#------------------------------------------------------------------------------ #$Date: 2021-04-16 04:01:04 +0300 (Fri, 16 Apr 2021) $ #$Revision: 264219 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/18/1561839.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_1561839 loop_ _publ_author_name 'Buch, Christian Dirk' 'Hansen, Steen H.' 'Mitcov, Dmitri' 'Tram, Camilla Mia' 'Nichol, Gary Stephen' 'Brechin, Euan K.' 'Piligkos, Stergios' _publ_section_title ; Design of Pure Heterodinuclear Lanthanoid Cryptate Complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC00987G _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C39 H45 N10 O9 Y Yb, N O3, 2.5(H2 O)' _chemical_formula_sum 'C39 H50 N11 O14.5 Y Yb' _chemical_formula_weight 1166.85 _space_group_crystal_system tetragonal _space_group_IT_number 92 _space_group_name_Hall 'P 4abw 2nw' _space_group_name_H-M_alt 'P 41 21 2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc2747pb _audit_creation_date 2021-02-03 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226) ; _audit_update_record ; 2021-02-03 deposited with the CCDC. 2021-04-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.5997(5) _cell_length_b 17.5997(5) _cell_length_c 28.9790(12) _cell_measurement_reflns_used 9671 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.282 _cell_measurement_theta_min 2.314 _cell_volume 8976.2(5) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0574 _diffrn_reflns_av_unetI/netI 0.0350 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 84780 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.876 _diffrn_reflns_theta_min 1.820 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.437 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1386 before and 0.0747 after correction. The Ratio of minimum to maximum transmission is 0.7287. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.727 _exptl_crystal_description block _exptl_crystal_F_000 4688 _exptl_crystal_size_max 0.282 _exptl_crystal_size_mid 0.141 _exptl_crystal_size_min 0.122 _refine_diff_density_max 1.463 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.093 _refine_ls_abs_structure_details ; Flack x determined using 4070 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.017(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 635 _refine_ls_number_reflns 10688 _refine_ls_number_restraints 118 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0282 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+6.2651P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.0710 _reflns_Friedel_coverage 0.776 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 9841 _reflns_number_total 10688 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc00987g2.cif _cod_data_source_block mo_d8v4659_0m_a _cod_original_cell_volume 8976.2(6) _cod_original_formula_sum 'C39 H50 N11 O14.50 Y Yb' _cod_database_code 1561839 _shelx_shelxl_version_number 2018/3 _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 0.679 _shelx_estimated_absorpt_t_min 0.444 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Shared sites {Yb1, Y1A} {Y2, Yb2A} 3. Restrained distances O13-H13B = O13-H13A = O13A-H13D = O13A-H13C = O16-H16E = O16_$3-H16D_$4 = O14- H14A 0.84 with sigma of 0.02 O15-H15 0.84 with sigma of 0.02 H14A-H14A_$1 = H16D_$4-H16D_$3 1.35 with sigma of 0.04 H16D-H16E = H13C-H13D = H13B-H13A 1.35 with sigma of 0.04 H15_$5-H15 1.35 with sigma of 0.04 O12A-N11A \\sim O11A-N11A \\sim O10A-N11A \\sim O10-N11 \\sim O11-N11 \\sim O12-N11 with sigma of 0.02 4. Restrained planarity O4, O5, O6, N9 with sigma of 0.1 O4A, O5, O6, N9 with sigma of 0.1 5. Uiso/Uaniso restraints and constraints Uanis(Yb1) = Uanis(Y1A) Uanis(Y2) = Uanis(Yb2A) 6. Rigid body (RIGU) restrains O10, O11, O12, N11 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O10A, O11A, O12A, N11A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O4, O5, O6, N9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O4, O4A, O6, N9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 7. Same fragment restrains {O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04 as in {O10, O11, O12, N11} {O7, O8, O9, N10} sigma for 1-2: 0.02, 1-3: 0.04 as in {O10A, O11A, O12A, N11A} 8. Others Sof(Yb2A)=Sof(Y1A)=1-FVAR(1) Sof(Yb1)=Sof(Y2)=FVAR(1) Sof(O4A)=1-FVAR(2) Sof(O4)=FVAR(2) Fixed Sof: O10(0.5) O11(0.5) O12(0.5) N11(0.5) O10A(0.5) O11A(0.5) O12A(0.5) N11A(0.5) O13(0.5) H13A(0.5) H13B(0.5) O13A(0.5) H13C(0.5) H13D(0.5) H16D(0.5) 9.a Everything fixed: O13, H13A, H13B, O13A, H13C, H13D, O14, H14A, O16, H16D, H16E 9.b Secondary CH2 refined with riding coordinates: C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A, H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B) 9.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C8(H8), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18), C21(H21), C23(H23), C26(H26), C27(H27) 9.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C) ; _shelx_res_file ; TITL mo_D8V4659_0m_a.res in P4(1)2(1)2 mo_d8v4659_0m_a.res created by SHELXL-2018/3 at 12:44:52 on 03-Feb-2021 CELL 0.71073 17.5997 17.5997 28.979 90 90 90 ZERR 8 0.0005 0.0005 0.0012 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.25+Z SYMM 0.5+Y,0.5-X,0.75+Z SYMM 0.5+X,0.5-Y,0.75-Z SYMM 0.5-X,0.5+Y,0.25-Z SYMM -X,-Y,0.5+Z SYMM +Y,+X,-Z SYMM -Y,-X,0.5-Z SFAC C H N O Y Yb UNIT 312 400 88 116 8 8 EQIV $1 1+Y,-1+X,1-Z EQIV $2 0.5-Y,-0.5+X,0.25+Z EQIV $3 0.5+Y,0.5-X,-0.25+Z EQIV $4 1.5-X,-0.5+Y,1.25-Z EQIV $5 +Y,+X,1-Z RIGU O10 > N11 RIGU O10A > N11A SADI O12A N11A O11A N11A O10A N11A O10 N11 O11 N11 O12 N11 DFIX 0.84 O13 H13b O13 H13a O13A H13d O13A H13c O16 H16e O16_$3 H16d_$4 O14 = H14A DANG 1.35 H14a H14a_$1 H16d_$4 H16d_$3 DANG 1.35 H16d H16e H13c H13d H13b H13a EADP Yb1 Y1A EADP Y2 Yb2A FLAT O4 O5 O6 N9 FLAT O4A O5 O6 N9 RIGU O4 O5 O6 N9 RIGU O4 O4A O6 N9 DANG 1.35 H15_$5 H15 DFIX 0.84 O15 H15 EXYZ Yb1 Y1A EXYZ Y2 Yb2A L.S. 16 PLAN 10 0 0 SIZE 0.122 0.141 0.282 TEMP -173.15 CONF HTAB O14 O8 HTAB O16 O14_$2 BIND H13a O13 HTAB BOND $H MORE -1 fmap 2 acta OMIT 1 1 1 OMIT 1 0 1 OMIT 0 1 1 OMIT 0 2 0 OMIT 1 2 0 OMIT 0 2 3 OMIT 1 2 1 OMIT 3 3 0 OMIT 0 4 1 OMIT 1 1 2 OMIT -1 2 1 REM REM REM WGHT 0.036900 6.265100 FVAR 0.20676 0.50422 0.43518 PART 1 YB1 6 0.857895 0.389150 0.603423 21.00000 0.01646 0.02327 = 0.01091 -0.00417 0.00369 -0.00494 PART 2 YB2A 6 0.946729 0.314637 0.507142 -21.00000 0.02712 0.01606 = 0.01170 0.00114 0.00665 -0.00001 Y1A 5 0.857895 0.389150 0.603423 -21.00000 0.01646 0.02327 = 0.01091 -0.00417 0.00369 -0.00494 PART 1 Y2 5 0.946729 0.314637 0.507142 21.00000 0.02712 0.01606 = 0.01170 0.00114 0.00665 -0.00001 PART 0 O1 4 0.824986 0.351906 0.530620 11.00000 0.02407 0.02329 = 0.01071 -0.00313 0.00354 -0.00334 O2 4 0.915532 0.276601 0.579865 11.00000 0.02774 0.02176 = 0.01364 0.00308 0.00517 0.00087 O3 4 0.958339 0.425101 0.553194 11.00000 0.02297 0.02129 = 0.02311 -0.00443 0.00901 -0.00694 PART 1 O4 4 0.821445 0.521193 0.546818 31.00000 0.03327 0.15811 = 0.03946 0.00383 0.00438 -0.02666 PART 2 O4A 4 0.776881 0.595582 0.578532 -31.00000 0.07003 0.04100 = 0.15027 0.02581 -0.03324 -0.02594 PART 0 O5 4 0.754949 0.467283 0.585627 11.00000 0.05038 0.03663 = 0.04398 -0.01854 -0.01443 0.01640 PART 1 O6 4 0.700952 0.540424 0.535978 11.00000 0.05452 0.05358 = 0.05555 0.00745 0.00864 0.02108 PART 0 O7 4 1.077025 0.310166 0.566487 11.00000 0.06254 0.03062 = 0.02405 -0.00312 0.00929 0.00602 O8 4 1.040448 0.218482 0.522670 11.00000 0.03008 0.02945 = 0.01930 0.00248 0.00251 0.00052 O9 4 1.131003 0.200022 0.571940 11.00000 0.06090 0.05985 = 0.05365 -0.00368 -0.02407 0.02808 N10 3 1.084627 0.242710 0.554378 11.00000 0.03898 0.03840 = 0.02241 0.00114 0.00182 0.01023 N1 3 0.747690 0.311324 0.615326 11.00000 0.02417 0.02140 = 0.01386 -0.00112 0.00313 -0.00540 N2 3 0.879251 0.373218 0.442373 11.00000 0.03846 0.02128 = 0.01405 0.00466 0.00651 0.00476 N3 3 0.928882 0.334264 0.667648 11.00000 0.01484 0.07245 = 0.01409 -0.00828 0.00046 0.00222 N4 3 0.888478 0.193408 0.495363 11.00000 0.03031 0.02073 = 0.02508 -0.00321 0.00834 -0.00204 N5 3 0.894710 0.511017 0.635484 11.00000 0.02540 0.03798 = 0.03367 -0.02113 0.01316 -0.01189 N6 3 1.058574 0.371459 0.472986 11.00000 0.02787 0.02468 = 0.01789 0.00286 0.01007 0.00360 N7 3 0.796193 0.414862 0.684503 11.00000 0.01826 0.04447 = 0.01490 -0.00818 0.00152 -0.00384 N8 3 0.982384 0.257584 0.424935 11.00000 0.03738 0.02736 = 0.01608 -0.00224 0.00817 0.00549 N9 3 0.750470 0.524189 0.561367 11.00000 0.03880 0.10079 = 0.03661 0.01893 0.00245 -0.02565 C1 1 0.756559 0.347260 0.512197 11.00000 0.02406 0.01813 = 0.01649 -0.00160 0.00138 -0.00335 C2 1 0.691989 0.325577 0.538123 11.00000 0.02616 0.02414 = 0.01276 -0.00437 -0.00055 -0.00576 C3 1 0.619932 0.326706 0.517738 11.00000 0.02549 0.02913 = 0.02232 -0.00691 -0.00228 -0.00918 AFIX 43 H3 2 0.577217 0.311910 0.535654 11.00000 -1.20000 AFIX 0 C4 1 0.608603 0.348863 0.471897 11.00000 0.03628 0.03021 = 0.01994 -0.00606 -0.01032 -0.00709 C5 1 0.672212 0.365671 0.446296 11.00000 0.04111 0.02161 = 0.01555 -0.00514 -0.00722 -0.00523 AFIX 43 H5 2 0.666022 0.379399 0.414815 11.00000 -1.20000 AFIX 0 C6 1 0.745920 0.363378 0.464768 11.00000 0.03357 0.01729 = 0.01238 -0.00300 0.00008 -0.00162 C7 1 0.529441 0.352038 0.452302 11.00000 0.03785 0.06618 = 0.02814 -0.00280 -0.01459 -0.01592 AFIX 137 H7A 2 0.496571 0.381090 0.473130 11.00000 -1.50000 H7B 2 0.509520 0.300324 0.449009 11.00000 -1.50000 H7C 2 0.530704 0.376766 0.422012 11.00000 -1.50000 AFIX 0 C8 1 0.693299 0.303161 0.586679 11.00000 0.02089 0.02280 = 0.02196 -0.00277 0.00448 -0.00848 AFIX 43 H8 2 0.648487 0.279832 0.598224 11.00000 -1.20000 AFIX 0 C9 1 0.807762 0.379412 0.433797 11.00000 0.04515 0.01591 = 0.01334 0.00073 0.00183 0.00146 AFIX 43 H9 2 0.794384 0.396413 0.403763 11.00000 -1.20000 AFIX 0 C10 1 0.920481 0.208625 0.598512 11.00000 0.01899 0.03049 = 0.02088 0.01218 0.00647 0.00213 C11 1 0.938916 0.200934 0.646091 11.00000 0.01791 0.05745 = 0.02500 0.01857 0.00400 0.00235 C12 1 0.948543 0.128750 0.665789 11.00000 0.02044 0.06913 = 0.04374 0.03973 0.00956 0.00770 AFIX 43 H12 2 0.962590 0.125328 0.697374 11.00000 -1.20000 AFIX 0 C13 1 0.938371 0.062410 0.640999 11.00000 0.02356 0.05406 = 0.07293 0.05163 0.01283 0.00552 C14 1 0.917880 0.069986 0.594779 11.00000 0.02335 0.03217 = 0.06198 0.02055 0.01761 0.00361 AFIX 43 H14 2 0.910305 0.025351 0.576928 11.00000 -1.20000 AFIX 0 C15 1 0.907955 0.141312 0.573483 11.00000 0.02539 0.02351 = 0.03748 0.01354 0.00988 0.00123 C16 1 0.948605 -0.015937 0.661544 11.00000 0.04280 0.06442 = 0.10861 0.06787 0.01726 0.01371 AFIX 137 H16A 2 0.968592 -0.011336 0.692984 11.00000 -1.50000 H16B 2 0.984362 -0.045091 0.642609 11.00000 -1.50000 H16C 2 0.899492 -0.042142 0.662350 11.00000 -1.50000 AFIX 0 C17 1 0.945643 0.265008 0.676275 11.00000 0.01281 0.07965 = 0.01630 0.01359 0.00241 0.00687 AFIX 43 H17 2 0.964847 0.254851 0.706285 11.00000 -1.20000 AFIX 0 C18 1 0.886754 0.138340 0.524598 11.00000 0.03244 0.01465 = 0.03933 -0.00080 0.00926 -0.00541 AFIX 43 H18 2 0.869907 0.090583 0.513250 11.00000 -1.20000 AFIX 0 C19 1 1.006163 0.483649 0.552219 11.00000 0.01515 0.02143 = 0.01827 0.00217 -0.00215 -0.00220 C20 1 0.995011 0.549086 0.580291 11.00000 0.01893 0.02122 = 0.02404 -0.00161 0.00258 -0.00316 C21 1 1.043953 0.611757 0.576817 11.00000 0.02057 0.02105 = 0.03090 -0.00233 -0.00419 -0.00143 AFIX 43 H21 2 1.033161 0.655525 0.594849 11.00000 -1.20000 AFIX 0 C22 1 1.107096 0.612970 0.548458 11.00000 0.02115 0.03137 = 0.02633 0.00556 -0.00127 -0.00956 C23 1 1.119620 0.549043 0.522584 11.00000 0.01408 0.03502 = 0.01977 0.00406 0.00013 -0.00301 AFIX 43 H23 2 1.163503 0.547532 0.503518 11.00000 -1.20000 AFIX 0 C24 1 1.071079 0.485455 0.522675 11.00000 0.01721 0.02555 = 0.01735 0.00654 0.00010 0.00251 C25 1 1.156358 0.682817 0.545874 11.00000 0.03320 0.04669 = 0.04505 -0.00865 0.01026 -0.02183 AFIX 137 H25A 2 1.198062 0.673962 0.524121 11.00000 -1.50000 H25B 2 1.177231 0.693908 0.576493 11.00000 -1.50000 H25C 2 1.125834 0.726028 0.535326 11.00000 -1.50000 AFIX 0 C26 1 0.938652 0.559285 0.616657 11.00000 0.02279 0.02642 = 0.03265 -0.01361 0.00307 -0.00425 AFIX 43 H26 2 0.934058 0.609705 0.628024 11.00000 -1.20000 AFIX 0 C27 1 1.094274 0.429834 0.488027 11.00000 0.02330 0.02595 = 0.02110 0.00753 0.00901 0.00190 AFIX 43 H27 2 1.142894 0.438164 0.474717 11.00000 -1.20000 AFIX 0 C28 1 0.731266 0.294807 0.664258 11.00000 0.02173 0.02926 = 0.01605 0.00499 0.00286 -0.00273 AFIX 23 H28A 2 0.773050 0.264793 0.678072 11.00000 -1.20000 H28B 2 0.683511 0.265443 0.667067 11.00000 -1.20000 AFIX 0 C29 1 0.723686 0.371304 0.688673 11.00000 0.02094 0.03792 = 0.01320 -0.00069 0.00451 -0.00473 AFIX 23 H29A 2 0.681649 0.400733 0.674678 11.00000 -1.20000 H29B 2 0.711613 0.363048 0.721661 11.00000 -1.20000 AFIX 0 C30 1 0.930950 0.386448 0.707730 11.00000 0.02244 0.10028 = 0.01605 -0.02151 -0.00229 -0.00285 AFIX 23 H30A 2 0.950952 0.436826 0.698598 11.00000 -1.20000 H30B 2 0.963343 0.365526 0.732602 11.00000 -1.20000 AFIX 0 C31 1 0.847843 0.392720 0.723751 11.00000 0.02046 0.07312 = 0.01522 -0.01509 0.00255 -0.00308 AFIX 23 H31A 2 0.831193 0.343299 0.736555 11.00000 -1.20000 H31B 2 0.844108 0.431186 0.748574 11.00000 -1.20000 AFIX 0 C32 1 0.851877 0.542098 0.675482 11.00000 0.04380 0.05816 = 0.04687 -0.03905 0.03021 -0.02771 AFIX 23 H32A 2 0.837798 0.595492 0.668967 11.00000 -1.20000 H32B 2 0.885117 0.541817 0.703041 11.00000 -1.20000 AFIX 0 C33 1 0.780437 0.496950 0.685843 11.00000 0.02872 0.04286 = 0.02985 -0.01936 0.01284 -0.00977 AFIX 23 H33A 2 0.761035 0.510999 0.716753 11.00000 -1.20000 H33B 2 0.740785 0.509498 0.662841 11.00000 -1.20000 AFIX 0 C34 1 0.929064 0.383705 0.401974 11.00000 0.04154 0.03669 = 0.01704 0.00796 0.01027 0.01069 AFIX 23 H34A 2 0.974648 0.413563 0.410450 11.00000 -1.20000 H34B 2 0.901721 0.410656 0.377005 11.00000 -1.20000 AFIX 0 C35 1 0.951378 0.304501 0.386566 11.00000 0.03804 0.04590 = 0.01157 0.00221 0.00664 0.00994 AFIX 23 H35A 2 0.906277 0.278738 0.373452 11.00000 -1.20000 H35B 2 0.990058 0.308445 0.361879 11.00000 -1.20000 AFIX 0 C36 1 0.876406 0.173352 0.446767 11.00000 0.04323 0.02896 = 0.02795 -0.01167 0.00736 -0.00591 AFIX 23 H36A 2 0.839469 0.208678 0.432499 11.00000 -1.20000 H36B 2 0.856098 0.121051 0.444314 11.00000 -1.20000 AFIX 0 C37 1 0.952460 0.178877 0.422399 11.00000 0.04483 0.02708 = 0.02903 -0.01214 0.01215 0.00354 AFIX 23 H37A 2 0.989033 0.143534 0.436994 11.00000 -1.20000 H37B 2 0.946458 0.163853 0.389680 11.00000 -1.20000 AFIX 0 C38 1 1.098340 0.335294 0.433099 11.00000 0.03866 0.03453 = 0.02269 0.00108 0.01803 0.00794 AFIX 23 H38A 2 1.153236 0.330867 0.440049 11.00000 -1.20000 H38B 2 1.092594 0.367750 0.405415 11.00000 -1.20000 AFIX 0 C39 1 1.065691 0.256428 0.423206 11.00000 0.03740 0.03348 = 0.01942 -0.00390 0.01083 0.00854 AFIX 23 H39A 2 1.082471 0.239341 0.392294 11.00000 -1.20000 H39B 2 1.085237 0.219837 0.446279 11.00000 -1.20000 AFIX 0 SAME 0.02 0.04 O7 > N10 PART 1 O10 4 0.546450 0.293796 0.707227 10.50000 0.06161 0.08554 = 0.10016 0.02702 0.00857 0.01299 O11 4 0.526008 0.263188 0.635571 10.50000 0.12042 0.08250 = 0.16335 -0.07096 0.11227 -0.06524 O12 4 0.502912 0.373584 0.658777 10.50000 0.16411 0.08498 = 0.11309 0.04186 0.06461 0.05492 N11 3 0.523554 0.308226 0.668795 10.50000 0.02675 0.03931 = 0.08147 0.00680 0.02449 -0.01025 SAME 0.02 0.04 O7 > N10 PART 2 O10A 4 0.425830 0.282625 0.549160 10.50000 0.15900 0.08586 = 0.06442 0.02148 -0.07618 -0.02463 O11A 4 0.511492 0.234956 0.590815 10.50000 0.04381 0.09812 = 0.12416 0.07991 0.02431 0.00946 O12A 4 0.432850 0.311053 0.620503 10.50000 0.20673 0.07332 = 0.08174 -0.02914 0.10130 -0.02083 N11A 3 0.455179 0.277082 0.587607 10.50000 0.03174 0.03825 = 0.02334 -0.00951 0.00462 -0.01829 PART 1 AFIX 1 O13 4 0.437800 0.264370 0.561150 10.50000 0.12649 0.05533 = 0.09394 -0.05811 0.01617 -0.01547 AFIX 1 H13A 2 0.435470 0.294050 0.589850 10.50000 -1.20000 AFIX 1 H13B 2 0.402240 0.305990 0.546630 10.50000 -1.20000 AFIX 1 PART 2 O13A 4 0.532020 0.302410 0.706160 10.50000 0.03574 0.06580 = 0.02684 0.02547 -0.01828 0.00615 AFIX 1 H13C 2 0.535730 0.347780 0.715580 10.50000 -1.20000 AFIX 1 H13D 2 0.521250 0.308890 0.677430 10.50000 -1.20000 AFIX 1 PART 0 O14 4 1.060260 0.060260 0.500000 10.50000 0.02481 0.02481 = 0.08614 -0.00269 0.00269 0.00220 AFIX 1 H14A 2 1.061250 0.100540 0.515750 11.00000 -1.20000 AFIX 0 O15 4 0.695528 0.695528 0.500000 10.50000 0.04290 0.04290 = 0.03600 0.00208 -0.00208 -0.01526 H15 2 0.697622 0.646633 0.505541 11.00000 -1.20000 AFIX 1 O16 4 0.550600 0.449400 0.750000 10.50000 0.05786 0.05786 = 0.04467 0.00560 0.00560 0.02925 AFIX 1 H16D 2 0.580320 0.456820 0.771350 10.50000 -1.20000 AFIX 1 H16E 2 0.517230 0.482770 0.750000 10.50000 -1.20000 AFIX 0 HKLF 4 REM mo_D8V4659_0m_a.res in P4(1)2(1)2 REM wR2 = 0.0710, GooF = S = 1.067, Restrained GooF = 1.094 for all data REM R1 = 0.0282 for 9841 Fo > 4sig(Fo) and 0.0341 for all 10688 data REM 635 parameters refined using 118 restraints END WGHT 0.0369 6.2770 REM Instructions for potential hydrogen bonds HTAB C8 O11 HTAB C8 O11A EQIV $7 y+1/2, -x+3/2, z-1/4 HTAB C9 O7_$7 EQIV $8 -y+3/2, x-1/2, z+1/4 HTAB C17 O6_$8 EQIV $9 -x+3/2, y+1/2, -z+5/4 HTAB C26 O11A_$9 EQIV $10 y+1, x, -z+1 HTAB C27 O10A_$10 HTAB C27 O13_$10 HTAB C28 O15_$8 EQIV $6 -y+1, -x+1, -z+3/2 HTAB C29 O10_$6 HTAB C30 N5 HTAB C30 O4_$8 HTAB C33 O10_$6 HTAB C33 O13A_$6 HTAB C33 O5 HTAB C34 N6 HTAB C34 O7_$7 HTAB C36 O12_$3 HTAB C36 O12A_$3 HTAB C37 O14 HTAB C39 O8 HTAB C39 O9_$1 HTAB O13 O11 HTAB O13A O16 HTAB O13A O12A HTAB O14 O8 HTAB O15 O6 HTAB O16 O10_$6 HTAB O16 O12_$6 HTAB O16 N11_$6 HTAB O16 O13A_$6 HTAB O16 O14_$2 REM Highest difference peak 1.463, deepest hole -0.582, 1-sigma level 0.093 Q1 1 0.7811 0.2348 0.3564 11.00000 0.05 1.46 Q2 1 0.2814 0.3012 0.5297 11.00000 0.05 0.98 Q3 1 1.2593 0.2593 0.5000 10.50000 0.05 0.83 Q4 1 0.3354 0.3525 0.5293 11.00000 0.05 0.67 Q5 1 0.3607 0.3184 0.5509 11.00000 0.05 0.57 Q6 1 0.5739 0.4418 0.7486 11.00000 0.05 0.54 Q7 1 0.5576 0.2373 0.6645 11.00000 0.05 0.41 Q8 1 0.8181 0.5648 0.5625 11.00000 0.05 0.37 Q9 1 0.4432 0.2994 0.6280 11.00000 0.05 0.36 Q10 1 0.3836 0.3225 0.6028 11.00000 0.05 0.35 ; _shelx_res_checksum 7834 _shelx_hkl_file ; 0 -1 0 2.90 0.90 -2 -1 0 1.70 3.40 1 -2 0 1.20 2.60 2 1 0 1.60 3.40 0 -2 0 78.19 5.30 0 2 0 67.89 6.30 -2 1 0 0.10 1.20 2 -1 0 1.10 2.10 1 2 0 4.10 4.40 -1 -2 0 -0.20 2.50 2 -3 0 373.56 19.30 -2 3 0 382.76 19.30 3 2 0 390.86 21.80 -3 -2 0 363.76 22.00 -1 3 0 1916.61 79.69 -1 3 0 1715.23 79.19 1 -3 0 1701.73 79.19 -3 -1 0 1723.13 79.79 3 1 0 1742.53 79.19 0 -3 0 2.10 3.50 0 3 0 2.50 5.00 -3 0 0 1.40 1.80 0 -3 0 -1.90 4.60 0 3 0 6.30 3.40 1 3 0 1969.90 88.49 -3 1 0 1869.01 85.59 -1 -3 0 1858.11 87.89 1 3 0 1951.10 86.29 -1 -3 0 1937.21 86.29 -3 2 0 316.07 16.70 2 3 0 312.47 20.90 -2 -3 0 320.37 20.90 3 -2 0 363.36 17.00 -2 -3 0 315.87 17.60 -3 -3 0 381.06 25.20 3 3 0 381.26 25.00 -3 3 0 433.66 21.10 3 -3 0 427.56 21.20 3 -4 0 473.15 24.60 -4 -3 0 491.85 28.90 4 3 0 474.65 28.10 -3 4 0 460.35 24.50 4 2 0 458.05 25.40 -4 -2 0 470.35 26.80 -2 4 0 478.45 24.00 2 -4 0 455.85 24.00 4 1 0 3797.92 167.38 -1 4 0 3742.33 167.98 -1 4 0 3716.63 168.88 -4 -1 0 3869.61 168.48 1 -4 0 3722.33 168.08 0 -4 0 4015.70 174.68 0 -4 0 3801.52 173.48 -4 0 0 3933.21 171.98 0 4 0 3824.82 173.38 -1 -4 0 3348.76 152.38 1 4 0 3480.65 154.98 -1 -4 0 3459.05 154.38 1 4 0 3349.96 152.28 2 4 0 289.17 22.00 -4 2 0 285.37 15.90 -2 -4 0 287.57 21.00 -2 -4 0 289.77 17.40 2 4 0 295.07 17.00 -3 -4 0 341.37 19.30 4 -3 0 333.17 18.60 3 4 0 337.27 24.50 -4 3 0 334.57 18.60 -3 -4 0 347.17 24.00 -4 -4 0 9718.53 440.56 4 4 0 9993.70 440.56 4 -4 0 9931.51 437.06 -4 -4 0 9769.82 437.46 -4 4 0 9999.00 436.96 4 -5 0 703.53 34.70 5 4 0 668.13 38.60 -4 5 0 685.43 34.40 -5 -4 0 676.13 39.50 5 3 0 5313.67 234.48 3 -5 0 5054.99 232.68 -5 -3 0 5316.77 235.78 -3 5 0 5209.48 232.58 -2 5 0 1031.70 50.09 5 2 0 1083.89 50.09 -5 -2 0 1031.40 51.79 -2 5 0 1065.79 49.70 2 -5 0 1027.80 49.80 1 -5 0 1174.98 56.19 -1 5 0 1191.48 56.09 -5 -1 0 1201.68 56.39 -1 5 0 1182.38 57.79 5 1 0 1237.98 54.49 0 5 0 8.50 5.70 0 5 0 13.10 9.20 0 -5 0 2.90 5.80 0 -5 0 7.80 7.10 -5 0 0 5.60 3.80 1 5 0 1285.17 64.09 1 5 0 1341.77 60.69 -1 -5 0 1308.37 62.89 -1 -5 0 1249.77 60.59 2 5 0 989.20 47.30 -5 2 0 1039.90 46.10 2 5 0 918.21 51.19 -2 -5 0 967.90 50.39 -2 -5 0 986.00 47.40 -3 -5 0 5006.00 225.08 -5 3 0 4969.60 220.78 -3 -5 0 4861.41 221.68 3 5 0 5053.59 225.78 5 -3 0 4934.31 220.78 4 5 0 533.85 35.00 -4 -5 0 565.14 34.60 -4 -5 0 537.55 30.00 5 -4 0 572.64 28.80 -5 4 0 566.04 28.80 -5 -5 0 6.10 11.30 -5 -5 0 4.50 7.20 5 -5 0 2.30 6.50 5 5 0 9.90 11.90 -5 5 0 -0.20 6.10 -6 -5 0 2716.83 126.99 -5 6 0 2624.94 121.49 5 -6 0 2722.43 121.89 -6 -5 0 2655.63 122.29 6 5 0 2627.04 125.59 -4 6 0 110.79 13.20 4 -6 0 111.69 13.60 6 4 0 95.89 13.90 -6 -4 0 104.49 15.20 -3 6 0 1363.96 62.89 6 3 0 1330.77 64.09 3 -6 0 1319.67 63.09 -6 -3 0 1359.96 66.39 -3 6 0 1288.27 62.79 -2 6 0 490.05 27.80 -2 6 0 492.55 26.30 6 2 0 462.35 25.50 2 -6 0 472.85 26.60 -6 -2 0 480.75 28.70 1 -6 0 2248.18 104.09 -1 6 0 2319.37 103.99 6 1 0 2282.37 101.19 -1 6 0 2248.38 105.99 -6 -1 0 2289.17 103.99 0 -6 0 291.17 19.00 -6 0 0 282.67 16.00 0 6 0 319.67 23.40 0 -6 0 316.37 21.00 0 6 0 282.77 18.20 1 6 0 2237.38 106.49 1 6 0 2257.67 102.59 -1 -6 0 2189.08 102.69 -1 -6 0 2286.57 104.99 -2 -6 0 496.25 30.40 2 6 0 454.45 26.20 2 6 0 466.35 32.00 -6 2 0 456.65 24.60 -2 -6 0 476.05 26.60 -6 3 0 1341.47 61.99 -3 -6 0 1334.57 67.39 -3 -6 0 1341.57 63.59 3 6 0 1304.37 68.59 4 6 0 84.59 16.50 -4 -6 0 121.49 17.50 -6 4 0 105.49 11.90 -4 -6 0 72.09 10.60 6 -4 0 114.99 12.10 -5 -6 0 2674.03 127.29 -5 -6 0 2650.53 122.89 -6 5 0 2757.52 121.79 5 6 0 2665.03 127.79 6 -5 0 2636.64 121.69 -6 -6 0 1999.60 95.19 6 -6 0 1936.61 88.79 -6 -6 0 1862.61 89.39 -6 6 0 1916.81 88.39 6 6 0 1812.22 94.09 6 -7 0 969.60 50.49 7 6 0 965.90 56.09 -7 -6 0 1057.59 51.69 -6 7 0 1036.10 50.49 -7 -6 0 1003.10 57.49 -7 -5 0 1663.43 82.59 7 5 0 1607.24 80.39 5 -7 0 1610.34 76.99 -5 7 0 1623.54 76.69 -7 -4 0 3317.27 153.48 -4 7 0 3319.77 148.89 -4 7 0 3195.28 148.59 4 -7 0 3374.86 149.39 7 4 0 3213.48 150.78 -7 -3 0 -2.60 10.20 -3 7 0 3.40 7.50 7 3 0 -2.50 7.70 3 -7 0 5.90 8.10 -3 7 0 16.90 8.40 2 -7 0 3350.16 153.78 7 2 0 3406.56 152.08 -7 -2 0 3521.65 155.58 -2 7 0 3391.86 153.58 -2 7 0 3308.67 155.18 -1 7 0 561.54 33.70 -1 7 0 534.35 29.70 1 -7 0 538.85 30.20 -7 -1 0 552.94 30.00 0 -7 0 5.00 7.40 0 7 0 5.30 6.70 -7 0 0 1.70 5.00 0 7 0 10.20 10.30 1 7 0 604.64 37.80 -1 -7 0 591.34 34.80 -1 -7 0 581.54 32.50 1 7 0 598.34 31.80 -2 -7 0 3290.47 153.48 -2 -7 0 3308.07 150.68 2 7 0 3320.57 155.48 2 7 0 3329.97 150.38 -7 2 0 3330.37 149.09 -7 3 0 1.40 6.00 3 7 0 -7.60 12.70 -3 -7 0 7.30 11.20 -3 -7 0 -4.60 7.60 3 7 0 -5.30 8.00 -4 -7 0 3455.65 160.28 4 7 0 3360.36 161.28 -4 -7 0 3384.46 155.88 -7 4 0 3497.45 154.38 -5 -7 0 1616.84 77.79 -5 -7 0 1618.44 82.59 -7 5 0 1631.44 76.09 5 7 0 1639.74 83.99 7 -5 0 1617.04 76.19 -6 -7 0 1105.29 54.49 -7 6 0 1098.09 52.59 7 -6 0 1054.09 52.89 6 7 0 1009.90 60.49 -6 -7 0 1065.59 60.19 -7 -7 0 -0.40 15.00 7 7 0 -3.50 16.00 -7 -7 0 -16.70 10.40 -7 7 0 5.50 9.30 7 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64.89 -3 -8 0 1368.86 69.09 -8 3 0 1325.87 62.59 3 8 0 1252.87 71.39 3 8 0 1364.96 64.89 -4 -8 0 1259.17 63.49 4 8 0 1334.07 71.39 -8 4 0 1273.07 61.59 -4 -8 0 1319.17 68.89 5 8 0 1680.13 88.99 -8 5 0 1690.63 80.09 -5 -8 0 1738.93 82.39 -5 -8 0 1718.13 87.59 -6 -8 0 66.59 13.00 8 -6 0 80.89 11.40 -6 -8 0 95.19 18.70 -8 6 0 90.89 11.80 6 8 0 65.89 18.90 7 8 0 50.59 19.30 8 -7 0 64.99 11.80 -8 7 0 64.09 11.60 -7 -8 0 40.40 17.60 -7 -8 0 70.79 13.90 8 8 0 5960.60 272.37 -8 -8 0 5867.11 273.27 8 -8 0 5884.21 265.97 -8 -8 0 5860.21 267.07 -8 8 0 5991.20 265.57 8 -9 0 10.70 11.40 -9 -8 0 0.50 13.30 -8 9 0 2.10 10.70 -9 -8 0 -7.90 17.40 9 8 0 2.30 17.00 -9 -7 0 1073.09 61.19 -7 9 0 966.20 51.59 9 7 0 1005.30 57.89 -9 -7 0 1007.60 53.49 -7 9 0 948.91 49.99 7 -9 0 1010.50 52.69 -6 9 0 323.17 22.80 -6 9 0 307.07 24.20 6 -9 0 283.37 24.80 -9 -6 0 317.17 25.60 -9 -6 0 280.37 32.70 9 6 0 281.27 28.80 5 -9 0 593.54 35.60 -5 9 0 598.74 35.00 -9 -5 0 608.64 42.20 -5 9 0 599.34 34.80 9 5 0 593.94 37.20 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103.39 -10 -14 0 1892.71 110.19 -14 10 0 1995.00 97.59 -11 -14 0 69.99 31.60 -14 11 0 113.09 14.90 -14 11 0 96.29 19.20 -11 -14 0 36.80 22.90 11 14 0 51.29 31.10 -12 -14 0 6.20 31.10 -14 12 0 37.40 18.20 -12 -14 0 11.20 22.90 -14 12 0 33.40 15.90 12 14 0 46.50 30.50 -13 -14 0 212.98 31.60 13 14 0 323.27 41.10 -13 -14 0 244.78 43.30 -14 13 0 303.87 33.30 -14 13 0 268.37 35.70 14 14 0 985.80 71.79 -14 14 0 917.31 59.09 -14 -14 0 993.70 65.49 -14 14 0 864.61 58.69 15 14 0 108.89 30.80 -14 15 0 116.49 26.30 -15 -14 0 87.29 27.50 14 -15 0 113.29 24.30 -14 15 0 93.59 24.00 -13 15 0 604.44 48.00 -15 -13 0 564.14 53.39 -13 15 0 618.94 49.99 13 -15 0 548.05 46.70 15 13 0 571.74 54.69 -12 15 0 453.15 45.70 15 12 0 470.25 48.50 -12 15 0 458.05 42.40 -15 -12 0 517.85 47.80 12 -15 0 540.85 44.50 11 -15 0 45.90 20.30 -15 -11 0 -45.40 29.50 -11 15 0 6.90 17.80 -15 -11 0 -9.40 21.70 15 11 0 -11.40 20.40 -11 15 0 26.30 22.70 -10 15 0 937.21 61.79 15 10 0 924.71 58.59 -15 -10 0 870.11 73.39 10 -15 0 1001.60 59.39 -10 15 0 913.61 57.49 -15 -10 0 883.51 60.29 15 9 0 135.59 22.50 -15 -9 0 134.09 24.30 -9 15 0 87.49 19.80 -9 15 0 141.19 26.50 9 -15 0 85.59 21.90 -15 -9 0 100.59 33.20 -15 -8 0 14.80 26.00 15 8 0 6.20 15.60 -8 15 0 43.00 18.10 -15 -8 0 36.00 18.80 8 -15 0 5.10 17.70 -8 15 0 66.19 22.90 -7 15 0 8.70 16.20 7 -15 0 4.50 18.60 -7 15 0 42.70 22.90 -15 -7 0 26.50 18.00 -15 -7 0 26.00 26.60 15 7 0 19.00 13.80 -6 15 0 432.56 39.30 -6 15 0 547.45 47.20 15 6 0 480.15 29.70 -15 -6 0 560.24 50.79 6 -15 0 550.74 43.10 -5 15 0 55.49 17.20 -15 -5 0 57.69 24.40 5 -15 0 65.19 20.70 -5 15 0 71.69 23.40 4 -15 0 1210.18 67.39 -4 15 0 1132.89 72.89 -15 -4 0 1219.58 72.89 -4 15 0 1156.68 65.29 -15 -3 0 -5.50 18.80 3 -15 0 -13.40 16.50 -3 15 0 -4.50 15.80 -3 15 0 9.50 23.40 -15 -2 0 654.13 50.29 -2 15 0 728.83 47.30 -2 15 0 685.73 56.59 2 -15 0 705.13 48.40 -15 -1 0 33.20 18.60 -1 15 0 70.69 26.10 1 -15 0 34.70 18.50 -1 15 0 42.60 17.80 0 15 0 -17.50 24.20 -15 0 0 -5.40 15.10 0 15 0 -6.50 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140.59 19.20 -11 -8 4 162.38 30.10 -7 11 -4 257.37 32.00 11 7 -4 231.08 28.70 -11 -7 -4 251.47 31.10 -7 11 -4 197.58 26.30 7 -11 -4 221.78 24.30 -11 -7 4 221.08 26.10 -7 11 4 198.48 23.30 -11 -7 4 145.79 27.00 7 -11 4 241.78 28.20 11 7 4 201.18 25.20 -11 -6 -4 871.51 58.49 11 6 -4 908.11 52.49 6 -11 -4 926.61 51.39 -6 11 -4 916.11 52.49 -6 11 -4 902.11 57.69 6 -11 4 960.30 54.09 -6 11 4 990.40 50.69 -11 -6 4 991.70 51.79 11 6 4 981.30 54.89 -11 -6 4 994.30 61.99 -5 11 -4 1564.44 77.49 11 5 -4 1596.44 75.79 -5 11 -4 1563.64 83.19 5 -11 -4 1615.14 76.19 -11 -5 -4 1582.74 82.79 11 5 4 1441.86 76.59 -11 -5 4 1479.55 83.39 5 -11 4 1488.85 78.29 -5 11 4 1527.35 75.39 -11 -5 4 1546.45 75.39 4 -11 -4 146.09 17.50 -4 11 -4 140.89 18.40 -4 11 -4 144.99 24.20 11 4 -4 121.19 17.60 -11 -4 -4 153.38 22.80 11 4 4 152.78 15.50 -4 11 4 182.48 24.40 -11 -4 4 146.89 23.30 -11 -4 4 173.98 20.40 4 -11 4 178.08 20.80 11 4 4 167.58 18.90 -4 11 4 170.48 21.60 -3 11 -4 987.80 53.59 -3 11 -4 1023.20 61.59 -11 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5 868.61 46.60 -4 -5 5 848.02 48.20 5 5 -5 75.19 14.40 5 5 -5 63.99 9.30 -5 5 -5 64.69 10.70 -5 5 -5 76.59 11.40 5 -5 -5 66.69 9.70 5 5 5 86.99 15.40 -5 5 5 79.29 9.40 -5 -5 5 84.39 10.60 -5 -5 5 100.39 17.20 5 -5 5 86.39 11.70 -5 6 -5 85.49 13.00 6 5 -5 100.29 15.30 5 -6 -5 83.69 11.20 -5 6 -5 77.19 11.20 -6 -5 5 72.79 10.50 6 5 5 49.40 13.60 -6 -5 5 49.70 14.70 5 -6 5 50.99 11.20 -5 6 5 51.99 7.70 4 -6 -5 1948.21 89.89 -4 6 -5 1937.51 91.89 6 4 -5 2024.10 93.49 -4 6 -5 1948.21 93.79 4 -6 5 1980.40 92.69 6 4 5 1937.31 94.59 -6 -4 5 2041.70 95.69 -6 -4 5 1895.81 90.59 -4 6 5 2010.60 89.89 3 -6 -5 2591.04 116.59 -3 6 -5 2593.54 118.29 -3 6 -5 2689.63 121.09 6 3 -5 2660.73 118.69 6 3 5 2541.05 119.79 -3 6 5 2562.74 116.59 -6 -3 5 2551.14 120.39 3 -6 5 2572.74 117.59 -6 -3 5 2521.45 116.59 3 -6 5 2508.75 118.69 -2 6 -5 1047.70 54.99 -2 6 -5 1097.79 58.49 6 2 -5 1086.29 54.19 2 -6 -5 1080.89 53.49 2 -6 5 1191.08 56.09 -6 -2 5 1164.78 56.29 6 2 5 1136.49 53.29 -2 6 5 1151.48 53.79 2 -6 5 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28.80 11 5 9 241.48 22.80 5 -11 9 215.88 30.60 -11 -5 9 233.58 24.60 4 -11 -9 1388.66 67.39 11 4 -9 1390.46 67.39 -4 11 -9 1475.85 71.69 -4 11 -9 1443.56 79.19 4 -11 9 1339.37 68.29 -11 -4 9 1304.07 66.39 11 4 9 1302.87 69.59 -11 -4 9 1313.87 74.69 4 -11 9 1290.67 72.19 11 4 9 1296.67 65.59 3 -11 -9 142.99 17.10 11 3 -9 166.88 18.30 -3 11 -9 204.78 30.60 -3 11 -9 143.79 19.80 3 -11 9 173.48 22.10 11 3 9 156.68 16.90 -11 -3 9 156.88 18.90 11 3 9 174.88 21.00 -11 -3 9 123.59 21.00 3 -11 9 172.48 24.70 11 2 -9 2075.79 99.29 2 -11 -9 2151.48 103.29 -2 11 -9 2255.57 105.89 -2 11 -9 2240.68 113.59 -11 -2 9 2162.38 100.19 -11 -2 9 2145.39 106.19 11 2 9 2196.48 99.89 2 -11 9 2223.18 107.69 2 -11 9 2221.88 106.99 11 2 9 2121.89 98.49 -1 11 -9 183.08 29.20 1 -11 -9 195.08 24.20 -1 11 -9 201.18 26.60 -11 -1 9 214.08 26.10 1 -11 9 220.48 24.40 1 -11 9 233.58 30.30 -11 -1 9 220.98 17.00 0 11 -9 3066.39 150.18 0 -11 -9 2951.80 140.49 0 11 -9 3090.29 141.99 0 11 9 3073.29 145.09 0 -11 9 3030.70 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539.55 54.79 -8 12 9 617.74 38.80 8 -12 9 611.64 46.60 12 8 9 568.74 48.10 -12 -8 9 581.84 42.40 -7 12 -9 7.50 17.20 -7 12 -9 38.10 22.80 7 -12 -9 15.70 12.80 12 7 -9 33.50 17.50 7 -12 9 23.40 19.10 -7 12 9 36.90 13.80 12 7 9 43.50 14.60 -12 -7 9 11.90 14.80 -12 -7 9 16.60 24.10 12 7 9 22.50 19.50 -6 12 -9 21.50 16.80 12 6 -9 33.50 15.60 6 -12 -9 40.60 13.40 -6 12 -9 48.50 24.50 -12 -6 9 32.00 22.00 12 6 9 39.30 18.00 6 -12 9 29.30 18.90 -12 -6 9 38.90 15.40 12 6 9 44.00 13.50 -5 12 -9 12.60 15.50 12 5 -9 18.40 13.30 -5 12 -9 0.30 22.10 5 -12 -9 25.60 13.00 12 5 9 7.40 14.70 5 -12 9 26.30 17.80 -12 -5 9 9.70 12.40 12 5 9 13.90 10.90 -12 -5 9 5.80 19.80 4 -12 -9 490.05 35.10 12 4 -9 476.85 32.60 -4 12 -9 477.05 38.50 -4 12 -9 463.55 47.90 -12 -4 9 522.75 33.80 -12 -4 9 588.14 44.80 12 4 9 593.24 31.70 12 4 9 556.74 35.00 4 -12 9 582.14 35.60 4 -12 9 571.44 42.20 3 -12 -9 1414.16 69.19 -3 12 -9 1474.75 82.49 12 3 -9 1386.26 65.19 -3 12 -9 1429.46 72.19 -12 -3 9 1313.17 66.49 3 -12 9 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680.33 44.10 -13 -5 10 734.73 55.39 -4 13 -10 650.13 57.29 13 4 -10 652.13 38.00 4 -13 -10 678.73 42.30 -4 13 -10 637.84 45.70 -13 -4 10 679.13 51.79 13 4 10 684.33 36.80 4 -13 10 739.03 42.70 -13 -4 10 685.23 40.40 4 -13 10 696.83 48.50 13 4 10 681.93 39.30 13 3 -10 24.20 8.80 -3 13 -10 -1.80 16.50 3 -13 -10 -0.70 13.40 -3 13 -10 24.50 26.10 -13 -3 10 24.50 11.70 3 -13 10 35.70 16.20 -13 -3 10 27.30 19.60 3 -13 10 7.90 17.90 13 3 10 19.10 7.80 13 3 10 27.40 7.00 2 -13 -10 518.55 37.10 -2 13 -10 516.35 52.89 -2 13 -10 520.75 40.10 2 -13 10 506.85 40.50 -13 -2 10 484.45 41.10 2 -13 10 533.35 41.50 -13 -2 10 536.35 31.30 1 -13 -10 212.68 27.10 -1 13 -10 211.38 34.90 -1 13 -10 235.48 27.90 -13 -1 10 205.88 19.00 1 -13 10 245.28 33.70 -1 13 10 224.58 29.60 -13 -1 10 214.78 30.10 1 -13 10 246.08 35.20 0 13 -10 2622.84 125.79 0 13 -10 2645.04 136.49 0 -13 -10 2625.64 124.39 0 -13 10 2664.03 130.69 0 13 10 2566.94 129.99 -13 0 10 2509.85 124.29 -13 0 10 2506.55 117.49 0 -13 10 2684.93 128.19 1 13 -10 198.18 33.40 -1 -13 -10 212.28 28.80 1 13 -10 203.18 23.90 -13 1 10 197.58 14.20 -1 -13 10 188.38 28.10 -1 -13 10 203.78 25.50 1 13 10 204.48 30.40 -13 1 10 210.68 14.60 -13 1 10 198.98 26.50 -2 -13 -10 565.24 39.90 2 13 -10 515.35 39.90 -13 2 -10 542.85 39.90 2 13 -10 502.85 51.79 -2 -13 10 524.25 40.60 -13 2 10 523.35 35.70 2 13 10 547.55 48.10 -2 -13 10 517.25 48.40 -13 3 -10 30.50 17.20 -3 -13 -10 -0.10 16.70 3 13 -10 -19.50 24.10 3 13 -10 24.20 16.40 -13 3 -10 33.10 12.20 3 13 10 -13.70 20.60 -3 -13 10 -10.10 21.90 -13 3 10 13.50 12.60 -3 -13 10 -4.60 16.50 -13 4 -10 783.32 48.90 -13 4 -10 790.62 42.40 4 13 -10 752.72 48.10 4 13 -10 795.02 61.79 -4 -13 -10 791.62 49.00 -4 -13 10 725.43 58.89 4 13 10 687.53 58.89 -13 4 10 738.53 43.50 -4 -13 10 796.92 51.89 5 13 -10 714.63 46.20 5 13 -10 748.13 59.89 -13 5 -10 662.33 39.50 -13 5 -10 653.63 46.30 -5 -13 -10 643.14 46.10 -5 -13 10 753.12 59.49 -13 5 10 672.93 40.00 -5 -13 10 727.83 49.50 5 13 10 715.83 58.09 -6 -13 -10 177.08 25.20 -13 6 -10 188.18 22.20 -13 6 -10 168.78 23.60 6 13 -10 184.88 34.10 6 13 -10 245.18 30.30 -13 6 10 172.78 21.80 -6 -13 10 145.49 31.70 -6 -13 10 145.29 25.30 6 13 10 169.78 34.30 7 13 -10 175.88 23.10 7 13 -10 158.88 32.00 -7 -13 -10 182.78 25.80 -13 7 -10 149.49 23.10 -13 7 -10 175.48 23.20 -13 7 10 188.98 14.00 -7 -13 10 197.48 26.80 7 13 10 201.18 36.30 -7 -13 10 158.48 33.50 -13 7 10 203.08 22.60 8 13 -10 105.19 20.50 -8 -13 -10 139.49 24.90 -13 8 -10 81.89 22.20 -13 8 -10 133.69 18.10 8 13 -10 86.79 29.90 -13 8 10 173.28 15.20 8 13 10 141.29 33.20 -8 -13 10 108.09 23.20 -8 -13 10 152.98 36.50 9 13 -10 328.47 48.80 -9 -13 -10 362.76 38.60 -13 9 -10 396.36 39.50 -13 9 -10 325.57 32.90 -9 -13 10 456.45 55.09 -13 9 10 438.06 25.60 9 13 10 424.86 52.59 -9 -13 10 435.06 41.90 -13 10 -10 433.06 37.90 -13 10 -10 441.76 42.60 10 13 -10 506.75 54.29 -10 -13 -10 455.95 44.10 10 13 10 471.25 55.39 -10 -13 10 508.65 59.89 -13 10 10 495.55 30.10 -10 -13 10 494.45 45.20 -11 -13 -10 770.52 54.69 -13 11 -10 766.52 54.29 11 13 -10 714.53 61.79 -13 11 -10 741.43 50.39 -13 11 10 668.33 41.30 -11 -13 10 814.82 69.79 11 13 10 684.43 65.29 -11 -13 10 750.22 54.99 -13 12 -10 394.86 42.20 12 13 -10 516.85 52.39 -12 -13 -10 502.35 47.70 -13 12 -10 448.16 45.60 -12 -13 10 424.06 56.69 12 13 10 386.66 54.09 -12 -13 10 356.26 45.30 -13 12 10 431.56 32.50 -13 -13 -10 326.87 43.60 13 13 -10 371.46 48.70 -13 13 -10 308.67 42.10 -13 13 -10 331.77 42.80 13 -13 -10 329.27 28.40 -13 -13 10 265.57 33.50 -13 13 10 312.77 30.90 -13 -13 10 260.67 44.40 13 13 10 417.36 55.19 -13 14 -10 110.19 28.30 -14 -13 -10 69.99 26.80 -13 14 -10 83.19 26.60 13 -14 -10 99.69 17.50 14 13 -10 115.49 31.30 -14 -13 10 96.79 27.00 14 13 10 116.59 32.00 -13 14 10 112.29 19.10 14 12 -10 89.19 28.00 12 -14 -10 74.69 16.80 -14 -12 -10 98.29 28.20 -12 14 -10 73.39 25.60 -12 14 -10 108.29 28.10 -14 -12 10 55.49 24.00 -14 -12 10 5.20 36.40 12 -14 10 75.69 26.60 14 12 10 51.79 26.90 14 11 -10 555.94 48.60 -11 14 -10 515.35 52.39 -11 14 -10 515.65 47.80 11 -14 -10 500.85 37.10 11 -14 10 494.85 49.20 -14 -11 10 438.26 46.30 -14 -11 10 533.55 68.19 14 11 10 498.05 51.69 14 10 -10 313.87 39.60 -10 14 -10 310.17 38.90 10 -14 -10 337.27 30.70 -10 14 -10 315.37 40.90 -14 -10 10 251.87 45.40 10 -14 10 288.27 42.00 -14 -10 10 259.17 31.20 14 10 10 274.37 34.80 -9 14 -10 29.90 20.70 9 -14 -10 26.10 15.40 -9 14 -10 40.30 27.90 14 9 -10 22.70 20.10 -14 -9 10 35.80 31.90 9 -14 10 28.90 22.00 14 9 10 26.90 21.30 -14 -9 10 36.20 19.60 14 9 10 28.50 17.10 -8 14 -10 119.29 23.70 -8 14 -10 147.39 32.60 8 -14 -10 114.89 18.50 14 8 -10 106.49 21.20 8 -14 10 67.49 24.00 -14 -8 10 85.29 21.50 14 8 10 159.28 25.20 14 8 10 128.29 19.00 -14 -8 10 94.79