#------------------------------------------------------------------------------ #$Date: 2020-04-21 02:36:04 +0300 (Tue, 21 Apr 2020) $ #$Revision: 250963 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240346.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_7240346 loop_ _publ_author_name 'Pereira Copetti, Jo\~ao Pedro' 'Salbego, Paulo Roberto dos Santos' 'Orlando, Tain\'ara' 'Rosa, J\'essica Maria Luis' 'Fiss, Gabriela Fehn' 'Gomes de Oliveira, Jo\~ao Paulo' 'de Almeida Vasconcellos, M\'ario Luiz Ara\'ujo' 'Zanatta, Nilo' 'Bonacorso, Helio Gauze' 'Martins, Marcos A. P.' _publ_section_title ; Substituent Effects in the Crystallization Mechanisms of 7-chloro-4-substituted-Quinolines ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00214C _journal_year 2020 _chemical_absolute_configuration none _chemical_formula_moiety 'C11 H10 Cl N O2' _chemical_formula_sum 'C11 H10 Cl N O2' _chemical_formula_weight 223.65 _chemical_melting_point ? _chemical_name_common 2-((7-chloroquinolin-4-yl)oxy)ethan-1-ol _chemical_name_systematic 2-((7-chloroquinolin-4-yl)oxy)ethan-1-ol _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-04-10 deposited with the CCDC. 2020-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.074(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.3139(2) _cell_length_b 25.5732(14) _cell_length_c 9.5710(5) _cell_measurement_reflns_used 6819 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 25.20 _cell_measurement_theta_min 2.32 _cell_volume 1032.52(9) _computing_cell_refinement 'BRUKER SAINT' _computing_data_collection 'BRUKER APEX-III' _computing_data_reduction 'BRUKER SOFTWARE' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 297(2) _diffrn_detector_area_resol_mean none _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 VENTURE Photon 100 diffractometer' _diffrn_measurement_method '2\%\f & \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0414 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 17777 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.128 _diffrn_reflns_theta_min 2.317 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.7057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 464 _exptl_crystal_size_max 0.247 _exptl_crystal_size_mid 0.123 _exptl_crystal_size_min 0.052 _exptl_transmission_factor_max none _exptl_transmission_factor_min none _refine_diff_density_max 0.226 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Flack x determined using 1410 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.026(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 273 _refine_ls_number_reflns 4540 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0411 _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^)+(0.0389P)^2^+0.1493P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.0844 _reflns_Friedel_coverage 0.941 _reflns_Friedel_fraction_full 0.988 _reflns_Friedel_fraction_max 0.981 _reflns_number_gt 3560 _reflns_number_total 4540 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00214c2.cif _cod_data_source_block shelx_CCDC1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value 'none' was changed to '?' -- the value is undefined or not given. data item '_exptl_crystal_density_meas' value 'none' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7240346 _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. ; _shelx_estimated_absorpt_t_min 0.919 _shelx_estimated_absorpt_t_max 0.982 _exptl_absorpt_special_details ; SADABS (version 2012/1; Bruker, 2012) was used to perform the numerical absortion correction based on the indexed faces of the crystal. ; _shelx_res_file ; TITL MMV0593_0m_a.res in P2(1) shelx.res created by SHELXL-2018/3 at 06:56:29 on 10-Apr-2020 CELL 0.71073 4.3139 25.5732 9.5710 90.000 102.074 90.000 ZERR 4.00 0.0002 0.0014 0.0005 0.000 0.002 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O CL UNIT 44 40 4 8 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.052 0.123 0.247 ACTA BOND $H CONF L.S. 15 TEMP 24.45 WGHT 0.038900 0.149300 FVAR 1.38230 CL1 5 1.295122 0.490357 1.006869 11.00000 0.04749 0.06201 = 0.04764 0.00676 0.00493 0.01185 CL1' 5 1.067073 0.310325 0.943439 11.00000 0.08758 0.07727 = 0.07266 0.01939 -0.00350 0.01306 O44 4 0.045795 0.670142 0.353574 11.00000 0.04425 0.07563 = 0.02861 -0.00476 -0.00184 0.00347 AFIX 147 H44 2 -0.054194 0.663504 0.272849 11.00000 -1.50000 AFIX 0 O41 4 0.219133 0.654071 0.648072 11.00000 0.04475 0.04541 = 0.02429 -0.00032 0.00032 0.00546 O44' 4 0.200169 0.562327 0.393030 11.00000 0.04176 0.06758 = 0.05550 -0.00418 0.00045 0.01180 AFIX 147 H44' 2 0.180351 0.594223 0.390291 11.00000 -1.50000 AFIX 0 C4A 1 0.589820 0.616811 0.834823 11.00000 0.03362 0.03795 = 0.02639 -0.00154 0.00636 -0.00736 N1 3 0.705648 0.657146 1.071406 11.00000 0.04709 0.04860 = 0.02673 -0.00806 0.00216 -0.00437 C8 1 0.977661 0.578945 1.031701 11.00000 0.03456 0.05437 = 0.02431 0.00344 0.00275 -0.00595 AFIX 43 H8 2 1.088810 0.579420 1.126085 11.00000 -1.20000 AFIX 0 O41' 4 0.113612 0.456521 0.466723 11.00000 0.07022 0.06503 = 0.04463 0.00971 0.00223 0.00801 C43 1 -0.167174 0.679489 0.444336 11.00000 0.03561 0.05701 = 0.03992 -0.00412 -0.00181 0.00563 AFIX 23 H43A 2 -0.286189 0.647907 0.453086 11.00000 -1.20000 H43B 2 -0.316130 0.706622 0.403740 11.00000 -1.20000 AFIX 0 C42 1 0.011871 0.696151 0.588957 11.00000 0.04480 0.04417 = 0.03200 0.00263 0.00582 0.00515 AFIX 23 H42A 2 0.134381 0.727389 0.580778 11.00000 -1.20000 H42B 2 -0.134515 0.703879 0.650536 11.00000 -1.20000 AFIX 0 C4 1 0.370991 0.657572 0.785703 11.00000 0.03510 0.04116 = 0.02642 0.00000 0.00557 -0.00716 C5 1 0.650899 0.575253 0.746955 11.00000 0.03737 0.04741 = 0.02469 -0.00159 0.00454 -0.00340 AFIX 43 H5 2 0.541333 0.573548 0.652430 11.00000 -1.20000 AFIX 0 C6 1 0.867224 0.537857 0.798800 11.00000 0.04127 0.04710 = 0.03337 -0.00356 0.00913 -0.00293 AFIX 43 H6 2 0.909124 0.510959 0.740019 11.00000 -1.20000 AFIX 0 C7 1 1.026302 0.540240 0.941558 11.00000 0.03186 0.04369 = 0.03471 0.00518 0.00764 -0.00121 C3 1 0.329929 0.696412 0.878894 11.00000 0.04807 0.03925 = 0.03908 -0.00456 0.00348 0.00373 AFIX 43 H3 2 0.191415 0.723995 0.849018 11.00000 -1.20000 AFIX 0 C2 1 0.501373 0.693587 1.020087 11.00000 0.05580 0.04751 = 0.03448 -0.01223 0.00484 -0.00145 AFIX 43 H2 2 0.466950 0.719811 1.082430 11.00000 -1.20000 AFIX 0 C8A 1 0.755168 0.618422 0.979338 11.00000 0.03237 0.04362 = 0.02674 0.00024 0.00598 -0.00932 C43' 1 -0.096302 0.539063 0.385671 11.00000 0.04058 0.08242 = 0.05007 0.02017 0.01486 0.01757 AFIX 23 H43C 2 -0.254296 0.556728 0.314259 11.00000 -1.20000 H43D 2 -0.157647 0.542285 0.477182 11.00000 -1.20000 AFIX 0 C42' 1 -0.081165 0.482836 0.347555 11.00000 0.04933 0.07515 = 0.04902 0.01916 -0.00115 -0.00138 AFIX 23 H42C 2 -0.292349 0.467833 0.327073 11.00000 -1.20000 H42D 2 0.009070 0.479115 0.263376 11.00000 -1.20000 AFIX 0 C4' 1 0.204532 0.407147 0.449429 11.00000 0.06228 0.05020 = 0.04834 0.00682 0.00954 -0.01663 C4A' 1 0.408401 0.385171 0.570072 11.00000 0.05108 0.04272 = 0.04404 0.00143 0.01430 -0.01068 C8A' 1 0.520160 0.333363 0.557802 11.00000 0.07158 0.04338 = 0.04812 -0.00318 0.01773 -0.01401 C8' 1 0.724919 0.310712 0.675843 11.00000 0.07164 0.03834 = 0.06083 0.00310 0.02306 -0.00080 AFIX 43 H8' 2 0.799694 0.276836 0.670136 11.00000 -1.20000 AFIX 0 C7' 1 0.811992 0.338478 0.797336 11.00000 0.05033 0.04790 = 0.05490 0.00869 0.00858 -0.00130 C3' 1 0.126184 0.377327 0.328463 11.00000 0.10963 0.06596 = 0.04582 0.00332 -0.00993 -0.02504 AFIX 43 H3' 2 -0.006278 0.390426 0.246633 11.00000 -1.20000 AFIX 0 C2' 1 0.249079 0.327009 0.330659 11.00000 0.17841 0.05865 = 0.05159 -0.01044 -0.00113 -0.02739 AFIX 43 H2' 2 0.190342 0.307543 0.247234 11.00000 -1.20000 AFIX 0 N1' 3 0.436974 0.304401 0.436855 11.00000 0.14244 0.04898 = 0.05358 -0.00730 0.00947 -0.01069 C5' 1 0.503047 0.411485 0.699362 11.00000 0.06432 0.04218 = 0.04926 -0.00427 0.00594 0.00372 AFIX 43 H5' 2 0.429271 0.445199 0.708827 11.00000 -1.20000 AFIX 0 C6' 1 0.700149 0.388853 0.811187 11.00000 0.07070 0.05022 = 0.04570 -0.00525 0.00362 0.00304 AFIX 43 H6' 2 0.760863 0.406833 0.897022 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM MMV0593_0m_a.res in P2(1) REM wR2 = 0.0844, GooF = S = 1.021, Restrained GooF = 1.021 for all data REM R1 = 0.0411 for 3560 Fo > 4sig(Fo) and 0.0624 for all 4540 data REM 273 parameters refined using 1 restraints END WGHT 0.0382 0.1534 REM Highest difference peak 0.226, deepest hole -0.183, 1-sigma level 0.035 Q1 1 1.0491 0.3063 0.8516 11.00000 0.05 0.23 Q2 1 0.8665 0.3105 0.9764 11.00000 0.05 0.15 Q3 1 0.4098 0.3545 0.5749 11.00000 0.05 0.14 Q4 1 0.5366 0.6423 0.8049 11.00000 0.05 0.14 Q5 1 1.2232 0.4861 1.1001 11.00000 0.05 0.13 Q6 1 1.3467 0.4779 0.9028 11.00000 0.05 0.13 Q7 1 0.6975 0.6193 0.9021 11.00000 0.05 0.13 Q8 1 0.7373 0.6558 1.1737 11.00000 0.05 0.13 Q9 1 -0.0173 0.3092 0.2335 11.00000 0.05 0.13 Q10 1 0.8511 0.3327 0.7128 11.00000 0.05 0.13 Q11 1 -0.1204 0.3933 0.2868 11.00000 0.05 0.13 Q12 1 0.9085 0.5421 1.0089 11.00000 0.05 0.12 Q13 1 0.7258 0.6117 0.7877 11.00000 0.05 0.12 Q14 1 0.5567 0.5978 0.8173 11.00000 0.05 0.12 Q15 1 0.4098 0.6817 0.8270 11.00000 0.05 0.12 Q16 1 0.2759 0.3124 0.2114 11.00000 0.05 0.12 Q17 1 -0.3690 0.4937 0.1743 11.00000 0.05 0.12 Q18 1 0.3767 0.3966 0.6455 11.00000 0.05 0.12 Q19 1 0.0887 0.4709 0.5587 11.00000 0.05 0.12 Q20 1 0.9893 0.5233 0.7377 11.00000 0.05 0.12 ; _shelx_res_checksum 219 _shelx_hkl_file ; -1 0 0 3465.25 97.19 -1 0 0 3570.14 97.69 -1 0 0 3414.76 97.19 1 0 0 3484.65 97.69 2 0 0 180.48 9.40 -2 0 0 163.18 7.80 -2 0 0 164.58 8.70 -2 0 0 175.58 7.80 -3 0 0 119.19 11.90 -3 0 0 122.39 13.10 -3 0 0 120.39 8.70 3 0 0 122.39 10.40 4 0 0 76.59 13.10 -4 0 0 64.19 10.70 -4 0 0 69.49 10.40 -4 0 0 70.39 9.10 -5 0 0 -7.30 10.40 -5 0 0 10.80 18.00 -5 0 0 8.90 13.60 -5 0 0 12.50 16.20 -1 -1 0 1456.55 41.40 1 -1 0 1515.35 41.70 1 -1 0 1472.05 42.40 -1 -1 0 1492.25 41.90 -1 -1 0 1544.75 41.90 -1 -1 0 1512.65 42.20 1 -1 0 1419.26 41.70 1 1 0 1481.15 41.40 -1 1 0 1487.65 42.30 -1 1 0 1432.76 41.20 -1 1 0 1482.25 41.70 -1 1 0 1477.95 41.70 1 1 0 1449.15 42.20 -2 -1 0 104.39 6.70 -2 -1 0 111.09 6.50 2 -1 0 93.29 8.00 -2 -1 0 99.29 7.80 -2 1 0 101.89 7.40 -2 1 0 106.79 6.20 -2 1 0 109.69 5.80 2 1 0 99.69 7.30 3 -1 0 256.97 15.10 -3 -1 0 255.87 14.80 -3 -1 0 268.77 12.70 -3 -1 0 258.07 11.70 -3 1 0 268.77 12.30 -3 1 0 279.37 11.90 -3 1 0 272.67 13.80 3 1 0 238.88 15.20 -3 1 0 270.57 12.80 -4 -1 0 21.50 9.80 -4 -1 0 23.90 9.70 -4 -1 0 18.80 8.10 -4 1 0 14.80 10.00 -4 1 0 14.20 7.20 4 1 0 45.30 11.70 -4 1 0 31.40 9.20 -5 -1 0 3.40 11.50 -5 -1 0 2.90 13.00 -5 -1 0 18.40 17.20 -5 1 0 21.20 13.30 -5 1 0 2.40 17.10 -5 1 0 5.20 11.50 -5 1 0 -5.60 14.60 1 -2 0 975.20 27.50 -1 -2 0 989.80 28.20 -1 -2 0 947.61 27.80 1 -2 0 963.80 27.70 -1 2 0 972.90 28.20 1 2 0 952.60 27.70 -1 2 0 994.70 27.70 -1 2 0 952.60 27.50 1 2 0 993.40 28.20 -1 2 0 985.40 28.40 -1 2 0 928.51 27.50 -2 -2 0 591.44 19.80 2 -2 0 610.24 20.50 -2 -2 0 630.44 19.20 2 -2 0 600.84 18.80 -2 -2 0 592.84 17.70 -2 -2 0 588.04 19.10 2 -2 0 615.04 18.70 -2 2 0 585.14 19.40 -2 2 0 610.24 19.90 2 2 0 598.24 19.80 -2 2 0 587.34 18.60 -2 2 0 638.64 18.60 2 2 0 582.94 17.40 3 -2 0 243.58 14.90 -3 -2 0 206.18 12.60 -3 -2 0 214.88 11.80 -3 -2 0 217.28 13.10 3 2 0 233.78 14.50 -3 2 0 241.88 11.00 -3 2 0 240.88 11.30 -3 2 0 274.77 13.30 -3 2 0 235.98 13.40 -4 -2 0 10.00 8.20 -4 -2 0 22.60 10.30 -4 2 0 8.40 6.80 -4 2 0 23.10 9.30 -4 2 0 15.40 8.30 4 2 0 31.20 11.50 -5 -2 0 81.79 13.00 -5 -2 0 70.69 18.80 -5 -2 0 56.59 13.20 -5 2 0 48.60 14.30 -5 2 0 55.79 11.30 -5 2 0 65.89 21.90 -5 2 0 59.29 15.80 0 -3 0 1.00 1.30 0 3 0 -1.60 1.60 -1 -3 0 2145.49 58.59 -1 -3 0 2086.99 57.99 1 -3 0 2099.59 58.59 -1 -3 0 2034.20 58.49 1 -3 0 2021.00 57.89 1 -3 0 2053.39 58.09 -1 3 0 2098.89 58.19 1 3 0 2136.19 58.69 -1 3 0 2106.99 58.39 -1 3 0 2002.60 58.69 -1 3 0 2091.19 58.99 -1 3 0 2006.60 57.99 1 3 0 2042.40 58.49 -2 -3 0 1016.60 29.50 -2 -3 0 981.60 29.90 2 -3 0 980.20 28.70 -2 -3 0 981.70 29.50 -2 -3 0 984.50 28.60 2 -3 0 972.40 28.90 2 3 0 963.20 28.20 -2 3 0 948.21 29.60 2 3 0 1001.90 30.20 -2 3 0 1014.80 28.80 -2 3 0 942.11 31.50 -2 3 0 953.80 27.70 -2 3 0 951.70 28.80 -3 -3 0 1285.57 39.30 -3 -3 0 1239.98 39.60 -3 -3 0 1296.47 40.80 -3 3 0 1326.37 38.80 -3 3 0 1307.27 38.90 -3 3 0 1333.07 41.00 3 3 0 1335.17 41.40 -3 3 0 1279.77 40.20 -4 -3 0 12.70 9.50 -4 -3 0 13.70 7.70 -4 3 0 4.10 8.10 4 3 0 7.90 11.20 -4 3 0 9.20 7.50 -4 3 0 -0.40 9.40 -5 -3 0 11.90 12.30 -5 -3 0 8.30 12.20 -5 3 0 0.60 14.10 5 3 0 7.00 19.50 -5 3 0 8.20 14.70 -5 3 0 12.00 11.10 0 -4 0 4057.79 110.99 0 -4 0 3770.32 110.09 0 4 0 4053.99 110.49 0 4 0 3930.61 110.79 -1 -4 0 2265.57 65.19 -1 -4 0 2387.06 64.89 1 -4 0 2438.26 64.49 -1 -4 0 2332.37 64.09 1 -4 0 2340.77 65.09 1 -4 0 2398.86 64.29 1 4 0 2317.27 65.19 -1 4 0 2328.97 64.49 -1 4 0 2058.79 65.59 1 4 0 2074.99 65.39 -1 4 0 2357.86 64.99 -1 4 0 2267.87 64.29 -2 -4 0 174.88 8.20 -2 -4 0 185.68 10.20 2 -4 0 170.28 7.00 -2 -4 0 157.38 8.20 -2 -4 0 191.08 8.30 2 -4 0 176.28 7.30 2 4 0 168.18 8.80 -2 4 0 160.28 7.00 2 4 0 150.48 7.30 -2 4 0 155.38 7.70 -2 4 0 162.58 8.90 -2 4 0 169.28 7.80 -3 -4 0 101.19 9.10 -3 -4 0 103.69 10.90 -3 -4 0 109.49 9.00 -3 4 0 104.69 9.00 -3 4 0 101.89 8.50 3 4 0 111.79 9.70 -3 4 0 90.09 10.10 -3 4 0 100.29 8.20 -4 -4 0 18.80 13.30 -4 -4 0 17.50 9.00 -4 -4 0 -7.20 10.80 -4 4 0 15.60 9.10 -4 4 0 6.90 7.00 4 4 0 8.80 10.50 -4 4 0 11.60 9.80 -5 -4 0 103.89 13.50 -5 -4 0 111.89 14.70 -5 4 0 111.99 17.10 -5 4 0 112.79 13.10 -5 4 0 144.99 18.30 5 4 0 128.49 20.80 0 -5 0 3.80 3.00 0 -5 0 -2.10 2.30 0 5 0 0.60 2.80 -1 -5 0 2131.39 60.99 1 -5 0 2132.09 61.19 1 -5 0 2286.97 62.19 1 -5 0 2245.88 61.49 -1 -5 0 2160.88 62.59 1 -5 0 2213.68 62.19 1 5 0 2102.39 61.19 -1 5 0 2255.17 62.29 -1 5 0 2199.58 62.19 -1 5 0 2182.08 61.29 1 5 0 2146.89 62.49 1 5 0 2183.98 62.09 -2 -5 0 928.41 29.40 2 -5 0 985.20 28.50 -2 -5 0 988.70 29.60 2 -5 0 1000.00 28.80 -2 -5 0 963.40 28.50 -2 5 0 1008.50 30.60 2 5 0 998.00 30.10 -2 5 0 960.00 28.70 -2 5 0 973.40 28.70 2 5 0 949.51 29.10 -2 5 0 937.81 29.80 -3 -5 0 38.80 7.10 -3 -5 0 24.50 6.10 -3 -5 0 28.60 7.90 -3 -5 0 21.90 6.40 3 5 0 23.40 3.50 -3 5 0 22.70 7.50 -3 5 0 22.90 7.20 3 5 0 28.40 7.20 -3 5 0 44.90 5.80 -3 5 0 18.00 4.90 -4 -5 0 405.76 18.10 -4 -5 0 377.76 21.00 -4 -5 0 389.96 20.50 4 5 0 406.36 23.50 -4 5 0 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9.30 1 6 -11 42.10 22.60 -1 6 11 82.89 11.30 0 -6 -11 72.39 22.40 0 -6 11 46.70 13.30 0 -6 11 33.20 15.50 0 6 -11 37.10 24.80 0 6 -11 62.69 19.90 1 -6 11 58.49 20.50 -1 -6 -11 14.30 25.70 -1 6 -11 29.50 25.80 -1 6 -11 35.60 22.40 -3 -7 11 18.50 17.90 3 -7 -11 6.90 28.20 -3 -7 11 -0.10 15.10 3 7 -11 -23.80 16.60 -3 7 11 7.70 18.50 -3 7 11 -1.50 19.20 3 7 -11 16.60 20.70 -2 -7 11 -0.50 13.80 -2 -7 11 16.00 14.90 2 -7 -11 -16.90 21.00 2 7 -11 9.40 18.60 2 7 -11 65.99 25.40 2 7 -11 -4.30 13.30 -2 7 11 28.90 16.80 -2 7 11 5.80 11.90 -1 -7 11 32.40 17.00 1 -7 -11 88.99 22.70 -1 -7 11 55.39 14.00 1 7 -11 56.29 10.50 -1 7 11 47.20 10.30 1 7 -11 70.29 24.40 0 -7 -11 64.09 23.00 0 -7 11 52.49 13.50 0 -7 11 56.59 16.80 0 7 -11 69.29 19.90 0 7 -11 69.69 25.20 -1 -7 -11 26.70 26.10 1 -7 11 19.30 19.70 -1 7 -11 -21.90 25.10 -1 7 -11 50.39 21.90 -3 -8 11 5.40 16.50 -3 -8 11 34.00 17.90 3 -8 -11 54.49 26.50 -3 8 11 6.10 19.10 3 8 -11 12.10 17.10 3 8 -11 -4.20 20.50 -3 8 11 9.30 19.70 -2 -8 11 74.79 17.00 2 -8 -11 45.90 23.70 -2 8 11 69.99 17.80 -2 8 11 46.30 14.00 2 8 -11 93.99 30.10 2 8 -11 78.19 14.10 -1 -8 11 78.19 14.70 1 -8 -11 83.09 23.10 -1 -8 11 99.19 15.80 1 8 -11 98.89 12.20 1 8 -11 109.79 23.00 -1 8 11 75.79 11.30 0 -8 -11 86.99 25.70 0 -8 11 111.89 18.80 0 -8 11 102.29 15.00 0 8 -11 85.99 24.00 2 -9 -11 13.70 23.30 -2 -9 11 10.20 13.80 -2 -9 11 13.60 14.60 2 9 -11 72.79 26.60 -2 9 11 0.90 13.90 -2 9 11 38.80 18.60 2 9 -11 18.80 13.70 1 -9 -11 59.19 25.20 -1 -9 11 68.59 15.30 -1 -9 11 60.69 14.70 -1 9 11 60.79 11.10 1 9 -11 60.99 11.90 1 9 -11 41.50 24.10 0 -9 -11 43.30 25.60 0 -9 11 27.90 13.70 0 -9 11 30.70 16.90 0 9 -11 -12.70 22.50 -2 -10 11 50.89 15.30 -2 -10 11 52.59 17.50 2 -10 -11 28.90 25.00 2 10 -11 52.89 27.20 -2 10 11 61.89 16.80 -2 10 11 42.50 15.20 2 10 -11 43.20 14.60 -1 -10 11 71.09 14.40 -1 -10 11 67.89 16.70 1 -10 -11 96.29 26.00 -1 10 11 50.79 11.10 1 10 -11 50.89 12.00 1 10 -11 91.99 25.30 0 -10 -11 -28.20 25.30 0 -10 11 29.60 17.90 0 -10 11 26.50 13.30 0 10 -11 55.89 25.00 -2 -11 11 64.69 18.00 2 -11 -11 48.40 23.00 -2 -11 11 22.40 15.90 -2 11 11 54.29 15.60 2 11 -11 52.69 14.90 2 11 -11 75.19 29.20 -2 11 11 86.09 19.90 1 -11 -11 30.30 26.20 -1 -11 11 35.40 17.00 -1 -11 11 30.70 13.40 1 11 -11 48.00 24.60 -1 11 11 29.40 11.10 1 11 -11 4.80 13.50 0 -11 11 -0.90 13.20 0 -11 -11 28.70 27.10 0 -11 11 19.30 18.30 0 11 -11 22.50 13.90 0 11 -11 4.90 27.00 2 -12 -11 9.00 26.00 -2 -12 11 16.60 15.10 -2 -12 11 17.10 16.70 2 12 -11 35.20 28.70 2 12 -11 15.90 14.80 -2 12 11 6.10 14.50 1 -12 -11 -55.79 25.80 -1 -12 11 -15.60 16.00 -1 -12 11 23.70 14.60 1 12 -11 3.50 25.30 1 12 -11 23.60 13.20 -1 12 11 21.40 12.00 0 -12 11 34.60 18.80 0 -12 -11 73.09 29.60 0 -12 11 42.30 13.70 0 12 -11 3.00 26.60 -2 -13 11 60.99 18.70 -2 -13 11 68.49 18.20 2 -13 -11 83.39 29.70 -2 13 11 82.89 16.90 2 13 -11 67.89 17.10 2 13 -11 73.29 28.90 1 -13 -11 16.30 27.50 -1 -13 11 6.40 14.30 -1 -13 11 29.80 17.70 1 13 -11 -0.80 25.60 1 13 -11 11.80 15.20 0 -13 11 34.10 18.70 0 -13 11 13.50 14.50 0 -13 -11 -72.49 28.50 0 13 -11 -30.10 25.20 1 -14 -11 -8.20 28.70 -1 -14 11 14.10 18.30 -1 -14 11 -5.60 13.90 1 14 -11 21.80 26.80 1 14 -11 4.40 14.60 2 0 -12 25.40 23.80 -2 0 12 8.70 18.00 -2 0 12 32.50 15.50 -1 0 12 -7.10 16.20 1 0 -12 -20.60 22.50 -1 0 12 -3.20 15.90 0 0 12 30.70 18.60 0 0 -12 31.50 21.30 -2 -1 12 30.60 15.80 -2 -1 12 0.00 20.90 2 -1 -12 49.70 24.00 2 1 -12 -5.10 23.80 -2 1 12 18.80 18.50 -2 1 12 -2.30 14.70 -1 -1 12 64.49 18.50 -1 -1 12 17.00 16.90 1 -1 -12 62.39 24.70 -1 1 12 4.40 19.10 -1 1 12 15.40 17.00 -1 1 12 22.80 12.60 1 1 -12 28.00 20.10 0 -1 12 22.90 18.70 0 1 12 -5.10 18.30 0 1 -12 -14.60 29.50 -2 -2 12 26.40 18.40 -2 -2 12 23.70 17.70 2 -2 -12 38.30 24.00 -2 2 12 7.30 14.40 2 2 -12 31.90 24.30 -2 2 12 -17.90 17.40 -2 2 12 19.80 16.20 1 -2 -12 59.69 24.20 -1 -2 12 -3.40 14.70 -1 -2 12 9.70 16.20 -1 2 12 17.00 17.70 1 2 -12 23.80 23.20 -1 2 12 -9.30 16.90 -1 2 12 2.10 14.50 -2 -3 12 -23.30 17.20 2 -3 -12 41.10 25.80 -2 3 12 1.80 15.50 -2 3 12 -10.40 17.70 2 3 -12 -0.80 23.00 -2 3 12 3.00 13.70 1 -3 -12 96.59 25.50 -1 -3 12 109.89 17.40 -1 -3 12 82.39 18.50 1 3 -12 62.19 21.10 -1 3 12 75.09 17.50 1 3 -12 79.49 28.90 -1 3 12 89.49 18.30 -2 -4 12 42.80 16.80 -2 -4 12 15.40 18.50 2 -4 -12 44.60 27.00 -2 4 12 14.80 19.20 -2 4 12 18.60 15.80 2 4 -12 19.70 23.80 -2 4 12 -5.20 15.30 -1 -4 12 54.99 17.50 -1 -4 12 17.20 16.90 1 -4 -12 33.80 26.40 1 4 -12 23.70 23.10 -1 4 12 42.10 18.40 1 4 -12 31.80 29.60 -1 -5 12 22.40 16.80 1 -5 -12 -8.40 23.60 -1 -5 12 12.70 16.50 -1 5 12 30.40 17.30 1 5 -12 10.80 22.10 1 5 -12 53.99 29.10 -1 -6 12 -11.20 16.00 1 -6 -12 -5.10 22.80 -1 -6 12 33.60 19.50 1 6 -12 6.80 28.40 1 6 -12 27.70 21.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number 0 _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.317 _diffrn_reflns_theta_max 27.128 _diffrn_reflns_av_unetI/netI 0.084069 _diffrn_reflns_number 17825 _diffrn_reflns_number_extinctions 0 _diffrn_reflns_number_accepted 17825 _diffrn_reflns_number_rejected 0 _diffrn_ambient_temperature 297(2) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.247 _exptl_crystal_size_mid 0.123 _exptl_crystal_size_min 0.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F000 460 _cell_length_a 4.3139(2) _cell_length_b 25.5732(14) _cell_length_c 9.5710(5) _cell_angle_alpha 90 _cell_angle_beta 102.074(2) _cell_angle_gamma 90 _cell_volume 1032.52(9) _cell_measurement_temperature 297(2) _cell_measurement_wavelength 0.71073 _cell_measurement_reflns_used 0 _cell_measurement_theta_max 0 _cell_measurement_theta_min 0 _exptl_absorpt_coefficient_mu 0.341 _exptl_absorpt_correction_type ? loop_ _atom_type_symbol _atom_type_number_in_cell C 42 H 36 N 8 O 6 Cl 4 _cell_formula_units_Z 2 _chemical_formula_moiety 'C21 H18 N4 O3 Cl2' _chemical_formula_sum 'C21 H18 N4 O3 Cl2' _chemical_compound_source ? _space_group_crystal_system ? _space_group_name_H-M_alt ' ' _space_group_name_Hall ? _space_group_IT_number 0 _computing_structure_solution ? _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_number_constraints 0 _refine_ls_number_restraints 0 ; _shelx_hkl_checksum 80014 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 1.2951(2) 0.49036(4) 1.00687(9) 0.0531(2) Uani 1 1 d . . . . . Cl1' Cl 1.0671(3) 0.31033(5) 0.94344(12) 0.0821(4) Uani 1 1 d . . . . . O44 O 0.0458(5) 0.67014(11) 0.3536(2) 0.0509(6) Uani 1 1 d . . . . . H44 H -0.054194 0.663504 0.272849 0.076 Uiso 1 1 calc R U . . . O41 O 0.2191(5) 0.65407(9) 0.6481(2) 0.0392(5) Uani 1 1 d . . . . . O44' O 0.2002(5) 0.56233(11) 0.3930(3) 0.0564(7) Uani 1 1 d . . . . . H44' H 0.180351 0.594223 0.390291 0.085 Uiso 1 1 calc R U . . . C4A C 0.5898(7) 0.61681(12) 0.8348(3) 0.0326(7) Uani 1 1 d . . . . . N1 N 0.7056(6) 0.65715(11) 1.0714(3) 0.0416(6) Uani 1 1 d . . . . . C8 C 0.9777(7) 0.57894(14) 1.0317(3) 0.0382(7) Uani 1 1 d . . . . . H8 H 1.088810 0.579420 1.126085 0.046 Uiso 1 1 calc R U . . . O41' O 0.1136(7) 0.45652(11) 0.4667(3) 0.0614(7) Uani 1 1 d . . . . . C43 C -0.1672(8) 0.67949(14) 0.4443(3) 0.0456(8) Uani 1 1 d . . . . . H43A H -0.286189 0.647907 0.453086 0.055 Uiso 1 1 calc R U . . . H43B H -0.316130 0.706622 0.403740 0.055 Uiso 1 1 calc R U . . . C42 C 0.0119(8) 0.69615(14) 0.5890(3) 0.0406(7) Uani 1 1 d . . . . . H42A H 0.134381 0.727389 0.580778 0.049 Uiso 1 1 calc R U . . . H42B H -0.134515 0.703879 0.650536 0.049 Uiso 1 1 calc R U . . . C4 C 0.3710(7) 0.65757(12) 0.7857(3) 0.0344(7) Uani 1 1 d . . . . . C5 C 0.6509(7) 0.57525(13) 0.7470(3) 0.0368(7) Uani 1 1 d . . . . . H5 H 0.541333 0.573548 0.652430 0.044 Uiso 1 1 calc R U . . . C6 C 0.8672(7) 0.53786(13) 0.7988(3) 0.0404(7) Uani 1 1 d . . . . . H6 H 0.909124 0.510959 0.740019 0.048 Uiso 1 1 calc R U . . . C7 C 1.0263(7) 0.54024(13) 0.9416(3) 0.0367(7) Uani 1 1 d . . . . . C3 C 0.3299(8) 0.69641(14) 0.8789(3) 0.0430(8) Uani 1 1 d . . . . . H3 H 0.191415 0.723995 0.849018 0.052 Uiso 1 1 calc R U . . . C2 C 0.5014(8) 0.69359(15) 1.0201(3) 0.0466(8) Uani 1 1 d . . . . . H2 H 0.466950 0.719811 1.082430 0.056 Uiso 1 1 calc R U . . . C8A C 0.7552(7) 0.61842(13) 0.9793(3) 0.0343(7) Uani 1 1 d . . . . . C43' C -0.0963(8) 0.53906(17) 0.3857(4) 0.0569(10) Uani 1 1 d . . . . . H43C H -0.254296 0.556728 0.314259 0.068 Uiso 1 1 calc R U . . . H43D H -0.157647 0.542285 0.477182 0.068 Uiso 1 1 calc R U . . . C42' C -0.0812(9) 0.48284(18) 0.3476(4) 0.0595(10) Uani 1 1 d . . . . . H42C H -0.292349 0.467833 0.327073 0.071 Uiso 1 1 calc R U . . . H42D H 0.009070 0.479115 0.263376 0.071 Uiso 1 1 calc R U . . . C4' C 0.2045(10) 0.40715(16) 0.4494(4) 0.0539(10) Uani 1 1 d . . . . . C4A' C 0.4084(8) 0.38517(14) 0.5701(4) 0.0453(8) Uani 1 1 d . . . . . C8A' C 0.5202(10) 0.33336(15) 0.5578(4) 0.0536(10) Uani 1 1 d . . . . . C8' C 0.7249(9) 0.31071(16) 0.6758(4) 0.0556(9) Uani 1 1 d . . . . . H8' H 0.799694 0.276836 0.670136 0.067 Uiso 1 1 calc R U . . . C7' C 0.8120(9) 0.33848(15) 0.7973(4) 0.0514(9) Uani 1 1 d . . . . . C3' C 0.1262(13) 0.37733(19) 0.3285(4) 0.0776(14) Uani 1 1 d . . . . . H3' H -0.006278 0.390426 0.246633 0.093 Uiso 1 1 calc R U . . . C2' C 0.2491(16) 0.3270(2) 0.3307(5) 0.100(2) Uani 1 1 d . . . . . H2' H 0.190342 0.307543 0.247234 0.120 Uiso 1 1 calc R U . . . N1' N 0.4370(11) 0.30440(15) 0.4369(4) 0.0833(11) Uani 1 1 d . . . . . C5' C 0.5030(9) 0.41149(14) 0.6994(4) 0.0528(9) Uani 1 1 d . . . . . H5' H 0.429271 0.445199 0.708827 0.063 Uiso 1 1 calc R U . . . C6' C 0.7001(10) 0.38885(15) 0.8112(4) 0.0568(10) Uani 1 1 d . . . . . H6' H 0.760863 0.406833 0.897022 0.068 Uiso 1 1 calc R U . . . 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 0.0475(4) 0.0620(6) 0.0476(5) 0.0068(4) 0.0049(4) 0.0119(5) Cl1' 0.0876(8) 0.0773(8) 0.0727(7) 0.0194(6) -0.0035(6) 0.0131(6) O44 0.0442(12) 0.0756(17) 0.0286(11) -0.0048(11) -0.0018(9) 0.0035(12) O41 0.0447(11) 0.0454(13) 0.0243(10) -0.0003(9) 0.0003(8) 0.0055(10) O44' 0.0418(13) 0.0676(17) 0.0555(14) -0.0042(14) 0.0005(11) 0.0118(13) C4A 0.0336(15) 0.0380(17) 0.0264(15) -0.0015(13) 0.0064(12) -0.0074(13) N1 0.0471(14) 0.0486(17) 0.0267(13) -0.0081(12) 0.0022(11) -0.0044(14) C8 0.0346(16) 0.054(2) 0.0243(14) 0.0034(14) 0.0028(12) -0.0059(15) O41' 0.0702(17) 0.065(2) 0.0446(14) 0.0097(12) 0.0022(13) 0.0080(14) C43 0.0356(17) 0.057(2) 0.0399(17) -0.0041(16) -0.0018(14) 0.0056(15) C42 0.0448(18) 0.0442(19) 0.0320(15) 0.0026(14) 0.0058(13) 0.0052(15) C4 0.0351(15) 0.0412(18) 0.0264(14) 0.0000(13) 0.0056(11) -0.0072(14) C5 0.0374(16) 0.0474(19) 0.0247(14) -0.0016(14) 0.0045(12) -0.0034(15) C6 0.0413(17) 0.047(2) 0.0334(16) -0.0036(15) 0.0091(13) -0.0029(15) C7 0.0319(15) 0.0437(19) 0.0347(16) 0.0052(14) 0.0076(12) -0.0012(13) C3 0.0481(19) 0.0392(19) 0.0391(18) -0.0046(15) 0.0035(14) 0.0037(16) C2 0.056(2) 0.048(2) 0.0345(17) -0.0122(15) 0.0048(15) -0.0015(18) C8A 0.0324(15) 0.0436(18) 0.0267(15) 0.0002(13) 0.0060(12) -0.0093(13) C43' 0.0406(19) 0.082(3) 0.050(2) 0.020(2) 0.0149(16) 0.0176(19) C42' 0.0493(19) 0.075(3) 0.049(2) 0.019(2) -0.0011(16) -0.001(2) C4' 0.062(2) 0.050(2) 0.048(2) 0.0068(18) 0.0095(18) -0.0166(19) C4A' 0.051(2) 0.043(2) 0.0440(19) 0.0014(15) 0.0143(16) -0.0107(16) C8A' 0.072(2) 0.043(2) 0.048(2) -0.0032(17) 0.0177(19) -0.0140(18) C8' 0.072(2) 0.038(2) 0.061(2) 0.0031(19) 0.023(2) -0.0008(19) C7' 0.050(2) 0.048(2) 0.055(2) 0.0087(18) 0.0086(17) -0.0013(17) C3' 0.110(4) 0.066(3) 0.046(2) 0.003(2) -0.010(2) -0.025(3) C2' 0.178(6) 0.059(3) 0.052(3) -0.010(2) -0.001(3) -0.027(3) N1' 0.142(3) 0.049(2) 0.054(2) -0.0073(19) 0.009(2) -0.011(2) C5' 0.064(2) 0.042(2) 0.049(2) -0.0043(17) 0.0059(18) 0.0037(18) C6' 0.071(3) 0.050(2) 0.046(2) -0.0053(18) 0.0036(18) 0.003(2) 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' Cl Cl 0.1484 0.1585 '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 C43 O44 H44 109.5 . . ? C4 O41 C42 118.1(2) . . ? C43' O44' H44' 109.5 . . ? C5 C4A C8A 118.9(3) . . ? C5 C4A C4 123.3(3) . . ? C8A C4A C4 117.8(3) . . ? C2 N1 C8A 117.2(2) . . ? C7 C8 C8A 118.7(3) . . ? C7 C8 H8 120.7 . . ? C8A C8 H8 120.7 . . ? C4' O41' C42' 118.7(3) . . ? O44 C43 C42 109.9(3) . . ? O44 C43 H43A 109.7 . . ? C42 C43 H43A 109.7 . . ? O44 C43 H43B 109.7 . . ? C42 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? O41 C42 C43 108.0(3) . . ? O41 C42 H42A 110.1 . . ? C43 C42 H42A 110.1 . . ? O41 C42 H42B 110.1 . . ? C43 C42 H42B 110.1 . . ? H42A C42 H42B 108.4 . . ? O41 C4 C3 125.6(3) . . ? O41 C4 C4A 115.4(3) . . ? C3 C4 C4A 119.0(3) . . ? C6 C5 C4A 120.8(3) . . ? C6 C5 H5 119.6 . . ? C4A C5 H5 119.6 . . ? C5 C6 C7 119.2(3) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 123.0(3) . . ? C8 C7 Cl1 118.9(2) . . ? C6 C7 Cl1 118.1(3) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? N1 C2 C3 125.3(3) . . ? N1 C2 H2 117.3 . . ? C3 C2 H2 117.3 . . ? N1 C8A C8 118.3(3) . . ? N1 C8A C4A 122.2(3) . . ? C8 C8A C4A 119.5(3) . . ? O44' C43' C42' 109.7(3) . . ? O44' C43' H43C 109.7 . . ? C42' C43' H43C 109.7 . . ? O44' C43' H43D 109.7 . . ? C42' C43' H43D 109.7 . . ? H43C C43' H43D 108.2 . . ? O41' C42' C43' 107.9(3) . . ? O41' C42' H42C 110.1 . . ? C43' C42' H42C 110.1 . . ? O41' C42' H42D 110.1 . . ? C43' C42' H42D 110.1 . . ? H42C C42' H42D 108.4 . . ? O41' C4' C3' 127.0(4) . . ? O41' C4' C4A' 114.9(3) . . ? C3' C4' C4A' 118.1(4) . . ? C5' C4A' C4' 123.4(3) . . ? C5' C4A' C8A' 118.8(3) . . ? C4' C4A' C8A' 117.8(3) . . ? N1' C8A' C8' 118.0(4) . . ? N1' C8A' C4A' 123.0(4) . . ? C8' C8A' C4A' 119.0(3) . . ? C7' C8' C8A' 119.4(4) . . ? C7' C8' H8' 120.3 . . ? C8A' C8' H8' 120.3 . . ? C8' C7' C6' 122.0(3) . . ? C8' C7' Cl1' 119.3(3) . . ? C6' C7' Cl1' 118.6(3) . . ? C4' C3' C2' 118.5(4) . . ? C4' C3' H3' 120.8 . . ? C2' C3' H3' 120.8 . . ? N1' C2' C3' 126.8(4) . . ? N1' C2' H2' 116.6 . . ? C3' C2' H2' 116.6 . . ? C2' N1' C8A' 115.8(4) . . ? C6' C5' C4A' 121.1(3) . . ? C6' C5' H5' 119.5 . . ? C4A' C5' H5' 119.5 . . ? C5' C6' C7' 119.7(3) . . ? C5' C6' H6' 120.2 . . ? C7' C6' H6' 120.2 . . ? 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 Cl1 C7 1.749(3) . ? Cl1' C7' 1.744(4) . ? O44 C43 1.411(4) . ? O44 H44 0.8200 . ? O41 C4 1.346(3) . ? O41 C42 1.437(4) . ? O44' C43' 1.399(4) . ? O44' H44' 0.8200 . ? C4A C5 1.414(4) . ? C4A C8A 1.418(4) . ? C4A C4 1.419(4) . ? N1 C2 1.306(4) . ? N1 C8A 1.372(4) . ? C8 C7 1.358(4) . ? C8 C8A 1.411(5) . ? C8 H8 0.9300 . ? O41' C4' 1.343(5) . ? O41' C42' 1.435(4) . ? C43 C42 1.499(4) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C4 C3 1.371(4) . ? C5 C6 1.356(4) . ? C5 H5 0.9300 . ? C6 C7 1.396(4) . ? C6 H6 0.9300 . ? C3 C2 1.400(5) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C43' C42' 1.488(6) . ? C43' H43C 0.9700 . ? C43' H43D 0.9700 . ? C42' H42C 0.9700 . ? C42' H42D 0.9700 . ? C4' C3' 1.368(6) . ? C4' C4A' 1.413(5) . ? C4A' C5' 1.393(5) . ? C4A' C8A' 1.423(5) . ? C8A' N1' 1.358(5) . ? C8A' C8' 1.405(5) . ? C8' C7' 1.347(5) . ? C8' H8' 0.9300 . ? C7' C6' 1.392(5) . ? C3' C2' 1.390(7) . ? C3' H3' 0.9300 . ? C2' N1' 1.296(6) . ? C2' H2' 0.9300 . ? C5' C6' 1.350(5) . ? C5' H5' 0.9300 . ? C6' H6' 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 O41 C42 C43 -171.0(3) . . . . ? O44 C43 C42 O41 -61.9(4) . . . . ? C42 O41 C4 C3 4.7(4) . . . . ? C42 O41 C4 C4A -175.5(3) . . . . ? C5 C4A C4 O41 0.7(4) . . . . ? C8A C4A C4 O41 -179.7(3) . . . . ? C5 C4A C4 C3 -179.5(3) . . . . ? C8A C4A C4 C3 0.2(4) . . . . ? C8A C4A C5 C6 -1.0(4) . . . . ? C4 C4A C5 C6 178.7(3) . . . . ? C4A C5 C6 C7 1.2(5) . . . . ? C8A C8 C7 C6 0.4(4) . . . . ? C8A C8 C7 Cl1 -178.5(2) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? C5 C6 C7 Cl1 178.1(2) . . . . ? O41 C4 C3 C2 178.4(3) . . . . ? C4A C4 C3 C2 -1.4(4) . . . . ? C8A N1 C2 C3 -0.2(5) . . . . ? C4 C3 C2 N1 1.5(5) . . . . ? C2 N1 C8A C8 179.2(3) . . . . ? C2 N1 C8A C4A -1.1(4) . . . . ? C7 C8 C8A N1 179.5(3) . . . . ? C7 C8 C8A C4A -0.2(4) . . . . ? C5 C4A C8A N1 -179.2(3) . . . . ? C4 C4A C8A N1 1.1(4) . . . . ? C5 C4A C8A C8 0.5(4) . . . . ? C4 C4A C8A C8 -179.2(3) . . . . ? C4' O41' C42' C43' -169.4(3) . . . . ? O44' C43' C42' O41' 69.0(4) . . . . ? C42' O41' C4' C3' -1.5(6) . . . . ? C42' O41' C4' C4A' 177.0(3) . . . . ? O41' C4' C4A' C5' 1.8(5) . . . . ? C3' C4' C4A' C5' -179.5(4) . . . . ? O41' C4' C4A' C8A' -178.5(3) . . . . ? C3' C4' C4A' C8A' 0.2(5) . . . . ? C5' C4A' C8A' N1' 179.0(4) . . . . ? C4' C4A' C8A' N1' -0.7(5) . . . . ? C5' C4A' C8A' C8' -0.7(5) . . . . ? C4' C4A' C8A' C8' 179.6(3) . . . . ? N1' C8A' C8' C7' 179.9(4) . . . . ? C4A' C8A' C8' C7' -0.3(5) . . . . ? C8A' C8' C7' C6' 1.4(6) . . . . ? C8A' C8' C7' Cl1' -179.8(3) . . . . ? O41' C4' C3' C2' 178.9(5) . . . . ? C4A' C4' C3' C2' 0.4(7) . . . . ? C4' C3' C2' N1' -0.5(9) . . . . ? C3' C2' N1' C8A' 0.0(9) . . . . ? C8' C8A' N1' C2' -179.7(4) . . . . ? C4A' C8A' N1' C2' 0.6(7) . . . . ? C4' C4A' C5' C6' -179.5(4) . . . . ? C8A' C4A' C5' C6' 0.8(6) . . . . ? C4A' C5' C6' C7' 0.2(6) . . . . ? C8' C7' C6' C5' -1.3(6) . . . . ? Cl1' C7' C6' C5' 179.8(3) . . . . ?