#------------------------------------------------------------------------------ #$Date: 2024-12-03 04:59:07 +0200 (Tue, 03 Dec 2024) $ #$Revision: 296196 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312715.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_2312715 loop_ _publ_author_name 'Kanthapazham, Rajakumar' 'Osipov, Artyom A.' 'Zherebtsov, Dmitry A.' 'Efremov, Andrey N.' 'Nayfert, Sergey A.' 'Adonin, Sergey A.' 'Spiridonova, Dar'ya V.' 'Atapin, Sergey V.' _publ_section_title ; Structures of hexamethyl-[1,1'-biphenyl]-4,4'-diammonium salts. ; _journal_coeditor_code AW5097 _journal_issue 6 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_paper_doi 10.1107/S2052520624009818 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety '2(C8 H5 O4), C18 H26 N2, 6(H2 O)' _chemical_formula_sum 'C34 H48 N2 O14' _chemical_formula_weight 708.74 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-02-07 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _cell_angle_alpha 90 _cell_angle_beta 99.836(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 12.9176(2) _cell_length_b 8.8157(2) _cell_length_c 15.5173(2) _cell_measurement_reflns_used 10931 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 79.4600 _cell_measurement_theta_min 3.4460 _cell_volume 1741.10(5) _computing_cell_refinement 'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.103a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 85.00 112.00 0.50 0.15 -- 47.38 125.00-120.00 54 2 \w 77.00 104.00 0.50 0.15 -- 47.38 125.00 -30.00 54 3 \w 75.00 110.00 0.50 0.15 -- 47.38 125.00 0.00 70 4 \w 75.00 119.00 0.50 0.15 -- 47.38 125.00 60.00 88 5 \w 74.00 119.00 0.50 0.15 -- 47.38 125.00 90.00 90 6 \w 113.00 176.00 0.50 0.80 -- 113.25 15.00-120.00 126 7 \w 43.00 71.00 0.50 0.80 -- 113.25 -61.00-180.00 56 8 \w 44.00 69.00 0.50 0.80 -- 113.25 -61.00-120.00 50 9 \w 44.00 71.00 0.50 0.80 -- 113.25 -61.00 -60.00 54 10 \w 48.00 100.00 0.50 0.80 -- 113.25 -77.00 30.00 104 11 \w 42.00 67.00 0.50 0.80 -- 113.25 -61.00 30.00 50 12 \w 42.00 67.00 0.50 0.80 -- 113.25 -61.00 60.00 50 13 \w 42.00 67.00 0.50 0.80 -- 113.25 -61.00 90.00 50 14 \w 43.00 70.00 0.50 0.80 -- 113.25 -61.00 120.00 54 15 \w 84.00 170.00 0.50 0.80 -- 113.25 105.00 145.00 172 16 \w 43.00 68.00 0.50 0.80 -- 113.25 -61.00-150.00 50 17 \w -64.00 -36.00 0.50 0.80 -- -106.00 61.00 -30.00 56 18 \w -103.00 -77.00 0.50 0.80 -- -106.00 77.00 -90.00 52 19 \w -64.00 -38.00 0.50 0.80 -- -106.00 77.00-180.00 52 20 \w -106.00 -80.00 0.50 0.80 -- -106.00 77.00-180.00 52 21 \w -58.00 -33.00 0.50 0.80 -- -106.00 77.00 -90.00 50 22 \w -69.00 -35.00 0.50 0.80 -- -106.00 61.00 -90.00 68 23 \w -58.00 -33.00 0.50 0.80 -- -106.00 61.00 0.00 50 24 \w 69.00 106.00 0.50 0.80 -- 113.25-105.00 44.00 74 25 \w 1.00 70.00 0.50 0.15 -- 47.38-105.00 44.00 138 26 \w -71.00 -46.00 0.50 0.80 -- -106.00 61.00 150.00 50 27 \w -105.00 -55.00 0.50 0.80 -- -106.00 105.00 145.00 100 28 \w -110.00 -75.00 0.50 0.80 -- -106.00 125.00 60.00 70 29 \w -70.00 -38.00 0.50 0.80 -- -106.00 125.00 60.00 64 30 \w -74.00 -10.00 0.50 0.15 -- -47.38 105.00 145.00 128 31 \w -176.00-118.00 0.50 0.80 -- -106.00 -30.00 60.00 116 32 \w -172.00-146.00 0.50 0.80 -- -106.00 -77.00 90.00 52 33 \w -117.00 -91.00 0.50 0.80 -- -106.00-105.00 44.00 52 34 \w -117.00 -86.00 0.50 0.80 -- -106.00 -77.00 90.00 62 35 \w -108.00 -73.00 0.50 0.15 -- -47.38-125.00 120.00 70 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1196620000 _diffrn_orient_matrix_UB_12 0.0134193000 _diffrn_orient_matrix_UB_13 0.0041315000 _diffrn_orient_matrix_UB_21 0.0047946000 _diffrn_orient_matrix_UB_22 -0.1682549000 _diffrn_orient_matrix_UB_23 -0.0259670000 _diffrn_orient_matrix_UB_31 -0.0176162000 _diffrn_orient_matrix_UB_32 0.0453154000 _diffrn_orient_matrix_UB_33 -0.0972549000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_unetI/netI 0.0221 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13802 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.977 _diffrn_reflns_theta_min 3.473 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.103a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.352 _exptl_crystal_description prism _exptl_crystal_F_000 756 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.249 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.037 _refine_ls_extinction_coef 0.00108(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 277 _refine_ls_number_reflns 3298 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.051 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0304 _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^)+(0.0399P)^2^+0.5555P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.0830 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3075 _reflns_number_total 3298 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file aw5097sup1.cif _cod_data_source_block tahmbc _cod_database_code 2312715 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C27 H28 O7 N2' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.949 _shelx_estimated_absorpt_t_min 0.857 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2. Others Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C12A)=Sof(H12A)=Sof(C13A)= Sof(H13A)=1-FVAR(1) Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1) 3.a Free rotating group: O7(H7A,H7B), O6(H6A,H6B), O5(H5A,H5B) 3.b Aromatic/amide H refined with riding coordinates: C2(H2), C5(H5), C3(H3), C6(H6), C12(H12), C13(H13), C15(H15), C16A(H16A), C16(H16), C15A(H15A), C12A(H12A), C13A(H13A) 3.c Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C) 3.d Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL tahmbc_a.res in P2(1)/c tahmbc.res created by SHELXL-2018/3 at 14:12:18 on 07-Feb-2024 REM Old TITL TAHMBC_auto in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.177, Rweak 0.031, Alpha 0.024 REM 0.765 for 245 systematic absences, Orientation as input REM Formula found by SHELXT: C17 N O7 CELL 1.54184 12.9176 8.8157 15.5173 90 99.836 90 ZERR 2 0.0002 0.0002 0.0002 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 68 96 4 28 L.S. 15 PLAN 2 SIZE 0.18 0.14 0.06 TEMP -173 CONF HTAB BOND list 4 MORE -1 BOND $H fmap 2 53 ACTA OMIT -4 140 REM REM REM WGHT 0.039900 0.555500 EXTI 0.001079 FVAR 0.57290 0.52032 O4 4 -0.371374 0.366775 0.497780 11.00000 0.01728 0.02135 = 0.02159 0.00300 -0.00125 -0.00016 O1 4 0.136722 0.301535 0.782421 11.00000 0.01570 0.02876 = 0.02506 0.00089 -0.00372 -0.00430 AFIX 147 H1 2 0.197253 0.329304 0.805742 11.00000 -1.50000 AFIX 0 O3 4 -0.368587 0.148601 0.569715 11.00000 0.01659 0.02170 = 0.02723 0.00430 -0.00281 -0.00410 O2 4 0.163679 0.464949 0.677672 11.00000 0.01649 0.03051 = 0.02604 -0.00207 0.00404 -0.00634 C1 1 -0.003154 0.345129 0.666963 11.00000 0.01549 0.02106 = 0.01781 -0.00438 0.00282 -0.00124 C7 1 0.107710 0.376494 0.708728 11.00000 0.01651 0.02096 = 0.02034 -0.00594 0.00336 -0.00030 C4 1 -0.211422 0.294551 0.588910 11.00000 0.01598 0.01915 = 0.01509 -0.00309 0.00217 -0.00101 C2 1 -0.060335 0.228517 0.696555 11.00000 0.01976 0.02544 = 0.02061 0.00379 -0.00220 -0.00312 AFIX 43 H2 2 -0.028708 0.166050 0.743664 11.00000 -1.20000 AFIX 0 C5 1 -0.154086 0.411562 0.559373 11.00000 0.01981 0.02479 = 0.02111 0.00488 0.00035 -0.00193 AFIX 43 H5 2 -0.186023 0.474645 0.512671 11.00000 -1.20000 AFIX 0 C3 1 -0.163381 0.203397 0.657381 11.00000 0.01916 0.02267 = 0.02285 0.00375 -0.00042 -0.00598 AFIX 43 H3 2 -0.201847 0.122797 0.677521 11.00000 -1.20000 AFIX 0 C6 1 -0.050385 0.436280 0.597989 11.00000 0.01982 0.02519 = 0.02360 0.00278 0.00405 -0.00596 AFIX 43 H6 2 -0.011433 0.515747 0.577277 11.00000 -1.20000 AFIX 0 C8 1 -0.325299 0.266051 0.549389 11.00000 0.01691 0.01819 = 0.01434 -0.00221 0.00170 -0.00062 N1 3 0.638129 0.546497 0.819567 11.00000 0.01408 0.01602 = 0.01591 0.00012 0.00029 0.00068 C11 1 0.746282 0.534048 0.872394 11.00000 0.01420 0.01845 = 0.01745 0.00272 -0.00074 -0.00026 C14 1 0.946459 0.507011 0.973553 11.00000 0.01686 0.01900 = 0.01845 0.00190 0.00002 -0.00073 C17 1 0.561700 0.460289 0.864265 11.00000 0.01550 0.02543 = 0.02446 0.00527 0.00423 0.00016 AFIX 137 H17A 2 0.582674 0.353431 0.869912 11.00000 -1.50000 H17B 2 0.491056 0.468025 0.829485 11.00000 -1.50000 H17C 2 0.561627 0.503305 0.922490 11.00000 -1.50000 AFIX 0 C18 1 0.601527 0.708690 0.809869 11.00000 0.02628 0.01672 = 0.02530 0.00109 -0.00527 0.00489 AFIX 137 H18A 2 0.596614 0.750405 0.867572 11.00000 -1.50000 H18B 2 0.532345 0.712790 0.772405 11.00000 -1.50000 H18C 2 0.651794 0.768458 0.783318 11.00000 -1.50000 AFIX 0 C19 1 0.633288 0.482636 0.729101 11.00000 0.02012 0.03104 = 0.01620 -0.00372 -0.00073 0.00391 AFIX 137 H19A 2 0.685824 0.533061 0.700364 11.00000 -1.50000 H19B 2 0.563110 0.499727 0.695018 11.00000 -1.50000 H19C 2 0.647774 0.373502 0.732967 11.00000 -1.50000 AFIX 0 PART 1 C12 1 0.773983 0.610451 0.948210 21.00000 0.01793 0.02244 = 0.02061 -0.00114 0.00576 0.00514 AFIX 43 H12 2 0.724085 0.674806 0.968249 21.00000 -1.20000 AFIX 0 C13 1 0.873736 0.596961 0.997441 21.00000 0.01808 0.02460 = 0.01492 -0.00266 -0.00028 0.00042 AFIX 43 H13 2 0.890683 0.653841 1.049958 21.00000 -1.20000 AFIX 0 C15 1 0.923632 0.431188 0.890924 21.00000 0.01411 0.02903 = 0.02426 -0.00647 0.00045 0.00601 AFIX 43 H15 2 0.976322 0.372657 0.870585 21.00000 -1.20000 AFIX 0 PART 2 C16A 1 0.798904 0.401192 0.873073 -21.00000 0.01826 0.01566 = 0.02118 -0.00299 -0.00087 -0.00080 AFIX 43 H16A 2 0.768218 0.317682 0.839320 -21.00000 -1.20000 AFIX 0 PART 1 C16 1 0.824251 0.443451 0.840599 21.00000 0.01919 0.02945 = 0.02014 -0.00792 0.00053 0.00188 AFIX 43 H16 2 0.808018 0.392705 0.785949 21.00000 -1.20000 AFIX 0 PART 2 C15A 1 0.897891 0.388110 0.923424 -21.00000 0.01688 0.01660 = 0.02519 0.00113 0.00228 0.00274 AFIX 43 H15A 2 0.934001 0.294186 0.923706 -21.00000 -1.20000 AFIX 6 PART 0 O7 4 0.412369 0.169932 0.980400 11.00000 0.01657 0.02023 = 0.03176 -0.00061 -0.00004 0.00264 H7A 2 0.480439 0.171181 0.984970 11.00000 -1.50000 H7B 2 0.391069 0.076943 0.984262 11.00000 -1.50000 AFIX 6 O6 4 0.317239 0.371648 0.863746 11.00000 0.01735 0.02114 = 0.02714 -0.00236 -0.00431 -0.00037 H6A 2 0.346293 0.303851 0.900901 11.00000 -1.50000 H6B 2 0.328773 0.461600 0.886355 11.00000 -1.50000 AFIX 6 O5 4 -0.369415 0.410803 0.318310 11.00000 0.01848 0.03069 = 0.02302 0.00439 -0.00041 -0.00660 H5A 2 -0.365631 0.398387 0.374380 11.00000 -1.50000 H5B 2 -0.309235 0.450397 0.312818 11.00000 -1.50000 AFIX 0 PART 2 C12A 1 0.783358 0.652127 0.929449 -21.00000 0.01461 0.01491 = 0.02009 -0.00048 0.00121 0.00136 AFIX 43 H12A 2 0.741925 0.739967 0.933695 -21.00000 -1.20000 AFIX 0 C13A 1 0.882482 0.637236 0.979704 -21.00000 0.01638 0.01706 = 0.02062 -0.00344 0.00088 -0.00135 AFIX 43 H13A 2 0.908532 0.715955 1.019348 -21.00000 -1.20000 AFIX 0 HKLF 4 REM tahmbc_a.res in P2(1)/c REM wR2 = 0.0830, GooF = S = 1.051, Restrained GooF = 1.051 for all data REM R1 = 0.0304 for 3075 Fo > 4sig(Fo) and 0.0324 for all 3298 data REM 277 parameters refined using 0 restraints END WGHT 0.0399 0.5555 REM Instructions for potential hydrogen bonds HTAB O1 O6 EQIV $2 x+1, -y+1/2, z+1/2 HTAB C17 O5_$2 HTAB C17 O6 EQIV $3 -x+1, -y+1, -z+2 HTAB C18 O7_$3 EQIV $4 -x, -y+1, -z+1 HTAB C18 O5_$4 EQIV $5 -x+1, y+1/2, -z+3/2 HTAB C18 O6_$5 HTAB C19 O5_$4 HTAB C12 O7_$3 REM Highest difference peak 0.249, deepest hole -0.182, 1-sigma level 0.037 Q1 1 1.0000 0.5000 1.0000 10.50000 0.05 0.25 Q2 1 -0.2622 0.2735 0.5676 11.00000 0.05 0.23 ; _shelx_res_checksum 63388 _shelx_hkl_file ; 0 0 -1 0.23 0.11 0 0 -1 0.19 0.14 0 0 -2 1.31 0.32 0 0 -2 0.88 0.30 0 0 -3 0.38 0.37 0 0 -3 0.15 0.38 0 0 -4 54.94 2.57 0 0 -4 49.33 2.65 0 0 -5 -0.54 0.59 0 0 -5 -0.22 0.49 0 0 -6 2312.41 64.02 0 0 -6 2178.03 64.47 0 0 -7 0.21 0.76 0 0 -7 0.17 0.59 0 0 -8 542.48 17.65 0 0 -8 510.21 18.05 0 0 -9 -0.23 0.62 0 0 -9 -0.59 0.88 0 0 -10 201.41 6.31 0 0 -10 198.74 6.26 0 0 -10 207.21 9.12 0 0 -11 0.15 0.37 0 0 -11 0.62 0.72 0 0 -11 -0.12 0.32 0 0 -11 0.14 0.33 0 0 -11 0.29 0.38 0 0 -12 25.08 1.59 0 0 -12 21.20 1.38 0 0 -12 21.88 1.50 0 0 -12 21.24 1.39 0 0 -12 23.81 1.28 0 0 -12 24.56 1.40 0 0 -13 0.17 0.45 0 0 -13 -0.07 0.45 0 0 -13 -0.11 0.31 0 0 -13 -0.07 0.34 0 0 -13 -0.07 0.46 0 0 -13 -0.09 0.50 0 0 -14 41.73 1.88 0 0 -14 43.41 2.14 0 0 -14 39.96 2.26 0 0 -14 43.88 2.28 0 0 -14 46.63 2.16 0 0 -15 -0.07 0.46 0 0 -15 -0.25 0.43 0 0 -15 -0.27 0.55 0 0 -15 -0.07 0.46 0 0 -15 0.34 0.49 0 0 -16 79.43 3.10 0 0 -16 80.63 3.10 0 0 -16 79.16 3.24 0 0 -16 80.32 3.33 0 0 -16 79.51 2.98 0 0 -17 0.16 0.36 0 0 -17 -0.21 0.39 0 0 -17 0.14 0.45 0 0 -18 5.96 0.58 0 0 -18 5.49 0.56 0 1 0 0.11 0.10 0 1 -1 528.17 15.80 0 1 -1 543.69 15.62 0 -1 -1 547.80 15.63 0 -1 -1 561.24 15.56 0 1 -1 584.74 15.59 0 -1 -2 1838.27 50.84 0 1 -2 1727.26 50.77 0 1 -2 1831.72 50.69 0 -1 -2 1897.76 50.70 0 1 -3 219.03 7.33 0 -1 -3 216.59 7.33 0 1 -3 240.17 7.25 0 -1 -3 223.19 7.17 0 -1 -4 99.24 4.13 0 1 -4 99.73 4.13 0 -1 -4 93.15 3.82 0 1 -4 99.32 3.92 0 1 -5 1543.75 44.66 0 -1 -5 1516.82 44.63 0 -1 -5 1538.83 44.24 0 1 -5 1588.39 44.30 0 1 -6 763.90 24.12 0 -1 -6 768.96 24.11 0 1 -6 790.74 23.68 0 -1 -6 791.65 23.60 0 -1 -7 461.55 16.27 0 1 -7 474.31 16.30 0 1 -7 475.99 15.77 0 -1 -7 504.01 15.82 0 -1 -8 16.24 2.21 0 1 -8 20.47 2.36 0 1 -8 16.69 2.00 0 -1 -8 22.83 2.19 0 1 -9 5.61 1.52 0 -1 -9 7.67 1.82 0 1 -9 5.82 1.34 0 -1 -9 7.78 1.47 0 1 -10 960.62 26.69 0 -1 -10 941.01 26.66 0 -1 -10 892.51 29.88 0 1 -10 955.29 30.15 0 -1 -10 935.07 26.64 0 -1 -11 426.34 12.96 0 -1 -11 405.99 12.83 0 -1 -11 428.13 12.87 0 -1 -11 431.88 16.15 0 1 -11 444.59 16.33 0 -1 -11 431.86 12.64 0 -1 -11 428.56 12.59 0 1 -11 440.73 12.69 0 -1 -11 418.38 12.91 0 1 -11 418.65 12.92 0 -1 -11 437.25 12.65 0 -1 -12 1.83 0.49 0 1 -12 3.54 0.53 0 -1 -12 1.80 0.60 0 1 -12 1.95 0.55 0 -1 -12 3.11 0.65 0 1 -12 2.19 0.60 0 -1 -12 2.14 0.56 0 -1 -12 2.99 0.64 0 1 -12 3.41 0.61 0 -1 -12 2.18 0.47 0 -1 -12 2.79 0.55 0 -1 -13 8.25 0.93 0 -1 -13 8.91 0.96 0 1 -13 8.65 0.93 0 -1 -13 9.15 1.06 0 -1 -13 11.09 0.95 0 1 -13 12.33 1.00 0 -1 -13 10.52 0.90 0 1 -13 10.67 1.09 0 -1 -13 9.89 1.05 0 -1 -13 10.16 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3 6 1.34 0.46 -13 -3 6 0.60 0.40 13 3 -5 86.50 3.08 13 -3 -5 83.82 3.05 -13 3 5 88.10 3.42 -13 3 5 83.73 3.21 -13 -3 5 80.86 3.17 13 3 -4 58.39 2.36 13 -3 -4 60.89 2.39 -13 3 4 63.12 2.74 -13 3 4 58.96 2.50 -13 -3 4 59.52 2.50 13 3 -3 67.83 2.58 13 -3 -3 65.90 2.56 -13 -3 3 62.26 2.65 -13 3 3 68.97 2.73 -13 3 3 65.29 2.91 -13 -3 2 3.53 0.52 -13 3 2 3.32 0.51 13 3 -2 3.26 0.48 13 -3 -2 2.57 0.49 -13 3 2 1.73 0.56 -13 -3 1 170.48 5.67 -13 3 1 182.61 5.74 -13 3 1 166.16 5.94 13 3 -1 172.18 5.53 13 -3 -1 170.90 5.53 -13 3 0 111.23 4.16 13 3 0 107.04 3.72 13 -3 0 108.35 3.74 -13 3 -1 19.58 1.13 13 -3 1 21.61 1.18 -13 3 -2 9.92 0.93 13 -3 2 9.93 0.76 13 -3 3 1.08 0.36 13 -3 4 3.14 0.43 13 -3 5 32.69 1.36 13 -3 6 5.33 0.44 -13 3 -6 5.21 0.58 -13 3 -7 98.33 3.08 -13 3 -8 43.32 1.48 13 -4 -11 117.47 3.60 13 4 -10 54.09 2.05 13 4 -9 35.25 1.57 13 4 -8 10.33 0.82 -13 4 8 10.02 0.78 13 4 -8 11.41 0.71 13 -4 -7 24.50 1.09 13 4 -7 25.92 1.16 -13 4 7 27.02 1.42 -13 4 6 5.97 0.72 13 4 -6 4.73 0.48 13 -4 -6 4.86 0.46 13 -4 -6 5.03 0.63 -13 4 5 41.17 1.98 13 -4 -5 38.49 1.56 -13 4 4 30.59 1.65 13 -4 -4 25.68 1.21 -13 4 3 40.45 1.99 13 -4 -3 36.43 1.53 13 -4 -2 0.98 0.26 -13 4 2 0.44 0.46 -13 4 1 0.89 0.32 13 -4 -1 0.71 0.30 -13 4 1 0.50 0.47 -13 4 0 2.05 0.41 13 -4 0 2.31 0.36 -13 4 -1 1.63 0.39 13 -4 1 1.87 0.33 -13 4 -1 1.69 0.51 -13 4 -2 65.99 2.64 -13 4 -2 67.14 2.46 13 -4 2 64.35 2.22 -13 4 -3 21.22 1.19 -13 4 -4 182.01 5.72 -13 4 -5 46.73 1.85 -13 4 -6 10.72 0.67 -13 4 -7 20.00 0.84 13 5 -10 0.81 0.24 13 5 -9 -0.16 0.24 13 5 -8 3.45 0.45 13 5 -8 3.41 0.35 -13 5 8 3.98 0.45 -13 5 7 0.81 0.34 13 5 -7 0.96 0.34 13 5 -7 0.98 0.23 -13 5 6 31.86 1.51 13 5 -6 29.36 1.34 13 5 -6 28.19 1.14 13 -5 -6 31.94 1.43 13 5 -5 9.26 0.70 -13 5 5 12.30 0.91 13 -5 -5 10.85 0.82 13 5 -4 22.25 1.09 -13 5 4 24.38 1.35 -13 5 3 -0.07 0.23 13 -5 -3 -0.05 0.38 -13 5 3 0.18 0.40 -13 5 2 35.42 1.51 13 -5 -2 39.66 1.76 -13 5 1 8.38 0.67 13 -5 -1 11.06 0.83 -13 5 0 2.35 0.38 13 -5 0 2.64 0.48 -13 5 0 2.06 0.46 -13 5 -1 2.28 0.39 -13 5 -1 3.37 0.43 13 -5 1 3.25 0.46 -13 5 -1 1.76 0.40 -13 5 -2 93.70 3.08 13 -5 2 95.36 3.12 -13 5 -2 91.76 3.09 -13 5 -3 44.60 1.61 13 -5 3 37.64 1.46 -13 5 -4 89.81 2.90 -13 5 -5 6.41 0.43 -13 6 7 8.48 0.54 -13 6 6 6.29 0.54 13 -6 -6 5.74 0.49 -13 6 5 42.19 1.69 13 -6 -5 41.26 1.63 -13 6 4 52.66 2.03 13 -6 -3 24.84 1.19 -13 6 2 5.93 0.57 -13 6 2 5.24 0.43 13 -6 -2 6.51 0.56 -13 6 1 0.78 0.23 -13 6 1 1.46 0.34 13 -6 -1 0.98 0.30 -13 6 0 0.61 0.23 -13 6 0 0.47 0.24 13 -6 0 0.64 0.25 -13 6 -1 1.02 0.22 13 -6 1 1.28 0.24 14 0 -13 0.07 0.15 -14 0 12 275.94 8.24 14 0 -12 285.46 8.15 14 0 -11 -0.14 0.27 14 0 -10 1.10 0.37 -14 0 9 -0.28 0.38 14 0 -9 0.18 0.36 -14 0 8 50.75 2.24 14 0 -8 52.74 2.15 -14 0 7 0.13 0.41 14 0 -7 0.11 0.40 -14 0 6 0.61 0.49 14 0 -6 1.02 0.47 -14 0 5 0.14 0.45 14 0 -5 -0.06 0.45 -14 0 4 17.76 1.26 14 0 -4 16.27 1.15 -14 0 3 0.14 0.41 14 0 -3 0.24 0.44 -14 0 2 10.43 0.97 14 0 -2 9.78 0.90 14 0 -1 0.18 0.44 -14 0 1 -0.07 0.44 14 0 0 49.92 2.17 14 0 1 0.06 0.41 14 0 2 33.14 1.62 14 0 3 -0.15 0.38 14 0 4 77.17 2.79 -14 0 -5 -0.13 0.24 14 0 5 0.11 0.31 -14 0 -6 45.37 1.63 -14 0 -7 0.57 0.15 -14 1 12 8.84 0.61 -14 -1 12 10.45 0.65 14 1 -12 10.84 0.60 14 -1 -12 10.27 0.60 -14 1 11 7.65 0.62 -14 -1 11 5.85 0.56 14 1 -11 6.95 0.53 14 -1 -11 7.24 0.56 -14 1 10 58.62 2.28 -14 -1 10 56.59 2.25 14 1 -10 60.06 2.18 14 -1 -10 58.26 2.16 -14 1 9 -0.11 0.38 -14 -1 9 -0.05 0.36 14 1 -9 0.04 0.33 14 -1 -9 0.35 0.34 -14 1 8 13.05 0.96 -14 -1 8 10.14 0.90 14 1 -8 11.34 0.84 14 -1 -8 13.73 0.91 -14 1 7 116.70 4.12 -14 -1 7 113.38 4.09 14 1 -7 115.21 3.97 14 -1 -7 118.54 3.99 -14 1 6 1.12 0.47 -14 -1 6 1.31 0.50 14 1 -6 0.54 0.41 14 -1 -6 1.41 0.46 14 1 -5 14.59 1.02 14 -1 -5 14.95 1.02 -14 1 5 13.81 1.07 -14 -1 5 14.31 1.10 14 1 -4 122.58 4.13 14 -1 -4 118.92 4.11 -14 1 4 116.43 4.25 -14 -1 4 112.45 4.21 14 1 -3 20.58 1.24 14 -1 -3 20.26 1.24 -14 1 3 21.13 1.34 -14 -1 3 20.22 1.32 14 1 -2 52.71 2.26 14 -1 -2 55.44 2.29 -14 -1 2 52.67 2.37 -14 1 2 51.95 2.36 -14 -1 1 20.53 1.32 -14 1 1 18.90 1.27 14 1 -1 22.39 1.28 14 -1 -1 21.18 1.26 14 1 0 120.78 4.17 14 -1 0 120.85 4.17 14 1 1 1.58 0.45 14 -1 1 2.23 0.50 14 1 2 3.34 0.55 14 -1 2 4.11 0.58 14 1 3 23.92 1.25 14 -1 3 24.32 1.25 -14 -1 -4 1.24 0.29 14 1 4 0.54 0.32 14 -1 4 1.17 0.38 -14 1 -5 2.04 0.36 -14 -1 -5 1.55 0.27 14 1 5 2.14 0.39 14 -1 5 1.84 0.37 -14 1 -6 124.07 3.58 14 -1 6 124.63 3.60 14 1 7 0.57 0.15 14 -1 7 1.19 0.17 -14 1 -7 0.95 0.20 14 -2 -12 0.23 0.13 14 -2 -11 0.36 0.22 14 2 -11 0.55 0.24 -14 -2 11 0.58 0.24 14 -2 -10 189.12 5.56 -14 2 10 176.30 5.62 -14 -2 10 186.82 5.65 14 2 -9 8.92 0.68 14 -2 -9 9.90 0.69 -14 2 9 10.64 0.77 -14 -2 9 9.50 0.75 14 2 -8 0.37 0.33 14 -2 -8 0.24 0.32 -14 2 8 0.35 0.39 -14 -2 8 0.45 0.35 14 2 -7 0.27 0.35 14 -2 -7 0.04 0.32 -14 2 7 0.05 0.37 -14 -2 7 -0.05 0.35 -14 2 6 23.54 1.32 -14 -2 6 21.50 1.29 14 2 -6 22.78 1.23 14 -2 -6 23.26 1.23 -14 2 6 22.55 1.25 -14 2 5 31.69 1.63 -14 -2 5 30.99 1.62 14 2 -5 30.92 1.50 14 -2 -5 31.46 1.52 -14 2 5 34.42 1.66 -14 2 4 21.64 1.30 -14 -2 4 22.33 1.33 -14 2 4 24.58 1.40 14 2 -4 22.16 1.23 14 -2 -4 22.76 1.24 14 2 -3 3.89 0.55 14 -2 -3 3.51 0.53 -14 -2 3 3.73 0.57 -14 2 3 4.13 0.57 -14 2 3 3.45 0.62 -14 -2 2 26.33 1.46 -14 2 2 26.93 1.48 -14 2 2 27.39 1.56 14 2 -2 26.95 1.38 14 -2 -2 26.50 1.37 14 2 -1 0.20 0.35 14 -2 -1 0.25 0.34 14 2 0 0.58 0.38 14 -2 0 -0.29 0.37 14 2 1 26.77 1.31 14 -2 1 25.11 1.30 14 2 2 19.13 1.07 14 -2 2 21.45 1.11 14 2 3 18.17 0.99 14 -2 3 18.98 1.00 14 -2 4 70.56 2.45 14 -2 5 53.42 1.88 14 -2 6 66.45 2.11 14 3 -11 29.45 1.14 14 -3 -10 4.18 0.31 14 -3 -9 0.07 0.17 14 3 -9 0.11 0.27 -14 -3 9 0.03 0.21 -14 -3 8 29.22 1.28 14 -3 -8 30.17 1.22 -14 -3 7 50.79 2.00 -14 3 7 55.53 2.06 14 -3 -7 53.34 1.94 -14 -3 6 56.54 2.16 14 -3 -6 55.82 2.06 -14 3 6 56.54 2.25 14 -3 -5 1.04 0.32 -14 -3 5 0.63 0.34 -14 3 5 0.22 0.36 -14 -3 4 48.81 1.98 14 -3 -4 48.71 1.89 -14 3 4 48.53 2.15 -14 -3 3 0.47 0.29 14 -3 -3 0.82 0.29 -14 3 3 0.50 0.41 -14 3 2 33.86 1.73 14 -3 -2 35.69 1.50 -14 3 1 20.41 1.27 14 -3 -1 20.57 1.05 14 -3 0 29.41 1.30 14 -3 1 2.99 0.40 14 -3 2 9.17 0.61 14 -3 3 34.62 1.32 -14 3 -4 17.42 0.90 14 -3 4 13.26 0.65 -14 3 -5 0.41 0.22 -14 3 -5 0.07 0.18 -14 3 -6 16.72 0.72 14 4 -9 2.29 0.33 14 4 -8 11.73 0.71 14 4 -7 149.32 4.66 -14 4 7 150.59 4.65 14 4 -6 14.56 0.85 -14 4 6 16.01 0.95 14 -4 -6 15.30 0.87 14 4 -5 13.32 0.79 -14 4 5 13.06 0.89 14 -4 -5 13.65 0.85 -14 4 4 0.26 0.34 14 4 -4 0.39 0.27 14 -4 -4 0.54 0.33 -14 4 3 3.77 0.56 -14 4 2 6.64 0.69 -14 4 1 67.56 2.60 -14 4 0 -0.03 0.21 -14 4 -1 18.49 0.90 14 -4 2 117.77 3.57 -14 4 -2 105.17 3.47 -14 4 -3 74.31 2.31 14 -4 3 64.03 2.17 -14 4 -4 5.99 0.42 -14 5 6 6.44 0.49 14 -5 -5 2.18 0.33 -14 5 5 2.13 0.36 -14 5 4 95.39 3.20 -14 5 3 27.55 1.27 14 -5 -2 164.84 5.01 -14 5 2 159.39 5.05 14 -5 -1 0.92 0.29 14 -5 0 73.30 2.45 14 -5 1 2.42 0.28 15 0 -11 -0.02 0.15 -15 0 10 7.33 0.55 15 0 -10 7.78 0.51 15 0 -9 0.18 0.27 -15 0 9 0.07 0.26 15 0 -8 2.09 0.38 -15 0 8 2.88 0.44 15 0 -7 0.15 0.30 -15 0 7 0.60 0.36 -15 0 6 62.29 2.41 15 0 -6 61.81 2.31 15 0 -5 -0.26 0.34 -15 0 5 -0.05 0.37 15 0 -4 1.88 0.44 -15 0 4 1.93 0.45 15 0 -3 -0.27 0.39 -15 0 3 -0.10 0.39 15 0 -2 1.58 0.43 -15 0 2 0.51 0.37 15 0 -1 -0.09 0.36 15 0 0 65.69 2.42 15 0 1 0.04 0.30 15 0 2 11.26 0.72 -15 0 -3 0.05 0.16 -15 1 10 13.74 0.72 -15 -1 10 14.99 0.74 15 1 -10 13.16 0.66 15 -1 -10 15.00 0.70 -15 1 9 12.09 0.73 -15 -1 9 11.91 0.73 15 1 -9 11.76 0.67 15 -1 -9 11.71 0.68 -15 1 8 28.23 1.28 -15 -1 8 27.03 1.26 15 1 -8 27.47 1.20 15 -1 -8 27.78 1.21 -15 1 7 0.64 0.33 -15 -1 7 1.72 0.40 15 1 -7 0.90 0.33 15 -1 -7 0.97 0.35 -15 1 6 2.40 0.43 -15 -1 6 1.94 0.42 15 1 -6 2.26 0.43 15 -1 -6 1.71 0.40 -15 1 5 103.75 3.63 -15 -1 5 102.57 3.62 15 1 -5 111.38 3.56 15 -1 -5 105.83 3.54 -15 1 4 48.33 2.02 -15 -1 4 46.88 2.00 15 1 -4 47.25 1.93 15 -1 -4 52.10 1.98 -15 1 3 4.90 0.55 -15 -1 3 4.10 0.53 15 1 -3 4.49 0.52 15 -1 -3 4.01 0.52 15 1 -2 5.70 0.58 15 -1 -2 5.73 0.58 15 1 -1 5.91 0.55 15 -1 -1 6.24 0.58 15 1 0 1.14 0.36 15 -1 0 1.10 0.35 15 1 1 0.55 0.28 15 -1 1 0.18 0.27 15 1 2 6.34 0.53 15 -1 2 6.40 0.54 15 1 3 0.35 0.22 15 -1 3 0.94 0.22 15 -1 4 14.78 0.68 -15 1 -4 16.16 0.68 15 -2 -9 60.93 1.99 15 2 -9 62.17 2.10 -15 -2 8 9.60 0.64 15 -2 -8 11.51 0.61 -15 -2 7 79.71 2.66 15 -2 -7 76.59 2.58 -15 2 6 20.90 1.04 -15 -2 6 19.67 1.01 15 -2 -6 19.74 0.96 -15 2 5 5.60 0.55 15 2 -5 4.96 0.47 15 -2 -5 4.91 0.50 -15 -2 5 4.36 0.51 15 2 -4 11.14 0.70 15 -2 -4 10.70 0.70 -15 -2 4 9.34 0.73 -15 2 4 12.22 0.79 15 2 -3 0.56 0.26 15 -2 -3 0.49 0.26 15 2 -2 63.86 2.31 15 -2 -2 68.67 2.35 15 2 -1 0.07 0.28 15 -2 -1 -0.17 0.28 15 -2 0 227.97 6.76 15 -2 1 69.43 2.34 15 -2 2 102.19 3.19 15 -2 3 28.64 1.06 -15 2 -4 1.30 0.22 15 3 -8 13.71 0.68 15 3 -7 3.79 0.39 15 -3 -6 22.52 0.92 15 3 -6 29.77 1.13 15 -3 -5 20.12 0.86 15 3 -5 23.12 0.99 15 -3 -4 0.54 0.18 15 3 -4 0.03 0.20 15 -3 -3 38.64 1.39 15 -3 -2 5.13 0.39 15 -3 -1 9.04 0.51 15 -3 0 10.70 0.53 -15 3 -1 93.23 2.85 15 -4 -4 1.66 0.30 15 -4 -2 9.76 0.60 15 -4 -1 36.92 1.39 15 -4 0 33.92 1.25 16 0 -7 0.04 0.16 -16 0 6 7.58 0.52 16 0 -6 7.96 0.50 16 0 -5 0.30 0.21 16 0 -4 13.35 0.70 16 0 -3 0.80 0.24 16 1 -7 10.79 0.53 16 -1 -7 12.40 0.56 16 1 -6 3.24 0.32 16 -1 -6 3.80 0.33 16 1 -5 30.58 1.17 16 -1 -5 30.84 1.17 16 1 -4 8.33 0.51 16 -1 -4 7.16 0.50 16 1 -3 3.21 0.34 16 -1 -3 3.34 0.34 16 1 -2 5.05 0.39 16 -1 -2 4.57 0.38 16 1 -1 49.70 1.69 16 -1 -1 50.37 1.70 16 1 0 -0.02 0.15 16 -1 0 0.21 0.16 16 -1 1 32.35 1.11 16 -2 -4 5.51 0.34 16 -2 -3 12.50 0.55 0 0 0 0.00 0.00 TITL TAHMBC_auto in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 12.917645 8.815726 15.517320 90.0000 99.8358 90.0000 ZERR 3.00 0.000224 0.000154 0.000235 0.0000 0.0016 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 81.00 84.00 6.00 21.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 12790 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.302 _oxdiff_exptl_absorpt_empirical_full_min 0.762 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O4 O -0.37137(6) 0.36677(9) 0.49778(5) 0.02061(18) Uani 1 1 d . . . . . O1 O 0.13672(6) 0.30154(9) 0.78242(5) 0.02402(19) Uani 1 1 d . . . . . H1 H 0.197253 0.329304 0.805742 0.036 Uiso 1 1 calc R U . . . O3 O -0.36859(6) 0.14860(9) 0.56972(5) 0.02261(19) Uani 1 1 d . . . . . O2 O 0.16368(6) 0.46495(9) 0.67767(5) 0.02430(19) Uani 1 1 d . . . . . C1 C -0.00315(8) 0.34513(12) 0.66696(7) 0.0181(2) Uani 1 1 d . . . . . C7 C 0.10771(8) 0.37649(12) 0.70873(7) 0.0192(2) Uani 1 1 d . . . . . C4 C -0.21142(8) 0.29455(12) 0.58891(6) 0.0168(2) Uani 1 1 d . . . . . C2 C -0.06034(9) 0.22852(13) 0.69656(7) 0.0226(2) Uani 1 1 d . . . . . H2 H -0.028708 0.166050 0.743664 0.027 Uiso 1 1 calc R U . . . C5 C -0.15409(9) 0.41156(13) 0.55937(7) 0.0223(2) Uani 1 1 d . . . . . H5 H -0.186023 0.474645 0.512671 0.027 Uiso 1 1 calc R U . . . C3 C -0.16338(9) 0.20340(13) 0.65738(7) 0.0220(2) Uani 1 1 d . . . . . H3 H -0.201847 0.122797 0.677521 0.026 Uiso 1 1 calc R U . . . C6 C -0.05038(9) 0.43628(13) 0.59799(7) 0.0228(2) Uani 1 1 d . . . . . H6 H -0.011433 0.515747 0.577277 0.027 Uiso 1 1 calc R U . . . C8 C -0.32530(8) 0.26605(12) 0.54939(6) 0.0166(2) Uani 1 1 d . . . . . N1 N 0.63813(6) 0.54650(10) 0.81957(5) 0.01560(19) Uani 1 1 d . . . . . C11 C 0.74628(8) 0.53405(12) 0.87239(7) 0.0171(2) Uani 1 1 d . . . . . C14 C 0.94646(8) 0.50701(12) 0.97355(7) 0.0185(2) Uani 1 1 d . . . . . C17 C 0.56170(8) 0.46029(13) 0.86427(7) 0.0217(2) Uani 1 1 d . . . . . H17A H 0.582674 0.353431 0.869912 0.033 Uiso 1 1 calc R U . . . H17B H 0.491056 0.468025 0.829485 0.033 Uiso 1 1 calc R U . . . H17C H 0.561627 0.503305 0.922490 0.033 Uiso 1 1 calc R U . . . C18 C 0.60153(9) 0.70869(12) 0.80987(7) 0.0239(2) Uani 1 1 d . . . . . H18A H 0.596614 0.750405 0.867572 0.036 Uiso 1 1 calc R U . . . H18B H 0.532345 0.712790 0.772405 0.036 Uiso 1 1 calc R U . . . H18C H 0.651794 0.768458 0.783318 0.036 Uiso 1 1 calc R U . . . C19 C 0.63329(9) 0.48264(14) 0.72910(7) 0.0229(2) Uani 1 1 d . . . . . H19A H 0.685824 0.533061 0.700364 0.034 Uiso 1 1 calc R U . . . H19B H 0.563110 0.499727 0.695018 0.034 Uiso 1 1 calc R U . . . H19C H 0.647774 0.373502 0.732967 0.034 Uiso 1 1 calc R U . . . C12 C 0.7740(4) 0.6105(6) 0.9482(3) 0.0200(9) Uani 0.520(7) 1 d . . P A 1 H12 H 0.724085 0.674806 0.968249 0.024 Uiso 0.520(7) 1 calc R U P A 1 C13 C 0.8737(5) 0.5970(6) 0.9974(4) 0.0196(9) Uani 0.520(7) 1 d . . P A 1 H13 H 0.890683 0.653841 1.049958 0.023 Uiso 0.520(7) 1 calc R U P A 1 C15 C 0.9236(2) 0.4312(4) 0.8909(3) 0.0228(8) Uani 0.520(7) 1 d . . P A 1 H15 H 0.976322 0.372657 0.870585 0.027 Uiso 0.520(7) 1 calc R U P A 1 C16A C 0.7989(3) 0.4012(4) 0.8731(3) 0.0189(8) Uani 0.480(7) 1 d . . P A 2 H16A H 0.768218 0.317682 0.839320 0.023 Uiso 0.480(7) 1 calc R U P A 2 C16 C 0.8243(2) 0.4435(4) 0.8406(3) 0.0233(8) Uani 0.520(7) 1 d . . P A 1 H16 H 0.808018 0.392705 0.785949 0.028 Uiso 0.520(7) 1 calc R U P A 1 C15A C 0.8979(3) 0.3881(4) 0.9234(3) 0.0197(8) Uani 0.480(7) 1 d . . P A 2 H15A H 0.934001 0.294186 0.923706 0.024 Uiso 0.480(7) 1 calc R U P A 2 O7 O 0.41237(6) 0.16993(9) 0.98040(5) 0.02334(19) Uani 1 1 d G . . . . H7A H 0.480439 0.171181 0.984970 0.035 Uiso 1 1 d G U . . . H7B H 0.391069 0.076943 0.984262 0.035 Uiso 1 1 d G U . . . O6 O 0.31724(6) 0.37165(9) 0.86375(5) 0.02283(19) Uani 1 1 d G . . . . H6A H 0.346293 0.303851 0.900901 0.034 Uiso 1 1 d G U . . . H6B H 0.328773 0.461600 0.886355 0.034 Uiso 1 1 d G U . . . O5 O -0.36942(6) 0.41080(10) 0.31831(5) 0.02453(19) Uani 1 1 d G . . . . H5A H -0.365631 0.398387 0.374380 0.037 Uiso 1 1 d G U . . . H5B H -0.309235 0.450397 0.312818 0.037 Uiso 1 1 d G U . . . C12A C 0.7834(4) 0.6521(6) 0.9294(3) 0.0167(9) Uani 0.480(7) 1 d . . P A 2 H12A H 0.741925 0.739967 0.933695 0.020 Uiso 0.480(7) 1 calc R U P A 2 C13A C 0.8825(5) 0.6372(7) 0.9797(4) 0.0183(10) Uani 0.480(7) 1 d . . P A 2 H13A H 0.908532 0.715955 1.019348 0.022 Uiso 0.480(7) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O4 0.0173(4) 0.0214(4) 0.0216(4) 0.0030(3) -0.0012(3) -0.0002(3) O1 0.0157(4) 0.0288(4) 0.0251(4) 0.0009(3) -0.0037(3) -0.0043(3) O3 0.0166(4) 0.0217(4) 0.0272(4) 0.0043(3) -0.0028(3) -0.0041(3) O2 0.0165(4) 0.0305(4) 0.0260(4) -0.0021(3) 0.0040(3) -0.0063(3) C1 0.0155(5) 0.0211(5) 0.0178(5) -0.0044(4) 0.0028(4) -0.0012(4) C7 0.0165(5) 0.0210(5) 0.0203(5) -0.0059(4) 0.0034(4) -0.0003(4) C4 0.0160(5) 0.0192(5) 0.0151(5) -0.0031(4) 0.0022(4) -0.0010(4) C2 0.0198(5) 0.0254(6) 0.0206(5) 0.0038(4) -0.0022(4) -0.0031(4) C5 0.0198(5) 0.0248(6) 0.0211(5) 0.0049(4) 0.0004(4) -0.0019(4) C3 0.0192(5) 0.0227(5) 0.0228(5) 0.0037(4) -0.0004(4) -0.0060(4) C6 0.0198(5) 0.0252(6) 0.0236(5) 0.0028(4) 0.0040(4) -0.0060(4) C8 0.0169(5) 0.0182(5) 0.0143(4) -0.0022(4) 0.0017(4) -0.0006(4) N1 0.0141(4) 0.0160(4) 0.0159(4) 0.0001(3) 0.0003(3) 0.0007(3) C11 0.0142(5) 0.0184(5) 0.0175(5) 0.0027(4) -0.0007(4) -0.0003(4) C14 0.0169(5) 0.0190(5) 0.0184(5) 0.0019(4) 0.0000(4) -0.0007(4) C17 0.0155(5) 0.0254(6) 0.0245(5) 0.0053(4) 0.0042(4) 0.0002(4) C18 0.0263(6) 0.0167(5) 0.0253(5) 0.0011(4) -0.0053(4) 0.0049(4) C19 0.0201(5) 0.0310(6) 0.0162(5) -0.0037(4) -0.0007(4) 0.0039(4) C12 0.0179(15) 0.022(2) 0.0206(19) -0.0011(14) 0.0058(12) 0.0051(16) C13 0.0181(16) 0.025(3) 0.0149(19) -0.0027(15) -0.0003(13) 0.0004(17) C15 0.0141(12) 0.0290(15) 0.0243(15) -0.0065(13) 0.0004(11) 0.0060(11) C16A 0.0183(13) 0.0157(13) 0.0212(16) -0.0030(11) -0.0009(12) -0.0008(10) C16 0.0192(13) 0.0294(15) 0.0201(14) -0.0079(12) 0.0005(11) 0.0019(11) C15A 0.0169(13) 0.0166(13) 0.0252(16) 0.0011(11) 0.0023(12) 0.0027(10) O7 0.0166(4) 0.0202(4) 0.0318(4) -0.0006(3) 0.0000(3) 0.0026(3) O6 0.0173(4) 0.0211(4) 0.0271(4) -0.0024(3) -0.0043(3) -0.0004(3) O5 0.0185(4) 0.0307(4) 0.0230(4) 0.0044(3) -0.0004(3) -0.0066(3) C12A 0.0146(15) 0.015(2) 0.020(2) -0.0005(14) 0.0012(13) 0.0014(14) C13A 0.0164(16) 0.017(2) 0.021(2) -0.0034(15) 0.0009(15) -0.0013(16) 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' 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 C7 O1 H1 109.5 . . ? C2 C1 C7 121.22(10) . . ? C2 C1 C6 119.55(10) . . ? C6 C1 C7 119.23(10) . . ? O1 C7 C1 113.14(9) . . ? O2 C7 O1 124.36(10) . . ? O2 C7 C1 122.49(10) . . ? C5 C4 C8 121.60(9) . . ? C3 C4 C5 119.11(10) . . ? C3 C4 C8 119.28(9) . . ? C1 C2 H2 120.0 . . ? C3 C2 C1 119.95(10) . . ? C3 C2 H2 120.0 . . ? C4 C5 H5 119.9 . . ? C6 C5 C4 120.17(10) . . ? C6 C5 H5 119.9 . . ? C4 C3 H3 119.6 . . ? C2 C3 C4 120.89(10) . . ? C2 C3 H3 119.6 . . ? C1 C6 H6 119.8 . . ? C5 C6 C1 120.32(10) . . ? C5 C6 H6 119.8 . . ? O4 C8 C4 117.14(9) . . ? O3 C8 O4 123.95(9) . . ? O3 C8 C4 118.90(9) . . ? C11 N1 C17 109.54(8) . . ? C11 N1 C18 111.83(8) . . ? C11 N1 C19 111.69(8) . . ? C18 N1 C17 107.82(8) . . ? C19 N1 C17 108.36(8) . . ? C19 N1 C18 107.46(8) . . ? C12 C11 N1 121.6(2) . . ? C12 C11 C16 118.7(2) . . ? C16A C11 N1 119.20(13) . . ? C16A C11 C12A 121.5(3) . . ? C16 C11 N1 119.71(12) . . ? C12A C11 N1 118.6(2) . . ? C13 C14 C14 122.0(3) . 3_767 ? C13 C14 C15 118.8(3) . . ? C15 C14 C14 119.02(15) . 3_767 ? C15A C14 C14 122.30(15) . 3_767 ? C15A C14 C13A 115.7(3) . . ? C13A C14 C14 121.6(3) . 3_767 ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C11 C12 H12 119.3 . . ? C11 C12 C13 121.4(4) . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 122.1(5) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C14 C15 H15 120.1 . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H15 120.1 . . ? C11 C16A H16A 120.3 . . ? C11 C16A C15A 119.4(2) . . ? C15A C16A H16A 120.3 . . ? C11 C16 H16 120.5 . . ? C15 C16 C11 119.0(2) . . ? C15 C16 H16 120.5 . . ? C14 C15A H15A 118.7 . . ? C16A C15A C14 122.6(2) . . ? C16A C15A H15A 118.7 . . ? H7A O7 H7B 109.5 . . ? H6A O6 H6B 109.5 . . ? H5A O5 H5B 104.5 . . ? C11 C12A H12A 121.0 . . ? C13A C12A C11 118.0(5) . . ? C13A C12A H12A 121.0 . . ? C14 C13A H13A 119.1 . . ? C12A C13A C14 121.9(5) . . ? C12A C13A H13A 119.1 . . ? 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 O4 C8 1.2732(13) . ? O1 H1 0.8400 . ? O1 C7 1.3185(14) . ? O3 C8 1.2428(13) . ? O2 C7 1.2174(14) . ? C1 C7 1.4934(14) . ? C1 C2 1.3889(16) . ? C1 C6 1.3930(16) . ? C4 C5 1.3924(15) . ? C4 C3 1.3909(15) . ? C4 C8 1.5149(14) . ? C2 H2 0.9500 . ? C2 C3 1.3834(15) . ? C5 H5 0.9500 . ? C5 C6 1.3881(16) . ? C3 H3 0.9500 . ? C6 H6 0.9500 . ? N1 C11 1.4982(13) . ? N1 C17 1.5058(13) . ? N1 C18 1.5054(13) . ? N1 C19 1.5038(13) . ? C11 C12 1.350(5) . ? C11 C16A 1.353(3) . ? C11 C16 1.437(3) . ? C11 C12A 1.397(5) . ? C14 C14 1.488(2) 3_767 ? C14 C13 1.330(6) . ? C14 C15 1.431(3) . ? C14 C15A 1.389(3) . ? C14 C13A 1.427(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C12 H12 0.9500 . ? C12 C13 1.386(8) . ? C13 H13 0.9500 . ? C15 H15 0.9500 . ? C15 C16 1.388(3) . ? C16A H16A 0.9500 . ? C16A C15A 1.385(3) . ? C16 H16 0.9500 . ? C15A H15A 0.9500 . ? O7 H7A 0.8701 . ? O7 H7B 0.8700 . ? O6 H6A 0.8698 . ? O6 H6B 0.8696 . ? O5 H5A 0.8700 . ? O5 H5B 0.8695 . ? C12A H12A 0.9500 . ? C12A C13A 1.387(8) . ? C13A H13A 0.9500 . ? 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 C1 C2 C3 C4 -0.65(17) . . . . ? C7 C1 C2 C3 179.11(10) . . . . ? C7 C1 C6 C5 -178.56(10) . . . . ? C4 C5 C6 C1 -0.51(17) . . . . ? C2 C1 C7 O1 -10.61(14) . . . . ? C2 C1 C7 O2 170.71(10) . . . . ? C2 C1 C6 C5 0.41(17) . . . . ? C5 C4 C3 C2 0.55(17) . . . . ? C5 C4 C8 O4 -10.62(14) . . . . ? C5 C4 C8 O3 170.41(10) . . . . ? C3 C4 C5 C6 0.03(16) . . . . ? C3 C4 C8 O4 168.24(9) . . . . ? C3 C4 C8 O3 -10.72(15) . . . . ? C6 C1 C7 O1 168.35(10) . . . . ? C6 C1 C7 O2 -10.34(16) . . . . ? C6 C1 C2 C3 0.16(17) . . . . ? C8 C4 C5 C6 178.90(10) . . . . ? C8 C4 C3 C2 -178.35(10) . . . . ? N1 C11 C12 C13 179.1(3) . . . . ? N1 C11 C16A C15A -178.5(2) . . . . ? N1 C11 C16 C15 -179.0(2) . . . . ? N1 C11 C12A C13A 178.3(3) . . . . ? C11 C12 C13 C14 -1.0(5) . . . . ? C11 C16A C15A C14 -0.4(5) . . . . ? C11 C12A C13A C14 0.7(6) . . . . ? C14 C14 C13 C12 179.9(3) 3_767 . . . ? C14 C14 C15 C16 -179.8(3) 3_767 . . . ? C14 C14 C15A C16A -179.0(3) 3_767 . . . ? C14 C14 C13A C12A 178.8(3) 3_767 . . . ? C14 C15 C16 C11 0.7(5) . . . . ? C17 N1 C11 C12 -73.5(3) . . . . ? C17 N1 C11 C16A 73.4(3) . . . . ? C17 N1 C11 C16 108.9(3) . . . . ? C17 N1 C11 C12A -97.3(3) . . . . ? C18 N1 C11 C12 46.0(3) . . . . ? C18 N1 C11 C16A -167.2(3) . . . . ? C18 N1 C11 C16 -131.6(3) . . . . ? C18 N1 C11 C12A 22.2(3) . . . . ? C19 N1 C11 C12 166.4(3) . . . . ? C19 N1 C11 C16A -46.7(3) . . . . ? C19 N1 C11 C16 -11.2(3) . . . . ? C19 N1 C11 C12A 142.7(3) . . . . ? C12 C11 C16 C15 3.3(4) . . . . ? C13 C14 C15 C16 -4.8(4) . . . . ? C15 C14 C13 C12 5.1(5) . . . . ? C16A C11 C12A C13A 7.9(5) . . . . ? C16 C11 C12 C13 -3.2(4) . . . . ? C15A C14 C13A C12A -8.5(5) . . . . ? C12A C11 C16A C15A -8.2(4) . . . . ? C13A C14 C15A C16A 8.3(4) . . . . ? _cod_database_fobs_code 2312715