 1.05199(15) 0.31459(11) 0.42957(9) 0.0267(3) Uani 1 1 d . . . . . H48 H 1.044817 0.381104 0.444447 0.032 Uiso 1 1 calc R U . . . C6 C 0.06831(14) 0.19396(11) 1.11974(9) 0.0291(3) Uani 1 1 d . . . . . C19 C 0.61182(16) 0.11475(11) 0.93693(9) 0.0291(3) Uani 1 1 d . . . . . H19 H 0.613162 0.046386 0.925474 0.035 Uiso 1 1 calc R U . . . C51 C 1.07530(16) 0.12151(11) 0.38445(9) 0.0294(3) Uani 1 1 d . . . . . H51 H 1.082585 0.055138 0.368520 0.035 Uiso 1 1 calc R U . . . C49 C 1.17089(15) 0.30414(12) 0.39675(9) 0.0301(3) Uani 1 1 d . . . . . H49 H 1.243587 0.363253 0.389290 0.036 Uiso 1 1 calc R U . . . C17 C 0.72449(15) 0.29470(11) 0.99785(9) 0.0291(3) Uani 1 1 d . . . . . H17 H 0.803795 0.350263 1.027972 0.035 Uiso 1 1 calc R U . . . C31 C 0.48626(15) 0.42834(11) 0.65917(9) 0.0284(3) Uani 1 1 d . . . . . H31 H 0.416733 0.437401 0.692976 0.034 Uiso 1 1 calc R U . . . C43 C 0.70255(15) 0.03155(11) 0.64950(10) 0.0298(3) Uani 1 1 d . . . . . H43 H 0.662743 -0.041077 0.642606 0.036 Uiso 1 1 calc R U . . . C50 C 1.18311(15) 0.20801(12) 0.37509(9) 0.0302(3) Uani 1 1 d . . . . . H50 H 1.264940 0.201055 0.353859 0.036 Uiso 1 1 calc R U . . . C30 C 0.45823(16) 0.40391(11) 0.57217(10) 0.0321(3) Uani 1 1 d . . . . . H30 H 0.369599 0.397446 0.545315 0.039 Uiso 1 1 calc R U . . . C38 C 0.56794(16) 0.19504(11) 0.16694(9) 0.0291(3) Uani 1 1 d . . . . . H38 H 0.550988 0.202190 0.110733 0.035 Uiso 1 1 calc R U . . . C23 C 0.17632(17) 0.18398(12) 0.62704(10) 0.0328(3) Uani 1 1 d . . . . . H23 H 0.094229 0.180922 0.594306 0.039 Uiso 1 1 calc R U . . . C3 C 0.17868(15) 0.06831(11) 1.02111(10) 0.0305(3) Uani 1 1 d . . . . . H3 H 0.220365 0.027234 0.986352 0.037 Uiso 1 1 calc R U . . . C25 C 0.39911(17) 0.16117(11) 0.63538(9) 0.0319(3) Uani 1 1 d . . . . . H25 H 0.469695 0.142279 0.608391 0.038 Uiso 1 1 calc R U . . . C33 C 0.65242(15) 0.46303(12) 0.79070(9) 0.0312(3) Uani 1 1 d . . . . . H33A H 0.570854 0.468945 0.817130 0.047 Uiso 1 1 calc R U . . . H33B H 0.730963 0.528138 0.809028 0.047 Uiso 1 1 calc R U . . . H33C H 0.677976 0.407412 0.807480 0.047 Uiso 1 1 calc R U . . . C37 C 0.64645(16) 0.13662(11) 0.18531(9) 0.0308(3) Uani 1 1 d . . . . . H37 H 0.686520 0.104558 0.142050 0.037 Uiso 1 1 calc R U . . . C5 C 0.09391(16) 0.11463(12) 1.15023(9) 0.0333(3) Uani 1 1 d . . . . . H5 H 0.072184 0.103719 1.204464 0.040 Uiso 1 1 calc R U . . . C44 C 0.74862(16) 0.09403(13) 0.72943(10) 0.0335(3) Uani 1 1 d . . . . . H44 H 0.738114 0.064599 0.777727 0.040 Uiso 1 1 calc R U . . . C24 C 0.27959(18) 0.15630(11) 0.58780(9) 0.0338(3) Uani 1 1 d . . . . . H24 H 0.267982 0.133969 0.528117 0.041 Uiso 1 1 calc R U . . . C45 C 0.80975(18) 0.19900(12) 0.73883(9) 0.0363(3) Uani 1 1 d . . . . . H45 H 0.842377 0.241850 0.793690 0.044 Uiso 1 1 calc R U . . . C40 C 0.43468(16) 0.31199(12) 0.21517(10) 0.0346(3) Uani 1 1 d . . . . . H40A H 0.381334 0.322784 0.261999 0.052 Uiso 1 1 calc R U . . . H40B H 0.370444 0.279552 0.162613 0.052 Uiso 1 1 calc R U . . . H40C H 0.500452 0.378498 0.209877 0.052 Uiso 1 1 calc R U . . . C4 C 0.15141(16) 0.05219(12) 1.10020(10) 0.0344(3) Uani 1 1 d . . . . . H4 H 0.171918 -0.001308 1.120161 0.041 Uiso 1 1 calc R U . . . C14 C 0.17861(17) 0.52196(14) 0.70182(11) 0.0394(4) Uani 1 1 d . . . . . H14A H 0.173283 0.463778 0.656321 0.059 Uiso 1 1 calc R U . . . H14B H 0.272132 0.574298 0.710055 0.059 Uiso 1 1 calc R U . . . H14C H 0.108825 0.551933 0.686743 0.059 Uiso 1 1 calc R U . . . C7 C 0.01413(17) 0.26795(13) 1.17376(11) 0.0401(4) Uani 1 1 d . . . . . H7A H -0.040423 0.233813 1.214199 0.060 Uiso 1 1 calc R U . . . H7B H -0.045455 0.290288 1.137913 0.060 Uiso 1 1 calc R U . . . H7C H 0.092917 0.328023 1.204441 0.060 Uiso 1 1 calc R U . . . 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 0.01920(17) 0.02046(16) 0.01928(17) 0.00337(12) 0.00123(12) 0.00836(13) Si2 0.02202(18) 0.02079(17) 0.01873(17) 0.00363(13) 0.00404(13) 0.00797(13) N4 0.0216(5) 0.0261(5) 0.0230(6) 0.0036(4) 0.0027(4) 0.0060(4) N3 0.0250(6) 0.0217(5) 0.0276(6) 0.0062(4) 0.0055(4) 0.0097(4) N2 0.0225(5) 0.0235(5) 0.0250(6) 0.0050(4) 0.0025(4) 0.0088(4) N1 0.0208(5) 0.0264(5) 0.0285(6) 0.0068(5) 0.0013(4) 0.0065(4) C9 0.0238(6) 0.0170(5) 0.0218(6) -0.0007(5) 0.0010(5) 0.0083(5) C21 0.0243(6) 0.0199(6) 0.0213(6) 0.0027(5) 0.0020(5) 0.0081(5) C41 0.0195(6) 0.0238(6) 0.0225(6) 0.0049(5) 0.0052(5) 0.0099(5) C8 0.0246(6) 0.0222(6) 0.0205(6) 0.0017(5) 0.0013(5) 0.0101(5) C28 0.0304(7) 0.0193(6) 0.0287(7) 0.0075(5) 0.0068(5) 0.0111(5) C15 0.0228(6) 0.0252(6) 0.0187(6) 0.0055(5) 0.0025(5) 0.0102(5) C35 0.0211(6) 0.0234(6) 0.0226(6) 0.0032(5) 0.0016(5) 0.0029(5) C2 0.0184(6) 0.0250(6) 0.0264(7) 0.0064(5) 0.0006(5) 0.0043(5) C26 0.0276(7) 0.0268(6) 0.0256(7) 0.0057(5) 0.0033(5) 0.0120(5) C47 0.0246(6) 0.0268(6) 0.0165(6) 0.0030(5) 0.0025(5) 0.0098(5) C13 0.0245(7) 0.0218(6) 0.0279(7) 0.0045(5) 0.0003(5) 0.0078(5) C32 0.0262(7) 0.0212(6) 0.0275(7) 0.0056(5) 0.0058(5) 0.0097(5) C20 0.0257(7) 0.0268(6) 0.0263(7) 0.0021(5) -0.0002(5) 0.0107(5) C22 0.0264(7) 0.0287(7) 0.0269(7) 0.0028(5) 0.0005(5) 0.0120(5) C16 0.0278(7) 0.0257(6) 0.0240(7) 0.0069(5) 0.0012(5) 0.0090(5) C1 0.0217(6) 0.0268(6) 0.0271(7) 0.0064(5) 0.0006(5) 0.0052(5) C12 0.0242(7) 0.0243(6) 0.0320(7) 0.0023(5) -0.0008(5) 0.0113(5) C10 0.0287(7) 0.0276(7) 0.0241(7) 0.0038(5) 0.0064(5) 0.0117(5) C39 0.0224(6) 0.0242(6) 0.0269(7) 0.0054(5) 0.0017(5) 0.0038(5) C29 0.0376(8) 0.0294(7) 0.0264(7) 0.0052(5) 0.0007(6) 0.0165(6) C52 0.0268(7) 0.0260(6) 0.0247(7) 0.0040(5) 0.0044(5) 0.0081(5) C42 0.0271(7) 0.0245(6) 0.0256(7) 0.0034(5) 0.0014(5) 0.0092(5) C27 0.0321(7) 0.0227(6) 0.0279(7) 0.0066(5) 0.0091(6) 0.0114(5) C34 0.0247(7) 0.0302(7) 0.0224(7) 0.0065(5) 0.0027(5) 0.0072(5) C46 0.0337(7) 0.0255(6) 0.0266(7) 0.0022(5) -0.0018(6) 0.0130(6) C11 0.0249(7) 0.0316(7) 0.0337(8) 0.0026(6) 0.0075(6) 0.0134(6) C36 0.0331(7) 0.0286(7) 0.0265(7) 0.0043(5) 0.0041(6) 0.0136(6) C18 0.0243(7) 0.0454(8) 0.0242(7) 0.0112(6) 0.0029(5) 0.0184(6) C48 0.0288(7) 0.0265(7) 0.0241(7) 0.0043(5) 0.0041(5) 0.0092(5) C6 0.0217(6) 0.0331(7) 0.0267(7) 0.0029(6) 0.0001(5) 0.0041(5) C19 0.0338(8) 0.0327(7) 0.0269(7) 0.0051(6) 0.0047(6) 0.0200(6) C51 0.0344(8) 0.0328(7) 0.0239(7) 0.0027(5) 0.0046(6) 0.0173(6) C49 0.0257(7) 0.0351(7) 0.0262(7) 0.0071(6) 0.0049(5) 0.0059(6) C17 0.0234(7) 0.0352(7) 0.0261(7) 0.0088(6) -0.0009(5) 0.0060(6) C31 0.0264(7) 0.0272(7) 0.0343(8) 0.0051(6) 0.0057(6) 0.0132(5) C43 0.0250(7) 0.0285(7) 0.0386(8) 0.0138(6) 0.0034(6) 0.0094(5) C50 0.0269(7) 0.0446(8) 0.0225(7) 0.0070(6) 0.0069(5) 0.0164(6) C30 0.0290(7) 0.0321(7) 0.0368(8) 0.0047(6) -0.0025(6) 0.0154(6) C38 0.0345(7) 0.0292(7) 0.0217(7) 0.0059(5) 0.0039(6) 0.0080(6) C23 0.0364(8) 0.0336(7) 0.0272(7) 0.0020(6) -0.0069(6) 0.0148(6) C3 0.0288(7) 0.0311(7) 0.0341(8) 0.0092(6) 0.0033(6) 0.0127(6) C25 0.0410(8) 0.0312(7) 0.0278(7) 0.0037(6) 0.0096(6) 0.0188(6) C33 0.0292(7) 0.0386(8) 0.0272(7) 0.0063(6) 0.0058(6) 0.0138(6) C37 0.0373(8) 0.0290(7) 0.0247(7) 0.0008(5) 0.0077(6) 0.0116(6) C5 0.0321(8) 0.0387(8) 0.0253(7) 0.0107(6) -0.0006(6) 0.0056(6) C44 0.0373(8) 0.0450(8) 0.0286(7) 0.0180(6) 0.0074(6) 0.0219(7) C24 0.0497(9) 0.0309(7) 0.0209(7) 0.0005(5) 0.0007(6) 0.0174(7) C45 0.0511(9) 0.0400(8) 0.0210(7) 0.0021(6) -0.0019(6) 0.0237(7) C40 0.0322(8) 0.0373(8) 0.0364(8) 0.0097(6) 0.0008(6) 0.0146(6) C4 0.0347(8) 0.0352(8) 0.0360(8) 0.0160(6) -0.0012(6) 0.0120(6) C14 0.0310(8) 0.0526(10) 0.0414(9) 0.0251(8) 0.0040(7) 0.0154(7) C7 0.0349(8) 0.0454(9) 0.0363(9) 0.0002(7) 0.0064(7) 0.0134(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -6 9 0.1066 0 6 -9 0.0972 -1 -6 -5 0.3127 4 -6 -5 0.2932 7 -2 -1 0.3382 4 3 4 0.2980 -1 6 6 0.2983 -5 -2 -3 0.3793 -5 8 0 0.2976 -1 9 -1 0.2624 -1 -8 1 0.2929 0 8 -6 0.1740 -3 8 -5 0.2162 -4 -5 5 0.3226 -7 2 0 0.4098 -4 7 -7 0.2784 -1 -6 9 0.1396 -4 1 9 0.2525 -1 0 10 0.2401 0 0 -10 0.2279 3 -1 -9 0.2200 -3 1 -9 0.2889 0 -4 -8 0.2875 -5 4 6 0.2944 0 -7 -5 0.3118 -6 7 -1 0.3365 -5 2 -6 0.3491 4 -2 7 0.2782 0 2 9 0.2703 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 C21 Si1 C8 114.69(6) . . ? C21 Si1 C15 108.54(6) . . ? C21 Si1 C1 103.24(6) . . ? C15 Si1 C8 108.72(6) . . ? C15 Si1 C1 111.97(6) . . ? C1 Si1 C8 109.65(6) . . ? C41 Si2 C27 111.98(6) . . ? C41 Si2 C34 105.16(6) . . ? C47 Si2 C41 109.13(6) . . ? C47 Si2 C27 108.61(6) . . ? C47 Si2 C34 111.02(6) . . ? C34 Si2 C27 110.93(6) . . ? C35 N4 C39 118.50(12) . . ? C28 N3 C32 118.13(12) . . ? C13 N2 C9 118.22(11) . . ? C6 N1 C2 118.36(12) . . ? N2 C9 C8 116.57(11) . . ? N2 C9 C10 122.50(12) . . ? C10 C9 C8 120.92(12) . . ? C26 C21 Si1 121.89(10) . . ? C26 C21 C22 117.65(12) . . ? C22 C21 Si1 120.20(10) . . ? C42 C41 Si2 120.74(10) . . ? C46 C41 Si2 122.08(10) . . ? C46 C41 C42 117.18(12) . . ? Si1 C8 H8A 108.7 . . ? Si1 C8 H8B 108.7 . . ? C9 C8 Si1 114.26(9) . . ? C9 C8 H8A 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N3 C28 C29 122.62(12) . . ? N3 C28 C27 116.24(12) . . ? C29 C28 C27 121.11(13) . . ? C20 C15 Si1 119.06(10) . . ? C16 C15 Si1 123.50(10) . . ? C16 C15 C20 117.24(12) . . ? N4 C35 C34 117.02(12) . . ? N4 C35 C36 122.19(13) . . ? C36 C35 C34 120.77(12) . . ? N1 C2 C1 117.10(12) . . ? N1 C2 C3 122.04(13) . . ? C3 C2 C1 120.82(13) . . ? C21 C26 H26 119.5 . . ? C25 C26 C21 121.06(13) . . ? C25 C26 H26 119.5 . . ? C52 C47 Si2 119.44(10) . . ? C48 C47 Si2 122.89(10) . . ? C48 C47 C52 117.60(12) . . ? N2 C13 C12 122.70(13) . . ? N2 C13 C14 117.28(12) . . ? C12 C13 C14 120.01(13) . . ? N3 C32 C31 122.54(13) . . ? N3 C32 C33 116.55(12) . . ? C31 C32 C33 120.90(12) . . ? C15 C20 H20 119.1 . . ? C19 C20 C15 121.83(13) . . ? C19 C20 H20 119.1 . . ? C21 C22 H22 119.3 . . ? C23 C22 C21 121.38(13) . . ? C23 C22 H22 119.3 . . ? C15 C16 H16 119.3 . . ? C17 C16 C15 121.31(13) . . ? C17 C16 H16 119.3 . . ? Si1 C1 H1A 107.5 . . ? Si1 C1 H1B 107.5 . . ? C2 C1 Si1 119.11(9) . . ? C2 C1 H1A 107.5 . . ? C2 C1 H1B 107.5 . . ? H1A C1 H1B 107.0 . . ? C13 C12 H12 120.6 . . ? C11 C12 C13 118.76(13) . . ? C11 C12 H12 120.6 . . ? C9 C10 H10 120.7 . . ? C11 C10 C9 118.57(13) . . ? C11 C10 H10 120.7 . . ? N4 C39 C38 122.40(13) . . ? N4 C39 C40 117.34(12) . . ? C38 C39 C40 120.25(13) . . ? C28 C29 H29 120.8 . . ? C30 C29 C28 118.46(13) . . ? C30 C29 H29 120.8 . . ? C47 C52 H52 119.4 . . ? C51 C52 C47 121.23(13) . . ? C51 C52 H52 119.4 . . ? C41 C42 H42 119.2 . . ? C43 C42 C41 121.70(13) . . ? C43 C42 H42 119.2 . . ? Si2 C27 H27A 108.7 . . ? Si2 C27 H27B 108.7 . . ? C28 C27 Si2 114.10(9) . . ? C28 C27 H27A 108.7 . . ? C28 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? Si2 C34 H34A 107.7 . . ? Si2 C34 H34B 107.7 . . ? C35 C34 Si2 118.61(9) . . ? C35 C34 H34A 107.7 . . ? C35 C34 H34B 107.7 . . ? H34A C34 H34B 107.1 . . ? C41 C46 H46 119.4 . . ? C45 C46 C41 121.24(13) . . ? C45 C46 H46 119.4 . . ? C12 C11 C10 119.23(13) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C35 C36 H36 120.7 . . ? C37 C36 C35 118.61(13) . . ? C37 C36 H36 120.7 . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C17 C18 C19 119.47(13) . . ? C47 C48 H48 119.4 . . ? C49 C48 C47 121.17(13) . . ? C49 C48 H48 119.4 . . ? N1 C6 C5 122.30(14) . . ? N1 C6 C7 116.85(14) . . ? C5 C6 C7 120.84(14) . . ? C20 C19 C18 119.87(13) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C52 C51 H51 119.9 . . ? C52 C51 C50 120.11(13) . . ? C50 C51 H51 119.9 . . ? C48 C49 H49 119.9 . . ? C50 C49 C48 120.12(13) . . ? C50 C49 H49 119.9 . . ? C16 C17 H17 119.9 . . ? C18 C17 C16 120.25(13) . . ? C18 C17 H17 119.9 . . ? C32 C31 H31 120.6 . . ? C30 C31 C32 118.79(13) . . ? C30 C31 H31 120.6 . . ? C42 C43 H43 120.1 . . ? C44 C43 C42 119.71(13) . . ? C44 C43 H43 120.1 . . ? C51 C50 H50 120.1 . . ? C49 C50 C51 119.75(13) . . ? C49 C50 H50 120.1 . . ? C29 C30 H30 120.3 . . ? C31 C30 C29 119.40(13) . . ? C31 C30 H30 120.3 . . ? C39 C38 H38 120.6 . . ? C37 C38 C39 118.83(13) . . ? C37 C38 H38 120.6 . . ? C22 C23 H23 120.1 . . ? C24 C23 C22 119.73(14) . . ? C24 C23 H23 120.1 . . ? C2 C3 H3 120.5 . . ? C4 C3 C2 119.08(14) . . ? C4 C3 H3 120.5 . . ? C26 C25 H25 120.0 . . ? C24 C25 C26 120.08(13) . . ? C24 C25 H25 120.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C37 H37 120.3 . . ? C38 C37 C36 119.43(13) . . ? C38 C37 H37 120.3 . . ? C6 C5 H5 120.6 . . ? C4 C5 C6 118.82(14) . . ? C4 C5 H5 120.6 . . ? C43 C44 H44 120.1 . . ? C45 C44 C43 119.83(13) . . ? C45 C44 H44 120.1 . . ? C23 C24 H24 119.9 . . ? C25 C24 C23 120.10(13) . . ? C25 C24 H24 119.9 . . ? C46 C45 H45 119.8 . . ? C44 C45 C46 120.31(14) . . ? C44 C45 H45 119.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C3 C4 C5 119.27(14) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 C21 1.8767(13) . ? Si1 C8 1.8925(13) . ? Si1 C15 1.8782(13) . ? Si1 C1 1.8912(14) . ? Si2 C41 1.8828(13) . ? Si2 C47 1.8771(13) . ? Si2 C27 1.8910(13) . ? Si2 C34 1.8906(14) . ? N4 C35 1.3451(18) . ? N4 C39 1.3464(18) . ? N3 C28 1.3435(19) . ? N3 C32 1.3475(17) . ? N2 C9 1.3462(17) . ? N2 C13 1.3424(18) . ? N1 C2 1.3483(18) . ? N1 C6 1.3430(19) . ? C9 C8 1.5030(18) . ? C9 C10 1.3933(19) . ? C21 C26 1.4007(19) . ? C21 C22 1.4011(19) . ? C41 C42 1.3999(19) . ? C41 C46 1.3947(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C28 C29 1.392(2) . ? C28 C27 1.5071(18) . ? C15 C20 1.3996(19) . ? C15 C16 1.3951(19) . ? C35 C34 1.5016(18) . ? C35 C36 1.3944(19) . ? C2 C1 1.4964(19) . ? C2 C3 1.393(2) . ? C26 H26 0.9500 . ? C26 C25 1.393(2) . ? C47 C52 1.4048(19) . ? C47 C48 1.3965(19) . ? C13 C12 1.390(2) . ? C13 C14 1.508(2) . ? C32 C31 1.388(2) . ? C32 C33 1.503(2) . ? C20 H20 0.9500 . ? C20 C19 1.388(2) . ? C22 H22 0.9500 . ? C22 C23 1.390(2) . ? C16 H16 0.9500 . ? C16 C17 1.395(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C12 H12 0.9500 . ? C12 C11 1.383(2) . ? C10 H10 0.9500 . ? C10 C11 1.388(2) . ? C39 C38 1.388(2) . ? C39 C40 1.502(2) . ? C29 H29 0.9500 . ? C29 C30 1.386(2) . ? C52 H52 0.9500 . ? C52 C51 1.386(2) . ? C42 H42 0.9500 . ? C42 C43 1.387(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C46 H46 0.9500 . ? C46 C45 1.390(2) . ? C11 H11 0.9500 . ? C36 H36 0.9500 . ? C36 C37 1.386(2) . ? C18 H18 0.9500 . ? C18 C19 1.388(2) . ? C18 C17 1.385(2) . ? C48 H48 0.9500 . ? C48 C49 1.395(2) . ? C6 C5 1.394(2) . ? C6 C7 1.502(2) . ? C19 H19 0.9500 . ? C51 H51 0.9500 . ? C51 C50 1.389(2) . ? C49 H49 0.9500 . ? C49 C50 1.381(2) . ? C17 H17 0.9500 . ? C31 H31 0.9500 . ? C31 C30 1.381(2) . ? C43 H43 0.9500 . ? C43 C44 1.383(2) . ? C50 H50 0.9500 . ? C30 H30 0.9500 . ? C38 H38 0.9500 . ? C38 C37 1.379(2) . ? C23 H23 0.9500 . ? C23 C24 1.388(2) . ? C3 H3 0.9500 . ? C3 C4 1.376(2) . ? C25 H25 0.9500 . ? C25 C24 1.381(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C37 H37 0.9500 . ? C5 H5 0.9500 . ? C5 C4 1.381(2) . ? C44 H44 0.9500 . ? C44 C45 1.377(2) . ? C24 H24 0.9500 . ? C45 H45 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C4 H4 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si1 C21 C26 C25 174.08(11) . . . . ? Si1 C21 C22 C23 -174.37(11) . . . . ? Si1 C15 C20 C19 174.48(11) . . . . ? Si1 C15 C16 C17 -173.74(10) . . . . ? Si2 C41 C42 C43 -178.65(10) . . . . ? Si2 C41 C46 C45 177.56(11) . . . . ? Si2 C47 C52 C51 -176.12(11) . . . . ? Si2 C47 C48 C49 176.06(11) . . . . ? N4 C35 C34 Si2 -100.43(13) . . . . ? N4 C35 C36 C37 -1.3(2) . . . . ? N4 C39 C38 C37 -1.8(2) . . . . ? N3 C28 C29 C30 -1.2(2) . . . . ? N3 C28 C27 Si2 94.72(13) . . . . ? N3 C32 C31 C30 0.2(2) . . . . ? N2 C9 C8 Si1 -85.93(13) . . . . ? N2 C9 C10 C11 0.0(2) . . . . ? N2 C13 C12 C11 -0.7(2) . . . . ? N1 C2 C1 Si1 88.30(13) . . . . ? N1 C2 C3 C4 3.6(2) . . . . ? N1 C6 C5 C4 3.0(2) . . . . ? C9 N2 C13 C12 1.64(19) . . . . ? C9 N2 C13 C14 -176.93(12) . . . . ? C9 C10 C11 C12 0.9(2) . . . . ? C21 Si1 C8 C9 51.03(11) . . . . ? C21 Si1 C15 C20 -63.26(12) . . . . ? C21 Si1 C15 C16 111.50(11) . . . . ? C21 Si1 C1 C2 167.36(10) . . . . ? C21 C26 C25 C24 0.0(2) . . . . ? C21 C22 C23 C24 0.3(2) . . . . ? C41 Si2 C47 C52 55.98(12) . . . . ? C41 Si2 C47 C48 -120.94(12) . . . . ? C41 Si2 C27 C28 -54.16(12) . . . . ? C41 Si2 C34 C35 -169.37(10) . . . . ? C41 C42 C43 C44 1.0(2) . . . . ? C41 C46 C45 C44 1.2(2) . . . . ? C8 Si1 C21 C26 118.42(11) . . . . ? C8 Si1 C21 C22 -67.70(12) . . . . ? C8 Si1 C15 C20 171.36(10) . . . . ? C8 Si1 C15 C16 -13.88(13) . . . . ? C8 Si1 C1 C2 -69.98(12) . . . . ? C8 C9 C10 C11 -178.76(12) . . . . ? C28 N3 C32 C31 -2.25(19) . . . . ? C28 N3 C32 C33 176.27(12) . . . . ? C28 C29 C30 C31 -0.9(2) . . . . ? C15 Si1 C21 C26 -3.37(13) . . . . ? C15 Si1 C21 C22 170.51(10) . . . . ? C15 Si1 C8 C9 172.72(9) . . . . ? C15 Si1 C1 C2 50.79(12) . . . . ? C15 C20 C19 C18 -0.9(2) . . . . ? C15 C16 C17 C18 -0.1(2) . . . . ? C35 N4 C39 C38 0.22(19) . . . . ? C35 N4 C39 C40 -178.34(12) . . . . ? C35 C36 C37 C38 -0.3(2) . . . . ? C2 N1 C6 C5 -1.0(2) . . . . ? C2 N1 C6 C7 178.18(12) . . . . ? C2 C3 C4 C5 -1.6(2) . . . . ? C26 C21 C22 C23 -0.2(2) . . . . ? C26 C25 C24 C23 0.1(2) . . . . ? C47 Si2 C41 C42 -82.22(11) . . . . ? C47 Si2 C41 C46 98.28(12) . . . . ? C47 Si2 C27 C28 -174.74(10) . . . . ? C47 Si2 C34 C35 -51.48(12) . . . . ? C47 C52 C51 C50 0.1(2) . . . . ? C47 C48 C49 C50 -0.2(2) . . . . ? C13 N2 C9 C8 177.53(11) . . . . ? C13 N2 C9 C10 -1.32(19) . . . . ? C13 C12 C11 C10 -0.6(2) . . . . ? C32 N3 C28 C29 2.77(19) . . . . ? C32 N3 C28 C27 -175.34(11) . . . . ? C32 C31 C30 C29 1.4(2) . . . . ? C20 C15 C16 C17 1.1(2) . . . . ? C22 C21 C26 C25 0.1(2) . . . . ? C22 C23 C24 C25 -0.3(2) . . . . ? C16 C15 C20 C19 -0.6(2) . . . . ? C1 Si1 C21 C26 -122.34(11) . . . . ? C1 Si1 C21 C22 51.54(12) . . . . ? C1 Si1 C8 C9 -64.56(11) . . . . ? C1 Si1 C15 C20 50.06(12) . . . . ? C1 Si1 C15 C16 -135.18(11) . . . . ? C1 C2 C3 C4 -174.11(13) . . . . ? C10 C9 C8 Si1 92.94(13) . . . . ? C39 N4 C35 C34 -177.21(11) . . . . ? C39 N4 C35 C36 1.36(19) . . . . ? C39 C38 C37 C36 1.8(2) . . . . ? C29 C28 C27 Si2 -83.42(14) . . . . ? C52 C47 C48 C49 -0.9(2) . . . . ? C52 C51 C50 C49 -1.3(2) . . . . ? C42 C41 C46 C45 -2.0(2) . . . . ? C42 C43 C44 C45 -1.8(2) . . . . ? C27 Si2 C41 C42 157.51(11) . . . . ? C27 Si2 C41 C46 -22.00(13) . . . . ? C27 Si2 C47 C52 178.31(11) . . . . ? C27 Si2 C47 C48 1.39(13) . . . . ? C27 Si2 C34 C35 69.38(12) . . . . ? C27 C28 C29 C30 176.81(12) . . . . ? C34 Si2 C41 C42 36.95(12) . . . . ? C34 Si2 C41 C46 -142.56(11) . . . . ? C34 Si2 C47 C52 -59.47(12) . . . . ? C34 Si2 C47 C48 123.61(12) . . . . ? C34 Si2 C27 C28 62.98(12) . . . . ? C34 C35 C36 C37 177.20(13) . . . . ? C46 C41 C42 C43 0.9(2) . . . . ? C36 C35 C34 Si2 80.97(15) . . . . ? C48 C47 C52 C51 1.0(2) . . . . ? C48 C49 C50 C51 1.3(2) . . . . ? C6 N1 C2 C1 175.52(11) . . . . ? C6 N1 C2 C3 -2.27(19) . . . . ? C6 C5 C4 C3 -1.5(2) . . . . ? C19 C18 C17 C16 -1.4(2) . . . . ? C17 C18 C19 C20 1.8(2) . . . . ? C43 C44 C45 C46 0.7(2) . . . . ? C3 C2 C1 Si1 -93.88(14) . . . . ? C33 C32 C31 C30 -178.27(13) . . . . ? C40 C39 C38 C37 176.73(14) . . . . ? C14 C13 C12 C11 177.86(14) . . . . ? C7 C6 C5 C4 -176.23(14) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0778 -6.1406 8.8915 -0.9966 -0.0793 0.0209 0.3866 5.9723 -8.8735 0.9927 0.0792 -0.0914 -1.0296 -5.6165 -5.3983 -0.0773 0.9585 0.2744 4.3554 -6.4298 -4.8586 -0.0635 0.8255 -0.5608 6.6078 -2.3130 -0.5441 -0.0001 0.0494 -0.9988 4.2147 2.9634 3.7250 0.0574 -0.6860 -0.7253 -0.8287 6.4183 5.6902 0.0793 -0.9968 0.0034 -4.7320 -2.3090 -3.2481 -0.0512 0.6056 0.7941 -4.5837 8.2586 -0.3348 0.5173 -0.6080 0.6023 -0.5945 8.7623 -0.6289 0.6499 -0.7595 -0.0280 -1.1067 -7.8956 0.6720 -0.6245 0.7284 0.2818 -0.2167 8.1537 -5.8115 0.9419 -0.3325 -0.0467 -2.7962 8.4470 -5.3475 0.8828 -0.3130 0.3503 -3.7203 -5.1526 4.6821 -0.7348 0.2574 0.6276 -6.5660 1.8536 0.3845 -0.0216 0.0043 0.9998 -4.1283 6.7082 -6.5045 0.8065 -0.0221 0.5909 -1.1944 -5.6062 8.7357 -0.9738 -0.0780 0.2135 -3.5225 0.7229 9.2152 -0.6007 -0.6355 0.4850 -1.2567 -0.0298 10.3487 -0.6814 -0.7196 0.1339 0.4586 0.2813 -10.4141 0.6877 0.7259 -0.0120 3.4163 -0.6862 -9.3056 0.6069 0.6421 -0.4684 -2.7821 1.2368 -9.0626 0.6064 0.6386 0.4737 -0.4569 -3.7673 -7.9947 0.2294 0.9576 0.1743 -5.0415 4.4378 6.0596 -0.1673 -0.7049 0.6893 0.4549 -6.8980 -4.7097 -0.1827 0.9816 0.0560 -5.7826 6.8230 -0.8306 0.4232 -0.3986 0.8136 -5.0654 2.3344 -6.1640 0.4562 0.3939 0.7980 4.4784 -2.2868 7.2193 -0.5311 -0.4576 -0.7132 0.3577 2.1495 9.2389 -0.4249 -0.8939 -0.1433