#------------------------------------------------------------------------------ #$Date: 2019-07-20 06:59:05 +0300 (Sat, 20 Jul 2019) $ #$Revision: 217185 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/84/2108441.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108441 loop_ _publ_author_name 'Bodart, Laurie' 'Tumanov, Nikolay' 'Wouters, Johan' _publ_section_title ; Structural variety of clofaziminium salts: effect of the counter-ion on clofaziminium conformation and crystal packing ; _journal_coeditor_code AW5025 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619007649 _journal_volume 75 _journal_year 2019 _chemical_formula_moiety 'C27 H23 Cl2 N4 + , C4 H3 O4 -' _chemical_formula_sum 'C31 H26 Cl2 N4 O4' _chemical_formula_weight 589.46 _chemical_name_common 'clofaziminium hydrogen fumarate' _chemical_name_systematic ; N-[(2E)-10-(4-chlorophenyl)-3-[(4-chlorophenyl)amino]-2,10-dihydrophenazin- 2-ylidene]propan-2-aminium (2E)-3-carboxyprop-2-enoate ; _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 102.5075(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.47882(9) _cell_length_b 26.0041(3) _cell_length_c 14.78241(16) _cell_measurement_reflns_used 8175 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 67.0660 _cell_measurement_theta_min 3.4850 _cell_volume 2806.66(6) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 295(2) _diffrn_detector_area_resol_mean 5.1856 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur Ruby Gemini ultra' _diffrn_measurement_method \w _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_unetI/netI 0.0190 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15078 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.108 _diffrn_reflns_theta_max 67.108 _diffrn_reflns_theta_min 3.503 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.450 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_correction_T_min 0.502 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R. C. Clark & J. S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'Metallic dark red' _exptl_crystal_density_diffrn 1.395 _exptl_crystal_description Plate _exptl_crystal_F_000 1224 _exptl_crystal_size_max 0.572 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.036 _refine_diff_density_max 0.458 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 383 _refine_ls_number_reflns 4944 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.006 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0485 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+1.5073P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1303 _refine_ls_wR_factor_ref 0.1355 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4394 _reflns_number_total 4944 _reflns_threshold_expression I>2\s(I) _cod_data_source_file aw5025sup1.cif _cod_data_source_block lb0211_CLZ-FA _cod_original_cell_volume 2806.65(6) _cod_database_code 2108441 _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_min 0.336 _shelx_estimated_absorpt_t_max 0.917 _shelx_res_file ; TITL lb0211_clz-fa_a.res in P2(1)/c lb0211_CLZ-FA.res created by SHELXL-2016/6 at 16:39:25 on 13-Jul-2018 REM Old TITL lb0211_CLZ-FA in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.244, Rweak 0.053, Alpha 0.114, Orientation as input REM Formula found by SHELXT: C31 N4 O6 CELL 1.54184 7.478817 26.004095 14.782414 90 102.5075 90 ZERR 4 0.000092 0.000328 0.000163 0 0.0012 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Cl UNIT 124 104 16 16 8 LIST 4 L.S. 10 PLAN 20 SIZE 0.036 0.13 0.57 TEMP 22 EQIV $1 x-1, y, z HTAB N3 O2_$1 HTAB N3 O3 HTAB N4 O3 EQIV $2 x+1, y, z HTAB O1 O3_$2 BOND $H CONF list 4 fmap 2 acta WGHT 0.070100 1.507300 FVAR 6.92155 CL1 5 0.033341 0.650114 0.062174 11.00000 0.10459 0.12875 = 0.06882 0.05393 -0.01260 -0.04069 CL2 5 0.742234 0.505373 1.120826 11.00000 0.11206 0.11850 = 0.04878 0.02935 -0.01812 -0.04924 N1 3 0.214304 0.544450 0.423709 11.00000 0.03706 0.03920 = 0.03448 -0.00145 0.00598 0.00142 N2 3 0.316105 0.479613 0.576965 11.00000 0.04232 0.04073 = 0.03977 0.00102 0.01057 0.00253 N3 3 0.566610 0.621487 0.768458 11.00000 0.05870 0.04289 = 0.03565 -0.00415 0.00578 0.00387 H3 2 0.538395 0.651662 0.777211 11.00000 0.06199 N4 3 0.510708 0.682586 0.614061 11.00000 0.05526 0.03903 = 0.03834 -0.00250 0.00101 0.00096 H4 2 0.554573 0.692857 0.668292 11.00000 0.05946 C1 1 0.062611 0.471899 0.333328 11.00000 0.03998 0.04751 = 0.04271 -0.00443 0.00635 0.00054 AFIX 43 H1 2 0.023411 0.492797 0.281793 11.00000 -1.20000 AFIX 0 C2 1 0.020378 0.420395 0.328820 11.00000 0.04428 0.04977 = 0.05218 -0.01269 0.00957 -0.00379 AFIX 43 H2 2 -0.049397 0.406777 0.274308 11.00000 -1.20000 AFIX 0 C3 1 0.080548 0.388342 0.404665 11.00000 0.04932 0.04118 = 0.06296 -0.00950 0.01908 -0.00582 AFIX 43 H3A 2 0.052421 0.353471 0.400142 11.00000 -1.20000 AFIX 0 C4 1 0.180895 0.407871 0.485874 11.00000 0.04896 0.04183 = 0.05148 -0.00022 0.01858 0.00195 AFIX 43 H4A 2 0.221835 0.386147 0.536061 11.00000 -1.20000 AFIX 0 C5 1 0.222560 0.460838 0.493824 11.00000 0.03541 0.04142 = 0.04078 -0.00173 0.01274 0.00283 C6 1 0.354413 0.529230 0.583942 11.00000 0.03283 0.03881 = 0.03799 0.00083 0.01008 0.00383 C7 1 0.441557 0.549465 0.671304 11.00000 0.04124 0.04406 = 0.03274 0.00369 0.00769 0.00438 AFIX 43 H7 2 0.469334 0.527308 0.721788 11.00000 -1.20000 AFIX 0 C8 1 0.486286 0.600086 0.684306 11.00000 0.03360 0.04549 = 0.03413 -0.00248 0.00798 0.00580 C9 1 0.451207 0.634566 0.603335 11.00000 0.03344 0.03893 = 0.03894 -0.00167 0.00784 0.00571 C10 1 0.357919 0.615578 0.516968 11.00000 0.04057 0.03842 = 0.03527 0.00192 0.00535 0.00398 AFIX 43 H10 2 0.329556 0.637737 0.466508 11.00000 -1.20000 AFIX 0 C11 1 0.308005 0.564697 0.506041 11.00000 0.03097 0.04179 = 0.03420 -0.00206 0.00776 0.00382 C12 1 0.164800 0.492819 0.415710 11.00000 0.03223 0.03937 = 0.04111 -0.00309 0.01090 0.00151 C13 1 0.173688 0.575861 0.340522 11.00000 0.04240 0.03818 = 0.03332 -0.00187 0.00529 0.00011 C14 1 0.311549 0.585539 0.294335 11.00000 0.04483 0.06403 = 0.04781 0.00647 0.01060 -0.00030 AFIX 43 H14 2 0.431313 0.575514 0.319615 11.00000 -1.20000 AFIX 0 C15 1 0.268801 0.610390 0.209833 11.00000 0.06458 0.08177 = 0.05477 0.01358 0.01910 -0.01322 AFIX 43 H15 2 0.360296 0.617896 0.178127 11.00000 -1.20000 AFIX 0 C16 1 0.090213 0.623982 0.172807 11.00000 0.06935 0.05427 = 0.04573 0.01101 -0.00277 -0.01591 C17 1 -0.044418 0.616690 0.220707 11.00000 0.05142 0.05502 = 0.05662 0.01000 -0.00351 0.00233 AFIX 43 H17 2 -0.162930 0.628135 0.196485 11.00000 -1.20000 AFIX 0 C18 1 -0.003007 0.592114 0.305641 11.00000 0.04467 0.05552 = 0.04647 0.00246 0.00845 0.00461 AFIX 43 H18 2 -0.093603 0.586619 0.338868 11.00000 -1.20000 AFIX 0 C19 1 0.608792 0.593058 0.852102 11.00000 0.04475 0.05158 = 0.03369 -0.00343 0.00529 -0.00489 C24 1 0.721367 0.550296 0.861737 11.00000 0.05117 0.06887 = 0.04367 0.00398 0.00729 0.00907 AFIX 43 H24 2 0.770213 0.539643 0.812091 11.00000 -1.20000 AFIX 0 C23 1 0.762268 0.523212 0.943900 11.00000 0.05625 0.07108 = 0.05239 0.00766 -0.00595 0.00048 AFIX 43 H23 2 0.836159 0.494118 0.949399 11.00000 -1.20000 AFIX 0 C22 1 0.692788 0.539691 1.017109 11.00000 0.06307 0.07707 = 0.03915 0.00760 -0.00745 -0.02394 C21 1 0.584351 0.582294 1.009901 11.00000 0.08034 0.10091 = 0.03568 -0.00993 0.01654 -0.01265 AFIX 43 H21 2 0.539924 0.593422 1.060651 11.00000 -1.20000 AFIX 0 C20 1 0.540309 0.609038 0.926841 11.00000 0.06933 0.06704 = 0.04215 -0.01211 0.01286 0.00279 AFIX 43 H20 2 0.464591 0.637745 0.921575 11.00000 -1.20000 AFIX 0 C25 1 0.484722 0.722256 0.541810 11.00000 0.09121 0.04015 = 0.04517 0.00336 -0.00117 0.00239 AFIX 13 H25 2 0.475304 0.705297 0.481758 11.00000 -1.20000 AFIX 0 C27 1 0.653353 0.757084 0.559361 11.00000 0.16027 0.07481 = 0.08003 0.02302 -0.01513 -0.05304 AFIX 137 H27A 2 0.657531 0.776730 0.614763 11.00000 -1.50000 H27B 2 0.646596 0.779996 0.507808 11.00000 -1.50000 H27C 2 0.761843 0.736400 0.566534 11.00000 -1.50000 AFIX 0 C26 1 0.307803 0.749641 0.540889 11.00000 0.17075 0.11985 = 0.07550 0.02105 0.01713 0.09138 AFIX 137 H26A 2 0.210360 0.724980 0.534589 11.00000 -1.50000 H26B 2 0.282430 0.773189 0.489690 11.00000 -1.50000 H26C 2 0.317395 0.768278 0.597798 11.00000 -1.50000 AFIX 0 O1 4 1.257989 0.758353 0.807840 11.00000 0.03760 0.06261 = 0.09196 -0.02095 0.02244 -0.00420 H1A 2 1.379147 0.750404 0.805892 11.00000 -1.50000 O2 4 1.214571 0.677479 0.766328 11.00000 0.04459 0.07142 = 0.19320 -0.05629 0.02829 -0.00299 O3 4 0.584539 0.737466 0.794661 11.00000 0.03395 0.06177 = 0.06963 -0.01977 0.01329 -0.00595 O4 4 0.654965 0.815934 0.850672 11.00000 0.05092 0.07134 = 0.13053 -0.04298 0.02891 -0.00458 C28 1 1.157959 0.717767 0.788158 11.00000 0.03735 0.05646 = 0.06732 -0.01589 0.00802 0.00094 C29 1 0.963123 0.723808 0.793856 11.00000 0.03503 0.05385 = 0.07019 -0.01353 0.00827 -0.00567 AFIX 43 H29 2 0.885494 0.695829 0.777270 11.00000 -1.20000 AFIX 0 C30 1 0.893642 0.765682 0.820534 11.00000 0.03497 0.05227 = 0.05973 -0.00782 0.01010 -0.00618 AFIX 43 H30 2 0.973923 0.792797 0.839842 11.00000 -1.20000 AFIX 0 C31 1 0.697013 0.774214 0.823008 11.00000 0.03779 0.05527 = 0.05665 -0.01342 0.01220 -0.00233 HKLF 4 REM lb0211_clz-fa_a.res in P2(1)/c REM R1 = 0.0485 for 4394 Fo > 4sig(Fo) and 0.0536 for all 4944 data REM 383 parameters refined using 0 restraints END WGHT 0.0597 1.4280 REM Highest difference peak 0.458, deepest hole -0.515, 1-sigma level 0.040 Q1 1 0.0363 0.6786 0.1067 11.00000 0.05 0.46 Q2 1 0.1446 0.6343 0.0603 11.00000 0.05 0.46 Q3 1 0.6359 0.5305 1.1268 11.00000 0.05 0.45 Q4 1 0.5209 0.7698 0.5821 11.00000 0.05 0.40 Q5 1 -0.0027 0.6513 0.0433 11.00000 0.05 0.27 Q6 1 0.3472 0.7524 0.5341 11.00000 0.05 0.22 Q7 1 0.7076 0.7904 0.9016 11.00000 0.05 0.18 Q8 1 0.1864 0.4777 0.4573 11.00000 0.05 0.17 Q9 1 0.3312 0.5498 0.5441 11.00000 0.05 0.17 Q10 1 0.5347 0.5902 0.8786 11.00000 0.05 0.17 Q11 1 0.8452 0.5184 1.1167 11.00000 0.05 0.16 Q12 1 0.4093 0.5790 0.6830 11.00000 0.05 0.16 Q13 1 0.0892 0.6072 0.3377 11.00000 0.05 0.15 Q14 1 0.4435 0.6176 0.6470 11.00000 0.05 0.15 Q15 1 0.2665 0.5505 0.4610 11.00000 0.05 0.15 Q16 1 0.4347 0.6202 0.5547 11.00000 0.05 0.14 Q17 1 0.1061 0.6389 0.2037 11.00000 0.05 0.14 Q18 1 0.7645 0.4958 1.1140 11.00000 0.05 0.13 Q19 1 0.6475 0.8177 0.7822 11.00000 0.05 0.13 Q20 1 1.2864 0.7326 0.8509 11.00000 0.05 0.13 ; _shelx_res_checksum 80312 _shelx_hkl_file ; 0 0 -1 33.2792 13.3934 5 0 0 -2 563.191 66.8629 5 0 0 -2 544.964 55.3641 17 0 0 -3 11.8617 30.2615 17 0 0 -3 69.9430 58.3169 5 0 0 -4 2879.19 169.682 17 0 0 -4 2782.59 203.039 5 0 0 -5 145.277 49.8995 17 0 0 -5 72.8807 72.1069 5 0 0 -6 71429.1 1002.97 17 0 0 -6 75975.8 1279.49 5 0 0 7 108.704 112.090 1 0 0 8 183720. 3080.96 1 0 0 9 188.474 191.252 1 0 0 -9 0.74138 55.8432 10 0 0 -10 62771.4 1017.45 10 0 0 -10 63178.8 1052.81 6 0 0 -11 129.259 105.978 6 0 0 -11 266.006 97.8217 10 0 0 12 7829.75 862.607 1 0 0 -12 8572.62 421.173 10 0 0 -12 8807.59 447.560 6 0 0 -12 8139.68 387.083 11 0 0 -13 88.6588 88.4743 10 0 0 -13 22.3827 78.0853 11 0 0 -13 151.615 111.062 6 0 0 -14 10771.1 500.944 6 0 0 -14 10205.1 433.037 11 0 0 -15 156.208 99.5815 6 0 0 -16 8706.30 399.616 6 0 0 -17 90.0215 57.2242 6 0 1 1 205074. 1101.11 1 0 -1 -2 4478.41 155.688 17 0 1 2 4592.22 225.017 1 0 1 -2 4834.89 188.973 5 0 -1 -3 10458.7 279.373 17 0 -1 -3 10739.6 325.595 5 0 1 -3 11073.4 347.648 5 0 1 -5 54044.6 821.823 17 0 1 5 55379.8 1246.34 1 0 1 -5 56881.6 1036.98 5 0 1 6 10120.5 604.371 1 0 1 -6 11715.7 518.405 5 0 1 -6 10717.6 395.571 17 0 1 -7 112.294 73.1275 5 0 1 7 152.265 119.291 1 0 1 -7 121.301 53.3970 17 0 1 -8 36941.7 1071.06 5 0 -1 8 34346.2 1339.08 1 0 1 8 35697.2 1372.47 1 0 1 -9 24631.5 594.732 10 0 -1 -9 24008.2 560.859 13 0 1 9 25316.2 1265.69 1 0 -1 9 24623.0 1246.25 1 0 -1 -9 25799.5 614.801 6 0 -1 -9 25061.4 597.400 10 0 -1 -10 1458.86 164.275 10 0 1 10 1405.84 335.117 1 0 1 -10 1670.82 185.045 6 0 1 -10 1393.47 153.464 11 0 1 -10 1559.37 165.476 10 0 -1 10 1228.00 298.436 1 0 -1 -10 1425.83 171.082 6 0 1 -11 270350. 2302.15 6 0 -1 -11 268095. 2293.85 6 0 1 11 275229. 4856.27 1 0 -1 -11 271744. 2253.38 10 0 -1 11 281613. 4853.19 1 0 -1 -11 272795. 2191.50 11 0 1 -11 272501. 2235.37 10 0 1 -11 273762. 2103.49 11 0 1 -12 4954.88 300.504 11 0 1 -12 5258.53 348.658 6 0 -1 -12 5240.28 322.485 11 0 1 -12 4947.08 319.412 10 0 -1 -12 5573.17 341.655 10 0 1 12 5711.14 738.733 1 0 -1 12 6522.40 791.205 1 0 -1 -12 5299.87 352.946 6 0 -1 -13 15199.6 576.555 10 0 -1 -13 14645.3 590.349 6 0 1 -13 14663.8 513.879 11 0 -1 -13 14167.3 527.426 11 0 1 -13 13908.3 549.654 10 0 1 -13 14287.1 582.259 6 0 1 -14-18.0523 94.0688 10 0 1 -14 1.21412 103.681 6 0 -1 -14 13.2508 91.1017 6 0 -1 -14 23.8520 70.3004 11 0 -1 -15 7975.82 370.080 11 0 -1 -15 8077.94 426.051 6 0 1 -15 8365.38 431.662 6 0 1 -16 4831.49 299.626 6 0 -1 -16 5069.98 308.395 6 0 1 -17 3468.29 221.966 6 0 -1 -17 3461.79 226.628 6 0 2 1 33770.4 519.190 1 0 2 -3 7256.49 297.976 5 0 2 3 6805.97 345.471 1 0 2 -4 285689. 2128.36 5 0 2 4 272214. 2506.82 1 0 2 -5 4452.67 302.306 5 0 2 5 3777.36 341.231 1 0 2 -6 2045.41 179.819 17 0 2 -6 2168.30 237.508 5 0 2 6 2217.22 299.141 1 0 2 -7 132085. 1950.69 5 0 2 7 136895. 2455.30 1 0 2 -7 132931. 1499.37 17 0 2 -8 119002. 1973.53 5 0 -2 -8 119027. 1209.21 10 0 2 8 115790. 2489.24 1 0 -2 -9 28131.8 636.591 10 0 -2 -9 28062.9 637.368 6 0 2 9 26508.7 1297.00 1 0 -2 -9 26709.4 587.764 16 0 -2 9 27738.6 1325.67 1 0 -2 -9 26491.0 598.739 13 0 -2 -10 4665.13 284.513 10 0 -2 10 4355.36 576.404 1 0 2 -10 4656.48 275.910 10 0 2 -10 4790.73 301.616 6 0 -2 -10 4386.42 258.542 16 0 -2 -10 5020.01 297.513 6 0 2 -10 5189.22 271.415 11 0 2 10 4528.50 583.555 1 0 2 -11 10261.4 457.778 6 0 -2 -11 10684.3 461.958 6 0 2 -11 10747.3 444.514 10 0 -2 -11 10607.5 450.422 10 0 -2 11 9151.34 890.018 1 0 2 -11 10624.1 408.894 11 0 2 11 9998.66 937.853 1 0 -2 12 48180.2 2143.88 1 0 2 -12 46236.8 972.307 10 0 -2 -12 47636.0 993.380 10 0 2 12 48157.1 2156.90 1 0 -2 -12 45565.8 945.644 11 0 2 -12 46606.6 888.033 11 0 -2 -12 46067.3 995.781 6 0 2 -12 45853.6 1005.47 6 0 -2 -13 35037.1 877.493 10 0 2 -13 35072.6 912.346 6 0 2 -13 35726.8 882.119 10 0 -2 -13 34422.0 889.081 6 0 -2 -13 34221.0 831.182 11 0 -2 -14 10410.3 453.754 11 0 2 -14 10253.9 489.747 6 0 -2 -14 10277.0 489.244 6 0 2 -14 10256.6 472.979 10 0 -2 -15 242.393 89.1863 11 0 -2 -15 318.483 106.095 6 0 2 -15 246.824 108.877 6 0 2 -16 2362.18 215.481 6 0 -2 -16 2177.25 208.796 6 0 -2 -17 57.3675 65.9645 6 0 2 -17-87.5149 66.1110 6 0 3 0 42.7547 49.3575 1 0 3 1 11167.6 352.036 1 0 3 2 222527. 1774.09 1 0 3 3 15402.2 536.313 1 0 3 -3 15010.8 453.711 5 0 3 5 123747. 1929.43 1 0 3 -5 123006. 1620.41 5 0 3 -6 183842. 2187.20 5 0 3 6 183872. 2619.84 1 0 3 7 686321. 5548.85 1 0 3 -7 701792. 4623.17 5 0 -3 -8-7.36373 55.6975 6 0 3 -8-5.68106 64.8422 5 0 3 8-73.2149 124.953 1 0 -3 -8 85.2881 53.7353 10 0 3 -9 80081.5 1783.93 5 0 -3 -9 77391.8 1040.71 13 0 3 9 78407.2 2226.18 1 0 -3 -9 76164.7 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247.431 9 0 25 -1 2736.37 278.622 9 0 25 -2 481.408 159.324 9 0 25 2 208.647 112.332 9 0 25 -3 371.952 127.940 9 0 25 3 101.175 93.5668 9 0 25 4 377.041 124.843 9 0 25 -4 396.829 138.058 9 0 25 5 1890.41 197.888 9 0 25 -5 1837.17 218.562 9 0 25 -6 1393.99 191.520 9 0 -25 -6 1654.14 164.466 16 0 -25 -6 1414.91 175.979 15 0 25 6 1647.28 178.413 9 0 -25 -7 232.528 89.7553 15 0 -25 -7 177.252 73.8723 16 0 25 -7 164.207 96.5455 9 0 -25 -8 2326.55 183.853 16 0 -25 -8 2231.22 199.561 15 0 -25 -9 2611.03 188.481 16 0 -25 -9 2979.23 215.209 15 0 26 0 8277.91 437.983 9 0 26 1 6524.05 389.163 9 0 -26 -1 6283.83 340.134 15 0 26 -1 6279.41 390.408 9 0 26 -2-24.8649 100.403 9 0 26 2 42.9304 89.0979 9 0 26 -3 2486.36 250.485 9 0 26 3 2914.22 261.650 9 0 -26 -4 247.405 113.389 15 0 26 4 174.328 101.339 9 0 26 -4 19.2606 98.2324 9 0 26 -5 1195.87 178.326 9 0 -26 -5 1293.26 170.252 15 0 26 5 1351.66 162.262 9 0 26 6 12.9113 66.2130 9 0 -26 -6-90.9142 82.8016 15 0 26 -6-203.049 99.4072 9 0 -26 -7 55.1372 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76.3903 4 -8 -7 4 693.799 109.907 4 -8 -7 4 752.531 133.150 3 -8 -7 3 859.303 117.424 4 -8 -7 3 925.797 136.390 3 -8 -7 2 19.5772 61.5241 8 -8 -7 2 109.630 75.3932 3 -8 -7 1 241.227 102.967 3 -8 -7 0 290.545 93.1295 3 -8 -7 -1 1683.85 178.459 3 -8 -7 -2 217.390 87.5224 3 -8 -7 -3 4415.67 250.018 3 -8 -8 9 3194.13 205.914 4 -8 -8 8 649.374 110.734 4 -8 -8 7 9685.94 385.667 4 -8 -8 6 9692.53 389.430 4 -8 -8 5-15.8312 57.9364 4 -8 -8 4-14.1676 65.8777 4 -8 -8 4 104.293 69.4446 3 -8 -8 3 96.8764 72.0436 8 -8 -8 3-2.57408 52.6936 4 -8 -8 3 86.5714 66.2781 3 -8 -8 2 1101.84 149.953 8 -8 -8 2 953.911 153.824 3 -8 -8 1 92.3527 78.5159 8 -8 -8 1-46.1027 66.5777 3 -8 -8 0 110.513 103.761 3 -8 -8 -1 1990.81 201.101 3 -8 -8 -2 1987.10 197.563 3 -8 -9 9 665.621 100.993 4 -8 -9 8 59.0520 51.6107 4 -8 -9 7 1409.17 152.916 4 -8 -9 6 2927.48 219.689 4 -8 -9 5 5219.66 288.010 4 -8 -9 4-39.3188 57.8778 8 -8 -9 4-16.1535 51.9944 4 -8 -9 4 53.3640 56.2862 3 -8 -9 3 103.104 65.8673 8 -8 -9 3 187.161 71.6054 4 -8 -9 2 3006.84 232.322 3 -8 -9 2 3080.66 231.094 8 -8 -9 1 38.5730 60.0328 8 -8 -9 1 176.416 75.7549 3 -8 -9 0 734.468 117.511 8 -8 -9 0 930.379 149.160 3 -8 -9 -1-71.1910 89.2038 3 -8 -9 -2 1418.51 172.705 3 -8 -10 8 166.758 67.5293 4 -8 -10 7 226.214 73.5682 4 -8 -10 6-66.3082 73.1861 4 -8 -10 5 81.6966 70.7871 4 -8 -10 4 3021.68 200.603 3 -8 -10 4 3243.94 226.539 4 -8 -10 4 3259.26 232.295 8 -8 -10 3 3835.65 231.182 3 -8 -10 3 3362.36 222.053 4 -8 -10 3 3798.39 254.413 8 -8 -10 2 2893.10 212.896 3 -8 -10 2 2945.32 227.283 8 -8 -10 1 493.720 100.903 8 -8 -10 1 462.092 104.920 3 -8 -10 0 2125.41 191.886 3 -8 -10 0 2189.50 193.566 8 -8 -10 -1 5573.99 302.710 3 -8 -11 8 566.719 99.4062 4 -8 -11 7-2.28998 57.4149 4 -8 -11 6 1873.46 173.669 4 -8 -11 5 400.615 96.4899 4 -8 -11 4 104.830 60.9376 8 -8 -11 4 26.8746 55.0783 4 -8 -11 3 733.799 130.529 8 -8 -11 3 585.892 102.322 4 -8 -11 3 681.876 100.876 3 -8 -11 2 664.623 121.030 8 -8 -11 2 493.468 92.5875 3 -8 -11 1 2020.17 171.328 3 -8 -11 1 2362.59 204.748 8 -8 -11 0 1548.17 163.254 8 -8 -11 0 1200.79 127.421 3 -8 -11 -1 157.739 63.5745 3 -8 -12 7 2353.47 184.591 4 -8 -12 6 489.748 103.458 4 -8 -12 5 5730.20 306.360 4 -8 -12 4 3247.35 239.161 4 -8 -12 4 2926.35 219.776 8 -8 -12 3 207.549 79.0086 8 -8 -12 3 143.576 68.6977 4 -8 -12 2 5277.54 317.016 8 -8 -12 1 372.229 102.779 8 -8 -12 0 3845.91 254.091 8 -8 -13 5 46.2986 53.9660 4 -8 -13 2 68.3678 81.4584 8 -8 -13 1 9494.53 391.596 8 0 0 0 0.00 0.00 0 TITL lb0211_CLZ-FA in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 7.478817 26.004095 14.782414 90.0000 102.5075 90.0000 ZERR 4.00 0.000092 0.000328 0.000163 0.0000 0.0012 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Cl UNIT 124.00 112.00 16.00 16.00 8.00 TREF HKLF 4 END ; _shelx_hkl_checksum 38703 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 Cl1 Cl 0.03334(13) 0.65011(4) 0.06217(5) 0.1055(4) Uani 1 1 d . . Cl2 Cl 0.74223(13) 0.50537(4) 1.12083(5) 0.0985(3) Uani 1 1 d . . N1 N 0.2143(2) 0.54445(6) 0.42371(10) 0.0372(3) Uani 1 1 d . . N2 N 0.3161(2) 0.47961(6) 0.57696(11) 0.0407(4) Uani 1 1 d . . N3 N 0.5666(3) 0.62149(7) 0.76846(11) 0.0464(4) Uani 1 1 d . . H3 H 0.538(4) 0.6517(11) 0.7772(18) 0.062(8) Uiso 1 1 d . . N4 N 0.5107(2) 0.68259(6) 0.61406(12) 0.0456(4) Uani 1 1 d . . H4 H 0.555(4) 0.6929(10) 0.6683(19) 0.059(7) Uiso 1 1 d . . C1 C 0.0626(3) 0.47190(8) 0.33333(14) 0.0438(4) Uani 1 1 d . . H1 H 0.023411 0.492797 0.281793 0.053 Uiso 1 1 calc R U C2 C 0.0204(3) 0.42039(8) 0.32882(15) 0.0489(5) Uani 1 1 d . . H2 H -0.049397 0.406777 0.274308 0.059 Uiso 1 1 calc R U C3 C 0.0805(3) 0.38834(8) 0.40467(15) 0.0501(5) Uani 1 1 d . . H3A H 0.052421 0.353471 0.400142 0.060 Uiso 1 1 calc R U C4 C 0.1809(3) 0.40787(8) 0.48587(15) 0.0463(5) Uani 1 1 d . . H4A H 0.221835 0.386147 0.536061 0.056 Uiso 1 1 calc R U C5 C 0.2226(2) 0.46084(7) 0.49382(13) 0.0385(4) Uani 1 1 d . . C6 C 0.3544(2) 0.52923(7) 0.58394(12) 0.0362(4) Uani 1 1 d . . C7 C 0.4416(3) 0.54946(8) 0.67130(12) 0.0394(4) Uani 1 1 d . . H7 H 0.469334 0.527308 0.721788 0.047 Uiso 1 1 calc R U C8 C 0.4863(2) 0.60009(7) 0.68431(12) 0.0376(4) Uani 1 1 d . . C9 C 0.4512(2) 0.63457(7) 0.60334(12) 0.0371(4) Uani 1 1 d . . C10 C 0.3579(3) 0.61558(7) 0.51697(12) 0.0385(4) Uani 1 1 d . . H10 H 0.329556 0.637737 0.466508 0.046 Uiso 1 1 calc R U C11 C 0.3080(2) 0.56470(7) 0.50604(12) 0.0355(4) Uani 1 1 d . . C12 C 0.1648(2) 0.49282(7) 0.41571(13) 0.0371(4) Uani 1 1 d . . C13 C 0.1737(3) 0.57586(7) 0.34052(12) 0.0384(4) Uani 1 1 d . . C14 C 0.3115(3) 0.58554(9) 0.29434(15) 0.0521(5) Uani 1 1 d . . H14 H 0.431313 0.575514 0.319615 0.063 Uiso 1 1 calc R U C15 C 0.2688(4) 0.61039(11) 0.20983(17) 0.0661(7) Uani 1 1 d . . H15 H 0.360296 0.617896 0.178127 0.079 Uiso 1 1 calc R U C16 C 0.0902(3) 0.62398(9) 0.17281(15) 0.0588(6) Uani 1 1 d . . C17 C -0.0444(3) 0.61669(9) 0.22071(16) 0.0567(6) Uani 1 1 d . . H17 H -0.162930 0.628135 0.196485 0.068 Uiso 1 1 calc R U C18 C -0.0030(3) 0.59211(9) 0.30564(14) 0.0491(5) Uani 1 1 d . . H18 H -0.093603 0.586619 0.338868 0.059 Uiso 1 1 calc R U C19 C 0.6088(3) 0.59306(8) 0.85210(13) 0.0438(4) Uani 1 1 d . . C24 C 0.7214(3) 0.55030(10) 0.86174(15) 0.0550(5) Uani 1 1 d . . H24 H 0.770213 0.539643 0.812091 0.066 Uiso 1 1 calc R U C23 C 0.7623(3) 0.52321(11) 0.94390(17) 0.0626(6) Uani 1 1 d . . H23 H 0.836159 0.494118 0.949399 0.075 Uiso 1 1 calc R U C22 C 0.6928(4) 0.53969(11) 1.01711(15) 0.0626(7) Uani 1 1 d . . C21 C 0.5844(4) 0.58229(13) 1.00990(16) 0.0717(8) Uani 1 1 d . . H21 H 0.539924 0.593422 1.060651 0.086 Uiso 1 1 calc R U C20 C 0.5403(4) 0.60904(10) 0.92684(15) 0.0594(6) Uani 1 1 d . . H20 H 0.464591 0.637745 0.921575 0.071 Uiso 1 1 calc R U C25 C 0.4847(4) 0.72226(9) 0.54181(16) 0.0613(6) Uani 1 1 d . . H25 H 0.475304 0.705297 0.481758 0.074 Uiso 1 1 calc R U C27 C 0.6534(6) 0.75708(14) 0.5594(2) 0.1113(15) Uani 1 1 d . . H27A H 0.657531 0.776730 0.614763 0.167 Uiso 1 1 calc R U H27B H 0.646596 0.779996 0.507808 0.167 Uiso 1 1 calc R U H27C H 0.761843 0.736400 0.566534 0.167 Uiso 1 1 calc R U C26 C 0.3078(7) 0.74964(17) 0.5409(3) 0.1235(17) Uani 1 1 d . . H26A H 0.210360 0.724980 0.534589 0.185 Uiso 1 1 calc R U H26B H 0.282430 0.773189 0.489690 0.185 Uiso 1 1 calc R U H26C H 0.317395 0.768278 0.597798 0.185 Uiso 1 1 calc R U O1 O 1.2580(2) 0.75835(7) 0.80784(13) 0.0628(5) Uani 1 1 d . . H1A H 1.379(5) 0.7504(13) 0.806(2) 0.094 Uiso 1 1 d . U O2 O 1.2146(2) 0.67748(8) 0.7663(2) 0.1027(9) Uani 1 1 d . . O3 O 0.58454(18) 0.73747(6) 0.79466(11) 0.0548(4) Uani 1 1 d . . O4 O 0.6550(2) 0.81593(8) 0.85067(17) 0.0829(6) Uani 1 1 d . . C28 C 1.1580(3) 0.71777(9) 0.78816(17) 0.0542(5) Uani 1 1 d . . C29 C 0.9631(3) 0.72381(9) 0.79386(17) 0.0535(5) Uani 1 1 d . . H29 H 0.885494 0.695829 0.777270 0.064 Uiso 1 1 calc R U C30 C 0.8936(3) 0.76568(9) 0.82053(15) 0.0490(5) Uani 1 1 d . . H30 H 0.973923 0.792797 0.839842 0.059 Uiso 1 1 calc R U C31 C 0.6970(3) 0.77421(9) 0.82301(15) 0.0496(5) Uani 1 1 d . . 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 0.1046(6) 0.1288(7) 0.0688(5) 0.0539(5) -0.0126(4) -0.0407(5) Cl2 0.1121(6) 0.1185(7) 0.0488(4) 0.0293(4) -0.0181(4) -0.0492(5) N1 0.0371(8) 0.0392(8) 0.0345(8) -0.0014(6) 0.0060(6) 0.0014(6) N2 0.0423(8) 0.0407(9) 0.0398(8) 0.0010(7) 0.0106(7) 0.0025(7) N3 0.0587(11) 0.0429(10) 0.0356(8) -0.0042(7) 0.0058(7) 0.0039(8) N4 0.0553(10) 0.0390(9) 0.0383(9) -0.0025(7) 0.0010(8) 0.0010(7) C1 0.0400(10) 0.0475(11) 0.0427(10) -0.0044(8) 0.0063(8) 0.0005(8) C2 0.0443(11) 0.0498(12) 0.0522(12) -0.0127(9) 0.0096(9) -0.0038(9) C3 0.0493(11) 0.0412(11) 0.0630(13) -0.0095(10) 0.0191(10) -0.0058(9) C4 0.0490(11) 0.0418(10) 0.0515(11) -0.0002(9) 0.0186(9) 0.0019(9) C5 0.0354(9) 0.0414(10) 0.0408(10) -0.0017(8) 0.0127(8) 0.0028(7) C6 0.0328(9) 0.0388(9) 0.0380(9) 0.0008(7) 0.0101(7) 0.0038(7) C7 0.0412(10) 0.0441(10) 0.0327(9) 0.0037(8) 0.0077(7) 0.0044(8) C8 0.0336(9) 0.0455(10) 0.0341(9) -0.0025(8) 0.0080(7) 0.0058(7) C9 0.0334(9) 0.0389(10) 0.0389(9) -0.0017(8) 0.0078(7) 0.0057(7) C10 0.0406(10) 0.0384(10) 0.0353(9) 0.0019(7) 0.0054(7) 0.0040(8) C11 0.0310(8) 0.0418(10) 0.0342(9) -0.0021(7) 0.0078(7) 0.0038(7) C12 0.0322(9) 0.0394(10) 0.0411(10) -0.0031(8) 0.0109(7) 0.0015(7) C13 0.0424(10) 0.0382(9) 0.0333(9) -0.0019(7) 0.0053(7) 0.0001(8) C14 0.0448(11) 0.0640(14) 0.0478(11) 0.0065(10) 0.0106(9) -0.0003(10) C15 0.0646(15) 0.0818(18) 0.0548(13) 0.0136(12) 0.0191(11) -0.0132(13) C16 0.0693(15) 0.0543(13) 0.0457(12) 0.0110(10) -0.0028(10) -0.0159(11) C17 0.0514(12) 0.0550(13) 0.0566(13) 0.0100(10) -0.0035(10) 0.0023(10) C18 0.0447(11) 0.0555(12) 0.0465(11) 0.0025(9) 0.0084(9) 0.0046(9) C19 0.0447(10) 0.0516(11) 0.0337(9) -0.0034(8) 0.0053(8) -0.0049(9) C24 0.0512(12) 0.0689(15) 0.0437(11) 0.0040(10) 0.0073(9) 0.0091(11) C23 0.0563(13) 0.0711(16) 0.0524(13) 0.0077(11) -0.0059(10) 0.0005(11) C22 0.0631(14) 0.0771(17) 0.0391(11) 0.0076(11) -0.0074(10) -0.0239(13) C21 0.0803(18) 0.101(2) 0.0357(11) -0.0099(12) 0.0165(11) -0.0127(16) C20 0.0693(15) 0.0670(15) 0.0422(11) -0.0121(10) 0.0129(10) 0.0028(12) C25 0.0912(18) 0.0402(11) 0.0452(12) 0.0034(9) -0.0012(11) 0.0024(11) C27 0.160(4) 0.075(2) 0.080(2) 0.0230(17) -0.015(2) -0.053(2) C26 0.171(4) 0.120(3) 0.076(2) 0.021(2) 0.017(2) 0.091(3) O1 0.0376(8) 0.0626(10) 0.0920(12) -0.0210(9) 0.0224(8) -0.0042(7) O2 0.0446(10) 0.0714(13) 0.193(3) -0.0563(15) 0.0283(13) -0.0030(9) O3 0.0340(7) 0.0618(9) 0.0696(10) -0.0198(8) 0.0133(7) -0.0059(6) O4 0.0509(10) 0.0713(12) 0.1305(17) -0.0430(12) 0.0289(10) -0.0046(8) C28 0.0373(11) 0.0565(13) 0.0673(14) -0.0159(11) 0.0080(10) 0.0009(9) C29 0.0350(10) 0.0538(12) 0.0702(14) -0.0135(11) 0.0083(10) -0.0057(9) C30 0.0350(10) 0.0523(12) 0.0597(12) -0.0078(10) 0.0101(9) -0.0062(9) C31 0.0378(10) 0.0553(13) 0.0567(12) -0.0134(10) 0.0122(9) -0.0023(9) 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' 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' Cl Cl 0.3639 0.7018 '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 C11 N1 C12 121.44(15) C11 N1 C13 120.56(15) C12 N1 C13 117.89(15) C6 N2 C5 118.66(16) C8 N3 C19 123.30(18) C8 N3 H3 116.6(19) C19 N3 H3 111.9(18) C9 N4 C25 126.02(18) C9 N4 H4 117.7(18) C25 N4 H4 115.7(18) C2 C1 C12 119.82(19) C2 C1 H1 120.1 C12 C1 H1 120.1 C1 C2 C3 120.92(19) C1 C2 H2 119.5 C3 C2 H2 119.5 C4 C3 C2 120.33(19) C4 C3 H3A 119.8 C2 C3 H3A 119.8 C3 C4 C5 120.3(2) C3 C4 H4A 119.9 C5 C4 H4A 119.9 N2 C5 C4 118.98(18) N2 C5 C12 122.10(17) C4 C5 C12 118.91(18) N2 C6 C7 118.91(17) N2 C6 C11 123.09(17) C7 C6 C11 117.99(17) C8 C7 C6 122.58(17) C8 C7 H7 118.7 C6 C7 H7 118.7 C7 C8 N3 124.35(17) C7 C8 C9 118.60(16) N3 C8 C9 117.03(17) N4 C9 C10 121.88(17) N4 C9 C8 118.74(17) C10 C9 C8 119.37(17) C11 C10 C9 120.91(17) C11 C10 H10 119.5 C9 C10 H10 119.5 N1 C11 C10 123.19(17) N1 C11 C6 116.54(16) C10 C11 C6 120.27(16) N1 C12 C1 122.29(17) N1 C12 C5 118.04(16) C1 C12 C5 119.67(18) C18 C13 C14 121.27(19) C18 C13 N1 119.83(17) C14 C13 N1 118.73(17) C13 C14 C15 118.8(2) C13 C14 H14 120.6 C15 C14 H14 120.6 C16 C15 C14 119.7(2) C16 C15 H15 120.2 C14 C15 H15 120.2 C17 C16 C15 121.3(2) C17 C16 Cl1 119.05(19) C15 C16 Cl1 119.6(2) C16 C17 C18 119.4(2) C16 C17 H17 120.3 C18 C17 H17 120.3 C13 C18 C17 119.3(2) C13 C18 H18 120.3 C17 C18 H18 120.3 C20 C19 C24 118.9(2) C20 C19 N3 119.4(2) C24 C19 N3 121.67(18) C23 C24 C19 121.0(2) C23 C24 H24 119.5 C19 C24 H24 119.5 C22 C23 C24 119.1(2) C22 C23 H23 120.4 C24 C23 H23 120.4 C21 C22 C23 121.0(2) C21 C22 Cl2 119.6(2) C23 C22 Cl2 119.4(2) C22 C21 C20 120.0(2) C22 C21 H21 120.0 C20 C21 H21 120.0 C19 C20 C21 120.0(2) C19 C20 H20 120.0 C21 C20 H20 120.0 N4 C25 C26 108.5(3) N4 C25 C27 108.6(2) C26 C25 C27 114.5(3) N4 C25 H25 108.4 C26 C25 H25 108.4 C27 C25 H25 108.4 C25 C27 H27A 109.5 C25 C27 H27B 109.5 H27A C27 H27B 109.5 C25 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C25 C26 H26A 109.5 C25 C26 H26B 109.5 H26A C26 H26B 109.5 C25 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C28 O1 H1A 109(2) O2 C28 O1 123.6(2) O2 C28 C29 121.0(2) O1 C28 C29 115.38(19) C30 C29 C28 124.4(2) C30 C29 H29 117.8 C28 C29 H29 117.8 C29 C30 C31 126.1(2) C29 C30 H30 116.9 C31 C30 H30 116.9 O4 C31 O3 124.88(19) O4 C31 C30 117.69(19) O3 C31 C30 117.42(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Cl1 C16 1.737(2) Cl2 C22 1.743(2) N1 C11 1.371(2) N1 C12 1.391(2) N1 C13 1.453(2) N2 C6 1.321(2) N2 C5 1.366(2) N3 C8 1.376(2) N3 C19 1.416(3) N3 H3 0.83(3) N4 C9 1.324(3) N4 C25 1.467(3) N4 H4 0.84(3) C1 C2 1.374(3) C1 C12 1.400(3) C1 H1 0.9300 C2 C3 1.391(3) C2 H2 0.9300 C3 C4 1.368(3) C3 H3A 0.9300 C4 C5 1.411(3) C4 H4A 0.9300 C5 C12 1.413(3) C6 C7 1.416(3) C6 C11 1.457(3) C7 C8 1.362(3) C7 H7 0.9300 C8 C9 1.473(3) C9 C10 1.405(3) C10 C11 1.375(3) C10 H10 0.9300 C13 C18 1.377(3) C13 C14 1.377(3) C14 C15 1.381(3) C14 H14 0.9300 C15 C16 1.375(4) C15 H15 0.9300 C16 C17 1.364(4) C17 C18 1.383(3) C17 H17 0.9300 C18 H18 0.9300 C19 C20 1.379(3) C19 C24 1.383(3) C24 C23 1.380(3) C24 H24 0.9300 C23 C22 1.367(4) C23 H23 0.9300 C22 C21 1.363(4) C21 C20 1.387(4) C21 H21 0.9300 C20 H20 0.9300 C25 C26 1.500(5) C25 C27 1.529(4) C25 H25 0.9800 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C26 H26A 0.9600 C26 H26B 0.9600 C26 H26C 0.9600 O1 C28 1.290(3) O1 H1A 0.94(4) O2 C28 1.200(3) O3 C31 1.282(3) O4 C31 1.224(3) C28 C29 1.486(3) C29 C30 1.304(3) C29 H29 0.9300 C30 C31 1.495(3) C30 H30 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O2 0.83(3) 2.48(3) 3.003(3) 122(2) 1_455 N3 H3 O3 0.83(3) 2.26(3) 3.040(3) 156(3) . N4 H4 O3 0.84(3) 2.17(3) 2.972(2) 160(2) . O1 H1A O3 0.94(4) 1.62(4) 2.550(2) 176(3) 1_655 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 C12 C1 C2 C3 -1.1(3) C1 C2 C3 C4 1.0(3) C2 C3 C4 C5 0.7(3) C6 N2 C5 C4 -179.91(16) C6 N2 C5 C12 -0.4(3) C3 C4 C5 N2 177.18(18) C3 C4 C5 C12 -2.3(3) C5 N2 C6 C7 176.24(16) C5 N2 C6 C11 -2.5(3) N2 C6 C7 C8 179.76(17) C11 C6 C7 C8 -1.4(3) C6 C7 C8 N3 178.23(17) C6 C7 C8 C9 -3.2(3) C19 N3 C8 C7 -1.3(3) C19 N3 C8 C9 -179.85(17) C25 N4 C9 C10 2.1(3) C25 N4 C9 C8 -178.7(2) C7 C8 C9 N4 -173.46(17) N3 C8 C9 N4 5.2(3) C7 C8 C9 C10 5.8(3) N3 C8 C9 C10 -175.57(17) N4 C9 C10 C11 175.65(18) C8 C9 C10 C11 -3.6(3) C12 N1 C11 C10 -179.39(17) C13 N1 C11 C10 4.4(3) C12 N1 C11 C6 0.7(2) C13 N1 C11 C6 -175.49(15) C9 C10 C11 N1 178.91(16) C9 C10 C11 C6 -1.2(3) N2 C6 C11 N1 2.4(2) C7 C6 C11 N1 -176.34(15) N2 C6 C11 C10 -177.49(17) C7 C6 C11 C10 3.7(2) C11 N1 C12 C1 177.30(16) C13 N1 C12 C1 -6.4(2) C11 N1 C12 C5 -3.4(2) C13 N1 C12 C5 172.86(15) C2 C1 C12 N1 178.81(17) C2 C1 C12 C5 -0.5(3) N2 C5 C12 N1 3.4(3) C4 C5 C12 N1 -177.15(16) N2 C5 C12 C1 -177.30(17) C4 C5 C12 C1 2.2(3) C11 N1 C13 C18 -107.6(2) C12 N1 C13 C18 76.1(2) C11 N1 C13 C14 77.1(2) C12 N1 C13 C14 -99.2(2) C18 C13 C14 C15 -2.4(3) N1 C13 C14 C15 172.8(2) C13 C14 C15 C16 -1.3(4) C14 C15 C16 C17 4.6(4) C14 C15 C16 Cl1 -174.4(2) C15 C16 C17 C18 -4.2(4) Cl1 C16 C17 C18 174.80(18) C14 C13 C18 C17 2.8(3) N1 C13 C18 C17 -172.32(19) C16 C17 C18 C13 0.5(3) C8 N3 C19 C20 -124.4(2) C8 N3 C19 C24 57.4(3) C20 C19 C24 C23 1.3(3) N3 C19 C24 C23 179.5(2) C19 C24 C23 C22 -1.2(4) C24 C23 C22 C21 0.0(4) C24 C23 C22 Cl2 179.46(19) C23 C22 C21 C20 1.2(4) Cl2 C22 C21 C20 -178.3(2) C24 C19 C20 C21 -0.1(4) N3 C19 C20 C21 -178.4(2) C22 C21 C20 C19 -1.1(4) C9 N4 C25 C26 89.0(3) C9 N4 C25 C27 -146.0(3) O2 C28 C29 C30 177.2(3) O1 C28 C29 C30 -3.0(4) C28 C29 C30 C31 176.9(2) C29 C30 C31 O4 179.5(3) C29 C30 C31 O3 -1.5(4) _cod_database_fobs_code 2108441