#------------------------------------------------------------------------------ #$Date: 2021-09-04 00:23:46 +0300 (Sat, 04 Sep 2021) $ #$Revision: 268443 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519018.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_4519018 loop_ _publ_author_name 'Huke, Cameron D.' 'Taylor, Laurence J.' 'Argent, Stephen P.' 'Kays, Deborah L.' _publ_section_title ; Catalyst-free Hydrophosphinylation of Isocyanates and Isothiocyanates under Low-Added-Solvent Conditions ; _journal_issue 32 _journal_name_full 'ACS Sustainable Chemistry & Engineering' _journal_page_first 10704 _journal_page_last 10709 _journal_paper_doi 10.1021/acssuschemeng.1c02907 _journal_volume 9 _journal_year 2021 _chemical_formula_moiety 'C19 H15 F N O2 P' _chemical_formula_sum 'C19 H15 F N O2 P' _chemical_formula_weight 339.29 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2021-02-18 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257) ; _cell_angle_alpha 80.225(3) _cell_angle_beta 85.954(3) _cell_angle_gamma 77.248(3) _cell_formula_units_Z 2 _cell_length_a 8.6254(3) _cell_length_b 8.9016(3) _cell_length_c 10.8499(3) _cell_measurement_reflns_used 7564 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 72.4960 _cell_measurement_theta_min 4.0980 _cell_volume 800.24(5) _computing_cell_refinement 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment 'N2 gas' _diffrn_ambient_temperature 120(2) _diffrn_crystal_treatment 'flash frozen in gaseous N2' _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.2349 _diffrn_detector_type 'Agilent Diffraction Atlas S2 detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 2.00 27.00 1.00 2.00 -- 38.00 87.00 10.05 25 2 \w 3.00 29.00 1.00 2.00 -- 38.00 86.00-110.08 26 3 \w 2.00 28.00 1.00 2.00 -- 38.00 90.00 109.76 26 4 \w -113.00 -55.00 1.00 2.00 -- -41.70 -57.00 60.00 58 5 \w -51.00 -14.00 1.00 2.00 -- -41.70 -57.00 60.00 37 6 \w -114.00 -21.00 1.00 2.00 -- -41.70 -38.00 -60.00 93 7 \w -8.00 23.00 1.00 2.00 -- -41.70 38.00 120.00 31 8 \w 27.00 93.00 1.00 2.00 -- 41.70-125.00-180.00 66 9 \w -28.00 65.00 1.00 2.00 -- 41.70 -57.00 -60.00 93 10 \w 8.00 33.00 1.00 2.00 -- 42.00 83.00-140.86 25 11 \w 13.00 38.00 1.00 2.00 -- 46.00 81.00 149.18 25 12 \w 31.00 79.00 1.00 2.00 -- 58.00 55.00-151.16 48 13 \w 28.00 58.00 1.00 2.00 -- 58.00 74.00 30.97 30 14 \w 32.00 58.00 1.00 2.00 -- 62.00 64.00 67.83 26 15 \w 32.00 66.00 1.00 2.00 -- 62.00 72.00 91.13 34 16 \w 32.00 70.00 1.00 2.00 -- 62.00 74.00-118.00 38 17 \w 31.00 57.00 1.00 2.00 -- 62.00 72.00 -69.45 26 18 \w 32.00 59.00 1.00 2.00 -- 62.00 72.00 -12.27 27 19 \w 34.00 60.00 1.00 2.00 -- 66.00 74.00-166.30 26 20 \w 35.00 63.00 1.00 2.00 -- 66.00 73.00 136.70 28 21 \w 103.00 134.00 1.00 5.00 -- 74.00 63.00 -6.26 31 22 \w 50.00 76.00 1.00 5.00 -- 74.00 63.00 -6.26 26 23 \w 46.00 75.00 1.00 5.00 -- 74.00 60.00 124.76 29 24 \w 43.00 69.00 1.00 5.00 -- 74.00 71.00 -47.40 26 25 \w 89.00 146.00 1.00 5.00 -- 82.00 66.00-157.46 57 26 \w 52.00 78.00 1.00 5.00 -- 82.00 66.00-157.46 26 27 \w 88.00 151.00 1.00 5.00 -- 86.00 66.00 26.18 63 28 \w 58.00 84.00 1.00 5.00 -- 86.00 66.00 26.18 26 29 \w 63.00 90.00 1.00 5.00 -- 86.00 51.00 6.33 27 30 \w 60.00 91.00 1.00 5.00 -- 90.00 64.00 122.00 31 31 \w 75.00 175.00 1.00 5.00 -- 104.05 61.00 150.00 100 32 \w 32.00 72.00 1.00 5.00 -- 104.05 -45.00 -90.00 40 33 \w 34.00 93.00 1.00 5.00 -- 104.05 -61.00 60.00 59 34 \w 78.00 120.00 1.00 5.00 -- 104.05 45.00 0.00 42 35 \w 75.00 130.00 1.00 5.00 -- 104.05 61.00 60.00 55 36 \w 75.00 176.00 1.00 5.00 -- 104.05 61.00 -60.00 101 37 \w 60.00 110.00 1.00 5.00 -- 104.05-125.00-150.00 50 38 \w 118.00 158.00 1.00 5.00 -- 104.05 61.00 -90.00 40 39 \w 27.00 79.00 1.00 5.00 -- 104.05 -94.00-120.00 52 40 \w 76.00 102.00 1.00 5.00 -- 104.05 61.00 -90.00 26 41 \w 76.00 102.00 1.00 5.00 -- 104.05 61.00-180.00 26 42 \w 30.00 108.00 1.00 5.00 -- 104.05-104.00 15.79 78 43 \w 77.00 145.00 1.00 5.00 -- 104.05 61.00 120.00 68 44 \w 115.00 166.00 1.00 5.00 -- 104.05 71.00-166.25 51 45 \w 31.00 108.00 1.00 5.00 -- 104.05-125.00 -30.00 77 46 \w 123.00 176.00 1.00 5.00 -- 104.05 61.00 30.00 53 47 \w 74.00 110.00 1.00 5.00 -- 104.05 71.00-166.25 36 48 \w 77.00 108.00 1.00 5.00 -- 104.05 61.00 30.00 31 49 \w 75.00 134.00 1.00 5.00 -- 104.05 61.00 90.00 59 50 \w 75.00 161.00 1.00 5.00 -- 104.05 61.00-120.00 86 51 \w 79.00 106.00 1.00 5.00 -- 104.05 -94.00 60.00 27 52 \w 34.00 74.00 1.00 5.00 -- 104.05 -94.00 60.00 40 53 \w 32.00 64.00 1.00 5.00 -- 104.05-125.00-120.00 32 54 \w 87.00 112.00 1.00 5.00 -- 104.05-125.00-120.00 25 55 \w 75.00 152.00 1.00 5.00 -- 104.05 61.00 0.00 77 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Atlas S2' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0189614000 _diffrn_orient_matrix_UB_12 0.1675032000 _diffrn_orient_matrix_UB_13 -0.0718527000 _diffrn_orient_matrix_UB_21 -0.0329479000 _diffrn_orient_matrix_UB_22 0.0644272000 _diffrn_orient_matrix_UB_23 0.1245654000 _diffrn_orient_matrix_UB_31 0.1792455000 _diffrn_orient_matrix_UB_32 -0.0094494000 _diffrn_orient_matrix_UB_33 0.0102242000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 12745 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.607 _diffrn_reflns_theta_min 4.137 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Agilent Diffraction microfocus tube' _exptl_absorpt_coefficient_mu 1.719 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.408 _exptl_crystal_description block _exptl_crystal_F_000 352 _exptl_crystal_recrystallization_method '2:1 THF:ethanol at -30C' _exptl_crystal_size_max 0.187 _exptl_crystal_size_mid 0.113 _exptl_crystal_size_min 0.037 _refine_diff_density_max 0.298 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 3141 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0277 _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^)+(0.0291P)^2^+0.4088P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.0714 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2941 _reflns_number_total 3141 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file sc1c02907_si_002.cif _cod_data_source_block ochdkl _cod_database_code 4519018 _nottingham_internal_coll_name OCHDKL _nottingham_internal_coll_number 18865 _nottingham_internal_coll_client CH/DLK _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_frame_time '2.00, 5.00' _nottingham_internal_coll_frame_width 1.00 _nottingham_internal_coll_user pcxch6 _nottingham_internal_coll_date 27/11/2020 _nottingham_internal_coll_location NOTTS _nottingham_internal_coll_instrument 'GVB, PL13110001' _nottingham_internal_process_date 03/12/2020 _nottingham_internal_process_user pcxch6 _nottingham_internal_solution_date 14/10/2020 _nottingham_internal_solution_user pcxch6 _nottingham_internal_refinement_date 14/10/2020 _nottingham_internal_refinement_user pcxch6 _nottingham_internal_self_archive_date 16/02/2021 _nottingham_internal_self_validation_date 16/02/2021 _nottingham_internal_self_validation_user pcxch6 _nottingham_internal_validation_date 17/02/2021 _nottingham_internal_validation_user pczspa _nottingham_internal_archive_date 17/02/2021 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C20 H18 N1 O2 P1' _chemical_oxdiff_usercomment 'OCHDKL #18865 GVB-1859 for CH/DLK in fomblin film on a micromount' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.939 _shelx_estimated_absorpt_t_min 0.739 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 2. Restrained distances N1-H1 0.88 with sigma of 0.02 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18) ; _shelx_res_file ; TITL ochdkl_a.res in P-1 ochdkl.res created by SHELXL-2018/3 at 10:52:13 on 18-Feb-2021 REM Old TITL OCHDKL in P-1 REM SHELXT solution in P-1: R1 0.079, Rweak 0.006, Alpha 0.029 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N O3 P CELL 1.54184 8.6254 8.9016 10.8499 80.225 85.954 77.248 ZERR 2 0.0003 0.0003 0.0003 0.003 0.003 0.003 LATT 1 SFAC C H F N O P UNIT 38 30 2 2 4 2 EQIV $1 1-X,1-Y,-Z DFIX 0.88 N1 H1 L.S. 20 PLAN 5 SIZE 0.037 0.113 0.187 TEMP -153(2) CONF HTAB N1 O1_$1 BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.029100 0.408800 FVAR 1.03993 P1 6 0.486706 0.398865 0.224999 11.00000 0.01830 0.01335 = 0.01305 -0.00248 0.00028 -0.00224 F1 3 0.048996 0.805725 0.253073 11.00000 0.02560 0.02796 = 0.02865 -0.00090 0.00770 -0.00519 O1 5 0.481493 0.355869 0.098639 11.00000 0.02616 0.01806 = 0.01473 -0.00391 0.00065 -0.00496 O2 5 0.351760 0.652217 0.331359 11.00000 0.03222 0.01863 = 0.01712 -0.00525 -0.00196 0.00023 N1 4 0.325037 0.682738 0.119255 11.00000 0.02046 0.01566 = 0.01504 -0.00384 0.00010 -0.00044 H1 2 0.370462 0.645685 0.053998 11.00000 -1.20000 C1 1 0.682898 0.407035 0.265945 11.00000 0.01871 0.01362 = 0.01921 -0.00527 0.00080 -0.00083 C2 1 0.773307 0.486543 0.175533 11.00000 0.02393 0.01832 = 0.01977 -0.00234 0.00037 -0.00360 AFIX 43 H2 2 0.732556 0.529398 0.095056 11.00000 -1.20000 AFIX 0 C3 1 0.922290 0.502112 0.204401 11.00000 0.02255 0.02365 = 0.02835 -0.00407 0.00485 -0.00644 AFIX 43 H3 2 0.983729 0.556062 0.143565 11.00000 -1.20000 AFIX 0 C4 1 0.982220 0.439211 0.321862 11.00000 0.01703 0.02794 = 0.03337 -0.00921 -0.00110 -0.00178 AFIX 43 H4 2 1.083941 0.451437 0.341348 11.00000 -1.20000 AFIX 0 C5 1 0.894587 0.358841 0.410652 11.00000 0.02237 0.02661 = 0.02297 -0.00478 -0.00392 0.00182 AFIX 43 H5 2 0.936804 0.314655 0.490447 11.00000 -1.20000 AFIX 0 C6 1 0.744619 0.342755 0.383037 11.00000 0.02114 0.01826 = 0.01906 -0.00331 0.00083 -0.00066 AFIX 43 H6 2 0.684252 0.287873 0.444106 11.00000 -1.20000 AFIX 0 C7 1 0.403114 0.275954 0.348343 11.00000 0.01597 0.01607 = 0.01577 -0.00115 -0.00051 -0.00150 C8 1 0.367154 0.140960 0.319022 11.00000 0.02237 0.01856 = 0.01767 -0.00324 -0.00252 -0.00259 AFIX 43 H8 2 0.388150 0.116670 0.236715 11.00000 -1.20000 AFIX 0 C9 1 0.300681 0.042261 0.410271 11.00000 0.02650 0.01850 = 0.02564 -0.00135 -0.00387 -0.00729 AFIX 43 H9 2 0.277384 -0.050295 0.390736 11.00000 -1.20000 AFIX 0 C10 1 0.268381 0.078854 0.529755 11.00000 0.02310 0.02312 = 0.02319 0.00315 0.00204 -0.00530 AFIX 43 H10 2 0.221745 0.011749 0.591747 11.00000 -1.20000 AFIX 0 C11 1 0.303660 0.212911 0.559613 11.00000 0.02477 0.02444 = 0.01709 -0.00307 0.00280 -0.00123 AFIX 43 H11 2 0.281133 0.237121 0.641842 11.00000 -1.20000 AFIX 0 C12 1 0.371652 0.311510 0.469785 11.00000 0.02106 0.01755 = 0.01866 -0.00407 0.00017 -0.00175 AFIX 43 H12 2 0.396793 0.402706 0.490428 11.00000 -1.20000 AFIX 0 C13 1 0.373554 0.602470 0.232095 11.00000 0.01794 0.01521 = 0.01754 -0.00306 -0.00034 -0.00328 C15 1 0.314357 0.946464 0.009080 11.00000 0.02227 0.02042 = 0.02007 -0.00334 0.00001 -0.00276 AFIX 43 H15 2 0.405493 0.907965 -0.039965 11.00000 -1.20000 AFIX 0 C16 1 0.243958 1.104159 -0.011392 11.00000 0.03391 0.01873 = 0.02367 0.00041 -0.00168 -0.00461 AFIX 43 H16 2 0.286318 1.173043 -0.074760 11.00000 -1.20000 AFIX 0 C17 1 0.111860 1.161116 0.060623 11.00000 0.03431 0.01664 = 0.02617 -0.00401 -0.00656 0.00389 AFIX 43 H17 2 0.065343 1.269495 0.047778 11.00000 -1.20000 AFIX 0 C18 1 0.047406 1.060973 0.151099 11.00000 0.02298 0.02566 = 0.02401 -0.00869 -0.00160 0.00358 AFIX 43 H18 2 -0.043515 1.099503 0.200346 11.00000 -1.20000 AFIX 0 C19 1 0.117376 0.904174 0.168631 11.00000 0.01964 0.02230 = 0.01802 -0.00259 -0.00080 -0.00436 C20 1 0.252527 0.844372 0.100826 11.00000 0.01896 0.01582 = 0.01690 -0.00316 -0.00425 -0.00117 HKLF 4 REM ochdkl_a.res in P-1 REM wR2 = 0.0714, GooF = S = 1.038, Restrained GooF = 1.038 for all data REM R1 = 0.0277 for 2941 Fo > 4sig(Fo) and 0.0297 for all 3141 data REM 220 parameters refined using 1 restraints END WGHT 0.0291 0.4090 REM Highest difference peak 0.298, deepest hole -0.336, 1-sigma level 0.041 Q1 1 0.4218 0.5065 0.2330 11.00000 0.05 0.30 Q2 1 0.5964 0.4047 0.2501 11.00000 0.05 0.29 Q3 1 0.4335 0.3309 0.2951 11.00000 0.05 0.28 Q4 1 0.7221 0.4534 0.2294 11.00000 0.05 0.21 Q5 1 0.2818 0.8982 0.0573 11.00000 0.05 0.21 ; _shelx_res_checksum 61160 _shelx_hkl_file ; 0 0 1 28.23 1.36 0 0 -1 29.81 1.24 0 0 2 876.56 23.63 0 0 -2 905.96 23.24 0 0 3 57.08 3.25 0 0 -3 61.34 2.94 0 0 -4 26.25 2.43 0 0 -4 24.73 1.66 0 0 4 23.90 2.38 0 0 -4 20.94 2.01 0 0 5 70.73 3.37 0 0 -5 73.16 4.63 0 0 -5 74.96 3.42 0 0 5 80.73 4.93 0 0 -5 68.50 4.16 0 0 -6 78.24 3.80 0 0 -6 76.55 3.76 0 0 6 67.12 5.07 0 0 -6 69.06 4.63 0 0 -7 136.42 5.89 0 0 -7 130.95 7.19 0 0 7 139.79 8.20 0 0 -8 90.28 7.14 0 0 8 90.23 7.10 0 0 -8 94.69 5.06 0 0 8 92.37 5.14 0 0 -8 91.27 4.97 0 0 8 84.47 5.10 0 0 -8 91.26 4.90 0 0 -9 788.86 28.35 0 0 9 800.62 28.37 0 0 -9 782.02 23.13 0 0 9 769.04 23.21 0 0 -9 761.08 23.10 0 0 9 724.52 23.21 0 0 -9 780.90 23.10 0 0 -10 0.60 1.26 0 0 10 2.09 1.33 0 0 -10 0.54 1.38 0 0 10 1.90 1.62 0 0 10 0.25 1.56 0 0 -11 47.14 3.56 0 0 -11 50.81 3.64 0 0 11 47.49 3.59 0 0 11 47.41 3.82 0 0 -12 103.19 4.89 0 0 12 102.98 5.25 0 0 -12 114.64 5.02 0 0 12 97.82 4.78 0 0 13 86.23 3.78 0 0 -13 72.66 3.21 0 1 -12 40.58 2.80 0 -1 12 40.14 2.94 0 -1 12 41.49 2.84 0 -1 11 161.54 7.38 0 1 -11 165.66 7.25 0 -1 11 162.44 7.28 0 1 -11 170.00 6.97 0 1 -10 21.24 2.68 0 1 -10 26.73 2.60 0 -1 10 16.49 2.53 0 -1 10 17.46 2.52 0 1 -10 21.09 2.48 0 1 -9 433.45 14.24 0 1 -9 421.28 13.95 0 1 -9 419.62 14.40 0 -1 9 413.65 14.77 0 -1 9 390.85 14.51 0 1 -9 438.66 18.60 0 1 -8 39.33 3.11 0 -1 8 38.26 3.14 0 1 -8 41.02 3.28 0 -1 8 35.90 3.36 0 -1 8 41.80 3.64 0 -1 8 40.06 4.85 0 1 -8 39.13 4.69 0 1 -7 795.63 23.02 0 1 -7 780.24 23.06 0 -1 7 779.94 23.46 0 1 -7 817.41 23.00 0 1 -7 817.29 25.37 0 1 -7 801.10 26.67 0 -1 7 819.18 26.99 0 -1 6 1015.72 30.96 0 1 -6 978.68 29.50 0 1 -6 1007.25 30.68 0 1 -6 1022.48 27.63 0 -1 5 5.95 1.72 0 1 -5 5.96 1.50 0 -1 5 7.72 1.76 0 -1 5 6.60 1.14 0 -1 4 2.93 1.33 0 1 -4 2.02 1.11 0 -1 4 3.62 1.25 0 -1 3 553.45 16.66 0 1 -3 564.52 16.53 0 -1 3 561.46 16.44 0 1 -3 574.25 16.89 0 -1 2 2086.18 52.99 0 1 -2 2055.54 52.79 0 -1 1 886.95 23.43 0 1 -1 909.45 23.23 0 -1 0 966.21 25.62 0 1 0 1013.24 25.26 0 -1 -1 6.46 0.94 0 1 1 6.68 0.77 0 -1 -1 7.28 0.52 0 1 2 8341.74 205.49 0 -1 -2 8252.35 205.39 0 -1 -3 4.58 1.17 0 1 3 3.41 1.03 0 -1 -3 4.36 1.26 0 1 3 6.08 1.21 0 1 4 6.31 1.46 0 -1 -4 5.20 1.20 0 -1 -4 7.54 1.14 0 -1 -4 6.88 1.19 0 1 5 3.94 1.41 0 -1 -5 4.26 1.36 0 -1 -5 3.25 1.00 0 -1 -5 5.50 1.08 0 1 5 4.92 0.93 0 1 6 18.30 1.72 0 -1 -6 18.65 1.76 0 -1 -6 15.01 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-4 4 0.79 0.57 -8 3 5 30.50 2.41 8 -3 -5 30.79 2.20 8 -3 -4 7.89 1.43 8 -3 -3 3.79 1.22 8 -3 -2 35.54 2.65 8 -3 -2 30.29 2.68 8 -3 -1 266.99 8.90 8 -3 -1 258.28 9.47 8 -3 0 3.77 1.35 8 -3 0 1.60 0.96 8 -3 1 30.23 2.54 8 -3 1 35.04 2.51 8 -3 2 41.08 2.97 8 -3 3 251.90 8.99 8 -3 4 28.48 2.35 8 -3 5 18.99 1.76 8 -3 6 15.05 1.38 8 -2 -7 30.38 1.84 8 -2 -6 8.79 1.18 8 -2 -5 6.56 1.20 8 -2 -5 6.00 1.28 8 -2 -4 46.94 2.95 8 -2 -4 44.21 3.18 8 -2 -3 -0.30 0.77 8 -2 -3 1.85 1.03 8 -2 -3 2.56 1.39 8 -2 -2 16.29 1.81 8 -2 -2 19.25 1.97 8 -2 -2 16.71 2.14 8 -2 -2 14.80 2.13 8 -2 -1 64.29 4.17 8 -2 -1 74.59 3.88 8 -2 -1 70.77 4.15 8 -2 0 8.08 1.58 8 -2 0 8.19 1.31 8 -2 0 11.56 1.80 8 -2 1 44.67 3.17 8 -2 1 50.62 3.64 8 -2 2 434.73 14.45 8 -2 3 586.52 18.27 -8 2 -4 400.70 13.27 8 -2 4 413.30 13.47 8 -2 5 45.03 3.14 8 -2 6 17.11 1.74 8 -2 7 2.37 0.80 8 -1 -7 13.04 1.43 -8 1 7 14.99 1.66 8 -1 -6 126.88 5.38 8 -1 -5 193.78 7.66 -8 1 5 218.70 8.80 8 -1 -4 22.25 2.36 8 -1 -4 24.71 2.37 8 -1 -3 4.50 1.47 8 -1 -3 5.49 1.43 8 -1 -3 6.96 1.29 8 -1 -2 166.16 7.18 8 -1 -2 163.14 7.29 8 -1 -2 161.10 6.91 8 -1 -2 163.83 6.99 -8 1 2 174.03 11.73 8 -1 -1 33.03 3.05 8 -1 -1 40.45 3.27 8 -1 -1 36.36 2.89 8 -1 -1 32.84 2.99 -8 1 1 39.80 5.49 8 -1 0 113.87 5.63 8 -1 0 110.01 5.35 8 -1 0 108.55 5.82 -8 1 0 104.44 9.00 8 -1 1 -0.86 1.21 8 -1 1 2.10 1.19 8 -1 1 3.13 1.63 -8 1 -1 -2.35 2.46 8 -1 2 26.04 2.30 8 -1 2 23.39 2.81 8 -1 2 20.80 2.34 8 -1 2 25.21 2.36 8 -1 3 40.61 3.31 -8 1 -3 43.08 5.50 8 -1 3 40.96 3.54 8 -1 4 254.85 9.68 8 -1 4 246.95 9.73 8 -1 5 23.31 2.14 8 -1 5 16.46 2.26 8 -1 6 134.14 5.85 8 -1 7 121.16 4.95 8 0 -8 74.12 3.17 8 0 -7 275.65 9.24 -8 0 7 298.32 9.45 8 0 -6 19.57 2.04 -8 0 5 12.29 1.97 8 0 -5 11.92 1.87 -8 0 4 23.20 2.71 8 0 -4 23.23 2.49 8 0 -3 3.66 1.44 8 0 -3 4.49 1.37 -8 0 3 5.78 2.69 8 0 -3 4.38 1.27 8 0 -2 39.79 3.26 8 0 -2 39.41 3.22 8 0 -2 44.65 3.48 8 0 -2 40.06 3.25 -8 0 2 42.99 5.63 8 0 -1 32.01 2.95 8 0 -1 33.07 3.11 8 0 -1 31.76 2.88 8 0 -1 33.64 3.17 -8 0 1 39.71 5.46 8 0 0 289.85 10.67 8 0 0 306.59 11.32 8 0 0 293.02 11.10 8 0 0 290.56 10.70 8 0 1 30.79 2.68 8 0 1 31.99 2.73 8 0 1 26.25 2.59 8 0 1 26.04 2.77 8 0 1 25.80 2.96 8 0 1 25.27 2.54 8 0 2 0.76 1.02 8 0 2 3.13 1.23 8 0 2 2.01 1.10 8 0 2 2.49 1.49 8 0 2 1.74 1.14 8 0 3 2.11 1.19 8 0 3 2.04 1.38 -8 0 -3 4.58 2.51 8 0 3 1.91 1.22 8 0 4 44.19 3.57 -8 0 -4 35.26 5.05 8 0 4 39.10 3.31 8 0 4 35.99 3.05 8 0 5 22.27 2.55 8 0 5 21.14 2.12 8 0 5 23.88 2.28 8 0 5 22.31 2.56 8 0 6 0.21 0.95 8 0 6 0.48 0.98 8 0 6 0.84 0.96 8 0 7 179.52 6.77 8 0 7 185.78 6.94 8 0 8 221.89 7.49 8 1 -7 95.16 4.23 8 1 -6 0.28 0.97 -8 -1 5 2.92 1.20 8 1 -5 6.13 1.55 -8 -1 4 46.85 3.75 8 1 -4 49.06 3.56 -8 -1 3 6.41 1.60 8 1 -3 6.80 1.82 8 1 -3 5.95 1.38 8 1 -2 8.93 1.91 8 1 -2 15.18 2.08 8 1 -1 665.35 19.72 8 1 -1 655.62 20.30 8 1 -1 677.52 20.60 8 1 -1 660.53 20.47 8 1 0 96.53 5.07 8 1 0 98.01 5.31 8 1 0 101.43 5.70 8 1 0 95.92 5.48 8 1 1 39.45 3.16 8 1 1 42.32 3.45 8 1 1 42.88 3.65 8 1 1 39.43 3.16 8 1 1 39.90 3.44 8 1 2 11.84 1.92 8 1 2 16.03 2.29 8 1 2 12.04 2.17 8 1 2 17.01 2.23 8 1 2 14.01 2.14 8 1 3 1.48 1.13 8 1 3 0.18 1.35 8 1 3 0.35 1.29 8 1 3 -0.91 1.14 8 1 3 1.99 1.26 8 1 4 13.04 2.14 8 1 4 10.18 1.76 8 1 4 13.17 2.11 8 1 4 11.39 1.96 8 1 5 241.04 9.64 8 1 5 245.77 8.95 8 1 5 256.59 9.18 8 1 5 244.49 9.45 8 1 6 15.14 2.09 8 1 6 16.32 1.94 8 1 6 20.69 2.23 8 1 7 58.82 3.58 8 1 7 55.93 3.38 8 1 7 54.47 3.18 8 1 8 73.39 3.61 8 1 8 71.49 3.64 8 1 9 56.31 2.75 8 2 -7 77.42 3.47 8 2 -6 18.34 1.80 -8 -2 5 14.48 2.05 8 2 -5 13.48 1.87 -8 -2 4 32.75 3.07 8 2 -4 27.51 2.66 8 2 -3 2.54 1.05 -8 -2 3 6.05 1.70 8 2 -3 3.18 1.41 8 2 -2 31.35 2.67 8 2 -2 28.51 2.87 8 2 -2 30.63 2.87 -8 -2 2 35.60 5.17 8 2 -1 94.46 5.00 8 2 -1 101.73 5.45 8 2 -1 88.99 5.14 -8 -2 1 98.67 8.18 8 2 0 20.27 2.58 8 2 0 15.08 2.38 8 2 0 13.21 2.07 8 2 0 18.37 2.22 8 2 1 45.72 3.61 8 2 1 49.20 3.82 8 2 1 46.29 3.60 8 2 1 45.16 3.43 8 2 1 50.37 3.65 8 2 2 2.19 1.32 8 2 2 2.56 1.44 8 2 2 2.13 1.39 8 2 2 0.74 1.13 8 2 3 80.37 4.83 8 2 3 73.12 4.57 8 2 3 77.24 4.70 8 2 3 75.94 4.60 8 2 4 49.36 3.68 -8 -2 -4 52.70 5.57 8 2 4 55.36 3.80 8 2 4 55.38 3.68 8 2 4 48.12 3.85 8 2 5 22.74 2.56 8 2 5 21.79 2.12 8 2 5 21.97 2.50 8 2 5 22.56 2.35 8 2 5 23.33 2.25 -8 -2 -5 18.26 3.44 8 2 6 17.97 2.21 8 2 6 22.46 2.19 8 2 6 20.12 2.06 8 2 7 1.83 0.99 8 2 7 1.92 0.95 8 2 8 164.15 6.29 8 2 8 157.93 6.19 8 2 9 8.58 1.16 8 3 -6 0.87 0.80 8 3 -6 0.48 0.70 -8 -3 5 28.44 2.71 8 3 -5 28.51 2.33 8 3 -5 36.35 2.50 8 3 -4 139.06 5.92 -8 -3 4 155.67 6.91 8 3 -4 140.04 6.15 8 3 -3 1.57 1.29 -8 -3 3 0.52 2.00 8 3 -3 0.64 1.00 8 3 -2 371.99 12.77 -8 -3 2 381.25 17.93 8 3 -2 380.50 12.78 8 3 -1 294.46 10.59 8 3 -1 276.56 10.44 8 3 0 69.26 4.36 8 3 0 65.26 4.35 -8 -3 0 73.47 6.87 8 3 0 70.48 4.45 8 3 1 3.74 1.46 8 3 1 1.46 1.41 8 3 1 2.17 1.63 8 3 1 2.39 1.42 8 3 2 14.12 2.13 8 3 2 12.14 2.10 8 3 2 12.68 1.99 8 3 2 11.74 1.82 8 3 2 9.59 1.72 8 3 3 0.93 1.18 8 3 3 3.06 1.39 8 3 3 -0.26 1.17 8 3 3 0.74 1.30 8 3 4 17.62 2.09 8 3 4 14.27 1.89 8 3 4 18.02 2.37 8 3 5 60.02 3.61 8 3 5 59.80 4.03 8 3 6 260.58 9.95 8 3 6 261.76 9.30 8 3 6 255.03 9.58 -8 -3 -7 288.44 9.57 8 3 7 276.66 9.73 8 3 7 287.72 10.20 8 3 8 11.50 1.51 8 3 8 13.22 1.59 8 3 9 291.77 8.79 8 3 9 286.38 9.02 8 4 -6 31.48 2.17 -8 -4 6 38.32 2.32 8 4 -5 123.57 5.11 8 4 -5 120.30 5.14 8 4 -4 3.93 1.11 -8 -4 4 3.12 1.23 8 4 -4 2.95 1.05 -8 -4 4 3.90 1.15 8 4 -4 3.25 1.05 8 4 -3 20.69 2.21 -8 -4 3 21.05 2.40 8 4 -3 19.82 2.07 8 4 -2 290.40 10.57 8 4 -2 280.10 10.03 -8 -4 2 305.56 15.45 8 4 -1 51.18 3.73 8 4 -1 51.77 3.55 -8 -4 1 54.20 5.85 8 4 0 1613.36 43.46 -8 -4 0 1625.11 49.46 8 4 0 1561.24 42.93 8 4 1 64.27 4.28 8 4 1 62.12 3.90 8 4 1 64.77 4.20 8 4 2 26.91 2.85 8 4 2 28.98 2.75 8 4 2 28.87 2.99 8 4 3 2.29 1.12 8 4 3 2.06 1.39 -8 -4 -4 55.24 5.80 8 4 4 57.61 3.97 8 4 4 60.52 4.17 8 4 5 12.51 1.89 8 4 5 13.70 2.05 8 4 6 7.04 1.51 8 4 6 4.74 1.14 8 4 7 191.45 7.17 -8 -4 -8 94.93 4.26 8 4 8 92.97 4.23 8 4 8 97.82 4.44 8 4 9 291.56 9.06 8 4 9 302.31 8.94 8 5 -5 16.04 1.55 8 5 -4 48.49 3.20 -8 -5 4 63.41 3.55 8 5 -3 1.12 1.11 8 5 -2 143.40 6.54 8 5 -1 53.45 3.32 8 5 -1 52.21 3.73 8 5 0 37.86 3.30 -8 -5 0 40.50 4.83 8 5 0 33.84 2.80 -8 -5 -1 286.98 13.98 8 5 1 272.01 10.01 8 5 1 286.00 10.58 -8 -5 -2 138.72 9.37 8 5 2 131.72 6.29 8 5 2 140.03 6.57 -8 -5 -3 1.36 1.97 8 5 3 2.29 1.37 8 5 3 2.22 1.23 8 5 4 21.59 2.36 8 5 4 22.09 2.47 8 5 5 37.09 2.98 8 5 5 35.19 3.02 8 5 6 9.13 1.56 8 5 6 12.16 1.81 8 5 7 139.97 5.54 8 5 8 5.65 0.97 8 5 8 3.65 1.00 8 6 -5 20.10 1.55 -8 -6 5 19.41 1.63 8 6 -4 386.72 12.05 -8 -6 4 399.77 12.03 8 6 -3 37.45 2.78 -8 -6 3 40.37 2.71 8 6 -2 82.09 4.52 -8 -6 2 87.34 4.23 8 6 -1 95.16 5.03 8 6 0 3.68 1.43 -8 -6 0 0.97 1.08 8 6 1 11.91 1.86 -8 -6 -1 12.25 1.81 8 6 1 13.12 1.72 8 6 2 8.53 1.58 8 6 2 6.48 1.50 8 6 3 174.62 7.32 8 6 3 163.24 7.04 8 6 4 46.02 3.41 8 6 4 50.49 3.33 8 6 5 409.51 13.42 8 6 5 408.28 12.85 8 6 6 180.20 7.03 8 6 6 168.01 6.33 -8 -6 -7 5.03 0.99 8 6 8 35.31 2.19 8 7 -4 100.77 3.96 8 7 -3 133.83 5.35 -8 -7 3 145.25 5.15 8 7 -2 7.59 1.33 -8 -7 2 4.53 1.24 8 7 -1 7.57 1.40 -8 -7 1 13.40 1.77 8 7 0 6.00 1.33 -8 -7 0 6.70 1.46 8 7 1 0.87 0.88 -8 -7 -1 3.05 1.14 8 7 1 0.69 0.88 8 7 2 6.99 1.31 8 7 2 9.07 1.53 8 7 3 7.60 1.40 8 7 3 10.70 1.55 8 7 4 18.74 2.09 8 7 4 23.17 1.95 8 7 5 9.30 1.45 8 7 5 8.40 1.18 8 7 6 104.08 4.63 -8 -7 -7 9.17 1.09 8 7 7 10.55 1.22 8 8 -2 28.06 1.81 8 8 -1 26.06 1.88 -8 -8 0 214.82 7.08 8 8 0 203.97 7.05 -8 -8 -1 28.75 2.03 8 8 1 27.44 2.01 8 8 2 75.43 3.58 8 8 2 84.53 3.63 8 8 3 -0.96 0.74 8 8 3 1.70 0.73 -8 -8 -4 34.83 2.24 8 8 4 32.53 2.26 8 8 5 82.12 3.73 8 8 6 56.30 2.74 9 -3 -2 27.92 1.91 9 -3 -1 20.12 1.62 9 -3 -1 20.86 1.63 9 -3 0 48.55 2.72 9 -3 1 6.68 1.10 9 -3 1 4.17 0.84 9 -3 2 92.13 3.95 9 -3 2 97.87 3.77 9 -3 3 133.79 4.76 9 -2 -4 11.36 1.11 9 -2 -3 97.63 3.82 9 -2 -2 6.21 1.02 9 -2 -2 6.92 1.25 9 -2 -1 48.13 2.98 9 -2 -1 49.24 2.93 9 -2 0 5.86 1.13 9 -2 0 4.03 1.13 9 -2 0 6.20 1.12 9 -2 1 6.13 1.31 9 -2 1 3.22 0.98 9 -2 2 1.48 0.92 9 -2 2 -0.76 0.86 9 -2 3 397.03 12.18 9 -2 3 402.95 12.21 9 -2 4 2.96 0.78 9 -2 4 5.09 1.05 9 -2 5 83.84 3.44 9 -1 -5 134.65 4.92 9 -1 -4 291.23 9.23 9 -1 -3 3.81 1.06 9 -1 -3 3.48 0.83 9 -1 -2 0.36 0.83 9 -1 -2 1.01 0.86 9 -1 -1 53.60 3.16 9 -1 -1 64.50 3.57 9 -1 -1 52.90 3.41 9 -1 -1 56.85 3.40 9 -1 0 2.44 0.84 9 -1 0 3.32 1.21 9 -1 0 4.23 1.36 9 -1 1 121.70 5.76 9 -1 1 131.77 5.85 9 -1 2 11.92 1.80 9 -1 2 10.84 1.75 9 -1 3 125.69 5.47 9 -1 3 120.86 5.50 9 -1 4 79.26 3.83 9 -1 4 78.50 4.04 9 -1 5 482.92 13.96 9 -1 5 532.17 14.76 9 -1 6 4.76 0.85 9 0 -6 32.31 1.95 9 0 -5 68.69 3.40 9 0 -4 203.69 7.36 9 0 -3 17.92 1.93 9 0 -2 233.93 8.49 9 0 -2 238.31 8.59 9 0 -1 368.69 12.40 9 0 -1 375.72 12.17 9 0 0 50.36 3.33 9 0 0 50.67 3.56 9 0 0 53.55 3.64 9 0 1 85.02 4.41 9 0 1 88.89 4.83 9 0 1 86.60 4.83 9 0 2 -0.74 1.05 9 0 2 -0.71 1.30 9 0 3 204.31 7.75 9 0 3 198.94 7.75 9 0 3 199.63 7.98 9 0 4 21.35 2.03 9 0 4 23.98 2.33 9 0 5 125.34 4.83 9 0 5 121.11 5.24 9 0 6 63.82 3.15 9 1 -6 111.10 4.27 9 1 -5 14.27 1.56 9 1 -4 48.10 3.05 9 1 -3 50.93 3.33 9 1 -2 56.75 3.60 9 1 -2 53.82 3.42 9 1 -1 94.69 4.92 9 1 -1 95.13 4.94 9 1 0 -0.04 1.13 9 1 0 1.29 1.36 9 1 0 -0.23 1.11 9 1 0 1.07 0.93 9 1 1 110.32 5.45 9 1 1 122.34 5.89 9 1 1 119.04 5.24 9 1 1 119.11 5.84 9 1 1 107.84 5.09 9 1 2 1.90 1.20 9 1 2 4.06 1.63 9 1 2 2.24 1.02 9 1 2 2.06 1.18 9 1 2 2.42 1.04 9 1 3 0.54 1.28 9 1 3 0.33 0.80 9 1 3 2.66 1.12 9 1 4 70.63 4.02 9 1 4 64.22 3.65 9 1 4 67.37 3.96 9 1 5 125.58 5.62 9 1 5 132.09 5.09 9 1 5 125.76 5.48 9 1 6 18.43 1.80 9 1 6 14.74 1.54 9 2 -6 3.81 0.73 9 2 -5 3.36 0.92 9 2 -4 7.89 1.37 9 2 -3 280.21 9.77 9 2 -2 2.45 1.27 9 2 -1 91.35 4.78 9 2 -1 73.86 3.98 9 2 0 49.71 3.61 9 2 0 53.55 3.68 9 2 0 45.93 3.19 9 2 1 17.79 2.28 9 2 1 21.33 2.42 9 2 1 18.58 2.27 9 2 1 18.90 2.13 9 2 2 147.83 6.58 9 2 2 150.06 6.61 9 2 2 151.84 6.40 9 2 2 134.77 6.35 9 2 2 140.97 6.32 9 2 3 0.68 1.14 9 2 3 1.09 1.13 9 2 3 2.15 1.06 9 2 3 1.46 1.10 9 2 4 6.51 1.37 9 2 4 9.07 1.49 9 2 4 6.99 1.47 9 2 4 5.55 1.33 9 2 5 18.56 2.06 9 2 5 21.97 2.02 9 2 6 367.97 11.52 9 2 6 343.60 10.59 9 2 7 41.93 2.54 9 3 -5 34.44 2.05 9 3 -4 4.91 1.10 9 3 -3 29.71 2.39 9 3 -3 30.54 2.17 9 3 -2 15.04 1.93 9 3 -2 15.77 1.71 9 3 -1 138.04 6.18 9 3 -1 140.15 5.98 9 3 0 152.54 6.73 9 3 0 157.56 6.62 9 3 1 6.44 1.73 9 3 1 7.15 1.52 9 3 2 39.52 2.90 9 3 2 35.83 2.91 9 3 3 3.83 1.41 9 3 3 2.66 1.11 9 3 3 2.32 1.56 9 3 4 203.84 7.49 9 3 4 203.07 7.96 9 3 4 194.23 7.78 9 3 5 47.85 2.78 9 3 5 47.26 3.24 9 3 5 46.61 3.14 9 3 6 25.52 2.21 9 3 7 2.13 0.92 9 4 -4 20.83 1.59 9 4 -3 1.88 0.89 9 4 -3 1.65 0.87 9 4 -2 323.92 10.38 9 4 -2 312.84 10.47 9 4 -1 455.71 14.17 9 4 -1 465.66 14.44 9 4 0 1.93 1.19 9 4 0 0.97 1.02 9 4 1 358.02 12.08 9 4 2 76.69 4.35 9 4 3 5.37 1.45 9 4 4 128.42 5.75 9 4 5 22.07 2.20 9 4 5 20.35 2.07 9 4 6 69.09 3.73 9 4 7 185.40 6.59 9 5 -4 37.86 2.09 9 5 -3 0.93 0.78 9 5 -2 105.33 4.74 9 5 -1 2.84 1.20 9 5 0 43.22 3.08 9 5 1 502.71 15.61 9 5 2 83.11 4.44 9 5 3 193.13 7.49 9 5 4 45.00 3.02 9 5 5 208.79 7.51 9 5 6 7.90 1.26 9 5 7 82.75 3.65 9 6 -3 14.93 1.33 9 6 -2 7.60 1.21 9 6 -1 61.62 3.37 9 6 0 23.54 2.14 9 6 1 19.37 1.97 9 6 2 61.28 3.53 9 6 3 137.13 5.63 9 6 4 58.07 3.18 9 6 5 35.56 2.26 9 7 -1 22.06 1.67 9 7 0 54.39 2.87 9 7 1 19.85 1.69 9 7 2 50.32 2.76 9 7 3 67.32 3.17 9 7 4 35.51 2.00 10 -1 0 272.46 8.42 10 -1 1 15.95 1.42 10 -1 2 37.30 2.08 10 0 -3 44.15 2.21 10 0 -2 1.06 0.67 10 0 -1 140.63 5.10 10 0 0 25.06 1.94 10 0 1 49.77 2.79 10 0 2 14.58 1.49 10 0 2 19.16 1.73 10 0 3 84.01 3.50 10 0 3 78.17 3.56 10 0 4 9.75 1.07 10 1 -3 75.32 3.32 10 1 -2 43.82 2.55 10 1 -1 283.93 9.13 10 1 0 9.53 1.37 10 1 1 428.43 12.97 10 1 2 -0.86 0.73 10 1 3 32.82 2.27 10 1 4 7.04 1.09 10 2 -3 142.89 5.17 10 2 -2 2.41 0.89 10 2 -1 187.53 6.77 10 2 0 18.64 1.85 10 2 1 76.49 3.46 10 2 2 -0.42 0.64 10 2 3 17.87 1.53 10 2 4 3.04 0.77 10 3 -3 -0.76 0.70 10 3 -2 121.45 4.69 10 3 -1 23.83 1.91 10 3 0 276.73 8.78 10 3 1 1.03 0.77 10 3 2 20.68 1.79 10 3 3 4.14 0.96 10 3 3 5.76 0.98 10 3 4 41.35 2.41 10 3 5 2.04 0.64 10 4 -1 0.93 0.61 10 4 0 3.43 0.86 10 4 1 13.07 1.47 10 4 2 463.89 13.70 10 4 3 6.35 1.12 10 4 3 4.78 0.89 10 4 4 54.51 2.82 10 4 4 51.88 2.67 10 4 5 95.65 3.79 10 5 -1 185.59 6.08 10 5 0 55.70 2.81 10 5 1 163.96 5.88 10 5 2 141.55 5.32 10 5 3 26.46 1.88 10 5 4 16.32 1.38 10 6 1 37.72 2.09 10 6 2 56.05 2.64 0 0 0 0.00 0.00 TITL OCHDKL in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.625421 8.901559 10.849883 80.2245 85.9541 77.2484 ZERR 1.00 0.000303 0.000270 0.000349 0.0026 0.0027 0.0028 LATT 1 SFAC C H N O P UNIT 20.00 18.00 1.00 2.00 1.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 5235 _olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount' _olex2_submission_original_sample_id OCHDKL _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.280 _oxdiff_exptl_absorpt_empirical_full_min 0.836 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.48671(4) 0.39887(3) 0.22500(3) 0.01507(9) Uani 1 1 d . . . . . F1 F 0.04900(10) 0.80572(9) 0.25307(7) 0.02833(19) Uani 1 1 d . . . . . O1 O 0.48149(11) 0.35587(10) 0.09864(8) 0.01952(19) Uani 1 1 d . . . . . O2 O 0.35176(12) 0.65222(10) 0.33136(8) 0.0232(2) Uani 1 1 d . . . . . N1 N 0.32504(13) 0.68274(12) 0.11925(10) 0.0174(2) Uani 1 1 d D . . . . H1 H 0.3705(18) 0.6457(17) 0.0540(13) 0.021 Uiso 1 1 d D U . . . C1 C 0.68290(15) 0.40704(14) 0.26595(11) 0.0173(2) Uani 1 1 d . . . . . C2 C 0.77331(16) 0.48654(15) 0.17553(12) 0.0209(3) Uani 1 1 d . . . . . H2 H 0.732556 0.529398 0.095056 0.025 Uiso 1 1 calc R U . . . C3 C 0.92229(16) 0.50211(16) 0.20440(13) 0.0249(3) Uani 1 1 d . . . . . H3 H 0.983729 0.556062 0.143565 0.030 Uiso 1 1 calc R U . . . C4 C 0.98222(16) 0.43921(16) 0.32186(14) 0.0261(3) Uani 1 1 d . . . . . H4 H 1.083941 0.451437 0.341348 0.031 Uiso 1 1 calc R U . . . C5 C 0.89459(17) 0.35884(16) 0.41065(13) 0.0248(3) Uani 1 1 d . . . . . H5 H 0.936804 0.314655 0.490447 0.030 Uiso 1 1 calc R U . . . C6 C 0.74462(16) 0.34276(15) 0.38304(12) 0.0201(3) Uani 1 1 d . . . . . H6 H 0.684252 0.287873 0.444106 0.024 Uiso 1 1 calc R U . . . C7 C 0.40311(14) 0.27595(14) 0.34834(11) 0.0164(2) Uani 1 1 d . . . . . C8 C 0.36715(15) 0.14096(15) 0.31902(12) 0.0197(3) Uani 1 1 d . . . . . H8 H 0.388150 0.116670 0.236715 0.024 Uiso 1 1 calc R U . . . C9 C 0.30068(16) 0.04226(15) 0.41027(13) 0.0233(3) Uani 1 1 d . . . . . H9 H 0.277384 -0.050295 0.390736 0.028 Uiso 1 1 calc R U . . . C10 C 0.26838(16) 0.07885(16) 0.52975(13) 0.0240(3) Uani 1 1 d . . . . . H10 H 0.221745 0.011749 0.591747 0.029 Uiso 1 1 calc R U . . . C11 C 0.30366(16) 0.21291(16) 0.55961(12) 0.0229(3) Uani 1 1 d . . . . . H11 H 0.281133 0.237121 0.641842 0.028 Uiso 1 1 calc R U . . . C12 C 0.37165(15) 0.31151(15) 0.46978(12) 0.0194(3) Uani 1 1 d . . . . . H12 H 0.396793 0.402706 0.490428 0.023 Uiso 1 1 calc R U . . . C13 C 0.37355(15) 0.60247(14) 0.23210(11) 0.0169(2) Uani 1 1 d . . . . . C15 C 0.31436(16) 0.94646(15) 0.00908(12) 0.0212(3) Uani 1 1 d . . . . . H15 H 0.405493 0.907965 -0.039965 0.025 Uiso 1 1 calc R U . . . C16 C 0.24396(18) 1.10416(16) -0.01139(13) 0.0260(3) Uani 1 1 d . . . . . H16 H 0.286318 1.173043 -0.074760 0.031 Uiso 1 1 calc R U . . . C17 C 0.11186(18) 1.16112(16) 0.06062(13) 0.0268(3) Uani 1 1 d . . . . . H17 H 0.065343 1.269495 0.047778 0.032 Uiso 1 1 calc R U . . . C18 C 0.04741(17) 1.06097(16) 0.15110(13) 0.0250(3) Uani 1 1 d . . . . . H18 H -0.043515 1.099503 0.200346 0.030 Uiso 1 1 calc R U . . . C19 C 0.11738(15) 0.90417(15) 0.16863(12) 0.0201(3) Uani 1 1 d . . . . . C20 C 0.25253(15) 0.84437(14) 0.10083(11) 0.0174(2) 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 P1 0.01830(17) 0.01335(15) 0.01305(15) -0.00248(11) 0.00028(11) -0.00224(11) F1 0.0256(4) 0.0280(4) 0.0286(4) -0.0009(3) 0.0077(3) -0.0052(3) O1 0.0262(5) 0.0181(4) 0.0147(4) -0.0039(3) 0.0007(3) -0.0050(4) O2 0.0322(5) 0.0186(4) 0.0171(4) -0.0053(3) -0.0020(4) 0.0002(4) N1 0.0205(5) 0.0157(5) 0.0150(5) -0.0038(4) 0.0001(4) -0.0004(4) C1 0.0187(6) 0.0136(5) 0.0192(6) -0.0053(5) 0.0008(5) -0.0008(5) C2 0.0239(7) 0.0183(6) 0.0198(6) -0.0023(5) 0.0004(5) -0.0036(5) C3 0.0225(7) 0.0236(7) 0.0283(7) -0.0041(5) 0.0048(5) -0.0064(5) C4 0.0170(6) 0.0279(7) 0.0334(7) -0.0092(6) -0.0011(5) -0.0018(5) C5 0.0224(7) 0.0266(7) 0.0230(6) -0.0048(5) -0.0039(5) 0.0018(5) C6 0.0211(6) 0.0183(6) 0.0191(6) -0.0033(5) 0.0008(5) -0.0007(5) C7 0.0160(6) 0.0161(6) 0.0158(6) -0.0012(4) -0.0005(4) -0.0015(5) C8 0.0224(6) 0.0186(6) 0.0177(6) -0.0032(5) -0.0025(5) -0.0026(5) C9 0.0265(7) 0.0185(6) 0.0256(7) -0.0014(5) -0.0039(5) -0.0073(5) C10 0.0231(7) 0.0231(7) 0.0232(7) 0.0032(5) 0.0020(5) -0.0053(5) C11 0.0248(7) 0.0244(7) 0.0171(6) -0.0031(5) 0.0028(5) -0.0012(5) C12 0.0211(6) 0.0175(6) 0.0187(6) -0.0041(5) 0.0002(5) -0.0018(5) C13 0.0179(6) 0.0152(6) 0.0175(6) -0.0031(5) -0.0003(5) -0.0033(5) C15 0.0223(6) 0.0204(6) 0.0201(6) -0.0033(5) 0.0000(5) -0.0028(5) C16 0.0339(8) 0.0187(6) 0.0237(7) 0.0004(5) -0.0017(6) -0.0046(6) C17 0.0343(8) 0.0166(6) 0.0262(7) -0.0040(5) -0.0066(6) 0.0039(5) C18 0.0230(7) 0.0257(7) 0.0240(7) -0.0087(5) -0.0016(5) 0.0036(5) C19 0.0196(6) 0.0223(6) 0.0180(6) -0.0026(5) -0.0008(5) -0.0044(5) C20 0.0190(6) 0.0158(6) 0.0169(6) -0.0032(5) -0.0042(5) -0.0012(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 6 1 0.0344 -5 2 0 0.0818 2 4 5 0.0499 -5 1 2 0.0938 -5 0 0 0.0919 -5 -4 -2 0.0755 5 -1 1 0.0591 5 4 1 0.0686 5 0 0 0.0653 0 5 -1 0.0216 -5 -4 0 0.0787 2 -1 6 0.0345 1 -4 3 0.0151 -1 -6 0 0.0132 1 -5 0 0.0151 0 -5 -2 0.0148 -1 -1 -7 0.0469 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 P1 C1 113.45(5) . . ? O1 P1 C7 113.77(5) . . ? O1 P1 C13 111.53(5) . . ? C1 P1 C13 102.14(5) . . ? C7 P1 C1 109.05(6) . . ? C7 P1 C13 106.03(6) . . ? C13 N1 H1 116.9(10) . . ? C13 N1 C20 122.72(10) . . ? C20 N1 H1 116.3(10) . . ? C2 C1 P1 117.35(9) . . ? C6 C1 P1 122.86(10) . . ? C6 C1 C2 119.76(12) . . ? C1 C2 H2 120.2 . . ? C3 C2 C1 119.59(12) . . ? C3 C2 H2 120.2 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.29(12) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 119.8 . . ? C5 C4 C3 120.34(13) . . ? C5 C4 H4 119.8 . . ? C4 C5 H5 120.0 . . ? C4 C5 C6 119.96(12) . . ? C6 C5 H5 120.0 . . ? C1 C6 H6 120.0 . . ? C5 C6 C1 120.05(12) . . ? C5 C6 H6 120.0 . . ? C8 C7 P1 117.35(9) . . ? C8 C7 C12 119.85(11) . . ? C12 C7 P1 122.79(9) . . ? C7 C8 H8 120.0 . . ? C9 C8 C7 119.94(12) . . ? C9 C8 H8 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 119.94(12) . . ? C10 C9 H9 120.0 . . ? C9 C10 H10 119.8 . . ? C9 C10 C11 120.47(12) . . ? C11 C10 H10 119.8 . . ? C10 C11 H11 119.9 . . ? C12 C11 C10 120.17(12) . . ? C12 C11 H11 119.9 . . ? C7 C12 H12 120.2 . . ? C11 C12 C7 119.63(12) . . ? C11 C12 H12 120.2 . . ? O2 C13 P1 120.57(9) . . ? O2 C13 N1 126.07(11) . . ? N1 C13 P1 113.35(9) . . ? C16 C15 H15 119.7 . . ? C16 C15 C20 120.50(12) . . ? C20 C15 H15 119.7 . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 119.97(13) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 119.8 . . ? C18 C17 C16 120.32(12) . . ? C18 C17 H17 119.8 . . ? C17 C18 H18 120.6 . . ? C19 C18 C17 118.87(13) . . ? C19 C18 H18 120.6 . . ? F1 C19 C18 118.52(12) . . ? F1 C19 C20 119.29(11) . . ? C18 C19 C20 122.17(12) . . ? C15 C20 N1 119.68(11) . . ? C19 C20 N1 122.16(11) . . ? C19 C20 C15 118.12(11) . . ? 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 P1 O1 1.4908(9) . ? P1 C1 1.7994(13) . ? P1 C7 1.7952(12) . ? P1 C13 1.8706(12) . ? F1 C19 1.3545(15) . ? O2 C13 1.2198(15) . ? N1 H1 0.864(13) . ? N1 C13 1.3520(16) . ? N1 C20 1.4227(16) . ? C1 C2 1.4040(18) . ? C1 C6 1.3925(18) . ? C2 H2 0.9500 . ? C2 C3 1.3852(19) . ? C3 H3 0.9500 . ? C3 C4 1.388(2) . ? C4 H4 0.9500 . ? C4 C5 1.383(2) . ? C5 H5 0.9500 . ? C5 C6 1.3909(19) . ? C6 H6 0.9500 . ? C7 C8 1.3963(17) . ? C7 C12 1.4011(17) . ? C8 H8 0.9500 . ? C8 C9 1.3884(18) . ? C9 H9 0.9500 . ? C9 C10 1.3844(19) . ? C10 H10 0.9500 . ? C10 C11 1.3882(19) . ? C11 H11 0.9500 . ? C11 C12 1.3857(18) . ? C12 H12 0.9500 . ? C15 H15 0.9500 . ? C15 C16 1.3876(19) . ? C15 C20 1.3903(18) . ? C16 H16 0.9500 . ? C16 C17 1.386(2) . ? C17 H17 0.9500 . ? C17 C18 1.383(2) . ? C18 H18 0.9500 . ? C18 C19 1.3794(19) . ? C19 C20 1.3862(18) . ? 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 N1 H1 O1 0.864(13) 2.019(14) 2.8210(14) 154.0(14) 2_665 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 P1 C1 C2 C3 177.15(10) . . . . ? P1 C1 C6 C5 -177.23(10) . . . . ? P1 C7 C8 C9 -179.31(10) . . . . ? P1 C7 C12 C11 178.55(10) . . . . ? F1 C19 C20 N1 -1.76(18) . . . . ? F1 C19 C20 C15 175.91(11) . . . . ? O1 P1 C1 C2 46.43(11) . . . . ? O1 P1 C1 C6 -135.58(10) . . . . ? O1 P1 C7 C8 10.27(12) . . . . ? O1 P1 C7 C12 -168.88(10) . . . . ? O1 P1 C13 O2 172.76(10) . . . . ? O1 P1 C13 N1 -8.37(11) . . . . ? C1 P1 C7 C8 -117.47(10) . . . . ? C1 P1 C7 C12 63.38(12) . . . . ? C1 P1 C13 O2 -65.74(12) . . . . ? C1 P1 C13 N1 113.13(10) . . . . ? C1 C2 C3 C4 0.2(2) . . . . ? C2 C1 C6 C5 0.71(18) . . . . ? C2 C3 C4 C5 0.8(2) . . . . ? C3 C4 C5 C6 -1.0(2) . . . . ? C4 C5 C6 C1 0.2(2) . . . . ? C6 C1 C2 C3 -0.90(18) . . . . ? C7 P1 C1 C2 174.35(9) . . . . ? C7 P1 C1 C6 -7.66(12) . . . . ? C7 P1 C13 O2 48.41(12) . . . . ? C7 P1 C13 N1 -132.72(9) . . . . ? C7 C8 C9 C10 0.8(2) . . . . ? C8 C7 C12 C11 -0.58(19) . . . . ? C8 C9 C10 C11 -0.7(2) . . . . ? C9 C10 C11 C12 0.0(2) . . . . ? C10 C11 C12 C7 0.64(19) . . . . ? C12 C7 C8 C9 -0.13(19) . . . . ? C13 P1 C1 C2 -73.74(10) . . . . ? C13 P1 C1 C6 104.25(11) . . . . ? C13 P1 C7 C8 133.22(10) . . . . ? C13 P1 C7 C12 -45.94(12) . . . . ? C13 N1 C20 C15 126.41(13) . . . . ? C13 N1 C20 C19 -55.96(17) . . . . ? C15 C16 C17 C18 -1.5(2) . . . . ? C16 C15 C20 N1 179.13(12) . . . . ? C16 C15 C20 C19 1.41(19) . . . . ? C16 C17 C18 C19 0.3(2) . . . . ? C17 C18 C19 F1 -176.78(12) . . . . ? C17 C18 C19 C20 1.7(2) . . . . ? C18 C19 C20 N1 179.75(12) . . . . ? C18 C19 C20 C15 -2.59(19) . . . . ? C20 N1 C13 P1 -172.94(9) . . . . ? C20 N1 C13 O2 5.9(2) . . . . ? C20 C15 C16 C17 0.6(2) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.2945 5.6932 0.9690 0.8784 0.4778 0.0089 -4.5329 2.2507 -0.2509 0.4810 0.2631 -0.8363 2.1718 4.3284 5.2642 0.3056 0.8630 0.4022 -4.9854 1.0503 1.6409 0.1526 0.4363 -0.8868 -5.4784 -0.1440 0.1814 0.0667 0.1938 -0.9788 -4.6962 -3.8862 -2.4722 -0.3843 -0.4036 -0.8303 5.1620 -0.9666 0.5462 -0.2990 -0.1643 0.9400 4.8234 3.9492 1.3020 0.4765 0.2577 0.8406 5.4429 -0.0793 0.1363 -0.1263 -0.1675 0.9778 -0.4496 5.1813 -1.3433 0.9729 0.1813 -0.1433 -4.9714 -3.6487 -0.1714 -0.5046 -0.0926 -0.8584 2.0459 -0.5472 6.3165 -0.5843 0.6842 0.4365 0.8448 -4.2051 3.4158 -0.9658 0.1267 0.2261 -0.9226 -5.7275 -0.3403 -0.9174 -0.3810 -0.1147 0.9843 -5.2656 -0.0121 -0.8998 -0.3732 0.2261 0.4667 -5.4957 -1.5525 -0.8179 -0.5628 0.1197 -0.7642 -0.8553 -7.0226 0.3758 -0.9047 -0.2007