#------------------------------------------------------------------------------ #$Date: 2021-06-26 00:36:34 +0300 (Sat, 26 Jun 2021) $ #$Revision: 266690 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/88/4518835.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_4518835 loop_ _publ_author_name 'Gonz\'alez, Bruno' 'Fag\'undez, Catherine' 'Peixoto de Abreu Lima, Alejandro' 'Suescun, Leopoldo' 'Sellanes, Diver' 'Seoane, Gustavo A.' 'Carrera, Ignacio' _publ_section_title ; Efficient Access to the Iboga Skeleton: Optimized Procedure to Obtain Voacangine from Voacanga africana Root Bark ; _journal_name_full 'ACS Omega' _journal_paper_doi 10.1021/acsomega.1c00745 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'Cl, C20 H27 N2 O' _chemical_formula_sum 'C20 H27 Cl N2 O' _chemical_formula_weight 346.88 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-12-10 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-12-10 deposited with the CCDC. 2021-02-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.3860(5) _cell_length_b 10.6137(8) _cell_length_c 18.3018(10) _cell_measurement_reflns_used 4468 _cell_measurement_temperature 100 _cell_measurement_theta_max 66.67 _cell_measurement_theta_min 4.82 _cell_volume 1823.2(2) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker APEXII CCD area detector' _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'Bruker Kappa/ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 25396 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.075 _diffrn_reflns_theta_min 4.816 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_target Mo _diffrn_source_type 'Siemens fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.910 _exptl_absorpt_correction_T_max 0.7530 _exptl_absorpt_correction_T_min 0.5948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1073 before and 0.0778 after correction. The Ratio of minimum to maximum transmission is 0.7899. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.264 _exptl_crystal_description irregular _exptl_crystal_F_000 744 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.201 _exptl_crystal_size_min 0.158 _refine_diff_density_max 0.372 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.053 _refine_ls_abs_structure_details ; Flack x determined using 1201 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.014(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 245 _refine_ls_number_reflns 3318 _refine_ls_number_restraints 76 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0604 _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^)+(0.0562P)^2^+1.6268P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1459 _refine_ls_wR_factor_ref 0.1482 _reflns_Friedel_coverage 0.734 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 3127 _reflns_number_total 3318 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao1c00745_si_001.cif _cod_data_source_block 19_a _cod_database_code 4518835 _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. ; _shelx_estimated_absorpt_t_max 0.752 _shelx_estimated_absorpt_t_min 0.637 _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 2. Restrained distances C18-C19 1.53 with sigma of 0.01 3. Rigid bond restraints C3, C4, C5, N1, C18, C19 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 N1, C5 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02 4. Uiso/Uaniso restraints and constraints C3 \\sim C4 \\sim C5 \\sim N1 \\sim C19 \\sim C18: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C17 \\sim C18 \\sim C19 \\sim C18A \\sim C19A: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 5. Same fragment restrains {C17, C18A, C19A} sigma for 1-2: 0.005, 1-3: 0.04 as {C17, C18, C19} 6. Others Sof(H17A)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19D)=Sof(H19E)= Sof(H19F)=1-FVAR(1) Sof(H17)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)= FVAR(1) 7.a Ternary CH refined with riding coordinates: C15(H15), C9(H9), C10(H10), C17(H17), C17(H17A) 7.b Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A, H16B), C18(H18A,H18B), C18A(H18C,H18D) 7.c Me refined with riding coordinates: C20(H20A,H20B,H20C) 7.d Aromatic/amide H refined with riding coordinates: C1(H1A), C3(H3), C4(H4) 7.e Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F) ; _shelx_res_file ; TITL 19_a.res in P2(1)2(1)2(1) 19_a.res created by SHELXL-2016/6 at 09:15:18 on 10-Dec-2020 REM Old TITL 19 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.216, Rweak 0.039, Alpha 0.012, Orientation as input REM Flack x = 0.075 ( 0.012 ) from Parsons' quotients REM Formula found by SHELXT: C20 N2 O Cl H27 REM ##### CELL 1.54178 9.386 10.6137 18.3018 90 90 90 ZERR 4 0.0005 0.0008 0.001 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl N O UNIT 80 108 4 8 4 DFIX 1.53 0.01 C18 C19 DELU C3 C4 C5 N1 C18 C19 DELU 0.02 0.02 N1 C5 SIMU 0.04 0.08 1.7 C3 C4 C5 N1 C19 C18 SIMU 0.005 0.01 2 C17 C18 C19 C18A C19A L.S. 50 PLAN 20 SIZE 0.158 0.201 0.26 TEMP -173.16 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.056200 1.626800 FVAR 0.85262 0.70413 CL1 3 0.991101 0.695940 0.628646 11.00000 0.03083 0.10839 = 0.03668 0.00365 0.00435 0.00225 O1 5 0.225078 0.214206 0.335763 11.00000 0.06050 0.08144 = 0.07276 0.03296 -0.01956 -0.03062 N2 4 0.676417 0.661880 0.603962 11.00000 0.02489 0.08714 = 0.02814 0.01690 0.00535 0.01014 H2 2 0.756894 0.665265 0.629118 11.00000 0.05629 N1 4 0.236366 0.510464 0.582207 11.00000 0.03330 0.08024 = 0.06551 0.02137 0.01643 0.00080 H1 2 0.165498 0.546273 0.606301 11.00000 -1.20000 C7 1 0.442825 0.506949 0.520695 11.00000 0.02564 0.06629 = 0.04737 0.02385 0.00525 0.00266 C11 1 0.702610 0.551177 0.554509 11.00000 0.02510 0.08050 = 0.03805 0.02272 0.00707 0.00802 AFIX 23 H11A 2 0.708890 0.474545 0.585180 11.00000 -1.20000 H11B 2 0.796595 0.562861 0.530909 11.00000 -1.20000 AFIX 0 C6 1 0.342842 0.429077 0.482982 11.00000 0.03406 0.06073 = 0.05402 0.02609 0.00496 -0.00220 C12 1 0.593697 0.527493 0.495255 11.00000 0.02757 0.07526 = 0.03971 0.01900 0.00740 -0.00042 AFIX 23 H12A 2 0.594543 0.600250 0.461409 11.00000 -1.20000 H12B 2 0.623905 0.452488 0.467077 11.00000 -1.20000 AFIX 0 C8 1 0.374022 0.557389 0.579918 11.00000 0.02612 0.07500 = 0.05663 0.02606 0.01180 0.00394 C15 1 0.537925 0.859435 0.610797 11.00000 0.04215 0.07481 = 0.03487 0.00832 0.00326 0.01150 AFIX 13 H15 2 0.526282 0.945805 0.589799 11.00000 -1.20000 AFIX 0 C13 1 0.644901 0.784401 0.565201 11.00000 0.04257 0.08024 = 0.03231 0.01240 0.00734 0.00673 AFIX 23 H13A 2 0.604817 0.767185 0.516172 11.00000 -1.20000 H13B 2 0.733794 0.833481 0.559067 11.00000 -1.20000 AFIX 0 C5 1 0.214869 0.433215 0.523581 11.00000 0.03001 0.07046 = 0.08693 0.03523 0.01217 -0.00393 C9 1 0.416934 0.653062 0.635654 11.00000 0.02602 0.08942 = 0.03737 0.01503 0.00998 0.01097 AFIX 13 H9 2 0.351927 0.641423 0.678414 11.00000 -1.20000 AFIX 0 C1 1 0.351476 0.355571 0.419147 11.00000 0.03683 0.06205 = 0.06374 0.03369 -0.00206 -0.00315 AFIX 43 H1A 2 0.437291 0.351714 0.391714 11.00000 -1.20000 AFIX 0 C10 1 0.569278 0.639875 0.664785 11.00000 0.02968 0.10229 = 0.03209 0.02667 0.01035 0.01618 AFIX 13 H10 2 0.582896 0.553589 0.685588 11.00000 -1.20000 AFIX 0 C14 1 0.396685 0.790602 0.609233 11.00000 0.03679 0.08424 = 0.04082 -0.00058 -0.00351 0.02220 AFIX 23 H14A 2 0.358176 0.790733 0.558874 11.00000 -1.20000 H14B 2 0.327566 0.834284 0.641293 11.00000 -1.20000 AFIX 0 C2 1 0.232674 0.289358 0.397356 11.00000 0.04940 0.07109 = 0.06352 0.02802 -0.01128 -0.02187 C3 1 0.105165 0.292470 0.438891 11.00000 0.04122 0.07502 = 0.11086 0.04125 -0.00515 -0.02034 AFIX 43 H3 2 0.025282 0.244270 0.423571 11.00000 -1.20000 AFIX 0 C4 1 0.096078 0.364556 0.501091 11.00000 0.04292 0.08451 = 0.09452 0.02961 0.01279 -0.01381 AFIX 43 H4 2 0.010050 0.367561 0.528383 11.00000 -1.20000 AFIX 0 C16 1 0.594548 0.868550 0.688831 11.00000 0.04232 0.11792 = 0.03476 0.00770 0.00006 -0.00347 AFIX 23 H16A 2 0.534643 0.927358 0.717451 11.00000 -1.20000 H16B 2 0.693102 0.901766 0.688216 11.00000 -1.20000 AFIX 0 C20 1 0.352073 0.207368 0.292567 11.00000 0.08784 0.12498 = 0.04671 0.01339 -0.01173 -0.04202 AFIX 33 H20A 2 0.335669 0.152138 0.250489 11.00000 -1.50000 H20B 2 0.377470 0.291878 0.275371 11.00000 -1.50000 H20C 2 0.429981 0.173409 0.322282 11.00000 -1.50000 AFIX 0 SAME 0.005 0.04 C17 C18A C19A C17 1 0.592731 0.738384 0.724563 11.00000 0.03454 0.11583 = 0.02871 0.01077 0.00622 0.01072 PART 1 AFIX 13 H17 2 0.507629 0.735481 0.757393 21.00000 -1.20000 AFIX 13 PART 0 PART 2 H17A 2 0.504191 0.736546 0.754936 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C18 1 0.728451 0.733329 0.774911 21.00000 0.03390 0.09819 = 0.02747 0.00877 0.00116 0.00385 AFIX 23 H18A 2 0.815610 0.739895 0.744686 21.00000 -1.20000 H18B 2 0.727210 0.804954 0.809557 21.00000 -1.20000 AFIX 0 C19 1 0.729128 0.610186 0.816689 21.00000 0.04254 0.09955 = 0.04117 0.02509 0.00088 0.00682 AFIX 137 H19A 2 0.723317 0.539725 0.782213 21.00000 -1.50000 H19B 2 0.647159 0.607600 0.849823 21.00000 -1.50000 H19C 2 0.817347 0.603538 0.845070 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C18A 1 0.707863 0.664380 0.770307 -21.00000 0.03410 0.10178 = 0.02764 0.00753 0.00424 0.00477 AFIX 23 H18C 2 0.670560 0.583207 0.788857 -21.00000 -1.20000 H18D 2 0.795947 0.649368 0.741854 -21.00000 -1.20000 AFIX 0 C19A 1 0.731150 0.758578 0.831239 -21.00000 0.03638 0.09322 = 0.03251 0.00055 -0.00416 0.00874 AFIX 137 H19D 2 0.805147 0.727196 0.864343 -21.00000 -1.50000 H19E 2 0.642122 0.770150 0.858398 -21.00000 -1.50000 H19F 2 0.761259 0.839378 0.810428 -21.00000 -1.50000 AFIX 0 HKLF 4 REM 19_a.res in P2(1)2(1)2(1) REM R1 = 0.0604 for 3127 Fo > 4sig(Fo) and 0.0632 for all 3318 data REM 245 parameters refined using 76 restraints END WGHT 0.0562 1.6269 REM Highest difference peak 0.372, deepest hole -0.366, 1-sigma level 0.053 Q1 1 0.9991 0.6153 0.6578 11.00000 0.05 0.37 Q2 1 0.5364 0.0184 0.2095 11.00000 0.05 0.26 Q3 1 0.5737 0.6635 0.7134 11.00000 0.05 0.26 Q4 1 0.5768 0.7895 0.6921 11.00000 0.05 0.26 Q5 1 0.2499 0.1541 0.3129 11.00000 0.05 0.25 Q6 1 0.4852 0.7990 0.6163 11.00000 0.05 0.23 Q7 1 0.2431 0.2239 0.3677 11.00000 0.05 0.22 Q8 1 0.0928 0.2989 0.4727 11.00000 0.05 0.22 Q9 1 0.2246 0.4357 0.5606 11.00000 0.05 0.22 Q10 1 0.9760 0.7622 0.6556 11.00000 0.05 0.20 Q11 1 0.4187 0.4628 0.2395 11.00000 0.05 0.20 Q12 1 0.3505 0.3633 0.4616 11.00000 0.05 0.20 Q13 1 0.0137 0.5313 0.6810 11.00000 0.05 0.19 Q14 1 0.0693 0.3428 0.4305 11.00000 0.05 0.18 Q15 1 0.4020 0.5806 0.6249 11.00000 0.05 0.18 Q16 1 0.5693 0.5548 0.6681 11.00000 0.05 0.17 Q17 1 0.3990 0.6657 0.6896 11.00000 0.05 0.17 Q18 1 0.1105 0.2482 0.4174 11.00000 0.05 0.16 Q19 1 0.7438 0.5645 0.7881 11.00000 0.05 0.16 Q20 1 0.2219 0.3838 0.5030 11.00000 0.05 0.16 ; _shelx_res_checksum 95909 _shelx_hkl_file ; 1 0 0 -0.10 0.90 1 0 0 -0.30 0.60 -1 0 0 0.40 0.90 -1 0 0 0.20 0.50 2 0 0 536.15 30.90 2 0 0 546.55 29.10 -2 0 0 551.44 27.70 -2 0 0 548.45 30.60 3 0 0 -1.80 1.60 -3 0 0 -0.10 1.30 -3 0 0 -1.00 1.90 3 0 0 0.80 2.90 4 0 0 12.60 4.20 -4 0 0 14.40 5.90 4 0 0 10.20 5.60 -4 0 0 14.20 3.60 -5 0 0 2.60 3.90 5 0 0 -3.10 6.70 5 0 0 0.20 3.30 -6 0 0 341.67 30.90 6 0 0 329.57 27.50 -7 0 0 1.30 3.00 -7 0 0 0.70 3.10 -7 0 0 0.40 8.10 -7 0 0 7.70 3.80 7 0 0 5.10 5.20 -7 0 0 1.30 3.30 7 0 0 5.70 3.60 -8 0 0 319.87 21.10 8 0 0 364.26 28.00 -8 0 0 328.87 22.40 -8 0 0 318.97 22.90 -8 0 0 318.07 23.20 8 0 0 356.66 24.50 9 0 0 -1.00 2.80 -9 0 0 1.70 2.80 -9 0 0 0.80 2.90 -9 0 0 0.70 3.20 -9 0 0 1.90 3.00 9 0 0 2.70 4.90 -10 0 0 261.57 18.50 10 0 0 256.97 21.50 -10 0 0 269.17 18.00 -10 0 0 255.37 18.00 10 0 0 278.27 19.70 11 0 0 0.20 2.60 -11 0 0 0.20 1.80 -11 0 0 -0.20 2.10 11 0 0 2.30 2.60 -11 0 0 2.40 2.00 0 0 1 3.50 0.70 0 0 1 0.20 0.30 0 0 -1 0.40 0.80 -1 0 1 3159.88 147.39 -1 0 1 3138.29 148.29 1 0 1 3096.69 147.89 1 0 -1 3050.19 147.39 -1 0 -1 3016.00 147.49 1 0 -1 3280.57 149.88 -1 0 -1 3287.97 148.79 2 0 1 1159.68 59.89 -2 0 1 1209.48 60.99 -2 0 1 1192.38 58.39 2 0 1 1208.98 59.59 -2 0 -1 1189.18 58.59 -2 0 -1 1216.88 61.29 2 0 -1 1158.68 59.09 2 0 -1 1265.97 62.79 -3 0 1 2662.43 124.59 3 0 1 2474.85 123.49 3 0 1 2397.26 121.69 -3 0 1 2430.46 119.69 3 0 -1 2523.35 121.59 -3 0 -1 2438.26 119.09 3 0 -1 2523.35 125.89 -3 0 -1 2544.75 124.69 4 0 1 219.48 19.90 -4 0 1 255.67 20.80 4 0 1 238.98 18.30 -4 0 1 227.88 15.70 -4 0 -1 266.77 21.30 -4 0 -1 233.68 15.30 4 0 -1 263.57 22.90 4 0 -1 245.58 18.20 -5 0 1 813.12 51.19 -5 0 1 735.43 50.09 5 0 1 842.52 48.60 5 0 1 783.62 50.99 5 0 -1 823.02 48.10 -5 0 -1 821.72 52.29 5 0 -1 828.12 54.39 6 0 1 364.46 28.60 -6 0 1 309.57 30.00 -6 0 -1 338.67 30.70 7 0 1 1624.14 85.39 -7 0 1 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0 -1 15.60 3.40 -11 0 -1 15.90 3.70 11 0 -1 10.80 4.10 11 0 -1 12.90 3.70 -11 0 -1 16.30 3.10 0 0 2 4678.83 212.88 0 0 2 4456.45 212.98 0 0 -2 4553.44 214.98 -1 0 2 2941.01 143.09 -1 0 2 3075.09 142.99 1 0 2 3149.28 143.49 -1 0 -2 2864.41 143.59 -1 0 -2 3021.70 143.89 1 0 -2 3164.48 146.39 -2 0 2 3.40 1.70 2 0 2 2.70 1.90 2 0 2 2.60 1.70 -2 0 2 5.80 2.60 -2 0 -2 3.70 1.80 -2 0 -2 2.00 1.90 2 0 -2 -0.30 2.80 -3 0 2 291.87 18.30 3 0 2 316.47 20.30 -3 0 2 312.87 21.30 3 0 2 294.67 20.10 -3 0 -2 303.07 22.10 -3 0 -2 307.57 18.30 3 0 -2 320.77 19.60 3 0 -2 298.97 24.20 -4 0 2 847.62 50.39 -4 0 2 873.71 45.80 4 0 2 813.02 49.70 4 0 2 892.11 48.90 4 0 -2 902.61 55.09 4 0 -2 900.61 48.10 -4 0 -2 818.02 44.30 -4 0 -2 886.51 51.99 -5 0 2 27.50 6.10 5 0 2 23.90 7.50 -5 0 2 33.50 9.60 -5 0 -2 37.60 10.70 5 0 -2 18.30 9.80 6 0 2 34.60 10.20 -6 0 2 34.50 10.90 6 0 -2 48.20 15.40 -6 0 -2 25.00 10.70 -7 0 2 755.82 54.99 -7 0 2 691.03 38.60 7 0 2 817.82 52.79 -7 0 2 688.23 40.00 7 0 2 717.23 45.00 -7 0 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11 6.80 2.00 3 -10 11 5.10 2.40 3 -10 11 9.90 2.60 3 -10 -11 0.50 3.50 2 -10 11 16.10 3.30 -2 10 11 9.70 2.30 2 -10 11 8.50 2.70 2 -10 11 14.30 3.70 2 -10 -11 3.30 4.50 2 -10 -11 10.40 4.40 2 -10 -11 0.20 4.50 -1 10 11 1.50 1.90 1 -10 11 1.00 1.80 1 -10 11 1.50 2.40 1 -10 11 0.90 2.40 1 -10 11 3.10 2.40 1 -10 -11 2.00 3.60 1 -10 -11 2.60 4.60 1 -10 -11 3.00 6.80 0 -10 11 8.80 3.40 0 -10 11 4.60 2.90 0 -10 11 6.50 2.80 0 -10 11 6.50 3.00 0 -10 -11 4.60 4.20 0 -10 -11 4.10 6.60 0 -10 -11 9.20 3.80 0 -10 -11 3.50 5.30 1 10 11 -0.50 2.00 -1 -10 11 -3.20 2.40 -1 -10 11 1.90 2.50 -1 -10 11 1.30 1.90 -1 -10 11 2.30 2.30 -1 -10 -11 2.80 3.00 -1 -10 -11 -0.60 3.30 -1 -10 -11 -0.60 6.70 -1 -10 -11 -0.90 3.40 -2 -10 11 8.00 3.00 -2 -10 11 12.10 3.40 -2 -10 11 8.50 2.70 -2 -10 11 12.50 3.50 2 10 11 14.00 3.20 -2 -10 -11 6.00 7.70 -2 -10 -11 5.40 5.80 -2 -10 -11 13.90 4.50 -2 -10 -11 2.60 3.20 3 10 11 5.70 2.40 -3 -10 11 3.40 2.10 -3 -10 11 3.60 2.30 -3 -10 11 5.50 2.70 -3 -10 11 10.20 3.20 -3 -10 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6.60 -2 -11 -5 9.50 7.80 -2 -11 -5 10.30 3.90 -3 -11 5 3.70 3.50 -3 -11 5 -0.60 1.90 -3 -11 5 -0.20 2.20 -3 -11 5 0.40 1.60 -3 -11 -5 0.60 2.80 -3 -11 -5 -1.20 5.00 -3 -11 -5 0.60 3.00 -3 -11 -5 3.20 3.20 -3 -11 -5 0.50 5.20 -4 -11 5 1.30 2.30 -4 -11 5 3.30 3.30 -4 -11 5 5.10 2.00 -4 -11 5 3.60 2.50 -4 -11 -5 3.00 5.60 -4 -11 -5 -3.70 2.60 -4 -11 -5 0.40 2.20 -4 -11 -5 3.70 3.10 4 11 -5 -6.00 2.90 -4 -11 -5 3.10 2.20 -4 -11 -5 -2.90 2.60 -5 -11 5 8.00 3.50 -5 -11 -5 7.50 3.30 -5 -11 -5 9.10 3.10 -5 -11 -5 4.70 2.60 4 -11 6 2.50 2.30 4 -11 6 6.40 3.00 4 -11 -6 5.70 3.10 4 -11 -6 0.40 2.70 3 -11 6 3.50 2.30 3 -11 6 4.00 2.90 3 -11 6 8.60 2.90 3 -11 -6 8.30 3.80 3 -11 -6 3.30 4.50 3 -11 -6 7.40 3.60 2 -11 6 2.60 2.90 2 -11 6 0.40 2.30 2 -11 6 4.20 2.50 2 -11 6 3.80 3.10 2 -11 -6 2.30 4.90 2 -11 -6 3.20 3.20 2 -11 -6 1.50 3.40 2 -11 -6 0.10 3.80 1 -11 6 16.40 4.40 1 -11 6 19.40 4.20 1 -11 6 13.00 4.40 1 -11 6 16.40 4.30 1 -11 -6 3.30 4.70 1 -11 -6 5.90 5.50 1 -11 -6 10.50 4.80 0 -11 6 18.00 4.80 0 -11 6 13.00 3.50 0 -11 6 12.20 3.70 0 -11 6 13.10 3.40 0 -11 6 16.10 5.10 0 -11 6 14.10 3.90 0 -11 -6 5.40 5.40 0 -11 -6 8.10 4.60 0 -11 -6 22.70 6.00 0 -11 -6 4.80 6.00 -1 -11 6 10.20 3.90 -1 -11 6 9.80 3.60 -1 -11 6 11.00 3.30 -1 -11 6 12.90 3.80 -1 -11 6 11.30 3.30 -1 -11 6 16.10 5.00 -1 -11 -6 2.70 4.80 -1 -11 -6 9.80 4.20 -1 -11 -6 7.50 4.60 -1 -11 -6 9.90 8.00 -2 -11 6 7.40 3.00 -2 -11 6 5.90 3.20 -2 -11 6 1.30 3.60 -2 -11 6 5.60 2.70 -2 -11 6 2.60 2.90 -2 -11 6 3.10 2.20 -2 -11 -6 5.30 4.10 -2 -11 -6 3.90 6.80 -2 -11 -6 5.90 3.50 -2 -11 -6 0.90 5.20 -2 -11 -6 8.40 3.80 -3 -11 6 12.10 3.40 -3 -11 6 8.90 3.10 -3 -11 6 11.60 3.00 -3 -11 6 13.10 4.50 -3 -11 -6 8.90 4.00 -3 -11 -6 7.20 3.90 -3 -11 -6 8.20 6.60 -3 -11 -6 4.80 6.50 -3 -11 -6 11.20 3.80 -3 -11 -6 4.70 2.00 -4 -11 6 1.70 2.10 -4 -11 6 1.80 2.40 -4 -11 6 0.40 1.90 -4 -11 6 5.70 3.60 -4 -11 -6 1.30 1.70 -4 -11 -6 7.30 3.40 -4 -11 -6 -0.40 5.50 -4 -11 -6 4.60 2.80 -4 -11 -6 1.70 3.00 4 11 -6 4.20 3.50 4 -11 7 -0.70 1.90 4 -11 -7 4.20 2.80 3 -11 7 5.80 2.50 3 -11 7 6.50 3.20 3 -11 7 4.90 2.30 3 -11 -7 1.70 3.90 3 -11 -7 8.30 3.90 3 -11 -7 7.30 3.50 2 -11 7 18.60 4.30 2 -11 7 11.30 3.90 2 -11 7 15.10 3.40 2 -11 7 14.60 3.90 2 -11 -7 8.90 4.30 2 -11 -7 2.60 4.10 2 -11 -7 2.20 4.90 1 -11 7 2.90 2.80 1 -11 7 3.90 2.60 1 -11 7 -0.30 1.70 1 -11 7 0.20 2.30 1 -11 -7 -0.40 3.20 1 -11 -7 -1.60 3.70 1 -11 -7 2.20 3.00 1 -11 -7 0.30 4.10 0 -11 7 9.00 3.20 0 -11 7 9.50 3.40 0 -11 7 8.40 3.60 0 -11 7 11.80 3.80 0 -11 7 6.90 2.70 0 -11 -7 -2.10 3.90 0 -11 -7 4.80 4.00 0 -11 -7 2.30 5.40 -1 -11 7 4.60 2.70 -1 -11 7 2.30 2.10 -1 -11 7 1.60 2.90 -1 -11 7 4.40 2.80 -1 -11 7 3.30 2.30 -1 -11 -7 2.10 4.10 -1 -11 -7 0.40 3.20 -1 -11 -7 2.70 7.70 -1 -11 -7 1.40 3.70 -2 -11 7 3.00 2.40 -2 -11 7 3.20 2.90 -2 -11 7 7.20 2.60 -2 -11 7 8.90 3.30 -2 -11 7 2.80 2.30 -2 -11 7 8.20 4.30 -2 -11 -7 3.90 6.10 -2 -11 -7 10.40 4.20 -2 -11 -7 0.40 4.70 -2 -11 -7 3.70 3.00 -2 -11 -7 8.00 3.70 -3 -11 7 7.20 2.30 -3 -11 7 -0.10 3.30 -3 -11 7 4.50 2.60 -3 -11 7 4.60 2.40 -3 -11 -7 -2.60 5.20 -3 -11 -7 1.20 2.70 -3 -11 -7 2.40 3.30 -3 -11 -7 0.70 5.70 -3 -11 -7 5.60 3.20 -4 -11 7 4.50 2.20 -4 -11 7 3.70 2.50 -4 -11 -7 7.10 3.00 -4 -11 -7 6.80 3.00 -4 -11 -7 5.70 3.10 4 -11 8 5.00 2.50 3 -11 8 0.60 2.20 3 -11 8 2.30 2.40 3 -11 8 -0.90 1.70 3 -11 -8 1.10 2.90 3 -11 -8 -0.40 3.30 2 -11 8 12.80 3.10 2 -11 8 12.30 3.60 2 -11 8 9.40 3.40 2 -11 8 11.70 3.40 2 -11 -8 2.30 4.80 2 -11 -8 12.60 4.40 2 -11 -8 2.10 4.20 1 -11 8 -0.20 2.20 1 -11 8 0.20 2.50 1 -11 8 -1.20 1.60 1 -11 8 -0.90 2.30 1 -11 -8 7.00 4.00 1 -11 -8 0.40 3.70 1 -11 -8 -0.70 4.30 0 -11 8 36.60 5.70 0 -11 8 26.30 4.70 0 -11 8 29.90 5.30 0 -11 8 45.90 5.90 0 -11 8 26.10 5.00 0 -11 -8 12.00 8.60 0 -11 -8 31.00 5.90 0 -11 -8 8.60 6.20 -1 -11 8 -0.80 2.00 -1 -11 8 3.00 2.30 -1 -11 8 2.80 2.20 -1 -11 8 0.10 2.40 -1 -11 -8 -1.80 4.40 -1 -11 -8 1.20 3.50 -1 -11 -8 -2.80 5.90 -1 -11 -8 -3.30 2.80 -2 -11 8 7.90 3.30 -2 -11 8 8.90 2.80 -2 -11 8 2.60 2.30 -2 -11 8 4.40 2.30 -2 -11 -8 -0.20 4.10 -2 -11 -8 7.70 3.20 -2 -11 -8 4.50 6.40 -2 -11 -8 7.60 3.80 -3 -11 8 2.80 2.30 -3 -11 8 1.50 1.90 -3 -11 -8 -1.30 2.30 -3 -11 -8 -0.90 2.70 -3 -11 -8 0.50 3.00 -3 -11 -8 0.20 5.10 -3 -11 -8 2.30 7.40 -4 -11 -8 4.00 4.70 3 -11 9 14.20 3.50 3 -11 9 10.90 2.70 3 -11 -9 3.50 4.60 2 -11 9 4.00 2.70 2 -11 9 3.20 2.00 2 -11 9 4.20 2.40 2 -11 -9 -3.30 3.90 2 -11 -9 1.20 3.80 1 -11 9 0.00 2.10 1 -11 9 2.80 2.60 1 -11 9 0.50 1.80 1 -11 9 1.10 2.50 1 -11 -9 -0.50 3.50 1 -11 -9 -0.50 4.20 1 -11 -9 -1.70 3.30 0 -11 9 29.70 5.10 0 -11 9 23.00 4.60 0 -11 9 24.10 4.20 0 -11 9 25.90 4.30 0 -11 -9 25.20 5.40 0 -11 -9 15.90 8.90 0 -11 -9 7.60 5.30 -1 -11 9 1.10 2.00 -1 -11 9 -0.10 2.10 -1 -11 9 3.20 2.10 -1 -11 9 0.60 2.40 -1 -11 -9 0.20 4.00 -1 -11 -9 7.50 4.20 -1 -11 -9 3.60 3.40 -1 -11 -9 -2.30 6.30 -2 -11 9 1.10 2.00 -2 -11 9 4.60 2.40 -2 -11 9 3.00 2.30 -2 -11 9 5.00 2.80 -2 -11 -9 -0.70 2.90 -2 -11 -9 4.60 2.80 -2 -11 -9 2.90 3.60 -2 -11 -9 -0.80 5.80 -3 -11 9 10.40 2.90 -3 -11 9 10.10 2.90 -3 -11 -9 8.60 3.20 -3 -11 -9 7.10 3.50 2 -11 10 3.60 2.00 2 -11 10 2.50 2.30 2 -11 10 4.90 2.60 2 -11 -10 -0.30 2.90 1 -11 10 3.10 2.40 1 -11 10 2.80 2.50 1 -11 10 1.70 2.00 1 -11 10 6.60 3.00 1 -11 -10 0.70 4.10 1 -11 -10 4.90 5.50 1 -11 -10 -1.70 3.80 0 -11 10 7.50 2.50 0 -11 10 9.70 3.20 0 -11 10 8.10 2.60 0 -11 -10 7.60 3.60 0 -11 -10 2.00 6.40 0 -11 -10 5.40 4.50 -1 -11 10 13.10 3.10 -1 -11 10 11.60 2.90 -1 -11 10 7.90 2.90 -1 -11 -10 2.00 3.00 -1 -11 -10 10.60 7.00 -1 -11 -10 1.80 5.40 -1 -11 -10 2.10 3.90 -2 -11 10 7.10 2.40 -2 -11 -10 6.80 5.50 -2 -11 -10 1.80 3.70 -2 -11 -10 7.80 3.10 1 -11 11 1.70 1.90 1 -11 11 2.40 2.80 0 -11 11 0.90 2.20 0 -11 11 -2.20 1.60 0 -11 11 -0.20 1.50 0 -11 -11 1.60 3.90 -1 -11 -11 1.80 5.10 3 -12 0 -0.20 3.00 3 -12 0 7.40 3.10 2 -12 0 -2.60 2.30 2 -12 0 -5.00 2.70 2 -12 0 0.70 2.70 1 -12 0 4.60 3.00 1 -12 0 3.10 3.70 0 -12 0 7.20 2.60 0 -12 0 11.50 4.40 0 -12 0 11.30 3.80 -1 -12 0 0.30 1.60 -1 -12 0 3.40 3.00 -1 -12 0 -3.50 2.60 -2 -12 0 3.40 2.60 -2 -12 0 4.60 2.20 -2 -12 0 6.30 3.90 -2 -12 0 0.40 3.50 -2 -12 0 3.30 2.70 -3 -12 0 6.50 3.80 -3 -12 0 8.50 3.60 -3 -12 0 5.50 2.80 -3 -12 0 6.30 3.50 -3 -12 0 6.90 2.30 3 -12 1 7.20 3.40 3 -12 1 3.90 3.00 3 -12 1 3.70 3.20 3 -12 -1 8.80 3.50 3 -12 -1 8.60 3.50 2 -12 1 10.70 3.60 2 -12 1 9.90 4.00 2 -12 1 11.10 4.20 2 -12 -1 6.70 3.50 2 -12 -1 9.40 3.90 2 -12 -1 4.30 3.40 1 -12 1 7.50 3.40 1 -12 1 10.20 4.30 1 -12 -1 -0.90 3.80 1 -12 -1 2.90 3.50 1 -12 -1 0.50 3.10 1 -12 -1 2.90 3.00 0 -12 1 3.60 2.30 0 -12 1 5.80 3.80 0 -12 1 -0.30 2.60 0 -12 -1 2.00 3.50 0 -12 -1 1.10 1.90 0 -12 -1 3.30 3.40 0 -12 -1 0.50 4.10 0 -12 -1 -0.90 2.60 -1 -12 1 8.00 2.40 -1 -12 1 6.10 3.10 -1 -12 1 5.70 3.20 -1 -12 1 13.50 3.90 -1 -12 -1 8.10 2.30 -1 -12 -1 3.90 3.30 -1 -12 -1 2.00 4.40 -2 -12 1 19.50 4.20 -2 -12 1 14.70 4.40 -2 -12 1 11.60 3.40 -2 -12 1 16.30 3.40 -2 -12 -1 16.80 4.10 -2 -12 -1 13.80 3.60 -2 -12 -1 12.40 4.60 -2 -12 -1 8.10 4.00 -2 -12 -1 3.50 4.60 -2 -12 -1 11.80 2.80 -3 -12 1 5.30 3.80 -3 -12 1 3.50 2.70 -3 -12 1 3.50 2.30 -3 -12 1 2.00 1.70 -3 -12 1 2.80 3.20 -3 -12 -1 4.40 2.00 -3 -12 -1 2.20 3.40 -3 -12 -1 1.40 2.70 -3 -12 -1 2.00 3.10 -3 -12 -1 0.10 2.10 3 -12 2 4.40 2.60 3 -12 2 3.10 3.00 3 -12 2 3.40 3.00 3 -12 -2 -1.60 2.40 3 -12 -2 -1.90 2.90 2 -12 2 1.10 2.60 2 -12 2 2.10 3.40 2 -12 2 1.70 3.00 2 -12 -2 -1.30 3.20 2 -12 -2 -1.80 4.40 2 -12 -2 2.70 3.10 1 -12 2 14.10 4.10 1 -12 2 4.20 4.10 1 -12 -2 5.00 4.60 1 -12 -2 13.80 4.90 1 -12 -2 0.30 4.10 0 -12 2 9.80 3.70 0 -12 2 11.90 3.10 0 -12 2 14.40 4.00 0 -12 -2 3.20 4.30 0 -12 -2 0.40 3.20 0 -12 -2 9.80 2.50 0 -12 -2 15.90 4.80 -1 -12 2 20.60 4.30 -1 -12 2 19.20 3.70 -1 -12 2 10.00 3.40 -1 -12 2 13.70 3.80 -1 -12 -2 6.20 5.20 -1 -12 -2 0.90 3.00 -2 -12 2 4.50 2.20 -2 -12 2 12.10 3.40 -2 -12 2 6.00 4.10 -2 -12 2 8.10 3.00 -2 -12 -2 10.00 4.00 -2 -12 -2 1.00 3.70 -2 -12 -2 2.40 3.30 -2 -12 -2 5.50 3.00 -2 -12 -2 7.30 2.30 -3 -12 2 6.30 3.50 -3 -12 2 2.30 2.40 -3 -12 2 4.70 2.10 -3 -12 2 7.10 2.60 -3 -12 -2 8.40 3.30 -3 -12 -2 3.40 2.60 -3 -12 -2 5.40 2.00 -3 -12 -2 0.20 3.10 3 -12 3 2.90 2.90 3 -12 3 1.80 2.20 3 -12 -3 2.60 2.80 2 -12 3 8.30 3.40 2 -12 3 12.40 3.90 2 -12 3 5.50 3.90 2 -12 -3 0.80 3.90 2 -12 -3 7.30 3.60 1 -12 3 13.60 3.40 1 -12 3 6.80 3.50 1 -12 -3 -0.40 4.00 1 -12 -3 14.00 4.60 1 -12 -3 0.90 3.60 0 -12 3 3.10 2.90 0 -12 3 3.60 2.30 0 -12 3 4.60 2.90 0 -12 -3 1.60 4.10 0 -12 -3 1.60 3.30 0 -12 -3 4.50 1.80 -1 -12 3 7.60 3.10 -1 -12 3 4.90 2.90 -1 -12 3 6.20 2.40 -1 -12 3 7.10 3.10 -1 -12 -3 5.20 1.90 -1 -12 -3 2.80 4.20 -1 -12 -3 3.80 4.40 -1 -12 -3 5.50 3.90 -2 -12 3 1.20 2.40 -2 -12 3 6.00 2.10 -2 -12 3 4.00 3.80 -2 -12 3 3.10 2.50 -2 -12 -3 1.40 3.90 -2 -12 -3 0.00 2.60 -2 -12 -3 2.70 1.70 -2 -12 -3 5.40 3.70 -2 -12 -3 1.40 3.10 -3 -12 3 2.60 2.60 -3 -12 3 5.70 3.60 -3 -12 3 3.60 2.00 -3 -12 3 5.70 2.60 -3 -12 -3 2.60 4.30 -3 -12 -3 3.20 3.00 -3 -12 -3 3.60 1.70 -3 -12 -3 3.00 3.10 -3 -12 -3 2.20 3.10 3 -12 4 2.40 2.50 3 -12 4 7.30 3.40 3 -12 -4 0.90 2.90 2 -12 4 4.90 2.30 2 -12 4 13.80 3.60 2 -12 4 6.60 3.30 2 -12 -4 1.90 3.70 2 -12 -4 4.60 3.20 1 -12 4 14.60 3.40 1 -12 4 16.60 4.00 1 -12 4 18.50 4.30 1 -12 -4 12.00 3.80 1 -12 -4 4.50 4.80 0 -12 4 2.10 2.40 0 -12 4 4.50 2.10 0 -12 4 4.20 2.90 0 -12 4 7.40 3.10 0 -12 -4 2.20 4.40 0 -12 -4 2.80 1.70 0 -12 -4 0.30 3.30 -1 -12 4 14.60 3.90 -1 -12 4 12.00 3.30 -1 -12 4 15.90 3.90 -1 -12 4 12.10 3.10 -1 -12 -4 2.10 4.70 -1 -12 -4 10.90 4.00 -1 -12 -4 6.80 2.20 -1 -12 -4 7.40 4.80 -2 -12 4 10.50 2.60 -2 -12 4 4.40 2.60 -2 -12 4 6.50 2.90 -2 -12 4 9.00 4.30 -2 -12 -4 7.20 6.30 -2 -12 -4 6.90 3.40 -2 -12 -4 2.50 1.80 -2 -12 -4 12.60 4.20 -2 -12 -4 1.70 3.70 -3 -12 4 5.30 2.50 -3 -12 4 5.60 2.70 -3 -12 -4 5.10 3.60 -3 -12 -4 11.80 5.60 2 -12 5 3.40 3.10 2 -12 5 8.30 3.10 2 -12 5 5.50 2.40 2 -12 -5 6.20 3.20 2 -12 -5 1.30 3.70 1 -12 5 1.70 2.00 1 -12 5 -0.10 2.50 1 -12 5 4.70 2.60 1 -12 -5 0.50 3.20 1 -12 -5 -1.90 3.50 1 -12 -5 3.40 2.90 0 -12 5 0.20 2.10 0 -12 5 3.50 2.60 0 -12 5 0.90 2.20 0 -12 -5 -1.30 2.70 0 -12 -5 1.50 4.20 -1 -12 5 1.60 2.30 -1 -12 5 0.50 2.40 -1 -12 5 -2.30 2.10 -1 -12 5 2.80 2.00 -1 -12 -5 1.20 3.90 -1 -12 -5 -0.30 4.70 -1 -12 -5 2.00 3.10 -2 -12 5 4.50 2.10 -2 -12 5 2.00 2.30 -2 -12 5 3.70 2.40 -2 -12 -5 6.90 5.30 -2 -12 -5 5.80 3.20 -2 -12 -5 -0.30 3.70 -2 -12 -5 3.70 6.10 2 -12 6 0.90 1.90 2 -12 6 -1.40 2.10 2 -12 -6 5.20 3.20 1 -12 6 3.70 3.70 1 -12 6 1.90 2.50 1 -12 6 2.00 2.10 1 -12 -6 0.20 4.10 1 -12 -6 0.30 2.90 0 -12 6 2.00 2.00 0 -12 6 2.00 2.30 0 -12 6 -0.60 2.20 0 -12 -6 1.80 4.00 0 -12 -6 -0.40 3.30 -1 -12 6 4.20 2.60 -1 -12 6 4.60 2.60 -1 -12 6 0.10 2.40 -1 -12 -6 4.90 4.30 -1 -12 -6 3.50 5.30 -2 -12 6 1.40 2.10 -2 -12 6 3.50 3.00 -2 -12 -6 3.00 3.70 1 -12 7 1.40 2.50 1 -12 7 3.50 3.30 1 -12 -7 1.20 3.80 0 -12 7 0.20 2.00 0 -12 7 0.00 2.40 0 -12 -7 0.40 3.60 0 -12 -7 -0.10 3.90 -1 -12 7 -0.40 1.90 -1 -12 -7 0.20 3.50 -1 -12 -7 2.00 5.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 49374 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' '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 Cl1 Cl 0.99110(12) 0.69594(16) 0.62865(6) 0.0586(4) Uani 1 1 d . . . . . O1 O 0.2251(5) 0.2142(5) 0.3358(2) 0.0716(13) Uani 1 1 d . . . . . N2 N 0.6764(4) 0.6619(5) 0.6040(2) 0.0467(11) Uani 1 1 d . . . . . H2 H 0.757(7) 0.665(5) 0.629(3) 0.056(16) Uiso 1 1 d . . . . . N1 N 0.2364(5) 0.5105(5) 0.5822(3) 0.0597(12) Uani 1 1 d . U . . . H1 H 0.165(8) 0.546(7) 0.606(4) 0.072 Uiso 1 1 d R . . . . C7 C 0.4428(5) 0.5069(5) 0.5207(3) 0.0464(12) Uani 1 1 d . . . . . C11 C 0.7026(5) 0.5512(6) 0.5545(3) 0.0479(13) Uani 1 1 d . . . . . H11A H 0.708890 0.474545 0.585180 0.057 Uiso 1 1 calc R . . . . H11B H 0.796595 0.562861 0.530909 0.057 Uiso 1 1 calc R . . . . C6 C 0.3428(5) 0.4291(5) 0.4830(3) 0.0496(13) Uani 1 1 d . . . . . C12 C 0.5937(5) 0.5275(6) 0.4953(3) 0.0475(12) Uani 1 1 d . . . . . H12A H 0.594543 0.600250 0.461409 0.057 Uiso 1 1 calc R . . . . H12B H 0.623905 0.452488 0.467077 0.057 Uiso 1 1 calc R . . . . C8 C 0.3740(5) 0.5574(6) 0.5799(3) 0.0526(13) Uani 1 1 d . . . . . C15 C 0.5379(5) 0.8594(6) 0.6108(3) 0.0506(13) Uani 1 1 d . . . . . H15 H 0.526282 0.945805 0.589799 0.061 Uiso 1 1 calc R . . . . C13 C 0.6449(5) 0.7844(6) 0.5652(3) 0.0517(13) Uani 1 1 d . . . . . H13A H 0.604817 0.767185 0.516172 0.062 Uiso 1 1 calc R . . . . H13B H 0.733794 0.833481 0.559067 0.062 Uiso 1 1 calc R . . . . C5 C 0.2149(5) 0.4332(6) 0.5236(4) 0.0625(16) Uani 1 1 d . U . . . C9 C 0.4169(5) 0.6531(6) 0.6357(3) 0.0509(13) Uani 1 1 d . . . . . H9 H 0.351927 0.641423 0.678414 0.061 Uiso 1 1 calc R . . . . C1 C 0.3515(6) 0.3556(5) 0.4191(3) 0.0542(14) Uani 1 1 d . . . . . H1A H 0.437291 0.351714 0.391714 0.065 Uiso 1 1 calc R . . . . C10 C 0.5693(5) 0.6399(6) 0.6648(3) 0.0547(15) Uani 1 1 d . . . . . H10 H 0.582896 0.553589 0.685588 0.066 Uiso 1 1 calc R . . . . C14 C 0.3967(5) 0.7906(6) 0.6092(3) 0.0540(13) Uani 1 1 d . . . . . H14A H 0.358176 0.790733 0.558874 0.065 Uiso 1 1 calc R . . . . H14B H 0.327566 0.834284 0.641293 0.065 Uiso 1 1 calc R . . . . C2 C 0.2327(6) 0.2894(6) 0.3974(3) 0.0613(15) Uani 1 1 d . . . . . C3 C 0.1052(6) 0.2925(7) 0.4389(5) 0.0757(19) Uani 1 1 d . U . . . H3 H 0.025282 0.244270 0.423571 0.091 Uiso 1 1 calc R . . . . C4 C 0.0961(7) 0.3646(7) 0.5011(4) 0.0740(18) Uani 1 1 d . U . . . H4 H 0.010050 0.367561 0.528383 0.089 Uiso 1 1 calc R . . . . C16 C 0.5945(6) 0.8685(7) 0.6888(3) 0.0650(17) Uani 1 1 d . . . . . H16A H 0.534643 0.927358 0.717451 0.078 Uiso 1 1 calc R . . . . H16B H 0.693102 0.901766 0.688216 0.078 Uiso 1 1 calc R . . . . C20 C 0.3521(8) 0.2074(9) 0.2926(3) 0.087(2) Uani 1 1 d . . . . . H20A H 0.335669 0.152138 0.250489 0.130 Uiso 1 1 calc R . . . . H20B H 0.377470 0.291878 0.275371 0.130 Uiso 1 1 calc R . . . . H20C H 0.429981 0.173409 0.322282 0.130 Uiso 1 1 calc R . . . . C17 C 0.5927(5) 0.7384(7) 0.7246(3) 0.0597(15) Uani 1 1 d D U . . . H17 H 0.507629 0.735481 0.757393 0.072 Uiso 0.704(10) 1 calc R . P A 1 H17A H 0.504191 0.736546 0.754936 0.072 Uiso 0.296(10) 1 calc R . P A 2 C18 C 0.7285(7) 0.7333(9) 0.7749(4) 0.0532(18) Uani 0.704(10) 1 d D U P A 1 H18A H 0.815610 0.739895 0.744686 0.064 Uiso 0.704(10) 1 calc R . P A 1 H18B H 0.727210 0.804954 0.809557 0.064 Uiso 0.704(10) 1 calc R . P A 1 C19 C 0.7291(9) 0.6102(9) 0.8167(4) 0.061(2) Uani 0.704(10) 1 d D U P A 1 H19A H 0.723317 0.539725 0.782213 0.092 Uiso 0.704(10) 1 calc GR . P A 1 H19B H 0.647159 0.607600 0.849823 0.092 Uiso 0.704(10) 1 calc GR . P A 1 H19C H 0.817347 0.603538 0.845070 0.092 Uiso 0.704(10) 1 calc GR . P A 1 C18A C 0.7079(18) 0.6644(16) 0.7703(8) 0.055(3) Uani 0.296(10) 1 d D U P A 2 H18C H 0.670560 0.583207 0.788857 0.065 Uiso 0.296(10) 1 calc R . P A 2 H18D H 0.795947 0.649368 0.741854 0.065 Uiso 0.296(10) 1 calc R . P A 2 C19A C 0.7312(18) 0.7586(19) 0.8312(8) 0.054(3) Uani 0.296(10) 1 d D U P A 2 H19D H 0.805147 0.727196 0.864343 0.081 Uiso 0.296(10) 1 calc GR . P A 2 H19E H 0.642122 0.770150 0.858398 0.081 Uiso 0.296(10) 1 calc GR . P A 2 H19F H 0.761259 0.839378 0.810428 0.081 Uiso 0.296(10) 1 calc GR . 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 Cl1 0.0308(5) 0.1084(11) 0.0367(5) 0.0036(6) 0.0044(4) 0.0023(6) O1 0.061(2) 0.081(3) 0.073(3) 0.033(2) -0.020(2) -0.031(2) N2 0.0249(18) 0.087(3) 0.0281(18) 0.0169(19) 0.0054(15) 0.010(2) N1 0.033(2) 0.080(3) 0.066(3) 0.021(3) 0.016(2) 0.001(2) C7 0.026(2) 0.066(3) 0.047(3) 0.024(2) 0.0053(19) 0.003(2) C11 0.025(2) 0.080(4) 0.038(2) 0.023(2) 0.0071(19) 0.008(2) C6 0.034(2) 0.061(3) 0.054(3) 0.026(3) 0.005(2) -0.002(2) C12 0.028(2) 0.075(3) 0.040(2) 0.019(2) 0.0074(19) 0.000(2) C8 0.026(2) 0.075(3) 0.057(3) 0.026(3) 0.012(2) 0.004(2) C15 0.042(3) 0.075(3) 0.035(2) 0.008(2) 0.0033(19) 0.012(2) C13 0.043(2) 0.080(4) 0.032(2) 0.012(2) 0.007(2) 0.007(3) C5 0.030(2) 0.070(4) 0.087(4) 0.035(3) 0.012(3) -0.004(2) C9 0.026(2) 0.089(4) 0.037(2) 0.015(3) 0.0100(19) 0.011(2) C1 0.037(2) 0.062(3) 0.064(3) 0.034(3) -0.002(2) -0.003(2) C10 0.030(2) 0.102(4) 0.032(2) 0.027(3) 0.0103(19) 0.016(3) C14 0.037(2) 0.084(4) 0.041(2) -0.001(3) -0.004(2) 0.022(3) C2 0.049(3) 0.071(4) 0.064(3) 0.028(3) -0.011(3) -0.022(3) C3 0.041(3) 0.075(4) 0.111(5) 0.041(4) -0.005(3) -0.020(3) C4 0.043(3) 0.085(4) 0.095(5) 0.030(4) 0.013(3) -0.014(3) C16 0.042(3) 0.118(5) 0.035(3) 0.008(3) 0.000(2) -0.003(3) C20 0.088(5) 0.125(6) 0.047(3) 0.013(4) -0.012(3) -0.042(5) C17 0.035(2) 0.116(4) 0.029(2) 0.011(2) 0.0062(19) 0.011(3) C18 0.034(3) 0.098(5) 0.027(3) 0.009(3) 0.001(2) 0.004(3) C19 0.043(4) 0.100(5) 0.041(4) 0.025(4) 0.001(3) 0.007(4) C18A 0.034(4) 0.102(6) 0.028(4) 0.008(5) 0.004(4) 0.005(5) C19A 0.036(6) 0.093(8) 0.033(6) 0.001(6) -0.004(5) 0.009(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2 O1 C20 115.9(5) . . ? C11 N2 H2 102(4) . . ? C11 N2 C13 115.0(3) . . ? C11 N2 C10 115.4(4) . . ? C13 N2 H2 112(4) . . ? C13 N2 C10 110.3(4) . . ? C10 N2 H2 101(4) . . ? C8 N1 H1 124(5) . . ? C5 N1 H1 123(4) . . ? C5 N1 C8 109.3(5) . . ? C6 C7 C12 123.5(5) . . ? C8 C7 C6 107.4(4) . . ? C8 C7 C12 129.1(5) . . ? N2 C11 H11A 108.1 . . ? N2 C11 H11B 108.1 . . ? N2 C11 C12 116.8(4) . . ? H11A C11 H11B 107.3 . . ? C12 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? C5 C6 C7 106.6(5) . . ? C1 C6 C7 133.2(5) . . ? C1 C6 C5 120.2(5) . . ? C7 C12 C11 116.0(4) . . ? C7 C12 H12A 108.3 . . ? C7 C12 H12B 108.3 . . ? C11 C12 H12A 108.3 . . ? C11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? N1 C8 C9 118.4(5) . . ? C7 C8 N1 108.8(6) . . ? C7 C8 C9 132.7(4) . . ? C13 C15 H15 109.8 . . ? C14 C15 H15 109.8 . . ? C14 C15 C13 108.3(5) . . ? C14 C15 C16 110.7(4) . . ? C16 C15 H15 109.8 . . ? C16 C15 C13 108.4(4) . . ? N2 C13 C15 108.7(4) . . ? N2 C13 H13A 109.9 . . ? N2 C13 H13B 109.9 . . ? C15 C13 H13A 109.9 . . ? C15 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N1 C5 C6 107.8(5) . . ? N1 C5 C4 131.6(6) . . ? C4 C5 C6 120.6(7) . . ? C8 C9 H9 106.6 . . ? C8 C9 C10 115.3(5) . . ? C8 C9 C14 113.2(4) . . ? C10 C9 H9 106.6 . . ? C10 C9 C14 108.0(5) . . ? C14 C9 H9 106.6 . . ? C6 C1 H1A 120.8 . . ? C2 C1 C6 118.5(5) . . ? C2 C1 H1A 120.8 . . ? N2 C10 C9 110.4(3) . . ? N2 C10 H10 109.6 . . ? N2 C10 C17 108.9(5) . . ? C9 C10 H10 109.6 . . ? C17 C10 C9 108.7(4) . . ? C17 C10 H10 109.6 . . ? C15 C14 C9 110.0(4) . . ? C15 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C9 C14 H14A 109.7 . . ? C9 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? O1 C2 C3 114.0(5) . . ? C1 C2 O1 124.9(6) . . ? C1 C2 C3 121.1(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 C2 120.6(6) . . ? C4 C3 H3 119.7 . . ? C5 C4 H4 120.5 . . ? C3 C4 C5 119.1(6) . . ? C3 C4 H4 120.5 . . ? C15 C16 H16A 109.7 . . ? C15 C16 H16B 109.7 . . ? C15 C16 C17 109.8(5) . . ? H16A C16 H16B 108.2 . . ? C17 C16 H16A 109.7 . . ? C17 C16 H16B 109.7 . . ? O1 C20 H20A 109.5 . . ? O1 C20 H20B 109.5 . . ? O1 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C10 C17 H17 107.1 . . ? C10 C17 H17A 105.3 . . ? C10 C17 C18 120.8(5) . . ? C10 C17 C18A 97.9(7) . . ? C16 C17 C10 108.3(4) . . ? C16 C17 H17 107.1 . . ? C16 C17 H17A 105.3 . . ? C16 C17 C18 105.8(5) . . ? C16 C17 C18A 132.1(9) . . ? C18 C17 H17 107.1 . . ? C18A C17 H17A 105.3 . . ? C17 C18 H18A 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? C19 C18 C17 109.2(6) . . ? C19 C18 H18A 109.8 . . ? C19 C18 H18B 109.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C18A H18C 111.9 . . ? C17 C18A H18D 111.9 . . ? H18C C18A H18D 109.6 . . ? C19A C18A C17 99.3(9) . . ? C19A C18A H18C 111.9 . . ? C19A C18A H18D 111.9 . . ? C18A C19A H19D 109.5 . . ? C18A C19A H19E 109.5 . . ? C18A C19A H19F 109.5 . . ? H19D C19A H19E 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? 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 C2 1.383(8) . ? O1 C20 1.432(9) . ? N2 H2 0.89(6) . ? N2 C11 1.503(8) . ? N2 C13 1.511(7) . ? N2 C10 1.518(5) . ? N1 H1 0.88(7) . ? N1 C8 1.385(7) . ? N1 C5 1.365(9) . ? C7 C6 1.428(8) . ? C7 C12 1.507(6) . ? C7 C8 1.371(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.511(7) . ? C6 C5 1.413(7) . ? C6 C1 1.407(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C8 C9 1.495(9) . ? C15 H15 1.0000 . ? C15 C13 1.529(7) . ? C15 C14 1.514(8) . ? C15 C16 1.527(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C5 C4 1.394(10) . ? C9 H9 1.0000 . ? C9 C10 1.532(6) . ? C9 C14 1.550(8) . ? C1 H1A 0.9500 . ? C1 C2 1.377(8) . ? C10 H10 1.0000 . ? C10 C17 1.529(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C2 C3 1.418(9) . ? C3 H3 0.9500 . ? C3 C4 1.374(11) . ? C4 H4 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.529(10) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C17 H17 1.0000 . ? C17 H17A 1.0000 . ? C17 C18 1.573(7) . ? C17 C18A 1.577(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.514(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18A H18C 0.9900 . ? C18A H18D 0.9900 . ? C18A C19A 1.514(10) . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ?