#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:42:08 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242528 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132576.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_4132576 loop_ _publ_author_name 'Liu, Liu Leo' 'Zhou, Jiliang' 'Andrews, Ryan' 'Stephan, Douglas W.' _publ_section_title ; A Room-Temperature-Stable Phosphanorcaradiene. ; _journal_issue 24 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7466 _journal_page_last 7470 _journal_paper_doi 10.1021/jacs.8b04930 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C F3 O3 S, C18 H37 N2 Si, 0.5(C6 H5 Cl)' _chemical_formula_sum 'C22 H39.5 Cl0.5 F3 N2 O3 S Si' _chemical_formula_weight 514.93 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2018-04-16 _audit_creation_method ; Olex2 1.2 (compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486) ; _cell_angle_alpha 90 _cell_angle_beta 98.018(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.2238(6) _cell_length_b 17.2610(12) _cell_length_c 17.5861(11) _cell_measurement_reflns_used 9899 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.68 _cell_measurement_theta_min 2.36 _cell_volume 2772.5(3) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_unetI/netI 0.0526 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 49941 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.877 _diffrn_reflns_theta_min 2.230 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0822 before and 0.0614 after correction. The Ratio of minimum to maximum transmission is 0.8749. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.234 _exptl_crystal_description needle _exptl_crystal_F_000 1100 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.340 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 336 _refine_ls_number_reflns 6613 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0468 _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^)+(0.0550P)^2^+1.1145P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1311 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4143 _reflns_number_total 6613 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04930_si_002.cif _cod_data_source_block 7 _cod_original_formula_sum 'C22 H39.50 Cl0.50 F3 N2 O3 S Si' _cod_database_code 4132576 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_max 0.992 _shelx_estimated_absorpt_t_min 0.951 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: Cl1S(0.5) C1S(0.5) C2S(0.5) H2S(0.5) C3S(0.5) H3S(0.5) C4S(0.5) H4S(0.5) C5S(0.5) H5S(0.5) C6S(0.5) H6S(0.5) 3.a Ternary CH refined with riding coordinates: C00C(H00C), C00F(H00F), C00G(H00G), C00J(H00J) 3.b Aromatic/amide H refined with riding coordinates: C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S) 3.c Idealised Me refined as rotating group: C00I(H00A,H00B,H00D), C00K(H00E,H00H,H00I), C00M(H00K,H00L,H00M), C00N(H00N, H00O,H00P), C00O(H00Q,H00R,H00S), C00P(H00T,H00U,H00V), C00R(H00W,H00X,H00Y), C00S(H00Z,H,HA), C00T(H00,HB,HC), C00U(H0AA,HD,HE), C00V(H1AA,HF,HG) ; _shelx_res_file ; mono_a.res created by SHELXL-2014/7 TITL mono_a.res in P2(1)/c REM Old TITL mono in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.199, Rweak 0.014, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C21 N2 O4 F3 Si S CELL 0.71073 9.2238 17.261 17.5861 90 98.018 90 ZERR 4 0.0006 0.0012 0.0011 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O F Si S Cl UNIT 88 158 8 12 12 4 4 2 L.S. 10 PLAN 40 SIZE 0.2 0.04 0.03 TEMP -123 BOND $H LIST 6 fmap 2 acta OMIT 0 1 1 OMIT -1 1 1 REM REM REM WGHT 0.055000 1.114500 FVAR 0.47394 S001 7 0.788481 0.715984 0.483678 11.00000 0.05319 0.04425 = 0.03909 0.00595 0.01351 -0.00384 SI02 6 0.874116 0.241256 0.751796 11.00000 0.03104 0.02605 = 0.03590 0.01092 0.00679 0.00473 N004 3 0.754179 0.443136 0.655455 11.00000 0.03095 0.02380 = 0.02346 0.00738 0.00681 0.00463 N005 3 0.565796 0.397963 0.825239 11.00000 0.02947 0.03060 = 0.02247 -0.00051 0.00672 -0.00110 F006 5 0.648482 0.671146 0.351542 11.00000 0.09281 0.08742 = 0.05444 -0.02539 0.01222 -0.01932 O007 4 0.915697 0.728012 0.446518 11.00000 0.04157 0.06941 = 0.07231 0.00368 0.02385 0.00314 C008 1 0.725504 0.399751 0.712661 11.00000 0.02406 0.02330 = 0.01950 0.00111 0.00160 -0.00083 C009 1 0.756598 0.330834 0.752094 11.00000 0.02717 0.02750 = 0.02086 0.00559 0.00362 -0.00123 C00A 1 0.656886 0.381503 0.776343 11.00000 0.02520 0.02598 = 0.02004 0.00177 0.00122 -0.00275 F00B 5 0.641186 0.791970 0.370193 11.00000 0.11772 0.06592 = 0.10573 0.02764 -0.01716 0.02339 C00C 1 0.864151 0.414619 0.607213 11.00000 0.03430 0.02778 = 0.02271 0.00472 0.00954 0.00226 AFIX 13 H00C 2 0.898191 0.362549 0.627278 11.00000 -1.20000 AFIX 0 O00D 4 0.758052 0.777704 0.533784 11.00000 0.07817 0.08675 = 0.06513 -0.03652 0.03557 -0.02753 F00E 5 0.510727 0.713737 0.429567 11.00000 0.04478 0.14718 = 0.11725 -0.04011 0.02289 -0.01144 C00F 1 0.481963 0.470818 0.820490 11.00000 0.03507 0.03540 = 0.03217 -0.00586 0.00871 0.00405 AFIX 13 H00F 2 0.514062 0.502110 0.777981 11.00000 -1.20000 AFIX 0 C00G 1 0.683190 0.519191 0.636571 11.00000 0.04279 0.02568 = 0.03391 0.01212 0.00681 0.00879 AFIX 13 H00G 2 0.722202 0.538734 0.589878 11.00000 -1.20000 AFIX 0 O00H 4 0.771024 0.639763 0.510533 11.00000 0.13560 0.06300 = 0.07848 0.04084 0.01547 -0.01548 C00I 1 0.996623 0.467369 0.614522 11.00000 0.03666 0.04165 = 0.03731 0.00213 0.00973 -0.00473 AFIX 137 H00A 2 0.967547 0.518400 0.593197 11.00000 -1.50000 H00B 2 1.070942 0.445019 0.586280 11.00000 -1.50000 H00D 2 1.037079 0.472815 0.668817 11.00000 -1.50000 AFIX 0 C00J 1 0.543629 0.340438 0.885928 11.00000 0.04154 0.03982 = 0.02699 0.00269 0.01570 -0.00465 AFIX 13 H00J 2 0.465265 0.361377 0.914175 11.00000 -1.20000 AFIX 0 C00K 1 0.796080 0.404215 0.524514 11.00000 0.04268 0.05121 = 0.02413 -0.00138 0.00517 -0.00298 AFIX 137 H00E 2 0.708792 0.371489 0.522418 11.00000 -1.50000 H00H 2 0.866925 0.379499 0.495594 11.00000 -1.50000 H00I 2 0.768409 0.454916 0.501936 11.00000 -1.50000 AFIX 0 C00M 1 0.519466 0.510882 0.614703 11.00000 0.04377 0.04896 = 0.03364 0.00891 -0.00047 0.01597 AFIX 137 H00K 2 0.499179 0.475982 0.570546 11.00000 -1.50000 H00L 2 0.476381 0.561801 0.601214 11.00000 -1.50000 H00M 2 0.476740 0.489477 0.658177 11.00000 -1.50000 AFIX 0 C00N 1 0.728560 0.577781 0.699975 11.00000 0.04607 0.02394 = 0.06253 0.00024 0.00654 0.00456 AFIX 137 H00N 2 0.694169 0.560481 0.747440 11.00000 -1.50000 H00O 2 0.685257 0.628291 0.684902 11.00000 -1.50000 H00P 2 0.835501 0.582340 0.708458 11.00000 -1.50000 AFIX 0 C00O 1 0.489013 0.264004 0.850808 11.00000 0.04093 0.04054 = 0.04442 0.00335 0.01295 -0.00902 AFIX 137 H00Q 2 0.399351 0.272668 0.814846 11.00000 -1.50000 H00R 2 0.468274 0.228606 0.891507 11.00000 -1.50000 H00S 2 0.564039 0.241229 0.823322 11.00000 -1.50000 AFIX 0 C00P 1 1.065715 0.274829 0.759209 11.00000 0.03296 0.04770 = 0.04976 0.00948 0.00060 0.00612 AFIX 137 H00T 2 1.127878 0.232207 0.746068 11.00000 -1.50000 H00U 2 1.099100 0.292051 0.811841 11.00000 -1.50000 H00V 2 1.071821 0.318042 0.723651 11.00000 -1.50000 AFIX 0 C00Q 1 0.640935 0.724171 0.405170 11.00000 0.04681 0.05217 = 0.06082 -0.00606 0.01435 -0.00018 C00R 1 0.515880 0.518075 0.893659 11.00000 0.07397 0.04795 = 0.04307 -0.01653 0.00822 0.00300 AFIX 137 H00W 2 0.480197 0.490519 0.936108 11.00000 -1.50000 H00X 2 0.467397 0.568593 0.886546 11.00000 -1.50000 H00Y 2 0.621932 0.525606 0.905536 11.00000 -1.50000 AFIX 0 C00S 1 0.816575 0.193084 0.658933 11.00000 0.05590 0.03500 = 0.06758 -0.01311 0.00480 0.00065 AFIX 137 H00Z 2 0.837127 0.227064 0.617088 11.00000 -1.50000 H 2 0.711368 0.182160 0.653411 11.00000 -1.50000 HA 2 0.870642 0.144421 0.656934 11.00000 -1.50000 AFIX 0 C00T 1 0.681929 0.333478 0.943519 11.00000 0.06677 0.06446 = 0.02602 0.01216 -0.00059 -0.01145 AFIX 137 H00 2 0.762516 0.315191 0.917300 11.00000 -1.50000 HB 2 0.665564 0.296513 0.983756 11.00000 -1.50000 HC 2 0.706938 0.384241 0.966661 11.00000 -1.50000 AFIX 0 C00U 1 0.318714 0.456328 0.799704 11.00000 0.03222 0.06135 = 0.07704 -0.01441 0.00581 0.00966 AFIX 137 H0AA 2 0.300646 0.428512 0.750718 11.00000 -1.50000 HD 2 0.266695 0.505977 0.795022 11.00000 -1.50000 HE 2 0.283537 0.425153 0.839971 11.00000 -1.50000 AFIX 0 C00V 1 0.852575 0.176238 0.833089 11.00000 0.07731 0.05780 = 0.08523 0.04615 0.03885 0.03402 AFIX 137 H1AA 2 0.751348 0.157569 0.828053 11.00000 -1.50000 HF 2 0.875809 0.204672 0.881488 11.00000 -1.50000 HG 2 0.919156 0.132028 0.832791 11.00000 -1.50000 AFIX 0 PART -1 CL1S 8 1.041384 0.990852 0.644536 10.50000 0.04745 0.06953 = 0.05055 0.01974 0.00238 0.00747 C1S 1 1.008662 0.998763 0.545103 10.50000 0.02744 0.04241 = 0.04393 0.00909 0.00165 0.00768 C2S 1 0.953748 0.944466 0.499576 10.50000 0.04293 0.00899 = 0.08422 -0.00905 0.00042 -0.00756 AFIX 43 H2S 2 0.929229 0.898482 0.524595 10.50000 -1.20000 AFIX 0 C3S 1 0.925837 0.942279 0.423429 10.50000 0.04422 0.04845 = 0.06758 -0.01393 -0.00148 -0.00020 AFIX 43 H3S 2 0.881583 0.899130 0.395772 10.50000 -1.20000 AFIX 0 C4S 1 0.966801 1.007954 0.388662 10.50000 0.05183 0.06873 = 0.05152 -0.00009 -0.00246 0.01015 AFIX 43 H4S 2 0.954767 1.010613 0.334188 10.50000 -1.20000 AFIX 0 C5S 1 1.026007 1.071224 0.431689 10.50000 0.04688 0.04250 = 0.04797 0.01015 0.01095 0.00582 AFIX 43 H5S 2 1.048907 1.116317 0.404766 10.50000 -1.20000 AFIX 0 C6S 1 1.052763 1.072410 0.509037 10.50000 0.02598 0.00846 = 0.06243 -0.00142 -0.00195 -0.00520 AFIX 43 H6S 2 1.095118 1.115375 0.537745 10.50000 -1.20000 AFIX 0 HKLF 4 REM mono_a.res in P2(1)/c REM R1 = 0.0468 for 4143 Fo > 4sig(Fo) and 0.0948 for all 6613 data REM 336 parameters refined using 0 restraints END WGHT 0.0550 1.1199 REM Highest difference peak 0.340, deepest hole -0.313, 1-sigma level 0.051 Q1 1 0.6202 0.7996 0.4229 11.00000 0.05 0.34 Q2 1 0.5588 0.7794 0.4219 11.00000 0.05 0.30 Q3 1 0.6760 0.6622 0.5010 11.00000 0.05 0.30 Q4 1 1.0380 0.2436 0.8026 11.00000 0.05 0.27 Q5 1 0.9772 0.2424 0.7691 11.00000 0.05 0.25 Q6 1 0.7604 0.7327 0.5426 11.00000 0.05 0.24 Q7 1 0.7677 0.6143 0.5031 11.00000 0.05 0.24 Q8 1 0.6710 0.4152 0.7450 11.00000 0.05 0.23 Q9 1 0.8047 0.1825 0.7056 11.00000 0.05 0.23 Q10 1 0.7822 0.6725 0.4808 11.00000 0.05 0.23 Q11 1 1.1544 0.2389 0.7945 11.00000 0.05 0.23 Q12 1 0.9829 0.2776 0.7374 11.00000 0.05 0.23 Q13 1 0.6885 0.7154 0.4649 11.00000 0.05 0.22 Q14 1 0.8180 0.2950 0.7794 11.00000 0.05 0.22 Q15 1 0.7418 0.3403 0.7840 11.00000 0.05 0.22 Q16 1 0.6760 0.6337 0.3891 11.00000 0.05 0.21 Q17 1 0.7572 0.7925 0.3699 11.00000 0.05 0.20 Q18 1 0.9032 0.6796 0.4672 11.00000 0.05 0.20 Q19 1 0.5733 0.6727 0.4970 11.00000 0.05 0.20 Q20 1 0.6018 0.5199 0.6281 11.00000 0.05 0.20 Q21 1 0.7593 0.3527 0.7260 11.00000 0.05 0.20 Q22 1 0.6985 0.1605 0.7078 11.00000 0.05 0.19 Q23 1 0.6599 0.6354 0.5221 11.00000 0.05 0.18 Q24 1 0.7441 0.2600 0.7853 11.00000 0.05 0.18 Q25 1 0.4625 0.4590 0.5867 11.00000 0.05 0.18 Q26 1 0.6946 0.7821 0.4989 11.00000 0.05 0.18 Q27 1 0.7174 0.1045 0.8139 11.00000 0.05 0.17 Q28 1 0.7672 0.1582 0.6848 11.00000 0.05 0.17 Q29 1 0.9078 0.1847 0.6980 11.00000 0.05 0.17 Q30 1 0.9539 0.1943 0.8016 11.00000 0.05 0.17 Q31 1 0.8960 0.1160 0.8145 11.00000 0.05 0.17 Q32 1 0.5790 0.6785 0.4631 11.00000 0.05 0.17 Q33 1 1.0854 0.2794 0.7070 11.00000 0.05 0.17 Q34 1 0.5432 0.2847 0.9859 11.00000 0.05 0.17 Q35 1 0.5008 0.4816 0.7913 11.00000 0.05 0.17 Q36 1 0.2612 0.5160 0.7760 11.00000 0.05 0.17 Q37 1 0.5281 0.4436 0.8364 11.00000 0.05 0.17 Q38 1 1.1220 0.2650 0.7060 11.00000 0.05 0.17 Q39 1 0.7878 0.2799 0.6989 11.00000 0.05 0.16 Q40 1 0.8470 0.2171 0.8000 11.00000 0.05 0.16 ; _shelx_res_checksum 58903 _shelx_hkl_file ; 1 0 0 0.10 0.70 1 0 0 0.30 0.90 1 0 0 1.10 0.80 1 0 0 0.70 0.50 -1 0 0 0.80 1.10 -1 0 0 0.80 0.80 1 0 0 4.40 1.60 2 0 0 62.19 3.70 2 0 0 69.49 3.70 -2 0 0 67.99 5.20 2 0 0 59.99 6.70 2 0 0 70.19 5.30 2 0 0 71.19 5.10 2 0 0 64.69 7.00 -2 0 0 56.09 6.90 3 0 0 250.07 10.30 3 0 0 250.17 11.30 -3 0 0 234.38 11.20 3 0 0 252.07 12.60 3 0 0 240.68 10.20 3 0 0 259.87 11.40 3 0 0 260.87 13.20 4 0 0 1795.42 71.79 4 0 0 1907.21 72.59 4 0 0 1877.61 73.99 4 0 0 1970.40 72.69 4 0 0 1863.51 71.79 5 0 0 616.74 25.50 5 0 0 653.03 26.90 5 0 0 634.64 28.90 5 0 0 663.63 25.60 5 0 0 684.33 26.80 6 0 0 153.18 7.90 6 0 0 151.58 9.90 6 0 0 152.88 10.40 6 0 0 156.08 8.00 6 0 0 155.18 13.20 7 0 0 313.47 16.50 7 0 0 358.76 20.50 7 0 0 348.97 20.00 7 0 0 320.37 14.40 8 0 0 103.99 11.40 8 0 0 130.59 8.20 9 0 0 33.20 9.50 10 0 0 10.30 9.70 11 0 0 37.50 12.30 12 0 0 12.20 12.80 12 0 0 21.40 17.30 -2 -1 0 734.53 28.50 2 -1 0 717.63 29.30 2 -1 0 721.53 28.60 2 -1 0 744.53 28.60 -2 -1 0 761.92 29.10 2 -1 0 749.62 29.90 -2 -1 0 770.42 29.40 -2 -1 0 713.43 29.90 2 -1 0 746.83 28.90 -2 -1 0 745.63 28.50 2 1 0 724.13 28.70 -2 1 0 750.62 29.90 2 1 0 767.42 29.40 -2 1 0 723.83 28.40 2 1 0 733.63 28.60 2 1 0 782.42 29.20 2 1 0 734.93 29.80 -3 -1 0 1.20 2.60 3 -1 0 1.80 2.80 3 -1 0 -0.70 2.00 3 -1 0 2.50 4.40 -3 -1 0 4.20 3.10 3 -1 0 -1.70 2.80 -3 -1 0 0.20 4.70 3 -1 0 -2.00 3.70 3 -1 0 1.10 2.00 3 1 0 -0.80 4.40 3 1 0 1.00 3.40 3 1 0 3.30 2.30 3 1 0 1.00 2.70 3 1 0 2.80 2.20 4 -1 0 352.76 14.90 -4 -1 0 356.16 15.30 -4 -1 0 356.76 17.60 4 -1 0 346.97 14.10 4 -1 0 332.07 14.00 4 -1 0 354.26 15.50 4 -1 0 343.57 15.20 4 -1 0 335.57 17.10 4 1 0 359.56 15.30 4 1 0 356.16 15.70 4 1 0 343.97 14.20 4 1 0 332.07 14.10 4 1 0 336.97 17.10 5 -1 0 384.36 15.90 5 -1 0 406.16 16.80 5 -1 0 393.96 16.00 -5 -1 0 376.16 17.00 5 -1 0 380.06 19.50 5 -1 0 396.76 17.50 5 -1 0 392.66 17.20 5 1 0 396.26 17.80 5 1 0 363.06 16.00 5 1 0 394.96 19.80 5 1 0 409.56 16.10 5 1 0 398.76 17.30 6 -1 0 1157.98 44.10 6 -1 0 1137.99 45.30 6 -1 0 1086.59 44.80 6 -1 0 1139.99 45.10 6 -1 0 1125.19 47.40 6 -1 0 1141.59 44.00 6 1 0 1089.69 44.10 6 1 0 1180.08 44.20 6 1 0 1131.49 45.10 6 1 0 1132.89 47.70 6 1 0 1180.48 45.60 7 -1 0 23.70 5.40 7 -1 0 16.00 7.10 7 -1 0 34.70 4.30 7 1 0 26.30 7.70 7 1 0 20.20 4.90 7 1 0 33.00 4.30 8 -1 0 212.78 11.00 8 -1 0 213.18 17.80 8 -1 0 183.68 12.90 8 1 0 221.38 11.00 8 1 0 226.58 18.30 9 -1 0 35.90 9.60 9 1 0 49.90 10.10 10 -1 0 92.49 12.60 10 1 0 87.49 12.50 11 -1 0 7.20 11.00 11 -1 0 22.90 15.80 11 1 0 10.80 11.40 12 -1 0 4.10 12.40 12 -1 0 14.00 17.70 12 1 0 -0.70 12.90 1 -2 0 3.50 1.70 1 -2 0 5.60 1.90 -1 -2 0 -4.10 1.40 1 -2 0 0.30 1.50 -1 -2 0 4.30 1.90 1 -2 0 -3.40 2.40 -1 2 0 3.70 1.40 -1 2 0 0.50 1.90 1 2 0 1.10 1.60 -1 2 0 0.10 2.50 1 2 0 4.40 1.90 -1 2 0 -3.10 1.30 1 2 0 -3.10 2.70 2 -2 0 2859.41 108.69 2 -2 0 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12.80 -7 -10 0 16.00 7.00 7 10 0 16.10 6.60 -7 10 0 24.50 6.60 8 -10 0 35.80 9.60 8 -10 0 36.70 14.90 -8 -10 0 52.89 13.40 8 10 0 59.19 7.80 9 -10 0 11.80 15.90 9 -10 0 11.80 9.90 -9 -10 0 31.60 13.60 9 10 0 25.10 7.90 -10 -10 0 4.60 13.60 10 -10 0 -10.20 16.00 10 -10 0 -2.00 11.00 10 10 0 -0.20 10.80 0 -11 0 -3.40 6.00 0 -11 0 -1.90 5.20 0 11 0 2.20 4.20 1 -11 0 328.67 16.50 -1 -11 0 321.77 15.50 1 -11 0 308.07 21.10 1 -11 0 313.67 15.50 -1 -11 0 286.87 19.70 -1 11 0 317.67 14.90 1 11 0 309.07 14.90 2 -11 0 20.80 5.60 -2 -11 0 17.60 7.80 2 -11 0 17.40 8.60 2 -11 0 19.40 6.10 -2 -11 0 18.60 5.50 2 11 0 22.90 4.90 -2 11 0 20.60 5.10 3 -11 0 1.80 8.40 -3 -11 0 0.60 7.30 3 -11 0 4.80 5.90 -3 -11 0 6.80 5.30 3 -11 0 2.50 5.30 3 11 0 2.30 4.90 -3 11 0 -4.80 4.50 -4 -11 0 178.78 10.90 4 -11 0 166.88 11.50 4 -11 0 161.68 20.20 -4 -11 0 175.48 14.60 4 -11 0 157.98 13.60 4 11 0 171.48 11.00 -4 11 0 167.08 10.60 -4 11 0 159.58 10.00 5 -11 0 15.70 10.10 5 -11 0 20.80 7.10 -5 -11 0 17.40 9.20 -5 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30.30 8.70 3 -12 0 25.80 10.30 -3 -12 0 33.10 6.40 3 -12 0 23.80 6.50 3 -12 0 30.20 7.10 -3 12 0 31.80 5.60 3 12 0 40.20 6.30 4 -12 0 27.90 11.30 4 -12 0 22.00 7.00 4 -12 0 25.40 7.30 -4 -12 0 27.50 6.20 -4 12 0 22.80 6.20 4 12 0 38.20 6.60 -4 12 0 26.50 5.60 5 -12 0 107.39 15.30 5 -12 0 133.09 12.30 -5 -12 0 170.68 16.30 -5 -12 0 133.79 9.90 5 -12 0 119.39 14.30 -5 12 0 143.49 9.30 5 12 0 138.09 11.20 -5 12 0 141.39 10.80 6 -12 0 -5.60 12.20 -6 -12 0 4.20 5.20 6 -12 0 -5.40 8.00 -6 -12 0 -6.90 7.50 6 -12 0 -9.40 7.30 -6 -12 0 -4.70 10.10 -6 12 0 -3.90 4.30 6 12 0 -0.70 6.50 -6 12 0 8.10 6.30 -7 -12 0 167.68 16.10 -7 -12 0 162.98 10.20 7 -12 0 106.19 12.10 7 -12 0 162.68 13.70 -7 -12 0 159.98 18.60 7 -12 0 122.09 18.30 7 12 0 162.98 13.10 -7 12 0 161.88 12.00 8 -12 0 46.20 9.00 -8 -12 0 62.79 14.00 8 -12 0 32.40 16.20 8 -12 0 26.50 10.00 8 12 0 49.00 8.40 -9 -12 0 7.20 13.50 9 -12 0 -17.10 9.30 9 -12 0 -17.30 15.90 9 12 0 2.00 8.20 10 -12 0 -9.30 16.90 10 -12 0 6.10 12.30 -10 -12 0 16.70 15.00 0 -13 0 -3.40 8.20 0 -13 0 -1.80 6.40 0 13 0 -1.00 5.10 0 13 0 0.50 2.60 -1 -13 0 808.42 32.80 1 -13 0 761.32 32.80 -1 -13 0 687.93 37.40 1 -13 0 790.12 38.80 1 -13 0 774.82 33.90 -1 13 0 778.22 32.20 1 13 0 808.82 32.40 2 -13 0 309.57 16.40 -2 -13 0 311.17 23.50 2 -13 0 324.97 24.80 2 -13 0 285.07 17.60 -2 -13 0 297.27 15.80 2 13 0 286.07 15.40 -2 13 0 299.47 15.10 3 -13 0 7.10 7.20 -3 -13 0 -1.20 9.00 3 -13 0 9.50 10.90 3 -13 0 7.60 6.50 -3 -13 0 10.10 6.20 -3 13 0 6.30 5.50 3 13 0 5.00 5.70 -4 -13 0 15.70 6.30 4 -13 0 2.60 7.40 4 -13 0 7.40 11.30 -4 -13 0 13.20 10.20 4 -13 0 18.80 7.20 -4 13 0 14.80 6.40 4 13 0 13.50 6.30 -4 13 0 24.60 5.70 5 -13 0 13.20 7.80 5 -13 0 1.00 12.50 -5 -13 0 13.30 6.00 5 -13 0 22.30 8.10 -5 -13 0 10.50 10.50 -5 13 0 15.10 5.30 -5 13 0 20.40 6.70 5 13 0 22.50 7.00 6 -13 0 1.40 8.10 6 -13 0 6.50 11.80 -6 -13 0 6.10 5.60 -6 -13 0 8.90 10.90 6 -13 0 3.00 8.10 -6 -13 0 7.70 8.40 -6 13 0 7.70 6.60 6 13 0 3.30 7.20 -6 13 0 5.70 4.80 -7 -13 0 14.30 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13.60 -5 14 0 82.19 8.90 -5 14 0 61.89 6.90 5 14 0 91.99 9.30 -6 -14 0 7.10 9.30 6 -14 0 27.30 8.80 -6 -14 0 30.90 12.20 6 -14 0 7.30 8.80 6 -14 0 6.70 12.50 -6 -14 0 17.00 6.20 -6 14 0 13.90 5.30 -6 14 0 19.10 7.10 6 14 0 18.30 7.90 -7 -14 0 126.99 10.20 -7 -14 0 139.39 17.00 7 -14 0 109.79 11.50 -7 -14 0 104.79 12.40 7 -14 0 117.19 18.90 7 -14 0 86.79 12.10 -7 14 0 128.79 11.90 7 14 0 154.28 13.80 -8 -14 0 27.00 14.20 8 -14 0 6.00 9.40 8 -14 0 -9.90 10.30 8 -14 0 7.30 16.50 8 14 0 11.90 8.40 9 -14 0 -10.30 11.60 9 -14 0 8.10 17.00 -9 -14 0 40.90 15.40 9 14 0 28.30 9.30 0 -15 0 2.30 9.70 0 -15 0 0.00 7.60 0 15 0 8.60 6.20 -1 -15 0 597.64 34.80 1 -15 0 621.54 35.00 1 -15 0 550.94 26.70 -1 -15 0 589.74 26.60 1 15 0 547.15 25.80 -1 15 0 564.74 25.80 2 -15 0 22.50 8.60 2 -15 0 7.20 12.10 -2 -15 0 -4.40 9.10 2 -15 0 7.90 7.10 -2 -15 0 15.10 7.50 -2 15 0 17.50 6.20 2 15 0 7.40 6.60 -3 -15 0 41.70 8.00 3 -15 0 30.60 8.00 3 -15 0 31.60 14.10 -3 -15 0 17.40 11.70 3 -15 0 33.10 8.50 -3 15 0 45.30 6.90 3 15 0 39.00 7.40 4 -15 0 19.00 8.60 -4 -15 0 8.60 10.20 -4 -15 0 19.40 7.00 4 -15 0 16.00 8.00 4 -15 0 24.10 14.20 -4 15 0 20.10 6.20 4 15 0 20.70 7.60 5 -15 0 1.00 8.50 5 -15 0 -1.10 8.20 -5 -15 0 -10.10 10.70 -5 -15 0 5.30 6.60 5 -15 0 -7.70 13.60 5 15 0 2.00 7.20 -5 15 0 1.90 5.50 -5 15 0 -3.30 7.00 -6 -15 0 -13.20 9.40 6 -15 0 0.80 8.80 -6 -15 0 5.10 6.20 6 -15 0 -12.60 14.00 -6 -15 0 -2.20 11.10 6 -15 0 -13.20 8.50 -6 15 0 3.40 5.40 -6 15 0 9.30 7.30 6 15 0 -5.50 7.30 7 -15 0 -5.00 9.80 -7 -15 0 7.20 7.30 7 -15 0 -3.30 15.90 -7 -15 0 6.30 10.10 -7 -15 0 11.50 12.90 7 -15 0 9.90 9.50 7 15 0 17.30 8.70 -7 15 0 28.40 10.50 -8 -15 0 56.19 15.70 8 -15 0 13.50 17.80 8 -15 0 33.40 10.80 8 -15 0 0.30 11.00 8 15 0 56.69 9.70 9 -15 0 -25.10 18.10 9 -15 0 -28.10 11.40 -9 -15 0 17.30 15.30 9 15 0 2.50 9.20 0 -16 0 74.49 14.70 0 -16 0 60.89 9.80 0 16 0 72.69 8.40 1 -16 0 111.69 15.90 -1 -16 0 89.99 10.40 1 -16 0 86.49 10.50 -1 -16 0 97.09 15.30 -1 16 0 99.89 9.30 1 16 0 122.69 10.10 -2 -16 0 34.50 8.20 2 -16 0 25.70 8.30 2 -16 0 49.30 9.70 -2 -16 0 32.60 12.80 2 -16 0 60.59 14.60 -2 16 0 49.40 7.60 2 16 0 51.49 8.00 3 -16 0 15.30 8.60 -3 -16 0 5.30 11.40 3 -16 0 9.90 7.80 3 -16 0 2.10 13.70 -3 -16 0 14.80 7.70 3 16 0 18.20 7.20 -3 16 0 10.80 6.40 -4 -16 0 52.19 8.60 -4 -16 0 74.69 14.40 4 -16 0 77.79 10.50 4 -16 0 50.19 9.50 4 -16 0 48.80 14.40 4 16 0 87.29 9.60 -4 16 0 62.19 7.80 5 -16 0 22.20 14.10 -5 -16 0 30.80 7.50 5 -16 0 45.30 10.00 -5 -16 0 12.60 12.60 5 -16 0 27.00 9.20 5 16 0 24.50 8.20 -5 16 0 20.10 8.20 -5 16 0 21.80 6.40 -6 -16 0 -15.40 10.00 -6 -16 0 5.80 12.60 6 -16 0 -0.80 9.10 6 -16 0 3.10 9.50 6 -16 0 -3.40 15.60 -6 -16 0 1.30 6.50 -6 16 0 -1.00 7.40 6 16 0 0.60 8.00 -6 16 0 -0.60 5.50 -7 -16 0 -3.30 13.20 7 -16 0 -7.80 9.90 7 -16 0 5.80 9.90 -7 -16 0 4.20 13.50 7 -16 0 -21.80 14.00 7 16 0 -2.70 8.50 8 -16 0 -4.90 16.80 8 -16 0 -16.50 10.90 -8 -16 0 37.00 15.20 8 -16 0 4.50 10.60 8 16 0 18.40 9.10 0 -17 0 -9.90 13.00 0 -17 0 9.00 8.20 0 17 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9.20 7 4 -9 45.50 9.40 7 4 -9 27.40 4.10 6 -4 -9 0.80 2.90 6 -4 -9 5.40 3.20 6 -4 -9 -1.80 4.70 -6 -4 9 10.10 8.10 6 -4 -9 5.00 6.90 6 4 -9 -6.10 7.60 6 4 -9 -2.40 3.30 5 -4 -9 -2.00 3.30 -5 -4 9 3.00 6.80 5 -4 -9 -2.80 3.40 5 -4 -9 1.30 5.80 5 -4 -9 -3.40 3.60 5 4 -9 -2.70 3.30 -5 4 9 -4.10 6.70 5 4 -9 -0.20 6.10 -5 4 9 -5.10 5.70 5 4 -9 4.80 3.90 -4 -4 9 342.27 20.40 -4 -4 9 330.07 17.70 4 -4 -9 339.47 14.60 4 -4 -9 364.86 18.70 4 -4 -9 322.97 14.40 4 4 -9 325.77 14.60 -4 4 9 342.97 16.40 4 4 -9 345.77 18.10 4 4 -9 292.17 15.30 -4 4 9 325.17 17.00 -3 -4 9 -0.30 6.50 3 -4 -9 -0.80 3.80 -3 -4 9 -1.70 2.90 -3 -4 9 -1.50 3.00 -3 -4 9 -2.10 6.30 3 -4 -9 6.80 5.10 3 4 -9 -2.60 2.30 3 4 -9 6.00 5.60 3 4 -9 2.10 3.60 -3 4 9 -1.50 4.40 -3 4 9 1.60 5.50 -3 4 9 -0.60 2.50 -3 4 9 -1.70 1.80 -3 4 9 2.70 5.80 -3 4 9 1.60 4.80 2 -4 -9 179.88 12.10 -2 -4 9 168.68 11.20 -2 -4 9 172.28 9.30 -2 -4 9 164.98 14.20 2 -4 -9 175.18 9.70 -2 -4 9 170.08 9.20 -2 4 9 164.88 10.20 -2 4 9 171.68 10.90 2 4 -9 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9 1.00 14.20 9 -4 9 23.80 9.70 9 -4 9 7.20 10.90 9 4 9 11.30 9.70 9 4 9 -0.80 9.70 10 -4 9 23.90 10.30 10 -4 9 0.50 12.20 10 -4 9 14.10 16.80 10 4 9 11.00 10.20 10 4 9 -8.70 10.50 11 -5 -9 9.20 14.60 11 5 -9 13.40 12.00 10 -5 -9 19.20 13.50 10 -5 -9 51.69 10.50 10 -5 -9 6.90 8.70 -10 -5 9 23.10 10.30 10 5 -9 43.40 11.40 9 -5 -9 -15.70 6.80 9 -5 -9 0.50 11.30 -9 -5 9 2.30 9.20 9 5 -9 0.20 10.00 -8 -5 9 65.49 10.70 8 -5 -9 65.99 12.10 8 -5 -9 54.39 8.00 8 5 -9 73.79 11.80 -7 -5 9 185.38 17.50 7 -5 -9 138.19 12.50 7 -5 -9 180.48 19.30 7 5 -9 171.08 17.10 7 5 -9 145.09 9.00 -6 -5 9 304.47 20.20 6 -5 -9 326.77 21.00 6 -5 -9 260.57 12.60 6 -5 -9 265.77 14.90 6 5 -9 269.07 12.90 6 5 -9 271.87 19.40 -5 -5 9 53.09 9.10 5 -5 -9 95.79 12.50 5 -5 -9 68.79 7.40 5 -5 -9 69.09 6.30 -5 5 9 68.69 8.80 5 5 -9 57.19 9.20 -5 5 9 70.79 7.90 5 5 -9 70.49 8.70 5 5 -9 73.69 6.70 -4 -5 9 28.10 2.60 4 -5 -9 36.30 4.50 -4 -5 9 30.40 4.10 -4 -5 9 42.80 7.10 4 -5 -9 38.80 6.80 4 -5 -9 31.60 3.30 -4 -5 9 26.50 7.50 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5 9 53.29 5.10 0 5 -9 61.09 6.10 0 5 9 63.39 8.00 0 5 9 58.59 6.10 0 5 -9 57.19 6.30 0 5 9 75.59 6.50 1 -5 9 3.30 5.40 -1 -5 -9 3.00 4.80 1 -5 9 5.00 6.30 1 -5 9 5.30 4.90 1 -5 9 5.70 5.10 1 5 9 6.30 4.50 -1 5 -9 2.90 4.00 -1 5 -9 4.00 4.30 1 5 9 6.30 3.10 1 5 9 3.90 5.00 2 -5 9 370.76 16.80 2 -5 9 387.26 20.20 -2 -5 -9 372.56 17.10 -2 -5 -9 351.56 17.50 2 -5 9 379.96 19.80 2 -5 9 366.56 19.40 2 -5 9 368.76 17.30 -2 5 -9 361.46 17.00 2 5 9 383.86 17.50 -2 5 -9 352.56 15.10 2 5 9 395.16 17.50 -2 5 -9 353.96 16.60 -3 -5 -9 121.09 9.20 3 -5 9 131.09 11.60 3 -5 9 113.09 12.40 -3 -5 -9 118.69 8.50 -3 -5 -9 124.89 10.00 3 -5 9 124.99 15.00 3 -5 9 115.69 10.10 3 -5 9 129.99 12.40 -3 5 -9 119.39 7.50 -3 5 -9 111.49 9.40 3 5 9 116.69 10.10 3 5 9 122.29 10.80 -4 -5 -9 355.86 17.10 4 -5 9 360.76 20.60 4 -5 9 341.67 18.60 -4 -5 -9 346.07 15.30 4 -5 9 354.26 17.70 4 -5 9 353.86 23.70 -4 -5 -9 358.66 18.70 4 5 9 358.86 19.30 4 5 9 370.36 17.90 -4 5 -9 339.07 17.00 5 -5 9 71.19 12.10 5 -5 9 67.99 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11.30 -8 -4 -14 14.80 8.10 -8 4 -14 9.10 7.90 8 4 14 13.00 10.60 8 4 14 42.20 11.10 -10 -5 14 64.99 14.50 10 5 -14 26.20 13.40 -9 -5 14 22.00 12.80 9 5 -14 7.70 12.10 -8 -5 14 6.70 11.40 8 5 -14 8.80 11.20 -7 -5 14 8.50 10.90 7 -5 -14 -1.00 8.80 7 5 -14 8.10 10.60 -6 -5 14 4.30 10.60 6 -5 -14 -0.60 7.80 6 -5 -14 11.50 5.80 6 5 -14 11.20 9.70 -6 5 14 13.30 8.90 6 5 -14 9.50 5.30 -5 -5 14 279.47 23.40 -5 -5 14 277.97 19.90 5 -5 -14 284.17 18.80 5 -5 -14 314.47 14.90 5 5 -14 281.17 20.90 -5 5 14 313.77 18.10 5 5 -14 272.87 15.10 -5 5 14 302.67 18.80 4 -5 -14 16.20 5.70 -4 -5 14 16.80 9.90 -4 -5 14 7.40 9.50 4 -5 -14 4.70 6.00 -4 -5 14 11.80 4.00 -4 5 14 8.60 3.20 -4 5 14 6.50 7.40 4 5 -14 8.20 8.20 -4 5 14 6.80 8.40 4 5 -14 14.50 5.60 3 -5 -14 87.99 12.10 -3 -5 14 79.29 6.80 -3 -5 14 40.90 10.20 -3 -5 14 72.69 11.10 3 -5 -14 69.19 7.50 3 5 -14 67.39 9.80 3 5 -14 71.99 7.50 -3 5 14 84.79 9.80 -3 5 14 73.09 6.20 -3 5 14 69.89 9.70 2 -5 -14 508.05 23.90 -2 -5 14 439.86 26.80 -2 -5 14 448.36 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-10.40 11.00 2 4 21 10.00 10.40 -2 4 -21 4.80 8.90 3 -4 21 -10.30 10.30 -3 -4 -21 8.70 9.10 3 -4 21 22.20 11.30 3 -4 21 -1.20 13.40 3 4 21 26.70 11.10 -3 4 -21 1.90 8.90 -5 -5 21 36.30 14.30 -5 -5 21 54.39 15.60 -5 5 21 46.50 13.00 5 5 -21 35.50 12.70 -4 -5 21 3.40 12.30 -4 -5 21 10.50 13.50 4 -5 -21 14.20 7.60 4 5 -21 3.60 10.60 -4 5 21 14.20 11.50 4 5 -21 -4.60 8.00 -3 -5 21 31.10 13.20 3 -5 -21 -3.80 7.10 -3 -5 21 -7.40 11.40 3 5 -21 -9.00 7.50 -3 5 21 6.70 11.20 3 5 -21 -1.90 9.30 2 -5 -21 0.40 7.60 -2 -5 21 14.00 12.90 -2 -5 21 13.20 11.60 2 5 -21 1.80 8.00 -2 5 21 6.00 7.50 -2 5 21 11.00 11.10 2 5 -21 -0.40 8.70 -1 -5 21 4.10 11.30 -1 -5 21 6.70 8.90 -1 -5 21 1.10 12.80 1 -5 -21 14.10 8.20 -1 -5 21 17.80 9.20 -1 5 21 14.40 8.50 1 5 -21 17.10 8.60 -1 5 21 5.10 11.10 1 5 -21 -1.70 8.50 0 -5 21 5.40 9.80 0 -5 21 9.60 12.50 0 -5 21 14.40 9.40 0 -5 21 11.60 10.80 0 -5 -21 12.70 8.70 0 5 -21 11.20 8.50 0 5 -21 9.80 8.90 0 5 21 12.80 9.10 0 5 21 -0.80 11.80 1 -5 21 15.30 10.00 1 -5 21 37.20 11.30 -1 -5 -21 12.10 8.60 1 -5 21 12.10 12.40 1 -5 21 14.80 10.70 1 5 21 30.30 10.00 -1 5 -21 19.00 9.10 2 -5 21 81.29 15.50 2 -5 21 97.39 13.50 -2 -5 -21 97.59 12.00 2 -5 21 69.59 12.40 -2 5 -21 73.79 11.60 2 5 21 101.89 12.60 -5 -6 21 25.90 13.90 -5 -6 21 46.50 15.60 5 6 -21 35.20 12.40 -5 6 21 53.49 13.20 -4 -6 21 -1.80 12.40 -4 -6 21 31.00 14.50 4 -6 -21 1.20 7.60 4 6 -21 -8.90 10.20 -4 6 21 12.60 11.50 4 6 -21 -17.40 7.90 -3 -6 21 9.70 13.00 -3 -6 21 0.00 12.30 3 -6 -21 -13.80 7.20 3 6 -21 -4.80 8.30 -3 6 21 15.40 11.20 3 6 -21 -4.20 9.40 -2 -6 21 11.80 8.90 2 -6 -21 11.40 8.30 -2 -6 21 -7.30 11.70 -2 -6 21 16.90 13.30 2 6 -21 1.90 8.90 2 6 -21 5.20 8.70 -2 6 21 6.40 11.20 -2 6 21 13.00 8.20 -1 -6 21 6.20 9.20 -1 -6 21 17.90 12.60 1 -6 -21 9.50 7.90 -1 -6 21 -8.30 11.00 1 6 -21 -7.50 8.30 1 6 -21 -3.50 8.20 -1 6 21 8.60 8.40 -1 6 21 9.90 11.50 -1 6 21 -1.70 9.90 0 -6 21 35.00 10.30 0 -6 21 12.20 12.80 0 -6 21 -1.20 10.90 0 -6 -21 15.30 8.70 0 -6 21 25.50 10.20 0 6 21 32.80 9.50 0 6 21 22.30 10.40 0 6 21 13.70 12.10 0 6 -21 16.40 9.10 0 6 -21 19.40 8.70 1 -6 21 8.40 11.00 1 -6 21 -1.60 9.80 1 -6 21 -11.40 11.90 1 -6 21 6.00 10.70 -1 -6 -21 0.30 8.60 1 6 21 21.30 9.90 -1 6 -21 -2.00 8.50 2 -6 21 29.30 11.50 2 -6 21 43.70 14.00 -2 -6 -21 39.90 10.30 2 -6 21 21.20 11.80 2 6 21 40.60 11.10 -2 6 -21 25.10 9.70 4 -7 -21 9.70 8.20 -4 -7 21 25.10 14.50 -4 -7 21 13.30 13.40 4 7 -21 9.40 10.90 -4 7 21 40.50 12.30 4 7 -21 15.60 8.70 3 -7 -21 14.10 8.20 -3 -7 21 23.70 14.30 -3 -7 21 17.50 13.00 3 7 -21 6.10 9.90 -3 7 21 22.20 11.30 3 7 -21 11.50 8.70 -2 -7 21 49.20 14.00 -2 -7 21 13.30 12.50 -2 -7 21 50.79 10.00 2 -7 -21 42.80 9.20 2 7 -21 26.50 10.40 -2 7 21 32.00 12.50 2 7 -21 32.10 9.40 -2 7 21 42.00 11.50 -2 7 21 65.79 12.90 1 -7 -21 6.10 8.00 -1 -7 21 34.00 13.20 -1 -7 21 1.80 11.90 -1 7 21 17.90 8.50 1 7 -21 3.80 8.80 -1 7 21 23.60 10.60 1 7 -21 -1.40 8.40 -1 7 21 17.50 11.50 0 -7 21 -7.20 12.70 0 -7 21 5.40 11.50 0 -7 21 6.20 9.50 0 -7 21 -9.90 9.80 0 -7 -21 2.30 8.20 0 7 21 25.80 9.30 0 7 21 15.80 9.90 0 7 21 -12.80 11.30 0 7 -21 -3.80 7.90 0 7 -21 4.80 8.80 1 -7 21 9.00 10.80 1 -7 21 28.20 13.60 1 -7 21 3.10 10.50 -1 -7 -21 9.30 9.00 1 -7 21 -12.40 11.00 -1 7 -21 2.70 8.50 1 7 21 8.40 9.80 4 -8 -21 4.30 8.20 -4 -8 21 -11.50 13.00 -4 -8 21 20.00 14.60 -4 8 21 23.80 11.60 4 8 -21 3.50 10.60 4 8 -21 6.20 8.60 3 -8 -21 15.20 8.50 -3 -8 21 11.80 12.70 -3 -8 21 22.90 14.70 -3 8 21 17.20 11.80 -3 8 21 39.10 12.00 3 8 -21 3.40 9.90 3 8 -21 14.30 9.10 -2 -8 21 -4.00 9.20 -2 -8 21 2.30 12.20 -2 -8 21 4.00 13.40 2 -8 -21 3.10 8.30 -2 8 21 3.00 10.90 2 8 -21 -0.40 8.70 2 8 -21 -8.80 9.00 -2 8 21 3.80 11.00 -1 -8 21 18.20 13.20 -1 -8 21 1.60 9.80 -1 -8 21 -3.20 11.70 1 -8 -21 3.00 8.20 -1 8 21 15.90 8.40 1 8 -21 4.90 8.60 -1 8 21 -1.40 11.00 -1 8 21 -2.90 9.30 1 8 -21 5.70 9.20 0 -8 21 -8.30 11.20 0 -8 21 21.00 13.00 0 -8 21 9.40 10.10 0 -8 -21 4.30 8.40 0 8 21 4.80 9.80 0 8 -21 8.70 8.80 0 8 -21 1.90 10.50 0 8 21 -5.40 11.40 0 8 21 8.20 9.10 1 -8 21 -1.10 11.00 1 -8 21 2.80 10.70 1 -8 21 -21.20 10.80 -1 -8 -21 -9.00 8.30 1 -8 21 0.60 12.80 -1 8 -21 -7.00 8.50 1 8 21 10.60 10.20 1 8 21 13.20 12.10 -3 -9 21 -10.80 12.10 -3 -9 21 30.80 14.70 3 -9 -21 2.70 8.40 -3 9 21 -7.50 10.70 -3 9 21 9.10 10.90 3 9 -21 -3.00 8.60 3 9 -21 -12.40 10.00 -2 -9 21 16.60 12.80 2 -9 -21 -3.70 8.20 -2 -9 21 15.00 14.10 -2 -9 21 -11.20 9.70 -2 9 21 -2.20 10.60 2 9 -21 0.00 9.80 -2 9 21 -15.30 10.40 2 9 -21 -16.00 8.50 1 -9 -21 45.50 10.00 -1 -9 21 61.89 14.80 -1 -9 21 42.70 13.70 -1 -9 21 65.09 11.20 1 9 -21 36.40 10.60 -1 9 21 73.09 9.90 -1 9 21 50.79 12.80 1 9 -21 73.69 11.10 -1 9 21 51.69 11.30 0 -9 -21 8.50 9.00 0 -9 21 39.40 14.10 0 -9 21 0.90 11.60 0 -9 21 27.00 11.20 0 9 21 11.80 11.90 0 9 21 24.10 10.20 0 9 21 39.20 9.90 0 9 -21 -2.80 8.60 -5 0 22 -5.70 12.20 -5 0 22 27.50 13.80 -4 0 22 15.80 12.90 -4 0 22 -0.80 11.80 4 0 -22 0.00 7.70 -3 0 22 54.29 13.90 3 0 -22 19.30 8.50 -3 0 22 14.90 11.80 -2 0 22 10.20 11.40 -2 0 22 61.39 13.90 -2 0 22 29.40 10.70 2 0 -22 19.40 8.70 -1 0 22 15.40 9.10 1 0 -22 0.90 8.10 -1 0 22 2.90 12.20 -1 0 22 -2.30 10.50 0 0 22 118.59 15.70 0 0 22 125.59 12.20 0 0 -22 127.59 12.70 0 0 22 83.99 13.00 -1 0 -22 84.29 11.60 1 0 22 82.09 15.00 1 0 22 107.49 12.20 -2 0 -22 9.60 9.60 2 0 22 21.20 10.80 2 0 22 -12.20 12.60 -5 -1 22 50.09 15.00 -5 -1 22 9.20 13.20 -5 1 22 60.79 14.70 -5 1 22 32.90 14.00 5 1 -22 45.10 12.20 4 -1 -22 -6.20 7.50 -4 -1 22 6.50 12.70 -4 -1 22 -0.70 12.40 -4 1 22 -3.90 12.20 -4 1 22 -6.60 11.50 4 1 -22 9.30 10.30 4 1 -22 -8.40 7.70 3 -1 -22 2.70 7.90 -3 -1 22 38.20 13.60 -3 -1 22 -3.40 11.80 -3 1 22 47.70 13.30 -3 1 22 27.70 12.40 3 1 -22 13.10 8.40 -2 -1 22 44.50 10.60 -2 -1 22 25.80 12.20 2 -1 -22 17.40 8.40 -2 -1 22 62.09 14.10 -2 1 22 15.30 11.50 -2 1 22 40.00 13.30 -2 1 22 29.00 11.30 2 1 -22 26.80 8.90 -1 -1 22 10.10 11.30 -1 -1 22 7.40 9.20 1 -1 -22 14.70 8.50 -1 -1 22 8.10 12.60 -1 1 22 10.10 10.90 -1 1 22 18.30 9.00 1 1 -22 8.80 8.40 -1 1 22 25.30 12.80 0 -1 22 2.60 10.60 0 -1 22 6.80 10.00 0 -1 -22 7.80 8.70 0 -1 22 18.80 12.40 0 1 22 20.40 9.30 0 1 -22 4.40 8.70 0 1 22 -2.20 10.00 0 1 22 6.80 11.90 -1 -1 -22 13.20 9.20 1 -1 22 -2.40 9.80 1 -1 22 10.10 12.30 -1 1 -22 13.10 8.80 1 1 22 14.50 13.20 1 1 22 7.10 9.70 2 -1 22 8.40 10.70 2 -1 22 -3.50 13.50 -2 -1 -22 -3.30 8.60 -2 1 -22 -13.00 8.40 2 1 22 -13.60 12.80 2 1 22 15.70 10.80 -5 -2 22 -5.40 12.90 -5 -2 22 15.50 14.20 -5 2 22 8.60 12.80 -5 2 22 -5.20 12.10 5 2 -22 9.00 11.20 4 -2 -22 -1.00 7.60 -4 -2 22 2.20 12.40 -4 -2 22 4.70 12.60 4 2 -22 -3.80 7.80 -4 2 22 -3.30 12.50 -4 2 22 2.80 11.90 4 2 -22 -3.00 9.70 3 -2 -22 -5.40 7.60 -3 -2 22 3.50 12.00 -3 -2 22 13.70 13.00 3 2 -22 -1.40 8.20 3 2 -22 1.60 9.30 -3 2 22 9.50 12.40 -3 2 22 -3.50 11.30 -2 -2 22 -7.20 10.00 -2 -2 22 19.30 13.30 2 -2 -22 12.70 8.10 -2 -2 22 -5.90 11.10 -2 2 22 9.40 12.10 -2 2 22 9.80 11.10 2 2 -22 -3.20 8.20 -2 2 22 9.40 11.60 2 2 -22 -1.10 8.80 -1 -2 22 25.70 13.00 -1 -2 22 9.20 11.40 -1 -2 22 11.00 9.30 1 -2 -22 18.10 8.80 -1 2 22 14.00 12.30 1 2 -22 5.80 8.60 1 2 -22 7.20 8.40 -1 2 22 4.70 10.50 -1 2 22 6.70 8.70 0 -2 22 19.50 10.10 0 -2 22 25.30 12.80 0 -2 -22 17.90 9.00 0 -2 22 6.40 10.70 0 2 22 28.10 12.50 0 2 22 35.10 9.80 0 2 -22 32.30 9.10 0 2 -22 15.40 8.80 1 -2 22 24.10 11.00 1 -2 22 38.90 13.80 -1 -2 -22 25.60 9.40 1 2 22 39.00 10.60 1 2 22 28.70 13.70 -1 2 -22 37.30 9.60 -4 -3 22 -3.90 11.80 -4 -3 22 25.70 14.00 4 -3 -22 4.60 7.70 4 3 -22 0.80 10.30 -4 3 22 -2.60 11.70 -4 3 22 9.00 12.50 4 3 -22 1.70 7.90 3 -3 -22 38.90 9.10 -3 -3 22 34.10 13.90 -3 -3 22 21.30 12.70 3 3 -22 21.00 8.50 -3 3 22 26.50 12.80 3 3 -22 15.80 10.20 2 -3 -22 33.20 8.90 -2 -3 22 31.70 11.70 -2 -3 22 41.30 13.50 -2 -3 22 23.50 12.10 2 3 -22 33.80 9.10 -2 3 22 31.30 12.80 2 3 -22 26.60 9.90 -1 -3 22 3.80 9.10 1 -3 -22 1.80 8.20 -1 -3 22 -6.50 10.70 -1 -3 22 10.50 13.00 1 3 -22 4.50 8.50 -1 3 22 9.20 11.70 1 3 -22 2.00 8.10 -1 3 22 1.50 8.30 0 -3 -22 3.90 8.40 0 -3 22 1.10 10.00 0 -3 22 2.30 10.60 0 -3 22 0.40 12.70 0 3 -22 2.10 7.80 0 3 22 25.50 9.30 0 3 -22 3.10 8.50 0 3 22 4.70 12.00 -1 -3 -22 -12.00 8.50 1 -3 22 9.90 12.80 1 -3 22 -4.00 10.70 1 3 22 -7.10 12.60 -1 3 -22 5.60 9.30 1 3 22 1.80 9.80 -4 -4 22 -8.60 13.60 -4 -4 22 -8.90 12.00 4 -4 -22 1.70 7.80 4 4 -22 -2.00 8.30 -4 4 22 10.40 12.30 4 4 -22 -2.80 10.00 -3 -4 22 0.50 11.90 -3 -4 22 21.80 13.50 3 -4 -22 25.40 8.60 3 4 -22 8.30 8.70 -3 4 22 7.10 12.30 3 4 -22 9.70 9.80 -2 -4 22 5.40 13.00 2 -4 -22 12.10 8.30 -2 -4 22 3.50 11.60 2 4 -22 8.80 9.00 -2 4 22 12.50 12.00 2 4 -22 -12.80 8.30 1 -4 -22 7.90 8.40 -1 -4 22 12.50 13.20 -1 -4 22 7.90 11.30 -1 -4 22 10.60 9.40 -1 4 22 4.30 11.50 1 4 -22 -1.40 8.60 1 4 -22 3.10 8.60 -1 4 22 10.60 8.60 0 -4 22 5.00 10.20 0 -4 -22 4.30 8.60 0 -4 22 3.70 10.80 0 -4 22 13.40 13.20 0 4 -22 6.10 8.30 0 4 22 8.10 12.20 0 4 -22 18.50 9.10 0 4 22 -1.00 9.40 1 -4 22 13.00 11.40 1 -4 22 8.40 10.80 -1 -4 -22 13.50 9.10 1 -4 22 22.10 13.60 1 4 22 -5.80 12.80 1 4 22 30.10 10.70 -1 4 -22 8.80 9.30 -4 -5 22 20.40 14.40 4 -5 -22 -0.30 7.90 -4 -5 22 1.20 12.80 4 5 -22 -12.60 10.30 -4 5 22 11.50 11.90 4 5 -22 -6.70 8.20 -3 -5 22 -1.30 11.90 -3 -5 22 8.80 13.90 3 -5 -22 7.30 8.10 -3 5 22 20.40 12.10 3 5 -22 3.60 10.40 3 5 -22 6.10 8.60 -2 -5 22 54.99 14.40 2 -5 -22 21.60 9.00 -2 -5 22 19.20 12.10 2 5 -22 34.90 10.90 -2 5 22 49.20 13.10 2 5 -22 25.50 9.30 -1 -5 22 8.50 9.30 -1 -5 22 14.60 13.20 -1 -5 22 7.80 11.60 1 -5 -22 19.30 8.70 -1 5 22 13.70 11.80 1 5 -22 2.50 8.70 -1 5 22 17.70 8.60 1 5 -22 3.00 9.00 0 -5 -22 -4.30 8.40 0 -5 22 -1.40 12.80 0 -5 22 5.60 11.00 0 -5 22 4.40 10.20 0 -5 22 18.90 9.50 0 5 22 2.80 9.40 0 5 -22 -1.90 8.40 0 5 22 11.20 12.30 0 5 -22 4.80 9.00 -1 -5 -22 8.00 9.10 1 -5 22 -2.30 11.10 1 -5 22 -0.10 12.80 1 -5 22 16.10 14.80 1 -5 22 19.20 10.20 1 5 22 17.10 10.40 1 5 22 -12.20 12.60 -1 5 -22 14.30 9.70 3 -6 -22 -6.00 7.90 -3 -6 22 14.10 13.90 -3 -6 22 -3.50 12.20 -3 6 22 19.40 12.10 3 6 -22 -10.20 9.80 3 6 -22 3.10 9.00 -2 -6 22 31.00 14.90 2 -6 -22 23.30 9.00 -2 -6 22 24.50 12.90 -2 -6 22 41.00 14.20 2 6 -22 7.60 9.10 2 6 -22 14.40 9.80 -2 6 22 27.40 12.10 1 -6 -22 47.70 10.00 -1 -6 22 15.30 12.20 -1 -6 22 68.09 14.90 1 6 -22 43.90 10.40 1 6 -22 20.20 10.00 -1 6 22 46.50 9.50 -1 6 22 34.20 13.00 0 -6 22 4.00 11.40 0 -6 -22 -2.40 8.70 0 -6 22 6.90 13.40 0 -6 22 21.00 9.90 0 -6 22 7.40 10.40 0 6 -22 17.70 9.50 0 6 -22 -13.50 12.60 0 6 22 11.40 9.60 0 6 22 8.50 12.50 -2 -7 22 42.30 14.70 2 -7 -22 34.60 9.50 -2 -7 22 13.80 13.00 -2 7 22 18.50 12.10 2 7 -22 31.30 10.00 2 7 -22 23.70 10.30 -3 0 23 18.10 13.80 -3 0 23 14.60 12.20 3 0 -23 -18.50 7.90 -2 0 23 5.90 11.30 -2 0 23 7.30 13.00 2 0 -23 -3.80 8.40 1 0 -23 -0.60 8.60 -1 0 23 2.10 9.30 -1 0 23 4.90 10.90 -1 0 23 14.00 12.90 -2 -1 23 3.30 13.10 2 -1 -23 1.90 8.50 -2 -1 23 -12.70 11.50 2 1 -23 12.70 9.60 2 1 -23 -15.00 8.20 -2 1 23 -0.40 12.90 -2 1 23 -2.20 11.20 -1 -1 23 -1.40 11.30 -1 -1 23 0.30 9.40 1 -1 -23 0.00 8.60 -1 -1 23 12.30 12.90 -1 1 23 3.80 11.20 -1 1 23 2.80 12.70 -1 1 23 -2.80 9.20 1 1 -23 6.10 8.90 1 1 -23 -4.00 8.80 2 -2 -23 -9.60 8.10 -2 -2 23 3.40 12.20 -2 -2 23 15.20 13.70 -2 2 23 4.90 11.30 2 2 -23 -1.90 8.60 2 2 -23 24.00 9.90 -2 2 23 6.70 12.80 -1 -2 23 15.40 12.00 1 -2 -23 -16.70 8.00 -1 -2 23 2.60 9.20 -1 -2 23 5.40 13.60 -1 2 23 -6.90 10.50 -1 2 23 7.80 13.00 1 2 -23 11.30 8.80 1 2 -23 15.50 9.10 -1 2 23 8.00 9.20 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 58371 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S001 S 0.78848(7) 0.71598(4) 0.48368(3) 0.04484(17) Uani 1 1 d . . . . Si02 Si 0.87412(7) 0.24126(3) 0.75180(3) 0.03079(15) Uani 1 1 d . . . . N004 N 0.75418(18) 0.44314(9) 0.65545(8) 0.0258(4) Uani 1 1 d . . . . N005 N 0.56580(18) 0.39796(9) 0.82524(9) 0.0272(4) Uani 1 1 d . . . . F006 F 0.6485(2) 0.67115(11) 0.35154(9) 0.0780(5) Uani 1 1 d . . . . O007 O 0.9157(2) 0.72801(11) 0.44652(11) 0.0596(5) Uani 1 1 d . . . . C008 C 0.7255(2) 0.39975(11) 0.71266(10) 0.0224(4) Uani 1 1 d . . . . C009 C 0.7566(2) 0.33083(11) 0.75209(10) 0.0252(4) Uani 1 1 d . . . . C00A C 0.6569(2) 0.38150(11) 0.77634(10) 0.0239(4) Uani 1 1 d . . . . F00B F 0.6412(2) 0.79197(11) 0.37019(12) 0.0996(7) Uani 1 1 d . . . . C00C C 0.8642(2) 0.41462(11) 0.60721(10) 0.0277(4) Uani 1 1 d . . . . H00C H 0.8982 0.3625 0.6273 0.033 Uiso 1 1 calc R . . . O00D O 0.7581(2) 0.77770(13) 0.53378(12) 0.0743(6) Uani 1 1 d . . . . F00E F 0.5107(2) 0.71374(14) 0.42957(13) 0.1020(7) Uani 1 1 d . . . . C00F C 0.4820(2) 0.47082(12) 0.82049(12) 0.0338(5) Uani 1 1 d . . . . H00F H 0.5141 0.5021 0.7780 0.041 Uiso 1 1 calc R . . . C00G C 0.6832(2) 0.51919(12) 0.63657(12) 0.0340(5) Uani 1 1 d . . . . H00G H 0.7222 0.5387 0.5899 0.041 Uiso 1 1 calc R . . . O00H O 0.7710(3) 0.63976(13) 0.51053(13) 0.0923(8) Uani 1 1 d . . . . C00I C 0.9966(2) 0.46737(14) 0.61452(12) 0.0381(5) Uani 1 1 d . . . . H00A H 0.9675 0.5184 0.5932 0.057 Uiso 1 1 calc GR . . . H00B H 1.0709 0.4450 0.5863 0.057 Uiso 1 1 calc GR . . . H00D H 1.0371 0.4728 0.6688 0.057 Uiso 1 1 calc GR . . . C00J C 0.5436(2) 0.34044(13) 0.88593(11) 0.0351(5) Uani 1 1 d . . . . H00J H 0.4653 0.3614 0.9142 0.042 Uiso 1 1 calc R . . . C00K C 0.7961(3) 0.40422(14) 0.52451(11) 0.0393(5) Uani 1 1 d . . . . H00E H 0.7088 0.3715 0.5224 0.059 Uiso 1 1 calc GR . . . H00H H 0.8669 0.3795 0.4956 0.059 Uiso 1 1 calc GR . . . H00I H 0.7684 0.4549 0.5019 0.059 Uiso 1 1 calc GR . . . C00M C 0.5195(3) 0.51088(14) 0.61470(12) 0.0427(6) Uani 1 1 d . . . . H00K H 0.4992 0.4760 0.5705 0.064 Uiso 1 1 calc GR . . . H00L H 0.4764 0.5618 0.6012 0.064 Uiso 1 1 calc GR . . . H00M H 0.4767 0.4895 0.6582 0.064 Uiso 1 1 calc GR . . . C00N C 0.7286(3) 0.57778(13) 0.69998(14) 0.0443(6) Uani 1 1 d . . . . H00N H 0.6942 0.5605 0.7474 0.066 Uiso 1 1 calc GR . . . H00O H 0.6853 0.6283 0.6849 0.066 Uiso 1 1 calc GR . . . H00P H 0.8355 0.5823 0.7085 0.066 Uiso 1 1 calc GR . . . C00O C 0.4890(3) 0.26400(13) 0.85081(13) 0.0413(6) Uani 1 1 d . . . . H00Q H 0.3994 0.2727 0.8148 0.062 Uiso 1 1 calc GR . . . H00R H 0.4683 0.2286 0.8915 0.062 Uiso 1 1 calc GR . . . H00S H 0.5640 0.2412 0.8233 0.062 Uiso 1 1 calc GR . . . C00P C 1.0657(2) 0.27483(14) 0.75921(14) 0.0440(6) Uani 1 1 d . . . . H00T H 1.1279 0.2322 0.7461 0.066 Uiso 1 1 calc GR . . . H00U H 1.0991 0.2921 0.8118 0.066 Uiso 1 1 calc GR . . . H00V H 1.0718 0.3180 0.7237 0.066 Uiso 1 1 calc GR . . . C00Q C 0.6409(3) 0.72417(16) 0.40517(16) 0.0526(7) Uani 1 1 d . . . . C00R C 0.5159(3) 0.51807(16) 0.89366(14) 0.0550(7) Uani 1 1 d . . . . H00W H 0.4802 0.4905 0.9361 0.082 Uiso 1 1 calc GR . . . H00X H 0.4674 0.5686 0.8865 0.082 Uiso 1 1 calc GR . . . H00Y H 0.6219 0.5256 0.9055 0.082 Uiso 1 1 calc GR . . . C00S C 0.8166(3) 0.19308(15) 0.65893(15) 0.0532(7) Uani 1 1 d . . . . H00Z H 0.8371 0.2271 0.6171 0.080 Uiso 1 1 calc GR . . . H H 0.7114 0.1822 0.6534 0.080 Uiso 1 1 calc GR . . . HA H 0.8706 0.1444 0.6569 0.080 Uiso 1 1 calc GR . . . C00T C 0.6819(3) 0.33348(16) 0.94352(12) 0.0531(7) Uani 1 1 d . . . . H00 H 0.7625 0.3152 0.9173 0.080 Uiso 1 1 calc GR . . . HB H 0.6656 0.2965 0.9838 0.080 Uiso 1 1 calc GR . . . HC H 0.7069 0.3842 0.9667 0.080 Uiso 1 1 calc GR . . . C00U C 0.3187(3) 0.45633(17) 0.79970(17) 0.0570(7) Uani 1 1 d . . . . H0AA H 0.3006 0.4285 0.7507 0.086 Uiso 1 1 calc GR . . . HD H 0.2667 0.5060 0.7950 0.086 Uiso 1 1 calc GR . . . HE H 0.2835 0.4252 0.8400 0.086 Uiso 1 1 calc GR . . . C00V C 0.8526(3) 0.17624(17) 0.83309(18) 0.0708(9) Uani 1 1 d . . . . H1AA H 0.7513 0.1576 0.8281 0.106 Uiso 1 1 calc GR . . . HF H 0.8758 0.2047 0.8815 0.106 Uiso 1 1 calc GR . . . HG H 0.9192 0.1320 0.8328 0.106 Uiso 1 1 calc GR . . . Cl1S Cl 1.0414(3) 0.99085(18) 0.64454(11) 0.0563(5) Uani 0.5 1 d . P A -1 C1S C 1.0087(5) 0.9988(3) 0.5451(3) 0.0382(10) Uani 0.5 1 d . P A -1 C2S C 0.954(3) 0.9445(10) 0.4996(16) 0.046(4) Uani 0.5 1 d . P A -1 H2S H 0.9292 0.8985 0.5246 0.055 Uiso 0.5 1 calc R P A -1 C3S C 0.9258(6) 0.9423(3) 0.4234(4) 0.0543(14) Uani 0.5 1 d . P A -1 H3S H 0.8816 0.8991 0.3958 0.065 Uiso 0.5 1 calc R P A -1 C4S C 0.9668(12) 1.0080(6) 0.3887(4) 0.058(2) Uani 0.5 1 d . P A -1 H4S H 0.9548 1.0106 0.3342 0.070 Uiso 0.5 1 calc R P A -1 C5S C 1.0260(6) 1.0712(3) 0.4317(3) 0.0454(12) Uani 0.5 1 d . P A -1 H5S H 1.0489 1.1163 0.4048 0.054 Uiso 0.5 1 calc R P A -1 C6S C 1.053(2) 1.0724(9) 0.5090(12) 0.033(2) Uani 0.5 1 d . P A -1 H6S H 1.0951 1.1154 0.5377 0.040 Uiso 0.5 1 calc R P A -1 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 S001 0.0532(4) 0.0443(4) 0.0391(3) 0.0059(3) 0.0135(3) -0.0038(3) Si02 0.0310(3) 0.0260(3) 0.0359(3) 0.0109(2) 0.0068(2) 0.0047(2) N004 0.0309(10) 0.0238(8) 0.0235(7) 0.0074(6) 0.0068(7) 0.0046(7) N005 0.0295(10) 0.0306(9) 0.0225(8) -0.0005(7) 0.0067(7) -0.0011(7) F006 0.0928(14) 0.0874(13) 0.0544(9) -0.0254(9) 0.0122(9) -0.0193(10) O007 0.0416(11) 0.0694(13) 0.0723(12) 0.0037(10) 0.0239(9) 0.0031(9) C008 0.0241(10) 0.0233(10) 0.0195(8) 0.0011(7) 0.0016(7) -0.0008(8) C009 0.0272(11) 0.0275(10) 0.0209(9) 0.0056(7) 0.0036(8) -0.0012(8) C00A 0.0252(11) 0.0260(10) 0.0200(8) 0.0018(7) 0.0012(8) -0.0027(8) F00B 0.1177(17) 0.0659(13) 0.1057(15) 0.0276(11) -0.0172(13) 0.0234(11) C00C 0.0343(12) 0.0278(10) 0.0227(9) 0.0047(8) 0.0095(8) 0.0023(9) O00D 0.0782(15) 0.0867(16) 0.0651(12) -0.0365(11) 0.0356(11) -0.0275(12) F00E 0.0448(11) 0.147(2) 0.1173(16) -0.0401(15) 0.0229(11) -0.0114(11) C00F 0.0351(13) 0.0354(12) 0.0322(10) -0.0059(9) 0.0087(9) 0.0040(9) C00G 0.0428(13) 0.0257(11) 0.0339(11) 0.0121(8) 0.0068(10) 0.0088(9) O00H 0.136(2) 0.0630(15) 0.0785(15) 0.0408(12) 0.0155(14) -0.0155(14) C00I 0.0367(13) 0.0417(13) 0.0373(11) 0.0021(10) 0.0097(10) -0.0047(10) C00J 0.0415(13) 0.0398(13) 0.0270(10) 0.0027(9) 0.0157(9) -0.0047(10) C00K 0.0427(14) 0.0512(15) 0.0241(10) -0.0014(9) 0.0052(9) -0.0030(11) C00M 0.0438(14) 0.0490(14) 0.0336(11) 0.0089(10) -0.0005(10) 0.0160(11) C00N 0.0461(15) 0.0239(11) 0.0625(15) 0.0002(10) 0.0065(12) 0.0046(10) C00O 0.0409(14) 0.0405(13) 0.0444(13) 0.0034(10) 0.0129(11) -0.0090(10) C00P 0.0330(13) 0.0477(15) 0.0498(13) 0.0095(11) 0.0006(11) 0.0061(11) C00Q 0.0468(16) 0.0522(17) 0.0608(16) -0.0061(13) 0.0143(13) -0.0002(12) C00R 0.074(2) 0.0480(16) 0.0431(14) -0.0165(11) 0.0082(13) 0.0030(13) C00S 0.0559(17) 0.0350(14) 0.0676(17) -0.0131(12) 0.0048(13) 0.0007(12) C00T 0.0668(18) 0.0645(18) 0.0260(11) 0.0122(11) -0.0006(11) -0.0114(14) C00U 0.0322(14) 0.0614(18) 0.0770(19) -0.0144(15) 0.0058(13) 0.0097(12) C00V 0.077(2) 0.0578(18) 0.085(2) 0.0462(16) 0.0389(17) 0.0340(16) Cl1S 0.0475(10) 0.0695(11) 0.0505(11) 0.0197(11) 0.0024(10) 0.0075(7) C1S 0.027(2) 0.042(3) 0.044(3) 0.009(2) 0.002(2) 0.008(2) C2S 0.043(5) 0.009(6) 0.084(8) -0.009(5) 0.000(4) -0.008(4) C3S 0.044(3) 0.048(3) 0.068(4) -0.014(3) -0.001(3) 0.000(2) C4S 0.052(4) 0.069(5) 0.052(5) 0.000(5) -0.002(5) 0.010(3) C5S 0.047(3) 0.042(3) 0.048(3) 0.010(2) 0.011(2) 0.006(2) C6S 0.026(4) 0.008(6) 0.062(6) -0.001(5) -0.002(4) -0.005(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O007 S001 C00Q 102.57(12) O00D S001 O007 114.48(12) O00D S001 C00Q 102.74(14) O00H S001 O007 115.14(14) O00H S001 O00D 116.38(14) O00H S001 C00Q 102.68(14) C00P Si02 C009 106.67(10) C00P Si02 C00V 109.92(13) C00S Si02 C009 106.10(10) C00S Si02 C00P 111.00(12) C00S Si02 C00V 111.24(15) C00V Si02 C009 111.77(11) C008 N004 C00C 118.26(15) C008 N004 C00G 123.19(16) C00G N004 C00C 118.55(15) C00A N005 C00F 121.74(16) C00A N005 C00J 119.20(17) C00F N005 C00J 119.04(16) N004 C008 C009 145.53(18) N004 C008 C00A 155.07(19) C009 C008 C00A 59.40(13) C008 C009 Si02 141.23(15) C00A C009 Si02 158.09(14) C00A C009 C008 60.68(13) N005 C00A C008 151.42(19) N005 C00A C009 148.66(18) C009 C00A C008 59.93(13) N004 C00C H00C 107.5 N004 C00C C00I 110.94(16) N004 C00C C00K 111.20(17) C00I C00C H00C 107.5 C00K C00C H00C 107.5 C00K C00C C00I 112.01(17) N005 C00F H00F 107.2 N005 C00F C00R 111.48(18) N005 C00F C00U 111.59(19) C00R C00F H00F 107.2 C00R C00F C00U 111.9(2) C00U C00F H00F 107.2 N004 C00G H00G 106.5 N004 C00G C00M 111.52(18) N004 C00G C00N 110.90(17) C00M C00G H00G 106.5 C00M C00G C00N 114.37(19) C00N C00G H00G 106.5 C00C C00I H00A 109.5 C00C C00I H00B 109.5 C00C C00I H00D 109.5 H00A C00I H00B 109.5 H00A C00I H00D 109.5 H00B C00I H00D 109.5 N005 C00J H00J 107.2 N005 C00J C00O 111.05(16) N005 C00J C00T 110.08(18) C00O C00J H00J 107.2 C00O C00J C00T 113.8(2) C00T C00J H00J 107.2 C00C C00K H00E 109.5 C00C C00K H00H 109.5 C00C C00K H00I 109.5 H00E C00K H00H 109.5 H00E C00K H00I 109.5 H00H C00K H00I 109.5 C00G C00M H00K 109.5 C00G C00M H00L 109.5 C00G C00M H00M 109.5 H00K C00M H00L 109.5 H00K C00M H00M 109.5 H00L C00M H00M 109.5 C00G C00N H00N 109.5 C00G C00N H00O 109.5 C00G C00N H00P 109.5 H00N C00N H00O 109.5 H00N C00N H00P 109.5 H00O C00N H00P 109.5 C00J C00O H00Q 109.5 C00J C00O H00R 109.5 C00J C00O H00S 109.5 H00Q C00O H00R 109.5 H00Q C00O H00S 109.5 H00R C00O H00S 109.5 Si02 C00P H00T 109.5 Si02 C00P H00U 109.5 Si02 C00P H00V 109.5 H00T C00P H00U 109.5 H00T C00P H00V 109.5 H00U C00P H00V 109.5 F006 C00Q S001 112.48(19) F006 C00Q F00E 105.9(2) F00B C00Q S001 112.04(19) F00B C00Q F006 106.1(2) F00B C00Q F00E 109.1(2) F00E C00Q S001 111.0(2) C00F C00R H00W 109.5 C00F C00R H00X 109.5 C00F C00R H00Y 109.5 H00W C00R H00X 109.5 H00W C00R H00Y 109.5 H00X C00R H00Y 109.5 Si02 C00S H00Z 109.5 Si02 C00S H 109.5 Si02 C00S HA 109.5 H00Z C00S H 109.5 H00Z C00S HA 109.5 H C00S HA 109.5 C00J C00T H00 109.5 C00J C00T HB 109.5 C00J C00T HC 109.5 H00 C00T HB 109.5 H00 C00T HC 109.5 HB C00T HC 109.5 C00F C00U H0AA 109.5 C00F C00U HD 109.5 C00F C00U HE 109.5 H0AA C00U HD 109.5 H0AA C00U HE 109.5 HD C00U HE 109.5 Si02 C00V H1AA 109.5 Si02 C00V HF 109.5 Si02 C00V HG 109.5 H1AA C00V HF 109.5 H1AA C00V HG 109.5 HF C00V HG 109.5 C2S C1S Cl1S 124.4(13) C2S C1S C6S 117.3(19) C6S C1S Cl1S 118.2(9) C1S C2S H2S 114.7 C1S C2S C3S 131(2) C3S C2S H2S 114.7 C2S C3S H3S 123.2 C2S C3S C4S 113.6(10) C4S C3S H3S 123.2 C3S C4S H4S 119.4 C3S C4S C5S 121.2(6) C5S C4S H4S 119.4 C4S C5S H5S 117.9 C6S C5S C4S 124.2(8) C6S C5S H5S 117.9 C1S C6S H6S 123.5 C5S C6S C1S 113.0(11) C5S C6S H6S 123.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S001 O007 1.4356(18) S001 O00D 1.435(2) S001 O00H 1.415(2) S001 C00Q 1.804(3) Si02 C009 1.889(2) Si02 C00P 1.847(2) Si02 C00S 1.843(3) Si02 C00V 1.850(2) N004 C008 1.310(2) N004 C00C 1.494(2) N004 C00G 1.484(2) N005 C00A 1.314(2) N005 C00F 1.473(3) N005 C00J 1.493(2) F006 C00Q 1.323(3) C008 C009 1.387(3) C008 C00A 1.397(3) C009 C00A 1.379(3) F00B C00Q 1.322(3) C00C H00C 1.0000 C00C C00I 1.515(3) C00C C00K 1.512(3) F00E C00Q 1.343(3) C00F H00F 1.0000 C00F C00R 1.519(3) C00F C00U 1.520(3) C00G H00G 1.0000 C00G C00M 1.512(3) C00G C00N 1.520(3) C00I H00A 0.9800 C00I H00B 0.9800 C00I H00D 0.9800 C00J H00J 1.0000 C00J C00O 1.513(3) C00J C00T 1.519(3) C00K H00E 0.9800 C00K H00H 0.9800 C00K H00I 0.9800 C00M H00K 0.9800 C00M H00L 0.9800 C00M H00M 0.9800 C00N H00N 0.9800 C00N H00O 0.9800 C00N H00P 0.9800 C00O H00Q 0.9800 C00O H00R 0.9800 C00O H00S 0.9800 C00P H00T 0.9800 C00P H00U 0.9800 C00P H00V 0.9800 C00R H00W 0.9800 C00R H00X 0.9800 C00R H00Y 0.9800 C00S H00Z 0.9800 C00S H 0.9800 C00S HA 0.9800 C00T H00 0.9800 C00T HB 0.9800 C00T HC 0.9800 C00U H0AA 0.9800 C00U HD 0.9800 C00U HE 0.9800 C00V H1AA 0.9800 C00V HF 0.9800 C00V HG 0.9800 Cl1S C1S 1.738(5) C1S C2S 1.290(17) C1S C6S 1.502(19) C2S H2S 0.9500 C2S C3S 1.33(3) C3S H3S 0.9500 C3S C4S 1.366(12) C4S H4S 0.9500 C4S C5S 1.396(11) C5S H5S 0.9500 C5S C6S 1.35(2) C6S H6S 0.9500