#------------------------------------------------------------------------------ #$Date: 2019-03-21 05:32:57 +0200 (Thu, 21 Mar 2019) $ #$Revision: 214247 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/83/2108385.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108385 loop_ _publ_author_name 'Han, Yang' 'Fu, Qiang' 'Zhang, Peng' 'Guan, Hongyu' 'Guo, Fang' _publ_section_title ; Acid--ammonium heterodimer and N~(ammonium)~--H···N~(pyridine)~ synthon preference in three salts of nicotinic acid with (1R,2R)-1,2-diphenylethylenediamine ; _journal_coeditor_code AW5017SUP1 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619000477 _journal_volume 75 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_moiety '2(C6 H4 N O2), 2(C7 H9 N)' _chemical_formula_sum 'C26 H26 N4 O4' _chemical_formula_weight 458.51 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2018-11-06 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 129.963(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 23.479(6) _cell_length_b 8.602(2) _cell_length_c 16.899(4) _cell_measurement_reflns_used 4568 _cell_measurement_temperature 273 _cell_measurement_theta_max 28.000 _cell_measurement_theta_min 3.413 _cell_volume 2615.9(11) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 273 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'CCD area detector' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 11704 _diffrn_reflns_point_group_measured_fraction_full 0.978 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_theta_full 25.243 _diffrn_reflns_theta_max 28.358 _diffrn_reflns_theta_min 3.414 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.7143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.164 _exptl_crystal_description plate _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.326 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details ; Flack x determined using 1504 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.3(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 368 _refine_ls_number_reflns 6271 _refine_ls_number_restraints 37 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0596 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+0.3861P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1518 _refine_ls_wR_factor_ref 0.1742 _reflns_Friedel_coverage 0.810 _reflns_Friedel_fraction_full 0.960 _reflns_Friedel_fraction_max 0.913 _reflns_number_gt 4303 _reflns_number_total 6271 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file aw5017sup1.cif _cod_data_source_block DPEN1-NA2 _cod_original_cell_volume 2616.1(11) _cod_database_code 2108385 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C19B) = Uanis(C19) Uanis(C18) = Uanis(C18A) Uanis(C16A) = Uanis(C16) 3. Others Sof(C19B)=Sof(H19B)=Sof(N4A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)= Sof(C18A)=Sof(C15A)=Sof(H15A)=1-FVAR(1) Sof(N4)=Sof(C18)=Sof(C17)=Sof(H17)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)= Sof(C19)=Sof(H19)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C1(H1), C8(H8) 4.b Aromatic/amide H refined with riding coordinates: C25(H25), C23(H23), C19B(H19B), C21(H21), C22(H22), C10(H10), C7(H7), C5(H5), C14(H14), C13(H13), C12(H12), C3(H3), C11(H11), C4(H4), C6(H6), C17(H17), C15(H15), C16(H16), C16A(H16A), C17A(H17A), C15A(H15A), C19(H19) ; _shelx_res_file ; TITL 20161229h_0m_a.res in C2 20161229h_0m.res created by SHELXL-2018/3 at 16:12:03 on 06-Nov-2018 REM Old TITL 20161229H_0m in C2/n #15 REM SHELXT solution in C2 REM R1 0.189, Rweak 0.047, Alpha 0.011, Orientation as input REM Flack x = 0.252 ( 0.335 ) from Parsons' quotients REM Formula found by SHELXT: C25 N3 O3 CELL 0.71076 23.4788 8.6025 16.8994 90 129.963 90 ZERR 4 0.0055 0.002 0.004 0 0.005 0 LATT -7 SYMM -X,+Y,-Z SFAC C H N O UNIT 104 104 16 16 ISOR 0.01 0.02 C15 C16 C17 C16A C15A C17A EADP C19B C19 EADP C18 C18A EADP C16A C16 L.S. 10 PLAN 2 TEMP -0.15 BOND $H list 4 conf fmap 2 acta REM REM REM WGHT 0.096200 0.386100 FVAR 0.60788 0.69727 O2 4 0.360058 0.415097 -0.058274 11.00000 0.05279 0.07443 = 0.06117 -0.01947 0.04147 -0.00978 N1 3 0.060360 0.798460 0.107544 11.00000 0.03698 0.04969 = 0.03297 -0.00020 0.02298 0.00186 O1 4 0.463874 0.484802 0.096403 11.00000 0.04528 0.09601 = 0.06486 -0.01449 0.03330 0.01396 N3 3 0.346545 0.688149 0.173372 11.00000 0.05459 0.05770 = 0.05053 0.00439 0.03699 0.01152 O4 4 0.554180 0.590779 0.400816 11.00000 0.08502 0.07956 = 0.06752 0.01213 0.05363 0.02655 N2 3 0.556693 0.695781 0.608265 11.00000 0.06356 0.04903 = 0.03903 0.00089 0.03494 0.00328 C24 1 0.349837 0.570443 0.047531 11.00000 0.04181 0.04391 = 0.04657 0.00415 0.03038 0.00428 C25 1 0.383175 0.619318 0.146045 11.00000 0.03728 0.05210 = 0.04124 0.00154 0.02415 0.00798 AFIX 43 H25 2 0.434075 0.603958 0.196901 11.00000 -1.20000 AFIX 0 O3 4 0.623009 0.501892 0.561370 11.00000 0.12834 0.11641 = 0.06225 0.00990 0.06589 0.04822 C26 1 0.395088 0.484309 0.026812 11.00000 0.04593 0.04775 = 0.05063 -0.00051 0.03608 0.00071 C1 1 0.020557 0.649946 0.058611 11.00000 0.04053 0.05434 = 0.03589 0.00176 0.02566 -0.00285 AFIX 13 H1 2 -0.016651 0.638175 0.067326 11.00000 -1.20000 AFIX 0 C2 1 0.073049 0.512839 0.110071 11.00000 0.05718 0.04885 = 0.03695 0.00077 0.02305 -0.00131 C23 1 0.274549 0.594620 -0.028459 11.00000 0.04622 0.07732 = 0.04340 -0.00648 0.02358 0.00686 AFIX 43 H23 2 0.250002 0.562070 -0.095868 11.00000 -1.20000 AFIX 0 PART 1 N4 3 0.654940 0.307144 0.329528 21.00000 0.05762 0.06346 = 0.03657 -0.00553 0.02549 0.00707 PART 0 PART 2 C19B 1 0.613314 0.358546 0.355480 -21.00000 0.04283 0.04745 = 0.03771 0.00781 0.02316 0.00167 AFIX 43 H19B 2 0.581400 0.436949 0.310247 -21.00000 -1.20000 AFIX 0 PART 0 C9 1 0.546984 0.980853 0.617964 11.00000 0.07688 0.04485 = 0.03907 0.00287 0.02490 0.00087 C21 1 0.273569 0.709815 0.097806 11.00000 0.05390 0.07283 = 0.06714 0.00350 0.04412 0.01831 AFIX 43 H21 2 0.246632 0.755895 0.114457 11.00000 -1.20000 AFIX 0 C8 1 0.539628 0.847128 0.553409 11.00000 0.07092 0.04889 = 0.04387 0.00108 0.03744 -0.00576 AFIX 13 H8 2 0.575532 0.862826 0.542585 11.00000 -1.20000 AFIX 0 C22 1 0.236536 0.667858 -0.002473 11.00000 0.03942 0.09897 = 0.05669 -0.00221 0.02158 0.01837 AFIX 43 H22 2 0.186058 0.688648 -0.052725 11.00000 -1.20000 AFIX 0 C20 1 0.603545 0.505729 0.473173 11.00000 0.06534 0.06133 = 0.04950 -0.00474 0.03761 0.00392 C10 1 0.514419 0.973442 0.662763 11.00000 0.12282 0.05461 = 0.05869 -0.00229 0.05882 0.00725 AFIX 43 H10 2 0.489349 0.883537 0.655269 11.00000 -1.20000 AFIX 0 C7 1 0.139443 0.513556 0.129056 11.00000 0.06588 0.07115 = 0.07980 0.01080 0.04166 0.01909 AFIX 43 H7 2 0.153493 0.602058 0.113754 11.00000 -1.20000 AFIX 0 C5 1 0.165824 0.255360 0.193050 11.00000 0.11078 0.06404 = 0.07094 -0.00440 0.01495 0.02351 AFIX 43 H5 2 0.197047 0.169215 0.221018 11.00000 -1.20000 AFIX 0 PART 1 C18 1 0.645655 0.412391 0.451336 21.00000 0.05293 0.03700 = 0.04045 0.00252 0.02901 0.00026 PART 0 C14 1 0.583974 1.113906 0.630781 11.00000 0.09654 0.06543 = 0.06784 -0.00317 0.03385 -0.01679 AFIX 43 H14 2 0.607081 1.122377 0.602366 11.00000 -1.20000 AFIX 0 C13 1 0.586713 1.239194 0.688053 11.00000 0.11516 0.05164 = 0.07856 -0.00775 0.01945 -0.00514 AFIX 43 H13 2 0.611721 1.329757 0.696439 11.00000 -1.20000 AFIX 0 C12 1 0.554860 1.230398 0.729421 11.00000 0.13717 0.07250 = 0.06023 -0.01347 0.02977 0.02361 AFIX 43 H12 2 0.557023 1.314264 0.766001 11.00000 -1.20000 AFIX 0 C3 1 0.052944 0.380559 0.133408 11.00000 0.09170 0.06337 = 0.05912 0.00528 0.03239 -0.01944 AFIX 43 H3 2 0.008544 0.376911 0.121888 11.00000 -1.20000 AFIX 0 C11 1 0.518225 1.096312 0.718358 11.00000 0.15103 0.07579 = 0.07122 -0.00595 0.06399 0.02673 AFIX 43 H11 2 0.496156 1.088745 0.748277 11.00000 -1.20000 AFIX 0 C4 1 0.101150 0.251253 0.175046 11.00000 0.13837 0.04572 = 0.07016 0.00951 0.03353 -0.00872 AFIX 43 H4 2 0.087904 0.161355 0.190344 11.00000 -1.20000 AFIX 0 C6 1 0.185501 0.385895 0.170250 11.00000 0.08525 0.08831 = 0.09987 0.00386 0.04189 0.03088 AFIX 43 H6 2 0.230194 0.388828 0.182542 11.00000 -1.20000 AFIX 0 PART 1 C17 1 0.708954 0.333611 0.528659 21.00000 0.11125 0.07572 = 0.03728 0.01019 0.03727 0.03949 AFIX 43 H17 2 0.727066 0.340833 0.596231 21.00000 -1.20000 AFIX 0 C15 1 0.715339 0.232530 0.404093 21.00000 0.09694 0.10127 = 0.05196 0.00681 0.04218 0.05205 AFIX 43 H15 2 0.738824 0.169534 0.387973 21.00000 -1.20000 AFIX 0 C16 1 0.745607 0.244332 0.506769 21.00000 0.10809 0.11941 = 0.05691 0.01143 0.03752 0.06785 AFIX 43 H16 2 0.789426 0.193072 0.558921 21.00000 -1.20000 AFIX 0 PART 0 H1A 2 0.028545 0.864635 0.094968 11.00000 0.03867 H2A 2 0.592640 0.708784 0.684207 11.00000 0.05401 H1B 2 0.095105 0.796029 0.181025 11.00000 0.05271 H2B 2 0.569303 0.633181 0.587398 11.00000 0.05569 H2C 2 0.513468 0.650879 0.594585 11.00000 0.07612 H1C 2 0.089691 0.841798 0.085748 11.00000 0.06098 PART 2 N4A 3 0.633171 0.256003 0.317357 -21.00000 0.06456 0.08941 = 0.03556 -0.00875 0.01648 0.02815 C16A 1 0.698350 0.138439 0.485837 -21.00000 0.10809 0.11941 = 0.05691 0.01143 0.03752 0.06785 AFIX 43 H16A 2 0.729839 0.059747 0.531243 -21.00000 -1.20000 AFIX 0 C17A 1 0.677634 0.254345 0.518384 -21.00000 0.07085 0.09661 = 0.06733 0.01329 0.04945 0.03535 AFIX 43 H17A 2 0.694052 0.256027 0.585209 -21.00000 -1.20000 AFIX 0 C18A 1 0.632961 0.364514 0.450173 -21.00000 0.05293 0.03700 = 0.04045 0.00252 0.02901 0.00026 C15A 1 0.672703 0.137892 0.385944 -21.00000 0.10949 0.10455 = 0.08021 -0.00650 0.05808 0.03776 AFIX 43 H15A 2 0.683080 0.051385 0.364104 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C19 1 0.620923 0.394859 0.351929 21.00000 0.04283 0.04745 = 0.03771 0.00781 0.02316 0.00167 AFIX 43 H19 2 0.578199 0.447667 0.298441 21.00000 -1.20000 AFIX 0 HKLF 4 REM 20161229h_0m_a.res in C2 REM wR2 = 0.1742, GooF = S = 1.032, Restrained GooF = 1.053 for all data REM R1 = 0.0596 for 4303 Fo > 4sig(Fo) and 0.0953 for all 6271 data REM 368 parameters refined using 37 restraints END WGHT 0.0962 0.3861 REM Highest difference peak 0.326, deepest hole -0.218, 1-sigma level 0.046 Q1 1 0.7065 -0.0969 0.6035 11.00000 0.05 0.33 Q2 1 0.6920 -0.0921 0.5363 11.00000 0.05 0.31 ; _shelx_res_checksum 48587 _shelx_hkl_file ; 4 0 0 1723.90 31.46 4 0 0 1657.87 31.33 -4 0 0 1683.55 31.49 -4 0 0 1618.88 31.31 6 0 0 645.22 12.93 -6 0 0 643.15 12.91 6 0 0 651.32 13.06 -6 0 0 636.39 13.14 -8 0 0 61.62 2.55 8 0 0 57.84 2.80 -8 0 0 60.31 2.96 -10 0 0 1565.91 31.13 -10 0 0 1630.65 31.68 -12 0 0 249.56 6.90 -12 0 0 248.20 7.30 -14 0 0 13.08 2.31 -14 0 0 11.76 2.50 -16 0 0 6.85 3.46 -16 0 0 8.82 2.34 -18 0 0 16.85 3.79 -18 0 0 20.75 3.23 -20 0 0 0.09 3.91 -20 0 0 0.61 3.15 -22 0 0 -0.25 5.02 -22 0 0 3.09 4.23 -24 0 0 42.46 7.39 3 -1 0 4435.51 82.62 3 -1 0 4558.02 82.77 3 1 0 4431.30 82.77 -5 -1 0 3142.71 59.72 -5 -1 0 3176.73 60.14 5 -1 0 3148.85 59.87 5 -1 0 3332.48 60.07 5 1 0 3209.53 59.81 -5 1 0 3142.72 59.93 -5 1 0 3282.54 60.08 5 1 0 3284.57 60.08 -7 -1 0 410.27 9.45 7 -1 0 425.10 9.23 -7 -1 0 423.96 8.98 -7 1 0 431.68 9.39 7 1 0 418.37 9.28 7 1 0 420.94 9.08 -7 1 0 425.58 9.21 9 -1 0 294.84 7.38 -9 -1 0 297.92 7.65 -9 -1 0 302.94 7.08 -9 1 0 293.20 7.49 -9 1 0 293.96 7.26 -11 -1 0 514.39 11.36 -11 -1 0 510.48 12.04 -11 1 0 505.59 11.85 -11 1 0 508.37 11.64 -13 -1 0 33.61 3.72 -13 -1 0 37.28 3.19 -13 1 0 42.61 3.65 -13 1 0 41.72 3.19 -15 -1 0 37.17 3.47 -15 -1 0 32.61 4.94 -15 1 0 37.00 4.20 -15 1 0 39.52 3.38 -17 -1 0 9.85 3.67 -17 -1 0 5.74 2.20 -17 1 0 6.18 2.49 -19 -1 0 46.37 5.15 -19 -1 0 46.83 6.28 -19 1 0 50.81 6.48 -19 1 0 55.23 5.64 -21 -1 0 -2.85 4.46 -21 -1 0 0.71 3.55 -21 1 0 -2.06 4.14 -21 1 0 -0.93 3.80 -23 -1 0 8.08 5.09 -23 -1 0 8.78 5.63 -23 1 0 -7.19 5.50 -23 1 0 6.77 5.36 0 -2 0 497.04 10.07 0 -2 0 493.52 9.71 0 -2 0 502.05 9.95 0 2 0 474.89 10.01 0 2 0 494.01 9.99 2 -2 0 2396.12 43.47 -2 -2 0 2263.78 43.79 2 -2 0 2398.54 43.59 2 -2 0 2241.76 43.67 -2 -2 0 2386.90 43.71 -2 2 0 2380.17 43.60 2 2 0 2273.16 43.73 2 2 0 2281.39 43.77 -2 2 0 2306.82 43.50 -2 2 0 2361.17 43.74 4 -2 0 1165.67 21.81 -4 -2 0 1094.52 22.14 4 -2 0 1090.35 21.97 -4 -2 0 1174.63 22.04 -4 -2 0 1118.76 21.55 4 -2 0 1112.31 21.77 4 2 0 1164.60 21.71 -4 2 0 1114.75 21.93 -4 2 0 1139.20 21.67 4 2 0 1157.90 22.14 -4 2 0 1121.12 22.02 6 -2 0 473.91 10.58 6 -2 0 499.90 10.73 -6 -2 0 515.57 10.65 -6 -2 0 503.00 10.18 -6 -2 0 487.16 10.87 6 2 0 500.35 10.37 -6 2 0 481.74 10.56 6 2 0 481.02 10.75 -6 2 0 513.47 10.17 -8 -2 0 503.05 11.64 -8 -2 0 510.65 10.83 8 -2 0 517.22 11.47 8 2 0 545.85 11.88 -8 2 0 500.11 11.30 -8 2 0 522.89 10.69 -10 -2 0 24.18 2.91 -10 -2 0 27.55 2.29 -10 2 0 21.94 2.71 -10 2 0 28.00 2.07 -10 2 0 28.17 2.53 -12 -2 0 267.88 7.94 -12 -2 0 264.63 6.96 -12 2 0 257.98 7.49 -12 2 0 260.38 6.45 -12 2 0 264.09 7.59 -14 -2 0 17.97 2.75 -14 2 0 25.92 3.29 -14 2 0 18.70 3.01 -14 2 0 21.64 2.55 -16 -2 0 26.76 3.99 -16 -2 0 21.64 3.45 -16 2 0 32.11 5.06 -16 2 0 26.61 4.08 -16 2 0 28.77 2.96 -18 -2 0 29.35 4.44 -18 2 0 34.76 5.68 -18 2 0 24.29 3.45 -20 -2 0 7.45 3.45 -20 -2 0 3.64 4.39 -20 2 0 12.66 4.00 -20 2 0 12.18 4.09 -22 -2 0 12.61 4.33 -22 -2 0 5.15 5.24 -22 2 0 10.53 5.28 1 -3 0 32.76 2.18 -1 -3 0 29.36 1.75 -1 -3 0 29.83 2.13 1 -3 0 26.32 1.91 1 -3 0 29.35 1.66 -1 -3 0 27.22 1.96 1 3 0 27.89 2.15 -1 3 0 25.60 1.95 -1 3 0 32.28 2.18 1 3 0 29.01 2.28 -1 3 0 29.30 2.09 3 -3 0 522.80 10.64 -3 -3 0 511.23 11.20 3 -3 0 510.37 11.06 3 -3 0 517.94 10.88 -3 3 0 521.75 10.93 3 3 0 519.09 11.26 -3 3 0 513.51 10.76 -3 3 0 510.49 11.12 -5 -3 0 235.80 5.54 5 -3 0 238.25 6.01 5 -3 0 250.43 6.22 -5 -3 0 243.89 6.43 -5 3 0 244.01 6.34 -5 3 0 235.33 6.13 -5 3 0 238.09 5.73 -7 -3 0 803.32 15.95 7 -3 0 791.01 16.65 -7 -3 0 792.76 16.99 -7 3 0 781.33 16.66 7 3 0 807.84 16.32 -7 3 0 819.73 16.05 9 -3 0 316.80 8.14 -9 -3 0 320.56 7.44 -9 -3 0 310.61 9.30 -9 3 0 328.24 7.34 -9 3 0 317.91 8.23 -11 -3 0 94.65 4.98 -11 -3 0 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6.50 12 -4 -19 19.47 5.47 -12 4 19 13.04 3.47 10 -4 -19 11.58 5.83 -10 -4 19 15.54 7.28 -10 4 19 15.01 3.33 8 -4 -19 14.54 7.12 -8 -4 19 12.30 8.72 -8 4 19 12.81 3.06 -23 -5 19 13.08 5.67 -23 -5 19 12.60 7.41 -23 5 19 7.16 4.05 -23 5 19 4.33 3.75 -21 -5 19 -1.70 5.37 -21 -5 19 3.79 8.84 -19 -5 19 12.87 5.55 -19 -5 19 10.86 9.19 -17 -5 19 15.07 8.17 17 -5 -19 6.98 4.71 -17 5 19 9.81 3.97 -15 -5 19 -0.42 6.67 15 -5 -19 3.85 4.67 -15 5 19 5.99 3.64 13 -5 -19 11.89 5.35 -13 -5 19 1.02 6.82 -13 5 19 6.08 3.70 11 -5 -19 -1.37 5.84 -11 5 19 0.51 3.27 -20 -6 19 4.91 6.19 -20 6 19 9.78 5.06 -18 -6 19 12.95 7.05 -18 6 19 3.72 4.93 16 -6 -19 4.28 5.14 -16 -6 19 -14.34 6.79 -16 6 19 4.56 4.88 -14 -6 19 21.88 13.63 14 -6 -19 6.95 5.84 -26 0 20 3.93 4.96 -24 0 20 -1.08 4.25 -22 0 20 2.58 4.08 -22 0 20 11.70 5.54 -20 0 20 -2.83 3.70 -20 0 20 0.18 3.81 -18 0 20 14.06 4.75 -16 0 20 24.67 4.77 -16 0 20 26.82 5.37 -14 0 20 14.34 5.80 12 0 -20 6.59 5.42 -12 0 20 12.51 3.60 10 0 -20 0.15 6.10 -10 0 20 2.46 3.23 8 0 -20 18.64 7.26 -27 -1 20 8.20 7.09 -27 1 20 8.78 4.77 -25 -1 20 4.19 5.47 -25 1 20 -1.36 5.00 -23 -1 20 2.97 4.38 -23 1 20 0.75 6.10 -21 -1 20 -2.69 3.71 -21 -1 20 4.47 4.26 -21 1 20 4.43 3.89 -21 1 20 1.58 4.37 -19 -1 20 8.93 4.59 -19 -1 20 3.16 4.15 -19 1 20 6.05 3.88 -19 1 20 1.41 4.18 -17 -1 20 1.38 4.03 -17 -1 20 -3.54 4.40 -17 1 20 7.27 3.88 -17 1 20 0.88 2.96 -17 1 20 5.22 4.75 -15 -1 20 11.86 5.19 15 -1 -20 5.33 4.72 -15 1 20 6.35 4.51 -15 1 20 11.02 4.22 13 -1 -20 36.22 6.13 -13 -1 20 32.79 7.28 -13 1 20 27.91 4.84 11 -1 -20 26.28 6.22 -11 -1 20 15.14 3.62 -11 -1 20 35.60 7.15 -11 1 20 21.76 3.46 -9 -1 20 6.95 8.14 9 -1 -20 21.33 6.29 -9 1 20 5.84 3.28 7 -1 -20 -3.81 8.05 -28 -2 20 3.31 7.08 -28 2 20 13.05 5.90 -26 -2 20 21.95 10.58 -26 2 20 1.24 4.69 -24 -2 20 10.42 5.70 -24 2 20 3.84 3.75 -22 -2 20 8.10 5.22 -22 -2 20 3.22 3.97 -22 2 20 5.10 3.40 -22 2 20 11.66 3.82 -20 -2 20 7.28 4.64 -20 -2 20 15.81 5.01 -20 2 20 14.49 3.95 -20 2 20 6.06 3.11 -20 2 20 24.95 4.63 -18 -2 20 35.55 5.02 -18 -2 20 34.84 5.48 18 -2 -20 28.35 4.68 -18 2 20 36.82 5.96 16 -2 -20 11.53 5.41 -16 -2 20 2.57 5.19 -16 2 20 3.65 3.93 -16 2 20 -0.32 2.92 14 -2 -20 8.09 4.96 -14 -2 20 8.19 9.74 -14 2 20 23.41 4.50 -14 2 20 14.61 3.39 12 -2 -20 13.56 5.57 -12 -2 20 11.19 6.84 -12 2 20 5.93 3.00 -12 2 20 11.39 4.75 10 -2 -20 7.51 6.39 -10 -2 20 5.30 7.81 -10 2 20 9.80 5.13 -10 2 20 5.25 2.99 8 -2 -20 -4.67 7.24 -8 -2 20 6.88 8.85 -8 2 20 1.01 3.99 -27 3 20 6.04 4.87 -25 3 20 6.15 4.50 -25 3 20 10.31 4.58 -23 -3 20 5.65 4.59 -23 -3 20 14.35 5.99 -23 3 20 9.07 3.90 -23 3 20 10.59 7.26 -21 -3 20 6.86 5.97 -21 -3 20 -2.47 4.19 -21 3 20 5.64 3.30 -21 3 20 4.85 3.51 -19 -3 20 23.20 5.11 -19 -3 20 27.16 5.67 19 -3 -20 11.19 4.44 -19 3 20 16.41 3.57 17 -3 -20 54.62 7.37 -17 -3 20 41.99 6.27 -17 3 20 37.94 6.19 15 -3 -20 -1.19 4.89 -15 3 20 -4.87 3.21 -15 3 20 -0.81 4.24 13 -3 -20 25.74 5.92 -13 -3 20 21.56 6.88 -11 -3 20 -2.69 7.06 11 -3 -20 4.26 6.01 -11 3 20 7.20 3.30 -9 -3 20 14.60 8.01 9 -3 -20 1.62 6.69 -9 3 20 7.18 3.24 -24 -4 20 8.77 5.34 -24 -4 20 15.33 8.03 -24 4 20 5.87 3.97 -24 4 20 3.00 4.22 -22 -4 20 7.28 5.23 -22 -4 20 -0.25 11.59 -22 4 20 -2.72 3.77 -20 -4 20 4.08 6.85 -20 -4 20 1.89 5.49 -20 4 20 1.57 3.94 -20 4 20 3.17 3.38 -18 -4 20 2.70 5.66 18 -4 -20 -2.25 4.71 -18 4 20 -0.21 3.92 16 -4 -20 4.76 5.08 -16 -4 20 16.82 7.86 -16 4 20 5.65 3.76 14 -4 -20 10.23 5.49 -14 -4 20 -9.10 7.12 -14 4 20 3.04 5.25 12 -4 -20 8.26 6.54 -12 -4 20 -5.32 8.50 -12 4 20 -1.82 3.38 -21 -5 20 0.11 5.89 -21 -5 20 3.58 6.78 -21 5 20 -9.96 4.93 -19 -5 20 4.50 6.11 -19 -5 20 4.25 6.31 -19 5 20 -4.53 4.66 17 -5 -20 11.62 5.38 -17 -5 20 8.70 7.21 15 -5 -20 12.41 5.73 -15 -5 20 15.80 8.96 -15 5 20 11.58 5.15 -26 0 21 -4.05 5.19 -24 0 21 -7.39 4.71 -22 0 21 -1.55 5.01 -20 0 21 -1.12 4.65 -20 0 21 4.10 4.62 -18 0 21 -2.62 4.99 -18 0 21 2.82 4.23 -16 0 21 29.69 6.37 -16 0 21 20.96 4.87 -16 0 21 22.28 3.90 -14 0 21 1.87 3.51 -14 0 21 7.18 6.92 -12 0 21 2.52 3.43 -27 -1 21 2.70 7.34 -25 -1 21 1.87 5.63 -25 1 21 11.55 4.45 -23 -1 21 7.07 5.20 -23 1 21 6.60 4.12 -21 -1 21 16.79 5.16 -21 -1 21 7.41 4.66 -21 1 21 15.29 4.37 -19 -1 21 33.15 5.33 -19 -1 21 31.45 5.71 -19 1 21 35.05 5.84 -19 1 21 35.19 4.82 -17 -1 21 16.91 5.99 -17 -1 21 19.13 6.07 -17 1 21 21.50 6.11 -17 1 21 8.27 4.46 15 -1 -21 -1.41 5.67 -15 -1 21 18.66 6.52 -15 1 21 8.64 6.36 -15 1 21 4.62 3.26 -13 -1 21 11.82 3.76 13 -1 -21 9.45 6.14 -13 1 21 19.74 5.22 -13 1 21 11.34 3.61 11 -1 -21 -2.19 7.30 -11 -1 21 0.77 8.88 -11 1 21 -3.35 3.36 -26 -2 21 18.20 6.98 -26 2 21 7.18 4.17 -24 -2 21 20.51 10.66 -24 2 21 10.64 3.99 -22 -2 21 5.80 5.74 -22 -2 21 7.19 4.74 -22 2 21 4.71 3.92 -22 2 21 5.27 3.53 -20 -2 21 4.39 4.31 -20 -2 21 1.98 5.20 -20 2 21 1.19 6.78 -20 2 21 1.45 3.25 -20 2 21 -0.31 4.46 -18 -2 21 14.49 6.06 -18 -2 21 15.72 5.22 -18 2 21 10.58 4.09 -18 2 21 7.39 3.43 -16 -2 21 8.31 6.57 16 -2 -21 14.88 5.45 -16 2 21 10.79 3.94 -16 2 21 14.25 5.22 -14 -2 21 -5.07 8.77 14 -2 -21 14.25 6.26 -14 2 21 -1.33 3.18 -14 2 21 2.83 4.79 12 -2 -21 19.04 6.50 -12 -2 21 3.71 8.06 -12 2 21 3.31 3.16 -23 -3 21 14.27 8.19 -23 -3 21 9.36 5.30 -23 3 21 5.28 3.90 -23 3 21 4.30 3.85 -21 -3 21 -8.30 5.03 -21 3 21 3.49 4.72 -21 3 21 0.28 3.94 19 -3 -21 0.54 5.00 -19 -3 21 10.94 6.06 -19 -3 21 10.62 6.00 -19 3 21 -0.03 4.23 -19 3 21 0.35 3.23 17 -3 -21 10.36 4.96 -17 -3 21 22.39 6.89 -17 3 21 7.56 6.00 -17 3 21 3.08 3.22 15 -3 -21 13.44 5.82 -15 -3 21 0.29 7.45 -15 3 21 3.97 3.57 -13 -3 21 11.09 9.24 13 -3 -21 11.28 6.53 -13 3 21 11.20 3.51 -20 -4 21 29.37 6.87 -20 -4 21 29.52 6.52 -20 4 21 17.89 4.33 18 -4 -21 9.29 5.58 -18 -4 21 9.82 7.25 -24 0 22 2.65 6.72 -22 0 22 23.95 5.40 -20 0 22 1.29 4.64 -20 0 22 11.09 5.65 -18 0 22 27.83 5.27 -18 0 22 21.84 6.70 -16 0 22 0.06 5.02 -16 0 22 16.50 7.10 -16 0 22 -0.14 3.66 -23 -1 22 27.12 6.81 -23 1 22 12.00 4.66 -21 -1 22 5.12 5.53 -21 -1 22 12.02 5.51 -21 1 22 11.55 3.94 -21 1 22 9.12 4.49 -19 -1 22 15.84 6.23 -19 1 22 10.59 4.70 -19 1 22 18.02 6.26 -17 -1 22 13.17 6.87 -17 -1 22 14.38 5.45 -17 1 22 -0.10 3.81 -17 1 22 9.15 4.85 -17 1 22 7.97 6.66 -15 -1 22 4.50 3.83 -15 -1 22 11.11 7.80 -15 1 22 5.75 3.70 -22 -2 22 -5.66 5.54 -22 2 22 5.59 4.82 -22 2 22 -4.75 4.17 -20 -2 22 11.05 8.52 -20 -2 22 -0.33 5.87 -20 2 22 -0.49 4.29 -20 2 22 5.54 4.40 -18 -2 22 2.34 6.27 -18 -2 22 19.32 7.44 -18 2 22 -0.88 3.58 -18 2 22 1.78 4.86 0 0 0 0.00 0.00 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.7143 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71078 23.486 8.620 16.905 90.000 130.007 89.970 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 16276 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -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 O2 O 0.36006(14) 0.4151(3) -0.0583(2) 0.0592(7) Uani 1 1 d . . . . . N1 N 0.06036(16) 0.7985(3) 0.1075(2) 0.0395(6) Uani 1 1 d . . . . . O1 O 0.46387(13) 0.4848(4) 0.0964(2) 0.0702(8) Uani 1 1 d . . . . . N3 N 0.34655(16) 0.6881(4) 0.1734(2) 0.0519(7) Uani 1 1 d . . . . . O4 O 0.55418(17) 0.5908(4) 0.4008(2) 0.0740(8) Uani 1 1 d . . . . . N2 N 0.5567(2) 0.6958(4) 0.6083(2) 0.0491(7) Uani 1 1 d . . . . . C24 C 0.34984(17) 0.5704(4) 0.0475(3) 0.0426(7) Uani 1 1 d . . . . . C25 C 0.38318(17) 0.6193(4) 0.1460(2) 0.0443(7) Uani 1 1 d . . . . . H25 H 0.434075 0.603958 0.196901 0.053 Uiso 1 1 calc R . . . . O3 O 0.6230(2) 0.5019(5) 0.5614(2) 0.0989(12) Uani 1 1 d . . . . . C26 C 0.39509(18) 0.4843(4) 0.0268(3) 0.0444(7) Uani 1 1 d . . . . . C1 C 0.02056(17) 0.6499(4) 0.0586(2) 0.0428(7) Uani 1 1 d . . . . . H1 H -0.016651 0.638175 0.067326 0.051 Uiso 1 1 calc R . . . . C2 C 0.0730(2) 0.5128(4) 0.1101(3) 0.0529(9) Uani 1 1 d . . . . . C23 C 0.2745(2) 0.5946(5) -0.0285(3) 0.0594(10) Uani 1 1 d . . . . . H23 H 0.250002 0.562070 -0.095868 0.071 Uiso 1 1 calc R . . . . N4 N 0.6549(6) 0.3071(12) 0.3295(8) 0.056(2) Uani 0.697(9) 1 d . . P A 1 C19B C 0.613(2) 0.359(4) 0.355(3) 0.0446(19) Uani 0.303(9) 1 d . . P A 2 H19B H 0.581400 0.436949 0.310247 0.054 Uiso 0.303(9) 1 calc R . P A 2 C9 C 0.5470(2) 0.9809(5) 0.6180(3) 0.0626(10) Uani 1 1 d . . . . . C21 C 0.2736(2) 0.7098(5) 0.0978(3) 0.0608(10) Uani 1 1 d . . . . . H21 H 0.246632 0.755895 0.114457 0.073 Uiso 1 1 calc R . . . . C8 C 0.5396(2) 0.8471(4) 0.5534(3) 0.0541(8) Uani 1 1 d . . . . . H8 H 0.575532 0.862826 0.542585 0.065 Uiso 1 1 calc R . . . . C22 C 0.2365(2) 0.6679(6) -0.0025(3) 0.0718(12) Uani 1 1 d . . . . . H22 H 0.186058 0.688648 -0.052725 0.086 Uiso 1 1 calc R . . . . C20 C 0.6035(2) 0.5057(5) 0.4732(3) 0.0582(9) Uani 1 1 d . . . . . C10 C 0.5144(3) 0.9734(5) 0.6628(3) 0.0783(13) Uani 1 1 d . . . . . H10 H 0.489349 0.883537 0.655269 0.094 Uiso 1 1 calc R . . . . C7 C 0.1394(2) 0.5136(6) 0.1291(4) 0.0760(12) Uani 1 1 d . . . . . H7 H 0.153493 0.602058 0.113754 0.091 Uiso 1 1 calc R . . . . C5 C 0.1658(4) 0.2554(8) 0.1931(4) 0.114(2) Uani 1 1 d . . . . . H5 H 0.197047 0.169215 0.221018 0.136 Uiso 1 1 calc R . . . . C18 C 0.6457(5) 0.4124(8) 0.4513(6) 0.0442(14) Uani 0.697(9) 1 d . . P A 1 C14 C 0.5840(3) 1.1139(6) 0.6308(4) 0.0904(16) Uani 1 1 d . . . . . H14 H 0.607081 1.122377 0.602366 0.108 Uiso 1 1 calc R . . . . C13 C 0.5867(4) 1.2392(7) 0.6881(5) 0.113(2) Uani 1 1 d . . . . . H13 H 0.611721 1.329757 0.696439 0.136 Uiso 1 1 calc R . . . . C12 C 0.5549(4) 1.2304(8) 0.7294(4) 0.114(3) Uani 1 1 d . . . . . H12 H 0.557023 1.314264 0.766001 0.137 Uiso 1 1 calc R . . . . C3 C 0.0529(3) 0.3806(6) 0.1334(4) 0.0831(14) Uani 1 1 d . . . . . H3 H 0.008544 0.376911 0.121888 0.100 Uiso 1 1 calc R . . . . C11 C 0.5182(4) 1.0963(7) 0.7184(4) 0.105(2) Uani 1 1 d . . . . . H11 H 0.496156 1.088745 0.748277 0.126 Uiso 1 1 calc R . . . . C4 C 0.1012(5) 0.2513(6) 0.1750(4) 0.109(2) Uani 1 1 d . . . . . H4 H 0.087904 0.161355 0.190344 0.131 Uiso 1 1 calc R . . . . C6 C 0.1855(3) 0.3859(8) 0.1702(5) 0.1039(19) Uani 1 1 d . . . . . H6 H 0.230194 0.388828 0.182542 0.125 Uiso 1 1 calc R . . . . C17 C 0.7090(6) 0.3336(10) 0.5287(5) 0.082(3) Uani 0.697(9) 1 d . U P A 1 H17 H 0.727066 0.340833 0.596231 0.099 Uiso 0.697(9) 1 calc R . P A 1 C15 C 0.7153(5) 0.2325(11) 0.4041(5) 0.087(3) Uani 0.697(9) 1 d . U P A 1 H15 H 0.738824 0.169534 0.387973 0.105 Uiso 0.697(9) 1 calc R . P A 1 C16 C 0.7456(6) 0.2443(13) 0.5068(6) 0.106(3) Uani 0.697(9) 1 d . U P A 1 H16 H 0.789426 0.193072 0.558921 0.127 Uiso 0.697(9) 1 calc R . P A 1 H1A H 0.029(2) 0.865(4) 0.095(3) 0.039(9) Uiso 1 1 d . . . . . H2A H 0.593(2) 0.709(5) 0.684(3) 0.054(10) Uiso 1 1 d . . . . . H1B H 0.095(2) 0.796(5) 0.181(3) 0.053(10) Uiso 1 1 d . . . . . H2B H 0.569(2) 0.633(5) 0.587(3) 0.056(11) Uiso 1 1 d . . . . . H2C H 0.513(3) 0.651(6) 0.595(3) 0.076(14) Uiso 1 1 d . . . . . H1C H 0.090(2) 0.842(5) 0.086(3) 0.061(11) Uiso 1 1 d . . . . . N4A N 0.6332(14) 0.256(3) 0.317(2) 0.075(7) Uani 0.303(9) 1 d . . P A 2 C16A C 0.6984(12) 0.138(3) 0.4858(13) 0.106(3) Uani 0.303(9) 1 d . U P A 2 H16A H 0.729839 0.059747 0.531243 0.127 Uiso 0.303(9) 1 calc R . P A 2 C17A C 0.6776(10) 0.254(3) 0.5184(14) 0.075(5) Uani 0.303(9) 1 d . U P A 2 H17A H 0.694052 0.256027 0.585209 0.089 Uiso 0.303(9) 1 calc R . P A 2 C18A C 0.6330(13) 0.365(2) 0.4502(17) 0.0442(14) Uani 0.303(9) 1 d . . P A 2 C15A C 0.6727(13) 0.138(3) 0.3859(15) 0.100(6) Uani 0.303(9) 1 d . U P A 2 H15A H 0.683080 0.051385 0.364104 0.120 Uiso 0.303(9) 1 calc R . P A 2 C19 C 0.6209(8) 0.3949(13) 0.3519(11) 0.0446(19) Uani 0.697(9) 1 d . . P A 1 H19 H 0.578199 0.447667 0.298441 0.054 Uiso 0.697(9) 1 calc R . P A 1 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 O2 0.0528(14) 0.0744(17) 0.0612(15) -0.0195(13) 0.0415(13) -0.0098(12) N1 0.0370(13) 0.0497(17) 0.0330(14) -0.0002(11) 0.0230(12) 0.0019(12) O1 0.0453(13) 0.096(2) 0.0649(16) -0.0145(16) 0.0333(13) 0.0140(14) N3 0.0546(16) 0.0577(18) 0.0505(15) 0.0044(14) 0.0370(14) 0.0115(14) O4 0.0850(19) 0.0796(19) 0.0675(18) 0.0121(15) 0.0536(16) 0.0266(17) N2 0.0636(19) 0.0490(18) 0.0390(16) 0.0009(13) 0.0349(16) 0.0033(14) C24 0.0418(16) 0.0439(17) 0.0466(18) 0.0042(14) 0.0304(15) 0.0043(14) C25 0.0373(15) 0.052(2) 0.0412(17) 0.0015(14) 0.0242(14) 0.0080(14) O3 0.128(3) 0.116(3) 0.0622(18) 0.0099(19) 0.0659(19) 0.048(2) C26 0.0459(17) 0.0477(18) 0.0506(19) -0.0005(16) 0.0361(16) 0.0007(14) C1 0.0405(15) 0.0543(19) 0.0359(15) 0.0018(14) 0.0257(13) -0.0028(14) C2 0.057(2) 0.049(2) 0.0370(17) 0.0008(15) 0.0231(16) -0.0013(16) C23 0.0462(18) 0.077(3) 0.0434(18) -0.0065(18) 0.0236(15) 0.0069(18) N4 0.058(5) 0.063(5) 0.037(4) -0.006(3) 0.025(4) 0.007(3) C19B 0.043(4) 0.047(6) 0.038(2) 0.008(4) 0.023(2) 0.002(4) C9 0.077(3) 0.045(2) 0.0391(18) 0.0029(15) 0.0249(18) 0.0009(18) C21 0.054(2) 0.073(3) 0.067(2) 0.003(2) 0.0441(19) 0.0183(18) C8 0.071(2) 0.049(2) 0.0439(17) 0.0011(15) 0.0374(17) -0.0058(17) C22 0.0394(18) 0.099(3) 0.057(2) -0.002(2) 0.0216(17) 0.018(2) C20 0.065(2) 0.061(2) 0.050(2) -0.0047(19) 0.0376(19) 0.004(2) C10 0.123(4) 0.055(2) 0.059(2) -0.002(2) 0.059(3) 0.007(2) C7 0.066(2) 0.071(3) 0.080(3) 0.011(2) 0.042(2) 0.019(2) C5 0.111(5) 0.064(3) 0.071(3) -0.004(3) 0.015(3) 0.024(3) C18 0.053(4) 0.037(4) 0.0405(19) 0.003(3) 0.029(2) 0.000(3) C14 0.097(3) 0.065(3) 0.068(3) -0.003(2) 0.034(3) -0.017(3) C13 0.115(5) 0.052(3) 0.079(4) -0.008(3) 0.019(4) -0.005(3) C12 0.137(6) 0.072(4) 0.060(3) -0.013(3) 0.030(3) 0.024(4) C3 0.092(3) 0.063(3) 0.059(3) 0.005(2) 0.032(2) -0.019(2) C11 0.151(5) 0.076(4) 0.071(3) -0.006(3) 0.064(3) 0.027(4) C4 0.138(5) 0.046(3) 0.070(3) 0.010(2) 0.034(4) -0.009(3) C6 0.085(3) 0.088(4) 0.100(4) 0.004(3) 0.042(3) 0.031(3) C17 0.111(6) 0.076(5) 0.037(3) 0.010(3) 0.037(4) 0.039(4) C15 0.097(5) 0.101(6) 0.052(3) 0.007(4) 0.042(4) 0.052(5) C16 0.108(5) 0.119(6) 0.057(3) 0.011(4) 0.038(4) 0.068(4) N4A 0.065(14) 0.089(18) 0.036(7) -0.009(10) 0.016(9) 0.028(10) C16A 0.108(5) 0.119(6) 0.057(3) 0.011(4) 0.038(4) 0.068(4) C17A 0.071(8) 0.097(11) 0.067(8) 0.013(8) 0.049(7) 0.035(7) C18A 0.053(4) 0.037(4) 0.0405(19) 0.003(3) 0.029(2) 0.000(3) C15A 0.109(11) 0.105(11) 0.080(9) -0.007(8) 0.058(8) 0.038(9) C19 0.043(4) 0.047(6) 0.038(2) 0.008(4) 0.023(2) 0.002(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 N1 H1A 107(2) . . C1 N1 H1B 114(2) . . C1 N1 H1C 116(2) . . H1A N1 H1B 103(3) . . H1A N1 H1C 110(3) . . H1B N1 H1C 105(3) . . C21 N3 C25 116.2(3) . . C8 N2 H2A 112(2) . . C8 N2 H2B 110(3) . . C8 N2 H2C 112(3) . . H2A N2 H2B 114(4) . . H2A N2 H2C 104(3) . . H2B N2 H2C 105(4) . . C25 C24 C26 119.6(3) . . C25 C24 C23 118.3(3) . . C23 C24 C26 122.0(3) . . N3 C25 C24 123.9(3) . . N3 C25 H25 118.0 . . C24 C25 H25 118.0 . . O2 C26 C24 117.2(3) . . O1 C26 O2 125.5(3) . . O1 C26 C24 117.3(3) . . N1 C1 C1 111.42(18) . 2 N1 C1 H1 108.0 . . N1 C1 C2 111.2(2) . . C1 C1 H1 108.0 2 . C2 C1 C1 110.1(2) . 2 C2 C1 H1 108.0 . . C7 C2 C1 120.9(4) . . C7 C2 C3 118.7(4) . . C3 C2 C1 120.3(4) . . C24 C23 H23 120.7 . . C22 C23 C24 118.6(3) . . C22 C23 H23 120.7 . . C15 N4 C19 119.0(11) . . N4A C19B H19B 115.3 . . N4A C19B C18A 129(3) . . C18A C19B H19B 115.3 . . C10 C9 C8 120.8(4) . . C14 C9 C8 121.1(4) . . C14 C9 C10 118.1(4) . . N3 C21 H21 118.3 . . N3 C21 C22 123.5(3) . . C22 C21 H21 118.3 . . N2 C8 C9 110.7(3) . . N2 C8 C8 111.4(2) . 2_656 N2 C8 H8 108.4 . . C9 C8 C8 109.5(3) . 2_656 C9 C8 H8 108.4 . . C8 C8 H8 108.4 2_656 . C23 C22 H22 120.3 . . C21 C22 C23 119.4(3) . . C21 C22 H22 120.3 . . O4 C20 O3 125.7(4) . . O4 C20 C18 114.8(4) . . O4 C20 C18A 119.5(9) . . O3 C20 C18 119.3(5) . . O3 C20 C18A 113.3(9) . . C9 C10 H10 119.3 . . C11 C10 C9 121.5(5) . . C11 C10 H10 119.3 . . C2 C7 H7 119.4 . . C2 C7 C6 121.3(5) . . C6 C7 H7 119.4 . . C4 C5 H5 120.1 . . C4 C5 C6 119.8(5) . . C6 C5 H5 120.1 . . C17 C18 C20 121.0(7) . . C17 C18 C19 117.0(9) . . C19 C18 C20 121.9(9) . . C9 C14 H14 120.4 . . C9 C14 C13 119.3(6) . . C13 C14 H14 120.4 . . C14 C13 H13 119.1 . . C12 C13 C14 121.7(6) . . C12 C13 H13 119.1 . . C13 C12 H12 120.2 . . C13 C12 C11 119.7(6) . . C11 C12 H12 120.2 . . C2 C3 H3 120.7 . . C2 C3 C4 118.7(6) . . C4 C3 H3 120.7 . . C10 C11 H11 120.1 . . C12 C11 C10 119.7(6) . . C12 C11 H11 120.1 . . C5 C4 C3 121.3(6) . . C5 C4 H4 119.3 . . C3 C4 H4 119.3 . . C7 C6 H6 119.9 . . C5 C6 C7 120.2(6) . . C5 C6 H6 119.9 . . C18 C17 H17 119.9 . . C16 C17 C18 120.3(7) . . C16 C17 H17 119.9 . . N4 C15 H15 118.9 . . N4 C15 C16 122.2(8) . . C16 C15 H15 118.9 . . C17 C16 C15 118.1(6) . . C17 C16 H16 121.0 . . C15 C16 H16 121.0 . . C19B N4A C15A 110(3) . . C17A C16A H16A 119.8 . . C17A C16A C15A 120.3(17) . . C15A C16A H16A 119.8 . . C16A C17A H17A 121.4 . . C18A C17A C16A 117.1(17) . . C18A C17A H17A 121.4 . . C19B C18A C20 117(2) . . C17A C18A C19B 119(2) . . C17A C18A C20 124.4(18) . . N4A C15A C16A 124(2) . . N4A C15A H15A 117.9 . . C16A C15A H15A 117.9 . . N4 C19 C18 123.3(12) . . N4 C19 H19 118.3 . . C18 C19 H19 118.3 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O2 C26 1.257(4) . N1 C1 1.482(4) . N1 H1A 0.85(4) . N1 H1B 0.95(4) . N1 H1C 1.04(4) . O1 C26 1.246(4) . N3 C25 1.347(4) . N3 C21 1.338(5) . O4 C20 1.246(5) . N2 C8 1.496(5) . N2 H2A 0.99(4) . N2 H2B 0.80(5) . N2 H2C 0.97(5) . C24 C25 1.374(5) . C24 C26 1.509(4) . C24 C23 1.379(5) . C25 H25 0.9300 . O3 C20 1.248(5) . C1 C1 1.549(6) 2 C1 H1 0.9800 . C1 C2 1.513(5) . C2 C7 1.375(6) . C2 C3 1.383(6) . C23 H23 0.9300 . C23 C22 1.375(6) . N4 C15 1.310(13) . N4 C19 1.32(2) . C19B H19B 0.9300 . C19B N4A 1.34(5) . C19B C18A 1.35(5) . C9 C8 1.517(6) . C9 C10 1.380(7) . C9 C14 1.367(7) . C21 H21 0.9300 . C21 C22 1.366(6) . C8 C8 1.551(8) 2_656 C8 H8 0.9800 . C22 H22 0.9300 . C20 C18 1.492(9) . C20 C18A 1.56(2) . C10 H10 0.9300 . C10 C11 1.378(7) . C7 H7 0.9300 . C7 C6 1.376(7) . C5 H5 0.9300 . C5 C4 1.344(10) . C5 C6 1.361(11) . C18 C17 1.371(11) . C18 C19 1.389(17) . C14 H14 0.9300 . C14 C13 1.422(9) . C13 H13 0.9300 . C13 C12 1.314(11) . C12 H12 0.9300 . C12 C11 1.378(10) . C3 H3 0.9300 . C3 C4 1.411(9) . C11 H11 0.9300 . C4 H4 0.9300 . C6 H6 0.9300 . C17 H17 0.9300 . C17 C16 1.370(11) . C15 H15 0.9300 . C15 C16 1.394(10) . C16 H16 0.9300 . N4A C15A 1.36(4) . C16A H16A 0.9300 . C16A C17A 1.37(2) . C16A C15A 1.38(3) . C17A H17A 0.9300 . C17A C18A 1.33(3) . C15A H15A 0.9300 . C19 H19 0.9300 . 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_4 N1 C1 C2 C7 -48.1(4) . . N1 C1 C2 C3 135.7(4) . . N3 C21 C22 C23 2.3(8) . . O4 C20 C18 C17 169.3(7) . . O4 C20 C18 C19 -13.9(8) . . O4 C20 C18A C19B 12(2) . . O4 C20 C18A C17A -170.3(16) . . C24 C23 C22 C21 -2.1(7) . . C25 N3 C21 C22 -0.8(6) . . C25 C24 C26 O2 166.1(3) . . C25 C24 C26 O1 -12.3(5) . . C25 C24 C23 C22 0.7(6) . . O3 C20 C18 C17 -5.7(9) . . O3 C20 C18 C19 171.1(6) . . O3 C20 C18A C19B 179.0(17) . . O3 C20 C18A C17A -3(2) . . C26 C24 C25 N3 -175.7(3) . . C26 C24 C23 C22 177.1(4) . . C1 C1 C2 C7 75.9(4) 2 . C1 C1 C2 C3 -100.3(4) 2 . C1 C2 C7 C6 -176.1(4) . . C1 C2 C3 C4 175.8(4) . . C2 C7 C6 C5 0.0(9) . . C2 C3 C4 C5 0.7(8) . . C23 C24 C25 N3 0.8(6) . . C23 C24 C26 O2 -10.2(5) . . C23 C24 C26 O1 171.4(4) . . N4 C15 C16 C17 2.1(18) . . C19B N4A C15A C16A -10(4) . . C9 C10 C11 C12 0.4(8) . . C9 C14 C13 C12 0.3(9) . . C21 N3 C25 C24 -0.8(5) . . C8 C9 C10 C11 -177.5(4) . . C8 C9 C14 C13 177.2(4) . . C20 C18 C17 C16 177.8(9) . . C20 C18 C19 N4 -176.6(7) . . C10 C9 C8 N2 -47.9(5) . . C10 C9 C8 C8 75.3(5) . 2_656 C10 C9 C14 C13 -0.8(7) . . C7 C2 C3 C4 -0.5(7) . . C18 C17 C16 C15 -2.0(17) . . C14 C9 C8 N2 134.1(4) . . C14 C9 C8 C8 -102.7(5) . 2_656 C14 C9 C10 C11 0.5(7) . . C14 C13 C12 C11 0.6(10) . . C13 C12 C11 C10 -0.9(9) . . C3 C2 C7 C6 0.1(7) . . C4 C5 C6 C7 0.1(10) . . C6 C5 C4 C3 -0.5(10) . . C17 C18 C19 N4 0.3(11) . . C15 N4 C19 C18 -0.3(13) . . N4A C19B C18A C20 177(2) . . N4A C19B C18A C17A -1(4) . . C16A C17A C18A C19B -2(3) . . C16A C17A C18A C20 -180.0(19) . . C17A C16A C15A N4A 7(4) . . C18A C19B N4A C15A 7(4) . . C15A C16A C17A C18A -1(4) . . C19 N4 C15 C16 -0.9(16) . . C19 C18 C17 C16 0.9(14) . . _cod_database_fobs_code 2108385