#------------------------------------------------------------------------------ #$Date: 2021-09-04 00:23:46 +0300 (Sat, 04 Sep 2021) $ #$Revision: 268443 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519023.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_4519023 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 'C18 H16 N O3 P' _chemical_formula_sum 'C18 H16 N O3 P' _chemical_formula_weight 325.29 _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 108.405(4) _cell_angle_beta 96.291(3) _cell_angle_gamma 90.405(3) _cell_formula_units_Z 4 _cell_length_a 8.4872(3) _cell_length_b 11.6741(5) _cell_length_c 16.8354(6) _cell_measurement_reflns_used 4724 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 72.0710 _cell_measurement_theta_min 3.9770 _cell_volume 1571.67(11) _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 4.2207 _diffrn_detector_type 'Agilent Diffraction Titan S2 detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.978 _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 -4.00 23.00 1.00 2.00 -- 30.00 88.00 -59.56 27 2 \w -12.00 13.00 1.00 2.00 -- 30.00 104.00 121.48 25 3 \w 3.00 30.00 1.00 2.00 -- 34.00 76.00-172.53 27 4 \w -2.00 23.00 1.00 2.00 -- 34.00 91.00 147.06 25 5 \w 19.00 59.00 1.00 2.00 -- 41.87 38.00-150.00 40 6 \w 27.00 95.00 1.00 2.00 -- 41.87-125.00-120.00 68 7 \w 19.00 104.00 1.00 2.00 -- 41.87 38.00 60.00 85 8 \w -27.00 66.00 1.00 2.00 -- 41.87 -57.00 0.00 93 9 \w 14.00 39.00 1.00 2.00 -- 46.00 80.00 32.47 25 10 \w 13.00 39.00 1.00 2.00 -- 46.00 81.00-124.63 26 11 \w 13.00 38.00 1.00 2.00 -- 46.00 82.00 170.36 25 12 \w 14.00 41.00 1.00 2.00 -- 46.00 80.00 -9.66 27 13 \w 25.00 73.00 1.00 2.00 -- 54.00 74.00 107.18 48 14 \w 79.00 116.00 1.00 2.00 -- 54.00 74.00 107.18 37 15 \w 29.00 62.00 1.00 2.00 -- 58.00 73.00 -66.37 33 16 \w 71.00 131.00 1.00 2.00 -- 58.00 73.00 -66.37 60 17 \w 34.00 61.00 1.00 2.00 -- 62.00 73.00-107.00 27 18 \w 34.00 61.00 1.00 2.00 -- 62.00 72.00 30.43 27 19 \w 36.00 70.00 1.00 2.00 -- 66.00 74.00 -58.88 34 20 \w 35.00 64.00 1.00 2.00 -- 66.00 74.00 57.66 29 21 \w 36.00 64.00 1.00 2.00 -- 66.00 74.00 147.37 28 22 \w 96.00 143.00 1.00 2.00 -- 70.00 73.00 119.85 47 23 \w 40.00 72.00 1.00 2.00 -- 70.00 73.00 119.85 32 24 \w 106.00 135.00 1.00 2.00 -- 70.00 73.00 -18.49 29 25 \w 40.00 73.00 1.00 2.00 -- 70.00 73.00 -18.49 33 26 \w 48.00 82.00 1.00 8.00 -- 74.00 60.00 103.09 34 27 \w 44.00 71.00 1.00 8.00 -- 74.00 73.00-157.02 27 28 \w 45.00 72.00 1.00 8.00 -- 74.00 69.00 176.52 27 29 \w 49.00 76.00 1.00 8.00 -- 78.00 69.00 23.60 27 30 \w 49.00 76.00 1.00 8.00 -- 78.00 69.00-128.64 27 31 \w 113.00 157.00 1.00 8.00 -- 86.00 72.00 115.09 44 32 \w 57.00 82.00 1.00 8.00 -- 86.00 72.00 115.09 25 33 \w 103.00 166.00 1.00 8.00 -- 94.00 72.00-123.25 63 34 \w 64.00 95.00 1.00 8.00 -- 94.00 72.00-123.25 31 35 \w 66.00 156.00 1.00 8.00 -- 94.00 65.00 56.82 90 36 \w 33.00 113.00 1.00 8.00 -- 101.44-125.00-180.00 80 37 \w 82.00 113.00 1.00 8.00 -- 101.44-125.00 -60.00 31 38 \w 35.00 70.00 1.00 8.00 -- 101.44 -45.00 -60.00 35 39 \w 76.00 169.00 1.00 8.00 -- 101.44 61.00 -60.00 93 40 \w 75.00 164.00 1.00 8.00 -- 101.44 61.00-180.00 89 41 \w 31.00 93.00 1.00 8.00 -- 101.44 -61.00 30.00 62 42 \w 77.00 104.00 1.00 8.00 -- 101.44 45.00 30.00 27 43 \w 32.00 90.00 1.00 8.00 -- 101.44 -61.00-150.00 58 44 \w 114.00 144.00 1.00 8.00 -- 101.44 61.00 -90.00 30 45 \w 75.00 103.00 1.00 8.00 -- 101.44 61.00 -90.00 28 46 \w 103.00 171.00 1.00 8.00 -- 101.44 59.00 -6.13 68 47 \w 75.00 101.00 1.00 8.00 -- 101.44 59.00 -6.13 26 48 \w 34.00 93.00 1.00 8.00 -- 101.44 -61.00 150.00 59 49 \w 79.00 149.00 1.00 8.00 -- 101.44 61.00 150.00 70 50 \w 146.00 171.00 1.00 8.00 -- 101.44 61.00 -30.00 25 51 \w 76.00 103.00 1.00 8.00 -- 101.44 61.00 -30.00 27 52 \w 29.00 110.00 1.00 8.00 -- 101.44-125.00 0.00 81 53 \w 111.00 163.00 1.00 8.00 -- 101.44 61.00 30.00 52 54 \w 77.00 106.00 1.00 8.00 -- 101.44 61.00 30.00 29 55 \w 71.00 112.00 1.00 8.00 -- 101.44 72.00 119.93 41 56 \w 35.00 112.00 1.00 8.00 -- 101.44-125.00 60.00 77 57 \w 76.00 158.00 1.00 8.00 -- 101.44 61.00 90.00 82 58 \w 75.00 130.00 1.00 8.00 -- 101.44 61.00-150.00 55 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Titan 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 -0.1332442000 _diffrn_orient_matrix_UB_12 -0.0835849000 _diffrn_orient_matrix_UB_13 -0.0605253000 _diffrn_orient_matrix_UB_21 -0.1096633000 _diffrn_orient_matrix_UB_22 0.1074068000 _diffrn_orient_matrix_UB_23 0.0133682000 _diffrn_orient_matrix_UB_31 0.0602801000 _diffrn_orient_matrix_UB_32 0.0292892000 _diffrn_orient_matrix_UB_33 -0.0747637000 _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 0.0653 _diffrn_reflns_av_unetI/netI 0.0497 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 27235 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.391 _diffrn_reflns_theta_min 3.995 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Agilent Diffraction microfocus tube' _exptl_absorpt_coefficient_mu 1.678 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.628 _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 1.375 _exptl_crystal_description plate _exptl_crystal_F_000 680 _exptl_crystal_recrystallization_method 'Recrystalised from ethanol at -30C' _exptl_crystal_size_max 0.255 _exptl_crystal_size_mid 0.177 _exptl_crystal_size_min 0.028 _refine_diff_density_max 0.464 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.049 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 498 _refine_ls_number_reflns 6105 _refine_ls_number_restraints 264 _refine_ls_restrained_S_all 1.006 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0388 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.2319P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.0953 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4613 _reflns_number_total 6105 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file sc1c02907_si_002.cif _cod_data_source_block ochdki _cod_database_code 4519023 _nottingham_internal_coll_name OCHDKI _nottingham_internal_coll_number 18862 _nottingham_internal_coll_client CH/DLK _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_frame_time '8.00, 2.00' _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 'GVA, PL13110002' _nottingham_internal_process_date 03/12/2020 _nottingham_internal_process_user pcxch6 _nottingham_internal_solution_date 14/12/2020 _nottingham_internal_solution_user pcxch6 _nottingham_internal_refinement_date 14/12/2020 _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 'C18 H16 N1 O3 P1' _chemical_oxdiff_usercomment 'OCHDKI #18862 GVA-1858 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 0.955 _shelx_estimated_absorpt_t_min 0.674 _reflns_odcompleteness_completeness 99.93 _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 C(H,H) groups, All N(H) groups 2. Restrained distances N1-H1 0.88 with sigma of 0.02 N2-H2A 0.88 with sigma of 0.02 O6A-C33 \\sim O6B-C33 with sigma of 0.02 O3A-C16A \\sim O3B-C16B with sigma of 0.02 C36A-C34A \\sim C36B-C34B with sigma of 0.04 O6A-C34A \\sim O6B-C34B with sigma of 0.02 C33-C36A \\sim C33-C36B with sigma of 0.02 C17A-C16A \\sim C17B-C16B with sigma of 0.02 C35A-C36A \\sim C35B-C36B with sigma of 0.02 C35A-C34A \\sim C35B-C34B with sigma of 0.02 C18A-C17A \\sim C18B-C17B with sigma of 0.02 C15-C16A \\sim C15-C16B with sigma of 0.04 O3A-C15 \\sim O3B-C15 with sigma of 0.02 O6A-C35A \\sim O6B-C35B with sigma of 0.04 C15-C18A \\sim C15-C18B with sigma of 0.02 C33-C35A \\sim C33-C35B with sigma of 0.04 O3A-C17A \\sim O3B-C17B with sigma of 0.04 C33-C34A \\sim C33-C34B with sigma of 0.04 C15-C17A \\sim C15-C17B with sigma of 0.04 C18A-C16A \\sim C18B-C16B with sigma of 0.04 3. Restrained planarity C33, O6B, C34B, C35B, C36B with sigma of 0.1 C15, O3B, C16B, C17B, C18B with sigma of 0.1 4. Uiso/Uaniso restraints and constraints C33 \\sim O6B \\sim C34B \\sim C35B \\sim C36B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C15 \\sim O3B \\sim C16B \\sim C17B \\sim C18B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O3A \\sim C15 \\sim C16A \\sim C17A \\sim C18A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O6A \\sim C33 \\sim C34A \\sim C35A \\sim C36A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 5. Rigid body (RIGU) restrains O6A, C33, C34A, C35A, C36A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O3A, C15, C16A, C17A, C18A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C33, O6B, C34B, C35B, C36B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C15, O3B, C16B, C17B, C18B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(O6B)=Sof(C34B)=Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=1-FVAR(1) Sof(O6A)=Sof(C34A)=Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=FVAR(1) Sof(O3B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=1-FVAR(2) Sof(O3A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=FVAR(2) 7.a Secondary CH2 refined with riding coordinates: C14(H14A,H14B), C32(H32A,H32B) 7.b 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), C16A(H16A), C17A(H17A), C18A(H18A), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C34A(H34A), C36A(H36A), C16B(H16B), C17B(H17B), C18B(H18B), C34B(H34B), C35B(H35B), C36B(H36B) ; _shelx_res_file ; TITL ochdki_a.res in P-1 ochdki.res created by SHELXL-2018/3 at 10:41:19 on 18-Feb-2021 REM Old TITL ochdki_a.res in P-1 REM SHELXT solution in P-1: R1 0.131, Rweak 0.007, Alpha 0.045 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C37 N2 O5 P2 CELL 1.54184 8.4872 11.6741 16.8354 108.405 96.291 90.405 ZERR 4 0.0003 0.0005 0.0006 0.004 0.003 0.003 LATT 1 SFAC C H N O P UNIT 72 64 4 12 4 EQIV $1 1-X,1-Y,2-Z EQIV $2 -X,1-Y,1-Z SADI O6A C33 O6B C33 SADI O3A C16A O3B C16B SADI 0.04 C36A C34A C36B C34B SADI O6A C34A O6B C34B SADI C33 C36A C33 C36B SADI C17A C16A C17B C16B SADI C35A C36A C35B C36B SADI C35A C34A C35B C34B SADI C18A C17A C18B C17B SADI 0.04 C15 C16A C15 C16B SADI O3A C15 O3B C15 SADI 0.04 O6A C35A O6B C35B SADI C15 C18A C15 C18B SADI 0.04 C33 C35A C33 C35B SADI 0.04 O3A C17A O3B C17B SADI 0.04 C33 C34A C33 C34B SADI 0.04 C15 C17A C15 C17B SADI 0.04 C18A C16A C18B C16B RIGU O6A C33 > C36A RIGU O3A C15 > C18A SIMU C33 O6B C34B > C36B RIGU C33 O6B C34B > C36B SIMU C15 O3B C16B > C18B RIGU C15 O3B C16B > C18B SIMU O3A C15 > C18A SIMU O6A C33 > C36A FLAT C33 O6B C34B C35B C36B FLAT C15 O3B C16B C17B C18B DFIX 0.88 N1 H1 DFIX 0.88 N2 H2a L.S. 20 0 0 PLAN 5 SIZE 0.028 0.177 0.255 TEMP -153(2) CONF HTAB N1 O1_$1 HTAB N2 O4_$2 BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 6 1 14 REM REM REM WGHT 0.037400 0.231900 FVAR 0.53500 0.67669 0.86400 P1 5 0.440394 0.328173 0.854203 11.00000 0.01970 0.02143 = 0.01524 0.00328 0.00359 -0.00129 O1 4 0.380435 0.403327 0.932871 11.00000 0.02421 0.02841 = 0.01781 0.00236 0.00667 -0.00164 O2 4 0.701519 0.338068 0.777465 11.00000 0.02537 0.03094 = 0.02218 0.00137 0.00782 -0.00224 PART 1 O3A 4 0.964783 0.658319 1.033302 31.00000 0.03068 0.03823 = 0.02467 0.01119 -0.00367 -0.00874 PART 0 N1 3 0.690916 0.488022 0.901738 11.00000 0.01984 0.02329 = 0.01809 0.00441 0.00587 -0.00014 H1 2 0.643734 0.513022 0.946929 11.00000 -1.20000 C1 1 0.313509 0.321354 0.760098 11.00000 0.02235 0.02031 = 0.02063 0.00567 0.00404 -0.00157 C2 1 0.164119 0.368908 0.770525 11.00000 0.02389 0.02332 = 0.02449 0.00789 0.00690 0.00110 AFIX 43 H2 2 0.133447 0.401910 0.825524 11.00000 -1.20000 AFIX 0 C3 1 0.060123 0.368128 0.700709 11.00000 0.02357 0.02534 = 0.03284 0.01259 0.00312 0.00260 AFIX 43 H3 2 -0.042056 0.399771 0.707907 11.00000 -1.20000 AFIX 0 C4 1 0.105379 0.321160 0.620456 11.00000 0.02789 0.02816 = 0.02508 0.01187 -0.00219 -0.00294 AFIX 43 H4 2 0.034810 0.321839 0.572750 11.00000 -1.20000 AFIX 0 C5 1 0.253822 0.273104 0.609731 11.00000 0.02994 0.03372 = 0.01734 0.00611 0.00335 -0.00316 AFIX 43 H5 2 0.284306 0.240977 0.554627 11.00000 -1.20000 AFIX 0 C6 1 0.357817 0.271735 0.678979 11.00000 0.02254 0.02868 = 0.02044 0.00576 0.00399 0.00160 AFIX 43 H6 2 0.458395 0.237354 0.671377 11.00000 -1.20000 AFIX 0 C7 1 0.476736 0.176078 0.852163 11.00000 0.02346 0.02425 = 0.02083 0.00785 0.00460 -0.00190 C8 1 0.383011 0.076709 0.800546 11.00000 0.02646 0.02844 = 0.03232 0.00514 0.00125 -0.00310 AFIX 43 H8 2 0.302054 0.086054 0.759666 11.00000 -1.20000 AFIX 0 C9 1 0.408673 -0.036426 0.809216 11.00000 0.03839 0.02389 = 0.04796 0.00719 0.00007 -0.00745 AFIX 43 H9 2 0.344392 -0.104405 0.774246 11.00000 -1.20000 AFIX 0 C10 1 0.525470 -0.050896 0.867552 11.00000 0.05292 0.03050 = 0.05051 0.02259 0.00217 -0.00310 AFIX 43 H10 2 0.542387 -0.128794 0.872574 11.00000 -1.20000 AFIX 0 C11 1 0.619091 0.047541 0.919288 11.00000 0.05680 0.03834 = 0.04203 0.02170 -0.01334 -0.00224 AFIX 43 H11 2 0.699532 0.037538 0.960176 11.00000 -1.20000 AFIX 0 C12 1 0.595074 0.160366 0.911218 11.00000 0.04068 0.03110 = 0.02662 0.01016 -0.00603 -0.00562 AFIX 43 H12 2 0.660030 0.227845 0.946351 11.00000 -1.20000 AFIX 0 C13 1 0.635915 0.388062 0.840473 11.00000 0.02001 0.02170 = 0.01854 0.00710 0.00369 0.00206 C14 1 0.836731 0.550653 0.894530 11.00000 0.02389 0.02632 = 0.02507 0.00467 0.00728 -0.00384 AFIX 23 H14A 2 0.825783 0.566843 0.839944 11.00000 -1.20000 H14B 2 0.926859 0.497396 0.894967 11.00000 -1.20000 AFIX 0 C15 1 0.871740 0.665855 0.963595 11.00000 0.01998 0.02703 = 0.02139 0.00856 0.00308 -0.00250 PART 1 C16A 1 0.984135 0.774038 1.088166 31.00000 0.04704 0.05375 = 0.02747 0.00030 0.00152 -0.02628 AFIX 43 H16A 2 1.043061 0.796229 1.142510 31.00000 -1.20000 AFIX 0 C17A 1 0.909398 0.850894 1.055087 31.00000 0.05163 0.03118 = 0.04698 -0.00768 0.01827 -0.01186 AFIX 43 H17A 2 0.905032 0.935737 1.080661 31.00000 -1.20000 AFIX 0 C18A 1 0.837207 0.780793 0.973723 31.00000 0.03325 0.02921 = 0.04318 0.00929 0.00863 0.00188 AFIX 43 H18A 2 0.776038 0.810085 0.934084 31.00000 -1.20000 AFIX 0 PART 0 P2 5 -0.006034 0.320922 0.362028 11.00000 0.01937 0.01921 = 0.01636 0.00490 0.00451 0.00082 O4 4 -0.072733 0.372392 0.443176 11.00000 0.02555 0.02263 = 0.01808 0.00447 0.00726 0.00076 O5 4 0.242308 0.363350 0.288208 11.00000 0.02473 0.02907 = 0.02105 0.00507 0.00851 -0.00029 PART 1 O6A 4 0.464051 0.676794 0.547575 21.00000 0.03100 0.03203 = 0.02312 0.00768 -0.00211 -0.00558 PART 0 N2 3 0.223424 0.501903 0.415950 11.00000 0.02079 0.02071 = 0.02079 0.00366 0.00783 -0.00171 H2A 2 0.169208 0.526670 0.459384 11.00000 -1.20000 C19 1 -0.140611 0.325190 0.272846 11.00000 0.02152 0.01707 = 0.02045 0.00571 0.00323 -0.00111 C20 1 -0.289312 0.371767 0.287870 11.00000 0.02415 0.02089 = 0.02419 0.00758 0.00769 0.00109 AFIX 43 H20 2 -0.316537 0.400132 0.343833 11.00000 -1.20000 AFIX 0 C21 1 -0.397734 0.376696 0.220951 11.00000 0.02092 0.02493 = 0.03203 0.01092 0.00417 0.00163 AFIX 43 H21 2 -0.499956 0.406608 0.231018 11.00000 -1.20000 AFIX 0 C22 1 -0.356640 0.338052 0.139823 11.00000 0.02337 0.03020 = 0.02521 0.01035 -0.00254 -0.00121 AFIX 43 H22 2 -0.430027 0.343062 0.094318 11.00000 -1.20000 AFIX 0 C23 1 -0.208650 0.291931 0.124445 11.00000 0.02695 0.03559 = 0.02035 0.00741 0.00261 -0.00129 AFIX 43 H23 2 -0.181115 0.265482 0.068506 11.00000 -1.20000 AFIX 0 C24 1 -0.100935 0.284394 0.190581 11.00000 0.02015 0.02931 = 0.02230 0.00708 0.00429 0.00173 AFIX 43 H24 2 -0.000384 0.251535 0.179895 11.00000 -1.20000 AFIX 0 C25 1 0.049330 0.166567 0.344060 11.00000 0.02148 0.02103 = 0.01974 0.00567 0.00103 0.00029 C26 1 -0.017030 0.104889 0.391804 11.00000 0.03270 0.02604 = 0.02575 0.00779 0.00692 0.00115 AFIX 43 H26 2 -0.084424 0.145104 0.432447 11.00000 -1.20000 AFIX 0 C27 1 0.015309 -0.015115 0.379983 11.00000 0.05017 0.02624 = 0.03607 0.01479 0.00482 -0.00218 AFIX 43 H27 2 -0.032093 -0.057428 0.411728 11.00000 -1.20000 AFIX 0 C28 1 0.115777 -0.073662 0.322494 11.00000 0.03959 0.01984 = 0.03278 0.00467 -0.00384 0.00259 AFIX 43 H28 2 0.138794 -0.155594 0.315324 11.00000 -1.20000 AFIX 0 C29 1 0.182772 -0.012768 0.275405 11.00000 0.03269 0.02650 = 0.03285 0.00288 0.00455 0.00517 AFIX 43 H29 2 0.252670 -0.052860 0.236139 11.00000 -1.20000 AFIX 0 C30 1 0.148645 0.106721 0.285067 11.00000 0.03141 0.02685 = 0.02976 0.00815 0.00903 0.00320 AFIX 43 H30 2 0.192982 0.147543 0.251488 11.00000 -1.20000 AFIX 0 C31 1 0.176215 0.402334 0.352508 11.00000 0.01844 0.02093 = 0.02093 0.00917 0.00436 0.00336 C32 1 0.361020 0.572741 0.408193 11.00000 0.02951 0.02950 = 0.04159 0.00400 0.01701 -0.00596 AFIX 23 H32A 2 0.345257 0.586951 0.352974 11.00000 -1.20000 H32B 2 0.456734 0.524967 0.409057 11.00000 -1.20000 AFIX 0 C33 1 0.388976 0.690131 0.475328 11.00000 0.02023 0.02869 = 0.02102 0.00812 0.00467 -0.00203 PART 1 C34A 1 0.490262 0.791969 0.602465 21.00000 0.03672 0.03983 = 0.02700 -0.00191 -0.00034 -0.01393 AFIX 43 H34A 2 0.541537 0.811337 0.658431 21.00000 -1.20000 AFIX 0 C35A 1 0.434335 0.873781 0.567117 21.00000 0.03648 0.02947 = 0.03455 -0.00191 0.01076 -0.00698 H35A 2 0.435460 0.961131 0.595346 21.00000 -1.20000 C36A 1 0.368562 0.805951 0.482904 21.00000 0.02592 0.03208 = 0.03292 0.01059 0.00629 -0.00064 AFIX 43 H36A 2 0.320198 0.837353 0.441002 21.00000 -1.20000 AFIX 0 PART 2 O3B 4 0.771133 0.757268 0.963451 -31.00000 0.03095 0.02809 = 0.02129 -0.00227 -0.00429 -0.00337 O6B 4 0.316824 0.779051 0.448297 -21.00000 0.03495 0.02277 = 0.03528 0.00352 0.00032 -0.00292 C16B 1 0.819005 0.852320 1.034243 -31.00000 0.03162 0.02969 = 0.00955 0.00062 -0.00763 0.00467 AFIX 43 H16B 2 0.769395 0.927619 1.049667 -31.00000 -1.20000 AFIX 0 C17B 1 0.942842 0.825582 1.078102 -31.00000 0.02996 0.02753 = 0.01561 0.01122 -0.00992 0.00728 AFIX 43 H17B 2 0.999281 0.877489 1.128686 -31.00000 -1.20000 AFIX 0 C18B 1 0.975905 0.704031 1.035197 -31.00000 0.02902 0.02477 = 0.03117 0.01465 -0.00628 -0.00309 AFIX 43 H18B 2 1.055775 0.657950 1.053099 -31.00000 -1.20000 AFIX 0 C34B 1 0.360109 0.889659 0.508064 -21.00000 0.04111 0.02334 = 0.04510 0.00301 0.00974 0.00152 AFIX 43 H34B 2 0.325353 0.965379 0.504775 -21.00000 -1.20000 AFIX 0 C35B 1 0.457928 0.874265 0.571038 -21.00000 0.03453 0.04021 = 0.03491 -0.00568 -0.00111 -0.00940 AFIX 43 H35B 2 0.507211 0.936137 0.619023 -21.00000 -1.20000 AFIX 0 C36B 1 0.474653 0.747752 0.552878 -21.00000 0.02260 0.04211 = 0.02510 0.00357 -0.00388 -0.00420 AFIX 43 H36B 2 0.534094 0.709547 0.587785 -21.00000 -1.20000 AFIX 0 HKLF 4 REM ochdki_a.res in P-1 REM wR2 = 0.0953, GooF = S = 1.025, Restrained GooF = 1.006 for all data REM R1 = 0.0388 for 4613 Fo > 4sig(Fo) and 0.0600 for all 6105 data REM 498 parameters refined using 264 restraints END WGHT 0.0374 0.2319 REM Highest difference peak 0.464, deepest hole -0.291, 1-sigma level 0.049 Q1 1 0.4611 0.2529 0.8593 11.00000 0.05 0.46 Q2 1 0.0238 0.2410 0.3546 11.00000 0.05 0.40 Q3 1 0.5457 0.3781 0.8417 11.00000 0.05 0.26 Q4 1 0.0966 0.3814 0.3569 11.00000 0.05 0.26 Q5 1 -0.0004 0.1411 0.3589 11.00000 0.05 0.20 ; _shelx_res_checksum 26293 _shelx_hkl_file ; 0 0 -2 206.65 10.73 0 0 -2 234.21 10.36 0 0 2 210.25 9.62 0 0 -2 219.40 10.68 0 0 3 8.71 3.64 0 0 -3 5.91 4.07 0 0 4 1508.68 37.06 0 0 -4 1511.18 43.96 0 0 4 1493.00 28.26 0 0 5 10.18 3.65 0 0 5 8.06 6.52 0 0 -5 11.03 5.30 0 0 5 10.09 2.65 0 0 6 301.14 23.68 0 0 6 354.80 21.52 0 0 6 297.01 19.09 0 0 -6 371.09 25.62 0 0 -6 346.73 26.36 0 0 7 8.18 4.96 0 0 7 14.98 10.40 0 0 7 18.91 7.43 0 0 -7 17.43 8.62 0 0 -7 13.19 9.46 0 0 -8 -3.61 9.47 0 0 8 -1.34 5.06 0 0 8 6.16 9.47 0 0 8 -3.85 6.47 0 0 -8 -0.96 3.83 0 0 -8 2.25 9.59 0 0 -9 35.12 10.50 0 0 9 36.22 13.42 0 0 9 36.43 10.10 0 0 -9 43.42 6.82 0 0 10 111.26 21.85 0 0 -10 131.09 21.08 0 0 10 120.95 20.93 0 0 10 116.81 20.95 0 0 10 107.46 17.21 0 0 -10 141.26 12.07 0 0 -11 -0.90 5.20 0 0 -11 -6.47 4.83 0 0 -11 2.34 6.76 0 0 11 8.43 10.73 0 0 11 -1.79 9.82 0 0 11 -4.80 11.73 0 0 11 -11.68 9.76 0 0 -11 2.45 6.39 0 0 -12 221.07 17.38 0 0 -12 216.70 16.34 0 0 12 187.77 31.60 0 0 12 219.35 33.10 0 0 -12 233.20 32.21 0 0 12 198.73 29.56 0 0 -12 220.06 16.39 0 0 12 230.61 31.80 0 0 -13 55.07 9.10 0 0 -13 49.06 8.96 0 0 13 59.86 19.65 0 0 -13 37.06 7.67 0 0 13 38.53 13.45 0 0 13 35.23 16.68 0 0 -14 228.27 17.40 0 0 -14 208.19 17.85 0 0 14 221.58 32.21 0 0 -14 235.66 18.02 0 0 14 222.07 35.44 0 0 14 187.06 32.84 0 0 -15 27.65 6.71 0 0 -15 25.81 6.96 0 0 -15 33.95 9.11 0 0 -16 109.19 12.93 0 0 -16 123.97 11.93 0 0 16 69.48 18.61 0 0 -16 99.36 11.42 0 0 16 113.13 24.78 0 0 -17 44.47 7.00 0 0 -17 49.25 7.24 0 0 -17 41.76 7.94 0 0 17 33.23 6.46 0 0 -18 23.30 4.40 0 0 18 11.19 3.73 0 0 -18 24.69 5.05 0 0 -18 25.78 5.78 0 1 -19 6.03 3.65 0 -1 18 115.13 11.13 0 1 -18 128.23 9.87 0 1 -18 123.28 9.96 0 1 -18 135.33 11.97 0 -1 17 31.09 21.05 0 1 -17 27.38 5.56 0 1 -17 34.23 6.58 0 1 -17 33.37 8.34 0 1 -16 6.64 6.46 0 -1 16 15.84 14.52 0 1 -16 4.21 4.57 0 1 -16 0.63 3.83 0 -1 16 3.95 9.60 0 1 -15 43.79 9.49 0 1 -15 48.47 8.37 0 -1 15 56.74 19.86 0 1 -15 60.49 9.36 0 -1 15 59.34 18.73 0 1 -14 219.70 16.68 0 -1 14 221.85 34.54 0 -1 14 192.23 32.91 0 -1 14 236.07 32.75 0 1 -14 217.15 16.60 0 1 -14 260.97 20.18 0 1 -13 332.99 20.25 0 1 -13 329.52 37.68 0 -1 13 302.67 37.93 0 -1 13 324.72 39.76 0 -1 13 277.46 33.89 0 1 -13 317.71 20.21 0 1 -13 278.99 16.82 0 1 -13 358.71 22.18 0 1 -12 1588.89 47.62 0 1 -12 1621.30 45.09 0 -1 12 1505.49 80.38 0 -1 12 1521.50 82.95 0 1 -12 1684.88 81.62 0 -1 12 1426.64 73.75 0 1 -12 1525.94 45.19 0 1 -12 1471.52 39.89 0 -1 12 1539.12 80.01 0 1 -11 95.64 10.86 0 1 -11 105.08 11.04 0 -1 11 71.10 16.33 0 1 -11 106.52 20.42 0 -1 11 88.08 20.41 0 -1 11 83.59 18.97 0 1 -11 91.09 10.30 0 -1 11 89.31 19.26 0 -1 10 38.60 12.27 0 1 -10 42.46 13.24 0 -1 10 28.97 12.18 0 1 -10 41.84 7.31 0 -1 10 41.37 13.20 0 1 -9 -3.23 5.73 0 -1 9 2.54 6.40 0 1 -9 5.74 3.68 0 -1 9 3.28 8.46 0 -1 9 3.38 5.04 0 -1 8 1.04 8.53 0 -1 8 9.51 4.95 0 -1 8 4.18 4.77 0 1 -8 6.16 7.00 0 -1 8 -1.88 6.19 0 -1 7 62.50 8.98 0 -1 7 63.40 9.09 0 -1 7 59.72 12.29 0 1 -7 55.49 11.50 0 -1 7 55.37 10.89 0 -1 6 19.57 4.55 0 -1 6 30.62 8.08 0 1 -6 20.07 7.36 0 -1 6 19.16 5.75 0 -1 5 26.58 7.03 0 1 -5 10.01 5.32 0 1 -5 16.85 6.15 0 -1 5 23.01 5.00 0 1 -4 8.04 4.10 0 -1 4 13.33 4.27 0 1 -4 10.43 4.23 0 1 -3 4.15 4.09 0 1 -3 -0.26 3.37 0 -1 3 2.72 3.27 0 -1 2 1602.59 30.38 0 1 -2 1615.61 34.69 0 1 -2 1563.73 32.43 0 1 -1 11.08 2.00 0 1 -1 10.60 2.57 0 -1 1 8.93 1.81 0 -1 1 8.77 1.77 0 -1 0 1481.97 27.46 0 1 0 1686.98 28.07 0 1 1 1.02 2.56 0 -1 -1 1.39 1.29 0 1 2 1459.68 34.85 0 -1 -2 1424.59 37.53 0 -1 -2 1406.23 29.01 0 1 3 51.40 7.16 0 1 3 52.14 8.45 0 -1 -3 61.21 9.72 0 -1 -3 57.03 5.91 0 1 4 27.73 6.39 0 1 4 29.20 7.05 0 1 4 28.37 7.75 0 -1 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361.85 31.19 0 4 4 194.79 21.63 0 -4 -4 199.60 20.03 0 4 4 203.57 20.48 0 4 4 202.81 22.67 0 -4 -4 192.47 24.44 0 -4 -5 10.15 8.27 0 4 5 4.51 8.24 0 -4 -5 3.91 5.95 0 4 5 -0.25 6.84 0 -4 -5 5.64 8.98 0 4 5 2.05 8.30 0 4 6 12.33 10.57 0 -4 -6 16.87 11.27 0 4 6 19.27 10.39 0 4 6 18.20 8.90 0 -4 -6 3.51 8.30 0 -4 -7 14.21 7.39 0 -4 -7 11.78 10.13 0 4 7 23.34 12.00 0 -4 -7 9.83 4.92 0 4 7 17.59 9.66 0 4 8 10.98 9.86 0 -4 -8 5.94 9.25 0 -4 -8 7.71 5.14 0 -4 -8 0.45 8.35 0 4 8 3.49 8.88 0 4 8 8.06 5.64 0 -4 -8 2.97 4.79 0 4 9 30.26 10.57 0 -4 -9 30.32 7.81 0 -4 -9 33.79 14.53 0 -4 -9 23.32 13.18 0 4 9 16.44 12.17 0 4 9 25.63 5.74 0 -4 -9 19.76 6.82 0 4 10 623.66 50.51 0 -4 -10 647.37 32.12 0 -4 -10 658.09 31.97 0 -4 -10 689.05 32.46 0 4 10 704.88 56.17 0 -4 -10 639.63 60.60 0 4 10 622.62 25.77 0 4 10 657.58 53.01 0 -4 -10 587.48 56.64 0 -4 -11 17.78 8.16 0 4 11 7.08 12.03 0 -4 -11 12.61 13.74 0 -4 -11 20.73 7.78 0 4 11 25.28 5.90 0 4 11 32.73 11.50 0 -4 -12 35.44 16.65 0 4 12 28.65 11.70 0 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231.98 18.52 0 5 8 217.30 30.81 0 -5 -8 190.17 33.24 0 5 8 208.38 14.78 0 -5 -8 185.93 16.72 0 5 9 92.75 20.89 0 -5 -9 101.22 13.48 0 -5 -9 85.16 24.97 0 -5 -9 124.08 28.32 0 5 9 98.66 22.26 0 5 9 110.30 11.36 0 -5 -9 90.80 12.66 0 5 10 58.71 19.19 0 -5 -10 40.71 9.76 0 -5 -10 35.44 10.93 0 -5 -10 43.01 20.96 0 5 10 46.82 17.90 0 5 10 40.51 7.44 0 -5 -10 34.83 9.09 0 -5 -11 3.67 5.48 0 -5 -11 1.82 9.57 0 5 11 26.19 15.36 0 -5 -11 2.96 4.89 0 5 11 5.01 5.70 0 5 11 2.80 3.87 0 5 11 19.68 10.33 0 -5 -12 238.66 18.99 0 5 12 281.10 18.08 0 5 12 252.09 15.65 0 -5 -12 249.54 19.70 0 5 12 260.00 36.17 0 5 13 -15.73 15.36 0 -5 -13 3.69 5.35 0 -5 -13 -3.80 4.48 0 5 13 -3.81 4.65 0 -5 -14 -2.62 4.76 0 5 14 -4.72 4.54 0 5 14 -4.24 4.86 0 -5 -14 -3.14 3.97 0 -5 -15 -0.56 3.23 0 -5 -15 -3.82 3.22 0 5 15 -1.21 3.68 0 5 16 4.49 2.45 0 6 -20 8.31 4.01 0 6 -19 11.75 5.54 0 6 -18 77.49 10.64 0 6 -17 69.72 8.10 0 -6 17 44.49 14.51 0 6 -17 68.57 10.74 0 6 -16 24.32 5.52 0 6 -16 32.05 8.81 0 -6 16 21.77 18.31 0 6 -15 86.89 9.84 0 6 -15 83.50 9.70 0 6 -15 86.24 12.45 0 -6 15 80.26 20.78 0 6 -14 127.69 14.32 0 6 -14 96.82 10.69 0 6 -14 109.06 22.96 0 6 -14 98.03 11.19 0 6 -14 101.57 11.04 0 -6 14 101.86 22.52 0 6 -13 3.70 5.43 0 6 -13 6.62 4.49 0 6 -13 1.74 10.96 0 6 -13 15.78 7.13 0 6 -13 9.35 4.34 0 -6 13 10.84 11.18 0 6 -12 145.52 14.25 0 6 -12 139.76 12.37 0 6 -12 165.24 28.63 0 -6 12 167.09 25.83 0 6 -12 149.47 13.21 0 6 -12 161.53 13.77 0 -6 12 139.65 25.08 0 -6 11 17.19 11.14 0 6 -11 29.90 6.63 0 6 -11 19.44 5.36 0 -6 11 15.65 11.62 0 6 -11 12.88 8.61 0 6 -11 23.54 6.35 0 6 -11 27.41 6.14 0 6 -11 21.44 4.70 0 -6 10 131.59 21.64 0 6 -10 150.91 12.45 0 6 -10 117.15 11.19 0 6 -10 130.23 11.71 0 6 -10 134.93 11.42 0 6 -10 128.02 12.19 0 -6 10 140.02 22.04 0 6 -10 103.52 21.37 0 6 -10 114.55 10.46 0 6 -9 13.43 9.10 0 -6 9 2.57 8.57 0 6 -9 2.42 3.87 0 -6 9 -5.37 7.67 0 6 -9 0.46 3.80 0 6 -8 699.62 25.40 0 6 -8 661.44 40.13 0 -6 8 716.40 45.51 0 6 -8 628.14 47.38 0 -6 8 727.64 44.70 0 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784.57 59.01 0 8 -7 249.70 17.17 0 -8 7 208.83 30.78 0 -8 7 235.01 15.82 0 -8 7 224.09 29.63 0 8 -7 260.27 16.34 0 8 -7 235.25 16.67 0 8 -7 252.53 17.66 0 -8 7 216.15 32.04 0 -8 6 207.59 14.73 0 -8 6 191.90 29.03 0 -8 6 201.50 27.56 0 8 -6 228.82 14.73 0 8 -6 207.80 15.24 0 -8 6 208.90 31.65 0 8 -6 217.31 15.71 0 -8 5 99.18 10.22 0 8 -5 107.50 10.31 0 8 -5 110.69 11.45 0 -8 5 87.94 10.19 0 -8 5 104.30 22.15 0 8 -5 103.66 18.44 0 -8 5 109.66 23.21 0 8 -5 91.31 10.80 0 -8 4 5.93 9.40 0 -8 4 -0.08 3.58 0 -8 4 -10.71 9.73 0 8 -4 -1.09 4.72 0 8 -4 -4.71 4.57 0 -8 4 -3.44 7.60 0 -8 4 -3.72 8.78 0 8 -4 -15.46 10.88 0 -8 4 -1.99 4.13 0 8 -4 3.60 5.55 0 -8 3 18.71 5.49 0 -8 3 26.92 15.13 0 -8 3 26.34 11.49 0 -8 3 18.04 7.58 0 8 -3 18.98 5.94 0 8 -3 14.11 5.16 0 -8 3 16.47 5.97 0 8 -3 20.25 6.07 0 8 -3 32.15 11.25 0 -8 3 27.06 15.57 0 -8 3 22.28 9.65 0 8 -2 46.78 14.88 0 -8 2 65.92 14.38 0 -8 2 54.27 7.93 0 -8 2 51.72 14.37 0 -8 2 45.88 16.86 0 -8 2 72.61 16.13 0 8 -2 49.92 7.97 0 8 -2 59.03 8.88 0 8 -2 56.84 7.49 0 -8 2 48.59 8.41 0 8 -2 49.56 8.04 0 8 -1 28.26 12.47 0 -8 1 21.38 11.03 0 -8 1 15.73 5.58 0 -8 1 16.02 5.67 0 8 -1 7.05 4.09 0 8 -1 22.87 6.20 0 8 -1 12.73 4.75 0 8 -1 19.70 5.23 0 -8 1 22.65 7.44 0 8 0 50.40 16.23 0 -8 0 43.71 15.81 0 -8 0 35.03 7.10 0 -8 0 54.28 9.09 0 -8 0 39.01 14.73 0 8 0 54.27 8.38 0 8 0 53.14 8.71 0 8 0 44.25 7.48 0 -8 0 49.49 8.91 0 8 0 45.22 7.50 0 8 1 19.67 12.13 0 -8 -1 7.65 12.92 0 -8 -1 25.41 7.01 0 -8 -1 22.54 6.91 0 -8 -1 35.60 17.73 0 8 1 21.05 6.15 0 8 1 22.48 6.36 0 8 1 23.85 5.78 0 -8 -2 90.27 22.44 0 8 2 123.72 10.70 0 -8 -2 111.90 12.63 0 -8 -2 84.34 10.86 0 8 2 98.08 11.33 0 8 2 115.87 11.74 0 8 2 73.04 19.29 0 -8 -2 77.47 21.44 0 -8 -3 142.89 26.36 0 -8 -3 192.43 16.18 0 -8 -3 203.44 16.74 0 8 3 172.74 12.86 0 -8 -3 191.95 15.13 0 8 3 179.80 14.87 0 8 3 192.42 15.04 0 -8 -3 211.91 35.36 0 8 3 198.01 31.37 0 -8 -4 592.04 29.20 0 -8 -4 653.99 30.90 0 -8 -4 588.67 27.43 0 8 4 635.18 25.29 0 -8 -4 538.18 54.71 0 8 4 614.60 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307.96 41.28 -2 9 -4 351.33 21.61 2 -9 4 372.85 21.09 2 -9 4 321.73 18.50 2 -9 5 39.43 7.84 -2 9 -5 31.43 6.47 -2 9 -5 32.59 7.56 2 -9 5 23.29 14.20 2 -9 5 30.73 7.60 2 -9 5 36.13 13.80 2 -9 5 43.88 8.08 -2 9 -5 36.69 9.18 2 -9 5 45.39 9.28 2 -9 6 21.77 7.17 2 -9 6 12.28 14.35 2 -9 6 25.42 10.36 2 -9 6 2.26 4.53 -2 9 -6 11.13 5.35 -2 9 -6 19.01 7.27 2 -9 6 -0.08 10.12 -2 9 -6 12.47 5.77 -2 9 -6 13.19 6.67 2 -9 7 3.72 6.47 2 -9 7 -6.00 13.48 -2 9 -7 1.11 6.07 2 -9 7 0.14 3.82 2 -9 7 19.34 12.33 -2 9 -7 5.63 6.34 2 -9 8 36.32 8.64 2 -9 8 47.26 17.87 -2 9 -8 34.42 7.81 2 -9 8 37.46 7.43 2 -9 8 47.15 18.73 -2 9 -8 28.90 8.26 2 -9 9 61.12 19.42 2 -9 9 85.00 12.13 2 -9 9 83.46 10.43 -2 9 -9 95.68 12.15 2 -9 9 83.06 20.48 -2 9 -9 92.00 12.23 2 -9 10 48.34 9.58 -2 9 -10 48.51 8.66 2 -9 10 51.17 8.65 2 -9 10 48.30 17.31 -2 9 -10 44.29 9.74 2 -9 11 19.98 6.68 2 -9 11 22.21 6.31 -2 9 -11 19.62 6.12 2 -9 11 9.45 13.30 -2 9 -11 22.50 7.58 2 -9 12 27.24 7.13 2 -9 12 16.79 6.03 2 -9 12 32.47 16.95 -2 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25.89 2 -5 0 260.41 13.77 2 -5 0 306.55 21.85 2 -5 1 151.95 20.08 -2 5 -1 137.27 15.75 2 -5 1 147.94 18.97 2 -5 1 140.34 9.96 2 -5 2 364.30 29.39 -2 5 -2 359.75 23.50 2 -5 2 361.41 21.18 2 -5 2 348.27 15.23 2 -5 2 389.24 28.63 2 -5 3 437.77 31.84 -2 5 -3 421.80 24.04 -2 5 -3 386.02 31.28 2 -5 3 442.27 17.26 2 -5 4 263.26 25.23 -2 5 -4 206.62 24.13 2 -5 4 236.84 18.34 2 -5 4 237.69 24.66 2 -5 5 38.92 12.63 2 -5 5 35.64 11.59 2 -5 5 27.35 9.98 2 -5 5 32.47 7.68 -2 5 -5 30.12 10.88 2 -5 6 2332.97 84.75 -2 5 -6 2525.15 91.41 2 -5 6 2631.55 73.52 2 -5 6 2418.68 84.42 2 -5 7 451.36 37.32 -2 5 -7 440.53 39.32 2 -5 7 462.09 32.06 2 -5 7 446.28 35.96 2 -5 8 1045.93 59.89 -2 5 -8 1004.98 62.28 2 -5 8 1129.48 59.49 2 -5 8 1051.38 29.36 2 -5 9 0.93 9.12 -2 5 -9 -0.42 3.29 2 -5 9 3.10 6.61 -2 5 -9 -6.12 7.53 2 -5 9 -1.19 2.81 -2 5 -10 270.41 35.17 2 -5 10 253.38 30.66 -2 5 -10 284.54 17.49 -2 5 -10 244.71 16.59 2 -5 10 244.78 32.40 2 -5 10 254.22 14.83 2 -5 11 -18.05 13.54 -2 5 -11 -5.60 8.64 -2 5 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44.24 9.15 -5 8 -4 30.95 8.33 5 -8 4 33.13 9.09 5 -8 4 34.66 8.29 5 -8 5 158.61 14.48 5 -8 5 147.34 14.10 5 -8 5 161.72 14.48 -5 8 -5 152.01 14.85 5 -8 5 169.36 16.61 5 -8 6 132.18 12.56 5 -8 6 138.11 13.83 5 -8 6 137.97 13.69 -5 8 -6 145.21 14.10 5 -8 6 134.29 14.54 -5 8 -6 133.72 12.64 -5 8 -7 11.30 5.14 5 -8 7 17.93 7.58 -5 8 -7 12.39 5.87 5 -8 7 12.06 5.93 -5 8 -8 22.02 6.52 5 -8 8 23.98 8.13 -5 8 -8 27.98 7.23 5 -8 8 27.63 7.18 -5 8 -9 -2.81 5.83 -5 8 -9 -1.69 4.63 5 -8 9 7.56 6.47 5 -8 9 3.25 5.47 -5 8 -10 35.01 8.36 5 -8 10 40.96 8.35 5 -8 10 37.39 7.77 -5 8 -11 35.20 7.59 5 -8 11 29.63 7.59 5 -8 11 30.77 6.91 -5 8 -12 82.08 10.35 5 -8 12 71.92 9.61 5 -8 12 86.22 9.70 -5 8 -13 -3.27 4.84 5 -8 13 1.33 4.15 -5 8 -14 162.70 11.91 5 -8 14 139.91 11.09 -5 8 -15 -1.63 3.31 5 -8 15 11.11 3.92 -5 7 12 16.88 3.84 -5 7 12 21.49 3.77 5 -7 -11 -4.63 3.03 -5 7 11 -0.12 3.22 5 -7 -10 8.25 3.48 -5 7 10 21.34 5.55 5 -7 -9 -4.30 4.00 -5 7 9 0.27 4.31 5 -7 -9 8.03 3.97 5 -7 -8 37.42 7.52 5 -7 -8 59.97 8.20 -5 7 8 52.53 8.96 5 -7 -8 47.81 7.64 5 -7 -7 309.72 18.99 5 -7 -7 359.06 20.56 -5 7 7 367.66 21.49 5 -7 -7 370.76 20.75 -5 7 7 406.82 21.40 5 -7 -7 399.58 24.24 5 -7 -6 33.91 7.66 -5 7 6 38.66 16.11 5 -7 -6 28.47 8.73 5 -7 -6 26.32 6.52 -5 7 6 33.07 8.03 5 -7 -5 72.61 10.55 -5 7 5 63.29 16.90 -5 7 5 49.80 8.17 5 -7 -5 54.67 11.32 5 -7 -5 61.70 9.24 -5 7 5 64.28 10.63 5 -7 -4 5.47 5.75 5 -7 -4 3.20 5.06 -5 7 4 4.49 6.85 -5 7 4 10.08 11.14 -5 7 4 -4.10 5.43 5 -7 -4 5.17 6.87 5 -7 -3 11.48 6.19 -5 7 3 9.43 5.62 5 -7 -3 3.74 5.46 -5 7 3 16.39 10.92 -5 7 3 14.37 6.08 5 -7 -3 6.09 6.05 5 -7 -2 8.04 5.09 -5 7 2 4.31 6.45 5 -7 -2 2.05 5.09 -5 7 2 1.42 8.60 -5 7 2 -1.36 5.25 5 -7 -2 12.95 7.57 5 -7 -1 57.89 9.83 5 -7 -1 73.05 10.13 -5 7 1 56.14 10.18 5 -7 -1 56.78 10.70 -5 7 1 62.33 10.02 5 -7 0 309.14 20.25 5 -7 0 282.23 18.50 -5 7 0 291.85 20.31 5 -7 0 293.73 20.75 -5 7 0 301.21 19.68 5 -7 1 65.53 10.21 -5 7 -1 61.32 9.58 5 -7 1 61.26 9.30 -5 7 -1 66.24 10.36 5 -7 1 65.05 11.07 5 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4 -0.97 8.50 5 -6 -4 -0.37 6.07 5 -6 -3 131.87 12.88 -5 6 3 134.01 13.48 5 -6 -3 113.87 13.48 -5 6 3 120.68 21.59 5 -6 -3 139.65 14.53 5 -6 -2 321.31 21.39 5 -6 -2 321.61 19.16 5 -6 -2 318.21 20.84 -5 6 2 327.48 20.15 5 -6 -1 15.25 5.59 5 -6 -1 8.39 6.22 5 -6 -1 14.28 6.96 -5 6 1 11.60 5.91 5 -6 0 28.84 7.50 5 -6 0 27.34 7.14 5 -6 0 19.72 6.74 -5 6 0 35.34 7.89 5 -6 1 169.82 13.23 -5 6 -1 162.97 13.77 -5 6 -1 160.65 14.63 5 -6 1 159.63 13.64 5 -6 1 187.40 15.85 5 -6 1 167.37 15.32 5 -6 2 143.01 13.64 5 -6 2 125.01 11.17 -5 6 -2 143.84 12.43 5 -6 2 120.24 11.98 -5 6 -2 129.82 13.35 5 -6 2 125.71 13.46 5 -6 3 2.14 5.45 -5 6 -3 -1.36 4.85 5 -6 3 -1.11 5.62 -5 6 -3 -7.62 5.77 -5 6 -3 -4.09 3.74 5 -6 3 5.18 6.52 5 -6 3 -1.28 3.44 -5 6 -4 196.69 16.89 5 -6 4 178.01 15.62 5 -6 4 182.72 13.95 -5 6 -4 181.63 14.64 5 -6 4 192.23 16.45 5 -6 5 80.50 10.58 -5 6 -5 86.98 11.83 -5 6 -5 77.05 10.35 -5 6 -5 90.76 10.99 5 -6 5 87.57 11.54 5 -6 5 81.58 10.00 -5 6 -6 50.35 17.85 5 -6 6 24.53 11.39 -5 6 -6 45.35 9.06 -5 6 -6 44.73 8.50 -5 6 -6 32.40 6.64 5 -6 6 49.96 9.19 5 -6 6 35.95 7.33 -5 6 -7 587.89 26.25 5 -6 7 635.96 29.74 -5 6 -7 595.61 28.96 -5 6 -7 552.43 51.87 5 -6 7 642.57 58.53 5 -6 7 662.99 27.86 5 -6 8 -7.68 14.58 -5 6 -8 -11.34 15.33 5 -6 8 6.64 4.84 -5 6 -8 8.55 5.27 -5 6 -8 7.61 4.38 5 -6 8 11.75 7.02 5 -6 8 7.95 5.23 5 -6 9 0.25 4.21 5 -6 9 -6.33 7.42 -5 6 -9 0.65 5.19 5 -6 10 21.00 5.86 5 -6 10 16.50 7.48 -5 6 -10 14.87 7.61 5 -6 11 17.81 5.49 5 -6 11 15.54 6.76 -5 6 -11 14.63 7.03 5 -6 12 39.87 7.14 5 -6 12 49.81 9.34 -5 6 -12 47.56 9.22 5 -6 13 10.62 4.54 5 -6 13 14.36 5.96 -5 6 -13 13.09 4.73 5 -6 14 13.47 4.36 -5 6 -14 22.35 7.06 5 -6 14 17.48 6.40 5 -6 15 2.43 3.85 -5 6 -15 5.88 5.10 5 -6 16 15.21 4.25 -5 6 -16 19.69 4.97 5 -5 -14 36.10 4.56 -5 5 14 35.78 4.55 5 -5 -13 57.98 7.00 -5 5 13 76.30 7.70 5 -5 -12 0.07 4.79 -5 5 12 -7.39 4.69 5 -5 -12 -1.94 3.65 5 -5 -11 6.03 5.63 -5 5 11 0.17 3.51 -5 5 11 -1.60 12.29 -5 5 11 -11.05 12.73 5 -5 -11 4.67 3.96 -5 5 10 4.88 9.38 5 -5 -10 5.24 5.73 -5 5 10 -1.19 4.30 5 -5 -10 3.75 4.62 -5 5 9 88.47 22.34 5 -5 -9 87.01 11.82 -5 5 9 80.69 10.45 5 -5 -9 81.19 10.80 5 -5 -8 96.69 11.53 5 -5 -8 88.97 12.28 -5 5 8 100.77 11.67 5 -5 -8 96.50 11.63 -5 5 8 133.94 27.53 5 -5 -8 105.98 13.58 5 -5 -7 338.87 20.84 5 -5 -7 372.84 23.29 -5 5 7 339.46 20.87 5 -5 -7 333.06 21.35 -5 5 7 318.25 39.97 -5 5 7 348.12 41.20 5 -5 -7 386.47 24.73 5 -5 -6 41.90 7.94 5 -5 -6 40.39 9.96 -5 5 6 27.36 7.94 5 -5 -6 36.87 8.34 -5 5 6 45.10 14.99 -5 5 6 37.72 15.87 5 -5 -6 31.60 8.18 5 -5 -5 -3.51 4.84 -5 5 5 9.36 5.91 5 -5 -5 -5.46 5.88 5 -5 -5 2.31 6.26 -5 5 5 2.43 11.86 -5 5 5 0.94 11.08 -5 5 5 1.91 4.49 5 -5 -5 -2.05 5.50 5 -5 -4 180.30 16.11 5 -5 -4 164.99 13.54 5 -5 -4 153.61 14.39 -5 5 4 177.71 14.76 -5 5 4 136.81 23.08 -5 5 4 180.93 28.09 -5 5 4 145.18 13.89 5 -5 -4 173.31 15.85 5 -5 -3 -0.97 4.54 5 -5 -3 8.42 4.87 5 -5 -3 4.08 6.12 -5 5 3 5.37 7.74 -5 5 3 4.78 7.61 -5 5 3 -1.44 4.35 5 -5 -3 7.66 5.53 5 -5 -2 2.80 5.26 5 -5 -2 -5.89 5.58 -5 5 2 -2.50 7.45 -5 5 2 -0.07 4.58 5 -5 -2 -0.02 5.39 5 -5 -2 -2.88 6.19 -5 5 1 88.34 10.30 5 -5 -1 74.06 8.97 5 -5 -1 97.47 11.77 -5 5 1 80.84 16.90 -5 5 1 78.13 9.97 5 -5 -1 81.14 10.66 5 -5 0 51.15 8.56 5 -5 0 48.75 8.45 5 -5 0 45.82 6.95 -5 5 0 46.95 7.90 -5 5 0 40.20 7.43 5 -5 0 51.27 9.35 5 -5 1 37.37 7.82 5 -5 1 38.82 6.29 5 -5 1 28.63 6.25 -5 5 -1 37.31 7.43 -5 5 -1 27.59 6.47 5 -5 1 32.10 8.01 5 -5 2 24.44 7.26 5 -5 2 28.51 5.57 -5 5 -2 28.14 6.10 5 -5 2 11.97 4.26 -5 5 -2 16.79 5.54 -5 5 -2 24.34 6.14 5 -5 2 25.65 6.78 -5 5 -3 2.37 4.04 5 -5 3 6.88 6.30 -5 5 -3 10.59 4.67 -5 5 -3 4.09 4.06 -5 5 -3 8.22 4.49 5 -5 3 3.64 5.34 5 -5 3 -0.32 3.64 5 -5 4 110.00 23.49 -5 5 -4 110.03 12.17 -5 5 -4 89.29 10.50 5 -5 4 107.65 12.01 5 -5 4 108.76 10.49 5 -5 5 122.07 25.53 -5 5 -5 102.08 20.84 5 -5 5 100.71 11.48 -5 5 -5 120.16 12.88 -5 5 -5 102.84 11.49 5 -5 5 125.33 12.81 5 -5 5 126.99 11.22 5 -5 6 777.76 32.10 -5 5 -6 778.97 32.96 -5 5 -6 775.36 32.15 -5 5 -6 768.35 29.15 5 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6.25 7 -7 -5 22.47 6.23 -7 7 4 5.04 5.03 -7 7 4 0.54 4.60 7 -7 -4 3.54 5.33 -7 7 3 70.12 10.30 7 -7 -3 76.20 10.74 -7 7 3 60.32 8.68 7 -7 -3 73.82 10.49 7 -7 -2 91.68 11.74 -7 7 2 94.29 11.50 7 -7 -2 95.96 12.13 -7 7 2 85.36 10.65 7 -7 -1 63.83 10.06 -7 7 1 59.97 9.93 7 -7 -1 61.64 10.13 -7 7 1 66.60 9.28 7 -7 0 3.39 5.56 -7 7 0 6.78 6.05 7 -7 0 7.56 6.52 -7 7 0 2.73 4.68 7 -7 1 67.82 10.88 -7 7 -1 71.43 10.58 7 -7 1 92.52 12.32 7 -7 2 -8.57 5.86 -7 7 -2 0.12 5.76 7 -7 2 -3.39 5.88 -7 7 -2 -1.95 4.35 -7 7 -3 11.93 5.95 7 -7 3 21.20 7.59 7 -7 3 16.52 6.30 -7 7 -4 23.36 6.67 7 -7 4 29.58 7.39 7 -7 4 23.41 6.69 -7 7 -5 7.77 5.08 7 -7 5 11.68 6.20 7 -7 5 5.71 5.13 -7 7 -6 22.61 5.71 7 -7 6 19.29 6.64 7 -7 6 20.13 6.44 7 -7 7 8.89 4.06 7 -7 7 12.26 5.09 7 -7 7 10.12 5.39 -7 7 -7 15.45 4.38 -7 7 -8 163.66 11.61 7 -7 8 155.79 10.93 7 -7 8 158.78 13.13 7 -7 8 160.49 13.52 -7 7 -9 11.12 4.87 7 -7 9 6.27 5.16 7 -7 9 -2.34 4.80 -7 7 -10 11.33 3.59 7 -7 10 9.44 4.68 7 -7 10 9.34 3.70 -7 7 -11 4.36 3.40 7 -7 11 6.55 3.75 7 -7 11 -1.89 3.46 -7 7 -12 157.30 9.30 -7 6 11 0.06 2.31 -7 6 10 37.38 5.26 7 -6 -10 40.87 5.49 -7 6 9 8.48 3.90 7 -6 -9 8.51 3.95 -7 6 9 13.96 4.64 7 -6 -8 -4.70 3.94 -7 6 8 0.01 3.93 7 -6 -7 131.58 11.64 -7 6 7 158.30 13.17 7 -6 -7 156.11 13.60 -7 6 7 138.28 10.96 7 -6 -6 23.40 5.97 -7 6 6 25.51 7.00 -7 6 6 24.38 5.96 7 -6 -6 31.80 7.79 7 -6 -5 57.12 8.68 -7 6 5 55.78 9.23 7 -6 -5 62.16 9.89 7 -6 -5 50.79 9.55 7 -6 -4 37.74 7.09 -7 6 4 40.29 9.56 7 -6 -4 42.41 8.06 7 -6 -4 47.38 9.59 7 -6 -3 2.71 5.98 7 -6 -3 -4.45 4.05 -7 6 3 2.59 5.59 7 -6 -3 -3.39 6.24 -7 6 2 243.31 17.83 7 -6 -2 231.52 18.48 7 -6 -2 235.39 18.46 7 -6 -1 1.97 5.61 -7 6 1 3.62 5.10 7 -6 -1 1.31 6.09 -7 6 0 205.73 15.49 7 -6 0 193.58 17.51 7 -6 0 186.63 16.56 7 -6 1 32.93 8.75 7 -6 1 19.39 7.64 -7 6 -2 115.90 11.53 7 -6 2 109.37 13.10 7 -6 2 116.09 12.89 -7 6 -2 102.00 12.51 7 -6 3 2.28 5.93 -7 6 -3 8.32 6.44 7 -6 3 5.10 6.05 -7 6 -3 2.61 4.51 7 -6 4 83.47 11.97 -7 6 -4 84.90 10.85 7 -6 4 87.91 12.01 -7 6 -4 71.85 11.43 -7 6 -5 29.62 7.04 7 -6 5 33.08 7.87 7 -6 5 30.19 8.13 -7 6 -5 22.33 5.85 -7 6 -6 9.35 5.32 7 -6 6 5.37 5.32 7 -6 6 0.51 6.15 -7 6 -6 3.65 4.83 7 -6 7 1.49 4.71 7 -6 7 1.91 5.83 -7 6 -7 -1.54 4.60 -7 6 -7 -2.77 3.98 7 -6 8 138.16 13.17 7 -6 8 125.59 12.83 -7 6 -8 116.38 10.79 -7 6 -8 120.82 11.79 7 -6 9 22.85 6.79 7 -6 9 22.16 6.59 -7 6 -9 19.80 6.14 -7 6 -9 10.75 3.85 7 -6 10 42.71 7.61 -7 6 -10 39.63 6.56 -7 6 -10 34.04 6.80 7 -6 10 47.83 7.70 -7 6 -11 -5.99 4.63 7 -6 11 -0.75 3.66 7 -6 11 5.43 4.05 -7 6 -12 37.31 5.60 7 -6 12 40.70 6.05 7 -6 12 29.07 5.32 -7 6 -13 6.11 3.04 -7 5 12 18.46 3.58 -7 5 11 2.51 3.20 7 -5 -11 -1.85 3.33 7 -5 -10 19.46 5.55 -7 5 10 16.51 4.65 7 -5 -9 118.76 11.95 -7 5 9 128.71 11.29 7 -5 -8 37.15 7.88 -7 5 8 38.32 7.29 7 -5 -7 -1.52 4.40 -7 5 7 2.36 5.29 7 -5 -7 2.52 4.77 7 -5 -6 4.02 4.52 -7 5 6 6.62 5.72 7 -5 -6 3.31 6.42 7 -5 -6 14.29 6.71 7 -5 -5 5.76 7.27 7 -5 -5 -5.41 5.42 -7 5 5 5.79 6.56 7 -5 -5 4.32 5.14 7 -5 -4 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14.58 3.69 7 7 -12 43.89 6.70 7 7 -12 51.89 6.40 7 7 -11 101.15 10.24 7 7 -11 92.49 8.66 7 7 -10 35.20 6.95 -7 -7 10 36.29 6.99 7 7 -9 16.98 6.05 -7 -7 9 13.60 5.53 -7 -7 8 6.88 5.06 7 7 -8 17.30 7.14 -7 -7 8 5.77 3.21 -7 -7 7 7.76 4.80 7 7 -7 -0.20 4.83 -7 -7 7 4.80 4.06 -7 -7 6 24.00 7.08 7 7 -6 34.17 6.71 7 7 -6 33.59 8.82 -7 -7 6 28.27 6.79 -7 -7 5 47.06 8.73 7 7 -5 54.07 10.49 7 7 -5 62.44 8.96 -7 -7 5 45.76 8.27 -7 -7 4 77.31 10.66 7 7 -4 57.16 10.95 7 7 -4 74.17 10.00 -7 -7 4 51.86 9.18 -7 -7 3 41.01 8.04 -7 -7 3 44.48 8.72 7 7 -3 34.65 8.15 7 7 -3 28.43 7.58 7 7 -2 87.79 11.99 -7 -7 2 96.48 11.16 -7 -7 2 89.11 11.92 7 7 -2 106.94 12.24 -7 -7 1 53.02 9.68 7 7 -1 67.04 9.85 7 7 -1 62.10 10.08 -7 -7 0 57.13 9.53 7 7 0 46.84 8.99 7 7 0 53.27 8.90 -7 -7 0 43.77 7.42 7 7 1 102.82 11.10 -7 -7 -1 102.19 10.57 -7 -7 -1 94.33 11.38 -7 -7 -1 91.97 10.41 7 7 1 97.81 9.16 7 7 2 90.91 9.54 -7 -7 -2 119.27 11.14 -7 -7 -2 104.52 11.80 -7 -7 -2 102.04 9.99 7 7 2 102.94 9.13 7 7 3 -1.32 3.62 -7 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5.95 6.10 8 -5 1 0.41 4.48 -8 5 -1 1.22 4.12 8 -5 2 8.74 6.78 8 -5 2 3.03 4.50 -8 5 -2 14.86 5.95 8 -5 3 179.99 14.40 -8 5 -3 186.61 15.57 8 -5 3 206.52 17.07 8 -5 4 51.04 9.00 -8 5 -4 43.09 7.16 8 -5 4 46.77 8.08 -8 5 -4 45.10 9.08 8 -5 5 5.96 5.67 -8 5 -5 8.35 3.95 -8 5 -5 10.37 4.95 8 -5 5 11.28 5.84 -8 5 -5 -1.09 4.54 -8 5 -6 123.56 10.51 8 -5 6 115.88 10.99 8 -5 7 29.05 5.90 8 -5 7 38.86 7.43 -8 5 -7 36.16 6.14 8 -5 8 6.63 4.03 8 -5 8 8.70 5.22 -8 5 -8 2.57 3.65 -8 5 -8 6.85 3.87 8 -5 9 36.30 5.54 8 -5 9 39.55 6.65 -8 5 -9 47.80 6.36 -8 5 -9 41.63 5.99 -8 5 -10 6.86 3.25 8 -5 10 2.78 3.36 -8 5 -10 0.85 2.68 8 -5 11 -1.30 2.85 8 -4 -11 19.25 4.19 8 -4 -10 2.71 3.10 -8 4 10 8.78 3.49 8 -4 -9 34.18 6.91 -8 4 9 36.35 6.02 8 -4 -8 62.83 8.53 -8 4 8 70.89 8.40 -8 4 7 25.80 6.02 8 -4 -7 35.39 7.58 -8 4 6 0.26 4.99 8 -4 -6 0.32 4.68 8 -4 -6 3.60 5.87 -8 4 6 2.12 3.63 8 -4 -6 -0.23 4.79 8 -4 -5 83.48 11.54 -8 4 5 85.08 10.31 8 -4 -5 92.00 10.32 -8 4 5 77.74 10.03 8 -4 -5 71.16 10.42 8 -4 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49.14 6.18 -9 -1 -6 42.19 5.43 -9 -1 -6 46.67 5.97 -9 -1 -7 6.07 2.96 9 1 7 0.19 2.45 9 2 -11 82.69 7.61 9 2 -10 133.76 10.65 9 2 -10 166.23 11.50 -9 -2 10 164.36 11.41 9 2 -9 4.00 4.82 -9 -2 9 -1.27 3.66 9 2 -9 4.46 4.04 9 2 -8 1.90 4.24 -9 -2 8 2.37 3.86 -9 -2 8 4.64 4.52 9 2 -8 4.51 3.63 9 2 -7 24.34 6.74 -9 -2 7 20.97 5.23 -9 -2 7 23.70 6.26 9 2 -7 19.81 5.72 9 2 -6 125.69 11.96 9 2 -6 135.02 13.09 -9 -2 6 122.65 10.80 -9 -2 6 121.23 12.19 -9 -2 6 125.45 11.85 9 2 -5 8.26 4.19 -9 -2 5 5.70 4.60 9 2 -5 13.13 4.99 -9 -2 5 8.72 4.23 -9 -2 5 3.72 4.50 9 2 -4 11.75 5.11 -9 -2 4 12.77 5.29 9 2 -4 12.72 5.95 -9 -2 4 11.87 5.61 -9 -2 4 6.83 4.63 9 2 -3 65.81 8.68 -9 -2 3 53.66 8.87 9 2 -3 50.62 8.84 -9 -2 3 67.42 9.73 -9 -2 3 59.97 8.45 9 2 -2 91.09 9.74 -9 -2 2 85.35 10.07 9 2 -2 78.60 10.43 -9 -2 2 100.79 11.91 -9 -2 2 100.84 10.47 -9 -2 1 -1.60 4.26 9 2 -1 -0.66 4.48 9 2 -1 -6.39 4.14 -9 -2 1 0.53 3.33 -9 -2 1 1.83 3.39 -9 -2 0 62.25 9.60 9 2 0 48.81 8.50 9 2 0 55.09 8.44 -9 -2 0 53.09 7.20 -9 -2 0 59.67 7.97 9 2 1 18.94 6.43 9 2 1 32.44 6.77 -9 -2 -1 19.15 5.36 -9 -2 -1 32.33 7.23 9 2 2 21.01 6.10 9 2 2 19.36 5.32 -9 -2 -2 20.52 5.03 -9 -2 -2 17.78 5.67 9 2 3 4.98 4.19 9 2 3 7.67 3.78 -9 -2 -3 0.96 3.38 -9 -2 -3 8.74 4.71 9 2 4 287.34 16.21 9 2 4 252.00 13.48 -9 -2 -4 293.30 15.87 -9 -2 -4 278.73 15.34 9 2 5 8.34 4.23 9 2 5 12.30 3.40 -9 -2 -5 18.63 4.40 -9 -2 -5 15.75 4.38 -9 -2 -6 1.35 2.55 9 2 6 -1.29 2.67 9 3 -11 4.85 2.75 -9 -3 11 5.84 3.01 9 3 -10 41.92 5.87 9 3 -10 41.17 5.97 -9 -3 10 53.26 6.81 9 3 -9 94.88 9.34 9 3 -9 93.14 9.26 -9 -3 9 83.01 8.86 9 3 -8 244.74 15.40 -9 -3 8 232.88 15.36 9 3 -8 255.33 15.59 9 3 -7 22.23 5.60 -9 -3 7 12.83 4.87 -9 -3 7 7.17 4.69 9 3 -7 8.31 4.27 9 3 -6 88.31 10.56 -9 -3 6 77.85 9.69 -9 -3 6 69.10 8.64 9 3 -6 79.34 9.64 9 3 -5 23.42 6.23 -9 -3 5 22.63 6.04 -9 -3 5 14.49 5.24 9 3 -5 17.58 5.32 9 3 -4 342.60 19.03 9 3 -4 345.11 19.08 -9 -3 4 327.06 19.79 -9 -3 4 360.52 19.81 -9 -3 4 376.03 20.37 9 3 -3 17.70 5.38 -9 -3 3 21.20 5.54 9 3 -3 14.80 4.66 -9 -3 3 20.07 6.03 -9 -3 3 27.46 7.07 9 3 -2 47.82 7.07 -9 -3 2 60.57 8.44 9 3 -2 54.63 8.08 -9 -3 2 58.78 9.64 -9 -3 2 46.48 7.72 -9 -3 1 -0.14 4.20 9 3 -1 3.64 4.66 9 3 -1 1.94 2.89 -9 -3 1 -4.66 3.91 -9 -3 1 -3.48 3.00 9 3 0 59.14 8.80 9 3 0 48.66 8.00 -9 -3 0 53.88 7.31 -9 -3 0 47.11 8.39 9 3 1 6.78 4.37 9 3 1 4.52 4.49 -9 -3 -1 2.86 3.82 -9 -3 -1 4.52 4.40 9 3 2 45.15 7.30 9 3 2 60.84 7.56 -9 -3 -2 51.73 7.52 -9 -3 -2 48.43 7.66 9 3 3 0.35 3.32 9 3 3 -6.66 3.94 -9 -3 -3 7.00 3.98 -9 -3 -3 1.09 3.01 9 3 4 174.34 11.66 9 3 4 165.46 10.47 -9 -3 -4 160.95 10.44 -9 -3 -4 150.74 10.92 -9 -3 -5 3.98 3.01 9 3 5 4.31 2.97 9 4 -11 89.00 7.40 -9 -4 10 17.87 4.47 9 4 -10 15.66 4.05 9 4 -9 73.29 8.00 9 4 -8 131.95 10.20 9 4 -8 132.24 11.13 -9 -4 8 109.63 8.99 9 4 -7 22.14 5.87 -9 -4 7 11.42 3.60 9 4 -7 14.40 4.43 9 4 -6 79.26 9.40 -9 -4 6 72.10 9.03 -9 -4 6 74.08 9.02 9 4 -6 85.06 9.49 9 4 -5 31.28 5.80 -9 -4 5 26.82 6.37 -9 -4 5 23.21 6.45 9 4 -5 25.56 5.98 9 4 -4 -2.32 4.54 -9 -4 4 3.95 3.79 -9 -4 4 2.36 4.63 9 4 -4 -1.69 4.01 9 4 -3 4.09 3.56 -9 -4 3 8.45 3.71 9 4 -3 5.18 3.77 -9 -4 3 11.93 5.42 -9 -4 3 6.44 3.61 -9 -4 2 65.41 9.02 9 4 -2 65.05 8.28 9 4 -2 52.56 8.20 9 4 -2 56.42 7.44 -9 -4 2 38.97 5.89 -9 -4 2 56.69 7.03 9 4 -1 -0.79 3.45 9 4 -1 -0.15 4.18 9 4 -1 3.52 3.04 -9 -4 1 5.43 3.73 -9 -4 1 -5.51 4.93 9 4 0 13.09 4.54 9 4 0 18.63 5.90 -9 -4 0 18.25 5.19 -9 -4 0 16.70 5.40 9 4 1 0.10 3.55 9 4 1 2.40 3.88 -9 -4 -1 1.11 3.40 -9 -4 -1 -1.58 3.81 9 4 2 -0.26 3.12 9 4 2 2.22 3.64 -9 -4 -2 0.27 3.12 -9 -4 -2 3.14 3.51 9 4 3 5.60 3.38 9 4 3 4.53 2.96 -9 -4 -3 3.49 3.08 -9 -4 -3 -0.41 2.79 -9 -4 -4 3.81 2.65 9 4 4 8.96 3.47 9 5 -11 1.53 2.28 9 5 -10 25.34 4.39 -9 -5 10 27.12 4.82 9 5 -9 2.63 2.95 9 5 -8 1.32 3.10 -9 -5 8 2.95 3.05 9 5 -7 3.36 3.37 -9 -5 7 6.90 3.57 9 5 -6 23.28 4.90 9 5 -6 30.06 5.97 -9 -5 6 26.48 6.35 9 5 -5 12.86 4.41 -9 -5 5 6.12 3.84 9 5 -4 40.72 6.45 -9 -5 4 47.62 7.81 -9 -5 3 5.92 4.10 9 5 -3 -7.19 3.49 9 5 -3 -0.94 3.38 -9 -5 3 1.82 3.11 -9 -5 3 2.09 3.51 9 5 -2 8.35 3.47 9 5 -2 7.25 4.37 9 5 -2 11.24 3.78 -9 -5 2 4.70 3.15 -9 -5 2 8.71 3.95 9 5 -1 4.14 3.10 9 5 -1 7.55 4.40 9 5 -1 -2.69 3.34 -9 -5 1 5.05 3.50 -9 -5 1 -4.09 4.13 9 5 0 241.53 12.62 9 5 0 267.71 14.61 -9 -5 0 251.34 13.74 -9 -5 0 252.07 14.51 9 5 1 1.42 2.55 9 5 1 0.71 3.11 -9 -5 -1 -2.97 3.31 -9 -5 -1 7.58 3.75 9 5 2 11.58 3.20 9 5 2 9.16 3.26 -9 -5 -2 10.96 3.02 -9 -5 -2 2.90 2.76 9 6 -10 11.54 3.01 9 6 -9 36.73 4.94 -9 -6 8 36.94 5.09 9 6 -8 51.42 6.30 -9 -6 7 -0.52 2.82 9 6 -7 4.75 3.15 -9 -6 6 10.78 3.85 9 6 -6 17.65 4.51 -9 -6 5 10.70 3.99 9 6 -5 12.36 4.00 -9 -6 4 43.79 6.77 9 6 -4 54.70 6.78 9 6 -3 12.64 3.58 -9 -6 3 14.46 4.61 -9 -6 3 2.64 2.80 9 6 -2 13.23 3.46 -9 -6 2 4.74 3.22 -9 -6 2 3.88 2.66 9 6 -1 -1.42 3.04 -9 -6 1 0.71 2.78 -9 -6 1 1.68 2.56 9 6 0 31.01 4.87 -9 -6 0 36.23 4.78 -9 -6 0 30.86 4.76 9 6 1 14.63 3.28 9 7 -8 70.30 6.28 9 7 -7 3.03 2.32 -9 -7 6 10.45 3.26 9 7 -6 24.03 4.37 -9 -7 5 14.46 3.66 9 7 -5 14.54 3.32 -9 -7 4 36.63 4.98 9 7 -4 31.59 4.46 -9 -7 3 16.70 3.97 10 -4 -2 5.39 3.13 10 -4 -1 1.97 2.77 10 -4 0 53.40 6.30 10 -4 1 78.19 7.36 10 -3 -3 20.50 4.10 10 -3 -2 23.75 4.75 10 -3 -2 4.73 2.84 10 -3 -1 67.03 7.33 10 -3 0 1.46 2.99 10 -3 1 8.83 3.45 10 -3 2 -0.13 2.92 10 -2 -6 8.02 2.84 -10 2 6 6.33 2.67 10 -2 -5 149.24 10.11 -10 2 5 155.48 9.15 -10 2 4 2.91 2.68 10 -2 -4 -5.89 3.39 10 -2 -3 40.08 6.00 -10 2 3 55.01 5.55 10 -2 -3 58.02 6.83 -10 2 2 -1.16 2.30 10 -2 -2 4.68 3.45 -10 2 1 58.02 6.48 10 -2 -1 61.56 7.03 -10 2 0 16.85 4.15 10 -2 0 18.04 4.63 10 -2 0 11.37 3.93 -10 2 -1 48.80 6.20 10 -2 1 40.67 5.27 10 -2 1 44.16 5.62 -10 2 -2 -0.88 2.49 10 -2 2 -11.57 3.82 -10 2 -3 7.81 2.96 -10 2 -4 3.67 2.54 10 -1 -7 121.03 8.84 -10 1 7 129.70 8.29 -10 1 6 1.38 2.77 10 -1 -6 2.09 3.25 -10 1 5 4.50 3.59 10 -1 -5 5.17 4.02 -10 1 4 3.14 3.16 10 -1 -4 19.08 5.09 -10 1 3 95.58 7.76 -10 1 3 102.86 8.72 10 -1 -3 102.13 9.44 -10 1 2 9.04 3.80 -10 1 2 14.26 4.69 10 -1 -2 10.42 3.69 -10 1 1 1.93 3.04 10 -1 -1 -5.67 3.94 -10 1 0 4.69 3.65 10 -1 0 -1.71 3.61 10 -1 0 4.99 3.21 -10 1 -1 45.48 6.30 10 -1 1 34.80 5.59 10 -1 1 34.55 5.54 -10 1 -2 3.48 3.08 10 -1 2 5.79 3.25 -10 1 -3 6.56 3.18 10 -1 3 16.07 3.84 -10 1 -4 2.26 2.41 10 0 -8 -5.79 3.31 10 0 -7 120.49 9.12 -10 0 6 25.78 4.65 10 0 -6 14.97 4.27 -10 0 5 131.17 9.71 10 0 -5 151.24 11.14 -10 0 4 1.48 3.16 -10 0 4 -3.83 3.29 10 0 -4 3.07 3.73 -10 0 3 2.11 2.66 -10 0 3 4.04 3.02 10 0 -3 1.22 3.59 -10 0 2 1.89 2.65 -10 0 2 1.49 2.52 10 0 -2 6.02 4.84 -10 0 1 16.55 4.74 10 0 -1 5.87 4.13 10 0 -1 11.15 4.35 -10 0 0 3.22 2.85 10 0 0 -0.49 3.28 -10 0 -1 3.12 3.50 10 0 1 1.15 3.00 -10 0 -2 2.27 3.00 10 0 2 1.98 2.76 -10 0 -3 -5.55 3.05 10 0 3 3.97 2.63 10 1 -8 -4.78 3.30 10 1 -7 7.14 3.61 -10 -1 6 21.37 4.17 10 1 -6 18.55 4.85 -10 -1 5 263.89 13.77 10 1 -5 259.88 14.68 -10 -1 4 49.33 6.06 -10 -1 4 51.84 6.40 10 1 -4 47.19 7.11 -10 -1 3 8.95 3.57 -10 -1 3 4.79 3.01 10 1 -3 6.29 4.38 -10 -1 2 3.76 2.86 10 1 -2 3.61 3.41 10 1 -2 3.65 3.69 -10 -1 1 50.62 6.63 10 1 -1 38.64 6.16 -10 -1 0 3.53 3.21 10 1 0 -1.86 3.34 -10 -1 -1 9.18 3.46 10 1 1 8.98 3.62 -10 -1 -2 9.89 3.51 10 1 2 14.11 3.67 10 1 3 2.63 2.49 10 2 -7 91.36 7.91 -10 -2 6 4.97 2.93 10 2 -6 7.81 3.05 10 2 -6 6.85 3.32 10 2 -5 49.74 5.54 -10 -2 5 38.59 5.27 -10 -2 5 56.84 6.54 10 2 -5 48.66 6.85 10 2 -4 -2.11 2.23 -10 -2 4 4.87 3.22 -10 -2 4 1.03 3.06 10 2 -4 4.11 3.34 10 2 -3 32.85 5.86 -10 -2 3 32.82 5.44 10 2 -3 34.66 4.74 -10 -2 2 0.08 3.62 10 2 -2 -1.90 3.27 -10 -2 1 1.83 3.07 10 2 -1 -5.95 3.14 -10 -2 0 45.96 6.14 10 2 0 45.88 5.94 -10 -2 -1 63.88 6.44 10 2 1 71.11 6.96 10 2 2 5.61 2.82 10 3 -7 188.02 10.02 10 3 -6 2.04 2.67 10 3 -6 1.12 2.22 10 3 -5 127.25 9.38 -10 -3 5 129.55 8.69 10 3 -5 129.53 8.48 10 3 -4 3.46 3.27 -10 -3 4 -2.61 3.08 10 3 -4 2.13 2.43 10 3 -3 3.89 3.45 -10 -3 3 2.45 2.84 10 3 -2 12.11 3.48 -10 -3 2 11.56 3.89 10 3 -1 106.61 8.00 -10 -3 1 128.50 9.22 10 3 0 9.20 3.08 -10 -3 0 11.97 3.35 -10 -4 3 45.76 5.38 -10 -4 2 14.71 3.32 0 0 0 0.00 0.00 TITL OCHDKI in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.487187 11.674078 16.835423 108.4045 96.2908 90.4050 ZERR 4.00 0.000312 0.000505 0.000603 0.0036 0.0031 0.0032 LATT 1 SFAC C H N O P UNIT 72.00 64.00 4.00 12.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 6557 _olex2_date_sample_data_collection 2020-12-14 _olex2_date_sample_submission 2020-12-03 _olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount' _olex2_submission_original_sample_id OCHDKI _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 1.184 _oxdiff_exptl_absorpt_empirical_full_min 0.837 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 0.44039(5) 0.32817(4) 0.85420(3) 0.01928(12) Uani 1 1 d . . . . . O1 O 0.38043(15) 0.40333(12) 0.93287(8) 0.0243(3) Uani 1 1 d . . . . . O2 O 0.70152(16) 0.33807(13) 0.77746(9) 0.0275(3) Uani 1 1 d . . . . . O3A O 0.9648(3) 0.6583(3) 1.03330(16) 0.0315(7) Uani 0.864(8) 1 d D U P A 1 N1 N 0.69092(18) 0.48802(14) 0.90174(10) 0.0206(3) Uani 1 1 d D . . . . H1 H 0.644(2) 0.5130(19) 0.9469(12) 0.025 Uiso 1 1 d D U . . . C1 C 0.3135(2) 0.32135(17) 0.76010(12) 0.0212(4) Uani 1 1 d . . . . . C2 C 0.1641(2) 0.36891(17) 0.77053(13) 0.0235(4) Uani 1 1 d . . . . . H2 H 0.133447 0.401910 0.825524 0.028 Uiso 1 1 calc R U . . . C3 C 0.0601(2) 0.36813(18) 0.70071(14) 0.0265(4) Uani 1 1 d . . . . . H3 H -0.042056 0.399771 0.707907 0.032 Uiso 1 1 calc R U . . . C4 C 0.1054(2) 0.32116(18) 0.62046(13) 0.0267(4) Uani 1 1 d . . . . . H4 H 0.034810 0.321839 0.572750 0.032 Uiso 1 1 calc R U . . . C5 C 0.2538(2) 0.27310(19) 0.60973(13) 0.0275(5) Uani 1 1 d . . . . . H5 H 0.284306 0.240977 0.554627 0.033 Uiso 1 1 calc R U . . . C6 C 0.3578(2) 0.27173(18) 0.67898(12) 0.0243(4) Uani 1 1 d . . . . . H6 H 0.458395 0.237354 0.671377 0.029 Uiso 1 1 calc R U . . . C7 C 0.4767(2) 0.17608(18) 0.85216(12) 0.0225(4) Uani 1 1 d . . . . . C8 C 0.3830(2) 0.07671(19) 0.80055(14) 0.0303(5) Uani 1 1 d . . . . . H8 H 0.302054 0.086054 0.759666 0.036 Uiso 1 1 calc R U . . . C9 C 0.4087(3) -0.0364(2) 0.80922(16) 0.0382(6) Uani 1 1 d . . . . . H9 H 0.344392 -0.104405 0.774246 0.046 Uiso 1 1 calc R U . . . C10 C 0.5255(3) -0.0509(2) 0.86755(17) 0.0427(6) Uani 1 1 d . . . . . H10 H 0.542387 -0.128794 0.872574 0.051 Uiso 1 1 calc R U . . . C11 C 0.6191(3) 0.0475(2) 0.91929(17) 0.0451(6) Uani 1 1 d . . . . . H11 H 0.699532 0.037538 0.960176 0.054 Uiso 1 1 calc R U . . . C12 C 0.5951(3) 0.1604(2) 0.91122(14) 0.0334(5) Uani 1 1 d . . . . . H12 H 0.660030 0.227845 0.946351 0.040 Uiso 1 1 calc R U . . . C13 C 0.6359(2) 0.38806(17) 0.84047(12) 0.0198(4) Uani 1 1 d . . . . . C14 C 0.8367(2) 0.55065(18) 0.89453(13) 0.0256(4) Uani 1 1 d . . . . . H14A H 0.825783 0.566843 0.839944 0.031 Uiso 1 1 calc R U . . . H14B H 0.926859 0.497396 0.894967 0.031 Uiso 1 1 calc R U . . . C15 C 0.8717(2) 0.66586(18) 0.96359(13) 0.0226(4) Uani 1 1 d D U . . . C16A C 0.9841(5) 0.7740(5) 1.0882(2) 0.0461(11) Uani 0.864(8) 1 d D U P A 1 H16A H 1.043061 0.796229 1.142510 0.055 Uiso 0.864(8) 1 calc R U P A 1 C17A C 0.9094(7) 0.8509(3) 1.0551(3) 0.0471(14) Uani 0.864(8) 1 d D U P A 1 H17A H 0.905032 0.935737 1.080661 0.057 Uiso 0.864(8) 1 calc R U P A 1 C18A C 0.8372(6) 0.7808(3) 0.9737(3) 0.0354(8) Uani 0.864(8) 1 d D U P A 1 H18A H 0.776038 0.810085 0.934084 0.043 Uiso 0.864(8) 1 calc R U P A 1 P2 P -0.00603(5) 0.32092(4) 0.36203(3) 0.01830(12) Uani 1 1 d . . . . . O4 O -0.07273(15) 0.37239(12) 0.44318(8) 0.0222(3) Uani 1 1 d . . . . . O5 O 0.24231(16) 0.36335(12) 0.28821(9) 0.0252(3) Uani 1 1 d . . . . . O6A O 0.4641(3) 0.6768(3) 0.54757(15) 0.0294(7) Uani 0.677(5) 1 d D U P B 1 N2 N 0.22342(19) 0.50190(14) 0.41595(11) 0.0210(3) Uani 1 1 d D . . . . H2A H 0.169(2) 0.5267(19) 0.4594(12) 0.025 Uiso 1 1 d D U . . . C19 C -0.1406(2) 0.32519(16) 0.27285(12) 0.0197(4) Uani 1 1 d . . . . . C20 C -0.2893(2) 0.37177(17) 0.28787(13) 0.0226(4) Uani 1 1 d . . . . . H20 H -0.316537 0.400132 0.343833 0.027 Uiso 1 1 calc R U . . . C21 C -0.3977(2) 0.37670(18) 0.22095(13) 0.0254(4) Uani 1 1 d . . . . . H21 H -0.499956 0.406608 0.231018 0.031 Uiso 1 1 calc R U . . . C22 C -0.3566(2) 0.33805(18) 0.13982(13) 0.0263(4) Uani 1 1 d . . . . . H22 H -0.430027 0.343062 0.094318 0.032 Uiso 1 1 calc R U . . . C23 C -0.2086(2) 0.29193(19) 0.12445(13) 0.0280(5) Uani 1 1 d . . . . . H23 H -0.181115 0.265482 0.068506 0.034 Uiso 1 1 calc R U . . . C24 C -0.1009(2) 0.28439(18) 0.19058(13) 0.0240(4) Uani 1 1 d . . . . . H24 H -0.000384 0.251535 0.179895 0.029 Uiso 1 1 calc R U . . . C25 C 0.0493(2) 0.16657(17) 0.34406(12) 0.0211(4) Uani 1 1 d . . . . . C26 C -0.0170(3) 0.10489(18) 0.39180(13) 0.0280(5) Uani 1 1 d . . . . . H26 H -0.084424 0.145104 0.432447 0.034 Uiso 1 1 calc R U . . . C27 C 0.0153(3) -0.0151(2) 0.37998(15) 0.0364(5) Uani 1 1 d . . . . . H27 H -0.032093 -0.057428 0.411728 0.044 Uiso 1 1 calc R U . . . C28 C 0.1158(3) -0.07366(19) 0.32249(14) 0.0322(5) Uani 1 1 d . . . . . H28 H 0.138794 -0.155594 0.315324 0.039 Uiso 1 1 calc R U . . . C29 C 0.1828(3) -0.01277(19) 0.27541(14) 0.0322(5) Uani 1 1 d . . . . . H29 H 0.252670 -0.052860 0.236139 0.039 Uiso 1 1 calc R U . . . C30 C 0.1486(2) 0.10672(19) 0.28507(14) 0.0291(5) Uani 1 1 d . . . . . H30 H 0.192982 0.147543 0.251488 0.035 Uiso 1 1 calc R U . . . C31 C 0.1762(2) 0.40233(17) 0.35251(12) 0.0193(4) Uani 1 1 d . . . . . C32 C 0.3610(3) 0.5727(2) 0.40819(16) 0.0343(5) Uani 1 1 d . . . . . H32A H 0.345257 0.586951 0.352974 0.041 Uiso 1 1 calc R U . . . H32B H 0.456734 0.524967 0.409057 0.041 Uiso 1 1 calc R U . . . C33 C 0.3890(2) 0.69013(18) 0.47533(13) 0.0231(4) Uani 1 1 d D U . . . C34A C 0.4903(4) 0.7920(4) 0.6025(3) 0.0379(10) Uani 0.677(5) 1 d D U P B 1 H34A H 0.541537 0.811337 0.658431 0.045 Uiso 0.677(5) 1 calc R U P B 1 C35A C 0.434(2) 0.8738(7) 0.5671(8) 0.036(2) Uani 0.677(5) 1 d D U P B 1 H35A H 0.435(5) 0.961(4) 0.595(3) 0.043 Uiso 0.677(5) 1 d . U P B 1 C36A C 0.3686(5) 0.8060(4) 0.4829(3) 0.0300(9) Uani 0.677(5) 1 d D U P B 1 H36A H 0.320198 0.837353 0.441002 0.036 Uiso 0.677(5) 1 calc R U P B 1 O3B O 0.771(2) 0.7573(13) 0.9635(9) 0.030(4) Uani 0.136(8) 1 d D U P A 2 O6B O 0.3168(8) 0.7791(5) 0.4483(4) 0.0327(16) Uani 0.323(5) 1 d D U P B 2 C16B C 0.819(3) 0.8523(13) 1.0342(9) 0.026(4) Uani 0.136(8) 1 d D U P A 2 H16B H 0.769395 0.927619 1.049667 0.031 Uiso 0.136(8) 1 calc R U P A 2 C17B C 0.943(3) 0.8256(19) 1.0781(12) 0.024(5) Uani 0.136(8) 1 d D U P A 2 H17B H 0.999281 0.877489 1.128686 0.029 Uiso 0.136(8) 1 calc R U P A 2 C18B C 0.976(3) 0.7040(19) 1.0352(13) 0.028(5) Uani 0.136(8) 1 d D U P A 2 H18B H 1.055775 0.657950 1.053099 0.033 Uiso 0.136(8) 1 calc R U P A 2 C34B C 0.3601(9) 0.8897(7) 0.5081(5) 0.038(2) Uani 0.323(5) 1 d D U P B 2 H34B H 0.325353 0.965379 0.504775 0.046 Uiso 0.323(5) 1 calc R U P B 2 C35B C 0.458(4) 0.8743(17) 0.5710(18) 0.041(6) Uani 0.323(5) 1 d D U P B 2 H35B H 0.507211 0.936137 0.619023 0.049 Uiso 0.323(5) 1 calc R U P B 2 C36B C 0.4747(8) 0.7478(10) 0.5529(6) 0.0322(18) Uani 0.323(5) 1 d D U P B 2 H36B H 0.534094 0.709547 0.587785 0.039 Uiso 0.323(5) 1 calc R U P B 2 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 0.0197(2) 0.0214(2) 0.0152(2) 0.00328(19) 0.00359(18) -0.00129(18) O1 0.0242(7) 0.0284(7) 0.0178(7) 0.0024(6) 0.0067(5) -0.0016(6) O2 0.0254(7) 0.0309(8) 0.0222(7) 0.0014(6) 0.0078(6) -0.0022(6) O3A 0.0307(10) 0.0382(16) 0.0247(10) 0.0112(11) -0.0037(8) -0.0087(11) N1 0.0198(8) 0.0233(8) 0.0181(8) 0.0044(7) 0.0059(6) -0.0001(6) C1 0.0223(9) 0.0203(9) 0.0206(10) 0.0057(8) 0.0040(8) -0.0016(7) C2 0.0239(10) 0.0233(10) 0.0245(10) 0.0079(8) 0.0069(8) 0.0011(8) C3 0.0236(10) 0.0253(10) 0.0328(12) 0.0126(9) 0.0031(9) 0.0026(8) C4 0.0279(10) 0.0282(10) 0.0251(11) 0.0119(9) -0.0022(8) -0.0029(8) C5 0.0299(10) 0.0337(11) 0.0173(10) 0.0061(9) 0.0034(8) -0.0032(9) C6 0.0225(10) 0.0287(10) 0.0204(10) 0.0058(8) 0.0040(8) 0.0016(8) C7 0.0235(9) 0.0242(10) 0.0208(10) 0.0079(8) 0.0046(8) -0.0019(8) C8 0.0265(10) 0.0284(11) 0.0323(12) 0.0051(9) 0.0012(9) -0.0031(8) C9 0.0384(12) 0.0239(11) 0.0480(15) 0.0072(10) 0.0001(11) -0.0074(9) C10 0.0529(15) 0.0305(12) 0.0505(16) 0.0226(11) 0.0022(12) -0.0031(11) C11 0.0568(16) 0.0383(13) 0.0420(15) 0.0217(12) -0.0133(12) -0.0022(12) C12 0.0407(12) 0.0311(11) 0.0266(11) 0.0102(9) -0.0060(10) -0.0056(9) C13 0.0200(9) 0.0217(9) 0.0185(10) 0.0071(8) 0.0037(7) 0.0021(7) C14 0.0239(10) 0.0263(10) 0.0251(11) 0.0047(8) 0.0073(8) -0.0038(8) C15 0.0200(9) 0.0270(10) 0.0214(10) 0.0086(8) 0.0031(8) -0.0025(7) C16A 0.047(2) 0.054(3) 0.0275(17) 0.0003(17) 0.0015(14) -0.0263(18) C17A 0.052(4) 0.0312(18) 0.047(3) -0.0077(17) 0.018(2) -0.0119(19) C18A 0.0333(19) 0.0292(16) 0.043(2) 0.0093(15) 0.0086(17) 0.0019(14) P2 0.0194(2) 0.0192(2) 0.0164(2) 0.00490(18) 0.00451(18) 0.00082(17) O4 0.0256(7) 0.0226(7) 0.0181(7) 0.0045(5) 0.0073(5) 0.0008(5) O5 0.0247(7) 0.0291(7) 0.0210(7) 0.0051(6) 0.0085(6) -0.0003(6) O6A 0.0310(12) 0.0320(16) 0.0231(13) 0.0077(12) -0.0021(9) -0.0056(11) N2 0.0208(8) 0.0207(8) 0.0208(8) 0.0037(7) 0.0078(6) -0.0017(6) C19 0.0215(9) 0.0171(9) 0.0205(10) 0.0057(7) 0.0032(7) -0.0011(7) C20 0.0241(10) 0.0209(9) 0.0242(10) 0.0076(8) 0.0077(8) 0.0011(7) C21 0.0209(9) 0.0249(10) 0.0320(12) 0.0109(9) 0.0042(8) 0.0016(8) C22 0.0234(10) 0.0302(11) 0.0252(11) 0.0104(9) -0.0025(8) -0.0012(8) C23 0.0270(10) 0.0356(11) 0.0204(10) 0.0074(9) 0.0026(8) -0.0013(9) C24 0.0201(9) 0.0293(10) 0.0223(10) 0.0071(8) 0.0043(8) 0.0017(8) C25 0.0215(9) 0.0210(9) 0.0197(10) 0.0057(8) 0.0010(7) 0.0003(7) C26 0.0327(11) 0.0260(10) 0.0258(11) 0.0078(9) 0.0069(9) 0.0011(8) C27 0.0502(14) 0.0262(11) 0.0361(13) 0.0148(10) 0.0048(11) -0.0022(10) C28 0.0396(12) 0.0198(10) 0.0328(12) 0.0047(9) -0.0038(10) 0.0026(9) C29 0.0327(11) 0.0265(11) 0.0329(12) 0.0029(9) 0.0045(9) 0.0052(9) C30 0.0314(11) 0.0269(11) 0.0298(11) 0.0081(9) 0.0090(9) 0.0032(8) C31 0.0184(9) 0.0209(9) 0.0209(10) 0.0092(8) 0.0044(7) 0.0034(7) C32 0.0295(11) 0.0295(11) 0.0416(13) 0.0040(10) 0.0170(10) -0.0060(9) C33 0.0202(9) 0.0287(10) 0.0210(10) 0.0081(8) 0.0047(8) -0.0020(8) C34A 0.037(2) 0.040(2) 0.027(2) -0.0019(18) -0.0003(16) -0.0139(16) C35A 0.036(5) 0.029(3) 0.035(4) -0.002(3) 0.011(3) -0.007(2) C36A 0.026(2) 0.032(2) 0.033(2) 0.011(2) 0.0063(17) -0.0006(17) O3B 0.031(8) 0.028(6) 0.021(6) -0.002(5) -0.004(6) -0.003(5) O6B 0.035(4) 0.023(3) 0.035(4) 0.004(3) 0.000(3) -0.003(2) C16B 0.032(10) 0.030(7) 0.010(6) 0.001(5) -0.008(7) 0.005(6) C17B 0.030(9) 0.028(9) 0.016(8) 0.011(6) -0.010(6) 0.007(7) C18B 0.029(8) 0.025(9) 0.031(8) 0.015(7) -0.006(6) -0.003(7) C34B 0.041(4) 0.023(4) 0.045(5) 0.003(3) 0.010(4) 0.002(3) C35B 0.035(9) 0.040(6) 0.035(7) -0.006(5) -0.001(6) -0.009(5) C36B 0.023(3) 0.042(5) 0.025(4) 0.004(4) -0.004(3) -0.004(3) 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' 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 7 -2 0.0265 -1 7 2 0.0180 5 3 -5 0.1058 0 3 -11 0.1102 5 0 5 0.0788 4 -1 6 0.0733 0 -7 -1 0.0100 1 7 -1 0.0265 1 7 1 0.0183 -1 -7 0 0.0068 -3 3 -8 0.0880 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 113.77(9) . . ? O1 P1 C7 113.53(9) . . ? O1 P1 C13 111.82(8) . . ? C1 P1 C13 105.01(9) . . ? C7 P1 C1 107.89(9) . . ? C7 P1 C13 104.04(9) . . ? C15 O3A C16A 105.8(3) . . ? C13 N1 H1 119.7(15) . . ? C13 N1 C14 119.63(16) . . ? C14 N1 H1 120.6(15) . . ? C2 C1 P1 116.83(15) . . ? C2 C1 C6 119.82(18) . . ? C6 C1 P1 123.35(15) . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.13(19) . . ? C3 C2 H2 119.9 . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 119.99(19) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 120.0 . . ? C3 C4 C5 120.07(19) . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 119.8 . . ? C6 C5 C4 120.43(19) . . ? C6 C5 H5 119.8 . . ? C1 C6 H6 120.2 . . ? C5 C6 C1 119.53(18) . . ? C5 C6 H6 120.2 . . ? C8 C7 P1 123.13(16) . . ? C12 C7 P1 117.21(15) . . ? C12 C7 C8 119.36(19) . . ? C7 C8 H8 120.3 . . ? C9 C8 C7 119.5(2) . . ? C9 C8 H8 120.3 . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.7(2) . . ? C10 C9 H9 119.7 . . ? C9 C10 H10 119.9 . . ? C9 C10 C11 120.2(2) . . ? C11 C10 H10 119.9 . . ? C10 C11 H11 120.2 . . ? C12 C11 C10 119.7(2) . . ? C12 C11 H11 120.2 . . ? C7 C12 H12 119.7 . . ? C11 C12 C7 120.6(2) . . ? C11 C12 H12 119.7 . . ? O2 C13 P1 120.48(14) . . ? O2 C13 N1 125.22(18) . . ? N1 C13 P1 114.26(14) . . ? N1 C14 H14A 109.1 . . ? N1 C14 H14B 109.1 . . ? N1 C14 C15 112.39(17) . . ? H14A C14 H14B 107.9 . . ? C15 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? O3A C15 C14 115.5(2) . . ? C18A C15 O3A 110.0(2) . . ? C18A C15 C14 134.5(3) . . ? O3B C15 C14 116.5(6) . . ? C18B C15 C14 135.2(9) . . ? C18B C15 O3B 108.1(10) . . ? O3A C16A H16A 124.6 . . ? C17A C16A O3A 110.9(3) . . ? C17A C16A H16A 124.6 . . ? C16A C17A H17A 126.9 . . ? C16A C17A C18A 106.3(3) . . ? C18A C17A H17A 126.9 . . ? C15 C18A C17A 107.0(3) . . ? C15 C18A H18A 126.5 . . ? C17A C18A H18A 126.5 . . ? O4 P2 C19 112.66(8) . . ? O4 P2 C25 112.50(9) . . ? O4 P2 C31 114.58(8) . . ? C19 P2 C25 107.89(9) . . ? C19 P2 C31 103.58(9) . . ? C25 P2 C31 104.89(9) . . ? C33 O6A C34A 105.1(3) . . ? C31 N2 H2A 120.4(15) . . ? C31 N2 C32 118.00(17) . . ? C32 N2 H2A 121.4(15) . . ? C20 C19 P2 117.85(15) . . ? C20 C19 C24 119.73(18) . . ? C24 C19 P2 122.43(14) . . ? C19 C20 H20 120.0 . . ? C21 C20 C19 120.02(19) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 C20 119.93(19) . . ? C22 C21 H21 120.0 . . ? C21 C22 H22 119.8 . . ? C21 C22 C23 120.34(19) . . ? C23 C22 H22 119.8 . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.1(2) . . ? C24 C23 H23 119.9 . . ? C19 C24 H24 120.1 . . ? C23 C24 C19 119.83(18) . . ? C23 C24 H24 120.1 . . ? C26 C25 P2 116.28(15) . . ? C30 C25 P2 124.29(16) . . ? C30 C25 C26 119.41(18) . . ? C25 C26 H26 120.0 . . ? C27 C26 C25 120.0(2) . . ? C27 C26 H26 120.0 . . ? C26 C27 H27 119.7 . . ? C28 C27 C26 120.5(2) . . ? C28 C27 H27 119.7 . . ? C27 C28 H28 120.1 . . ? C27 C28 C29 119.8(2) . . ? C29 C28 H28 120.1 . . ? C28 C29 H29 119.8 . . ? C28 C29 C30 120.4(2) . . ? C30 C29 H29 119.8 . . ? C25 C30 H30 120.1 . . ? C29 C30 C25 119.9(2) . . ? C29 C30 H30 120.1 . . ? O5 C31 P2 118.85(14) . . ? O5 C31 N2 124.62(18) . . ? N2 C31 P2 116.50(14) . . ? N2 C32 H32A 108.8 . . ? N2 C32 H32B 108.8 . . ? N2 C32 C33 113.74(18) . . ? H32A C32 H32B 107.7 . . ? C33 C32 H32A 108.8 . . ? C33 C32 H32B 108.8 . . ? O6A C33 C32 111.2(2) . . ? C36A C33 O6A 111.7(3) . . ? C36A C33 C32 137.0(3) . . ? O6B C33 C32 109.6(3) . . ? O6B C33 C36B 106.8(5) . . ? C36B C33 C32 143.2(5) . . ? O6A C34A H34A 124.3 . . ? C35A C34A O6A 111.3(5) . . ? C35A C34A H34A 124.3 . . ? C34A C35A H35A 126(3) . . ? C34A C35A C36A 105.8(6) . . ? C36A C35A H35A 129(3) . . ? C33 C36A C35A 106.2(6) . . ? C33 C36A H36A 126.9 . . ? C35A C36A H36A 126.9 . . ? C16B O3B C15 107.0(10) . . ? C33 O6B C34B 108.4(6) . . ? O3B C16B H16B 124.5 . . ? C17B C16B O3B 110.9(14) . . ? C17B C16B H16B 124.5 . . ? C16B C17B H17B 126.7 . . ? C16B C17B C18B 106.7(14) . . ? C18B C17B H17B 126.7 . . ? C15 C18B C17B 107.2(13) . . ? C15 C18B H18B 126.4 . . ? C17B C18B H18B 126.4 . . ? O6B C34B H34B 125.1 . . ? C35B C34B O6B 109.8(9) . . ? C35B C34B H34B 125.1 . . ? C34B C35B H35B 126.5 . . ? C34B C35B C36B 107.1(12) . . ? C36B C35B H35B 126.5 . . ? C33 C36B C35B 107.9(11) . . ? C33 C36B H36B 126.1 . . ? C35B C36B H36B 126.1 . . ? 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 1.4843(14) . ? P1 C1 1.795(2) . ? P1 C7 1.795(2) . ? P1 C13 1.862(2) . ? O2 C13 1.232(2) . ? O3A C15 1.368(3) . ? O3A C16A 1.371(4) . ? N1 H1 0.868(16) . ? N1 C13 1.331(2) . ? N1 C14 1.469(2) . ? C1 C2 1.394(3) . ? C1 C6 1.399(3) . ? C2 H2 0.9500 . ? C2 C3 1.388(3) . ? C3 H3 0.9500 . ? C3 C4 1.387(3) . ? C4 H4 0.9500 . ? C4 C5 1.389(3) . ? C5 H5 0.9500 . ? C5 C6 1.387(3) . ? C6 H6 0.9500 . ? C7 C8 1.390(3) . ? C7 C12 1.389(3) . ? C8 H8 0.9500 . ? C8 C9 1.390(3) . ? C9 H9 0.9500 . ? C9 C10 1.367(4) . ? C10 H10 0.9500 . ? C10 C11 1.383(4) . ? C11 H11 0.9500 . ? C11 C12 1.380(3) . ? C12 H12 0.9500 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.477(3) . ? C15 C18A 1.337(4) . ? C15 O3B 1.372(12) . ? C15 C18B 1.362(17) . ? C16A H16A 0.9500 . ? C16A C17A 1.328(6) . ? C17A H17A 0.9500 . ? C17A C18A 1.422(5) . ? C18A H18A 0.9500 . ? P2 O4 1.4845(14) . ? P2 C19 1.7982(19) . ? P2 C25 1.8051(19) . ? P2 C31 1.8577(19) . ? O5 C31 1.233(2) . ? O6A C33 1.364(3) . ? O6A C34A 1.370(4) . ? N2 H2A 0.879(16) . ? N2 C31 1.330(2) . ? N2 C32 1.467(3) . ? C19 C20 1.395(3) . ? C19 C24 1.395(3) . ? C20 H20 0.9500 . ? C20 C21 1.391(3) . ? C21 H21 0.9500 . ? C21 C22 1.381(3) . ? C22 H22 0.9500 . ? C22 C23 1.388(3) . ? C23 H23 0.9500 . ? C23 C24 1.387(3) . ? C24 H24 0.9500 . ? C25 C26 1.393(3) . ? C25 C30 1.392(3) . ? C26 H26 0.9500 . ? C26 C27 1.385(3) . ? C27 H27 0.9500 . ? C27 C28 1.379(3) . ? C28 H28 0.9500 . ? C28 C29 1.381(3) . ? C29 H29 0.9500 . ? C29 C30 1.389(3) . ? C30 H30 0.9500 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.473(3) . ? C33 C36A 1.332(5) . ? C33 O6B 1.381(6) . ? C33 C36B 1.384(9) . ? C34A H34A 0.9500 . ? C34A C35A 1.340(14) . ? C35A H35A 0.98(4) . ? C35A C36A 1.435(11) . ? C36A H36A 0.9500 . ? O3B C16B 1.367(14) . ? O6B C34B 1.381(8) . ? C16B H16B 0.9500 . ? C16B C17B 1.314(17) . ? C17B H17B 0.9500 . ? C17B C18B 1.420(17) . ? C18B H18B 0.9500 . ? C34B H34B 0.9500 . ? C34B C35B 1.33(3) . ? C35B H35B 0.9500 . ? C35B C36B 1.422(19) . ? C36B H36B 0.9500 . ? 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 0.868(16) 1.984(17) 2.807(2) 158(2) 2_667 yes N2 H2A O4 0.879(16) 1.959(17) 2.812(2) 163(2) 2_566 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 179.25(15) . . . . ? P1 C1 C6 C5 -178.27(15) . . . . ? P1 C7 C8 C9 -173.13(18) . . . . ? P1 C7 C12 C11 173.4(2) . . . . ? O1 P1 C1 C2 -10.06(18) . . . . ? O1 P1 C1 C6 169.80(16) . . . . ? O1 P1 C7 C8 109.17(19) . . . . ? O1 P1 C7 C12 -64.45(19) . . . . ? O1 P1 C13 O2 -178.43(15) . . . . ? O1 P1 C13 N1 -0.55(17) . . . . ? O3A C15 C18A C17A -1.2(4) . . . . ? O3A C16A C17A C18A -0.1(5) . . . . ? N1 C14 C15 O3A 90.5(2) . . . . ? N1 C14 C15 C18A -92.2(4) . . . . ? N1 C14 C15 O3B -69.2(9) . . . . ? N1 C14 C15 C18B 103.8(16) . . . . ? C1 P1 C7 C8 -17.9(2) . . . . ? C1 P1 C7 C12 168.51(17) . . . . ? C1 P1 C13 O2 -54.59(18) . . . . ? C1 P1 C13 N1 123.28(15) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? C2 C1 C6 C5 1.6(3) . . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C4 C5 C6 C1 -1.3(3) . . . . ? C6 C1 C2 C3 -0.6(3) . . . . ? C7 P1 C1 C2 116.84(16) . . . . ? C7 P1 C1 C6 -63.30(19) . . . . ? C7 P1 C13 O2 58.66(18) . . . . ? C7 P1 C13 N1 -123.46(15) . . . . ? C7 C8 C9 C10 -0.4(4) . . . . ? C8 C7 C12 C11 -0.5(4) . . . . ? C8 C9 C10 C11 0.5(4) . . . . ? C9 C10 C11 C12 -0.6(4) . . . . ? C10 C11 C12 C7 0.6(4) . . . . ? C12 C7 C8 C9 0.4(3) . . . . ? C13 P1 C1 C2 -132.65(15) . . . . ? C13 P1 C1 C6 47.22(19) . . . . ? C13 P1 C7 C8 -129.05(18) . . . . ? C13 P1 C7 C12 57.33(19) . . . . ? C13 N1 C14 C15 174.30(18) . . . . ? C14 N1 C13 P1 -174.38(14) . . . . ? C14 N1 C13 O2 3.4(3) . . . . ? C14 C15 C18A C17A -178.6(3) . . . . ? C14 C15 O3B C16B 176.8(8) . . . . ? C14 C15 C18B C17B -176.6(12) . . . . ? C15 O3A C16A C17A -0.6(4) . . . . ? C15 O3B C16B C17B 0.1(17) . . . . ? C16A O3A C15 C14 179.1(2) . . . . ? C16A O3A C15 C18A 1.1(3) . . . . ? C16A C17A C18A C15 0.7(5) . . . . ? P2 C19 C20 C21 -179.83(15) . . . . ? P2 C19 C24 C23 -178.86(15) . . . . ? P2 C25 C26 C27 177.96(17) . . . . ? P2 C25 C30 C29 -179.31(16) . . . . ? O4 P2 C19 C20 -1.43(18) . . . . ? O4 P2 C19 C24 178.32(15) . . . . ? O4 P2 C25 C26 18.29(18) . . . . ? O4 P2 C25 C30 -163.46(16) . . . . ? O4 P2 C31 O5 177.72(14) . . . . ? O4 P2 C31 N2 -4.07(18) . . . . ? O6A C33 C36A C35A -0.5(9) . . . . ? O6A C34A C35A C36A -0.6(13) . . . . ? N2 C32 C33 O6A 79.6(2) . . . . ? N2 C32 C33 C36A -105.1(4) . . . . ? N2 C32 C33 O6B -94.5(3) . . . . ? N2 C32 C33 C36B 95.2(7) . . . . ? C19 P2 C25 C26 -106.59(16) . . . . ? C19 P2 C25 C30 71.65(19) . . . . ? C19 P2 C31 O5 -59.17(17) . . . . ? C19 P2 C31 N2 119.04(15) . . . . ? C19 C20 C21 C22 -1.5(3) . . . . ? C20 C19 C24 C23 0.9(3) . . . . ? C20 C21 C22 C23 1.3(3) . . . . ? C21 C22 C23 C24 0.0(3) . . . . ? C22 C23 C24 C19 -1.1(3) . . . . ? C24 C19 C20 C21 0.4(3) . . . . ? C25 P2 C19 C20 123.36(15) . . . . ? C25 P2 C19 C24 -56.89(18) . . . . ? C25 P2 C31 O5 53.86(17) . . . . ? C25 P2 C31 N2 -127.93(15) . . . . ? C25 C26 C27 C28 1.4(3) . . . . ? C26 C25 C30 C29 -1.1(3) . . . . ? C26 C27 C28 C29 -1.0(3) . . . . ? C27 C28 C29 C30 -0.5(3) . . . . ? C28 C29 C30 C25 1.6(3) . . . . ? C30 C25 C26 C27 -0.4(3) . . . . ? C31 P2 C19 C20 -125.80(15) . . . . ? C31 P2 C19 C24 53.95(18) . . . . ? C31 P2 C25 C26 143.47(15) . . . . ? C31 P2 C25 C30 -38.29(19) . . . . ? C31 N2 C32 C33 171.23(18) . . . . ? C32 N2 C31 P2 -176.20(15) . . . . ? C32 N2 C31 O5 1.9(3) . . . . ? C32 C33 C36A C35A -175.8(8) . . . . ? C32 C33 O6B C34B -173.1(4) . . . . ? C32 C33 C36B C35B 168.3(18) . . . . ? C33 O6A C34A C35A 0.2(9) . . . . ? C33 O6B C34B C35B 0.8(19) . . . . ? C34A O6A C33 C32 176.8(2) . . . . ? C34A O6A C33 C36A 0.2(3) . . . . ? C34A C35A C36A C33 0.7(13) . . . . ? O3B C15 C18B C17B -3(2) . . . . ? O3B C16B C17B C18B -2(2) . . . . ? O6B C33 C36B C35B -2.2(19) . . . . ? O6B C34B C35B C36B -2(3) . . . . ? C16B C17B C18B C15 3(3) . . . . ? C18B C15 O3B C16B 2.0(14) . . . . ? C34B C35B C36B C33 3(3) . . . . ? C36B C33 O6B C34B 0.9(6) . . . . ? 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 0.1107 7.4825 -1.8362 -0.5290 0.7670 0.3631 -0.8067 6.5883 2.0497 -0.5673 0.8235 -0.0089 4.9201 2.7113 -5.0500 -0.5765 -0.3158 0.7536 -0.3961 3.1272 -10.6918 0.4385 0.2364 0.8671 4.6513 -0.2620 4.5983 -0.8762 -0.4767 -0.0711 4.4156 -1.3649 5.5333 -0.8092 -0.5569 -0.1875 -0.1386 -7.0418 -0.5447 0.6400 -0.7484 -0.1739 1.0835 7.2110 -1.1593 -0.6769 0.6402 0.3632 0.6867 6.8995 0.7368 -0.7128 0.6756 0.1884 -0.8292 -7.0389 -0.0568 0.7023 -0.6659 -0.2519 -3.2089 2.9820 -7.9962 0.6623 0.5653 0.4917