#------------------------------------------------------------------------------ #$Date: 2021-07-17 08:39:27 +0300 (Sat, 17 Jul 2021) $ #$Revision: 267614 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/32/7243239.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_7243239 loop_ _publ_author_name 'Jacobs, Frederick J. F.' 'Venter, Gertruida J. S.' 'Fourie, Eleanor' 'Kroon, Robin E.' 'Brink, Alice' _publ_section_title ; Substitution reactivity and structural variability induced by tryptamine on the biomimetic rhenium tricarbonyl complex ; _journal_issue 39 _journal_name_full 'RSC Advances' _journal_page_first 24443 _journal_page_last 24455 _journal_paper_doi 10.1039/D1RA03750A _journal_volume 11 _journal_year 2021 _chemical_formula_moiety 'C39 H32 N2 O4 P1 Re1' _chemical_formula_sum 'C39 H32 N2 O4 P Re' _chemical_formula_weight 809.83 _chemical_name_common fac-[Re(CO)3(5Me-Sal-Trypt)(PPh3)] _chemical_name_systematic fac-Tricarbonyl-{2-[(2-Indol-3-yl-ethyl)liminomethyl)]-5-methylphenolato}-triphenylphosphine-rhenium(I) _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2020-02-06T12:17:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2021-01-20 deposited with the CCDC. 2021-07-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.455(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.5060(7) _cell_length_b 26.642(2) _cell_length_c 12.3068(8) _cell_measurement_reflns_used 9953 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.27 _cell_measurement_theta_min 2.38 _cell_volume 3303.6(4) _computing_cell_refinement 'SAINT-Plus (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'SAINT-Plus (Bruker, 2016)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 Venture 4K Kappa Photon III C28' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'I\mS 3.0 microfocus (Mo)' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 42725 _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 27.999 _diffrn_reflns_theta_min 1.887 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.771 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.4959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2016)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 1608 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Methanol' _exptl_crystal_size_max 0.239 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.027 _refine_diff_density_max 1.482 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 429 _refine_ls_number_reflns 7965 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.029 _refine_ls_R_factor_gt 0.0236 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+3.0572P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0566 _reflns_number_gt 7146 _reflns_number_total 7965 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL V1_20Ffj2_0m_a.res in P2(1)/n shelx.res created by SHELXL-2018/3 at 08:35:53 on 05-Feb-2020 CELL 0.71073 10.5060 26.6424 12.3068 90.000 106.455 90.000 ZERR 4.00 0.0007 0.0017 0.0008 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P RE UNIT 156 128 8 16 4 4 MERG 2 OMIT -4.00 56.00 EQIV $1 x, y, z EQIV $2 x+1/2, -y+1/2, z+1/2 EQIV $3 x-1, y, z HTAB C46 O4_$1 HTAB N2 O4_$2 HTAB C14 O1_$3 FMAP 2 PLAN 20 SIZE 0.027 0.137 0.239 ACTA BOND $H CONF LIST 4 L.S. 4 TEMP -173.15 WGHT 0.000000 3.057200 FVAR 0.22746 RE1 6 0.613828 0.354925 0.602538 11.00000 0.01780 0.01653 = 0.02187 0.00017 0.00988 0.00052 P1 5 0.495831 0.378944 0.745812 11.00000 0.01769 0.01713 = 0.02013 0.00094 0.00872 0.00037 O1 4 0.746012 0.338434 0.411514 11.00000 0.04430 0.03810 = 0.03908 -0.00225 0.02780 0.00111 O2 4 0.835806 0.300937 0.779368 11.00000 0.02588 0.03124 = 0.03647 0.00335 0.00800 0.00717 O3 4 0.779982 0.451478 0.660864 11.00000 0.03032 0.02844 = 0.04003 -0.00015 0.01073 -0.00938 O4 4 0.452113 0.387853 0.479873 11.00000 0.01983 0.02100 = 0.02854 0.00272 0.00891 0.00034 N1 3 0.498344 0.285857 0.562446 11.00000 0.02215 0.01768 = 0.02274 -0.00063 0.01050 -0.00087 N2 3 0.856392 0.116505 0.704721 11.00000 0.03445 0.03453 = 0.03996 0.00835 0.01605 0.00984 C1 1 0.697428 0.342699 0.483791 11.00000 0.02532 0.02173 = 0.02903 0.00090 0.01032 0.00027 C2 1 0.753164 0.321888 0.712481 11.00000 0.02312 0.02120 = 0.02625 -0.00125 0.01173 0.00125 C3 1 0.714940 0.416012 0.637857 11.00000 0.02402 0.02563 = 0.02346 0.00159 0.01044 0.00156 C11 1 0.374610 0.283105 0.506606 11.00000 0.02794 0.02166 = 0.02205 -0.00386 0.01176 -0.00563 AFIX 43 H11 2 0.337785 0.250303 0.494978 11.00000 -1.20000 AFIX 0 C12 1 0.286152 0.323310 0.460104 11.00000 0.02399 0.02378 = 0.02023 -0.00274 0.00561 -0.00290 C13 1 0.150434 0.312146 0.422784 11.00000 0.02890 0.03339 = 0.02811 -0.00022 0.00313 -0.00848 AFIX 43 H13 2 0.122369 0.278419 0.425988 11.00000 -1.20000 AFIX 0 C14 1 0.057147 0.348498 0.381828 11.00000 0.02148 0.04357 = 0.04314 0.00247 -0.00226 -0.00758 AFIX 43 H14 2 -0.034279 0.339809 0.358213 11.00000 -1.20000 AFIX 0 C15 1 0.095539 0.398362 0.374513 11.00000 0.02490 0.04037 = 0.03883 0.00253 0.00131 0.00327 C16 1 0.229570 0.410125 0.409160 11.00000 0.02622 0.02660 = 0.02954 0.00029 0.00385 0.00037 AFIX 43 H16 2 0.256024 0.443888 0.403431 11.00000 -1.20000 AFIX 0 C17 1 0.327165 0.373816 0.452325 11.00000 0.02221 0.02619 = 0.01680 -0.00150 0.00611 -0.00141 C18 1 -0.005445 0.439108 0.330926 11.00000 0.02707 0.04607 = 0.07756 0.00899 -0.00692 0.00469 AFIX 137 H18A 2 0.033138 0.471709 0.359285 11.00000 -1.50000 H18B 2 -0.083779 0.432898 0.357231 11.00000 -1.50000 H18C 2 -0.031388 0.439223 0.247907 11.00000 -1.50000 AFIX 0 C19 1 0.565182 0.237588 0.601862 11.00000 0.03205 0.01939 = 0.03389 0.00274 0.01578 0.00224 AFIX 23 H19A 2 0.497113 0.210885 0.590259 11.00000 -1.20000 H19B 2 0.609254 0.239966 0.684232 11.00000 -1.20000 AFIX 0 C20 1 0.668756 0.222248 0.541732 11.00000 0.04020 0.02593 = 0.03703 0.00467 0.02323 0.00723 AFIX 23 H20A 2 0.625524 0.218819 0.459422 11.00000 -1.20000 H20B 2 0.737623 0.248624 0.552741 11.00000 -1.20000 AFIX 0 C21 1 0.732102 0.173424 0.588164 11.00000 0.03640 0.02858 = 0.03455 0.00545 0.02139 0.00518 C22 1 0.828432 0.166885 0.687001 11.00000 0.03309 0.03035 = 0.04078 0.00010 0.01863 0.00313 AFIX 43 H22 2 0.870388 0.193098 0.736625 11.00000 -1.20000 AFIX 0 C23 1 0.773685 0.089611 0.617680 11.00000 0.02969 0.03119 = 0.03917 0.00987 0.02077 0.00938 C24 1 0.694060 0.124701 0.541685 11.00000 0.03249 0.02457 = 0.03685 0.00607 0.02194 0.00666 C25 1 0.600753 0.107010 0.444613 11.00000 0.03529 0.03463 = 0.03344 0.00559 0.01770 0.00854 AFIX 43 H25 2 0.547371 0.129887 0.391755 11.00000 -1.20000 AFIX 0 C26 1 0.586754 0.055918 0.426119 11.00000 0.04138 0.03593 = 0.04669 -0.00307 0.02079 0.00055 AFIX 43 H26 2 0.523827 0.043493 0.360098 11.00000 -1.20000 AFIX 0 C27 1 0.665814 0.022240 0.505183 11.00000 0.04329 0.02436 = 0.06391 0.00454 0.02983 0.00214 AFIX 43 H27 2 0.653420 -0.012790 0.491940 11.00000 -1.20000 AFIX 0 C28 1 0.759489 0.038100 0.600037 11.00000 0.03425 0.02735 = 0.05337 0.01188 0.02608 0.00965 AFIX 43 H28 2 0.812912 0.014900 0.651987 11.00000 -1.20000 AFIX 0 C29 1 0.593166 0.369227 0.892764 11.00000 0.02298 0.01674 = 0.02144 -0.00012 0.00796 0.00260 C30 1 0.538460 0.349844 0.974790 11.00000 0.02485 0.02191 = 0.02585 0.00191 0.01180 0.00198 AFIX 43 H30 2 0.446993 0.341263 0.955096 11.00000 -1.20000 AFIX 0 C31 1 0.617194 0.343077 1.084899 11.00000 0.03388 0.02810 = 0.02416 0.00339 0.01216 0.00475 AFIX 43 H31 2 0.579774 0.329503 1.140323 11.00000 -1.20000 AFIX 0 C32 1 0.749788 0.355978 1.114404 11.00000 0.03380 0.02650 = 0.02214 0.00187 0.00717 0.00646 AFIX 43 H32 2 0.803622 0.350828 1.189807 11.00000 -1.20000 AFIX 0 C33 1 0.804647 0.376412 1.034442 11.00000 0.02361 0.02508 = 0.02705 -0.00145 0.00572 0.00160 AFIX 43 H33 2 0.895538 0.385884 1.055388 11.00000 -1.20000 AFIX 0 C34 1 0.726735 0.383051 0.923635 11.00000 0.02391 0.02142 = 0.02514 0.00076 0.01149 -0.00005 AFIX 43 H34 2 0.764421 0.397021 0.868778 11.00000 -1.20000 AFIX 0 C35 1 0.340975 0.345675 0.733942 11.00000 0.02243 0.02308 = 0.01947 -0.00018 0.01104 -0.00319 C36 1 0.218429 0.369255 0.694127 11.00000 0.02533 0.02512 = 0.03038 -0.00388 0.01077 -0.00074 AFIX 43 H36 2 0.213888 0.404205 0.678193 11.00000 -1.20000 AFIX 0 C37 1 0.102430 0.341347 0.677752 11.00000 0.02212 0.04083 = 0.03759 -0.01100 0.00954 -0.00239 AFIX 43 H37 2 0.018590 0.357210 0.649245 11.00000 -1.20000 AFIX 0 C38 1 0.108725 0.290705 0.702772 11.00000 0.03072 0.03498 = 0.04556 -0.01264 0.02125 -0.01357 AFIX 43 H38 2 0.029201 0.271942 0.691901 11.00000 -1.20000 AFIX 0 C39 1 0.230248 0.267219 0.743559 11.00000 0.03931 0.02362 = 0.03253 -0.00379 0.02021 -0.00907 AFIX 43 H39 2 0.234051 0.232498 0.761777 11.00000 -1.20000 AFIX 0 C40 1 0.346732 0.294292 0.757938 11.00000 0.02968 0.02191 = 0.02461 -0.00070 0.01280 -0.00249 AFIX 43 H40 2 0.430208 0.277940 0.784033 11.00000 -1.20000 AFIX 0 C41 1 0.449744 0.445021 0.744797 11.00000 0.01587 0.01929 = 0.02344 -0.00100 0.00753 -0.00030 C42 1 0.414479 0.465570 0.836385 11.00000 0.02224 0.02374 = 0.02668 0.00209 0.01099 0.00171 AFIX 43 H42 2 0.416189 0.445296 0.900284 11.00000 -1.20000 AFIX 0 C43 1 0.376809 0.515678 0.834404 11.00000 0.02325 0.02606 = 0.02933 -0.00451 0.01136 0.00241 AFIX 43 H43 2 0.353469 0.529722 0.897092 11.00000 -1.20000 AFIX 0 C44 1 0.373426 0.545018 0.740853 11.00000 0.02328 0.01829 = 0.03220 -0.00192 0.00868 0.00285 AFIX 43 H44 2 0.347568 0.579234 0.739486 11.00000 -1.20000 AFIX 0 C45 1 0.407350 0.524918 0.649556 11.00000 0.02402 0.02256 = 0.02802 0.00444 0.00975 0.00067 AFIX 43 H45 2 0.404692 0.545285 0.585590 11.00000 -1.20000 AFIX 0 C46 1 0.445421 0.474890 0.651057 11.00000 0.02058 0.02122 = 0.02219 -0.00033 0.00827 -0.00036 AFIX 43 H46 2 0.468507 0.461080 0.588027 11.00000 -1.20000 AFIX 0 H2 2 0.910513 0.102454 0.769793 11.00000 0.08465 HKLF 4 REM V1_20Ffj2_0m_a.res in P2(1)/n REM wR2 = 0.0566, GooF = S = 1.066, Restrained GooF = 1.066 for all data REM R1 = 0.0236 for 7146 Fo > 4sig(Fo) and 0.0290 for all 7965 data REM 429 parameters refined using 0 restraints END WGHT 0.0000 3.0579 REM Highest difference peak 1.482, deepest hole -0.853, 1-sigma level 0.092 Q1 1 0.5496 0.3577 0.5474 11.00000 0.05 1.48 Q2 1 0.6839 0.3302 0.6623 11.00000 0.05 0.78 Q3 1 0.6093 0.4046 0.5960 11.00000 0.05 0.55 Q4 1 0.5379 0.3175 0.5411 11.00000 0.05 0.50 Q5 1 0.6910 0.3873 0.6598 11.00000 0.05 0.49 Q6 1 0.5490 0.3689 0.8188 11.00000 0.05 0.48 Q7 1 0.6312 0.3212 0.5253 11.00000 0.05 0.40 Q8 1 0.3461 0.3200 0.7190 11.00000 0.05 0.39 Q9 1 0.3083 0.3478 0.4573 11.00000 0.05 0.38 Q10 1 0.6336 0.3943 0.5426 11.00000 0.05 0.37 Q11 1 0.7467 0.3855 0.9809 11.00000 0.05 0.37 Q12 1 0.4136 0.4939 0.6572 11.00000 0.05 0.36 Q13 1 0.5150 0.3623 0.6584 11.00000 0.05 0.36 Q14 1 0.4188 0.4587 0.6850 11.00000 0.05 0.36 Q15 1 0.7857 0.2179 0.5426 11.00000 0.05 0.36 Q16 1 0.5949 0.3927 0.6848 11.00000 0.05 0.35 Q17 1 0.4143 0.3562 0.7255 11.00000 0.05 0.35 Q18 1 0.5780 0.5493 0.6263 11.00000 0.05 0.34 Q19 1 0.9550 0.1934 0.7667 11.00000 0.05 0.34 Q20 1 0.6831 0.2745 0.6128 11.00000 0.05 0.33 ; _cod_data_source_file d1ra03750a2.cif _cod_data_source_block v1_20ffj2_0m_a _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7243239 _iucr_refine_reflections_details ; 1 0 0 1.10 0.40 -1 0 0 0.80 0.50 2 0 0 343.47 22.80 -2 0 0 350.76 22.90 2 0 0 329.57 23.30 -2 0 0 326.87 23.30 3 0 0 0.30 0.80 -3 0 0 -0.70 0.80 3 0 0 1.30 1.40 -3 0 0 0.90 1.00 -4 0 0 1527.25 100.69 -4 0 0 1369.16 100.09 4 0 0 1540.65 101.49 4 0 0 1607.04 100.39 5 0 0 1.50 1.40 5 0 0 -0.30 2.00 -5 0 0 1.00 1.80 6 0 0 561.24 38.30 -6 0 0 552.14 39.00 6 0 0 570.24 40.30 7 0 0 -1.10 2.40 7 0 0 0.20 1.60 8 0 0 1574.74 107.19 8 0 0 1543.85 104.39 9 0 0 3.50 7.30 9 0 0 1.40 2.20 10 0 0 415.66 33.00 10 0 0 408.36 29.40 11 0 0 4.30 4.90 11 0 0 1.00 3.20 12 0 0 99.89 9.90 13 0 0 -8.10 5.50 -1 -1 0 3255.87 238.28 1 1 0 3975.30 238.88 2 -1 0 3734.43 251.37 -2 -1 0 3695.93 251.97 -2 1 0 4261.87 251.57 -2 1 0 3559.74 251.37 3 -1 0 235.18 15.20 -3 -1 0 224.48 16.20 3 -1 0 223.48 16.20 -3 -1 0 224.58 15.70 3 1 0 245.88 15.60 -3 1 0 183.98 15.10 -3 1 0 212.08 15.40 3 1 0 227.48 16.20 4 -1 0 602.74 40.90 -4 -1 0 579.54 41.50 -4 -1 0 592.24 42.10 4 -1 0 591.34 42.20 -4 1 0 604.44 41.20 -4 1 0 692.13 41.00 4 1 0 557.44 42.00 4 1 0 634.54 41.20 5 -1 0 826.32 58.09 5 -1 0 856.81 56.49 -5 -1 0 803.82 57.19 5 1 0 841.02 58.09 -5 1 0 807.32 56.89 5 1 0 860.51 56.79 -5 1 0 888.01 56.39 -6 -1 0 918.51 68.59 6 -1 0 1052.19 67.89 6 -1 0 982.90 69.89 -6 1 0 1064.79 68.59 6 1 0 1061.09 68.19 6 1 0 967.40 69.79 -6 1 0 1026.20 67.69 7 -1 0 138.29 12.90 7 -1 0 135.69 10.50 7 1 0 131.39 12.60 7 1 0 136.29 10.80 8 -1 0 752.42 54.19 8 -1 0 764.32 51.39 8 1 0 758.22 51.59 8 1 0 734.73 53.99 9 -1 0 377.46 32.10 9 -1 0 371.86 26.80 9 1 0 381.76 36.20 9 1 0 383.46 27.20 10 -1 0 384.66 27.50 10 -1 0 348.77 30.60 10 1 0 396.96 27.80 10 1 0 393.66 31.00 11 -1 0 7.30 5.70 11 -1 0 7.30 3.20 11 1 0 7.40 5.70 11 1 0 8.30 4.10 12 -1 0 177.78 15.00 12 1 0 185.38 15.20 13 -1 0 135.39 16.80 13 1 0 126.99 15.00 13 1 0 144.99 16.90 -1 -2 0 375.76 26.10 -1 -2 0 378.06 25.90 1 -2 0 432.76 26.20 -1 -2 0 363.76 26.20 1 2 0 397.26 26.10 1 2 0 383.56 25.90 -2 -2 0 162.98 11.20 -2 -2 0 160.28 11.70 2 -2 0 158.28 11.00 -2 -2 0 168.28 12.00 2 -2 0 167.48 11.50 -2 2 0 146.69 11.10 2 2 0 160.88 11.90 2 2 0 164.28 11.60 -2 2 0 185.88 11.50 -3 -2 0 534.95 36.60 3 -2 0 569.24 35.90 3 -2 0 521.25 35.50 -3 -2 0 605.54 36.40 -3 2 0 475.45 35.70 3 2 0 520.75 36.60 -3 2 0 515.35 35.70 3 2 0 520.35 36.00 4 -2 0 210.58 14.50 -4 -2 0 214.38 15.40 4 -2 0 200.98 15.90 -4 -2 0 218.48 16.00 4 2 0 214.88 15.00 4 2 0 203.68 15.80 -4 2 0 201.08 14.70 5 -2 0 287.97 21.70 5 -2 0 282.17 19.90 -5 -2 0 318.27 21.90 -5 -2 0 280.57 21.00 5 2 0 285.07 20.50 -5 2 0 266.37 20.30 -5 2 0 307.97 20.20 5 2 0 281.67 21.60 6 -2 0 28.20 5.20 -6 -2 0 24.00 5.60 6 -2 0 22.20 3.00 6 2 0 23.90 5.10 -6 2 0 25.40 4.10 -6 2 0 27.50 3.10 7 -2 0 1925.21 128.69 7 -2 0 1924.11 131.29 7 2 0 1874.41 130.99 7 2 0 1917.11 129.19 -7 2 0 2021.60 128.69 8 -2 0 87.59 7.60 8 -2 0 90.09 10.30 8 2 0 84.59 8.30 8 2 0 94.29 10.40 9 -2 0 30.90 7.00 9 -2 0 37.00 4.90 9 2 0 27.20 10.40 9 2 0 29.80 4.90 10 -2 0 9.80 5.50 10 -2 0 6.70 3.10 10 2 0 7.00 4.60 10 2 0 9.80 3.30 11 -2 0 683.93 50.69 11 -2 0 650.03 46.20 11 2 0 638.24 46.80 11 2 0 720.93 50.89 12 -2 0 3.10 3.50 12 2 0 5.30 3.90 13 -2 0 0.90 4.90 13 2 0 1.10 5.20 13 2 0 8.60 5.40 0 -3 0 0.20 0.50 0 -3 0 0.10 0.40 0 -3 0 0.20 0.60 0 3 0 0.60 0.50 0 3 0 2.00 1.00 0 3 0 2.10 0.60 -1 -3 0 2388.56 154.18 -1 -3 0 2575.44 154.38 1 -3 0 2515.35 154.38 -1 -3 0 2159.28 154.28 1 3 0 2385.86 154.28 -1 3 0 2235.28 154.38 1 3 0 2210.58 154.28 1 3 0 2207.68 154.18 -2 -3 0 863.71 56.89 -2 -3 0 795.62 57.29 2 -3 0 906.71 57.29 -2 -3 0 896.51 57.59 2 3 0 848.62 57.29 -2 3 0 812.52 57.09 2 3 0 873.01 57.59 -3 -3 0 487.75 35.20 3 -3 0 494.35 34.60 -3 -3 0 506.25 34.90 -3 -3 0 509.35 34.20 3 -3 0 491.95 34.00 3 3 0 594.34 34.90 -3 3 0 485.55 34.10 3 3 0 493.55 35.20 -3 3 0 532.75 34.50 -4 -3 0 3.70 1.00 -4 -3 0 5.10 2.10 -4 -3 0 5.00 2.00 4 -3 0 3.10 1.00 4 3 0 1.70 1.80 -4 3 0 4.00 1.40 -4 3 0 6.40 1.60 4 3 0 5.70 1.80 -5 -3 0 506.85 35.00 5 -3 0 497.45 33.10 5 -3 0 498.85 35.10 -5 -3 0 503.45 33.00 -5 -3 0 494.85 34.30 -5 3 0 439.76 33.30 5 3 0 512.15 33.90 -5 3 0 470.35 33.40 5 3 0 489.15 34.90 -6 -3 0 679.13 47.50 6 -3 0 670.53 47.60 6 -3 0 661.13 45.20 -6 -3 0 640.74 46.60 -6 3 0 695.33 45.60 6 3 0 677.73 46.10 6 3 0 670.73 47.40 7 -3 0 434.16 31.10 7 -3 0 405.86 28.20 -7 3 0 416.06 28.40 7 3 0 389.26 28.90 7 3 0 399.96 30.60 8 -3 0 186.88 13.90 8 -3 0 182.28 16.90 8 3 0 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7.20 -7 -12 3 36.30 5.40 -7 12 3 36.10 3.90 7 12 -3 34.20 5.90 7 12 -3 36.40 6.20 -7 12 3 34.40 6.10 -6 -12 3 691.13 50.59 6 -12 -3 694.03 51.39 -6 -12 3 726.03 50.19 -6 -12 3 684.63 50.29 -6 12 3 735.33 48.60 6 12 -3 773.72 50.69 -6 12 3 759.12 51.09 6 12 -3 693.33 50.29 -5 -12 3 1.40 2.40 -5 -12 3 3.40 2.20 -5 -12 3 4.80 2.80 5 -12 -3 6.90 3.40 -5 12 3 3.60 3.00 5 12 -3 0.50 2.10 -5 12 3 3.90 1.60 5 12 -3 2.50 2.20 -4 -12 3 1021.60 69.69 -4 -12 3 949.90 69.39 4 -12 -3 1164.58 71.19 -4 -12 3 972.80 69.09 4 12 -3 924.81 69.19 4 12 -3 987.00 69.29 -4 12 3 1117.79 70.39 -4 12 3 1023.80 68.39 -3 -12 3 4.70 1.90 3 -12 -3 3.30 3.00 -3 -12 3 4.70 2.20 -3 -12 3 2.30 2.10 3 12 -3 3.00 2.50 -3 12 3 4.80 2.40 3 12 -3 1.10 1.60 -2 -12 3 502.55 32.90 2 -12 -3 453.85 34.20 -2 -12 3 475.65 33.60 2 -12 -3 455.35 34.40 -2 -12 3 434.96 33.20 2 12 -3 484.95 34.10 2 12 -3 481.05 33.10 -2 12 3 468.05 33.90 2 12 -3 505.95 34.30 1 -12 -3 144.69 13.50 -1 -12 3 157.78 12.90 -1 -12 3 167.68 12.90 -1 -12 3 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36.40 8.80 6 6 9 50.19 9.00 7 -6 9 -1.90 5.50 7 -6 9 5.20 3.50 7 6 9 -4.80 6.00 7 6 9 0.90 4.50 8 -6 9 35.90 9.20 8 -6 9 40.20 6.30 8 6 9 51.59 10.10 8 6 9 24.70 9.30 -13 -7 9 0.00 5.40 13 -7 -9 -6.60 5.10 -13 7 9 5.10 10.90 13 7 -9 -4.90 7.80 -13 7 9 2.70 5.30 13 7 -9 3.90 5.70 12 -7 -9 365.96 30.50 -12 -7 9 420.86 36.60 12 7 -9 316.77 29.90 -12 7 9 413.06 29.30 -12 7 9 331.57 31.90 12 7 -9 418.96 29.70 -11 -7 9 92.69 12.00 11 -7 -9 80.19 12.80 11 7 -9 95.89 12.30 -11 7 9 66.49 12.70 11 7 -9 78.29 9.60 -11 7 9 88.99 10.00 10 -7 -9 40.70 8.10 -10 -7 9 37.90 7.10 -10 7 9 23.70 8.30 -10 7 9 39.10 6.70 10 7 -9 43.10 6.60 10 7 -9 47.60 8.30 9 -7 -9 140.69 13.20 -9 -7 9 128.99 12.80 9 7 -9 146.49 11.70 9 7 -9 119.89 15.20 -8 -7 9 1181.98 82.49 8 7 -9 1151.48 82.89 -8 7 9 1263.47 82.39 -7 -7 9 1.50 3.10 -7 7 9 0.70 2.80 7 7 -9 1.50 3.10 6 -7 -9 18.80 5.90 -6 -7 9 13.50 3.90 -6 7 9 18.50 5.90 -6 7 9 15.20 4.20 -5 -7 9 24.40 4.60 5 -7 -9 28.20 5.00 -5 7 9 20.80 6.50 5 7 -9 25.00 5.10 -5 7 9 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9.80 6 -7 9 110.19 13.00 6 -7 9 103.89 10.00 -6 -7 -9 107.49 13.40 6 7 9 113.49 13.00 7 -7 9 51.79 6.80 7 -7 9 48.40 9.20 7 7 9 61.39 10.40 7 7 9 57.89 9.60 8 -7 9 46.20 6.40 8 -7 9 38.00 12.30 8 7 9 52.79 10.40 8 7 9 27.30 9.40 -13 -8 9 102.59 13.00 13 -8 -9 84.29 12.60 13 8 -9 97.49 12.40 12 -8 -9 32.40 8.10 -12 -8 9 27.90 6.80 -12 8 9 19.80 5.90 -12 8 9 23.30 9.90 12 8 -9 22.70 7.40 12 8 -9 20.90 6.30 -11 -8 9 104.29 12.40 11 -8 -9 116.49 12.90 11 8 -9 142.79 12.20 -11 8 9 78.59 14.20 11 8 -9 96.09 12.70 -11 8 9 139.09 12.40 10 -8 -9 942.11 62.99 -10 -8 9 939.91 62.59 10 8 -9 977.10 61.19 -10 8 9 762.42 63.69 -10 8 9 866.41 61.29 10 8 -9 776.12 62.09 -9 -8 9 260.57 20.60 9 8 -9 235.08 18.80 9 8 -9 262.17 21.00 -8 -8 9 5.40 3.50 8 8 -9 1.90 2.40 -8 8 9 7.10 3.20 8 8 -9 0.00 3.20 -8 8 9 -2.20 4.30 7 -8 -9 295.37 23.00 -7 -8 9 273.57 22.10 -7 8 9 287.37 22.20 6 -8 -9 632.54 45.80 -6 8 9 650.93 45.50 -5 -8 9 177.68 15.00 5 8 -9 171.68 15.20 -5 8 9 189.38 15.20 4 -8 -9 33.70 5.20 -4 -8 9 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9 79.59 9.00 -6 -8 -9 66.69 11.30 6 8 9 96.79 11.50 -7 -8 -9 -2.90 6.40 7 -8 9 11.90 5.90 7 -8 9 13.30 3.80 7 8 9 2.90 6.50 7 8 9 18.50 6.20 8 -8 9 157.58 13.80 8 -8 9 188.28 19.50 8 8 9 193.58 19.00 8 8 9 127.29 21.30 -12 -9 9 12.80 5.00 -12 -9 9 19.40 5.80 12 -9 -9 20.10 6.10 -12 9 9 13.10 8.90 12 9 -9 12.20 5.30 12 9 -9 11.00 7.30 -12 9 9 13.00 5.30 -11 -9 9 422.06 33.50 11 -9 -9 433.56 34.30 -11 9 9 458.25 33.00 11 9 -9 444.86 32.80 10 -9 -9 15.60 5.20 -10 -9 9 9.70 4.50 10 9 -9 10.70 3.90 10 9 -9 6.90 4.60 -10 9 9 1.40 6.70 -10 9 9 20.30 5.10 -9 -9 9 266.07 20.20 -9 9 9 270.17 21.90 9 9 -9 219.18 19.90 9 9 -9 220.88 18.10 -8 -9 9 51.99 8.00 8 9 -9 44.40 8.00 -8 9 9 60.79 8.30 -7 -9 9 417.76 30.30 7 -9 -9 361.86 30.60 -7 9 9 439.26 30.30 6 -9 -9 3.40 3.90 -6 -9 9 5.40 3.30 -6 9 9 2.40 2.80 5 -9 -9 1158.98 89.79 -5 -9 9 1378.06 89.99 5 9 -9 1345.07 90.49 -5 9 9 1399.36 90.29 4 -9 -9 222.58 17.00 -4 -9 9 224.08 17.10 4 9 -9 221.28 17.40 -4 9 9 210.78 17.10 -4 9 9 172.38 17.90 -3 -9 9 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214.28 20.50 7 9 9 167.68 19.80 7 9 9 213.58 20.20 8 -9 9 2.60 3.50 8 -9 9 13.40 7.10 8 9 9 5.60 7.10 8 9 9 5.30 16.20 12 -10 -9 -2.90 5.20 -12 -10 9 -3.10 4.60 -12 -10 9 -2.20 3.80 12 10 -9 0.80 5.20 -12 10 9 4.90 4.60 -12 10 9 1.00 17.50 12 10 -9 5.40 6.40 11 -10 -9 87.89 11.40 -11 -10 9 80.49 10.80 -11 10 9 68.69 13.30 -11 10 9 96.79 10.20 11 10 -9 91.49 12.00 11 10 -9 78.99 10.00 -10 -10 9 37.40 7.30 -10 10 9 49.60 7.30 10 10 -9 35.70 6.10 -10 10 9 36.40 9.00 10 10 -9 33.20 7.20 -9 -10 9 757.12 51.69 9 10 -9 684.43 49.70 9 10 -9 727.53 52.09 -9 10 9 629.94 53.09 -9 10 9 801.52 52.69 -8 -10 9 9.00 3.80 -8 10 9 -3.10 3.70 -8 10 9 9.90 4.10 -7 -10 9 296.57 24.10 7 -10 -9 326.77 25.60 -7 10 9 332.87 24.30 -7 10 9 297.97 30.60 -6 -10 9 217.58 17.80 6 -10 -9 217.08 18.40 -6 10 9 218.78 17.70 -5 -10 9 407.16 28.40 5 -10 -9 323.77 28.30 -5 10 9 429.76 28.70 5 10 -9 365.36 28.60 4 -10 -9 85.49 8.80 -4 -10 9 88.09 8.60 -4 10 9 75.99 8.60 4 10 -9 68.99 8.50 -4 10 9 80.59 10.40 -3 -10 9 978.90 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16.70 -6 13 14 187.98 17.60 -6 13 14 146.69 20.50 -5 -13 14 96.29 11.60 5 -13 -14 65.39 9.50 -5 -13 14 82.69 10.20 -5 13 14 66.09 13.90 -5 13 14 69.49 10.50 4 -13 -14 15.40 6.00 -4 -13 14 12.10 5.40 -4 -13 14 10.10 5.00 -4 13 14 -2.20 4.20 -4 13 14 0.50 8.50 3 -13 -14 183.88 17.50 -3 -13 14 220.08 19.30 -3 13 14 196.58 18.20 -3 13 14 152.68 19.80 -2 -13 14 152.28 14.80 2 -13 -14 136.89 15.50 -2 -13 14 186.18 17.60 -2 13 14 152.88 15.80 -1 -13 14 8.10 4.60 1 -13 -14 4.40 7.80 -1 13 14 17.40 8.40 -1 13 14 11.20 5.80 0 -13 14 7.70 5.20 0 13 14 -1.00 7.90 0 13 14 0.70 7.40 1 -13 14 43.80 7.20 1 -13 14 37.80 9.30 -1 -13 -14 31.90 11.60 1 13 14 63.99 10.60 1 13 14 44.70 9.70 -7 -14 14 9.80 5.10 -7 -14 14 14.60 5.70 7 14 -14 -2.30 7.90 -7 14 14 5.20 5.40 -7 14 14 20.40 11.90 -6 -14 14 0.10 4.40 -6 -14 14 2.20 3.90 -6 14 14 1.80 5.20 -6 14 14 -2.20 17.50 -5 -14 14 32.70 7.50 5 -14 -14 31.40 7.70 -5 -14 14 32.10 6.90 -5 14 14 12.50 10.00 -5 14 14 23.70 7.00 -4 -14 14 369.56 28.80 -4 -14 14 360.76 30.50 4 -14 -14 380.76 30.60 -4 14 14 361.86 32.30 -4 14 14 358.76 29.80 -3 -14 14 3.00 4.50 3 -14 -14 -5.50 6.30 -3 14 14 5.40 5.20 -3 14 14 -12.30 8.40 2 -14 -14 22.90 7.40 -2 -14 14 22.10 7.10 -2 -14 14 19.00 6.50 -2 14 14 21.00 8.70 -2 14 14 26.20 7.20 -1 -14 14 -4.00 4.40 -1 -14 14 -3.10 4.80 -1 14 14 -1.70 4.10 -1 14 14 -9.00 9.90 0 -14 14 261.17 21.20 0 -14 14 277.97 24.40 0 14 14 225.08 23.40 -1 -14 -14 -12.80 16.80 1 -14 14 6.00 5.20 1 14 14 1.60 8.50 1 14 14 6.00 8.10 -7 -15 14 66.29 11.60 -7 -15 14 72.59 10.90 -7 15 14 51.49 9.30 -6 -15 14 218.98 21.20 -6 -15 14 215.98 19.60 -6 15 14 211.48 23.90 -6 15 14 233.78 20.80 -5 -15 14 62.99 11.20 -5 -15 14 64.69 10.00 -5 15 14 76.89 13.90 -5 15 14 71.49 10.30 -4 -15 14 42.00 8.20 -4 -15 14 36.30 7.40 4 -15 -14 35.70 8.30 -4 15 14 48.30 8.90 -4 15 14 11.10 10.20 -3 -15 14 19.80 7.00 -3 -15 14 25.90 7.10 3 -15 -14 17.00 7.80 -3 15 14 25.80 6.90 -3 15 14 22.70 10.30 -2 -15 14 339.87 27.70 -2 15 14 334.17 27.30 -2 15 14 271.77 28.00 1 -15 -14 0.50 7.30 -1 -15 14 15.40 5.80 -1 -15 14 31.60 6.80 -1 15 14 13.40 5.60 -1 15 14 28.00 9.20 0 -15 14 32.90 7.10 0 -15 -14 16.20 11.30 0 -15 14 10.60 6.10 0 15 14 4.90 8.80 -6 -16 14 11.70 6.50 -6 -16 14 -0.90 4.60 -6 16 14 -17.60 13.80 -6 16 14 10.60 6.00 -5 -16 14 116.89 13.70 -5 -16 14 110.89 12.50 -5 16 14 119.79 13.80 -5 16 14 80.29 16.00 -4 -16 14 105.19 12.70 -4 -16 14 107.09 11.90 -4 16 14 101.09 12.90 -4 16 14 68.29 14.70 -3 -16 14 26.10 7.50 -3 -16 14 29.30 6.10 -3 16 14 17.70 10.20 -3 16 14 32.50 8.00 -2 -16 14 40.60 8.80 -2 16 14 36.30 8.70 -2 16 14 36.50 10.40 -1 -16 14 301.47 25.80 -1 -16 14 335.07 28.90 1 -16 -14 257.27 26.80 -1 16 14 285.37 27.00 0 -16 14 10.30 6.90 0 -16 14 5.70 4.90 0 16 14 11.50 10.10 -6 -17 14 -2.60 5.50 -6 -17 14 -4.10 4.40 -6 17 14 12.70 5.80 6 17 -14 3.70 12.20 -5 -17 14 206.58 19.20 -5 -17 14 182.58 16.80 -5 17 14 179.88 17.80 -5 17 14 122.39 20.00 -4 -17 14 -5.70 4.50 -4 -17 14 1.30 5.00 -4 17 14 3.80 5.10 -3 -17 14 344.97 29.20 -3 -17 14 359.56 27.20 -3 17 14 284.27 29.60 -3 17 14 357.36 28.80 -2 -17 14 17.90 6.20 -2 -17 14 18.20 6.40 -2 17 14 13.80 9.70 -2 17 14 18.90 7.50 -1 -17 14 12.10 6.10 -1 17 14 23.10 9.60 -5 -18 14 59.39 9.00 -5 -18 14 63.59 11.60 -5 18 14 76.69 12.10 -4 -18 14 180.08 18.40 -4 -18 14 182.98 16.70 -4 18 14 113.59 18.60 -4 18 14 192.68 18.20 -3 -18 14 12.50 6.40 -3 -18 14 26.20 6.70 -3 18 14 15.50 7.20 -2 -18 14 22.40 6.50 -2 -18 14 25.60 8.40 -2 18 14 11.70 10.50 -2 18 14 12.70 7.10 -9 0 15 138.39 15.30 -8 0 15 -0.60 4.80 -7 0 15 6.40 4.20 -6 0 15 -2.20 3.80 -5 0 15 361.06 28.90 -4 0 15 -1.10 4.10 -3 0 15 33.40 7.90 -2 0 15 4.60 4.20 -1 0 15 252.07 21.70 0 0 15 10.30 5.50 1 0 15 120.99 13.70 -9 -1 15 -2.10 4.80 -9 1 15 1.30 4.90 -8 -1 15 23.90 6.40 -8 1 15 37.60 7.80 -7 -1 15 403.46 32.90 -7 1 15 439.36 33.30 -6 -1 15 33.30 6.70 -6 1 15 33.70 7.30 -5 -1 15 25.80 6.60 -5 1 15 24.10 5.60 -4 -1 15 135.39 13.60 -4 1 15 124.99 13.60 -3 -1 15 145.39 15.20 -3 1 15 175.68 16.00 -2 -1 15 51.39 8.50 -2 1 15 35.30 8.40 -1 -1 15 16.10 6.10 -1 1 15 19.10 5.90 0 -1 15 92.89 12.10 0 1 15 101.89 12.80 1 -1 15 170.68 16.50 1 1 15 133.39 18.30 1 1 15 181.58 16.60 -9 -2 15 6.10 4.80 -9 2 15 19.70 6.10 -8 -2 15 364.86 29.50 -8 2 15 368.56 29.50 -7 -2 15 5.20 4.80 -7 2 15 9.00 5.70 -6 -2 15 401.66 31.10 -6 2 15 383.56 30.90 -5 -2 15 36.20 7.10 -5 2 15 33.50 6.80 -4 -2 15 96.59 11.30 -4 2 15 85.99 11.10 -3 -2 15 14.60 5.40 -3 2 15 18.50 5.60 -2 -2 15 94.99 11.50 -2 2 15 97.89 11.70 -1 -2 15 9.00 5.80 -1 2 15 19.10 5.30 0 -2 15 21.70 6.50 0 2 15 43.80 8.40 1 -2 15 16.50 6.00 1 2 15 -0.10 5.80 1 2 15 12.20 5.90 1 2 15 1.50 9.10 -8 -3 15 113.89 14.20 -8 3 15 162.98 15.20 -7 -3 15 117.89 13.20 -7 3 15 129.89 13.80 -6 -3 15 181.28 17.10 -6 3 15 179.18 17.20 -5 -3 15 -0.60 4.00 -5 3 15 -1.10 4.30 -4 -3 15 347.47 28.30 -4 3 15 360.56 28.60 -3 -3 15 2.90 4.20 -3 3 15 1.80 5.10 -2 -3 15 55.69 9.30 -2 3 15 59.49 9.00 -1 -3 15 6.10 4.80 -1 3 15 1.40 4.80 -1 3 15 15.20 9.30 0 -3 15 228.88 18.90 0 3 15 202.58 18.80 0 3 15 161.88 20.80 1 -3 15 35.90 8.10 1 -3 15 27.20 6.70 1 3 15 31.80 7.80 1 3 15 42.20 10.40 1 3 15 11.20 6.90 -8 -4 15 68.09 11.10 -8 4 15 59.09 9.80 -8 4 15 90.09 22.10 -7 -4 15 14.70 5.40 -7 4 15 13.10 5.40 -6 -4 15 28.70 6.90 -6 4 15 45.80 8.70 -5 -4 15 270.07 23.00 -5 4 15 280.57 23.30 -4 -4 15 26.30 6.10 -4 4 15 25.30 5.60 -3 -4 15 79.49 9.90 -3 4 15 62.49 16.70 -3 4 15 62.29 9.60 -2 -4 15 67.19 10.20 -2 4 15 67.19 12.40 -2 4 15 62.59 9.90 -1 -4 15 271.77 22.10 -1 4 15 212.08 24.90 -1 4 15 269.07 22.40 0 -4 15 7.00 5.70 0 4 15 2.20 4.60 0 4 15 -9.30 8.30 1 -4 15 115.29 12.90 1 -4 15 97.39 12.10 1 4 15 94.09 12.60 1 4 15 64.49 13.50 1 4 15 100.49 12.50 -8 -5 15 35.20 7.60 -8 5 15 47.80 23.00 -8 5 15 35.70 8.40 -7 -5 15 468.45 36.20 -7 5 15 475.25 36.40 -6 -5 15 9.60 5.10 -6 5 15 3.60 4.90 -6 5 15 10.00 10.90 -5 -5 15 16.10 4.50 -5 5 15 13.10 9.70 -5 5 15 11.20 4.50 -4 -5 15 13.80 5.20 -4 5 15 10.20 5.60 -4 5 15 -2.20 9.30 -3 -5 15 204.48 18.40 -3 5 15 192.18 22.60 -3 5 15 204.18 18.60 -2 -5 15 1.10 4.50 -2 5 15 17.90 9.00 -2 5 15 1.10 4.10 -1 -5 15 17.60 6.00 -1 5 15 18.80 6.00 -1 5 15 11.40 9.50 0 -5 15 30.00 7.60 0 -5 15 39.30 6.90 0 5 15 17.70 7.20 0 5 15 24.60 6.40 0 5 15 -6.20 8.60 1 -5 15 162.18 16.20 1 -5 15 168.58 16.00 1 5 15 156.48 18.60 1 5 15 143.59 16.30 1 5 15 157.98 15.80 -8 -6 15 193.98 18.40 -8 6 15 198.28 18.70 -7 -6 15 3.30 4.60 -7 6 15 10.10 10.80 -7 6 15 3.90 5.00 -6 -6 15 146.29 14.00 -6 6 15 137.99 14.40 -6 6 15 96.09 18.00 -5 -6 15 96.29 11.70 -5 6 15 113.09 12.40 -5 6 15 92.89 16.10 -4 -6 15 31.60 6.80 -4 6 15 32.40 10.10 -4 6 15 27.90 6.80 -3 -6 15 24.40 6.20 -3 6 15 27.80 6.80 -3 6 15 40.80 10.50 -2 -6 15 46.60 8.70 -2 6 15 40.60 15.30 -2 6 15 40.00 8.10 -1 -6 15 131.49 15.00 -1 -6 15 120.39 13.20 -1 6 15 127.89 14.00 0 -6 15 28.50 7.10 0 -6 15 35.10 7.60 0 6 15 29.70 9.80 0 6 15 23.40 6.90 0 6 15 33.20 9.10 1 -6 15 8.00 5.50 1 -6 15 15.60 6.20 1 6 15 12.10 6.60 1 6 15 15.70 6.80 -8 -7 15 207.48 19.30 -8 7 15 198.48 19.20 -7 -7 15 -1.50 3.70 -7 7 15 -4.20 4.50 -7 7 15 -4.10 9.40 -6 -7 15 102.09 11.90 -6 7 15 82.49 15.90 -6 7 15 112.69 12.60 -5 -7 15 5.70 4.00 -5 7 15 -0.50 4.80 -5 7 15 6.20 9.40 -4 -7 15 282.77 22.80 -4 7 15 241.38 26.40 -4 7 15 285.37 23.40 -3 -7 15 18.70 6.00 -3 7 15 25.70 6.10 -3 7 15 1.80 8.80 -2 -7 15 100.19 11.80 -2 7 15 95.19 11.90 -1 -7 15 12.60 5.40 -1 7 15 16.70 9.00 -1 7 15 16.10 6.00 0 -7 15 324.37 26.50 0 -7 15 340.57 26.00 0 7 15 273.27 25.80 0 7 15 286.47 25.60 1 -7 15 3.50 4.80 1 -7 15 -7.00 4.90 1 7 15 -7.10 9.30 1 7 15 5.50 7.40 1 7 15 -4.40 5.40 -8 -8 15 204.18 18.20 -8 8 15 171.38 18.10 -7 -8 15 9.50 5.30 -7 8 15 2.70 5.10 -7 8 15 -1.80 10.00 -6 -8 15 142.29 15.20 -6 8 15 174.48 31.40 -6 8 15 167.28 15.90 -5 -8 15 76.29 10.10 -5 8 15 74.49 13.70 -5 8 15 74.79 11.30 -4 -8 15 161.58 14.90 -4 8 15 161.98 15.60 -4 8 15 109.49 17.70 -3 -8 15 11.70 5.00 -3 8 15 10.00 9.00 -3 8 15 3.20 4.60 -2 -8 15 268.17 22.10 -2 -8 15 269.47 24.10 -2 8 15 236.08 22.20 -1 -8 15 131.69 13.10 -1 8 15 115.89 13.10 -1 8 15 92.99 15.80 0 -8 15 8.30 5.50 0 -8 15 0.10 8.10 0 8 15 6.10 5.40 0 8 15 3.00 7.80 0 8 15 -5.70 8.30 -7 -9 15 349.77 29.30 -7 9 15 380.56 29.80 -6 -9 15 5.90 3.80 -6 9 15 3.80 5.20 -6 9 15 -17.00 11.60 -5 -9 15 6.90 5.50 -5 9 15 1.40 4.70 -5 9 15 4.60 9.60 -4 -9 15 115.29 12.40 -4 9 15 81.39 14.80 -4 9 15 110.09 12.50 -3 -9 15 188.48 18.30 -3 -9 15 180.58 16.50 -3 9 15 169.88 16.70 -3 9 15 146.59 19.70 -2 -9 15 8.50 4.70 -2 -9 15 3.70 5.10 -2 9 15 -0.60 8.40 -2 9 15 6.10 4.90 -1 -9 15 38.50 8.30 -1 -9 15 38.30 8.60 -1 9 15 43.50 8.90 0 -9 15 79.99 10.60 0 9 15 36.50 10.10 0 9 15 39.90 11.40 0 9 15 69.09 10.40 -7 -10 15 18.60 6.20 -7 10 15 6.70 5.70 -6 -10 15 22.50 6.00 -6 10 15 22.40 12.20 -6 10 15 29.10 7.20 -5 -10 15 372.56 30.00 -5 -10 15 363.16 27.70 -5 10 15 264.67 31.40 -5 10 15 346.57 28.10 -4 -10 15 6.90 5.00 -4 -10 15 18.60 5.80 -4 10 15 1.50 5.00 -4 10 15 7.40 9.20 -3 -10 15 39.80 9.30 -3 -10 15 32.60 7.40 -3 10 15 18.20 11.10 -3 10 15 25.30 6.20 -2 -10 15 -1.50 4.60 -2 -10 15 3.70 5.50 -2 10 15 -1.10 4.60 -2 10 15 -5.80 8.90 -1 -10 15 248.98 21.50 -1 -10 15 232.48 20.40 -1 10 15 177.98 23.00 -1 10 15 235.48 21.40 0 -10 15 4.00 5.50 0 -10 15 7.90 5.60 0 10 15 19.30 7.10 0 10 15 11.20 10.30 -7 -11 15 46.50 8.70 -7 -11 15 41.40 9.50 -7 11 15 43.30 8.90 -6 -11 15 84.69 11.20 -6 -11 15 94.49 14.70 -6 11 15 94.99 12.10 -6 11 15 73.59 16.00 -5 -11 15 -1.70 4.30 -5 -11 15 5.60 4.90 -5 11 15 8.40 5.30 -4 -11 15 167.48 17.50 -4 -11 15 159.88 15.90 -4 11 15 123.99 19.00 -4 11 15 176.78 16.90 -3 -11 15 169.48 16.80 -3 -11 15 140.59 14.10 -3 11 15 101.69 17.50 -3 11 15 133.79 15.00 -2 -11 15 14.20 6.90 -2 -11 15 19.30 6.00 -2 11 15 17.10 9.90 -2 11 15 15.50 5.80 -1 -11 15 25.20 7.50 -1 -11 15 30.10 7.00 -1 11 15 18.90 9.90 -1 11 15 15.80 6.60 -6 -12 15 230.98 22.90 -6 -12 15 228.78 21.00 -6 12 15 248.68 22.00 -5 -12 15 3.50 5.00 -5 -12 15 -2.80 4.40 -5 12 15 -1.90 11.90 -5 12 15 8.30 6.00 -4 -12 15 75.99 12.40 -4 -12 15 60.79 9.10 -4 12 15 58.09 14.50 -4 12 15 63.49 10.40 -3 -12 15 7.00 5.30 -3 -12 15 0.50 4.30 -3 12 15 -18.90 9.40 -3 12 15 0.20 5.50 -2 -12 15 298.07 25.10 -2 -12 15 292.27 23.40 -2 12 15 224.68 25.90 -2 12 15 282.37 24.40 -1 -12 15 -4.20 4.80 -1 -12 15 -1.40 5.20 -1 12 15 4.60 5.10 -1 12 15 -10.10 8.70 -6 -13 15 71.59 12.90 -6 -13 15 100.69 11.90 -6 13 15 91.39 13.30 -5 -13 15 46.90 10.90 -5 -13 15 53.29 9.10 -5 13 15 37.40 13.70 -5 13 15 50.59 9.10 -4 -13 15 216.08 19.80 -4 -13 15 179.28 17.40 -4 13 15 137.79 28.90 -4 13 15 188.68 18.70 -3 -13 15 78.29 10.80 -3 -13 15 75.59 12.30 -3 13 15 74.59 11.30 -3 13 15 61.59 13.60 -2 -13 15 13.30 6.20 -2 -13 15 11.10 5.50 -2 13 15 19.40 10.10 -2 13 15 9.60 6.20 -4 -14 15 20.50 7.40 -4 -14 15 19.70 6.10 -4 14 15 32.00 7.90 -4 14 15 39.20 13.50 -3 -14 15 29.20 7.40 -3 -14 15 39.90 8.90 -3 14 15 30.60 8.10 -3 14 15 43.90 21.00 -6 0 16 422.76 33.70 -5 0 16 1.80 5.20 -4 0 16 114.19 13.10 -3 0 16 -2.30 4.00 -2 0 16 160.48 16.30 -1 0 16 1.90 5.60 -6 -1 16 22.20 6.70 -6 1 16 22.10 6.90 -5 -1 16 239.98 20.70 -5 1 16 205.88 20.30 -4 -1 16 114.09 13.00 -4 1 16 102.69 12.70 -3 -1 16 0.90 4.40 -3 1 16 3.70 5.20 -2 -1 16 44.10 8.80 -2 1 16 42.00 8.50 -1 -1 16 111.59 13.70 -1 1 16 119.69 14.20 -6 -2 16 -6.70 4.80 -6 2 16 8.30 5.40 -5 -2 16 34.40 7.90 -5 2 16 31.60 7.30 -4 -2 16 6.80 5.10 -4 2 16 9.60 6.00 -3 -2 16 207.98 19.50 -3 2 16 222.68 20.10 -2 -2 16 8.70 5.80 -2 2 16 10.60 5.50 -1 -2 16 1.10 5.10 -1 2 16 -2.00 5.30 -6 -3 16 17.80 5.80 -6 3 16 2.30 5.60 -5 -3 16 244.48 22.30 -5 3 16 264.67 22.70 -4 -3 16 23.10 6.30 -4 3 16 17.10 6.70 -3 -3 16 -1.90 4.50 -3 3 16 -0.10 5.30 -2 -3 16 -3.20 4.90 -2 3 16 0.20 11.10 -2 3 16 -7.50 4.70 -6 -4 16 215.88 20.30 -6 4 16 222.18 20.70 -5 -4 16 4.80 5.20 -5 4 16 -15.90 12.40 -5 4 16 10.00 5.70 -4 -4 16 83.49 11.30 -4 4 16 104.99 12.60 -4 4 16 86.99 22.40 -3 -4 16 46.60 9.30 -3 4 16 67.89 14.40 -3 4 16 56.49 9.80 -2 -4 16 54.29 9.10 -2 4 16 67.29 14.80 -2 4 16 38.60 8.60 -6 -5 16 35.30 8.20 -6 5 16 49.50 8.60 -5 -5 16 37.30 7.30 -5 5 16 47.20 8.80 -5 5 16 29.70 14.00 -4 -5 16 210.98 19.50 -4 5 16 206.28 19.60 -3 -5 16 3.50 5.20 -3 5 16 3.50 5.10 -3 5 16 27.50 11.20 -2 -5 16 66.79 10.40 -2 5 16 57.29 9.80 -2 5 16 48.50 13.70 -5 -6 16 18.00 6.30 -5 6 16 13.10 6.30 -5 6 16 4.00 12.00 -4 -6 16 8.00 5.80 -4 6 16 5.50 16.10 -4 6 16 6.60 5.80 -3 -6 16 95.49 12.80 -3 6 16 133.69 13.90 -3 6 16 70.29 15.10 -2 -6 16 89.19 11.80 -2 6 16 82.49 12.10 -2 6 16 64.99 14.50 -5 -7 16 225.38 19.30 -5 7 16 195.68 29.70 -5 7 16 170.38 19.10 -4 -7 16 17.20 6.40 -4 7 16 20.80 7.20 -4 7 16 21.20 12.30 -3 -7 16 -1.60 4.70 -3 7 16 6.10 12.30 -3 7 16 -5.00 4.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Re1 0.61383(2) 0.35493(2) 0.60254(2) 0.01786(4) Uani d 1 . . Re P1 0.49583(6) 0.37894(2) 0.74581(6) 0.01763(13) Uani d 1 . . P O1 0.7460(2) 0.33843(8) 0.4115(2) 0.0372(5) Uani d 1 . . O O2 0.8358(2) 0.30094(7) 0.77937(19) 0.0314(5) Uani d 1 . . O O3 0.7800(2) 0.45148(7) 0.66086(19) 0.0328(5) Uani d 1 . . O O4 0.45211(17) 0.38785(6) 0.47987(17) 0.0227(4) Uani d 1 . . O N1 0.4983(2) 0.28586(8) 0.56245(19) 0.0200(4) Uani d 1 . . N N2 0.8564(3) 0.11650(10) 0.7047(3) 0.0352(6) Uani d 1 . . N C1 0.6974(3) 0.34270(10) 0.4838(3) 0.0248(6) Uani d 1 . . C C2 0.7532(3) 0.32189(9) 0.7125(2) 0.0225(5) Uani d 1 . . C C3 0.7149(3) 0.41601(10) 0.6379(2) 0.0236(5) Uani d 1 . . C C11 0.3746(3) 0.28310(10) 0.5066(2) 0.0229(5) Uani d 1 . . C H11 0.337785 0.250303 0.494978 0.028 Uiso calc 1 . . H C12 0.2862(3) 0.32331(10) 0.4601(2) 0.0228(5) Uani d 1 . . C C13 0.1504(3) 0.31215(11) 0.4228(3) 0.0311(6) Uani d 1 . . C H13 0.122369 0.278419 0.425988 0.037 Uiso calc 1 . . H C14 0.0571(3) 0.34850(12) 0.3818(3) 0.0384(8) Uani d 1 . . C H14 -0.034279 0.339809 0.358213 0.046 Uiso calc 1 . . H C15 0.0955(3) 0.39836(12) 0.3745(3) 0.0363(7) Uani d 1 . . C C16 0.2296(3) 0.41012(11) 0.4092(3) 0.0283(6) Uani d 1 . . C H16 0.256024 0.443888 0.403431 0.034 Uiso calc 1 . . H C17 0.3272(3) 0.37382(10) 0.4523(2) 0.0216(5) Uani d 1 . . C C18 -0.0054(3) 0.43911(14) 0.3309(4) 0.0547(11) Uani d 1 . . C H18A 0.033138 0.471709 0.359285 0.082 Uiso calc 1 . . H H18B -0.083779 0.432898 0.357231 0.082 Uiso calc 1 . . H H18C -0.031388 0.439223 0.247907 0.082 Uiso calc 1 . . H C19 0.5652(3) 0.23759(10) 0.6019(3) 0.0271(6) Uani d 1 . . C H19A 0.497113 0.210885 0.590259 0.033 Uiso calc 1 . . H H19B 0.609254 0.239966 0.684232 0.033 Uiso calc 1 . . H C20 0.6688(3) 0.22225(11) 0.5417(3) 0.0319(7) Uani d 1 . . C H20A 0.625524 0.218819 0.459422 0.038 Uiso calc 1 . . H H20B 0.737623 0.248624 0.552741 0.038 Uiso calc 1 . . H C21 0.7321(3) 0.17342(11) 0.5882(3) 0.0308(6) Uani d 1 . . C C22 0.8284(3) 0.16688(11) 0.6870(3) 0.0331(7) Uani d 1 . . C H22 0.870388 0.193098 0.736625 0.04 Uiso calc 1 . . H C23 0.7737(3) 0.08961(11) 0.6177(3) 0.0311(6) Uani d 1 . . C C24 0.6941(3) 0.12470(10) 0.5417(3) 0.0288(6) Uani d 1 . . C C25 0.6008(3) 0.10701(11) 0.4446(3) 0.0328(7) Uani d 1 . . C H25 0.547371 0.129887 0.391755 0.039 Uiso calc 1 . . H C26 0.5868(3) 0.05592(12) 0.4261(3) 0.0396(8) Uani d 1 . . C H26 0.523827 0.043493 0.360098 0.048 Uiso calc 1 . . H C27 0.6658(3) 0.02224(12) 0.5052(3) 0.0408(8) Uani d 1 . . C H27 0.65342 -0.01279 0.49194 0.049 Uiso calc 1 . . H C28 0.7595(3) 0.03810(11) 0.6000(3) 0.0355(7) Uani d 1 . . C H28 0.812912 0.0149 0.651987 0.043 Uiso calc 1 . . H C29 0.5932(3) 0.36923(9) 0.8928(2) 0.0200(5) Uani d 1 . . C C30 0.5385(3) 0.34984(9) 0.9748(2) 0.0233(5) Uani d 1 . . C H30 0.446993 0.341263 0.955096 0.028 Uiso calc 1 . . H C31 0.6172(3) 0.34308(11) 1.0849(2) 0.0279(6) Uani d 1 . . C H31 0.579774 0.329503 1.140323 0.033 Uiso calc 1 . . H C32 0.7498(3) 0.35598(10) 1.1144(3) 0.0276(6) Uani d 1 . . C H32 0.803622 0.350828 1.189807 0.033 Uiso calc 1 . . H C33 0.8046(3) 0.37641(10) 1.0344(2) 0.0255(6) Uani d 1 . . C H33 0.895538 0.385884 1.055388 0.031 Uiso calc 1 . . H C34 0.7267(3) 0.38305(9) 0.9236(2) 0.0226(5) Uani d 1 . . C H34 0.764421 0.397021 0.868778 0.027 Uiso calc 1 . . H C35 0.3410(3) 0.34568(9) 0.7339(2) 0.0206(5) Uani d 1 . . C C36 0.2184(3) 0.36925(10) 0.6941(3) 0.0264(6) Uani d 1 . . C H36 0.213888 0.404205 0.678193 0.032 Uiso calc 1 . . H C37 0.1024(3) 0.34135(12) 0.6778(3) 0.0333(7) Uani d 1 . . C H37 0.01859 0.35721 0.649245 0.04 Uiso calc 1 . . H C38 0.1087(3) 0.29071(11) 0.7028(3) 0.0349(7) Uani d 1 . . C H38 0.029201 0.271942 0.691901 0.042 Uiso calc 1 . . H C39 0.2302(3) 0.26722(10) 0.7436(3) 0.0298(6) Uani d 1 . . C H39 0.234051 0.232498 0.761777 0.036 Uiso calc 1 . . H C40 0.3467(3) 0.29429(10) 0.7579(2) 0.0243(5) Uani d 1 . . C H40 0.430208 0.27794 0.784033 0.029 Uiso calc 1 . . H C41 0.4497(2) 0.44502(9) 0.7448(2) 0.0191(5) Uani d 1 . . C C42 0.4145(3) 0.46557(10) 0.8364(2) 0.0234(5) Uani d 1 . . C H42 0.416189 0.445296 0.900284 0.028 Uiso calc 1 . . H C43 0.3768(3) 0.51568(10) 0.8344(3) 0.0254(6) Uani d 1 . . C H43 0.353469 0.529722 0.897092 0.03 Uiso calc 1 . . H C44 0.3734(3) 0.54502(10) 0.7409(2) 0.0244(6) Uani d 1 . . C H44 0.347568 0.579234 0.739486 0.029 Uiso calc 1 . . H C45 0.4073(3) 0.52492(10) 0.6496(2) 0.0244(5) Uani d 1 . . C H45 0.404692 0.545285 0.58559 0.029 Uiso calc 1 . . H C46 0.4454(2) 0.47489(9) 0.6511(2) 0.0209(5) Uani d 1 . . C H46 0.468507 0.46108 0.588027 0.025 Uiso calc 1 . . H H2 0.911(5) 0.1025(18) 0.770(4) 0.085(16) Uiso d 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re1 0.01780(6) 0.01653(5) 0.02187(6) 0.00052(4) 0.00988(4) 0.00017(4) P1 0.0177(3) 0.0171(3) 0.0201(3) 0.0004(2) 0.0087(3) 0.0009(2) O1 0.0443(13) 0.0381(11) 0.0391(13) 0.0011(10) 0.0278(11) -0.0022(10) O2 0.0259(10) 0.0312(10) 0.0365(12) 0.0072(8) 0.0080(9) 0.0033(9) O3 0.0303(11) 0.0284(10) 0.0400(13) -0.0094(9) 0.0107(10) -0.0001(9) O4 0.0198(9) 0.0210(9) 0.0285(10) 0.0003(7) 0.0089(8) 0.0027(7) N1 0.0222(11) 0.0177(10) 0.0227(11) -0.0009(8) 0.0105(9) -0.0006(8) N2 0.0344(14) 0.0345(14) 0.0400(16) 0.0098(11) 0.0160(13) 0.0084(12) C1 0.0253(14) 0.0217(12) 0.0290(15) 0.0003(10) 0.0103(12) 0.0009(10) C2 0.0231(13) 0.0212(12) 0.0263(14) 0.0012(10) 0.0117(11) -0.0013(10) C3 0.0240(13) 0.0256(13) 0.0235(14) 0.0016(11) 0.0104(11) 0.0016(10) C11 0.0279(14) 0.0217(12) 0.0221(13) -0.0056(10) 0.0118(11) -0.0039(10) C12 0.0240(13) 0.0238(13) 0.0202(13) -0.0029(10) 0.0056(11) -0.0027(10) C13 0.0289(15) 0.0334(15) 0.0281(15) -0.0085(12) 0.0031(12) -0.0002(12) C14 0.0215(15) 0.0436(18) 0.043(2) -0.0076(13) -0.0023(14) 0.0025(14) C15 0.0249(15) 0.0404(17) 0.0388(18) 0.0033(13) 0.0013(13) 0.0025(14) C16 0.0262(14) 0.0266(14) 0.0295(15) 0.0004(11) 0.0039(12) 0.0003(11) C17 0.0222(13) 0.0262(13) 0.0168(12) -0.0014(10) 0.0061(10) -0.0015(10) C18 0.0271(17) 0.046(2) 0.078(3) 0.0047(15) -0.0069(18) 0.0090(19) C19 0.0321(15) 0.0194(12) 0.0339(16) 0.0022(11) 0.0158(13) 0.0027(11) C20 0.0402(17) 0.0259(14) 0.0370(17) 0.0072(12) 0.0232(14) 0.0047(12) C21 0.0364(16) 0.0286(14) 0.0345(17) 0.0052(12) 0.0214(14) 0.0055(12) C22 0.0331(16) 0.0303(15) 0.0408(18) 0.0031(12) 0.0186(14) 0.0001(13) C23 0.0297(15) 0.0312(15) 0.0392(18) 0.0094(12) 0.0208(14) 0.0099(13) C24 0.0325(15) 0.0246(13) 0.0369(17) 0.0067(11) 0.0219(13) 0.0061(12) C25 0.0353(16) 0.0346(15) 0.0334(17) 0.0085(13) 0.0177(14) 0.0056(13) C26 0.0414(18) 0.0359(17) 0.047(2) 0.0005(14) 0.0208(16) -0.0031(14) C27 0.0433(19) 0.0244(14) 0.064(2) 0.0021(13) 0.0298(18) 0.0045(14) C28 0.0342(16) 0.0273(14) 0.053(2) 0.0096(12) 0.0261(16) 0.0119(14) C29 0.0230(13) 0.0167(11) 0.0214(13) 0.0026(9) 0.0080(11) -0.0001(9) C30 0.0249(13) 0.0219(12) 0.0259(14) 0.0020(10) 0.0118(11) 0.0019(10) C31 0.0339(16) 0.0281(14) 0.0242(15) 0.0048(11) 0.0122(13) 0.0034(11) C32 0.0338(16) 0.0265(14) 0.0221(14) 0.0065(11) 0.0072(12) 0.0019(11) C33 0.0236(13) 0.0251(13) 0.0271(15) 0.0016(11) 0.0057(11) -0.0015(11) C34 0.0239(13) 0.0214(12) 0.0251(14) 0.0000(10) 0.0115(11) 0.0008(10) C35 0.0224(13) 0.0231(12) 0.0195(13) -0.0032(10) 0.0110(11) -0.0002(9) C36 0.0253(14) 0.0251(13) 0.0304(15) -0.0007(11) 0.0108(12) -0.0039(11) C37 0.0221(14) 0.0408(16) 0.0376(18) -0.0024(12) 0.0095(13) -0.0110(13) C38 0.0307(16) 0.0350(16) 0.0456(19) -0.0136(13) 0.0212(14) -0.0126(14) C39 0.0393(16) 0.0236(13) 0.0325(16) -0.0091(12) 0.0202(14) -0.0038(11) C40 0.0297(14) 0.0219(12) 0.0246(14) -0.0025(10) 0.0128(11) -0.0007(10) C41 0.0159(11) 0.0193(11) 0.0234(13) -0.0003(9) 0.0075(10) -0.0010(9) C42 0.0222(13) 0.0237(13) 0.0267(14) 0.0017(10) 0.0110(11) 0.0021(10) C43 0.0233(13) 0.0261(13) 0.0293(15) 0.0024(10) 0.0114(12) -0.0045(11) C44 0.0233(13) 0.0183(12) 0.0322(15) 0.0029(10) 0.0087(11) -0.0019(10) C45 0.0240(13) 0.0226(13) 0.0280(15) 0.0007(10) 0.0098(11) 0.0044(10) C46 0.0206(12) 0.0212(12) 0.0222(13) -0.0004(10) 0.0083(10) -0.0003(10) 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 88.07(11) . . ? C2 Re1 C1 92.11(12) . . ? C3 Re1 C1 88.47(11) . . ? C2 Re1 O4 176.66(9) . 1 ? C3 Re1 O4 95.21(9) . 1 ? C1 Re1 O4 88.59(10) . 1 ? C2 Re1 O4 176.66(9) . . ? C3 Re1 O4 95.21(9) . . ? C1 Re1 O4 88.59(10) . . ? O4 Re1 O4 0.00(8) 1 . ? C2 Re1 N1 92.13(10) . . ? C3 Re1 N1 179.73(9) . . ? C1 Re1 N1 91.69(10) . . ? O4 Re1 N1 84.59(7) 1 . ? O4 Re1 N1 84.59(7) . . ? C2 Re1 P1 92.98(8) . . ? C3 Re1 P1 88.66(8) . . ? C1 Re1 P1 174.07(8) . . ? O4 Re1 P1 86.50(5) 1 . ? O4 Re1 P1 86.50(5) . . ? N1 Re1 P1 91.16(6) . . ? C35 P1 C41 103.86(11) . . ? C35 P1 C29 104.31(12) . . ? C41 P1 C29 102.51(12) . . ? C35 P1 Re1 115.30(9) . . ? C41 P1 Re1 115.10(8) . . ? C29 P1 Re1 114.22(8) . . ? C17 O4 Re1 127.41(16) . . ? C11 N1 C19 116.0(2) . . ? C11 N1 Re1 125.50(17) . . ? C19 N1 Re1 118.49(17) . . ? C23 N2 C22 109.0(3) . . ? C23 N2 H2 124(3) . . ? C22 N2 H2 126(3) . . ? O1 C1 Re1 175.9(2) . . ? O2 C2 Re1 178.4(2) . . ? O3 C3 Re1 177.3(2) . . ? N1 C11 C12 127.9(2) . . ? N1 C11 H11 116 . . ? C12 C11 H11 116 . . ? C13 C12 C17 118.5(2) . . ? C13 C12 C11 117.3(2) . . ? C17 C12 C11 124.1(2) . . ? C14 C13 C12 121.8(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 118.8(3) . . ? C16 C15 C18 119.9(3) . . ? C14 C15 C18 121.4(3) . . ? C15 C16 C17 122.1(3) . . ? C15 C16 H16 119 . . ? C17 C16 H16 119 . . ? O4 C17 C16 118.2(2) 1 . ? O4 C17 C16 118.2(2) . . ? O4 C17 C12 123.4(2) 1 . ? O4 C17 C12 123.4(2) . . ? C16 C17 C12 118.4(2) . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 114.1(2) . . ? N1 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? N1 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? C21 C20 C19 110.3(2) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C24 107.2(3) . . ? C22 C21 C20 126.3(3) . . ? C24 C21 C20 126.3(3) . . ? C21 C22 N2 109.8(3) . . ? C21 C22 H22 125.1 . . ? N2 C22 H22 125.1 . . ? N2 C23 C28 130.7(3) . . ? N2 C23 C24 107.2(3) . . ? C28 C23 C24 122.1(3) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 C21 134.3(3) . . ? C23 C24 C21 106.8(3) . . ? C26 C25 C24 119.4(3) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H26 120 . . ? C27 C26 H26 120 . . ? C28 C27 C26 122.4(3) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C23 117.3(3) . . ? C27 C28 H28 121.3 . . ? C23 C28 H28 121.3 . . ? C30 C29 C34 119.3(3) . . ? C30 C29 P1 122.6(2) . . ? C34 C29 P1 118.0(2) . . ? C31 C30 C29 120.1(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120 . . ? C34 C33 H33 120 . . ? C33 C34 C29 120.1(3) . . ? C33 C34 H34 120 . . ? C29 C34 H34 120 . . ? C36 C35 C40 119.8(2) . . ? C36 C35 P1 121.7(2) . . ? C40 C35 P1 118.4(2) . . ? C35 C36 C37 119.6(3) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 120.3(3) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.3(3) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 120.1(3) . . ? C38 C39 H39 120 . . ? C40 C39 H39 120 . . ? C39 C40 C35 119.9(3) . . ? C39 C40 H40 120.1 . . ? C35 C40 H40 120.1 . . ? C46 C41 C42 119.5(2) . . ? C46 C41 P1 120.24(19) . . ? C42 C41 P1 120.3(2) . . ? C43 C42 C41 120.1(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 119.8(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 120.4(2) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 120.1(3) . . ? C44 C45 H45 120 . . ? C46 C45 H45 120 . . ? C45 C46 C41 120.1(2) . . ? C45 C46 H46 120 . . ? C41 C46 H46 120 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 C2 . 1.904(3) ? Re1 C3 . 1.925(3) ? Re1 C1 . 1.934(3) ? Re1 O4 1 2.1171(18) ? Re1 O4 . 2.1171(18) ? Re1 N1 . 2.182(2) ? Re1 P1 . 2.5087(7) ? P1 C35 . 1.822(3) ? P1 C41 . 1.825(2) ? P1 C29 . 1.826(3) ? O1 C1 . 1.150(3) ? O2 C2 . 1.157(3) ? O3 C3 . 1.153(3) ? O4 O4 1 0.000(5) ? O4 C17 . 1.314(3) ? N1 C11 . 1.289(3) ? N1 C19 . 1.480(3) ? N2 C23 . 1.374(4) ? N2 C22 . 1.378(4) ? N2 H2 . 0.92(5) ? C11 C12 . 1.427(4) ? C11 H11 . 0.95 ? C12 C13 . 1.401(4) ? C12 C17 . 1.424(4) ? C13 C14 . 1.368(4) ? C13 H13 . 0.95 ? C14 C15 . 1.399(4) ? C14 H14 . 0.95 ? C15 C16 . 1.387(4) ? C15 C18 . 1.506(4) ? C16 C17 . 1.400(4) ? C16 H16 . 0.95 ? C18 H18A . 0.98 ? C18 H18B . 0.98 ? C18 H18C . 0.98 ? C19 C20 . 1.535(4) ? C19 H19A . 0.99 ? C19 H19B . 0.99 ? C20 C21 . 1.499(4) ? C20 H20A . 0.99 ? C20 H20B . 0.99 ? C21 C22 . 1.355(5) ? C21 C24 . 1.429(4) ? C22 H22 . 0.95 ? C23 C28 . 1.391(4) ? C23 C24 . 1.416(4) ? C24 C25 . 1.395(5) ? C25 C26 . 1.381(4) ? C25 H25 . 0.95 ? C26 C27 . 1.409(5) ? C26 H26 . 0.95 ? C27 C28 . 1.363(5) ? C27 H27 . 0.95 ? C28 H28 . 0.95 ? C29 C30 . 1.395(4) ? C29 C34 . 1.395(4) ? C30 C31 . 1.385(4) ? C30 H30 . 0.95 ? C31 C32 . 1.380(4) ? C31 H31 . 0.95 ? C32 C33 . 1.385(4) ? C32 H32 . 0.95 ? C33 C34 . 1.389(4) ? C33 H33 . 0.95 ? C34 H34 . 0.95 ? C35 C36 . 1.391(4) ? C35 C40 . 1.398(3) ? C36 C37 . 1.393(4) ? C36 H36 . 0.95 ? C37 C38 . 1.381(4) ? C37 H37 . 0.95 ? C38 C39 . 1.382(4) ? C38 H38 . 0.95 ? C39 C40 . 1.388(4) ? C39 H39 . 0.95 ? C40 H40 . 0.95 ? C41 C46 . 1.392(4) ? C41 C42 . 1.394(4) ? C42 C43 . 1.391(4) ? C42 H42 . 0.95 ? C43 C44 . 1.384(4) ? C43 H43 . 0.95 ? C44 C45 . 1.380(4) ? C44 H44 . 0.95 ? C45 C46 . 1.390(3) ? C45 H45 . 0.95 ? C46 H46 . 0.95 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C46 H46 O4 0.95 2.34 3.147(3) 142.4 1 yes N2 H2 O4 0.92(5) 2.51(5) 3.250(4) 138(4) 4_666 yes C14 H14 O1 0.95 2.57 3.401(4) 145.9 1_455 yes 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 C19 N1 C11 C12 179.2(3) . . . . ? Re1 N1 C11 C12 -0.6(4) . . . . ? N1 C11 C12 C13 -167.5(3) . . . . ? N1 C11 C12 C17 10.8(4) . . . . ? C17 C12 C13 C14 -1.5(5) . . . . ? C11 C12 C13 C14 176.9(3) . . . . ? C12 C13 C14 C15 0.9(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C13 C14 C15 C18 -179.3(4) . . . . ? C14 C15 C16 C17 -0.8(5) . . . . ? C18 C15 C16 C17 178.8(3) . . . . ? Re1 O4 C17 O4 0E1(10) . . . 1 ? O4 O4 C17 C16 0.00(12) 1 . . . ? Re1 O4 C17 C16 152.9(2) . . . . ? O4 O4 C17 C12 0.00(11) 1 . . . ? Re1 O4 C17 C12 -29.5(4) . . . . ? C15 C16 C17 O4 177.9(3) . . . 1 ? C15 C16 C17 O4 177.9(3) . . . . ? C15 C16 C17 C12 0.2(4) . . . . ? C13 C12 C17 O4 -176.7(3) . . . 1 ? C11 C12 C17 O4 5.1(4) . . . 1 ? C13 C12 C17 O4 -176.7(3) . . . . ? C11 C12 C17 O4 5.1(4) . . . . ? C13 C12 C17 C16 0.9(4) . . . . ? C11 C12 C17 C16 -177.4(3) . . . . ? C11 N1 C19 C20 111.0(3) . . . . ? Re1 N1 C19 C20 -69.1(3) . . . . ? N1 C19 C20 C21 179.3(3) . . . . ? C19 C20 C21 C22 -78.4(4) . . . . ? C19 C20 C21 C24 95.6(4) . . . . ? C24 C21 C22 N2 1.5(3) . . . . ? C20 C21 C22 N2 176.5(3) . . . . ? C23 N2 C22 C21 -2.0(3) . . . . ? C22 N2 C23 C28 -176.8(3) . . . . ? C22 N2 C23 C24 1.6(3) . . . . ? N2 C23 C24 C25 179.8(3) . . . . ? C28 C23 C24 C25 -1.6(4) . . . . ? N2 C23 C24 C21 -0.7(3) . . . . ? C28 C23 C24 C21 177.9(3) . . . . ? C22 C21 C24 C25 178.9(3) . . . . ? C20 C21 C24 C25 4.0(5) . . . . ? C22 C21 C24 C23 -0.5(3) . . . . ? C20 C21 C24 C23 -175.4(3) . . . . ? C23 C24 C25 C26 1.1(4) . . . . ? C21 C24 C25 C26 -178.2(3) . . . . ? C24 C25 C26 C27 0.3(5) . . . . ? C25 C26 C27 C28 -1.4(5) . . . . ? C26 C27 C28 C23 0.9(5) . . . . ? N2 C23 C28 C27 178.8(3) . . . . ? C24 C23 C28 C27 0.6(4) . . . . ? C35 P1 C29 C30 -12.3(2) . . . . ? C41 P1 C29 C30 95.8(2) . . . . ? Re1 P1 C29 C30 -139.06(19) . . . . ? C35 P1 C29 C34 169.3(2) . . . . ? C41 P1 C29 C34 -82.7(2) . . . . ? Re1 P1 C29 C34 42.5(2) . . . . ? C34 C29 C30 C31 -1.9(4) . . . . ? P1 C29 C30 C31 179.7(2) . . . . ? C29 C30 C31 C32 0.7(4) . . . . ? C30 C31 C32 C33 0.9(4) . . . . ? C31 C32 C33 C34 -1.3(4) . . . . ? C32 C33 C34 C29 0.1(4) . . . . ? C30 C29 C34 C33 1.5(4) . . . . ? P1 C29 C34 C33 179.9(2) . . . . ? C41 P1 C35 C36 19.0(3) . . . . ? C29 P1 C35 C36 126.1(2) . . . . ? Re1 P1 C35 C36 -107.8(2) . . . . ? C41 P1 C35 C40 -165.7(2) . . . . ? C29 P1 C35 C40 -58.6(2) . . . . ? Re1 P1 C35 C40 67.5(2) . . . . ? C40 C35 C36 C37 -0.5(4) . . . . ? P1 C35 C36 C37 174.8(2) . . . . ? C35 C36 C37 C38 1.2(5) . . . . ? C36 C37 C38 C39 -0.4(5) . . . . ? C37 C38 C39 C40 -1.0(5) . . . . ? C38 C39 C40 C35 1.7(4) . . . . ? C36 C35 C40 C39 -1.0(4) . . . . ? P1 C35 C40 C39 -176.4(2) . . . . ? C35 P1 C41 C46 -108.9(2) . . . . ? C29 P1 C41 C46 142.7(2) . . . . ? Re1 P1 C41 C46 18.0(2) . . . . ? C35 P1 C41 C42 69.0(2) . . . . ? C29 P1 C41 C42 -39.4(2) . . . . ? Re1 P1 C41 C42 -164.02(18) . . . . ? C46 C41 C42 C43 -0.7(4) . . . . ? P1 C41 C42 C43 -178.7(2) . . . . ? C41 C42 C43 C44 0.5(4) . . . . ? C42 C43 C44 C45 -0.1(4) . . . . ? C43 C44 C45 C46 -0.1(4) . . . . ? C44 C45 C46 C41 -0.2(4) . . . . ? C42 C41 C46 C45 0.6(4) . . . . ? P1 C41 C46 C45 178.5(2) . . . . ?