#------------------------------------------------------------------------------ #$Date: 2024-11-27 01:34:49 +0200 (Wed, 27 Nov 2024) $ #$Revision: 296127 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249641.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_7249641 loop_ _publ_author_name 'Kenguva, Gowtham' 'Rekha Rout, Smruti' 'Shaikh, Tabrez R.' 'Baidya, Debjani' 'Shelke, Nikita' 'Sanphui, Palash' 'Dandela, Rambabu' _publ_section_title ; Exploring Novel Cocrystals of Milrinone: A Cardioprotective Drug Combined with Nutraceuticals and NSAID ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00990H _journal_year 2024 _chemical_formula_moiety 'C12 H9 N3 O, C7 H6 O3' _chemical_formula_sum 'C19 H15 N3 O4' _chemical_formula_weight 349.34 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-02-26 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-09-21 deposited with the CCDC. 2024-11-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.0102(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.0120(3) _cell_length_b 16.7621(7) _cell_length_c 12.6282(5) _cell_measurement_reflns_used 4192 _cell_measurement_temperature 293.15 _cell_measurement_theta_max 56 _cell_measurement_theta_min 3 _cell_volume 1695.68(12) _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293.15 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device_type 'Bruker APEX4' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1065 _diffrn_reflns_av_unetI/netI 0.0590 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 35954 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.493 _diffrn_reflns_theta_min 2.818 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.368 _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.167 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.039 _refine_ls_extinction_coef 0.091(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2019/2 (Sheldrick 2019)' _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4192 _refine_ls_number_restraints 26 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0514 _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^)+(0.0679P)^2^+0.4292P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1286 _refine_ls_wR_factor_ref 0.1809 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2403 _reflns_number_total 4192 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00990h2.cif _cod_data_source_block ml_sesa_r _cod_database_code 7249641 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.986 _shelx_estimated_absorpt_t_min 0.977 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O1-H1 0.88 with sigma of 0.02 O2-C15 \\sim O2A-C15 with sigma of 0.02 O2-C16 \\sim O2A-C16A with sigma of 0.02 O3-C16 \\sim O3A-C16A with sigma of 0.02 O3-C17 \\sim O3A-C17 with sigma of 0.02 O2-O3 \\sim O2A-O3A with sigma of 0.04 C15-C16 \\sim C15-C16A with sigma of 0.04 C16-C17 \\sim C16A-C17 with sigma of 0.04 3. Rigid body (RIGU) restrains O3, O3A, C16A, C16, O2A, O2 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(O3A)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(O2A)=1-FVAR(1) Sof(O2)=Sof(O3)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C16(H16A,H16B), C16A(H16C,H16D) 5.b Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C18(H18), C19(H19) 5.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C) ; _shelx_res_file ; TITL ml_sesa_r P -1 R = 0.06 New:P21/c ml_sesa_r.res created by SHELXL-2019/3 at 18:22:43 on 26-Feb-2024 CELL 0.71073 8.012 16.7621 12.6282 90 91.0102 90 ZERR 4 0.0003 0.0007 0.0005 0 0.0003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 76 60 12 16 DFIX 0.88 O1 H1 SADI O2 C15 O2A C15 SADI O2 C16 O2A C16A SADI O3 C16 O3A C16A SADI O3 C17 O3A C17 SADI 0.04 O2 O3 O2A O3A SADI 0.04 C15 C16 C15 C16A SADI 0.04 C16 C17 C16A C17 RIGU O3 O3A C16A C16 O2A O2 L.S. 15 PLAN 5 SIZE 0.14 0.18 0.24 TEMP 20 CONF BOND $H MORE -1 fmap 2 acta REM REM REM WGHT 0.067900 0.429200 EXTI 0.091232 FVAR 1.33003 0.40646 O1 4 -0.563929 -0.463332 -0.363006 11.00000 0.08549 0.08172 = 0.08413 -0.01720 -0.02969 0.01092 H1 2 -0.639984 -0.455033 -0.417068 11.00000 -1.50000 PART 1 O2 4 -0.323788 -0.327738 -0.063806 21.00000 0.07077 0.06238 = 0.08471 -0.00822 -0.04058 0.00766 O3 4 -0.462033 -0.211758 -0.096526 21.00000 0.06864 0.05350 = 0.07868 0.00983 -0.00916 -0.00237 PART 0 O4 4 -1.366304 -0.572746 -1.058904 11.00000 0.06292 0.07649 = 0.06856 -0.00930 -0.02355 0.01059 N1 3 -1.039598 -0.720766 -1.067791 11.00000 0.07903 0.08209 = 0.09427 -0.02836 -0.02504 0.01073 N2 3 -1.302254 -0.490222 -0.921634 11.00000 0.05238 0.05929 = 0.06232 -0.00031 -0.01182 0.00824 H2 2 -1.393571 -0.464047 -0.935001 11.00000 -1.20000 N3 3 -0.770363 -0.460495 -0.534756 11.00000 0.06299 0.09278 = 0.05938 -0.00860 -0.00831 -0.00196 C1 1 -1.079156 -0.666713 -1.018102 11.00000 0.05486 0.06450 = 0.06544 -0.00728 -0.01775 0.00210 C2 1 -1.124356 -0.598622 -0.955655 11.00000 0.04620 0.05561 = 0.05615 -0.00068 -0.00772 -0.00125 C3 1 -1.271025 -0.555794 -0.984979 11.00000 0.05076 0.05943 = 0.05189 0.00223 -0.00954 -0.00193 C4 1 -1.212600 -0.466523 -0.835933 11.00000 0.05264 0.05731 = 0.05597 0.00098 -0.00477 -0.00179 C5 1 -1.282331 -0.395434 -0.779887 11.00000 0.07577 0.06692 = 0.07727 -0.01074 -0.01022 0.01450 AFIX 137 H5A 2 -1.237725 -0.347539 -0.809995 11.00000 -1.50000 H5B 2 -1.252197 -0.398014 -0.706052 11.00000 -1.50000 H5C 2 -1.401731 -0.395221 -0.787719 11.00000 -1.50000 AFIX 0 C6 1 -1.073127 -0.509302 -0.807170 11.00000 0.04639 0.05804 = 0.05246 0.00038 -0.00488 -0.00277 C7 1 -1.031784 -0.576404 -0.869495 11.00000 0.04453 0.06150 = 0.05689 -0.00078 -0.00819 0.00242 AFIX 43 H7 2 -0.938021 -0.606297 -0.850803 11.00000 -1.20000 AFIX 0 C8 1 -0.970007 -0.491037 -0.712777 11.00000 0.04884 0.06578 = 0.05112 -0.00389 -0.00270 -0.00133 C9 1 -0.922400 -0.551480 -0.644188 11.00000 0.05984 0.06709 = 0.05715 -0.00477 -0.00678 0.00400 AFIX 43 H9 2 -0.957585 -0.603621 -0.656217 11.00000 -1.20000 AFIX 0 C10 1 -0.822824 -0.533536 -0.558381 11.00000 0.06860 0.07968 = 0.05761 -0.00374 -0.01001 0.00910 AFIX 43 H10 2 -0.789878 -0.575068 -0.513880 11.00000 -1.20000 AFIX 0 C11 1 -0.816061 -0.402559 -0.600321 11.00000 0.07661 0.08222 = 0.06626 -0.00860 -0.01159 -0.01896 AFIX 43 H11 2 -0.780109 -0.350964 -0.585318 11.00000 -1.20000 AFIX 0 C12 1 -0.913486 -0.414580 -0.689084 11.00000 0.07353 0.07118 = 0.06193 0.00137 -0.01211 -0.01346 AFIX 43 H12 2 -0.941569 -0.371988 -0.733100 11.00000 -1.20000 AFIX 0 C13 1 -0.547430 -0.397568 -0.301561 11.00000 0.05251 0.06778 = 0.05807 -0.00151 -0.00602 0.00104 C14 1 -0.439595 -0.404223 -0.215176 11.00000 0.05314 0.06210 = 0.06635 0.00308 -0.00876 0.00759 AFIX 43 H14 2 -0.380388 -0.450911 -0.201381 11.00000 -1.20000 AFIX 0 C15 1 -0.424459 -0.338939 -0.151296 11.00000 0.04802 0.06134 = 0.05431 0.00646 -0.00630 0.00302 PART 1 C16 1 -0.337949 -0.246343 -0.033694 21.00000 0.09254 0.07030 = 0.10056 -0.00942 -0.02754 0.01829 AFIX 23 H16A 2 -0.366660 -0.242459 0.040428 21.00000 -1.20000 H16B 2 -0.232657 -0.219049 -0.043754 21.00000 -1.20000 AFIX 0 PART 0 C17 1 -0.509593 -0.269229 -0.169309 11.00000 0.06292 0.06047 = 0.05904 0.00273 -0.00617 0.00589 C18 1 -0.614123 -0.261729 -0.254033 11.00000 0.07478 0.06831 = 0.07158 0.00747 -0.01514 0.01787 AFIX 43 H18 2 -0.670967 -0.214338 -0.267565 11.00000 -1.20000 AFIX 0 C19 1 -0.633336 -0.327563 -0.320104 11.00000 0.06137 0.07770 = 0.05888 0.00754 -0.01503 0.00695 AFIX 43 H19 2 -0.705921 -0.324286 -0.378226 11.00000 -1.20000 AFIX 0 PART 2 O3A 4 -0.473358 -0.216142 -0.088898 -21.00000 0.11790 0.07663 = 0.07084 -0.01721 -0.02727 0.03159 C16A 1 -0.380780 -0.260445 -0.015273 -21.00000 0.08528 0.07412 = 0.06766 -0.01105 -0.02027 0.01560 AFIX 23 H16C 2 -0.448729 -0.271923 0.045693 -21.00000 -1.20000 H16D 2 -0.284668 -0.229753 0.008676 -21.00000 -1.20000 AFIX 0 O2A 4 -0.326338 -0.333405 -0.061680 -21.00000 0.07134 0.07355 = 0.05538 0.00230 -0.00991 0.01221 HKLF 4 1 -1 0 0 0 0 -1 0 -1 0 REM ml_sesa_r P -1 R = 0.06 New:P21/c REM wR2 = 0.1809, GooF = S = 1.076, Restrained GooF = 1.074 for all data REM R1 = 0.0514 for 2403 Fo > 4sig(Fo) and 0.1065 for all 4192 data REM 271 parameters refined using 26 restraints END WGHT 0.0674 0.4332 REM Highest difference peak 0.167, deepest hole -0.197, 1-sigma level 0.039 Q1 1 -0.8450 -0.3420 -0.5438 11.00000 0.05 0.17 Q2 1 -1.4950 -0.5840 -1.1163 11.00000 0.05 0.16 Q3 1 -0.6762 -0.4480 -0.4568 11.00000 0.05 0.15 Q4 1 -0.4902 -0.3270 -0.1459 11.00000 0.05 0.14 Q5 1 -1.0793 -0.5719 -0.9359 11.00000 0.05 0.14 ; _shelx_res_checksum 83748 _shelx_hkl_file ; -2 0 0 3613.09 354.26 -2 0 0 3556.91 356.57 -2 0 0 3575.20 355.63 -2 0 0 3886.44 355.82 2 0 0 3879.60 355.82 2 0 0 3708.45 357.70 2 0 0 3312.78 355.66 2 0 0 3605.42 356.80 2 0 0 3408.91 356.86 -3 0 0 1915.71 181.02 -3 0 0 1877.66 183.19 -3 0 0 1818.41 184.44 -3 0 0 1944.26 183.27 3 0 0 1757.37 184.63 3 0 0 1696.29 184.81 3 0 0 1767.39 185.71 3 0 0 1899.75 183.24 3 0 0 1757.43 183.43 -4 0 0 3.23 2.72 -4 0 0 4.33 3.75 -4 0 0 3.47 5.19 -4 0 0 8.13 5.41 4 0 0 3.89 3.61 4 0 0 5.43 5.22 4 0 0 8.46 5.90 4 0 0 1.03 5.30 4 0 0 4.93 5.03 -5 0 0 9.97 5.61 -5 0 0 3.55 7.39 -5 0 0 2.36 4.43 -5 0 0 5.28 3.63 5 0 0 11.32 6.01 5 0 0 9.26 6.05 5 0 0 7.04 6.43 5 0 0 3.65 6.02 5 0 0 12.41 8.76 -6 0 0 336.43 39.94 -6 0 0 306.80 41.49 -6 0 0 312.12 34.78 -6 0 0 334.93 40.69 6 0 0 273.80 44.67 6 0 0 294.98 41.46 6 0 0 352.99 45.40 6 0 0 298.59 42.97 6 0 0 360.23 41.11 -7 0 0 118.78 25.54 -7 0 0 126.60 23.02 -7 0 0 131.59 16.07 7 0 0 132.51 28.57 7 0 0 123.06 29.91 7 0 0 98.79 22.35 -8 0 0 191.51 20.59 -8 0 0 177.12 34.04 8 0 0 156.92 35.45 8 0 0 230.57 44.27 8 0 0 157.41 29.74 -9 0 0 -3.11 9.52 9 0 0 -17.04 12.60 9 0 0 -13.66 8.49 9 0 0 -11.20 14.25 10 0 0 11.29 15.08 10 0 0 -18.98 9.74 10 -1 0 -5.70 12.00 10 -1 0 19.21 16.01 -10 1 0 6.88 11.70 9 -1 0 -2.17 8.62 9 -1 0 -12.87 10.28 9 -1 0 -6.83 11.40 -9 1 0 -12.54 8.10 8 -1 0 -2.39 5.65 8 -1 0 -8.79 10.97 8 -1 0 -12.34 4.98 -8 1 0 1.82 7.23 -8 1 0 8.60 8.70 7 -1 0 -5.00 4.95 7 -1 0 2.09 7.41 7 -1 0 -6.36 6.46 7 -1 0 3.15 8.49 -7 1 0 2.15 7.49 -7 1 0 -1.86 5.47 6 -1 0 -1.35 4.42 6 -1 0 -3.25 5.75 6 -1 0 -6.08 5.68 6 -1 0 8.76 7.33 6 -1 0 -2.56 3.62 -6 1 0 -0.34 1.18 -6 1 0 -1.47 4.84 -6 1 0 -0.92 4.80 -6 1 0 -7.40 3.34 5 -1 0 -2.87 3.26 5 -1 0 5.43 6.62 5 -1 0 2.64 7.68 5 -1 0 -1.78 5.07 -5 1 0 3.11 1.67 -5 1 0 1.06 4.18 -5 1 0 -3.69 3.04 -5 1 0 -3.74 4.22 4 -1 0 -2.83 3.73 4 -1 0 -2.18 3.59 4 -1 0 2.00 3.51 4 -1 0 -3.94 2.67 4 -1 0 1.92 5.00 -4 1 0 1.09 2.91 -4 1 0 1.09 3.55 -4 1 0 -2.79 3.03 -4 1 0 -0.49 1.27 3 -1 0 -1.91 3.18 3 -1 0 -5.46 4.68 3 -1 0 4.78 4.57 3 -1 0 -1.83 2.83 3 -1 0 -3.62 2.93 -3 1 0 -1.29 1.16 -3 1 0 2.94 3.91 -3 1 0 5.59 3.86 -3 1 0 0.72 4.29 2 -1 0 -2.61 2.58 2 -1 0 -4.01 1.60 2 -1 0 -6.93 2.19 2 -1 0 -5.88 3.28 2 -1 0 -4.06 2.72 -2 1 0 -2.70 2.32 -2 1 0 -2.51 2.93 -2 1 0 -4.64 2.25 1 -1 0 0.75 1.51 1 -1 0 -0.77 1.25 1 -1 0 -0.37 1.32 1 -1 0 -0.85 0.64 -1 1 0 0.40 1.06 -1 1 0 0.52 1.26 -1 1 0 -2.54 1.17 -1 -1 0 -9.97 1.11 -1 -1 0 -8.12 1.90 -1 -1 0 -8.85 1.37 -1 -1 0 -8.31 1.92 1 1 0 -6.70 1.83 1 1 0 -9.39 1.91 1 1 0 -7.91 2.99 1 1 0 -3.83 2.93 -2 -1 0 -5.10 3.09 -2 -1 0 -3.87 2.95 -2 -1 0 -2.89 1.99 -2 -1 0 -2.94 1.74 -2 -1 0 -1.69 2.68 2 1 0 -3.40 2.31 2 1 0 0.10 3.94 2 1 0 -0.21 4.45 2 1 0 2.51 2.37 -3 -1 0 -0.19 3.78 -3 -1 0 -0.31 3.58 -3 -1 0 -0.61 3.08 -3 -1 0 -1.75 2.85 3 1 0 -6.34 3.28 3 1 0 0.06 3.13 3 1 0 -1.01 2.38 3 1 0 -3.26 2.49 3 1 0 1.86 4.88 -4 -1 0 -5.75 2.81 -4 -1 0 1.15 4.68 -4 -1 0 -0.95 2.42 -4 -1 0 -0.97 5.69 4 1 0 -1.16 3.94 4 1 0 -2.53 3.06 4 1 0 -3.82 4.50 4 1 0 -1.16 3.59 -5 -1 0 0.97 3.68 -5 -1 0 -3.16 4.87 -5 -1 0 3.25 5.83 -5 -1 0 -0.25 5.38 5 1 0 9.89 7.41 5 1 0 2.01 5.43 5 1 0 -4.05 3.00 5 1 0 1.60 6.85 -6 -1 0 6.65 6.34 -6 -1 0 -1.50 3.67 -6 -1 0 -0.72 4.57 -6 -1 0 -3.78 2.87 6 1 0 -8.38 3.79 6 1 0 -2.56 5.56 6 1 0 0.68 5.47 6 1 0 0.95 5.88 -7 -1 0 1.58 7.04 -7 -1 0 9.12 9.35 -7 -1 0 -3.39 4.20 7 1 0 19.66 11.10 7 1 0 -3.86 9.70 7 1 0 -3.08 7.69 -8 -1 0 -16.49 7.00 -8 -1 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2 13.92 3.72 3 -6 2 4.72 5.27 4 -6 2 3.95 4.10 4 -6 2 5.36 4.58 4 -6 2 12.45 5.91 4 -6 2 -1.70 4.67 4 -6 2 11.55 4.74 4 -6 2 8.07 3.87 5 -6 2 -4.79 4.15 5 -6 2 -1.73 4.18 5 -6 2 -6.10 4.12 5 -6 2 4.69 6.32 5 -6 2 4.67 5.54 6 -6 2 311.25 41.68 6 -6 2 338.39 38.33 6 -6 2 276.17 40.18 6 -6 2 314.68 40.94 6 -6 2 256.79 36.91 7 -6 2 -12.18 10.55 7 -6 2 -2.84 7.12 7 -6 2 11.91 10.60 7 -6 2 8.30 11.07 7 -6 2 3.44 9.47 8 -6 2 2.65 7.18 8 -6 2 0.60 9.39 8 -6 2 8.16 12.58 8 -6 2 31.71 12.17 9 -6 2 -9.65 7.63 9 -6 2 -14.94 10.36 9 -6 2 33.09 17.09 10 5 -2 16.59 10.79 10 5 -2 21.19 17.27 -10 -5 2 -4.58 10.92 -10 -5 2 10.99 13.21 9 5 -2 92.54 21.86 9 5 -2 118.99 35.99 -9 -5 2 120.62 31.04 -9 -5 2 83.98 21.25 8 5 -2 13.17 12.57 -8 -5 2 -6.43 7.80 -8 -5 2 11.90 11.72 7 5 -2 85.31 18.68 7 5 -2 50.35 21.76 7 5 -2 76.41 24.72 -7 -5 2 65.25 18.31 -7 -5 2 101.28 26.55 6 5 -2 154.03 31.43 6 5 -2 170.60 23.00 6 5 -2 171.03 34.66 -6 -5 2 153.59 26.06 -6 -5 2 110.30 28.67 -6 -5 2 154.68 28.03 5 5 -2 15.47 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31.60 8.58 3 -4 2 25.35 7.94 3 -4 2 23.10 6.63 3 -4 2 23.48 5.50 3 -4 2 24.78 5.79 3 -4 2 23.97 5.59 3 -4 2 18.67 5.87 -4 4 -2 1917.39 181.06 4 -4 2 1688.66 179.36 4 -4 2 1885.72 181.07 4 -4 2 1744.41 180.70 4 -4 2 1797.93 174.23 4 -4 2 1633.23 177.93 4 -4 2 1820.17 179.75 4 -4 2 1755.13 173.82 -5 4 -2 162.90 15.41 -5 4 -2 137.35 15.48 -5 4 -2 129.33 22.67 5 -4 2 128.16 21.47 5 -4 2 135.30 23.64 5 -4 2 95.32 21.06 -6 4 -2 557.27 62.86 6 -4 2 560.65 63.63 6 -4 2 602.37 64.66 6 -4 2 530.95 63.97 6 -4 2 476.34 61.12 6 -4 2 516.57 65.17 -7 4 -2 6.52 4.50 -7 4 -2 15.14 6.43 7 -4 2 23.84 13.96 7 -4 2 1.67 8.82 7 -4 2 18.77 9.39 7 -4 2 32.66 14.99 7 -4 2 13.60 9.25 -8 4 -2 6.45 6.36 -8 4 -2 -1.58 4.92 8 -4 2 -6.10 9.67 8 -4 2 -0.63 8.06 8 -4 2 -1.69 11.03 -9 4 -2 -16.00 6.24 -9 4 -2 -11.35 5.93 9 -4 2 -21.31 8.97 9 -4 2 6.82 12.61 9 -4 2 -11.53 11.16 10 -4 2 1.54 11.93 10 -4 2 -13.80 7.69 10 3 -2 -3.48 11.56 10 3 -2 -7.87 15.07 -10 -3 2 16.51 15.31 -10 -3 2 2.43 12.15 9 3 -2 -9.25 13.23 9 3 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3 -2 2.81 6.24 7 -3 2 -5.61 6.94 7 -3 2 0.04 5.75 7 -3 2 6.93 11.40 7 -3 2 3.51 8.95 -8 3 -2 -0.93 5.67 -8 3 -2 -13.62 4.98 8 -3 2 -2.04 8.79 8 -3 2 -13.27 7.51 8 -3 2 -9.46 4.09 -9 3 -2 3.70 9.22 -9 3 -2 1.32 7.49 9 -3 2 21.87 15.24 9 -3 2 21.95 11.65 9 -3 2 -12.66 11.72 -10 3 -2 -26.63 9.98 10 -3 2 -1.73 13.49 10 -3 2 -1.05 10.98 10 2 -2 33.73 22.12 10 2 -2 15.72 11.98 -10 -2 2 0.79 8.27 -10 -2 2 -1.10 15.09 9 2 -2 60.58 23.50 9 2 -2 46.10 21.57 9 2 -2 66.56 18.90 -9 -2 2 60.89 14.44 -9 -2 2 85.49 25.27 8 2 -2 146.11 36.49 8 2 -2 176.49 31.37 8 2 -2 210.61 40.64 -8 -2 2 179.67 26.78 -8 -2 2 188.00 37.77 7 2 -2 188.34 39.96 7 2 -2 227.71 31.67 7 2 -2 255.28 38.45 -7 -2 2 238.41 31.35 -7 -2 2 186.08 37.37 6 2 -2 390.86 52.00 6 2 -2 330.01 51.54 6 2 -2 408.93 46.12 6 2 -2 343.89 50.04 -6 -2 2 377.66 44.97 -6 -2 2 347.45 46.26 -6 -2 2 463.60 47.42 -6 -2 2 352.24 49.41 5 2 -2 719.51 76.81 5 2 -2 663.70 81.67 5 2 -2 672.73 83.09 5 2 -2 729.84 81.96 5 2 -2 663.04 78.80 -5 -2 2 672.86 81.20 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15.09 -1 -3 -20 -7.89 11.38 1 3 20 -5.50 9.89 -2 -3 -20 10.81 12.57 2 3 20 -6.59 12.58 -3 -3 -20 12.68 14.04 -3 -3 -20 0.49 5.84 3 3 20 -10.57 8.48 -4 -3 -20 6.38 8.53 4 3 20 -27.62 14.46 4 -4 -20 16.18 12.39 4 -4 -20 -0.20 10.94 -4 4 20 -14.05 13.86 3 -4 -20 -1.38 7.58 -3 4 20 3.63 9.91 2 -4 -20 6.61 7.88 1 -4 -20 37.08 14.39 -1 4 20 2.78 15.22 0 -4 -20 32.63 13.68 0 4 20 22.03 19.11 -1 -4 -20 2.21 9.29 -1 -4 -20 4.90 14.02 1 4 20 -13.43 14.95 -2 -4 -20 1.36 8.14 -2 -4 -20 -14.51 9.89 2 4 20 -9.75 9.39 -3 -4 -20 28.55 14.67 -3 -4 -20 2.68 15.35 3 4 20 -13.55 16.87 -4 -4 -20 11.19 10.35 -4 -4 -20 -32.65 13.53 4 4 20 -12.55 18.68 3 -5 -20 -7.52 10.54 2 -5 -20 -9.87 9.06 -2 5 20 -17.97 13.05 1 -5 -20 -3.87 10.44 -1 5 20 -9.02 13.82 0 -5 -20 38.07 20.43 0 -5 -20 69.69 21.04 0 5 20 30.78 17.82 -1 -5 -20 13.60 12.30 -1 -5 -20 15.65 10.91 1 5 20 9.20 20.26 -2 -5 -20 -2.02 10.85 -2 -5 -20 2.55 15.55 2 5 20 -24.05 17.43 -3 -5 -20 22.11 18.62 -3 -5 -20 -25.36 10.87 3 5 20 -32.78 17.07 2 -6 -20 11.94 9.73 -2 6 20 -20.33 8.00 1 -6 -20 -4.91 11.44 1 -6 -20 -1.25 10.16 -1 6 20 -8.88 17.54 0 -6 -20 9.29 12.49 0 -6 -20 12.11 10.86 0 6 20 -28.04 15.04 -1 -6 -20 36.36 19.94 -1 -6 -20 10.67 15.37 1 6 20 21.15 20.22 -2 -6 -20 -16.04 13.08 2 6 20 -25.53 17.25 1 -7 -20 -6.98 13.40 1 -7 -20 18.40 13.58 -1 7 20 -21.28 12.63 0 -7 -20 25.37 15.88 0 -7 -20 38.17 20.73 0 7 20 13.71 22.77 -1 -7 -20 25.76 19.46 -1 -7 -20 -2.16 10.73 1 7 20 16.40 17.54 1 5 -21 29.22 11.42 -1 -5 21 8.19 9.79 0 5 -21 -2.52 9.46 0 -5 21 -8.66 8.19 -1 5 -21 11.92 10.30 1 -5 21 12.40 9.51 2 4 -21 8.53 10.06 -2 -4 21 -5.35 9.07 1 4 -21 3.41 9.86 -1 -4 21 -8.91 6.83 0 4 -21 8.45 8.49 0 -4 21 -6.40 7.76 -1 4 -21 3.46 8.86 1 -4 21 -1.66 8.34 -2 4 -21 12.92 11.25 2 -4 21 -5.87 7.27 3 3 -21 5.46 11.73 -3 -3 21 -2.97 6.44 2 3 -21 -9.90 8.26 -2 -3 21 -10.18 8.33 1 3 -21 15.01 11.10 1 3 -21 2.95 7.70 -1 -3 21 7.62 11.23 0 3 -21 4.27 10.37 0 -3 21 0.76 8.34 -1 3 -21 -0.25 8.38 1 -3 21 4.05 9.14 -2 3 -21 0.21 8.79 2 -3 21 3.05 10.84 -3 3 -21 6.28 11.12 3 2 -21 22.81 12.22 3 2 -21 -20.22 7.36 -3 -2 21 -19.24 8.05 2 2 -21 -6.85 7.70 2 2 -21 -6.57 10.15 -2 -2 21 -13.89 6.40 1 2 -21 8.91 11.36 -1 -2 21 -4.73 8.74 0 2 -21 11.71 11.66 0 -2 21 1.47 6.90 -1 2 -21 12.33 10.56 1 -2 21 4.10 10.96 -2 2 -21 16.79 9.70 2 -2 21 -17.93 8.83 -3 2 -21 12.79 11.21 3 -2 21 10.21 13.23 3 1 -21 6.63 12.45 3 1 -21 -5.21 10.12 -3 -1 21 3.50 12.42 2 1 -21 8.29 11.47 2 1 -21 7.78 10.19 -2 -1 21 -4.67 8.76 1 1 -21 0.27 9.48 -1 -1 21 -10.21 6.75 0 1 -21 14.74 11.59 0 1 -21 6.16 14.37 0 -1 21 1.13 9.17 -1 1 -21 11.73 9.64 1 -1 21 -0.96 7.07 -2 1 -21 22.54 11.05 2 -1 21 -1.53 10.62 -3 1 -21 19.32 11.73 3 -1 21 -0.06 12.53 3 0 -21 -0.52 9.22 3 0 -21 -0.36 8.88 -3 0 21 7.21 11.18 2 0 -21 20.53 12.85 -2 0 21 -10.56 9.25 1 0 -21 -5.61 8.64 -1 0 21 -4.31 10.23 0 0 -21 15.90 9.27 0 0 21 -10.96 8.29 -1 0 -21 9.49 9.76 1 0 21 -11.26 9.99 -2 0 -21 12.25 11.39 2 0 21 12.80 15.16 -3 0 -21 -7.30 10.43 3 0 21 -4.40 11.66 3 -1 -21 1.48 8.59 3 -1 -21 29.70 12.72 -3 1 21 22.74 12.46 2 -1 -21 0.69 5.88 -2 1 21 -15.28 8.79 1 -1 -21 8.41 11.62 -1 1 21 3.04 10.33 0 -1 -21 -5.46 10.06 0 1 21 -13.02 13.42 -1 -1 -21 10.61 11.85 1 1 21 -1.23 13.37 -2 -1 -21 0.46 11.03 2 1 21 8.66 12.09 -3 -1 -21 -2.73 10.98 3 1 21 -0.39 12.96 2 -2 -21 11.09 10.58 -2 2 21 -13.86 10.23 1 -2 -21 10.49 9.68 -1 2 21 2.08 11.17 0 -2 -21 8.67 12.99 -1 -2 -21 4.63 11.17 1 2 21 -1.07 10.60 -2 -2 -21 1.94 11.91 2 2 21 -13.02 10.72 -3 -2 -21 -26.39 11.64 3 2 21 -14.65 15.15 3 -3 -21 6.08 12.79 -3 3 21 -30.70 11.44 2 -3 -21 -0.66 11.01 -2 3 21 -29.64 13.29 1 -3 -21 10.48 10.06 -1 3 21 -6.48 8.67 0 -3 -21 7.46 11.43 0 3 21 6.84 13.21 -1 -3 -21 2.82 12.48 1 3 21 24.65 19.26 -2 -3 -21 -3.93 14.94 2 3 21 -2.19 16.34 -3 -3 -21 -15.54 11.22 2 -4 -21 -0.25 8.41 -2 4 21 -9.41 10.11 1 -4 -21 -19.03 9.73 -1 4 21 -28.12 12.39 0 -4 -21 -0.24 13.52 0 4 21 -26.30 12.42 -1 -4 -21 -11.07 8.09 1 4 21 -21.50 16.57 -2 -4 -21 -27.92 11.88 -2 -4 -21 0.90 9.74 2 4 21 28.09 19.51 1 -5 -21 17.49 13.70 -1 5 21 -14.25 15.69 0 -5 -21 9.58 11.95 0 5 21 -13.99 16.16 -1 -5 -21 9.40 15.11 -1 -5 -21 18.12 15.99 1 5 21 15.30 16.32 0 3 -22 16.85 12.75 0 -3 22 -7.89 9.24 1 2 -22 3.90 11.05 0 2 -22 -0.90 11.94 0 -2 22 -2.09 9.22 -1 2 -22 5.96 10.03 1 -2 22 -9.08 9.23 1 1 -22 1.13 10.73 -1 -1 22 -17.18 7.83 0 1 -22 -13.38 10.75 0 -1 22 -13.53 10.43 -1 1 -22 4.28 11.42 1 -1 22 24.86 16.61 1 0 -22 10.05 11.71 -1 0 22 3.01 10.30 0 0 -22 18.43 12.17 0 0 22 -0.86 11.97 -1 0 -22 -17.51 9.86 1 -1 -22 2.26 10.89 -1 1 22 4.57 10.31 0 -1 -22 12.53 13.02 -1 -1 -22 8.15 12.55 1 1 22 -10.95 11.91 1 -2 -22 16.53 12.85 -1 2 22 -17.33 11.39 0 -2 -22 7.86 13.18 0 2 22 -4.22 16.26 -1 -2 -22 -10.12 11.22 1 2 22 -31.98 13.23 0 -3 -22 3.02 13.37 0 3 22 -30.45 13.74 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5743 _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 0.71091 8.017 12.631 16.776 89.989 89.989 90.007 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 76014 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 -0.5639(2) -0.46333(11) -0.36301(15) 0.0841(6) Uani 1 1 d D . . . . H1 H -0.640(4) -0.455(2) -0.417(2) 0.126 Uiso 1 1 d D U . . . O2 O -0.324(2) -0.3277(11) -0.0638(12) 0.073(5) Uani 0.41(4) 1 d D . P A 1 O3 O -0.4620(19) -0.2118(8) -0.0965(12) 0.067(4) Uani 0.41(4) 1 d D . P A 1 O4 O -1.36630(19) -0.57275(10) -1.05890(13) 0.0696(5) Uani 1 1 d . . . . . N1 N -1.0396(3) -0.72077(14) -1.06779(19) 0.0854(7) Uani 1 1 d . . . . . N2 N -1.3023(2) -0.49022(11) -0.92163(15) 0.0581(5) Uani 1 1 d . . . . . H2 H -1.394(3) -0.4640(14) -0.9350(19) 0.070 Uiso 1 1 d . U . . . N3 N -0.7704(2) -0.46049(14) -0.53476(16) 0.0718(6) Uani 1 1 d . . . . . C1 C -1.0792(3) -0.66671(14) -1.01810(19) 0.0618(6) Uani 1 1 d . . . . . C2 C -1.1244(2) -0.59862(12) -0.95565(16) 0.0528(5) Uani 1 1 d . . . . . C3 C -1.2710(2) -0.55579(13) -0.98498(16) 0.0541(5) Uani 1 1 d . . . . . C4 C -1.2126(3) -0.46652(13) -0.83593(17) 0.0554(5) Uani 1 1 d . . . . . C5 C -1.2823(3) -0.39543(15) -0.7799(2) 0.0735(7) Uani 1 1 d . . . . . H5A H -1.237725 -0.347539 -0.809995 0.110 Uiso 1 1 calc R U . . . H5B H -1.252197 -0.398014 -0.706052 0.110 Uiso 1 1 calc R U . . . H5C H -1.401731 -0.395221 -0.787719 0.110 Uiso 1 1 calc R U . . . C6 C -1.0731(2) -0.50930(12) -0.80717(16) 0.0524(5) Uani 1 1 d . . . . . C7 C -1.0318(2) -0.57640(13) -0.86950(16) 0.0544(5) Uani 1 1 d . . . . . H7 H -0.938021 -0.606297 -0.850803 0.065 Uiso 1 1 calc R U . . . C8 C -0.9700(2) -0.49104(13) -0.71278(16) 0.0553(5) Uani 1 1 d . . . . . C9 C -0.9224(3) -0.55148(15) -0.64419(17) 0.0615(6) Uani 1 1 d . . . . . H9 H -0.957585 -0.603621 -0.656217 0.074 Uiso 1 1 calc R U . . . C10 C -0.8228(3) -0.53354(16) -0.55838(18) 0.0688(6) Uani 1 1 d . . . . . H10 H -0.789878 -0.575068 -0.513880 0.083 Uiso 1 1 calc R U . . . C11 C -0.8161(3) -0.40256(17) -0.6003(2) 0.0752(7) Uani 1 1 d . . . . . H11 H -0.780109 -0.350964 -0.585318 0.090 Uiso 1 1 calc R U . . . C12 C -0.9135(3) -0.41458(15) -0.68908(19) 0.0690(6) Uani 1 1 d . . . . . H12 H -0.941569 -0.371988 -0.733100 0.083 Uiso 1 1 calc R U . . . C13 C -0.5474(3) -0.39757(14) -0.30156(17) 0.0595(6) Uani 1 1 d . . . . . C14 C -0.4396(3) -0.40422(14) -0.21518(18) 0.0606(6) Uani 1 1 d . . . . . H14 H -0.380388 -0.450911 -0.201381 0.073 Uiso 1 1 calc R U . . . C15 C -0.4245(2) -0.33894(13) -0.15130(16) 0.0546(5) Uani 1 1 d D . . . . C16 C -0.338(4) -0.2463(12) -0.034(2) 0.088(6) Uani 0.41(4) 1 d D . P A 1 H16A H -0.366660 -0.242459 0.040428 0.106 Uiso 0.41(4) 1 calc R U P A 1 H16B H -0.232657 -0.219049 -0.043754 0.106 Uiso 0.41(4) 1 calc R U P A 1 C17 C -0.5096(3) -0.26923(14) -0.16931(17) 0.0609(6) Uani 1 1 d D . . . . C18 C -0.6141(3) -0.26173(15) -0.2540(2) 0.0718(7) Uani 1 1 d . . . . . H18 H -0.670967 -0.214338 -0.267565 0.086 Uiso 1 1 calc R U . . . C19 C -0.6333(3) -0.32756(15) -0.32010(18) 0.0662(6) Uani 1 1 d . . . . . H19 H -0.705921 -0.324286 -0.378226 0.079 Uiso 1 1 calc R U . . . O3A O -0.4734(17) -0.2161(6) -0.0889(9) 0.089(3) Uani 0.59(4) 1 d D . P A 2 C16A C -0.381(2) -0.2604(9) -0.0153(10) 0.076(3) Uani 0.59(4) 1 d D . P A 2 H16C H -0.448729 -0.271923 0.045693 0.091 Uiso 0.59(4) 1 calc R U P A 2 H16D H -0.284668 -0.229753 0.008676 0.091 Uiso 0.59(4) 1 calc R U P A 2 O2A O -0.3263(14) -0.3334(8) -0.0617(7) 0.067(3) Uani 0.59(4) 1 d D . 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 0.0855(13) 0.0817(13) 0.0841(13) -0.0172(10) -0.0297(10) 0.0109(9) O2 0.071(9) 0.062(6) 0.085(10) -0.008(6) -0.041(7) 0.008(5) O3 0.069(6) 0.053(6) 0.079(7) 0.010(5) -0.009(4) -0.002(4) O4 0.0629(9) 0.0765(11) 0.0686(10) -0.0093(8) -0.0236(8) 0.0106(8) N1 0.0790(14) 0.0821(15) 0.0943(16) -0.0284(13) -0.0250(12) 0.0107(12) N2 0.0524(10) 0.0593(11) 0.0623(11) -0.0003(9) -0.0118(8) 0.0082(8) N3 0.0630(12) 0.0928(16) 0.0594(12) -0.0086(11) -0.0083(9) -0.0020(10) C1 0.0549(12) 0.0645(14) 0.0654(13) -0.0073(12) -0.0177(10) 0.0021(10) C2 0.0462(10) 0.0556(12) 0.0562(12) -0.0007(9) -0.0077(8) -0.0012(8) C3 0.0508(11) 0.0594(13) 0.0519(11) 0.0022(9) -0.0095(9) -0.0019(9) C4 0.0526(11) 0.0573(13) 0.0560(12) 0.0010(9) -0.0048(9) -0.0018(9) C5 0.0758(15) 0.0669(15) 0.0773(15) -0.0107(12) -0.0102(12) 0.0145(12) C6 0.0464(10) 0.0580(12) 0.0525(11) 0.0004(9) -0.0049(8) -0.0028(9) C7 0.0445(10) 0.0615(13) 0.0569(12) -0.0008(10) -0.0082(8) 0.0024(9) C8 0.0488(10) 0.0658(14) 0.0511(11) -0.0039(10) -0.0027(8) -0.0013(9) C9 0.0598(12) 0.0671(14) 0.0571(12) -0.0048(11) -0.0068(10) 0.0040(10) C10 0.0686(14) 0.0797(17) 0.0576(13) -0.0037(12) -0.0100(11) 0.0091(12) C11 0.0766(16) 0.0822(18) 0.0663(15) -0.0086(13) -0.0116(12) -0.0190(13) C12 0.0735(15) 0.0712(16) 0.0619(14) 0.0014(11) -0.0121(11) -0.0135(12) C13 0.0525(11) 0.0678(14) 0.0581(12) -0.0015(11) -0.0060(9) 0.0010(10) C14 0.0531(11) 0.0621(14) 0.0663(13) 0.0031(11) -0.0088(10) 0.0076(9) C15 0.0480(10) 0.0613(13) 0.0543(11) 0.0065(10) -0.0063(9) 0.0030(9) C16 0.093(9) 0.070(6) 0.101(10) -0.009(6) -0.028(8) 0.018(6) C17 0.0629(13) 0.0605(14) 0.0590(13) 0.0027(10) -0.0062(10) 0.0059(10) C18 0.0748(15) 0.0683(15) 0.0716(15) 0.0075(12) -0.0151(12) 0.0179(12) C19 0.0614(13) 0.0777(16) 0.0589(13) 0.0075(12) -0.0150(10) 0.0069(11) O3A 0.118(7) 0.077(6) 0.071(5) -0.017(4) -0.027(4) 0.032(5) C16A 0.085(6) 0.074(6) 0.068(4) -0.011(3) -0.020(3) 0.016(4) O2A 0.071(6) 0.074(5) 0.055(5) 0.002(4) -0.010(4) 0.012(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 _geom_angle_publ_flag C13 O1 H1 111(2) . . ? C15 O2 C16 107.4(11) . . ? C17 O3 C16 106.0(10) . . ? C3 N2 H2 116.7(16) . . ? C4 N2 H2 116.3(16) . . ? C4 N2 C3 126.76(18) . . ? C11 N3 C10 117.0(2) . . ? N1 C1 C2 178.6(2) . . ? C3 C2 C1 118.26(18) . . ? C7 C2 C1 121.20(18) . . ? C7 C2 C3 120.52(19) . . ? O4 C3 N2 120.41(19) . . ? O4 C3 C2 125.5(2) . . ? N2 C3 C2 114.05(18) . . ? N2 C4 C5 114.55(19) . . ? N2 C4 C6 118.6(2) . . ? C6 C4 C5 126.8(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 117.76(18) . . ? C4 C6 C8 123.32(19) . . ? C7 C6 C8 118.85(18) . . ? C2 C7 C6 122.25(19) . . ? C2 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C9 C8 C6 120.0(2) . . ? C9 C8 C12 117.1(2) . . ? C12 C8 C6 122.9(2) . . ? C8 C9 H9 120.5 . . ? C10 C9 C8 119.1(2) . . ? C10 C9 H9 120.5 . . ? N3 C10 C9 124.0(2) . . ? N3 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? N3 C11 H11 118.3 . . ? N3 C11 C12 123.5(2) . . ? C12 C11 H11 118.3 . . ? C8 C12 H12 120.3 . . ? C11 C12 C8 119.4(2) . . ? C11 C12 H12 120.3 . . ? O1 C13 C14 116.1(2) . . ? O1 C13 C19 123.6(2) . . ? C19 C13 C14 120.4(2) . . ? C13 C14 H14 121.6 . . ? C15 C14 C13 116.7(2) . . ? C15 C14 H14 121.6 . . ? O2 C15 C17 107.5(8) . . ? C14 C15 O2 129.2(8) . . ? C14 C15 C17 123.2(2) . . ? C14 C15 O2A 125.9(5) . . ? O2A C15 C17 110.9(5) . . ? O2 C16 H16A 110.1 . . ? O2 C16 H16B 110.1 . . ? O3 C16 O2 107.9(11) . . ? O3 C16 H16A 110.1 . . ? O3 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? C15 C17 O3 110.7(7) . . ? C15 C17 O3A 109.3(5) . . ? C18 C17 O3 128.4(7) . . ? C18 C17 C15 120.7(2) . . ? C18 C17 O3A 130.0(5) . . ? C17 C18 H18 121.3 . . ? C17 C18 C19 117.5(2) . . ? C19 C18 H18 121.3 . . ? C13 C19 C18 121.6(2) . . ? C13 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C17 O3A C16A 104.5(7) . . ? O3A C16A H16C 109.6 . . ? O3A C16A H16D 109.6 . . ? O3A C16A O2A 110.2(8) . . ? H16C C16A H16D 108.1 . . ? O2A C16A H16C 109.6 . . ? O2A C16A H16D 109.6 . . ? C15 O2A C16A 102.8(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 H1 0.918(18) . ? O1 C13 1.353(3) . ? O2 C15 1.369(10) . ? O2 C16 1.421(12) . ? O3 C16 1.388(12) . ? O3 C17 1.380(11) . ? O4 C3 1.229(2) . ? N1 C1 1.150(3) . ? N2 H2 0.87(3) . ? N2 C3 1.385(3) . ? N2 C4 1.348(3) . ? N3 C10 1.327(3) . ? N3 C11 1.324(3) . ? C1 C2 1.437(3) . ? C2 C3 1.421(3) . ? C2 C7 1.358(3) . ? C4 C5 1.499(3) . ? C4 C6 1.371(3) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.415(3) . ? C6 C8 1.471(3) . ? C7 H7 0.9300 . ? C8 C9 1.382(3) . ? C8 C12 1.390(3) . ? C9 H9 0.9300 . ? C9 C10 1.368(3) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C11 C12 1.369(3) . ? C12 H12 0.9300 . ? C13 C14 1.384(3) . ? C13 C19 1.378(3) . ? C14 H14 0.9300 . ? C14 C15 1.364(3) . ? C15 C17 1.370(3) . ? C15 O2A 1.370(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.353(3) . ? C17 O3A 1.377(8) . ? C18 H18 0.9300 . ? C18 C19 1.390(3) . ? C19 H19 0.9300 . ? O3A C16A 1.393(9) . ? C16A H16C 0.9700 . ? C16A H16D 0.9700 . ? C16A O2A 1.428(9) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C13 C14 C15 -178.7(2) . . . . ? O1 C13 C19 C18 179.1(2) . . . . ? O2 C15 C17 O3 1.8(12) . . . . ? O2 C15 C17 C18 177.2(10) . . . . ? O3 C17 C18 C19 175.6(9) . . . . ? N2 C4 C6 C7 -0.2(3) . . . . ? N2 C4 C6 C8 -177.35(19) . . . . ? N3 C11 C12 C8 0.5(4) . . . . ? C1 C2 C3 O4 1.5(3) . . . . ? C1 C2 C3 N2 -178.65(19) . . . . ? C1 C2 C7 C6 179.6(2) . . . . ? C3 N2 C4 C5 -176.9(2) . . . . ? C3 N2 C4 C6 1.4(3) . . . . ? C3 C2 C7 C6 -1.8(3) . . . . ? C4 N2 C3 O4 177.3(2) . . . . ? C4 N2 C3 C2 -2.6(3) . . . . ? C4 C6 C7 C2 0.4(3) . . . . ? C4 C6 C8 C9 132.5(2) . . . . ? C4 C6 C8 C12 -48.8(3) . . . . ? C5 C4 C6 C7 178.0(2) . . . . ? C5 C4 C6 C8 0.8(4) . . . . ? C6 C8 C9 C10 178.28(19) . . . . ? C6 C8 C12 C11 -179.1(2) . . . . ? C7 C2 C3 O4 -177.2(2) . . . . ? C7 C2 C3 N2 2.7(3) . . . . ? C7 C6 C8 C9 -44.6(3) . . . . ? C7 C6 C8 C12 134.1(2) . . . . ? C8 C6 C7 C2 177.72(19) . . . . ? C8 C9 C10 N3 1.4(4) . . . . ? C9 C8 C12 C11 -0.4(3) . . . . ? C10 N3 C11 C12 0.3(4) . . . . ? C11 N3 C10 C9 -1.3(4) . . . . ? C12 C8 C9 C10 -0.5(3) . . . . ? C13 C14 C15 O2 -177.4(12) . . . . ? C13 C14 C15 C17 -0.1(3) . . . . ? C13 C14 C15 O2A 179.3(7) . . . . ? C14 C13 C19 C18 0.5(4) . . . . ? C14 C15 C17 O3 -176.0(8) . . . . ? C14 C15 C17 C18 -0.6(4) . . . . ? C14 C15 C17 O3A 177.4(7) . . . . ? C14 C15 O2A C16A -169.1(9) . . . . ? C15 O2 C16 O3 7(3) . . . . ? C15 C17 C18 C19 1.1(4) . . . . ? C15 C17 O3A C16A -7.5(11) . . . . ? C16 O2 C15 C14 172.4(16) . . . . ? C16 O2 C15 C17 -5(2) . . . . ? C16 O3 C17 C15 2.4(18) . . . . ? C16 O3 C17 C18 -172.6(16) . . . . ? C17 O3 C16 O2 -6(3) . . . . ? C17 C15 O2A C16A 10.3(12) . . . . ? C17 C18 C19 C13 -1.1(4) . . . . ? C17 O3A C16A O2A 14.2(15) . . . . ? C18 C17 O3A C16A 170.2(8) . . . . ? C19 C13 C14 C15 0.1(3) . . . . ? O3A C17 C18 C19 -176.4(9) . . . . ? O3A C16A O2A C15 -15.2(15) . . . . ? O2A C15 C17 C18 180.0(6) . . . . ? O2A C15 C17 O3A -2.0(9) . . . . ?