#------------------------------------------------------------------------------ #$Date: 2019-11-10 19:05:48 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225985 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/59/4515905.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_4515905 loop_ _publ_author_name 'Hu, Xing-Mei' 'Luo, Da-Yun' 'Zi, Quan-Xing' 'Lin, Jun' 'Yan, Sheng-Jiao' _publ_section_title ; Diastereoselective Synthesis of Morphan Derivatives by Michael and Hetero-Michael Addition of 1,1-Enediamines to Quinone Monoketals. ; _journal_issue 1 _journal_name_full 'ACS omega' _journal_page_first 8 _journal_page_last 21 _journal_paper_doi 10.1021/acsomega.7b01493 _journal_volume 3 _journal_year 2018 _chemical_formula_moiety 'C19 H25 N3 O5' _chemical_formula_sum 'C19 H25 N3 O5' _chemical_formula_weight 375.42 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2017-09-28 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 96.021(2) _cell_angle_gamma 90 _cell_formula_units_Z 16 _cell_length_a 21.969(4) _cell_length_b 17.259(3) _cell_length_c 20.669(3) _cell_measurement_reflns_used 3667 _cell_measurement_temperature 297 _cell_measurement_theta_max 20.129 _cell_measurement_theta_min 2.409 _cell_volume 7794(2) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 297.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_unetI/netI 0.0882 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 28452 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.681 _diffrn_reflns_theta_min 2.360 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 100 _diffrn_standards_number 1 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.0806 before and 0.0609 after correction. The Ratio of minimum to maximum transmission is 0.6906. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.280 _exptl_crystal_description block _exptl_crystal_F_000 3200 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.308 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.038 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 566 _refine_ls_number_reflns 7389 _refine_ls_number_restraints 231 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.1522 _refine_ls_R_factor_gt 0.0643 _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^)+(0.0727P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1321 _refine_ls_wR_factor_ref 0.1639 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3590 _reflns_number_total 7389 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao7b01493_si_005.cif _cod_data_source_block hxm2bf_0m _cod_database_code 4515905 _shelx_shelxl_version_number 2016/6 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C38A-C34A 1.4 with sigma of 0.02 C38-C34 1.4 with sigma of 0.02 C34-C33 = C32-C31 = C36-C35 1.4 with sigma of 0.02 C34-C35 = C36-C31 = C32-C33 1.4 with sigma of 0.02 C34A-C33A = C32A-C31A = C36A-C35A 1.4 with sigma of 0.02 C34A-C35A = C36A-C31A = C32A-C33A 1.4 with sigma of 0.02 H5-H37A 2.3 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains N6, C31, C31A, C32, C32A, C33, C33A, C34, C34A, C35, C35A, C36, C36A, C37, C37A, C38, C38A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(H6B)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)= Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(H37C)= Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=1-FVAR(1) Sof(H6A)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)= Sof(C35)=Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)= Sof(H38A)=Sof(H38B)=FVAR(1) 6.a Ternary CH refined with riding coordinates: C3(H3A), C7(H7), C10(H10), C22(H22), C26(H26), C29(H29) 6.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C27(H27A,H27B), C37(H37A,H37B), C37A(H37C,H37D), C38(H38A,H38B), C38A(H38C,H38D) 6.c Aromatic/amide H refined with riding coordinates: N2(H2), N3(H3), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), N5(H5), N6(H6A), N6(H6B), C31(H31), C31A(H31A), C32(H32), C32A(H32A), C33(H33), C33A(H33A), C35(H35), C35A(H35A), C36(H36), C36A(H36A) 6.d Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6C,H6D,H6E), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C) ; _shelx_res_file ; TITL hxm2bf_0m C 1 2/c 1 R = 0.13 hxm2bf_0m.res created by SHELXL-2016/6 at 18:16:43 on 28-Sep-2017 CELL 0.71073 21.969 17.259 20.669 90 96.021 90 ZERR 16 0.004 0.003 0.003 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C 2.310 20.844 1.02 10.208 1.589 0.569 0.865 51.651 0.216 0.003 0.002 = 11.5 0.68 12.01 SFAC H SFAC N 12.213 0.006 3.132 9.893 2.013 28.998 1.166 0.583 -11.529 0.006 = 0.003 19.6 0.68 14.01 SFAC O 3.049 13.277 2.287 5.701 1.546 0.324 0.867 32.909 0.251 0.011 0.006 = 32.5 0.68 16 UNIT 304 400 48 80 DFIX 1.4 C38A C34A DFIX 1.4 C38 C34 DFIX 1.4 C34 C33 C32 C31 C36 C35 DFIX 1.4 C34 C35 C36 C31 C32 C33 DFIX 1.4 C34A C33A C32A C31A C36A C35A DFIX 1.4 C34A C35A C36A C31A C32A C33A DFIX 2.3 H5 H37a RIGU N6 C31 > C38A ISOR 0.01 0.02 C31 C32 C33 C34 C35 C36 C37 C38 C38A C37A C34A C33A C32A = C31A C36A C35A N6 L.S. 5 PLAN -20 TEMP 24 CONF bond $h fmap 2 acta SHEL 999 0.82 OMIT 1 1 1 OMIT 1 1 0 OMIT 0 0 2 OMIT -1 1 1 OMIT 0 2 1 OMIT 1 1 2 REM REM REM WGHT 0.072700 FVAR 0.20057 0.49946 O1 4 0.116987 0.751179 0.503989 11.00000 0.10220 0.08166 = 0.08862 0.00775 0.04518 0.05674 O2 4 0.070484 0.745583 0.404682 11.00000 0.08410 0.11855 = 0.10317 0.03905 0.03256 0.07652 O3 4 0.250068 0.691924 0.346351 11.00000 0.07204 0.04650 = 0.08150 0.01118 0.03646 0.01795 O4 4 0.213445 0.593815 0.276210 11.00000 0.08539 0.07172 = 0.04817 0.01115 0.01300 0.02826 O5 4 0.093366 0.479475 0.415477 11.00000 0.05759 0.11501 = 0.14869 0.02227 0.02604 -0.01232 N1 3 0.114578 0.724619 0.446030 11.00000 0.07252 0.06595 = 0.08822 0.02525 0.03363 0.04274 N2 3 0.239487 0.588363 0.450530 11.00000 0.04021 0.04295 = 0.05190 0.00478 0.01229 0.01891 AFIX 43 H2 2 0.267144 0.568180 0.477956 11.00000 -1.20000 AFIX 0 N3 3 0.213278 0.667100 0.532602 11.00000 0.05975 0.03628 = 0.06095 0.00123 0.02555 0.01500 AFIX 43 H3 2 0.193720 0.707659 0.542944 11.00000 -1.20000 AFIX 0 C1 1 0.157234 0.675326 0.426460 11.00000 0.05288 0.05085 = 0.06452 0.01613 0.02665 0.03069 C2 1 0.204256 0.644154 0.471732 11.00000 0.04323 0.03597 = 0.05751 0.00942 0.02577 0.01547 C3 1 0.233992 0.559937 0.384543 11.00000 0.03973 0.04646 = 0.05335 0.00261 0.01622 0.01362 AFIX 13 H3A 2 0.274656 0.543349 0.374629 11.00000 -1.20000 AFIX 0 C4 1 0.213212 0.625205 0.338801 11.00000 0.06011 0.05386 = 0.05102 0.00980 0.01979 0.01779 C5 1 0.313656 0.681404 0.341208 11.00000 0.07868 0.06570 = 0.10950 -0.00543 0.04849 -0.00104 AFIX 137 H5A 2 0.318977 0.655327 0.301163 11.00000 -1.50000 H5B 2 0.331357 0.650805 0.377157 11.00000 -1.50000 H5C 2 0.333512 0.730988 0.341836 11.00000 -1.50000 AFIX 0 C6 1 0.194537 0.643359 0.222215 11.00000 0.15038 0.11162 = 0.05920 0.02622 0.02175 0.04646 AFIX 137 H6C 2 0.203914 0.619141 0.182640 11.00000 -1.50000 H6D 2 0.215784 0.691915 0.227582 11.00000 -1.50000 H6E 2 0.151243 0.652225 0.220239 11.00000 -1.50000 AFIX 0 C7 1 0.150403 0.651328 0.356474 11.00000 0.05848 0.06758 = 0.06951 0.01908 0.01527 0.03046 AFIX 13 H7 2 0.136627 0.695916 0.329446 11.00000 -1.20000 AFIX 0 C8 1 0.103917 0.584755 0.343573 11.00000 0.05104 0.10996 = 0.09132 0.00620 0.00279 0.02835 AFIX 23 H8A 2 0.064444 0.600894 0.355902 11.00000 -1.20000 H8B 2 0.099051 0.572520 0.297516 11.00000 -1.20000 AFIX 0 C9 1 0.125189 0.514503 0.381489 11.00000 0.04779 0.08161 = 0.07996 -0.00211 0.00257 0.00084 C10 1 0.190263 0.489767 0.374284 11.00000 0.05612 0.05235 = 0.05979 0.00068 0.01160 0.00909 AFIX 13 H10 2 0.190987 0.473320 0.328990 11.00000 -1.20000 AFIX 0 C11 1 0.209322 0.420256 0.416165 11.00000 0.07501 0.05651 = 0.08917 0.00494 0.01164 0.00039 AFIX 137 H11A 2 0.250199 0.405319 0.409116 11.00000 -1.50000 H11B 2 0.181837 0.378007 0.404815 11.00000 -1.50000 H11C 2 0.208025 0.433326 0.461146 11.00000 -1.50000 AFIX 0 C12 1 0.252926 0.630545 0.583595 11.00000 0.05438 0.05042 = 0.05983 -0.00424 0.01453 0.00645 AFIX 23 H12A 2 0.260206 0.666155 0.619889 11.00000 -1.20000 H12B 2 0.292020 0.619573 0.567682 11.00000 -1.20000 AFIX 0 C13 1 0.226440 0.555683 0.607366 11.00000 0.06301 0.05405 = 0.06166 0.00657 0.01806 0.01637 AFIX 23 H13A 2 0.224320 0.517760 0.572566 11.00000 -1.20000 H13B 2 0.253817 0.535584 0.643333 11.00000 -1.20000 AFIX 0 C14 1 0.163946 0.565439 0.629124 11.00000 0.06172 0.04520 = 0.05339 0.00805 0.01599 0.00557 C15 1 0.156634 0.587564 0.691302 11.00000 0.07810 0.09114 = 0.06707 0.00036 0.02465 -0.00529 AFIX 43 H15 2 0.190897 0.596449 0.720771 11.00000 -1.20000 AFIX 0 C16 1 0.098406 0.596933 0.710961 11.00000 0.11211 0.10768 = 0.10758 -0.01746 0.06452 -0.01543 AFIX 43 H16 2 0.093877 0.611037 0.753617 11.00000 -1.20000 AFIX 0 C17 1 0.048172 0.585461 0.667799 11.00000 0.07693 0.10800 = 0.15769 0.00345 0.06096 0.00452 AFIX 43 H17 2 0.009225 0.592531 0.680630 11.00000 -1.20000 AFIX 0 C18 1 0.055032 0.563677 0.605977 11.00000 0.06336 0.13173 = 0.12017 0.00863 0.02017 -0.01665 AFIX 43 H18 2 0.020692 0.555598 0.576431 11.00000 -1.20000 AFIX 0 C19 1 0.112435 0.553494 0.586800 11.00000 0.07573 0.09198 = 0.07502 -0.00339 0.02271 -0.01173 AFIX 43 H19 2 0.116479 0.538210 0.544316 11.00000 -1.20000 AFIX 0 O6 4 0.323025 0.485603 0.519992 11.00000 0.04524 0.05318 = 0.08132 0.00281 0.02236 0.02505 O7 4 0.383215 0.522934 0.447985 11.00000 0.07014 0.04912 = 0.07292 0.01952 0.02410 0.02310 O8 4 0.473682 0.358855 0.612228 11.00000 0.06363 0.05787 = 0.07782 -0.00547 -0.01813 0.01527 O9 4 0.416895 0.247386 0.623644 11.00000 0.09976 0.05748 = 0.06560 0.01928 0.01116 0.01997 O10 4 0.323484 0.235965 0.418054 11.00000 0.09944 0.11493 = 0.09967 -0.03107 -0.02224 0.00342 N4 3 0.369293 0.472491 0.489330 11.00000 0.04189 0.04484 = 0.05241 -0.00098 0.00780 0.01603 N5 3 0.479369 0.318659 0.480788 11.00000 0.04492 0.04585 = 0.08508 0.00421 0.02412 0.02305 AFIX 43 H5 2 0.510457 0.307164 0.460606 11.00000 -1.20000 AFIX 0 N6 3 0.475634 0.436400 0.429701 11.00000 0.08723 0.06078 = 0.10143 0.01843 0.05607 0.02631 PART 1 AFIX 43 H6A 2 0.471248 0.485121 0.436603 21.00000 -1.20000 AFIX 43 PART 0 PART 2 H6B 2 0.453896 0.476150 0.417203 -21.00000 -1.20000 AFIX 0 PART 0 C20 1 0.400699 0.406301 0.501740 11.00000 0.03723 0.03625 = 0.04872 -0.00219 0.00935 0.01329 C21 1 0.453206 0.387878 0.469405 11.00000 0.04795 0.04518 = 0.05667 0.00134 0.01373 0.01504 C22 1 0.458659 0.262116 0.524820 11.00000 0.04826 0.04109 = 0.07379 0.00296 0.00253 0.02090 AFIX 13 H22 2 0.494316 0.232231 0.543106 11.00000 -1.20000 AFIX 0 C23 1 0.433049 0.304949 0.580488 11.00000 0.05820 0.04206 = 0.05359 0.00377 -0.00177 0.01195 C24 1 0.533248 0.329390 0.636026 11.00000 0.07887 0.10668 = 0.13124 -0.01011 -0.05372 0.02446 AFIX 137 H24A 2 0.556657 0.320440 0.600046 11.00000 -1.50000 H24B 2 0.528718 0.281609 0.658812 11.00000 -1.50000 H24C 2 0.554038 0.366499 0.665067 11.00000 -1.50000 AFIX 0 C25 1 0.389352 0.275195 0.679053 11.00000 0.20319 0.09930 = 0.06461 0.02341 0.04315 0.02389 AFIX 137 H25A 2 0.349775 0.296492 0.665106 11.00000 -1.50000 H25B 2 0.414821 0.314612 0.700580 11.00000 -1.50000 H25C 2 0.385010 0.233112 0.708592 11.00000 -1.50000 AFIX 0 C26 1 0.378782 0.352234 0.550612 11.00000 0.04101 0.04111 = 0.05248 -0.00113 0.00936 0.01273 AFIX 13 H26 2 0.362618 0.382729 0.584973 11.00000 -1.20000 AFIX 0 C27 1 0.328231 0.297940 0.520281 11.00000 0.04473 0.05439 = 0.08155 0.00547 0.00750 0.00050 AFIX 23 H27A 2 0.312792 0.267157 0.554273 11.00000 -1.20000 H27B 2 0.294607 0.328586 0.499667 11.00000 -1.20000 AFIX 0 C28 1 0.351418 0.245519 0.471202 11.00000 0.07070 0.05460 = 0.07434 -0.00417 0.00298 -0.00939 C29 1 0.412028 0.205247 0.491052 11.00000 0.07094 0.04238 = 0.07703 -0.00634 0.00915 0.00876 AFIX 13 H29 2 0.403957 0.166667 0.523879 11.00000 -1.20000 AFIX 0 C30 1 0.436565 0.160920 0.436081 11.00000 0.12043 0.07387 = 0.11669 -0.04035 0.01587 0.01415 AFIX 137 H30A 2 0.445397 0.196447 0.402568 11.00000 -1.50000 H30B 2 0.406517 0.124075 0.418523 11.00000 -1.50000 H30C 2 0.473331 0.134151 0.452318 11.00000 -1.50000 AFIX 0 PART 1 C31 1 0.663033 0.419354 0.213449 21.00000 0.07992 0.08909 = 0.07617 0.01131 0.04787 -0.00741 AFIX 43 H31 2 0.689560 0.415744 0.181347 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C31A 1 0.657350 0.396091 0.203459 -21.00000 0.11561 0.14185 = 0.11679 0.00694 0.05262 0.00776 AFIX 43 H31A 2 0.682649 0.393290 0.170170 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C32 1 0.640771 0.489179 0.230026 21.00000 0.09565 0.07023 = 0.11075 0.03307 0.03764 -0.00623 AFIX 43 H32 2 0.647377 0.532622 0.205074 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C32A 1 0.622361 0.337030 0.212961 -21.00000 0.11469 0.09990 = 0.09824 0.00423 0.02830 0.03587 AFIX 43 H32A 2 0.624609 0.291606 0.189123 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C33 1 0.609871 0.496095 0.281131 21.00000 0.10126 0.04722 = 0.08818 -0.00733 0.01849 -0.00180 AFIX 43 H33 2 0.597729 0.545100 0.293393 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C33A 1 0.582645 0.343727 0.258547 -21.00000 0.11450 0.08018 = 0.08546 0.02077 0.03156 0.02462 AFIX 43 H33A 2 0.560099 0.299954 0.267015 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C34 1 0.595430 0.433971 0.316059 21.00000 0.07161 0.06238 = 0.07365 -0.01298 0.02783 -0.02337 PART 0 PART 2 C34A 1 0.573038 0.407642 0.292370 -21.00000 0.06431 0.09348 = 0.04596 0.01493 0.01529 0.02412 PART 0 PART 1 C35 1 0.610845 0.363562 0.295827 21.00000 0.12009 0.06085 = 0.09079 0.01556 0.05486 0.00259 AFIX 43 H35 2 0.597870 0.319598 0.316488 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C35A 1 0.612302 0.468158 0.283448 -21.00000 0.12122 0.10489 = 0.09725 -0.00331 0.02729 0.00339 AFIX 43 H35A 2 0.608175 0.513971 0.306271 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C36 1 0.646136 0.355827 0.244113 21.00000 0.08658 0.06292 = 0.10081 0.00130 0.04191 0.01363 AFIX 43 H36 2 0.657869 0.307000 0.230982 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C36A 1 0.658481 0.463287 0.241056 -21.00000 0.10055 0.12113 = 0.10913 0.03005 0.02490 -0.01594 AFIX 43 H36A 2 0.687534 0.502026 0.238377 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C37 1 0.510356 0.411538 0.369719 21.00000 0.08940 0.08720 = 0.10101 -0.01122 0.04510 -0.00491 AFIX 23 H37A 2 0.518399 0.356275 0.371452 21.00000 -1.20000 H37B 2 0.485091 0.422732 0.329460 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C37A 1 0.536233 0.427579 0.404627 -21.00000 0.04418 0.08337 = 0.03316 -0.00721 0.01114 0.00279 AFIX 23 H37C 2 0.559676 0.386416 0.427415 -21.00000 -1.20000 H37D 2 0.559465 0.475376 0.409753 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C38 1 0.558437 0.446990 0.371249 21.00000 0.13301 0.11704 = 0.12321 -0.07867 0.07247 -0.07559 AFIX 23 H38A 2 0.583360 0.433455 0.411186 21.00000 -1.20000 H38B 2 0.549432 0.501904 0.373286 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C38A 1 0.521358 0.407531 0.332665 -21.00000 0.06307 0.15564 = 0.05085 0.00049 0.00675 0.02046 AFIX 23 H38C 2 0.502735 0.356521 0.329787 -21.00000 -1.20000 H38D 2 0.490953 0.444084 0.313849 -21.00000 -1.20000 AFIX 0 HKLF 4 REM hxm2bf_0m C 1 2/c 1 R = 0.13 REM R1 = 0.0643 for 3590 Fo > 4sig(Fo) and 0.1522 for all 7389 data REM 566 parameters refined using 231 restraints END WGHT 0.0727 0.0000 REM Highest difference peak 0.308, deepest hole -0.251, 1-sigma level 0.038 Q1 1 0.5276 0.4725 0.3387 11.00000 0.05 0.31 Q2 1 0.0570 0.7242 0.3614 11.00000 0.05 0.20 Q3 1 0.5796 0.4343 0.3845 11.00000 0.05 0.19 Q4 1 0.3339 0.4849 0.5757 11.00000 0.05 0.16 Q5 1 0.5804 0.4056 0.4399 11.00000 0.05 0.15 Q6 1 0.5314 0.3118 0.6947 11.00000 0.05 0.15 Q7 1 0.1524 0.6947 0.5175 11.00000 0.05 0.15 Q8 1 0.4879 0.3557 0.3534 11.00000 0.05 0.14 Q9 1 0.5426 0.3060 0.2372 11.00000 0.05 0.13 Q10 1 0.2444 0.6821 0.2883 11.00000 0.05 0.13 Q11 1 0.5332 0.3778 0.4048 11.00000 0.05 0.13 Q12 1 0.4218 0.2395 0.7181 11.00000 0.05 0.13 Q13 1 0.2201 0.6210 0.3957 11.00000 0.05 0.13 Q14 1 0.1038 0.5575 0.5065 11.00000 0.05 0.13 Q15 1 0.1632 0.6572 0.4652 11.00000 0.05 0.13 Q16 1 0.1300 0.7377 0.4518 11.00000 0.05 0.12 Q17 1 0.4631 0.4193 0.3832 11.00000 0.05 0.12 Q18 1 0.3147 0.7457 0.3094 11.00000 0.05 0.12 Q19 1 0.1922 0.6316 0.5110 11.00000 0.05 0.12 Q20 1 0.1764 0.6803 0.5504 11.00000 0.05 0.12 ; _shelx_res_checksum 84013 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22 22.10 9.63 2 -8 22 14.59 9.69 4 -8 22 17.23 10.10 -6 -8 -22 -6.61 8.36 6 -8 22 12.01 9.93 -8 -8 -22 -4.56 8.02 8 -8 22 2.35 11.96 -10 -8 -22 -1.39 8.72 11 -9 -22 -5.72 10.64 -9 -9 22 25.01 8.94 9 -9 -22 8.42 10.20 -7 -9 22 4.34 7.49 7 -9 -22 5.35 9.50 5 -9 -22 -0.25 8.64 -5 -9 22 19.56 8.98 3 -9 -22 11.09 8.95 -3 -9 22 11.03 8.56 1 -9 -22 7.38 9.26 -1 -9 22 4.09 8.46 1 -9 22 14.57 9.41 3 -9 22 12.90 10.78 -5 -9 -22 -10.19 8.10 5 -9 22 16.91 11.41 -7 -9 -22 -17.48 7.91 -9 -9 -22 3.72 9.20 -8 -10 22 24.26 9.69 8 -10 -22 18.62 10.44 6 -10 -22 12.42 9.38 -6 -10 22 11.34 8.57 4 -10 -22 16.02 10.44 -4 -10 22 15.75 8.80 2 -10 -22 16.85 8.96 -2 -10 22 8.29 8.61 0 -10 22 13.51 9.30 0 -10 -22 17.45 15.79 2 -10 22 18.86 10.60 4 -10 22 24.01 10.66 -6 -10 -22 -5.35 8.16 6 10 22 34.28 8.02 7 -11 -22 14.69 10.80 5 -11 -22 5.11 8.95 -5 -11 22 5.48 8.34 -3 -11 22 10.99 8.41 3 -11 -22 12.89 8.86 -1 -11 22 17.94 9.27 1 -11 -22 11.82 9.10 1 -11 22 15.59 10.34 3 -11 22 19.30 11.15 5 11 22 34.67 9.17 4 -12 -22 11.76 10.12 2 -12 -22 18.08 9.61 4 12 22 16.20 8.89 -16 0 23 9.32 7.10 -14 0 23 10.40 7.09 14 0 -23 -2.91 9.71 -12 0 23 9.11 6.36 12 0 -23 -3.31 10.18 -10 0 23 10.11 6.81 -8 0 23 12.92 8.44 -6 0 23 11.25 7.93 -4 0 23 14.52 9.71 -2 0 23 17.25 9.31 0 0 -23 6.02 8.21 0 0 23 -3.39 10.24 2 0 23 11.86 10.55 4 0 23 4.07 10.49 6 0 23 13.62 11.49 8 0 23 -0.60 11.74 10 0 23 -12.27 11.32 -17 -1 23 13.42 10.47 -17 1 23 18.04 6.80 -15 -1 23 17.72 7.79 -15 1 23 5.82 6.63 -13 -1 23 8.58 6.45 13 -1 -23 -13.13 8.85 -13 1 23 10.30 6.17 -11 -1 23 8.88 6.88 11 -1 -23 -2.87 9.33 -11 1 23 15.58 7.39 -9 -1 23 21.98 8.66 9 -1 -23 0.13 9.11 -9 1 23 21.50 8.34 -7 -1 23 16.57 8.52 7 -1 -23 11.94 9.42 -7 1 23 13.62 7.68 5 -1 -23 -0.85 8.91 -5 -1 23 14.97 9.52 -5 1 23 16.40 8.36 -3 -1 23 18.36 9.51 3 -1 -23 -0.55 8.56 -3 1 23 13.71 9.50 -1 -1 23 9.14 9.70 1 -1 -23 1.07 8.49 -1 1 23 23.68 10.91 1 -1 23 11.47 10.26 1 1 23 -0.59 10.83 3 -1 23 9.69 10.37 3 1 23 -14.95 9.86 5 -1 23 -0.38 10.57 5 1 23 -9.68 11.87 7 -1 23 4.58 11.32 7 1 23 4.15 12.77 9 -1 23 6.84 11.74 9 1 23 11.86 12.39 -16 -2 23 14.57 8.71 -16 2 23 23.88 9.22 14 -2 -23 2.76 10.31 -14 -2 23 16.84 7.99 -14 2 23 11.54 6.26 -12 -2 23 19.27 7.99 12 -2 -23 -9.56 9.35 -12 2 23 7.99 6.01 10 -2 -23 4.13 9.72 -10 -2 23 -4.46 6.43 -10 2 23 5.23 5.89 8 -2 -23 -3.27 10.07 -8 -2 23 6.71 7.59 -8 2 23 12.90 7.18 -6 -2 23 20.15 9.74 6 -2 -23 7.23 10.47 -6 2 23 23.01 8.32 -4 -2 23 6.72 9.70 4 -2 -23 -1.21 8.74 -4 2 23 4.64 8.80 2 -2 -23 -8.98 9.26 -2 -2 23 7.06 10.03 -2 2 23 6.77 9.43 0 -2 -23 2.21 9.26 0 -2 23 9.19 9.71 0 2 23 11.20 10.88 2 -2 23 20.65 10.54 2 2 23 16.96 10.45 4 -2 23 -0.30 10.22 4 2 23 16.90 11.09 6 -2 23 8.35 11.03 6 2 23 5.01 12.28 8 -2 23 13.11 12.03 8 2 23 -7.66 12.61 10 2 23 22.04 13.55 -15 -3 23 11.47 7.08 13 -3 -23 -6.75 10.77 -13 -3 23 6.56 6.82 -11 -3 23 17.09 7.73 11 -3 -23 -10.73 10.43 -11 3 23 10.48 6.06 -9 -3 23 20.92 8.18 9 -3 -23 1.52 9.58 -9 3 23 9.12 6.28 -7 -3 23 7.68 7.81 7 -3 -23 -16.91 8.59 -7 3 23 17.79 7.96 5 -3 -23 -0.64 10.46 -5 -3 23 18.12 9.79 -5 3 23 25.66 9.19 3 -3 -23 -2.38 10.03 -3 -3 23 16.31 9.17 -3 3 23 12.17 9.13 1 -3 -23 6.17 9.96 -1 -3 23 12.80 9.93 -1 3 23 14.86 9.51 1 -3 23 23.41 10.64 1 3 23 2.87 9.58 3 -3 23 7.05 10.05 3 3 23 12.92 11.70 5 -3 23 0.64 11.56 5 3 23 3.95 12.23 7 -3 23 10.07 11.03 7 3 23 0.56 12.36 9 -3 23 21.35 14.29 9 3 23 -0.46 13.54 -14 -4 23 14.67 8.47 12 -4 -23 -8.30 9.55 -12 -4 23 13.93 7.37 -10 -4 23 15.63 7.81 10 -4 -23 -8.52 10.32 8 -4 -23 -2.02 10.51 -8 -4 23 13.14 8.19 -6 -4 23 -3.41 7.36 6 -4 -23 -13.75 8.74 -6 4 23 7.66 7.18 4 -4 -23 1.99 9.32 -4 -4 23 15.81 9.17 -4 4 23 19.02 7.90 2 -4 -23 0.38 10.05 -2 -4 23 9.03 9.88 -2 4 23 22.74 9.57 0 -4 23 4.16 9.52 0 -4 -23 2.32 9.73 0 4 23 21.35 10.94 2 -4 23 16.91 10.36 2 4 23 7.43 11.28 4 -4 23 1.75 11.28 4 4 23 14.97 12.02 6 -4 23 20.06 12.24 6 4 23 -6.42 11.79 8 -4 23 5.74 11.32 8 4 23 16.92 13.83 10 4 23 -7.79 12.37 13 -5 -23 -10.68 10.95 -13 -5 23 10.48 8.27 -11 -5 23 10.21 7.50 11 -5 -23 -2.68 10.05 9 -5 -23 -19.47 8.93 -9 -5 23 13.10 7.88 -7 -5 23 13.83 8.58 7 -5 -23 2.15 9.69 -5 -5 23 32.98 10.53 5 -5 -23 3.75 9.61 3 -5 -23 -17.88 9.27 -3 -5 23 10.07 8.62 1 -5 -23 -5.52 9.51 -1 -5 23 29.05 11.08 -1 5 23 11.80 9.47 1 -5 23 21.28 10.37 1 5 23 10.85 10.29 3 -5 23 15.72 10.19 3 5 23 12.63 11.56 5 -5 23 19.56 12.04 5 5 23 6.59 11.95 7 -5 23 10.12 10.69 7 5 23 8.13 11.65 9 5 23 3.58 12.30 11 5 23 -4.04 13.93 -12 -6 23 9.25 8.39 12 -6 -23 -9.16 12.42 10 -6 -23 13.51 10.74 -10 -6 23 12.89 8.12 -8 -6 23 13.36 9.06 8 -6 -23 2.18 10.75 6 -6 -23 -0.07 9.50 -6 -6 23 6.47 8.23 4 -6 -23 -10.28 9.61 -4 -6 23 12.01 8.76 2 -6 -23 9.46 9.46 -2 -6 23 2.04 8.29 0 -6 23 9.44 9.08 2 -6 23 10.27 9.80 4 -6 23 21.90 10.24 4 6 23 12.60 16.48 6 -6 23 8.85 10.20 6 6 23 13.63 12.86 8 6 23 20.87 13.81 10 6 23 2.99 12.57 11 -7 -23 2.33 13.02 -11 -7 23 9.82 9.02 -9 -7 23 20.14 8.45 9 -7 -23 -5.26 10.61 -7 -7 23 11.80 8.52 7 -7 -23 -1.00 9.52 5 -7 -23 5.33 9.45 -5 -7 23 21.96 9.01 3 -7 -23 2.85 8.83 -3 -7 23 19.97 10.06 -1 -7 23 7.36 9.01 1 -7 -23 0.37 9.16 1 -7 23 26.02 11.40 3 -7 23 13.66 10.41 5 -7 23 12.84 10.47 10 -8 -23 -2.57 11.34 -8 -8 23 11.42 7.85 8 -8 -23 -0.51 9.57 -6 -8 23 13.19 9.10 6 -8 -23 -3.01 8.99 -4 -8 23 10.55 8.82 4 -8 -23 10.74 10.68 2 -8 -23 14.46 10.22 -2 -8 23 21.49 9.62 0 -8 23 17.61 9.95 2 -8 23 13.09 10.83 4 -8 23 11.47 10.30 7 -9 -23 9.63 10.13 -5 -9 23 -0.13 7.78 5 -9 -23 5.97 10.35 -3 -9 23 31.78 10.84 3 -9 -23 5.07 9.11 -1 -9 23 11.13 9.08 1 -9 -23 6.65 9.44 1 -9 23 16.84 9.86 3 -9 23 11.87 11.34 6 -10 -23 9.39 9.72 4 -10 -23 0.14 10.02 2 -10 -23 16.38 8.98 3 -11 -23 16.10 9.58 1 -11 -23 13.24 15.98 -14 0 24 10.74 6.83 12 0 -24 -10.60 9.62 -12 0 24 6.25 7.37 -10 0 24 11.06 7.72 10 0 -24 -6.01 9.42 -8 0 24 10.06 7.81 8 0 -24 0.45 10.10 -6 0 24 31.52 10.09 6 0 -24 17.76 9.91 4 0 -24 10.52 10.38 -4 0 24 23.87 10.27 2 0 -24 -9.78 9.28 -2 0 24 9.95 10.35 0 0 24 1.38 9.93 2 0 24 6.89 10.46 4 0 24 9.89 11.20 6 0 24 16.59 12.00 8 0 24 3.20 13.48 -15 -1 24 11.58 10.15 -15 1 24 20.89 7.54 -13 -1 24 4.35 6.60 -13 1 24 5.01 6.12 11 -1 -24 -6.39 10.57 -11 -1 24 17.93 7.54 -11 1 24 0.86 7.06 9 -1 -24 -7.37 8.87 -9 -1 24 4.21 7.96 -9 1 24 7.14 7.19 7 -1 -24 -5.73 10.23 -7 -1 24 13.07 9.24 -7 1 24 13.47 8.89 -5 -1 24 23.44 10.27 5 -1 -24 -2.78 10.06 -5 1 24 8.03 8.26 3 -1 -24 -5.75 9.78 -3 -1 24 14.61 10.27 -3 1 24 16.55 9.01 1 -1 -24 -8.28 9.30 -1 -1 24 -1.96 8.74 -1 1 24 17.71 9.94 1 -1 24 1.33 11.29 1 1 24 25.62 11.78 3 -1 24 8.93 10.51 3 1 24 10.49 11.97 5 -1 24 24.50 13.01 5 1 24 -8.77 10.73 7 -1 24 15.08 13.48 7 1 24 2.27 11.63 -14 -2 24 16.19 9.08 -14 2 24 15.33 7.45 -12 -2 24 18.11 8.29 12 -2 -24 -4.78 10.20 -12 2 24 2.61 5.94 -10 -2 24 5.95 7.28 10 -2 -24 -15.22 9.11 -10 2 24 19.02 7.78 -8 -2 24 18.72 8.51 8 -2 -24 -4.16 9.31 -8 2 24 10.21 8.03 -6 -2 24 16.62 8.88 6 -2 -24 -6.56 9.15 -6 2 24 16.25 7.89 -4 -2 24 17.51 10.67 4 -2 -24 -1.08 10.27 -4 2 24 9.68 9.32 2 -2 -24 -1.83 10.14 -2 -2 24 13.93 9.65 -2 2 24 19.09 9.51 0 -2 24 -4.71 10.23 0 2 24 20.75 11.42 2 -2 24 25.52 12.48 2 2 24 12.52 10.82 4 -2 24 9.59 11.05 4 2 24 2.25 11.03 6 -2 24 12.22 11.80 6 2 24 9.34 11.55 8 2 24 10.90 12.53 -13 -3 24 4.53 7.67 11 -3 -24 -16.95 10.61 -11 -3 24 10.88 7.64 9 -3 -24 -14.48 9.30 -9 -3 24 9.11 7.94 -9 3 24 7.05 6.32 -7 -3 24 14.90 9.15 7 -3 -24 2.60 9.73 -7 3 24 5.16 7.56 5 -3 -24 -7.32 10.29 -5 -3 24 6.68 9.38 -5 3 24 22.51 9.38 3 -3 -24 8.23 10.26 -3 -3 24 10.77 9.20 -3 3 24 18.39 8.79 -1 -3 24 21.55 10.84 1 -3 -24 -3.83 9.75 -1 3 24 23.73 11.08 1 -3 24 25.11 11.29 1 3 24 23.25 10.76 3 -3 24 13.73 10.48 3 3 24 19.39 12.29 5 -3 24 9.00 12.01 5 3 24 5.96 11.54 7 3 24 14.86 12.42 9 3 24 17.55 16.44 -12 -4 24 27.67 9.79 -10 -4 24 27.46 8.94 10 -4 -24 6.75 11.54 8 -4 -24 -10.00 10.42 -8 -4 24 13.17 8.45 -6 -4 24 12.53 9.50 6 -4 -24 -7.63 9.43 -4 -4 24 4.06 8.49 4 -4 -24 -1.22 9.16 -4 4 24 15.42 8.82 2 -4 -24 -8.16 10.09 -2 -4 24 19.57 10.91 -2 4 24 15.93 9.64 0 -4 24 21.15 10.98 0 4 24 1.68 10.44 2 -4 24 6.64 9.70 2 4 24 12.94 11.73 4 -4 24 37.07 12.93 4 4 24 16.72 12.80 6 -4 24 32.70 18.47 6 4 24 7.20 11.85 8 4 24 4.95 13.16 -9 -5 24 14.83 8.45 9 -5 -24 -16.50 10.49 -7 -5 24 17.26 10.15 7 -5 -24 -4.69 9.85 5 -5 -24 -5.72 9.41 -5 -5 24 15.33 9.18 3 -5 -24 4.74 9.67 -3 -5 24 28.32 10.01 1 -5 -24 -2.83 9.77 -1 -5 24 5.10 8.92 1 -5 24 15.68 10.26 1 5 24 19.78 11.03 3 -5 24 18.34 11.08 3 5 24 5.91 11.35 5 -5 24 -6.50 11.29 5 5 24 7.00 11.02 7 5 24 15.47 13.88 8 -6 -24 1.99 10.33 -8 -6 24 11.22 8.68 -6 -6 24 15.83 9.34 6 -6 -24 -1.01 9.87 4 -6 -24 4.41 9.82 -4 -6 24 3.21 8.60 -2 -6 24 18.99 9.79 2 -6 -24 -2.92 8.87 0 -6 24 19.15 9.89 2 -6 24 6.60 11.15 4 -6 24 7.09 11.77 8 6 24 2.42 14.19 -7 -7 24 5.53 13.12 7 -7 -24 -13.15 9.49 -5 -7 24 9.88 9.00 5 -7 -24 2.92 9.73 -3 -7 24 6.46 9.11 3 -7 -24 3.40 10.44 1 -7 -24 18.95 15.44 -1 -7 24 22.05 11.20 1 -7 24 9.60 9.49 6 -8 -24 -1.60 10.40 4 -8 -24 -0.51 9.21 2 -8 -24 8.81 9.12 5 -9 -24 6.06 10.44 3 -9 -24 17.28 10.82 2 -10 -24 15.06 9.24 -12 0 25 11.21 6.82 10 0 -25 -9.37 12.45 -10 0 25 22.06 8.98 -8 0 25 1.96 8.22 8 0 -25 -0.56 9.68 -6 0 25 10.67 9.35 6 0 -25 -0.09 9.49 4 0 -25 -6.12 10.32 -4 0 25 18.78 10.47 2 0 -25 -3.51 9.72 -2 0 25 6.21 9.28 0 0 25 8.47 11.50 2 0 25 15.13 10.98 4 0 25 10.85 11.82 -13 1 25 25.93 7.80 -11 -1 25 17.03 7.87 -11 1 25 15.01 8.15 -9 -1 25 12.26 8.35 9 -1 -25 1.71 9.91 -9 1 25 14.58 8.59 7 -1 -25 -7.31 9.46 -7 -1 25 11.44 8.68 -7 1 25 27.84 9.32 -5 -1 25 21.44 9.70 5 -1 -25 -2.72 9.50 -5 1 25 11.46 8.57 -3 -1 25 14.18 10.49 3 -1 -25 1.31 9.52 -3 1 25 17.77 9.45 -1 -1 25 19.05 11.12 1 -1 -25 -6.63 11.03 -1 1 25 23.77 11.57 1 -1 25 13.61 10.97 1 1 25 8.95 10.66 3 -1 25 39.82 13.86 3 1 25 35.40 13.42 5 -1 25 21.31 14.37 5 1 25 16.05 12.30 -12 2 25 13.63 6.66 -10 -2 25 15.22 8.93 -10 2 25 16.49 8.12 8 -2 -25 -18.20 9.45 -8 -2 25 6.01 8.04 -8 2 25 11.26 7.45 6 -2 -25 -8.95 9.28 -6 -2 25 18.71 9.48 -6 2 25 18.58 8.45 4 -2 -25 -10.77 9.14 -4 -2 25 7.64 10.25 -4 2 25 10.97 9.92 -2 -2 25 7.79 9.67 2 -2 -25 -1.18 10.50 -2 2 25 30.10 11.30 0 -2 25 19.41 10.86 0 2 25 10.72 10.41 2 -2 25 7.02 10.65 2 2 25 9.02 10.82 4 -2 25 21.52 12.16 4 2 25 3.46 11.28 6 2 25 24.25 12.81 -9 -3 25 6.24 9.07 9 -3 -25 -18.93 9.46 7 -3 -25 -10.41 11.08 -7 -3 25 16.81 9.19 -7 3 25 21.28 8.32 5 -3 -25 -6.51 9.51 -5 -3 25 16.19 9.49 -5 3 25 10.92 9.07 3 -3 -25 -5.06 9.27 -3 -3 25 14.47 9.91 -3 3 25 16.91 9.88 -1 -3 25 11.52 9.87 -1 3 25 9.89 10.27 1 -3 25 13.60 10.84 1 3 25 16.79 11.02 3 -3 25 1.67 11.83 3 3 25 22.84 11.64 5 3 25 8.50 12.96 8 -4 -25 8.86 11.77 -8 -4 25 14.73 10.88 -6 -4 25 16.76 9.58 6 -4 -25 5.11 10.09 4 -4 -25 0.79 10.07 -4 -4 25 9.02 9.30 2 -4 -25 -14.59 10.49 -2 -4 25 15.37 9.55 -2 4 25 25.89 10.38 0 -4 25 18.82 10.33 0 4 25 13.30 10.84 2 -4 25 3.85 12.19 2 4 25 18.51 12.22 4 4 25 10.67 11.61 6 4 25 30.35 14.03 7 -5 -25 -5.65 9.96 5 -5 -25 -3.64 10.75 -5 -5 25 16.35 10.25 -3 -5 25 2.93 9.80 3 -5 -25 -2.36 9.36 -1 -5 25 10.90 11.27 3 5 25 19.25 11.63 5 5 25 13.38 12.64 6 -6 -25 3.43 11.23 4 -6 -25 -1.32 9.75 2 -6 -25 -3.73 10.30 5 -7 -25 -8.76 10.71 3 -7 -25 7.06 9.81 4 -8 -25 12.09 11.27 2 -8 -25 -5.50 15.00 -10 0 26 5.08 8.62 -8 0 26 26.70 9.66 -6 0 26 65.44 12.83 6 0 -26 14.26 12.00 -4 0 26 16.31 9.69 4 0 -26 -5.03 9.55 -2 0 26 35.01 12.20 2 0 -26 6.33 9.75 0 0 26 18.30 11.55 2 0 26 24.27 14.73 -9 1 26 27.25 8.61 -7 -1 26 17.78 9.46 7 -1 -26 0.52 12.88 -7 1 26 29.39 9.51 -5 -1 26 7.20 9.29 5 -1 -26 -9.12 9.85 -5 1 26 9.77 8.79 3 -1 -26 -17.60 10.28 -3 -1 26 20.64 10.45 -3 1 26 12.98 10.85 3 1 -26 -5.44 10.13 -1 -1 26 19.68 10.51 -1 1 26 25.29 11.19 1 -1 26 24.47 13.58 1 1 26 13.00 11.25 3 1 26 15.55 18.45 -8 2 26 22.75 9.15 6 -2 -26 -3.31 11.48 -6 2 26 32.56 10.55 4 -2 -26 -17.96 10.89 -4 -2 26 22.10 12.23 -4 2 26 30.00 9.76 -2 -2 26 24.75 13.54 2 -2 -26 -18.14 10.22 -2 2 26 6.36 9.52 0 2 26 25.21 11.32 2 2 26 15.52 11.37 5 -3 -26 -13.03 9.61 -5 3 26 21.18 9.61 3 -3 -26 -10.67 10.74 -3 3 26 29.05 11.07 -1 3 26 21.90 10.51 1 3 26 23.74 12.83 3 3 26 11.53 11.59 4 -4 -26 -11.31 9.81 0 4 26 7.52 10.08 2 4 26 26.04 12.04 5 -5 -26 -19.25 12.48 3 -5 -26 -1.98 10.98 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46198 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.11699(11) 0.75118(13) 0.50399(13) 0.0883(8) Uani 1 1 d . . . . . O2 O 0.07048(11) 0.74558(15) 0.40468(13) 0.1003(9) Uani 1 1 d . . . . . O3 O 0.25007(10) 0.69192(11) 0.34635(10) 0.0647(6) Uani 1 1 d . . . . . O4 O 0.21344(10) 0.59381(12) 0.27621(10) 0.0680(6) Uani 1 1 d . . . . . O5 O 0.09337(11) 0.47948(16) 0.41548(15) 0.1060(10) Uani 1 1 d . . . . . N1 N 0.11458(13) 0.72462(15) 0.44603(17) 0.0738(9) Uani 1 1 d . . . . . N2 N 0.23949(9) 0.58836(11) 0.45053(11) 0.0445(6) Uani 1 1 d . . . . . H2 H 0.267144 0.568180 0.477956 0.053 Uiso 1 1 calc R . . . . N3 N 0.21328(10) 0.66710(12) 0.53260(13) 0.0510(6) Uani 1 1 d . . . . . H3 H 0.193720 0.707659 0.542944 0.061 Uiso 1 1 calc R . . . . C1 C 0.15723(13) 0.67533(16) 0.42646(16) 0.0546(8) Uani 1 1 d . . . . . C2 C 0.20426(12) 0.64415(15) 0.47173(15) 0.0441(7) Uani 1 1 d . . . . . C3 C 0.23399(12) 0.55994(15) 0.38454(14) 0.0457(7) Uani 1 1 d . . . . . H3A H 0.274656 0.543349 0.374629 0.055 Uiso 1 1 calc R . . . . C4 C 0.21321(13) 0.62521(17) 0.33880(15) 0.0540(8) Uani 1 1 d . . . . . C5 C 0.31366(15) 0.68140(19) 0.34121(19) 0.0819(11) Uani 1 1 d . . . . . H5A H 0.318977 0.655327 0.301163 0.123 Uiso 1 1 calc GR . . . . H5B H 0.331357 0.650805 0.377157 0.123 Uiso 1 1 calc GR . . . . H5C H 0.333512 0.730988 0.341836 0.123 Uiso 1 1 calc GR . . . . C6 C 0.1945(2) 0.6434(2) 0.22222(18) 0.1063(15) Uani 1 1 d . . . . . H6C H 0.203914 0.619141 0.182640 0.159 Uiso 1 1 calc GR . . . . H6D H 0.215784 0.691915 0.227582 0.159 Uiso 1 1 calc GR . . . . H6E H 0.151243 0.652225 0.220239 0.159 Uiso 1 1 calc GR . . . . C7 C 0.15040(14) 0.65133(19) 0.35647(16) 0.0646(9) Uani 1 1 d . . . . . H7 H 0.136627 0.695916 0.329446 0.078 Uiso 1 1 calc R . . . . C8 C 0.10392(15) 0.5848(2) 0.34357(19) 0.0844(11) Uani 1 1 d . . . . . H8A H 0.064444 0.600894 0.355902 0.101 Uiso 1 1 calc R . . . . H8B H 0.099051 0.572520 0.297516 0.101 Uiso 1 1 calc R . . . . C9 C 0.12519(15) 0.5145(2) 0.38149(18) 0.0701(10) Uani 1 1 d . . . . . C10 C 0.19026(13) 0.48977(16) 0.37428(15) 0.0557(8) Uani 1 1 d . . . . . H10 H 0.190987 0.473320 0.328990 0.067 Uiso 1 1 calc R . . . . C11 C 0.20932(15) 0.42026(17) 0.41617(17) 0.0733(10) Uani 1 1 d . . . . . H11A H 0.250199 0.405319 0.409116 0.110 Uiso 1 1 calc GR . . . . H11B H 0.181837 0.378007 0.404815 0.110 Uiso 1 1 calc GR . . . . H11C H 0.208025 0.433326 0.461146 0.110 Uiso 1 1 calc GR . . . . C12 C 0.25293(13) 0.63054(16) 0.58360(15) 0.0543(8) Uani 1 1 d . . . . . H12A H 0.260206 0.666155 0.619889 0.065 Uiso 1 1 calc R . . . . H12B H 0.292020 0.619573 0.567682 0.065 Uiso 1 1 calc R . . . . C13 C 0.22644(13) 0.55568(16) 0.60737(15) 0.0588(8) Uani 1 1 d . . . . . H13A H 0.224320 0.517760 0.572566 0.071 Uiso 1 1 calc R . . . . H13B H 0.253817 0.535584 0.643333 0.071 Uiso 1 1 calc R . . . . C14 C 0.16395(15) 0.56544(16) 0.62912(16) 0.0527(8) Uani 1 1 d . . . . . C15 C 0.15663(17) 0.5876(2) 0.69130(18) 0.0776(10) Uani 1 1 d . . . . . H15 H 0.190897 0.596449 0.720771 0.093 Uiso 1 1 calc R . . . . C16 C 0.0984(2) 0.5969(2) 0.7110(2) 0.1054(15) Uani 1 1 d . . . . . H16 H 0.093877 0.611037 0.753617 0.126 Uiso 1 1 calc R . . . . C17 C 0.0482(2) 0.5855(3) 0.6678(3) 0.1108(16) Uani 1 1 d . . . . . H17 H 0.009225 0.592531 0.680630 0.133 Uiso 1 1 calc R . . . . C18 C 0.05503(19) 0.5637(3) 0.6060(3) 0.1043(14) Uani 1 1 d . . . . . H18 H 0.020692 0.555598 0.576431 0.125 Uiso 1 1 calc R . . . . C19 C 0.11243(17) 0.5535(2) 0.58680(19) 0.0799(11) Uani 1 1 d . . . . . H19 H 0.116479 0.538210 0.544316 0.096 Uiso 1 1 calc R . . . . O6 O 0.32303(8) 0.48560(10) 0.51999(10) 0.0588(6) Uani 1 1 d . . . . . O7 O 0.38321(9) 0.52293(11) 0.44799(10) 0.0629(6) Uani 1 1 d . . . . . O8 O 0.47368(9) 0.35885(12) 0.61223(11) 0.0682(6) Uani 1 1 d . . . . . O9 O 0.41690(11) 0.24739(12) 0.62364(11) 0.0741(7) Uani 1 1 d . . . . . O10 O 0.32348(13) 0.23597(16) 0.41805(14) 0.1070(9) Uani 1 1 d . . . . . N4 N 0.36929(10) 0.47249(13) 0.48933(12) 0.0462(6) Uani 1 1 d . . . . . N5 N 0.47937(10) 0.31866(13) 0.48079(12) 0.0574(7) Uani 1 1 d . . . . . H5 H 0.510457 0.307164 0.460606 0.069 Uiso 1 1 calc DR . . . . N6 N 0.47563(13) 0.43640(16) 0.42970(14) 0.0799(9) Uani 1 1 d . U . . . H6A H 0.471248 0.485121 0.436603 0.096 Uiso 0.499(9) 1 calc R . P A 1 H6B H 0.453896 0.476150 0.417203 0.096 Uiso 0.501(9) 1 calc R . P A 2 C20 C 0.40070(11) 0.40630(14) 0.50174(13) 0.0404(7) Uani 1 1 d . . . . . C21 C 0.45321(12) 0.38788(16) 0.46940(14) 0.0494(7) Uani 1 1 d . . . . . C22 C 0.45866(13) 0.26212(16) 0.52482(15) 0.0547(8) Uani 1 1 d . . . . . H22 H 0.494316 0.232231 0.543106 0.066 Uiso 1 1 calc R . . . . C23 C 0.43305(13) 0.30495(16) 0.58049(15) 0.0518(8) Uani 1 1 d . . . . . C24 C 0.53325(16) 0.3294(2) 0.6360(2) 0.1102(16) Uani 1 1 d . . . . . H24A H 0.556657 0.320440 0.600046 0.165 Uiso 1 1 calc GR . . . . H24B H 0.528718 0.281609 0.658812 0.165 Uiso 1 1 calc GR . . . . H24C H 0.554038 0.366499 0.665067 0.165 Uiso 1 1 calc GR . . . . C25 C 0.3894(2) 0.2752(2) 0.67905(19) 0.1203(17) Uani 1 1 d . . . . . H25A H 0.349775 0.296492 0.665106 0.180 Uiso 1 1 calc GR . . . . H25B H 0.414821 0.314612 0.700580 0.180 Uiso 1 1 calc GR . . . . H25C H 0.385010 0.233112 0.708592 0.180 Uiso 1 1 calc GR . . . . C26 C 0.37878(11) 0.35223(15) 0.55061(14) 0.0446(7) Uani 1 1 d . . . . . H26 H 0.362618 0.382729 0.584973 0.053 Uiso 1 1 calc R . . . . C27 C 0.32823(13) 0.29794(17) 0.52028(16) 0.0602(9) Uani 1 1 d . . . . . H27A H 0.312792 0.267157 0.554273 0.072 Uiso 1 1 calc R . . . . H27B H 0.294607 0.328586 0.499667 0.072 Uiso 1 1 calc R . . . . C28 C 0.35142(16) 0.24552(18) 0.4712(2) 0.0669(9) Uani 1 1 d . . . . . C29 C 0.41203(14) 0.20525(17) 0.49105(16) 0.0634(9) Uani 1 1 d . . . . . H29 H 0.403957 0.166667 0.523879 0.076 Uiso 1 1 calc R . . . . C30 C 0.43657(19) 0.1609(2) 0.4361(2) 0.1034(14) Uani 1 1 d . . . . . H30A H 0.445397 0.196447 0.402568 0.155 Uiso 1 1 calc GR . . . . H30B H 0.406517 0.124075 0.418523 0.155 Uiso 1 1 calc GR . . . . H30C H 0.473331 0.134151 0.452318 0.155 Uiso 1 1 calc GR . . . . C31 C 0.6630(7) 0.4194(7) 0.2134(8) 0.079(3) Uani 0.499(9) 1 d D U P A 1 H31 H 0.689560 0.415744 0.181347 0.095 Uiso 0.499(9) 1 calc R . P A 1 C31A C 0.6574(10) 0.3961(9) 0.2035(10) 0.122(6) Uani 0.501(9) 1 d D U P A 2 H31A H 0.682649 0.393290 0.170170 0.146 Uiso 0.501(9) 1 calc R . P A 2 C32 C 0.6408(6) 0.4892(6) 0.2300(7) 0.090(3) Uani 0.499(9) 1 d D U P A 1 H32 H 0.647377 0.532622 0.205074 0.108 Uiso 0.499(9) 1 calc R . P A 1 C32A C 0.6224(6) 0.3370(7) 0.2130(6) 0.103(4) Uani 0.501(9) 1 d D U P A 2 H32A H 0.624609 0.291606 0.189123 0.124 Uiso 0.501(9) 1 calc R . P A 2 C33 C 0.6099(7) 0.4961(6) 0.2811(7) 0.078(3) Uani 0.499(9) 1 d D U P A 1 H33 H 0.597729 0.545100 0.293393 0.094 Uiso 0.499(9) 1 calc R . P A 1 C33A C 0.5826(5) 0.3437(6) 0.2585(5) 0.092(3) Uani 0.501(9) 1 d D U P A 2 H33A H 0.560099 0.299954 0.267015 0.110 Uiso 0.501(9) 1 calc R . P A 2 C34 C 0.5954(4) 0.4340(5) 0.3161(5) 0.068(3) Uani 0.499(9) 1 d D U P A 1 C34A C 0.5730(4) 0.4076(6) 0.2924(4) 0.067(2) Uani 0.501(9) 1 d D U P A 2 C35 C 0.6108(5) 0.3636(5) 0.2958(5) 0.087(3) Uani 0.499(9) 1 d D U P A 1 H35 H 0.597870 0.319598 0.316488 0.105 Uiso 0.499(9) 1 calc R . P A 1 C35A C 0.6123(8) 0.4682(8) 0.2834(9) 0.107(4) Uani 0.501(9) 1 d D U P A 2 H35A H 0.608175 0.513971 0.306271 0.128 Uiso 0.501(9) 1 calc R . P A 2 C36 C 0.6461(5) 0.3558(5) 0.2441(5) 0.081(3) Uani 0.499(9) 1 d D U P A 1 H36 H 0.657869 0.307000 0.230982 0.097 Uiso 0.499(9) 1 calc R . P A 1 C36A C 0.6585(7) 0.4633(9) 0.2411(7) 0.109(5) Uani 0.501(9) 1 d D U P A 2 H36A H 0.687534 0.502026 0.238377 0.131 Uiso 0.501(9) 1 calc R . P A 2 C37 C 0.5104(5) 0.4115(6) 0.3697(6) 0.090(3) Uani 0.499(9) 1 d . U P A 1 H37A H 0.518399 0.356275 0.371452 0.108 Uiso 0.499(9) 1 calc DR . P A 1 H37B H 0.485091 0.422732 0.329460 0.108 Uiso 0.499(9) 1 calc R . P A 1 C37A C 0.5362(3) 0.4276(5) 0.4046(4) 0.053(2) Uani 0.501(9) 1 d . U P A 2 H37C H 0.559676 0.386416 0.427415 0.064 Uiso 0.501(9) 1 calc R . P A 2 H37D H 0.559465 0.475376 0.409753 0.064 Uiso 0.501(9) 1 calc R . P A 2 C38 C 0.5584(5) 0.4470(5) 0.3712(6) 0.120(4) Uani 0.499(9) 1 d D U P A 1 H38A H 0.583360 0.433455 0.411186 0.144 Uiso 0.499(9) 1 calc R . P A 1 H38B H 0.549432 0.501904 0.373286 0.144 Uiso 0.499(9) 1 calc R . P A 1 C38A C 0.5214(4) 0.4075(7) 0.3327(4) 0.090(3) Uani 0.501(9) 1 d D U P A 2 H38C H 0.502735 0.356521 0.329787 0.108 Uiso 0.501(9) 1 calc R . P A 2 H38D H 0.490953 0.444084 0.313849 0.108 Uiso 0.501(9) 1 calc R . P A 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 O1 0.1022(19) 0.0817(17) 0.089(2) 0.0077(15) 0.0452(16) 0.0567(14) O2 0.0841(17) 0.119(2) 0.103(2) 0.0391(17) 0.0326(16) 0.0765(16) O3 0.0720(15) 0.0465(12) 0.0815(16) 0.0112(11) 0.0365(12) 0.0179(11) O4 0.0854(16) 0.0717(14) 0.0482(14) 0.0111(11) 0.0130(12) 0.0283(12) O5 0.0576(15) 0.115(2) 0.149(3) 0.0223(19) 0.0260(17) -0.0123(15) N1 0.073(2) 0.0660(18) 0.088(2) 0.0253(17) 0.0336(18) 0.0427(16) N2 0.0402(13) 0.0430(13) 0.0519(16) 0.0048(11) 0.0123(11) 0.0189(11) N3 0.0598(16) 0.0363(13) 0.0610(19) 0.0012(13) 0.0255(14) 0.0150(12) C1 0.0529(18) 0.0508(18) 0.065(2) 0.0161(16) 0.0266(16) 0.0307(15) C2 0.0432(16) 0.0360(15) 0.058(2) 0.0094(15) 0.0258(15) 0.0155(13) C3 0.0397(16) 0.0465(16) 0.053(2) 0.0026(14) 0.0162(14) 0.0136(13) C4 0.060(2) 0.0539(19) 0.051(2) 0.0098(16) 0.0198(16) 0.0178(16) C5 0.079(2) 0.066(2) 0.110(3) -0.005(2) 0.048(2) -0.0010(19) C6 0.150(4) 0.112(3) 0.059(3) 0.026(2) 0.022(3) 0.046(3) C7 0.058(2) 0.068(2) 0.070(3) 0.0191(18) 0.0153(18) 0.0305(18) C8 0.051(2) 0.110(3) 0.091(3) 0.006(2) 0.003(2) 0.028(2) C9 0.048(2) 0.082(3) 0.080(3) -0.002(2) 0.0026(19) 0.0008(19) C10 0.0561(19) 0.0524(19) 0.060(2) 0.0007(15) 0.0116(16) 0.0091(15) C11 0.075(2) 0.057(2) 0.089(3) 0.0049(18) 0.012(2) 0.0004(17) C12 0.0544(18) 0.0504(18) 0.060(2) -0.0042(16) 0.0145(16) 0.0065(15) C13 0.063(2) 0.0541(19) 0.062(2) 0.0066(16) 0.0181(16) 0.0164(16) C14 0.062(2) 0.0452(17) 0.053(2) 0.0081(15) 0.0160(18) 0.0056(15) C15 0.078(3) 0.091(3) 0.067(3) 0.000(2) 0.025(2) -0.005(2) C16 0.112(4) 0.108(3) 0.108(4) -0.017(3) 0.065(3) -0.015(3) C17 0.077(3) 0.108(4) 0.158(5) 0.003(3) 0.061(4) 0.005(3) C18 0.063(3) 0.132(4) 0.120(4) 0.009(3) 0.020(3) -0.017(2) C19 0.076(3) 0.092(3) 0.075(3) -0.003(2) 0.023(2) -0.012(2) O6 0.0452(11) 0.0532(12) 0.0813(15) 0.0028(11) 0.0224(11) 0.0250(10) O7 0.0701(14) 0.0491(12) 0.0729(15) 0.0195(11) 0.0241(12) 0.0231(11) O8 0.0636(14) 0.0579(13) 0.0778(16) -0.0055(12) -0.0181(12) 0.0153(11) O9 0.0998(18) 0.0575(13) 0.0656(16) 0.0193(12) 0.0112(13) 0.0200(12) O10 0.099(2) 0.115(2) 0.100(2) -0.0311(18) -0.0222(18) 0.0034(17) N4 0.0419(14) 0.0448(14) 0.0524(16) -0.0010(12) 0.0078(12) 0.0160(12) N5 0.0449(14) 0.0458(14) 0.085(2) 0.0042(13) 0.0241(13) 0.0230(12) N6 0.087(2) 0.0608(17) 0.101(2) 0.0184(16) 0.0561(18) 0.0263(15) C20 0.0372(15) 0.0363(15) 0.0487(18) -0.0022(13) 0.0093(13) 0.0133(12) C21 0.0480(17) 0.0452(17) 0.057(2) 0.0013(15) 0.0137(15) 0.0150(14) C22 0.0483(17) 0.0411(17) 0.074(2) 0.0030(16) 0.0025(16) 0.0209(14) C23 0.0582(19) 0.0421(17) 0.054(2) 0.0038(15) -0.0018(16) 0.0120(15) C24 0.079(3) 0.107(3) 0.131(4) -0.010(3) -0.054(3) 0.024(2) C25 0.203(5) 0.099(3) 0.065(3) 0.023(2) 0.043(3) 0.024(3) C26 0.0410(16) 0.0411(15) 0.0525(19) -0.0011(14) 0.0094(14) 0.0127(13) C27 0.0447(17) 0.0544(19) 0.082(2) 0.0055(17) 0.0075(17) 0.0005(15) C28 0.071(2) 0.055(2) 0.074(3) -0.0042(19) 0.003(2) -0.0094(18) C29 0.071(2) 0.0424(18) 0.077(2) -0.0063(16) 0.0091(18) 0.0088(16) C30 0.120(3) 0.074(3) 0.117(3) -0.040(2) 0.016(3) 0.014(2) C31 0.080(6) 0.089(5) 0.076(7) 0.011(5) 0.048(5) -0.007(5) C31A 0.116(8) 0.142(8) 0.117(9) 0.007(6) 0.053(7) 0.008(6) C32 0.096(7) 0.070(5) 0.111(7) 0.033(5) 0.038(5) -0.006(5) C32A 0.115(7) 0.100(6) 0.098(7) 0.004(5) 0.028(5) 0.036(5) C33 0.101(6) 0.047(4) 0.088(6) -0.007(4) 0.018(5) -0.002(5) C33A 0.115(6) 0.080(5) 0.085(6) 0.021(4) 0.032(5) 0.025(5) C34 0.072(5) 0.062(4) 0.074(6) -0.013(4) 0.028(4) -0.023(4) C34A 0.064(5) 0.093(5) 0.046(5) 0.015(4) 0.015(4) 0.024(4) C35 0.120(7) 0.061(4) 0.091(6) 0.016(4) 0.055(5) 0.003(5) C35A 0.121(7) 0.105(8) 0.097(7) -0.003(7) 0.027(6) 0.003(6) C36 0.087(6) 0.063(4) 0.101(7) 0.001(4) 0.042(5) 0.014(4) C36A 0.101(8) 0.121(8) 0.109(8) 0.030(6) 0.025(6) -0.016(7) C37 0.089(6) 0.087(5) 0.101(8) -0.011(6) 0.045(5) -0.005(4) C37A 0.044(4) 0.083(5) 0.033(4) -0.007(3) 0.011(3) 0.003(3) C38 0.133(6) 0.117(6) 0.123(7) -0.079(5) 0.072(5) -0.076(5) C38A 0.063(5) 0.156(7) 0.051(5) 0.000(5) 0.007(4) 0.020(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C4 O3 C5 116.4(2) C4 O4 C6 117.3(2) O1 N1 C1 122.8(3) O2 N1 O1 118.7(3) O2 N1 C1 118.5(3) C2 N2 H2 118.0 C2 N2 C3 124.1(2) C3 N2 H2 118.0 C2 N3 H3 117.0 C2 N3 C12 126.0(2) C12 N3 H3 117.0 N1 C1 C2 121.1(3) N1 C1 C7 117.3(3) C2 C1 C7 121.5(2) N2 C2 C1 117.5(3) N3 C2 N2 119.8(2) N3 C2 C1 122.8(2) N2 C3 H3A 108.0 N2 C3 C4 109.1(2) N2 C3 C10 112.7(2) C4 C3 H3A 108.0 C4 C3 C10 110.8(2) C10 C3 H3A 108.0 O3 C4 C3 114.1(2) O3 C4 C7 104.8(2) O4 C4 O3 111.1(2) O4 C4 C3 105.0(2) O4 C4 C7 115.1(3) C3 C4 C7 106.9(2) O3 C5 H5A 109.5 O3 C5 H5B 109.5 O3 C5 H5C 109.5 H5A C5 H5B 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 O4 C6 H6C 109.5 O4 C6 H6D 109.5 O4 C6 H6E 109.5 H6C C6 H6D 109.5 H6C C6 H6E 109.5 H6D C6 H6E 109.5 C1 C7 C4 108.1(3) C1 C7 H7 109.1 C1 C7 C8 111.8(3) C4 C7 H7 109.1 C4 C7 C8 109.7(3) C8 C7 H7 109.1 C7 C8 H8A 109.6 C7 C8 H8B 109.6 H8A C8 H8B 108.1 C9 C8 C7 110.5(3) C9 C8 H8A 109.6 C9 C8 H8B 109.6 O5 C9 C8 123.0(3) O5 C9 C10 121.8(3) C8 C9 C10 115.1(3) C3 C10 H10 106.6 C9 C10 C3 110.2(2) C9 C10 H10 106.6 C11 C10 C3 114.3(3) C11 C10 C9 112.0(3) C11 C10 H10 106.6 C10 C11 H11A 109.5 C10 C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11B 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 N3 C12 H12A 109.0 N3 C12 H12B 109.0 N3 C12 C13 112.7(2) H12A C12 H12B 107.8 C13 C12 H12A 109.0 C13 C12 H12B 109.0 C12 C13 H13A 108.9 C12 C13 H13B 108.9 H13A C13 H13B 107.7 C14 C13 C12 113.3(2) C14 C13 H13A 108.9 C14 C13 H13B 108.9 C15 C14 C13 121.0(3) C15 C14 C19 118.1(3) C19 C14 C13 120.8(3) C14 C15 H15 119.7 C14 C15 C16 120.6(4) C16 C15 H15 119.7 C15 C16 H16 120.0 C17 C16 C15 120.0(4) C17 C16 H16 120.0 C16 C17 H17 120.1 C18 C17 C16 119.8(4) C18 C17 H17 120.1 C17 C18 H18 119.9 C17 C18 C19 120.3(4) C19 C18 H18 119.9 C14 C19 C18 121.2(4) C14 C19 H19 119.4 C18 C19 H19 119.4 C23 O8 C24 115.8(2) C23 O9 C25 115.2(2) O6 N4 O7 118.1(2) O6 N4 C20 118.4(2) O7 N4 C20 123.5(2) C21 N5 H5 118.0 C21 N5 C22 124.0(2) C22 N5 H5 118.0 C21 N6 H6A 117.8 C21 N6 H6B 117.8 C21 N6 C37 124.3(4) C21 N6 C37A 124.4(4) C37 N6 H6A 117.8 C37A N6 H6B 117.8 N4 C20 C21 121.5(2) N4 C20 C26 117.7(2) C21 C20 C26 120.8(2) N5 C21 C20 118.1(3) N6 C21 N5 120.1(3) N6 C21 C20 121.9(2) N5 C22 H22 107.9 N5 C22 C23 108.3(2) N5 C22 C29 112.7(3) C23 C22 H22 107.9 C23 C22 C29 111.9(2) C29 C22 H22 107.9 O8 C23 O9 111.3(2) O8 C23 C22 114.0(2) O8 C23 C26 105.5(2) O9 C23 C22 105.9(2) O9 C23 C26 113.4(2) C26 C23 C22 106.8(2) O8 C24 H24A 109.5 O8 C24 H24B 109.5 O8 C24 H24C 109.5 H24A C24 H24B 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 O9 C25 H25A 109.5 O9 C25 H25B 109.5 O9 C25 H25C 109.5 H25A C25 H25B 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C20 C26 C23 108.4(2) C20 C26 H26 108.8 C20 C26 C27 112.1(2) C23 C26 H26 108.8 C23 C26 C27 109.9(2) C27 C26 H26 108.8 C26 C27 H27A 109.4 C26 C27 H27B 109.4 H27A C27 H27B 108.0 C28 C27 C26 111.4(2) C28 C27 H27A 109.4 C28 C27 H27B 109.4 O10 C28 C27 121.6(3) O10 C28 C29 121.9(3) C27 C28 C29 116.5(3) C22 C29 H29 106.3 C28 C29 C22 110.8(2) C28 C29 H29 106.3 C30 C29 C22 113.0(3) C30 C29 C28 113.5(3) C30 C29 H29 106.3 C29 C30 H30A 109.5 C29 C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30B 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C32 C31 H31 120.6 C36 C31 H31 120.6 C36 C31 C32 118.8(11) C32A C31A H31A 118.6 C32A C31A C36A 122.8(16) C36A C31A H31A 118.6 C31 C32 H32 119.6 C33 C32 C31 120.8(11) C33 C32 H32 119.6 C31A C32A H32A 121.0 C31A C32A C33A 118.1(13) C33A C32A H32A 121.0 C32 C33 H33 119.1 C32 C33 C34 121.7(10) C34 C33 H33 119.1 C32A C33A H33A 117.1 C34A C33A C32A 125.7(10) C34A C33A H33A 117.1 C33 C34 C38 118.0(9) C35 C34 C33 118.2(8) C35 C34 C38 123.6(8) C33A C34A C35A 114.9(9) C33A C34A C38A 117.9(9) C35A C34A C38A 127.2(11) C34 C35 H35 119.8 C34 C35 C36 120.4(8) C36 C35 H35 119.8 C34A C35A H35A 118.7 C34A C35A C36A 122.6(12) C36A C35A H35A 118.7 C31 C36 C35 119.3(9) C31 C36 H36 120.3 C35 C36 H36 120.3 C31A C36A C35A 115.1(15) C31A C36A H36A 122.5 C35A C36A H36A 122.5 N6 C37 H37A 109.8 N6 C37 H37B 109.8 H37A C37 H37B 108.2 C38 C37 N6 109.4(11) C38 C37 H37A 109.8 C38 C37 H37B 109.8 N6 C37A H37C 110.8 N6 C37A H37D 110.8 N6 C37A C38A 104.7(6) H37C C37A H37D 108.9 C38A C37A H37C 110.8 C38A C37A H37D 110.8 C34 C38 H38A 108.2 C34 C38 H38B 108.2 C37 C38 C34 116.5(10) C37 C38 H38A 108.2 C37 C38 H38B 108.2 H38A C38 H38B 107.3 C34A C38A C37A 116.7(8) C34A C38A H38C 108.1 C34A C38A H38D 108.1 C37A C38A H38C 108.1 C37A C38A H38D 108.1 H38C C38A H38D 107.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 N1 1.279(3) O2 N1 1.275(3) O3 C4 1.407(3) O3 C5 1.424(3) O4 C4 1.403(3) O4 C6 1.432(4) O5 C9 1.204(4) N1 C1 1.358(3) N2 H2 0.8600 N2 C2 1.338(3) N2 C3 1.443(3) N3 H3 0.8600 N3 C2 1.314(3) N3 C12 1.440(4) C1 C2 1.425(4) C1 C7 1.497(4) C3 H3A 0.9800 C3 C4 1.510(4) C3 C10 1.547(4) C4 C7 1.532(4) C5 H5A 0.9600 C5 H5B 0.9600 C5 H5C 0.9600 C6 H6C 0.9600 C6 H6D 0.9600 C6 H6E 0.9600 C7 H7 0.9800 C7 C8 1.542(5) C8 H8A 0.9700 C8 H8B 0.9700 C8 C9 1.492(5) C9 C10 1.514(4) C10 H10 0.9800 C10 C11 1.513(4) C11 H11A 0.9600 C11 H11B 0.9600 C11 H11C 0.9600 C12 H12A 0.9700 C12 H12B 0.9700 C12 C13 1.520(4) C13 H13A 0.9700 C13 H13B 0.9700 C13 C14 1.498(4) C14 C15 1.366(4) C14 C19 1.371(4) C15 H15 0.9300 C15 C16 1.392(5) C16 H16 0.9300 C16 C17 1.359(6) C17 H17 0.9300 C17 C18 1.355(6) C18 H18 0.9300 C18 C19 1.372(5) C19 H19 0.9300 O6 N4 1.273(3) O7 N4 1.279(3) O8 C23 1.404(3) O8 C24 1.442(4) O9 C23 1.405(3) O9 C25 1.433(4) O10 C28 1.212(4) N4 C20 1.345(3) N5 H5 0.8600 N5 C21 1.336(3) N5 C22 1.440(3) N6 H6A 0.8600 N6 H6B 0.8600 N6 C21 1.305(3) N6 C37 1.582(10) N6 C37A 1.486(8) C20 C21 1.428(3) C20 C26 1.492(4) C22 H22 0.9800 C22 C23 1.524(4) C22 C29 1.533(4) C23 C26 1.521(4) C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 H26 0.9800 C26 C27 1.536(4) C27 H27A 0.9700 C27 H27B 0.9700 C27 C28 1.488(4) C28 C29 1.520(4) C29 H29 0.9800 C29 C30 1.515(4) C30 H30A 0.9600 C30 H30B 0.9600 C30 H30C 0.9600 C31 H31 0.9300 C31 C32 1.358(13) C31 C36 1.338(12) C31A H31A 0.9300 C31A C32A 1.304(14) C31A C36A 1.395(15) C32 H32 0.9300 C32 C33 1.320(13) C32A H32A 0.9300 C32A C33A 1.355(11) C33 H33 0.9300 C33 C34 1.349(12) C33A H33A 0.9300 C33A C34A 1.335(11) C34 C35 1.340(10) C34 C38 1.485(11) C34A C35A 1.379(13) C34A C38A 1.477(10) C35 H35 0.9300 C35 C36 1.391(10) C35A H35A 0.9300 C35A C36A 1.411(14) C36 H36 0.9300 C36A H36A 0.9300 C37 H37A 0.9700 C37 H37B 0.9700 C37 C38 1.218(15) C37A H37C 0.9700 C37A H37D 0.9700 C37A C38A 1.529(14) C38 H38A 0.9700 C38 H38B 0.9700 C38A H38C 0.9700 C38A H38D 0.9700 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 O1 N1 C1 C2 6.4(5) O1 N1 C1 C7 -177.4(3) O2 N1 C1 C2 -174.1(3) O2 N1 C1 C7 2.2(4) O3 C4 C7 C1 -63.4(3) O3 C4 C7 C8 174.5(2) O4 C4 C7 C1 174.2(2) O4 C4 C7 C8 52.1(3) O5 C9 C10 C3 -130.8(4) O5 C9 C10 C11 -2.4(5) N1 C1 C2 N2 171.3(3) N1 C1 C2 N3 -7.6(4) N1 C1 C7 C4 157.4(3) N1 C1 C7 C8 -81.9(3) N2 C3 C4 O3 54.0(3) N2 C3 C4 O4 175.9(2) N2 C3 C4 C7 -61.4(3) N2 C3 C10 C9 67.2(3) N2 C3 C10 C11 -60.0(3) N3 C12 C13 C14 -55.1(4) C1 C7 C8 C9 -62.2(3) C2 N2 C3 C4 32.0(3) C2 N2 C3 C10 -91.5(3) C2 N3 C12 C13 -74.6(3) C2 C1 C7 C4 -26.4(4) C2 C1 C7 C8 94.3(3) C3 N2 C2 N3 -179.0(2) C3 N2 C2 C1 2.1(4) C3 C4 C7 C1 58.0(3) C3 C4 C7 C8 -64.1(3) C4 C3 C10 C9 -55.4(3) C4 C3 C10 C11 177.4(2) C4 C7 C8 C9 57.7(4) C5 O3 C4 O4 -63.2(3) C5 O3 C4 C3 55.4(3) C5 O3 C4 C7 171.9(3) C6 O4 C4 O3 -57.0(3) C6 O4 C4 C3 179.1(3) C6 O4 C4 C7 61.9(4) C7 C1 C2 N2 -4.7(4) C7 C1 C2 N3 176.4(3) C7 C8 C9 O5 129.3(4) C7 C8 C9 C10 -50.8(4) C8 C9 C10 C3 49.2(4) C8 C9 C10 C11 177.7(3) C10 C3 C4 O3 178.6(2) C10 C3 C4 O4 -59.5(3) C10 C3 C4 C7 63.3(3) C12 N3 C2 N2 -9.3(4) C12 N3 C2 C1 169.6(3) C12 C13 C14 C15 -86.3(4) C12 C13 C14 C19 92.7(4) C13 C14 C15 C16 179.6(3) C13 C14 C19 C18 -178.8(3) C14 C15 C16 C17 -1.2(6) C15 C14 C19 C18 0.3(5) C15 C16 C17 C18 1.1(7) C16 C17 C18 C19 -0.3(7) C17 C18 C19 C14 -0.4(6) C19 C14 C15 C16 0.6(5) O6 N4 C20 C21 -179.7(2) O6 N4 C20 C26 0.4(4) O7 N4 C20 C21 0.7(4) O7 N4 C20 C26 -179.2(2) O8 C23 C26 C20 62.9(3) O8 C23 C26 C27 -174.3(2) O9 C23 C26 C20 -175.1(2) O9 C23 C26 C27 -52.3(3) O10 C28 C29 C22 135.2(3) O10 C28 C29 C30 6.7(5) N4 C20 C21 N5 -175.3(2) N4 C20 C21 N6 4.7(5) N4 C20 C26 C23 -153.3(2) N4 C20 C26 C27 85.2(3) N5 C22 C23 O8 -54.0(3) N5 C22 C23 O9 -176.7(2) N5 C22 C23 C26 62.1(3) N5 C22 C29 C28 -70.2(3) N5 C22 C29 C30 58.5(3) N6 C37 C38 C34 -176.6(8) N6 C37A C38A C34A 170.5(7) C20 C26 C27 C28 64.1(3) C21 N5 C22 C23 -32.7(4) C21 N5 C22 C29 91.6(3) C21 N6 C37 C38 -130.2(9) C21 N6 C37A C38A 109.5(7) C21 C20 C26 C23 26.8(3) C21 C20 C26 C27 -94.7(3) C22 N5 C21 N6 178.6(3) C22 N5 C21 C20 -1.4(4) C22 C23 C26 C20 -58.8(3) C22 C23 C26 C27 64.0(3) C23 C22 C29 C28 52.1(3) C23 C22 C29 C30 -179.2(3) C23 C26 C27 C28 -56.5(3) C24 O8 C23 O9 65.8(3) C24 O8 C23 C22 -53.9(4) C24 O8 C23 C26 -170.8(3) C25 O9 C23 O8 57.8(4) C25 O9 C23 C22 -177.8(3) C25 O9 C23 C26 -60.9(4) C26 C20 C21 N5 4.6(4) C26 C20 C21 N6 -175.4(3) C26 C27 C28 O10 -132.7(3) C26 C27 C28 C29 46.9(4) C27 C28 C29 C22 -44.4(4) C27 C28 C29 C30 -172.8(3) C29 C22 C23 O8 -178.9(2) C29 C22 C23 O9 58.5(3) C29 C22 C23 C26 -62.7(3) C31 C32 C33 C34 -5(2) C31A C32A C33A C34A 5(2) C32 C31 C36 C35 -6(2) C32 C33 C34 C35 -3(2) C32 C33 C34 C38 -177.6(14) C32A C31A C36A C35A -10(3) C32A C33A C34A C35A -7.0(17) C32A C33A C34A C38A 170.9(9) C33 C34 C35 C36 6.4(17) C33 C34 C38 C37 122.8(14) C33A C34A C35A C36A 1(2) C33A C34A C38A C37A 125.4(10) C34 C35 C36 C31 -2.0(17) C34A C35A C36A C31A 7(2) C35 C34 C38 C37 -51.5(18) C35A C34A C38A C37A -57.1(16) C36 C31 C32 C33 9(2) C36A C31A C32A C33A 4(3) C37 N6 C21 N5 29.7(7) C37 N6 C21 C20 -150.3(6) C37A N6 C21 N5 -12.4(6) C37A N6 C21 C20 167.7(5) C38 C34 C35 C36 -179.4(9) C38A C34A C35A C36A -176.7(12)