#------------------------------------------------------------------------------ #$Date: 2018-10-25 05:40:06 +0300 (Thu, 25 Oct 2018) $ #$Revision: 211615 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/12/2021288.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_2021288 loop_ _publ_author_name 'Owczarzak, Agata' 'Przyby\/l, Anna K.' 'Kubicki, Maciej' _publ_section_title ; Different cationic forms of (--)-cytisine in the crystal structures of its simple inorganic salts ; _journal_coeditor_code YF3149 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229618012585 _journal_volume 74 _journal_year 2018 _chemical_absolute_configuration rmad _chemical_formula_iupac 'C22 H31 N4 O2 +, 3I -' _chemical_formula_moiety 'C22 H31 N4 O2 +, 3(I -)' _chemical_formula_sum 'C22 H31 I3 N4 O2' _chemical_formula_weight 764.21 _chemical_name_common ; Hydrogen dicytisinium triiodide ; _chemical_name_systematic ; Hydrogen bis(6-Oxo-7,11-diazatricyclo[7.3.1.0^2,7^]trideca-2,4-dien-11-ium) triiodide ; _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' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.9767(3) _cell_length_b 14.1131(6) _cell_length_c 25.7250(10) _cell_measurement_reflns_used 2627 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 25.5490 _cell_measurement_theta_min 3.3200 _cell_volume 2896.0(2) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2015) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2008) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 295(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1544 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Agilent Xcalibur Eos' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 7561 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 2.887 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 3.260 _exptl_absorpt_correction_T_max 0.04273 _exptl_absorpt_correction_T_min 0.02153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.753 _exptl_crystal_description prism _exptl_crystal_F_000 1464 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _platon_squeeze_details ; ; _refine_diff_density_max 1.762 _refine_diff_density_min -0.988 _refine_ls_abs_structure_details ; Flack x determined using 1314 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 280 _refine_ls_number_reflns 4691 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.998 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0478 _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^)+(0.0866P)^2^+3.3053P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1323 _refine_ls_wR_factor_ref 0.1399 _reflns_number_gt 3988 _reflns_number_total 4691 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yf3149sup1.cif _cod_data_source_block 9 _cod_database_code 2021288 _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_hkl_file ; 0 0 -4 236042 43294 500593 -47.65 0.00 1.0000 0 0 4 229281 40842 510559 -47.65 0.00 1.0000 0 0 -633141616 517791 31271536 6.58 0.00 1.0000 0 0 633017254 516765 31150738 6.58 0.00 1.0000 0 0 -831158454 643655 37966404 23.15 0.00 1.0000 0 0 831775720 641737 38647460 23.15 0.00 1.0000 0 0 1085918800 1263241 82574968 -7.27 0.01 1.0000 0 0 -1085249824 1264399 81919168 -7.27 -0.01 1.0000 0 0 -12 9639345 302041 11502802 -11.45 0.00 1.0000 0 0 12 9891440 299483 11778040 -11.45 0.00 1.0000 0 0 -14 7521709 239100 7178927 2.52 0.01 1.0000 0 0 -1611597953 314079 10889331 4.22 0.00 1.0000 0 0 -1819200578 459841 19185212 -0.07 -0.01 1.0000 0 0 -20 2480093 147346 2353182 -1.63 0.01 1.0000 0 0 -22 2199183 147832 2147148 0.70 0.00 1.0000 0 0 -24 895674 95330 810803 1.83 0.00 1.0000 0 0 -26 964512 107635 967715 -0.07 0.00 1.0000 0 0 -28 2809661 174071 2648637 -1.95 0.00 1.0000 0 0 -30 81241 52531 101067 -1.31 0.00 1.0000 0 1 4 5781578 133007 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-0.01 1.0000 -10 -2 4 95689 54165 105022 -0.17 0.86 1.0000 -10 -2 5 210 53555 -41444 -0.49 0.31 1.0000 -10 -2 6 58388 54006 63728 0.04 0.78 1.0000 -10 -2 7 172989 60716 175381 0.39 -0.33 1.0000 -10 -2 8 9006 46406 7548 -0.65 -0.30 1.0000 -10 -2 9 132013 55964 133697 0.26 0.08 1.0000 -10 3 0 206497 57923 213465 -0.30 0.00 1.0000 -10 3 -1 75279 47240 72704 0.35 -0.04 1.0000 -10 3 -2 332487 68151 316815 -0.20 -0.59 1.0000 0 0 0 241 0 0 -0.20 -0.59 1.0000 0 0 0 241 0 0 -0.20 -0.59 1.0000 ; _shelx_hkl_checksum 47258 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P2(1)2(1)2(1) CELL 0.71073 7.9767 14.1131 25.7250 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0006 0.0010 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O I UNIT 88 124 16 8 12 omit 0 50 omit 4 1 0 omit 3 0 7 omit 4 0 4 FMAP 2 PLAN -10 ACTA BOND $H conf HTAB O2A O2B HTAB O2B O2A EQIV $1 x-1/2, -y+1/2, -z+1 HTAB C11A O2A_$1 EQIV $2 x-1, y, z HTAB C11A I1_$2 HTAB N12A I2_$1 HTAB N12A I1 HTAB C3B O2A EQIV $3 -x+3/2, -y+1, z+1/2 HTAB C7B I1_$3 EQIV $4 x+1, y, z HTAB C9B I2_$4 EQIV $5 x+1/2, -y+1/2, -z+1 HTAB C10B I1_$5 HTAB N12B I3 HTAB N12B I2 L.S. 10 WGHT 0.086600 3.305300 FVAR 25.14345 N1A 3 0.334413 0.468854 0.507747 11.00000 0.05503 0.05417 = 0.03331 -0.00481 -0.00831 -0.00847 C2A 1 0.492931 0.479339 0.528824 11.00000 0.06578 0.06015 = 0.04939 -0.01913 -0.00080 0.01033 O2A 4 0.546070 0.410411 0.556703 11.00000 0.08458 0.06735 = 0.06918 -0.00229 -0.03399 0.01259 AFIX 3 H2 2 0.670710 0.409620 0.583329 11.00000 -1.20000 AFIX 0 C3A 1 0.572974 0.562327 0.519647 11.00000 0.04215 0.06056 = 0.07457 -0.00577 -0.01418 -0.00450 AFIX 43 H3A 2 0.678966 0.570928 0.533948 11.00000 -1.20000 AFIX 0 C4A 1 0.511324 0.628971 0.492619 11.00000 0.07970 0.06407 = 0.09155 -0.00355 -0.01267 -0.02267 AFIX 43 H4A 2 0.572019 0.684541 0.487791 11.00000 -1.20000 AFIX 0 C5A 1 0.346247 0.619052 0.469113 11.00000 0.07781 0.05718 = 0.09368 0.00798 -0.02617 0.00056 AFIX 43 H5A 2 0.300391 0.666394 0.448372 11.00000 -1.20000 AFIX 0 C6A 1 0.262627 0.537280 0.478976 11.00000 0.04881 0.04274 = 0.05968 -0.00856 -0.00666 0.00375 C7A 1 0.087368 0.520386 0.456140 11.00000 0.04420 0.06726 = 0.06693 -0.00802 -0.01925 0.01208 AFIX 13 H7A 2 0.029282 0.581453 0.454031 11.00000 -1.20000 AFIX 0 C8A 1 -0.013705 0.454743 0.492147 11.00000 0.04792 0.08543 = 0.06733 -0.02836 0.00408 0.00516 AFIX 23 H8A 2 -0.024136 0.482442 0.526504 11.00000 -1.20000 H8B 2 -0.125115 0.444094 0.478209 11.00000 -1.20000 AFIX 0 C9A 1 0.083315 0.362611 0.494661 11.00000 0.06109 0.07092 = 0.06663 0.01757 -0.00922 -0.02568 AFIX 13 H9A 2 0.018280 0.318870 0.516311 11.00000 -1.20000 AFIX 0 C10A 1 0.251799 0.378487 0.522065 11.00000 0.07054 0.07763 = 0.06208 0.02703 -0.02614 -0.00669 AFIX 23 H10A 2 0.233800 0.377587 0.559353 11.00000 -1.20000 H10B 2 0.326353 0.326450 0.513558 11.00000 -1.20000 AFIX 0 C11A 1 0.096741 0.318164 0.440778 11.00000 0.06136 0.05860 = 0.07251 0.01072 -0.01455 -0.00903 AFIX 23 H11A 2 0.163751 0.260941 0.442894 11.00000 -1.20000 H11B 2 -0.014277 0.300590 0.428785 11.00000 -1.20000 AFIX 0 N12A 3 0.172796 0.383038 0.403379 11.00000 0.05547 0.08801 = 0.04598 -0.01128 -0.00968 -0.01568 AFIX 23 H12A 2 0.165665 0.357317 0.371868 11.00000 -1.20000 H12B 2 0.281120 0.389017 0.410993 11.00000 -1.20000 AFIX 0 C13A 1 0.097062 0.478359 0.401621 11.00000 0.05350 0.06694 = 0.06469 0.00971 -0.01343 -0.00734 AFIX 23 H13A 2 -0.014658 0.474374 0.386892 11.00000 -1.20000 H13B 2 0.163962 0.519259 0.379531 11.00000 -1.20000 AFIX 0 N1B 3 0.898990 0.439742 0.689196 11.00000 0.04358 0.04158 = 0.04731 0.00300 0.00990 0.00343 C2B 1 0.774167 0.447232 0.652749 11.00000 0.04402 0.04508 = 0.04435 0.01658 -0.00911 -0.01163 O2B 4 0.795884 0.408798 0.609730 11.00000 0.05659 0.06373 = 0.03859 -0.01098 -0.00499 0.00574 C3B 1 0.632079 0.499851 0.667578 11.00000 0.04120 0.06289 = 0.05840 -0.00138 -0.00457 0.00307 AFIX 43 H3B 2 0.542999 0.506623 0.644552 11.00000 -1.20000 AFIX 0 C4B 1 0.624348 0.540234 0.714646 11.00000 0.03172 0.06528 = 0.10829 -0.00403 0.01291 0.01092 AFIX 43 H4B 2 0.531596 0.576928 0.723280 11.00000 -1.20000 AFIX 0 C5B 1 0.749782 0.528662 0.750221 11.00000 0.05667 0.05072 = 0.07204 -0.01470 0.01623 -0.00660 AFIX 43 H5B 2 0.738599 0.553727 0.783475 11.00000 -1.20000 AFIX 0 C6B 1 0.892862 0.479826 0.736788 11.00000 0.05483 0.04278 = 0.04301 -0.00578 0.00441 -0.00269 C7B 1 1.036539 0.466590 0.774850 11.00000 0.06691 0.05245 = 0.04616 -0.00974 -0.00595 0.00361 AFIX 13 H7B 2 1.047289 0.524345 0.795735 11.00000 -1.20000 AFIX 0 C8B 1 1.201603 0.450600 0.745476 11.00000 0.04498 0.08468 = 0.07146 0.02417 -0.02421 -0.01081 AFIX 23 H8C 2 1.227579 0.504904 0.723812 11.00000 -1.20000 H8D 2 1.293144 0.440908 0.769721 11.00000 -1.20000 AFIX 0 C9B 1 1.175688 0.363341 0.712425 11.00000 0.04944 0.06964 = 0.06623 -0.00908 0.00019 0.00300 AFIX 13 H9B 2 1.282745 0.348996 0.695473 11.00000 -1.20000 AFIX 0 C10B 1 1.047345 0.384010 0.669416 11.00000 0.04209 0.07239 = 0.04529 0.00111 0.00574 0.01728 AFIX 23 H10C 2 1.101571 0.419404 0.641811 11.00000 -1.20000 H10D 2 1.008184 0.324572 0.654888 11.00000 -1.20000 AFIX 0 C11B 1 1.130908 0.278154 0.747282 11.00000 0.08476 0.06880 = 0.05314 0.01616 -0.01230 0.01209 AFIX 23 H11C 2 1.102609 0.224870 0.725140 11.00000 -1.20000 H11D 2 1.229535 0.260658 0.767142 11.00000 -1.20000 AFIX 0 N12B 3 0.994540 0.293817 0.782887 11.00000 0.07693 0.06076 = 0.05487 0.01815 -0.01602 -0.00289 AFIX 23 H12D 2 0.992994 0.246491 0.805747 11.00000 -1.20000 H12C 2 0.898876 0.291523 0.765126 11.00000 -1.20000 AFIX 0 C13B 1 1.000064 0.383252 0.811497 11.00000 0.10490 0.08059 = 0.02703 0.00263 -0.01267 -0.02453 AFIX 23 H13C 2 1.086553 0.379934 0.837941 11.00000 -1.20000 H13D 2 0.893477 0.393507 0.828755 11.00000 -1.20000 AFIX 0 I1 5 0.605016 0.368321 0.398248 11.00000 0.05009 0.07673 = 0.05585 -0.00458 -0.00394 -0.00207 I2 5 0.628290 0.230828 0.714231 11.00000 0.06371 0.06647 = 0.05352 -0.00448 0.00832 -0.01562 I3 5 0.966846 0.147173 0.888524 11.00000 0.13332 0.06576 = 0.06767 0.01094 0.01557 0.02242 HKLF 4 REM shelxt_a.res in P2(1)2(1)2(1) REM R1 = 0.0478 for 3988 Fo > 4sig(Fo) and 0.0588 for all 4691 data REM 280 parameters refined using 0 restraints END WGHT 0.0649 6.9818 REM Highest difference peak 1.762, deepest hole -0.988, 1-sigma level 0.113 Q1 1 0.8332 0.1379 0.8802 11.00000 0.05 1.76 Q2 1 0.6086 0.3019 0.7075 11.00000 0.05 0.85 Q3 1 0.6181 0.2998 0.4070 11.00000 0.05 0.50 Q4 1 0.6217 0.7594 0.4971 11.00000 0.05 0.50 Q5 1 0.6722 0.4254 0.3802 11.00000 0.05 0.48 Q6 1 0.6329 0.3124 0.4211 11.00000 0.05 0.45 Q7 1 0.6266 0.4269 0.4230 11.00000 0.05 0.42 Q8 1 0.7543 0.2611 0.7165 11.00000 0.05 0.41 Q9 1 0.8457 0.1539 0.7015 11.00000 0.05 0.39 Q10 1 0.6211 0.3539 0.4331 11.00000 0.05 0.39 ; _shelx_res_checksum 6574 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy N N1A 0.3344(14) 0.4689(8) 0.5077(4) 0.048(3) Uani d 1 C C2A 0.4929(19) 0.4793(11) 0.5288(6) 0.058(4) Uani d 1 O O2A 0.5461(15) 0.4104(8) 0.5567(4) 0.074(3) Uani d 1 H H2 0.6707 0.4096 0.5833 0.088 Uiso d 1 C C3A 0.5730(17) 0.5623(11) 0.5196(7) 0.059(4) Uani d 1 H H3A 0.6790 0.5709 0.5339 0.071 Uiso calc 1 C C4A 0.511(2) 0.6290(13) 0.4926(7) 0.078(5) Uani d 1 H H4A 0.5720 0.6845 0.4878 0.094 Uiso calc 1 C C5A 0.346(2) 0.6191(12) 0.4691(7) 0.076(5) Uani d 1 H H5A 0.3004 0.6664 0.4484 0.091 Uiso calc 1 C C6A 0.2626(17) 0.5373(10) 0.4790(6) 0.050(3) Uani d 1 C C7A 0.0874(17) 0.5204(11) 0.4561(6) 0.059(4) Uani d 1 H H7A 0.0293 0.5815 0.4540 0.071 Uiso calc 1 C C8A -0.0137(19) 0.4547(12) 0.4921(7) 0.067(4) Uani d 1 H H8A -0.0241 0.4824 0.5265 0.080 Uiso calc 1 H H8B -0.1251 0.4441 0.4782 0.080 Uiso calc 1 C C9A 0.0833(19) 0.3626(12) 0.4947(6) 0.066(4) Uani d 1 H H9A 0.0183 0.3189 0.5163 0.079 Uiso calc 1 C C10A 0.252(2) 0.3785(13) 0.5221(6) 0.070(4) Uani d 1 H H10A 0.2338 0.3776 0.5594 0.084 Uiso calc 1 H H10B 0.3264 0.3264 0.5136 0.084 Uiso calc 1 C C11A 0.097(2) 0.3182(11) 0.4408(6) 0.064(4) Uani d 1 H H11A 0.1638 0.2609 0.4429 0.077 Uiso calc 1 H H11B -0.0143 0.3006 0.4288 0.077 Uiso calc 1 N N12A 0.1728(15) 0.3830(10) 0.4034(5) 0.063(3) Uani d 1 H H12A 0.1657 0.3573 0.3719 0.076 Uiso calc 1 H H12B 0.2811 0.3890 0.4110 0.076 Uiso calc 1 C C13A 0.0971(19) 0.4784(11) 0.4016(6) 0.062(4) Uani d 1 H H13A -0.0147 0.4744 0.3869 0.074 Uiso calc 1 H H13B 0.1640 0.5193 0.3795 0.074 Uiso calc 1 N N1B 0.8990(14) 0.4397(7) 0.6892(4) 0.044(2) Uani d 1 C C2B 0.7742(16) 0.4472(9) 0.6527(5) 0.044(3) Uani d 1 O O2B 0.7959(11) 0.4088(7) 0.6097(4) 0.053(2) Uani d 1 C C3B 0.6321(17) 0.4999(10) 0.6676(6) 0.054(3) Uani d 1 H H3B 0.5430 0.5066 0.6446 0.065 Uiso calc 1 C C4B 0.6243(17) 0.5402(11) 0.7146(7) 0.068(4) Uani d 1 H H4B 0.5316 0.5769 0.7233 0.082 Uiso calc 1 C C5B 0.7498(18) 0.5287(10) 0.7502(6) 0.060(4) Uani d 1 H H5B 0.7386 0.5537 0.7835 0.072 Uiso calc 1 C C6B 0.8929(18) 0.4798(9) 0.7368(5) 0.047(3) Uani d 1 C C7B 1.0365(19) 0.4666(10) 0.7748(6) 0.055(3) Uani d 1 H H7B 1.0473 0.5243 0.7957 0.066 Uiso calc 1 C C8B 1.2016(18) 0.4506(13) 0.7455(7) 0.067(5) Uani d 1 H H8C 1.2276 0.5049 0.7238 0.080 Uiso calc 1 H H8D 1.2931 0.4409 0.7697 0.080 Uiso calc 1 C C9B 1.1757(17) 0.3633(11) 0.7124(6) 0.062(4) Uani d 1 H H9B 1.2827 0.3490 0.6955 0.074 Uiso calc 1 C C10B 1.0473(15) 0.3840(11) 0.6694(5) 0.053(3) Uani d 1 H H10C 1.1016 0.4194 0.6418 0.064 Uiso calc 1 H H10D 1.0082 0.3246 0.6549 0.064 Uiso calc 1 C C11B 1.131(2) 0.2782(12) 0.7473(6) 0.069(4) Uani d 1 H H11C 1.1026 0.2249 0.7251 0.083 Uiso calc 1 H H11D 1.2295 0.2607 0.7671 0.083 Uiso calc 1 N N12B 0.9945(18) 0.2938(8) 0.7829(5) 0.064(3) Uani d 1 H H12D 0.9930 0.2465 0.8057 0.077 Uiso calc 1 H H12C 0.8989 0.2915 0.7651 0.077 Uiso calc 1 C C13B 1.000(3) 0.3833(12) 0.8115(5) 0.071(5) Uani d 1 H H13C 1.0866 0.3799 0.8379 0.085 Uiso calc 1 H H13D 0.8935 0.3935 0.8288 0.085 Uiso calc 1 I I1 0.60502(11) 0.36832(7) 0.39825(4) 0.0609(3) Uani d 1 I I2 0.62829(13) 0.23083(7) 0.71423(4) 0.0612(3) Uani d 1 I I3 0.9668(2) 0.14717(8) 0.88852(5) 0.0889(4) Uani d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1A 0.055(6) 0.054(6) 0.033(5) -0.008(5) -0.008(5) -0.005(5) C2A 0.066(9) 0.060(9) 0.049(8) 0.010(8) -0.001(7) -0.019(7) O2A 0.085(7) 0.067(7) 0.069(7) 0.013(6) -0.034(6) -0.002(6) C3A 0.042(7) 0.061(9) 0.075(10) -0.004(6) -0.014(7) -0.006(8) C4A 0.080(10) 0.064(10) 0.092(13) -0.023(10) -0.013(10) -0.004(10) C5A 0.078(10) 0.057(9) 0.094(12) 0.001(9) -0.026(10) 0.008(9) C6A 0.049(7) 0.043(7) 0.060(8) 0.004(6) -0.007(7) -0.009(7) C7A 0.044(7) 0.067(9) 0.067(9) 0.012(7) -0.019(7) -0.008(8) C8A 0.048(8) 0.085(11) 0.067(10) 0.005(8) 0.004(7) -0.028(9) C9A 0.061(9) 0.071(10) 0.067(9) -0.026(8) -0.009(7) 0.018(8) C10A 0.071(9) 0.078(11) 0.062(9) -0.007(9) -0.026(8) 0.027(9) C11A 0.061(9) 0.059(8) 0.073(10) -0.009(8) -0.015(9) 0.011(8) N12A 0.055(6) 0.088(9) 0.046(7) -0.016(6) -0.010(5) -0.011(7) C13A 0.054(7) 0.067(9) 0.065(9) -0.007(7) -0.013(8) 0.010(8) N1B 0.044(5) 0.042(5) 0.047(6) 0.003(5) 0.010(5) 0.003(5) C2B 0.044(7) 0.045(7) 0.044(7) -0.012(6) -0.009(6) 0.017(6) O2B 0.057(5) 0.064(6) 0.039(5) 0.006(4) -0.005(4) -0.011(5) C3B 0.041(7) 0.063(8) 0.058(8) 0.003(7) -0.005(7) -0.001(7) C4B 0.032(6) 0.065(9) 0.108(13) 0.011(7) 0.013(9) -0.004(10) C5B 0.057(9) 0.051(9) 0.072(10) -0.007(7) 0.016(8) -0.015(8) C6B 0.055(7) 0.043(7) 0.043(7) -0.003(7) 0.004(7) -0.006(6) C7B 0.067(8) 0.052(8) 0.046(8) 0.004(7) -0.006(7) -0.010(7) C8B 0.045(7) 0.085(12) 0.071(11) -0.011(8) -0.024(7) 0.024(9) C9B 0.049(7) 0.070(9) 0.066(9) 0.003(7) 0.000(7) -0.009(9) C10B 0.042(6) 0.072(9) 0.045(7) 0.017(7) 0.006(6) 0.001(7) C11B 0.085(11) 0.069(10) 0.053(8) 0.012(10) -0.012(9) 0.016(7) N12B 0.077(8) 0.061(7) 0.055(8) -0.003(6) -0.016(7) 0.018(6) C13B 0.105(12) 0.081(11) 0.027(6) -0.025(10) -0.013(8) 0.003(7) I1 0.0501(4) 0.0767(6) 0.0559(5) -0.0021(5) -0.0039(4) -0.0046(5) I2 0.0637(5) 0.0665(6) 0.0535(5) -0.0156(5) 0.0083(5) -0.0045(5) I3 0.1333(11) 0.0658(6) 0.0677(7) 0.0224(7) 0.0156(7) 0.0109(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' I I -0.4742 1.8119 '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 C6A N1A C2A 121.9(12) C6A N1A C10A 124.4(11) C2A N1A C10A 113.6(11) O2A C2A C3A 126.7(15) O2A C2A N1A 116.1(14) C3A C2A N1A 117.1(14) C2A O2A H2 126.7 C4A C3A C2A 123.6(15) C4A C3A H3A 118.2 C2A C3A H3A 118.2 C3A C4A C5A 120.5(16) C3A C4A H4A 119.8 C5A C4A H4A 119.8 C6A C5A C4A 116.7(15) C6A C5A H5A 121.7 C4A C5A H5A 121.7 N1A C6A C5A 120.3(13) N1A C6A C7A 119.1(12) C5A C6A C7A 120.5(14) C13A C7A C6A 111.5(12) C13A C7A C8A 110.3(13) C6A C7A C8A 109.9(12) C13A C7A H7A 108.4 C6A C7A H7A 108.4 C8A C7A H7A 108.4 C9A C8A C7A 106.0(12) C9A C8A H8A 110.5 C7A C8A H8A 110.5 C9A C8A H8B 110.5 C7A C8A H8B 110.5 H8A C8A H8B 108.7 C8A C9A C11A 110.5(13) C8A C9A C10A 110.0(14) C11A C9A C10A 114.6(15) C8A C9A H9A 107.1 C11A C9A H9A 107.1 C10A C9A H9A 107.1 N1A C10A C9A 113.6(11) N1A C10A H10A 108.8 C9A C10A H10A 108.8 N1A C10A H10B 108.8 C9A C10A H10B 108.8 H10A C10A H10B 107.7 N12A C11A C9A 111.7(12) N12A C11A H11A 109.3 C9A C11A H11A 109.3 N12A C11A H11B 109.3 C9A C11A H11B 109.3 H11A C11A H11B 107.9 C11A N12A C13A 114.9(12) C11A N12A H12A 108.5 C13A N12A H12A 108.5 C11A N12A H12B 108.5 C13A N12A H12B 108.5 H12A N12A H12B 107.5 N12A C13A C7A 110.3(12) N12A C13A H13A 109.6 C7A C13A H13A 109.6 N12A C13A H13B 109.6 C7A C13A H13B 109.6 H13A C13A H13B 108.1 C6B N1B C2B 124.2(12) C6B N1B C10B 123.6(11) C2B N1B C10B 112.3(10) O2B C2B N1B 118.2(12) O2B C2B C3B 125.7(12) N1B C2B C3B 116.1(13) C2B O2B H2 112.4 C4B C3B C2B 120.4(13) C4B C3B H3B 119.8 C2B C3B H3B 119.8 C3B C4B C5B 121.4(13) C3B C4B H4B 119.3 C5B C4B H4B 119.3 C4B C5B C6B 119.9(14) C4B C5B H5B 120.0 C6B C5B H5B 120.0 N1B C6B C5B 117.9(13) N1B C6B C7B 120.4(12) C5B C6B C7B 121.7(12) C6B C7B C8B 110.4(11) C6B C7B C13B 110.3(13) C8B C7B C13B 110.6(14) C6B C7B H7B 108.5 C8B C7B H7B 108.5 C13B C7B H7B 108.5 C9B C8B C7B 106.2(12) C9B C8B H8C 110.5 C7B C8B H8C 110.5 C9B C8B H8D 110.5 C7B C8B H8D 110.5 H8C C8B H8D 108.7 C8B C9B C10B 110.0(12) C8B C9B C11B 109.9(13) C10B C9B C11B 114.4(13) C8B C9B H9B 107.4 C10B C9B H9B 107.4 C11B C9B H9B 107.4 N1B C10B C9B 112.3(11) N1B C10B H10C 109.2 C9B C10B H10C 109.2 N1B C10B H10D 109.2 C9B C10B H10D 109.2 H10C C10B H10D 107.9 N12B C11B C9B 115.2(13) N12B C11B H11C 108.5 C9B C11B H11C 108.5 N12B C11B H11D 108.5 C9B C11B H11D 108.5 H11C C11B H11D 107.5 C11B N12B C13B 115.5(14) C11B N12B H12D 108.4 C13B N12B H12D 108.4 C11B N12B H12C 108.4 C13B N12B H12C 108.4 H12D N12B H12C 107.5 N12B C13B C7B 111.0(11) N12B C13B H13C 109.4 C7B C13B H13C 109.4 N12B C13B H13D 109.4 C7B C13B H13D 109.4 H13C C13B H13D 108.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1A C6A 1.345(18) N1A C2A 1.384(19) N1A C10A 1.48(2) C2A O2A 1.281(18) C2A C3A 1.35(2) O2A H2 1.2074 C3A C4A 1.27(2) C3A H3A 0.9300 C4A C5A 1.46(3) C4A H4A 0.9300 C5A C6A 1.36(2) C5A H5A 0.9300 C6A C7A 1.535(19) C7A C13A 1.52(2) C7A C8A 1.54(2) C7A H7A 0.9800 C8A C9A 1.51(2) C8A H8A 0.9700 C8A H8B 0.9700 C9A C11A 1.53(2) C9A C10A 1.534(19) C9A H9A 0.9800 C10A H10A 0.9700 C10A H10B 0.9700 C11A N12A 1.460(19) C11A H11A 0.9700 C11A H11B 0.9700 N12A C13A 1.48(2) N12A H12A 0.8900 N12A H12B 0.8900 C13A H13A 0.9700 C13A H13B 0.9700 N1B C6B 1.350(16) N1B C2B 1.372(16) N1B C10B 1.509(16) C2B O2B 1.245(16) C2B C3B 1.41(2) O2B H2 1.2076 C3B C4B 1.34(2) C3B H3B 0.9300 C4B C5B 1.37(2) C4B H4B 0.9300 C5B C6B 1.38(2) C5B H5B 0.9300 C6B C7B 1.52(2) C7B C8B 1.53(2) C7B C13B 1.54(2) C7B H7B 0.9800 C8B C9B 1.51(2) C8B H8C 0.9700 C8B H8D 0.9700 C9B C10B 1.535(19) C9B C11B 1.54(2) C9B H9B 0.9800 C10B H10C 0.9700 C10B H10D 0.9700 C11B N12B 1.44(2) C11B H11C 0.9700 C11B H11D 0.9700 N12B C13B 1.46(2) N12B H12D 0.8900 N12B H12C 0.8900 C13B H13C 0.9700 C13B H13D 0.9700 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O2A H2 O2B . 1.21 1.21 2.415(13) 179.7 N12A H12A I2 4_456 0.89 2.56 3.444(12) 174.0 N12A H12B I1 . 0.89 2.62 3.456(12) 156.8 N12B H12D I3 . 0.89 2.56 3.423(12) 164.3 N12B H12C I2 . 0.89 2.67 3.528(13) 163.3 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 C6A N1A C2A O2A 178.1(13) C10A N1A C2A O2A 0.8(18) C6A N1A C2A C3A 0.6(19) C10A N1A C2A C3A -176.7(14) O2A C2A C3A C4A -178.1(18) N1A C2A C3A C4A -1(2) C2A C3A C4A C5A 0(3) C3A C4A C5A C6A 2(3) C2A N1A C6A C5A 1(2) C10A N1A C6A C5A 178.0(15) C2A N1A C6A C7A 179.2(12) C10A N1A C6A C7A -4(2) C4A C5A C6A N1A -2(2) C4A C5A C6A C7A 179.7(14) N1A C6A C7A C13A -91.9(16) C5A C6A C7A C13A 86.3(18) N1A C6A C7A C8A 30.7(18) C5A C6A C7A C8A -151.2(15) C13A C7A C8A C9A 62.6(15) C6A C7A C8A C9A -60.7(15) C7A C8A C9A C11A -61.3(15) C7A C8A C9A C10A 66.2(16) C6A N1A C10A C9A 8(2) C2A N1A C10A C9A -174.6(13) C8A C9A C10A N1A -40.0(19) C11A C9A C10A N1A 85.2(18) C8A C9A C11A N12A 56.2(17) C10A C9A C11A N12A -68.7(17) C9A C11A N12A C13A -50.8(17) C11A N12A C13A C7A 51.5(16) C6A C7A C13A N12A 64.9(16) C8A C7A C13A N12A -57.5(15) C6B N1B C2B O2B 178.4(12) C10B N1B C2B O2B 0.3(16) C6B N1B C2B C3B -0.6(17) C10B N1B C2B C3B -178.8(12) O2B C2B C3B C4B -178.2(14) N1B C2B C3B C4B 1(2) C2B C3B C4B C5B -3(2) C3B C4B C5B C6B 4(2) C2B N1B C6B C5B 2.3(18) C10B N1B C6B C5B -179.8(12) C2B N1B C6B C7B 179.2(12) C10B N1B C6B C7B -2.8(19) C4B C5B C6B N1B -4(2) C4B C5B C6B C7B 179.0(13) N1B C6B C7B C8B 27.8(18) C5B C6B C7B C8B -155.4(14) N1B C6B C7B C13B -94.8(16) C5B C6B C7B C13B 82.1(16) C6B C7B C8B C9B -59.0(15) C13B C7B C8B C9B 63.3(15) C7B C8B C9B C10B 67.8(15) C7B C8B C9B C11B -59.0(16) C6B N1B C10B C9B 10.1(18) C2B N1B C10B C9B -171.8(11) C8B C9B C10B N1B -42.9(17) C11B C9B C10B N1B 81.3(16) C8B C9B C11B N12B 51.9(18) C10B C9B C11B N12B -72.3(17) C9B C11B N12B C13B -45.7(18) C11B N12B C13B C7B 47.4(19) C6B C7B C13B N12B 65.3(18) C8B C7B C13B N12B -57.1(18) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.035 0.222 0.129 78 16 ' ' 2 -0.036 0.722 0.371 78 16 ' ' 3 0.464 0.778 0.629 78 16 ' ' 4 0.535 0.278 0.871 78 16 ' ' _cod_database_fobs_code 2021288