#------------------------------------------------------------------------------ #$Date: 2020-06-05 14:27:41 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252907 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/74/7157457.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_7157457 loop_ _publ_author_name 'Sarkar, Parantap' 'Inaba, Yuya' 'Shirakura, Hayato' 'Yoneda, Tomoki' 'Inokuma, Yasuhide' _publ_section_title ; Modular synthesis of oligoacetylacetones via site-selective silylation of acetylacetone derivatives. ; _journal_issue 17 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 3297 _journal_page_last 3302 _journal_paper_doi 10.1039/d0ob00501k _journal_volume 18 _journal_year 2020 _chemical_formula_moiety 'C20 H30 O4' _chemical_formula_sum 'C20 H30 O4' _chemical_formula_weight 334.44 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 98.444(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.8166(4) _cell_length_b 12.8538(5) _cell_length_c 14.9915(7) _cell_measurement_reflns_used 10446 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 29.3310 _cell_measurement_theta_min 2.6020 _cell_volume 1871.13(14) _computing_cell_refinement 'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)' _computing_molecular_graphics 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_publication_material 'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 123(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0222 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 23195 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.995 _diffrn_reflns_theta_min 2.332 _diffrn_source 'Rotating-anode X-ray tube (dual wavelength)' _diffrn_source_type 'Rigaku (Mo) X-ray DW Source' _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.450 _exptl_crystal_size_min 0.320 _refine_diff_density_max 0.539 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 4072 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0562 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+1.2193P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1483 _refine_ls_wR_factor_ref 0.1528 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3605 _reflns_number_total 4072 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00501k3.cif _cod_data_source_block Compound3b _cod_depositor_comments 'Adding full bibliography for 7157456--7157460.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7157457 _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_min 0.953 _shelx_estimated_absorpt_t_max 0.975 _shelx_res_file ; TITL CyHex_dimer_a.res in P2(1)/n CyHex_dimer_a.res created by SHELXL-2018/3 at 16:10:02 on 25-Jan-2020 REM Yadorkari-X generated CELL 0.71073 9.8166 12.8538 14.9915 90.0000 98.4440 90.0000 ZERR 4.0 0.0004 0.0005 0.0007 0.0000 0.0040 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H O UNIT 80 120 16 SIZE 0.60 0.45 0.32 TEMP -150.0 L.S. 10 FMAP 2 PLAN -20 ACTA CONF LIST 4 OMIT -10.000000 54.000000 WGHT 0.072400 1.219300 FVAR 0.53473 C1 1 0.883589 0.219569 0.409154 11.00000 0.03696 0.03484 = 0.04594 0.00439 0.00392 0.00873 AFIX 137 H1 2 0.869710 0.160558 0.367416 11.00000 -1.50000 H2 2 0.806386 0.223691 0.443686 11.00000 -1.50000 H3 2 0.969628 0.209969 0.450591 11.00000 -1.50000 AFIX 0 C2 1 0.891358 0.318918 0.356420 11.00000 0.02465 0.02880 = 0.02604 -0.00711 0.00365 -0.00173 C3 1 0.755719 0.377009 0.322327 11.00000 0.02083 0.02333 = 0.02187 -0.00094 0.00340 -0.00495 C4 1 0.704140 0.418450 0.407585 11.00000 0.01713 0.02314 = 0.02214 0.00374 0.00027 -0.00184 C5 1 0.769136 0.516580 0.449920 11.00000 0.01856 0.02320 = 0.02227 0.00263 0.00330 -0.00267 AFIX 23 H4 2 0.734386 0.577266 0.412711 11.00000 -1.20000 H5 2 0.870188 0.513124 0.451379 11.00000 -1.20000 AFIX 0 C6 1 0.736717 0.530935 0.545354 11.00000 0.01885 0.02333 = 0.02412 0.00153 0.00379 0.00067 AFIX 23 H6 2 0.772996 0.598871 0.569234 11.00000 -1.20000 H7 2 0.635649 0.531136 0.544326 11.00000 -1.20000 AFIX 0 C7 1 0.799958 0.444833 0.606418 11.00000 0.01487 0.02574 = 0.02266 0.00178 0.00246 -0.00106 C8 1 0.744173 0.427244 0.696202 11.00000 0.01749 0.03026 = 0.02463 0.00500 0.00552 -0.00059 C9 1 0.605070 0.371380 0.670554 11.00000 0.01965 0.02757 = 0.02973 0.00896 0.00475 -0.00033 C10 1 0.604615 0.264466 0.630751 11.00000 0.04290 0.02672 = 0.05155 0.00622 0.01267 -0.00817 AFIX 137 H8 2 0.609735 0.212580 0.679026 11.00000 -1.50000 H9 2 0.684187 0.256626 0.598757 11.00000 -1.50000 H10 2 0.519626 0.254245 0.588430 11.00000 -1.50000 AFIX 0 C11 1 0.647304 0.301507 0.274147 11.00000 0.02323 0.02978 = 0.02744 -0.00519 0.00321 -0.00612 AFIX 23 H11 2 0.638049 0.241233 0.313930 11.00000 -1.20000 H12 2 0.557026 0.337156 0.262728 11.00000 -1.20000 AFIX 0 C12 1 0.685530 0.262773 0.184971 11.00000 0.03030 0.03429 = 0.03122 -0.01082 0.00450 -0.00453 AFIX 23 H13 2 0.772503 0.222749 0.196463 11.00000 -1.20000 H14 2 0.612479 0.215812 0.155565 11.00000 -1.20000 AFIX 0 C13 1 0.702962 0.353772 0.122579 11.00000 0.04073 0.04725 = 0.02292 -0.00508 0.00410 -0.00052 AFIX 23 H15 2 0.613812 0.390255 0.107070 11.00000 -1.20000 H16 2 0.731083 0.327306 0.066003 11.00000 -1.20000 AFIX 0 C14 1 0.811067 0.430009 0.167185 11.00000 0.03815 0.03303 = 0.02781 0.00019 0.01255 0.00135 AFIX 23 H17 2 0.815221 0.490752 0.127072 11.00000 -1.20000 H18 2 0.902439 0.395847 0.175309 11.00000 -1.20000 AFIX 0 C15 1 0.779553 0.467509 0.258744 11.00000 0.02843 0.02405 = 0.02641 0.00066 0.00833 -0.00032 AFIX 23 H19 2 0.696374 0.512019 0.249385 11.00000 -1.20000 H20 2 0.857288 0.510533 0.287782 11.00000 -1.20000 AFIX 0 C16 1 0.722997 0.532261 0.741255 11.00000 0.04070 0.03795 = 0.02919 -0.00494 0.01752 -0.01334 AFIX 23 H21 2 0.807879 0.574367 0.743506 11.00000 -1.20000 H22 2 0.647317 0.570444 0.704206 11.00000 -1.20000 AFIX 0 C17 1 0.688386 0.519503 0.837176 11.00000 0.06305 0.05562 = 0.03377 -0.01017 0.02622 -0.02430 AFIX 23 H23 2 0.684374 0.588894 0.865329 11.00000 -1.20000 H24 2 0.596618 0.486694 0.834394 11.00000 -1.20000 AFIX 0 C18 1 0.795192 0.452961 0.894884 11.00000 0.06472 0.10582 = 0.02392 0.00286 0.01058 -0.03659 AFIX 23 H25 2 0.768575 0.444372 0.955645 11.00000 -1.20000 H26 2 0.885654 0.488421 0.901737 11.00000 -1.20000 AFIX 0 C19 1 0.807449 0.345646 0.851973 11.00000 0.03552 0.08681 = 0.03281 0.02582 0.00346 -0.00507 AFIX 23 H27 2 0.878985 0.304334 0.889825 11.00000 -1.20000 H28 2 0.718775 0.308167 0.848876 11.00000 -1.20000 AFIX 0 C20 1 0.845417 0.356854 0.756951 11.00000 0.02022 0.06035 = 0.03103 0.01933 0.00146 0.00320 AFIX 23 H29 2 0.846436 0.287128 0.729005 11.00000 -1.20000 H30 2 0.939326 0.386324 0.761215 11.00000 -1.20000 AFIX 0 O1 3 1.000769 0.352070 0.341310 11.00000 0.02028 0.04817 = 0.04764 -0.00203 0.00633 -0.00225 O2 3 0.614649 0.373323 0.439752 11.00000 0.02614 0.03114 = 0.03430 0.00010 0.00988 -0.00898 O3 3 0.890590 0.390043 0.585196 11.00000 0.02280 0.03695 = 0.03170 0.00733 0.00865 0.01014 O4 3 0.498354 0.412078 0.681755 11.00000 0.01851 0.04774 = 0.05643 0.00170 0.00912 0.00344 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM CyHex_dimer_a.res in P2(1)/n REM wR2 = 0.1528, GooF = S = 1.058, Restrained GooF = 1.058 for all data REM R1 = 0.0562 for 3605 Fo > 4sig(Fo) and 0.0619 for all 4072 data REM 219 parameters refined using 0 restraints END WGHT 0.0724 1.2198 REM Highest difference peak 0.539, deepest hole -0.318, 1-sigma level 0.051 Q1 1 0.7100 0.2665 0.2512 11.00000 0.05 0.54 Q2 1 0.7452 0.4776 0.1898 11.00000 0.05 0.52 Q3 1 0.8597 0.4266 0.2547 11.00000 0.05 0.51 Q4 1 0.5949 0.3224 0.1935 11.00000 0.05 0.51 Q5 1 1.0478 0.3000 0.3753 11.00000 0.05 0.51 Q6 1 0.8167 0.3424 0.3238 11.00000 0.05 0.49 Q7 1 0.7366 0.3896 0.3706 11.00000 0.05 0.43 Q8 1 0.6210 0.3449 0.3962 11.00000 0.05 0.36 Q9 1 0.6655 0.4111 0.1329 11.00000 0.05 0.35 Q10 1 0.7681 0.4345 0.6511 11.00000 0.05 0.34 Q11 1 0.7410 0.5178 0.4973 11.00000 0.05 0.31 Q12 1 0.6803 0.4019 0.6840 11.00000 0.05 0.31 Q13 1 0.7695 0.4191 0.2939 11.00000 0.05 0.29 Q14 1 0.7432 0.4676 0.4280 11.00000 0.05 0.29 Q15 1 0.9161 0.2666 0.3788 11.00000 0.05 0.29 Q16 1 0.7817 0.3892 0.7239 11.00000 0.05 0.28 Q17 1 0.6928 0.5215 0.7922 11.00000 0.05 0.28 Q18 1 0.7725 0.4936 0.5769 11.00000 0.05 0.27 Q19 1 0.7272 0.4747 0.7150 11.00000 0.05 0.27 Q20 1 0.6032 0.3195 0.6431 11.00000 0.05 0.26 ; _shelx_res_checksum 51845 _shelx_hkl_file ; 0 0 2 4346.53 152.55 0 0 3 0.30 0.23 0 0 4 3347.96 113.98 0 0 -4 3100.08 114.04 0 0 5 0.15 0.23 0 0 -5 0.24 0.36 0 0 6 102.11 3.74 0 0 -6 99.28 3.81 0 0 -7 -0.31 0.47 0 0 7 -0.79 0.76 0 0 7 -0.17 0.41 0 0 8 209.00 7.42 0 0 -8 199.17 7.50 0 0 8 201.19 7.65 0 0 -9 0.04 0.54 0 0 9 0.46 0.62 0 0 9 0.06 0.77 0 0 9 -0.21 0.41 0 0 10 238.20 8.81 0 0 10 228.52 8.79 0 0 10 234.35 8.51 0 0 -10 230.87 8.58 0 0 -11 -0.09 0.56 0 0 11 0.11 0.54 0 0 11 -0.29 0.80 0 0 11 -1.09 0.89 0 0 -12 245.42 9.09 0 0 12 254.11 9.40 0 0 12 239.31 9.41 0 0 12 244.30 9.01 0 0 13 0.75 0.61 0 0 13 0.09 1.03 0 0 -13 -0.31 0.70 0 0 13 1.48 1.00 0 0 -14 197.37 7.22 0 0 14 190.56 7.14 0 0 14 208.20 7.67 0 0 14 191.59 7.65 0 0 15 0.82 0.67 0 0 15 -0.31 1.05 0 0 -15 0.87 1.02 0 0 15 -0.21 1.16 0 0 -15 -0.28 0.68 0 0 16 2.62 1.31 0 0 16 3.98 1.29 0 0 -16 3.03 0.81 0 0 -16 1.69 1.05 0 0 16 2.30 0.77 0 0 17 0.12 1.34 0 0 17 0.99 1.23 0 0 17 -0.29 0.78 0 0 -17 0.43 0.78 0 0 -17 0.30 1.10 0 0 -18 6.13 1.35 0 0 18 5.10 1.54 0 0 18 5.97 1.56 0 0 -18 7.70 1.04 0 1 2 13.92 0.52 0 -1 -2 8.50 0.52 0 -1 -3 -0.06 0.29 0 -1 -3 -0.09 0.39 0 1 4 309.85 11.50 0 -1 -4 319.21 11.58 0 -1 -4 343.09 11.52 0 1 5 189.45 7.49 0 1 5 209.91 7.40 0 -1 -5 213.62 7.39 0 -1 -5 203.77 7.47 0 -1 -6 19.08 1.01 0 1 6 18.53 1.09 0 1 6 17.46 1.06 0 1 6 20.15 0.93 0 -1 -6 19.94 0.92 0 1 7 1441.82 49.86 0 1 7 1378.76 50.02 0 1 7 1407.80 50.06 0 -1 -7 1411.06 49.96 0 -1 -8 2.72 0.58 0 -1 8 1.85 0.40 0 -1 8 2.28 0.62 0 1 -8 1.72 0.48 0 1 8 2.21 0.68 0 1 8 3.22 0.48 0 1 8 2.02 0.61 0 1 9 116.04 4.34 0 1 -9 109.65 4.36 0 1 9 119.94 4.60 0 -1 9 122.51 4.60 0 -1 9 112.26 4.29 0 1 9 116.05 4.62 0 -1 -9 112.04 4.43 0 -1 -10 33.52 1.62 0 1 -10 31.61 1.57 0 -1 10 32.44 1.50 0 1 10 33.65 1.81 0 -1 10 30.46 1.76 0 1 10 33.66 1.54 0 1 10 34.78 1.90 0 1 11 1.06 0.54 0 -1 11 1.63 0.77 0 1 -11 1.22 0.63 0 -1 11 0.56 0.51 0 1 11 1.21 0.86 0 -1 -11 1.26 0.67 0 1 11 1.02 0.90 0 -1 12 247.45 9.52 0 1 12 257.24 9.60 0 -1 12 238.44 9.51 0 -1 12 247.98 9.17 0 1 12 247.03 9.55 0 -1 -12 261.09 9.31 0 1 12 250.61 9.19 0 1 -12 248.70 9.22 0 -1 13 2.10 1.15 0 1 13 1.46 1.06 0 -1 13 0.86 0.99 0 1 -13 1.45 0.66 0 1 13 1.96 1.04 0 -1 -13 2.68 0.84 0 -1 13 1.52 0.65 0 1 13 1.82 0.67 0 -1 14 72.47 3.43 0 1 14 67.87 3.44 0 1 14 70.87 3.46 0 1 14 68.70 2.97 0 -1 14 66.70 3.38 0 -1 14 67.41 2.93 0 -1 -14 70.46 3.09 0 1 -14 72.55 3.00 0 -1 -15 2.76 0.90 0 1 15 3.01 0.80 0 -1 15 2.48 1.20 0 1 15 3.08 1.22 0 -1 15 2.86 0.73 0 -1 15 4.47 1.31 0 1 -15 2.55 0.75 0 1 15 6.54 1.34 0 -1 16 -0.11 1.14 0 1 16 0.12 1.27 0 -1 -16 -0.12 0.82 0 1 -16 0.45 0.75 0 -1 16 0.11 1.17 0 -1 16 0.73 0.67 0 1 -16 0.65 1.00 0 1 16 0.40 0.72 0 1 -17 6.96 1.29 0 -1 17 6.79 1.54 0 1 -17 7.37 0.94 0 -1 17 8.28 1.60 0 1 17 5.96 1.42 0 1 17 9.18 1.02 0 -1 -17 6.88 1.04 0 -1 17 6.49 0.91 0 1 -18 13.98 1.60 0 -1 18 10.65 1.70 0 1 18 12.51 1.88 0 -1 18 14.38 1.85 0 1 -18 14.33 1.21 0 -1 -18 13.89 1.31 0 -2 0 1282.12 45.06 0 -2 1 46.04 1.63 0 2 -1 44.98 1.62 0 -2 1 42.31 1.67 0 -2 -1 42.37 1.68 0 -2 2 37.45 1.41 0 2 2 34.19 1.52 0 -2 2 39.09 1.44 0 2 2 36.09 1.49 0 -2 -2 40.39 1.54 0 2 3 8.00 0.61 0 -2 -3 7.24 0.55 0 -2 3 6.66 0.44 0 -2 -3 7.87 0.48 0 2 3 7.25 0.54 0 2 4 370.27 14.25 0 2 4 423.55 14.32 0 -2 -4 411.39 14.29 0 -2 -4 401.08 14.21 0 -2 -5 1.09 0.32 0 2 5 0.98 0.44 0 -2 -5 0.55 0.42 0 2 5 0.98 0.32 0 -2 -6 281.74 9.77 0 2 6 272.86 9.76 0 -2 -6 255.13 9.83 0 2 6 272.71 9.91 0 2 7 97.62 3.58 0 -2 -7 95.14 3.70 0 -2 -7 92.32 3.56 0 2 7 88.84 3.73 0 2 8 53.99 2.41 0 -2 -8 49.34 2.26 0 2 8 55.28 2.20 0 -2 -8 53.88 2.16 0 -2 -9 165.83 6.45 0 2 9 172.70 6.61 0 2 9 175.64 6.38 0 -2 -10 9.68 0.89 0 2 10 10.37 0.81 0 2 10 10.35 1.09 0 2 11 71.96 2.96 0 2 11 73.39 3.28 0 -2 11 75.83 3.25 0 2 -11 67.28 2.91 0 -2 11 73.15 2.88 0 -2 -11 72.30 3.06 0 -2 12 9.74 1.28 0 2 12 9.27 1.25 0 -2 12 8.69 0.81 0 -2 -12 9.07 1.00 0 2 -12 10.87 0.93 0 2 12 9.14 0.90 0 -2 13 36.77 1.77 0 -2 13 34.29 2.12 0 -2 -13 35.11 1.95 0 2 -13 39.79 1.82 0 2 13 38.46 2.28 0 2 13 37.24 1.84 0 2 -14 136.42 5.39 0 -2 14 139.95 5.40 0 2 14 142.83 5.46 0 -2 -14 138.07 5.54 0 -2 14 142.14 5.85 0 2 14 146.14 5.92 0 -2 -15 2.29 0.88 0 -2 15 3.71 0.77 0 2 -15 4.01 0.78 0 2 15 5.64 1.27 0 -2 15 4.64 1.23 0 -2 15 1.56 1.17 0 -2 -16 -0.20 0.86 0 -2 16 0.58 0.74 0 -2 16 0.68 1.24 0 2 16 0.71 1.21 0 2 -16 0.66 0.69 0 -2 16 0.55 1.16 0 2 -17 3.93 0.89 0 -2 17 3.84 0.85 0 2 17 3.20 1.52 0 -2 17 5.55 1.48 0 -2 -17 3.93 1.03 0 -2 17 5.82 1.46 0 2 -18 18.12 1.31 0 -2 18 14.23 1.84 0 2 -18 16.64 1.70 0 -2 -18 17.12 1.44 0 2 18 15.56 1.99 0 -2 18 15.53 1.88 0 3 0 -0.05 0.28 0 -3 0 -0.10 0.26 0 3 -1 17.21 0.73 0 3 1 15.19 0.77 0 3 -1 16.66 0.72 0 -3 1 16.97 0.70 0 -3 -1 17.21 0.77 0 -3 -2 177.84 6.41 0 3 -2 165.00 6.28 0 -3 2 181.96 6.29 0 -3 2 193.60 6.36 0 3 -2 168.90 6.33 0 -3 3 1209.24 44.43 0 -3 -3 1300.89 44.52 0 3 3 1270.47 44.50 0 -3 3 1266.70 44.39 0 3 3 1286.59 44.53 0 3 4 257.30 9.05 0 -3 -4 251.69 9.01 0 -3 4 252.39 8.90 0 -3 -4 251.53 8.94 0 3 4 240.12 8.98 0 -3 4 241.08 8.88 0 -3 -5 61.30 2.45 0 -3 5 61.20 2.43 0 -3 -5 58.71 2.52 0 3 5 64.04 2.53 0 3 5 69.25 2.62 0 3 6 5.01 0.68 0 -3 -6 4.31 0.62 0 3 6 3.56 0.58 0 -3 -6 5.24 0.54 0 -3 6 4.32 0.55 0 -3 -7 113.85 4.19 0 -3 -7 117.17 4.31 0 3 7 114.58 4.38 0 -3 -8 5.43 0.73 0 -3 -8 7.61 0.68 0 3 8 5.65 0.80 0 -3 -9 176.07 6.76 0 -3 -9 179.59 6.65 0 3 9 181.88 6.92 0 -3 -10 70.75 2.92 0 3 10 79.03 3.30 0 -3 -10 70.62 3.06 0 3 11 111.30 4.78 0 -3 -11 116.63 4.60 0 3 12 55.36 2.82 0 -3 -12 52.07 2.50 0 -3 13 78.51 3.65 0 -3 -13 85.03 3.49 0 -3 13 77.19 3.24 0 3 13 86.01 3.82 0 -3 -14 6.19 1.04 0 3 14 8.82 1.44 0 -3 14 6.18 0.77 0 -3 14 8.10 1.27 0 -3 -15 2.19 0.92 0 3 -15 2.90 0.77 0 3 15 0.89 1.25 0 -3 15 2.70 0.74 0 -3 15 3.88 1.22 0 3 16 6.20 1.46 0 3 -16 5.57 0.83 0 -3 16 5.01 0.84 0 -3 16 5.62 1.26 0 -3 -16 4.01 0.99 0 -3 17 3.60 1.37 0 -3 -17 4.29 1.05 0 3 17 4.09 1.45 0 3 -17 4.98 0.87 0 -3 17 4.89 0.85 0 3 18 4.63 1.53 0 -3 -18 7.96 1.17 0 3 -18 6.18 0.98 0 4 0 288.31 10.71 0 -4 0 311.26 10.69 0 4 1 58.40 2.31 0 -4 -1 60.71 2.29 0 -4 1 61.28 2.24 0 4 -1 60.28 2.26 0 4 -1 59.33 2.27 0 -4 -2 34.20 1.44 0 4 -2 33.64 1.43 0 4 -2 35.07 1.37 0 -4 2 33.57 1.45 0 -4 2 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0.88 4 4 17 3.35 1.55 4 -4 17 1.40 1.19 -4 -5 18 47.34 2.79 4 5 -17 7.23 1.03 4 -5 -17 7.09 1.44 -4 -5 17 5.04 1.29 4 -5 -17 4.15 1.22 -4 5 17 5.53 1.60 -4 -5 17 5.58 1.56 4 -5 -16 4.36 1.26 4 -5 -16 6.32 1.21 4 5 -16 8.36 0.96 -4 -5 16 4.45 1.14 -4 5 16 5.75 1.59 -4 -5 16 3.49 1.38 -4 -5 15 2.67 1.21 4 -5 -15 0.41 1.10 -4 5 15 0.98 0.53 4 5 -15 1.36 0.75 -4 -5 15 0.11 0.26 -4 5 15 0.90 1.29 4 -5 -15 0.41 0.90 4 -5 -14 45.09 1.89 4 5 -14 44.91 2.13 4 -5 -14 45.02 2.35 -4 5 14 46.42 1.88 -4 -5 14 44.46 1.74 -4 -5 14 43.86 2.52 4 -5 -14 45.22 2.60 -4 -5 13 0.81 1.02 4 -5 -13 0.96 1.10 -4 5 13 1.09 0.48 4 -5 -13 1.53 0.90 4 5 -13 1.23 0.63 4 -5 -13 1.36 0.53 4 5 -12 132.90 5.03 4 -5 -12 124.79 5.21 4 -5 -12 136.16 4.93 4 -5 -12 138.74 5.33 -4 5 12 130.09 4.87 -4 -5 12 135.49 5.42 -4 -5 11 0.82 0.94 -4 5 11 1.75 0.50 4 -5 -11 1.68 0.53 4 5 -11 2.77 0.67 4 -5 -11 1.58 0.84 4 -5 -11 1.18 0.86 4 5 -10 179.11 6.62 4 -5 -10 167.18 6.77 4 -5 -10 177.35 6.57 -4 5 10 185.22 6.52 -4 -5 10 175.24 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1.06 1.18 5 8 -14 -0.10 0.72 5 -8 -14 0.45 1.13 5 -8 -14 0.53 0.69 5 -8 -13 3.45 1.31 -5 -8 13 2.17 1.14 5 -8 -13 3.32 0.73 5 8 -13 2.59 0.72 5 -8 -13 3.06 1.15 -5 8 13 3.51 0.69 5 -8 -12 31.14 1.68 5 8 -12 35.29 1.62 5 -8 -12 33.37 2.05 -5 8 12 34.58 1.65 5 -8 -12 30.51 2.25 -5 -8 12 33.20 2.09 -5 -8 11 0.78 1.04 5 -8 -11 0.48 1.04 5 8 -11 0.66 0.58 5 -8 -11 0.16 1.02 5 -8 -11 -1.06 0.86 -5 8 11 0.33 0.56 5 -8 -11 0.33 1.21 -5 -8 10 -0.35 0.95 5 -8 -10 0.90 1.00 5 8 -10 0.70 0.54 5 -8 -10 -0.23 0.94 5 -8 -10 -0.15 0.74 5 -8 -10 -0.76 1.09 5 -8 -9 147.48 5.88 5 8 -9 144.17 5.33 5 -8 -9 142.21 5.75 5 -8 -9 145.37 5.48 5 8 -9 140.05 5.36 5 -8 -9 145.45 6.07 -5 -8 9 142.79 5.66 -5 -8 8 2.06 0.90 5 8 -8 3.51 0.66 5 -8 -8 2.51 1.04 5 8 -8 2.33 0.50 5 -8 -8 2.95 0.64 5 -8 -8 3.34 1.31 -5 -8 7 38.00 1.83 5 8 -7 37.56 1.57 5 -8 -7 36.77 1.67 5 8 -7 36.84 1.73 -5 -8 7 36.91 1.85 5 8 -6 114.35 4.36 5 8 -6 112.28 4.44 -5 -8 6 116.53 4.50 5 8 -6 115.67 4.23 5 -8 -6 113.50 4.32 -5 -8 6 113.35 4.43 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11 1 -1 2.64 0.97 11 -1 -1 3.51 1.01 11 -1 -1 2.10 0.59 11 -1 -1 3.03 0.99 11 1 -1 2.08 0.76 11 1 0 -0.20 0.31 11 1 0 -0.23 0.41 11 -1 0 0.15 0.53 11 -1 0 0.49 0.95 11 1 0 0.16 0.98 11 -1 0 0.07 0.87 11 1 0 -0.35 0.72 11 -1 1 71.12 3.40 11 1 1 73.90 2.77 11 -1 1 74.73 2.86 11 1 1 71.92 3.41 11 1 1 67.75 3.06 11 1 2 4.57 0.55 11 -1 2 4.55 0.62 11 -1 2 4.85 1.21 11 1 2 5.58 1.24 11 1 2 4.73 0.91 11 -1 3 1.34 0.56 11 -1 3 -0.09 1.11 11 1 3 -0.76 1.11 11 -1 4 13.39 0.91 11 -1 4 12.64 1.61 11 1 4 11.69 1.54 11 -1 5 42.09 2.58 11 -1 5 42.23 1.93 11 1 5 42.74 2.60 11 -2 -13 6.84 1.54 11 -2 -13 5.44 1.40 11 -2 -12 10.42 1.65 11 -2 -12 11.41 1.52 11 2 -12 10.04 1.26 11 2 -12 9.55 1.35 11 -2 -11 -1.04 1.29 11 -2 -11 0.37 1.17 11 2 -11 1.38 0.98 11 2 -11 0.97 1.03 11 -2 -10 0.60 1.18 11 -2 -10 -0.60 1.08 11 2 -10 1.37 0.85 11 2 -10 -0.52 1.00 11 -2 -9 6.47 1.19 11 2 -9 7.74 1.07 11 2 -9 7.65 1.12 11 -2 -9 6.94 1.31 11 -2 -8 33.57 2.14 11 -2 -8 33.12 1.92 11 2 -8 31.33 1.78 11 2 -8 28.52 1.73 11 -2 -7 22.46 1.30 11 -2 -7 27.11 1.62 11 -2 -7 24.83 1.43 11 -2 -7 24.10 1.82 11 2 -7 24.76 1.44 11 2 -7 23.57 1.51 11 2 -6 15.86 1.22 11 2 -6 17.71 1.13 11 -2 -6 16.30 1.57 11 -2 -6 18.26 1.36 11 -2 -6 16.91 1.19 11 2 -5 4.72 0.82 11 -2 -5 6.45 0.94 11 2 -5 7.01 0.93 11 2 -5 5.79 0.71 11 -2 -5 5.23 0.89 11 -2 -5 6.44 1.22 11 -2 -4 28.74 1.67 11 2 -4 27.36 1.65 11 2 -4 28.04 1.30 11 -2 -4 27.80 1.54 11 -2 -4 28.22 1.92 11 2 -4 26.64 1.49 11 2 -3 1.22 0.86 11 2 -3 1.88 0.67 11 2 -3 1.87 0.46 11 -2 -3 1.21 0.73 11 -2 -3 1.02 1.06 11 -2 -3 2.52 0.89 11 -2 -2 7.62 1.10 11 2 -2 7.92 1.12 11 2 -2 6.02 0.53 11 2 -2 4.28 0.62 11 2 -2 6.19 0.49 11 -2 -2 7.09 0.78 11 -2 -2 5.09 1.16 11 2 -2 4.45 0.71 11 -2 -1 0.61 0.94 11 2 -1 0.53 0.93 11 2 -1 0.38 0.37 11 2 -1 0.64 0.34 11 2 -1 0.42 0.53 11 -2 -1 0.49 0.61 11 -2 -1 1.35 0.99 11 2 -1 0.88 0.58 11 2 0 51.98 1.93 11 2 0 53.00 2.13 11 -2 0 54.05 2.64 11 2 0 49.16 1.95 11 -2 0 51.11 2.15 11 2 0 51.36 2.57 11 -2 0 43.63 2.47 11 2 0 45.52 2.10 11 -2 1 1.51 1.05 11 2 1 0.25 1.05 11 -2 1 0.43 0.57 11 2 1 0.30 0.60 11 -2 2 145.91 5.47 11 -2 2 153.36 6.03 11 2 2 140.81 5.99 11 -2 3 31.70 1.50 11 -2 3 30.74 2.07 11 2 3 28.00 2.10 11 -2 4 144.54 5.37 11 -2 4 139.91 5.94 11 2 4 139.80 5.99 -11 2 -5 23.68 1.65 11 -2 5 24.46 1.35 11 -2 5 26.56 1.97 11 2 5 23.02 1.97 11 -2 6 3.87 0.79 11 -3 -12 5.07 1.46 11 -3 -12 3.62 1.29 11 -3 -11 5.98 1.51 11 -3 -11 8.05 1.45 11 -3 -10 7.53 1.35 11 -3 -10 8.59 1.53 11 -3 -9 4.86 1.18 11 3 -9 4.54 1.03 11 3 -9 3.67 0.88 11 -3 -9 4.06 1.31 11 -3 -8 10.34 1.26 11 3 -8 11.96 1.11 11 3 -8 10.84 1.01 11 -3 -8 10.02 1.55 11 3 -7 170.55 6.52 11 -3 -7 184.89 6.62 11 -3 -7 161.43 6.48 11 -3 -7 174.62 6.77 11 -3 -7 172.44 7.09 11 3 -7 179.32 6.53 11 -3 -6 3.26 0.82 11 3 -6 5.02 0.76 11 -3 -6 5.20 1.31 11 3 -6 3.16 0.69 11 -3 -6 2.41 0.97 11 -3 -6 2.44 0.76 11 3 -5 10.09 0.83 11 -3 -5 10.60 1.06 11 3 -5 8.65 0.70 11 -3 -5 9.31 1.38 11 -3 -5 8.66 1.05 11 3 -4 0.83 0.56 11 -3 -4 1.51 0.79 11 3 -4 1.43 0.84 11 3 -4 1.07 0.42 11 -3 -4 1.59 0.79 11 -3 -4 1.69 1.11 11 3 -3 26.51 1.62 11 3 -3 23.17 1.04 11 -3 -3 27.48 1.47 11 -3 -3 25.33 1.59 11 -3 -3 23.72 1.83 11 3 -3 25.81 1.19 11 3 -2 6.70 0.58 11 3 -2 6.79 0.43 11 3 -2 7.90 0.60 11 -3 -2 7.25 0.84 11 -3 -2 6.22 1.17 11 3 -2 5.73 1.06 11 -3 -2 7.35 1.03 11 3 -1 0.91 0.61 11 3 -1 0.82 0.46 11 -3 -1 0.63 0.64 11 -3 -1 0.25 0.99 11 3 -1 1.74 0.93 11 -3 -1 1.83 0.96 11 -3 0 14.83 1.37 11 3 0 12.51 1.38 11 3 0 12.01 0.74 11 3 0 12.72 0.97 11 -3 0 13.60 0.97 11 3 1 36.96 1.85 11 -3 1 40.50 1.80 11 3 1 41.59 2.36 11 -3 1 39.64 2.28 11 3 2 1.85 1.08 11 -3 2 1.29 0.64 11 3 2 2.43 0.71 11 -3 2 2.30 1.11 11 3 3 9.05 1.38 11 -3 3 8.21 0.85 11 -3 3 10.21 1.42 11 3 4 7.27 1.47 -11 3 -4 7.65 1.18 11 -3 4 8.44 0.84 11 -3 4 7.07 1.37 -11 3 -5 34.81 2.13 11 -3 5 37.78 1.79 11 3 5 40.00 2.50 11 -3 5 38.40 2.39 -11 3 -6 4.94 1.26 11 -3 6 5.70 0.84 11 -4 -11 3.91 1.25 11 -4 -11 4.66 1.44 11 -4 -10 9.55 1.40 11 -4 -10 9.98 1.65 11 -4 -9 32.11 2.28 11 -4 -9 24.39 1.86 11 -4 -8 0.80 0.99 11 -4 -8 1.48 1.32 11 -4 -7 16.11 1.18 11 -4 -7 14.93 1.10 11 -4 -7 15.92 1.77 11 -4 -7 15.53 1.42 11 -4 -6 120.26 5.01 11 -4 -6 130.30 4.86 11 -4 -6 122.20 5.35 11 -4 -6 118.79 4.85 11 -4 -5 1.91 0.79 11 -4 -5 1.44 1.19 11 -4 -5 1.46 0.91 11 -4 -5 1.78 0.79 11 -4 -4 9.49 1.08 11 -4 -4 8.70 1.03 11 -4 -4 10.04 1.46 11 -4 -4 9.08 1.02 11 4 -3 17.15 0.93 11 -4 -3 17.80 1.35 11 -4 -3 14.12 1.17 11 -4 -3 12.11 1.56 11 -4 -2 48.23 2.35 11 4 -2 46.37 2.36 11 4 -2 43.25 1.86 11 -4 -2 45.45 2.10 11 -4 -2 40.44 2.42 11 4 -1 -0.25 0.67 11 4 -1 -0.28 0.51 11 -4 -1 -0.37 0.63 11 4 -1 -0.25 0.90 11 -4 -1 -0.30 0.92 11 4 0 17.21 1.20 11 -4 0 18.47 1.18 11 -4 0 19.36 1.54 11 4 0 18.02 1.55 11 -4 1 0.33 0.95 11 4 1 0.10 0.69 11 -4 1 0.54 0.67 11 4 1 -0.91 1.08 11 -4 2 0.17 1.06 11 -4 2 1.55 0.66 11 4 2 0.16 0.73 11 4 2 1.44 1.09 11 -4 3 7.45 0.84 11 4 3 7.03 0.93 11 -4 3 7.75 1.28 11 4 3 7.87 1.40 -11 4 -4 6.79 1.26 11 -4 4 10.69 0.95 11 -4 4 7.33 1.29 11 4 4 8.05 1.41 -11 4 -5 35.84 2.15 11 -4 5 34.16 1.74 11 -4 6 28.65 1.54 -11 4 -6 26.10 1.95 11 -4 7 15.31 1.21 11 -5 -10 4.74 1.30 11 -5 -10 2.85 1.46 11 -5 -9 6.55 1.27 11 -5 -9 3.93 1.51 11 -5 -8 18.38 1.57 11 -5 -8 18.62 1.89 11 -5 -7 1.56 0.78 11 -5 -7 3.84 0.86 11 -5 -7 3.12 1.44 11 -5 -7 1.47 1.15 11 -5 -6 1.89 0.77 11 -5 -6 0.89 1.24 11 -5 -5 55.64 2.69 11 -5 -5 52.22 2.99 11 -5 -5 59.06 2.61 11 5 -4 2.16 0.61 11 -5 -4 0.12 0.86 11 -5 -4 0.73 1.22 11 -5 -4 1.97 0.89 11 5 -3 4.04 0.59 11 -5 -3 2.24 0.86 11 -5 -3 2.86 1.13 11 -5 -3 3.28 0.94 11 5 -2 2.76 0.59 11 -5 -2 3.24 0.85 11 -5 -2 1.30 1.08 11 5 -1 23.13 1.26 11 -5 -1 26.49 1.45 11 5 0 1.41 0.81 11 -5 0 0.91 0.71 11 5 1 0.59 0.72 11 -5 1 1.47 0.73 11 5 1 1.12 1.13 11 -5 2 16.45 1.08 11 5 2 13.71 1.21 11 5 2 13.35 1.56 11 -5 3 6.72 1.25 11 -5 3 8.60 0.90 11 5 3 7.84 1.05 11 5 3 6.57 1.40 -11 5 -4 11.61 1.48 11 -5 4 13.15 1.07 -11 5 -5 4.70 1.31 11 -5 5 5.33 0.88 -11 5 -6 5.39 1.38 11 -5 6 9.57 1.03 -11 5 -7 3.69 1.29 11 -5 7 4.43 0.94 11 -6 -9 12.71 1.45 11 -6 -9 14.47 1.88 11 -6 -8 16.67 1.93 11 -6 -8 17.75 1.60 11 -6 -7 2.77 1.39 11 -6 -7 2.14 1.09 11 -6 -6 2.25 0.86 11 -6 -6 1.51 1.33 11 -6 -6 1.57 1.06 11 -6 -5 4.95 0.99 11 6 -5 7.36 0.76 11 -6 -5 3.93 1.39 11 -6 -5 3.43 1.03 11 -6 -4 8.80 1.12 11 6 -4 7.51 0.80 11 -6 -4 7.63 1.07 11 -6 -4 7.17 1.41 11 -6 -3 8.24 1.11 11 6 -3 7.61 0.75 11 6 -2 1.68 0.63 11 -6 -2 0.76 1.10 11 -6 -2 2.24 0.98 11 6 -1 -1.05 0.69 11 -6 -1 0.91 0.77 11 -6 -1 1.31 0.98 11 -6 0 -0.31 0.78 11 6 1 1.08 0.82 11 -6 1 1.20 0.77 11 6 2 2.40 0.96 11 -6 2 1.67 0.76 11 -6 3 15.22 1.16 11 6 3 16.66 1.36 -11 6 -4 5.03 1.34 11 -6 4 5.19 0.89 -11 6 -5 0.98 1.28 11 -6 5 2.18 0.86 -11 6 -6 24.43 2.04 11 -6 6 22.90 1.47 11 -7 -7 0.50 1.37 11 -7 -7 1.07 1.12 11 -7 -6 4.51 0.97 11 7 -6 6.52 0.78 11 -7 -6 3.90 1.14 11 -7 -5 0.48 0.90 11 7 -5 0.97 0.68 11 -7 -5 -0.35 1.22 11 -7 -5 0.80 1.00 11 -7 -4 3.85 1.02 11 7 -4 3.81 0.71 11 -7 -4 3.32 0.97 11 -7 -4 3.82 1.32 11 -7 -3 9.47 1.27 11 7 -3 10.63 0.90 11 -7 -3 9.84 1.10 11 -7 -2 2.37 1.09 11 7 -2 1.01 0.67 11 -7 -2 2.25 0.86 11 7 -1 0.80 0.73 11 -7 -1 4.16 0.92 11 -7 -1 3.27 1.08 11 -7 0 1.54 0.82 11 -7 0 1.52 1.02 11 7 1 0.22 0.93 11 -7 1 1.01 0.81 11 -7 1 0.09 1.04 11 7 2 -0.08 0.97 11 -7 2 2.42 0.82 -11 7 -3 0.83 1.30 11 7 3 -0.47 1.02 11 -7 3 1.47 0.82 -11 7 -4 19.39 1.91 11 -7 4 23.95 1.45 11 8 -8 28.66 1.61 11 8 -7 17.09 1.23 11 8 -6 1.23 0.71 11 -8 -5 48.25 2.44 11 8 -5 46.61 2.14 11 -8 -5 43.78 2.79 11 -8 -4 14.47 1.37 11 8 -4 12.58 1.08 11 -8 -4 14.62 1.37 11 -8 -4 12.35 1.60 11 -8 -3 2.72 1.09 11 8 -3 2.70 0.82 11 -8 -3 4.50 1.03 11 -8 -3 2.93 1.29 11 -8 -2 8.90 1.25 11 8 -2 6.84 0.89 11 -8 -2 8.06 1.06 11 -8 -1 20.26 1.66 11 -8 -1 16.90 1.31 11 -8 0 16.48 1.54 11 -8 0 14.62 1.25 11 8 1 5.98 1.20 11 -8 1 4.59 0.91 11 8 2 3.96 1.09 11 8 3 0.34 1.11 11 9 -6 21.76 1.42 11 -9 -5 2.62 1.12 11 9 -5 2.25 0.85 11 -9 -4 18.74 1.63 11 9 -4 17.30 1.29 11 -9 -3 18.43 1.66 11 9 -3 18.53 1.36 11 -9 -2 4.35 1.24 11 9 2 20.77 1.76 11 -10 -4 1.34 1.18 12 0 -8 31.43 1.99 12 0 -7 0.30 1.00 12 0 -7 -0.11 0.84 12 0 -6 32.66 1.74 12 0 -6 31.61 1.92 12 0 -5 1.18 0.80 12 0 -5 0.93 0.72 12 0 -5 -0.56 0.93 12 0 -4 14.92 1.32 12 0 -4 16.94 1.39 12 0 -3 -0.58 0.97 12 0 -2 72.84 3.35 12 0 -1 0.17 1.06 12 0 0 0.26 1.06 12 0 1 0.83 1.14 12 0 2 20.95 1.78 12 0 3 -0.71 1.12 12 -1 -11 0.48 1.28 12 -1 -11 -0.27 1.18 12 -1 -10 0.09 1.28 12 -1 -10 0.92 1.12 12 -1 -9 13.68 1.58 12 -1 -9 18.06 1.49 12 -1 -8 -0.09 1.10 12 -1 -8 1.72 0.98 12 -1 -7 16.45 1.38 12 -1 -7 17.00 1.60 12 -1 -6 0.56 0.82 12 -1 -6 1.25 1.11 12 -1 -5 0.32 0.79 12 -1 -5 1.10 0.79 12 1 -5 0.57 0.80 12 -1 -5 -0.16 0.99 12 1 -4 1.02 0.85 12 -1 -4 0.05 0.71 12 -1 -4 0.14 0.87 12 -1 -4 1.06 1.09 12 1 -3 104.02 4.35 12 -1 -3 101.26 3.99 12 -1 -3 98.07 4.38 12 -1 -3 107.91 4.38 12 -1 -2 0.71 0.99 12 1 -2 0.46 0.96 12 -1 -2 0.74 0.60 12 -1 -2 0.08 1.02 12 -1 -1 4.66 1.10 12 1 -1 2.03 1.02 12 -1 -1 4.14 0.65 12 -1 -1 3.90 1.09 12 -1 0 0.26 1.00 12 1 0 0.17 1.06 12 -1 1 8.91 1.39 12 1 1 10.75 1.38 12 -1 2 0.67 1.23 12 1 2 0.29 1.18 12 -1 3 3.13 1.32 12 1 3 1.42 1.19 12 -2 -11 -1.27 1.51 12 -2 -11 0.65 1.19 12 -2 -10 3.72 1.41 12 -2 -10 1.91 1.19 12 -2 -9 33.14 2.07 12 -2 -9 32.69 2.23 12 -2 -8 28.74 1.81 12 -2 -8 27.99 2.09 12 -2 -7 14.23 1.35 12 -2 -7 14.72 1.61 12 -2 -6 -0.73 0.98 12 -2 -6 0.47 1.09 12 -2 -5 4.63 0.96 12 2 -5 5.27 0.98 12 -2 -5 4.47 0.95 12 -2 -5 4.10 1.30 12 -2 -4 1.76 0.92 12 -2 -4 2.78 0.81 12 2 -4 0.91 0.94 12 -2 -4 -0.18 1.08 12 -2 -3 0.68 0.98 12 -2 -3 2.38 0.75 12 -2 -3 0.44 1.12 12 2 -3 0.07 0.96 12 -2 -2 82.33 3.59 12 2 -2 76.75 3.53 12 -2 -2 77.52 3.13 12 -2 -2 73.38 3.58 12 2 -1 1.17 1.08 12 -2 -1 1.29 0.62 12 -2 -1 0.86 1.11 12 -2 -1 0.34 1.08 12 2 0 0.62 1.04 12 -2 0 -0.56 0.60 12 -2 0 -0.64 1.12 12 -2 0 -0.66 1.09 12 2 1 4.92 1.30 12 -2 1 6.66 1.33 12 -2 2 103.20 4.51 12 2 2 93.61 4.40 12 -3 -11 0.91 1.31 12 -3 -10 9.52 1.61 12 -3 -10 11.67 1.46 12 -3 -9 44.79 2.42 12 -3 -9 40.68 2.66 12 -3 -8 9.17 1.55 12 -3 -8 12.55 1.37 12 -3 -7 2.46 1.03 12 -3 -7 2.12 1.28 12 -3 -6 45.47 2.34 12 -3 -6 46.01 2.67 12 -3 -5 35.32 1.92 12 -3 -5 29.97 1.82 12 -3 -5 33.94 1.78 12 -3 -5 30.19 2.22 12 -3 -4 48.44 2.46 12 -3 -4 47.37 2.30 12 -3 -4 46.75 2.71 12 3 -3 59.25 2.93 12 -3 -3 61.62 2.95 12 -3 -3 61.67 2.67 12 -3 -3 58.32 3.10 12 -3 -2 3.33 1.06 12 -3 -2 2.77 0.76 12 3 -2 1.14 1.06 12 -3 -2 2.46 1.30 12 -3 -1 28.19 1.92 12 3 -1 29.68 1.95 12 -3 -1 28.01 1.50 12 -3 -1 26.88 1.92 12 -3 0 1.51 1.03 12 -3 0 -0.92 0.69 12 -3 0 -0.26 1.06 12 3 0 -0.18 1.02 12 -3 1 16.52 1.62 12 -3 1 16.21 1.08 12 3 1 15.08 1.56 12 3 2 0.70 1.24 12 -3 2 0.78 1.30 12 -4 -10 6.84 1.56 12 -4 -9 8.67 1.62 12 -4 -9 14.45 1.44 12 -4 -8 29.25 1.96 12 -4 -8 26.62 2.18 12 -4 -7 5.86 1.18 12 -4 -7 5.94 1.49 12 -4 -6 15.84 1.42 12 -4 -6 16.25 1.71 12 -4 -5 10.72 1.17 12 -4 -5 9.67 1.13 12 -4 -5 10.95 1.60 12 -4 -5 11.14 1.13 12 -4 -4 1.45 1.07 12 -4 -4 0.54 0.87 12 -4 -4 -0.73 1.25 12 -4 -4 0.27 0.93 12 -4 -3 1.14 0.82 12 -4 -3 2.36 1.01 12 -4 -3 0.10 1.21 12 -4 -2 53.24 2.33 12 -4 -2 46.37 2.75 12 -4 -2 49.57 2.57 12 -4 -1 10.67 1.00 12 4 -1 10.92 1.39 12 -4 -1 7.47 1.40 12 -4 -1 12.41 1.40 12 -4 0 6.01 0.84 12 4 0 6.74 1.31 12 -4 0 5.44 1.26 12 -4 0 8.79 1.28 12 -4 1 14.31 1.06 12 4 1 13.31 1.60 12 -4 1 15.41 1.52 12 -4 2 23.84 1.37 12 4 2 24.43 1.99 12 -5 -8 14.59 1.83 12 -5 -8 14.84 1.52 12 -5 -7 24.02 1.77 12 -5 -7 26.74 2.23 12 -5 -6 4.48 1.13 12 -5 -6 4.98 1.47 12 -5 -5 64.15 2.98 12 -5 -5 64.11 3.38 12 -5 -4 49.10 2.47 12 -5 -4 47.20 2.37 12 -5 -4 50.35 2.44 12 -5 -4 41.07 2.73 12 -5 -3 45.64 2.39 12 -5 -3 44.16 2.18 12 -5 -3 43.48 2.34 12 -5 -3 41.47 2.55 12 -5 -2 19.42 1.63 12 -5 -2 18.79 1.30 12 -5 -2 19.70 1.53 12 -5 -1 10.87 1.36 12 -5 -1 10.60 1.05 12 -5 0 0.63 1.04 12 -5 0 0.78 0.75 12 -5 1 0.56 0.75 12 -5 1 -0.37 1.14 12 -5 2 16.29 1.20 12 -5 3 11.86 1.06 12 -6 -6 46.36 2.36 12 -6 -6 36.00 2.60 12 -6 -5 0.78 0.98 12 -6 -5 0.92 1.33 12 -6 -4 10.00 1.27 12 -6 -4 10.60 1.22 12 -6 -4 7.88 1.56 12 -6 -3 42.09 2.14 12 -6 -3 47.02 2.37 12 -6 -2 23.61 1.51 12 -6 -2 19.11 1.84 12 -6 -1 7.01 1.00 12 -6 -1 5.48 1.25 12 -6 -1 9.45 1.32 12 -6 0 0.48 0.81 12 -6 0 0.09 1.07 12 -6 1 0.76 0.83 12 -6 2 0.61 0.82 12 -6 3 1.46 0.88 12 -7 -4 27.33 1.87 12 -7 -3 4.60 1.25 12 -7 -2 4.61 1.24 12 -7 -2 2.63 1.20 12 -8 -3 1.57 1.16 13 0 -2 0.34 1.00 13 0 -1 9.35 1.34 13 0 0 0.09 1.19 13 1 -2 0.51 1.07 13 -1 -2 0.26 1.22 13 1 -1 1.44 1.21 13 -1 -1 -0.92 1.19 13 1 0 0.38 1.20 13 -1 0 1.83 1.28 13 2 -2 57.88 2.98 13 -2 -2 60.99 3.00 13 -2 -1 -0.65 1.14 13 2 -1 0.18 1.12 13 2 0 3.75 1.30 13 -3 -2 1.28 1.26 13 3 -2 0.09 1.12 13 -3 -1 27.62 2.03 13 3 -1 25.46 1.93 13 -4 -2 53.74 2.87 0 0 0 0.00 0.00 TITL CyHex_dimer in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 9.816614 12.853841 14.991467 90.0000 98.4443 90.0000 ZERR 4.00 0.000429 0.000550 0.000735 0.0000 0.0042 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H O UNIT 80.00 120.00 16.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 93741 loop_ _space_group_symop_operation_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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8836(2) 0.21957(15) 0.40915(14) 0.0395(4) Uani 1 1 d . . . . . H1 H 0.869710 0.160558 0.367416 0.059 Uiso 1 1 calc R U . . . H2 H 0.806386 0.223691 0.443686 0.059 Uiso 1 1 calc R U . . . H3 H 0.969628 0.209969 0.450591 0.059 Uiso 1 1 calc R U . . . C2 C 0.89136(16) 0.31892(13) 0.35642(11) 0.0265(3) Uani 1 1 d . . . . . C3 C 0.75572(15) 0.37701(12) 0.32233(10) 0.0220(3) Uani 1 1 d . . . . . C4 C 0.70414(14) 0.41845(11) 0.40759(10) 0.0211(3) Uani 1 1 d . . . . . C5 C 0.76914(14) 0.51658(11) 0.44992(10) 0.0213(3) Uani 1 1 d . . . . . H4 H 0.734386 0.577266 0.412711 0.026 Uiso 1 1 calc R U . . . H5 H 0.870188 0.513124 0.451379 0.026 Uiso 1 1 calc R U . . . C6 C 0.73672(15) 0.53094(11) 0.54535(10) 0.0220(3) Uani 1 1 d . . . . . H6 H 0.772996 0.598871 0.569234 0.026 Uiso 1 1 calc R U . . . H7 H 0.635649 0.531136 0.544326 0.026 Uiso 1 1 calc R U . . . C7 C 0.79996(14) 0.44483(12) 0.60642(10) 0.0211(3) Uani 1 1 d . . . . . C8 C 0.74417(15) 0.42724(12) 0.69620(10) 0.0239(3) Uani 1 1 d . . . . . C9 C 0.60507(15) 0.37138(12) 0.67055(11) 0.0255(3) Uani 1 1 d . . . . . C10 C 0.6046(2) 0.26447(14) 0.63075(14) 0.0398(4) Uani 1 1 d . . . . . H8 H 0.609735 0.212580 0.679026 0.060 Uiso 1 1 calc R U . . . H9 H 0.684187 0.256626 0.598757 0.060 Uiso 1 1 calc R U . . . H10 H 0.519626 0.254245 0.588430 0.060 Uiso 1 1 calc R U . . . C11 C 0.64730(16) 0.30151(13) 0.27415(11) 0.0269(3) Uani 1 1 d . . . . . H11 H 0.638049 0.241233 0.313930 0.032 Uiso 1 1 calc R U . . . H12 H 0.557026 0.337156 0.262728 0.032 Uiso 1 1 calc R U . . . C12 C 0.68553(18) 0.26277(14) 0.18497(11) 0.0319(4) Uani 1 1 d . . . . . H13 H 0.772503 0.222749 0.196463 0.038 Uiso 1 1 calc R U . . . H14 H 0.612479 0.215812 0.155565 0.038 Uiso 1 1 calc R U . . . C13 C 0.70296(19) 0.35377(16) 0.12258(11) 0.0370(4) Uani 1 1 d . . . . . H15 H 0.613812 0.390255 0.107070 0.044 Uiso 1 1 calc R U . . . H16 H 0.731083 0.327306 0.066003 0.044 Uiso 1 1 calc R U . . . C14 C 0.81107(18) 0.43001(14) 0.16718(11) 0.0322(4) Uani 1 1 d . . . . . H17 H 0.815221 0.490752 0.127072 0.039 Uiso 1 1 calc R U . . . H18 H 0.902439 0.395847 0.175309 0.039 Uiso 1 1 calc R U . . . C15 C 0.77955(16) 0.46751(12) 0.25874(11) 0.0259(3) Uani 1 1 d . . . . . H19 H 0.696374 0.512019 0.249385 0.031 Uiso 1 1 calc R U . . . H20 H 0.857288 0.510533 0.287782 0.031 Uiso 1 1 calc R U . . . C16 C 0.72300(19) 0.53226(14) 0.74125(12) 0.0347(4) Uani 1 1 d . . . . . H21 H 0.807879 0.574367 0.743506 0.042 Uiso 1 1 calc R U . . . H22 H 0.647317 0.570444 0.704206 0.042 Uiso 1 1 calc R U . . . C17 C 0.6884(2) 0.51950(18) 0.83718(13) 0.0489(5) Uani 1 1 d . . . . . H23 H 0.684374 0.588894 0.865329 0.059 Uiso 1 1 calc R U . . . H24 H 0.596618 0.486694 0.834394 0.059 Uiso 1 1 calc R U . . . C18 C 0.7952(3) 0.4530(2) 0.89488(14) 0.0644(8) Uani 1 1 d . . . . . H25 H 0.768575 0.444372 0.955645 0.077 Uiso 1 1 calc R U . . . H26 H 0.885654 0.488421 0.901737 0.077 Uiso 1 1 calc R U . . . C19 C 0.8074(2) 0.3456(2) 0.85197(13) 0.0519(6) Uani 1 1 d . . . . . H27 H 0.878985 0.304334 0.889825 0.062 Uiso 1 1 calc R U . . . H28 H 0.718775 0.308167 0.848876 0.062 Uiso 1 1 calc R U . . . C20 C 0.84542(17) 0.35685(17) 0.75695(12) 0.0374(4) Uani 1 1 d . . . . . H29 H 0.846436 0.287128 0.729005 0.045 Uiso 1 1 calc R U . . . H30 H 0.939326 0.386324 0.761215 0.045 Uiso 1 1 calc R U . . . O1 O 1.00077(12) 0.35207(11) 0.34131(9) 0.0386(3) Uani 1 1 d . . . . . O2 O 0.61465(11) 0.37332(9) 0.43975(8) 0.0300(3) Uani 1 1 d . . . . . O3 O 0.89059(11) 0.39004(10) 0.58520(8) 0.0300(3) Uani 1 1 d . . . . . O4 O 0.49835(12) 0.41208(11) 0.68175(10) 0.0405(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0370(9) 0.0348(9) 0.0459(11) 0.0044(8) 0.0039(8) 0.0087(8) C2 0.0246(7) 0.0288(8) 0.0260(8) -0.0071(6) 0.0037(6) -0.0017(6) C3 0.0208(7) 0.0233(7) 0.0219(7) -0.0009(6) 0.0034(5) -0.0050(6) C4 0.0171(6) 0.0231(7) 0.0221(7) 0.0037(5) 0.0003(5) -0.0018(5) C5 0.0186(7) 0.0232(7) 0.0223(7) 0.0026(5) 0.0033(5) -0.0027(5) C6 0.0189(7) 0.0233(7) 0.0241(7) 0.0015(6) 0.0038(5) 0.0007(5) C7 0.0149(6) 0.0257(7) 0.0227(7) 0.0018(6) 0.0025(5) -0.0011(5) C8 0.0175(7) 0.0303(8) 0.0246(7) 0.0050(6) 0.0055(5) -0.0006(6) C9 0.0196(7) 0.0276(8) 0.0297(8) 0.0090(6) 0.0047(6) -0.0003(6) C10 0.0429(10) 0.0267(9) 0.0516(11) 0.0062(8) 0.0127(8) -0.0082(7) C11 0.0232(7) 0.0298(8) 0.0274(8) -0.0052(6) 0.0032(6) -0.0061(6) C12 0.0303(8) 0.0343(9) 0.0312(9) -0.0108(7) 0.0045(7) -0.0045(7) C13 0.0407(10) 0.0473(11) 0.0229(8) -0.0051(7) 0.0041(7) -0.0005(8) C14 0.0382(9) 0.0330(9) 0.0278(8) 0.0002(7) 0.0125(7) 0.0014(7) C15 0.0284(8) 0.0241(7) 0.0264(8) 0.0007(6) 0.0083(6) -0.0003(6) C16 0.0407(10) 0.0380(9) 0.0292(9) -0.0049(7) 0.0175(7) -0.0133(8) C17 0.0631(13) 0.0556(12) 0.0338(10) -0.0102(9) 0.0262(9) -0.0243(11) C18 0.0647(15) 0.106(2) 0.0239(9) 0.0029(11) 0.0106(9) -0.0366(15) C19 0.0355(10) 0.0868(17) 0.0328(10) 0.0258(11) 0.0035(8) -0.0051(10) C20 0.0202(8) 0.0603(12) 0.0310(9) 0.0193(8) 0.0015(6) 0.0032(7) O1 0.0203(6) 0.0482(8) 0.0476(8) -0.0020(6) 0.0063(5) -0.0022(5) O2 0.0261(6) 0.0311(6) 0.0343(6) 0.0001(5) 0.0099(5) -0.0090(5) O3 0.0228(5) 0.0370(6) 0.0317(6) 0.0073(5) 0.0087(4) 0.0101(5) O4 0.0185(6) 0.0477(8) 0.0564(8) 0.0017(6) 0.0091(5) 0.0034(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 O1 C2 C1 120.76(16) . . ? O1 C2 C3 120.93(15) . . ? C1 C2 C3 118.31(14) . . ? C4 C3 C11 108.61(12) . . ? C4 C3 C15 110.52(12) . . ? C11 C3 C15 110.02(12) . . ? C4 C3 C2 105.38(12) . . ? C11 C3 C2 110.67(13) . . ? C15 C3 C2 111.52(12) . . ? O2 C4 C5 121.28(14) . . ? O2 C4 C3 120.80(13) . . ? C5 C4 C3 117.92(12) . . ? C4 C5 C6 111.25(12) . . ? C7 C6 C5 110.91(12) . . ? O3 C7 C6 121.22(13) . . ? O3 C7 C8 120.78(13) . . ? C6 C7 C8 117.99(12) . . ? C16 C8 C20 111.93(15) . . ? C16 C8 C9 110.29(13) . . ? C20 C8 C9 110.20(13) . . ? C16 C8 C7 110.06(13) . . ? C20 C8 C7 108.74(12) . . ? C9 C8 C7 105.41(12) . . ? O4 C9 C10 120.14(16) . . ? O4 C9 C8 121.32(15) . . ? C10 C9 C8 118.53(14) . . ? C12 C11 C3 112.03(13) . . ? C13 C12 C11 110.62(14) . . ? C12 C13 C14 110.98(14) . . ? C13 C14 C15 112.14(14) . . ? C14 C15 C3 112.70(13) . . ? C17 C16 C8 112.39(15) . . ? C18 C17 C16 111.36(18) . . ? C17 C18 C19 110.92(17) . . ? C20 C19 C18 110.50(18) . . ? C19 C20 C8 112.42(15) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.510(2) . ? C2 O1 1.207(2) . ? C2 C3 1.547(2) . ? C3 C4 1.537(2) . ? C3 C11 1.540(2) . ? C3 C15 1.543(2) . ? C4 O2 1.2104(18) . ? C4 C5 1.511(2) . ? C5 C6 1.522(2) . ? C6 C7 1.510(2) . ? C7 O3 1.2132(18) . ? C7 C8 1.542(2) . ? C8 C16 1.537(2) . ? C8 C20 1.539(2) . ? C8 C9 1.541(2) . ? C9 O4 1.2045(19) . ? C9 C10 1.498(2) . ? C11 C12 1.524(2) . ? C12 C13 1.523(3) . ? C13 C14 1.525(3) . ? C14 C15 1.529(2) . ? C16 C17 1.534(2) . ? C17 C18 1.521(4) . ? C18 C19 1.534(4) . ? C19 C20 1.531(3) . ? 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 O1 C2 C3 C4 -111.86(16) . . . . ? C1 C2 C3 C4 68.14(17) . . . . ? O1 C2 C3 C11 130.92(16) . . . . ? C1 C2 C3 C11 -49.08(19) . . . . ? O1 C2 C3 C15 8.1(2) . . . . ? C1 C2 C3 C15 -171.91(14) . . . . ? C11 C3 C4 O2 18.80(19) . . . . ? C15 C3 C4 O2 139.58(14) . . . . ? C2 C3 C4 O2 -99.82(16) . . . . ? C11 C3 C4 C5 -161.52(13) . . . . ? C15 C3 C4 C5 -40.74(17) . . . . ? C2 C3 C4 C5 79.87(15) . . . . ? O2 C4 C5 C6 15.1(2) . . . . ? C3 C4 C5 C6 -164.53(12) . . . . ? C4 C5 C6 C7 64.42(16) . . . . ? C5 C6 C7 O3 16.8(2) . . . . ? C5 C6 C7 C8 -162.15(12) . . . . ? O3 C7 C8 C16 138.15(16) . . . . ? C6 C7 C8 C16 -42.85(18) . . . . ? O3 C7 C8 C20 15.2(2) . . . . ? C6 C7 C8 C20 -165.78(14) . . . . ? O3 C7 C8 C9 -102.92(16) . . . . ? C6 C7 C8 C9 76.08(16) . . . . ? C16 C8 C9 O4 3.8(2) . . . . ? C20 C8 C9 O4 127.89(17) . . . . ? C7 C8 C9 O4 -114.94(17) . . . . ? C16 C8 C9 C10 -176.34(14) . . . . ? C20 C8 C9 C10 -52.27(19) . . . . ? C7 C8 C9 C10 64.89(17) . . . . ? C4 C3 C11 C12 175.81(13) . . . . ? C15 C3 C11 C12 54.71(18) . . . . ? C2 C3 C11 C12 -68.98(17) . . . . ? C3 C11 C12 C13 -57.95(18) . . . . ? C11 C12 C13 C14 57.04(19) . . . . ? C12 C13 C14 C15 -54.7(2) . . . . ? C13 C14 C15 C3 52.70(19) . . . . ? C4 C3 C15 C14 -171.82(13) . . . . ? C11 C3 C15 C14 -51.88(17) . . . . ? C2 C3 C15 C14 71.31(16) . . . . ? C20 C8 C16 C17 -50.39(19) . . . . ? C9 C8 C16 C17 72.68(19) . . . . ? C7 C8 C16 C17 -171.43(14) . . . . ? C8 C16 C17 C18 53.8(2) . . . . ? C16 C17 C18 C19 -57.4(2) . . . . ? C17 C18 C19 C20 57.9(2) . . . . ? C18 C19 C20 C8 -54.9(2) . . . . ? C16 C8 C20 C19 51.3(2) . . . . ? C9 C8 C20 C19 -71.8(2) . . . . ? C7 C8 C20 C19 173.14(16) . . . . ?