#------------------------------------------------------------------------------ #$Date: 2022-08-19 02:41:48 +0100 (Fri, 19 Aug 2022) $ #$Revision: 277317 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244148.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_2244148 loop_ _publ_author_name 'Priyanka, Prabhakar' 'Jayanna, Bidarur K.' 'Kiran Kumar, Haruvegowda' Vinaya 'Divakara, Thayamma R.' 'Yathirajan, Hemmige S.' 'Parkin, Sean' _publ_section_title ; Synthesis and crystal structure of ebastinium hydrogen fumarate ; _journal_coeditor_code HB8035 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022008118 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C32 H40 N O2 +, C4 H3 O4 -' _chemical_formula_moiety 'C32 H40 N O2 +, C4 H3 O4 -' _chemical_formula_sum 'C36 H43 N O6' _chemical_formula_weight 585.71 _chemical_name_common ; Ebastinium hydrogen fumarate ; _chemical_name_systematic ; 1-[4-(4-tert-Butylphenyl)-4-oxobutyl]-4-(diphenylmethoxy)piperidin-1-ium (E)-3-carboxy-1-hydroxyprop-2-en-1-olate ; _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 direct _atom_sites_solution_secondary difmap _audit_creation_method 'SHELXL-2019/2 and CIFFIX' _cell_angle_alpha 90 _cell_angle_beta 90.975(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 27.091(3) _cell_length_b 6.2408(5) _cell_length_c 18.685(2) _cell_measurement_reflns_used 9606 _cell_measurement_temperature 90.0(2) _cell_measurement_theta_max 27.29 _cell_measurement_theta_min 2.26 _cell_volume 3158.6(5) _computing_cell_refinement ; APEX3 (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; APEX3 (Bruker, 2016) ; _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) and publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2019/2 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 90.0(2) _diffrn_detector_area_resol_mean 7.41 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 Venture dual source' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 55813 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.474 _diffrn_reflns_theta_min 2.180 _diffrn_source microsource _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.232 _exptl_crystal_description plate _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.520 _refine_diff_density_min -0.189 _refine_ls_extinction_coef 0.0017(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2019/2 (Sheldrick 2015b) ; _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 578 _refine_ls_number_reflns 7224 _refine_ls_number_restraints 445 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0469 _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^)+(0.0333P)^2^+1.5370P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1030 _refine_ls_wR_factor_ref 0.1137 _reflns_number_gt 5164 _reflns_number_total 7224 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file hb8035sup1.cif _cod_data_source_block I _cod_original_cell_volume 3158.6(6) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2244148 _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 0.980 _shelx_estimated_absorpt_t_max 0.998 _shelx_hkl_file ; 2 0 0 1.52366 0.90652 2 -2 0 0 1.83636 1.06917 2 -2 0 0 2.38464 0.83749 2 2 0 0 1.34809 1.00029 2 3 0 0 0.57903 1.37927 2 -3 0 0 1.59789 1.44589 2 -3 0 0 1.89988 1.17949 2 3 0 0 1.68726 1.27928 2 -4 0 0 2686.38 107.060 2 4 0 0 2681.01 106.007 2 4 0 0 2675.75 105.642 2 -4 0 0 2685.83 104.112 2 5 0 0 -0.1376 1.45947 2 5 0 0 0.51549 1.81669 2 -5 0 0 0.02681 1.88919 2 -5 0 0 1.26262 1.53661 2 6 0 0 2320.71 93.7739 2 6 0 0 2322.19 91.9398 2 -6 0 0 2325.24 93.1271 2 -6 0 0 2322.55 92.1935 2 -7 0 0 1.17858 1.59602 2 7 0 0 -0.2353 1.56730 2 -7 0 0 -0.6194 1.93117 2 7 0 0 -2.3756 1.35376 2 8 0 0 170.940 9.98246 2 8 0 0 172.870 10.5735 2 -8 0 0 177.343 10.8188 2 -8 0 0 167.847 9.94663 2 -9 0 0 1.03348 1.92443 2 -9 0 0 0.33298 2.39265 2 9 0 0 -0.8373 1.72986 2 10 0 0 129.541 9.25668 2 10 0 0 132.880 8.77978 2 -10 0 0 139.748 9.84593 2 -10 0 0 125.433 8.75894 2 11 0 0 5.95959 2.75981 2 -11 0 0 4.15308 3.60440 2 11 0 0 3.04570 2.75304 2 -12 0 0 52.8884 6.93127 2 12 0 0 51.9912 5.96817 2 13 0 0 3.53392 2.94938 2 -13 0 0 9.55173 4.11386 2 -14 0 0 31.5772 6.28815 2 -15 0 0 7.48776 4.63373 2 15 0 0 6.44258 3.56092 2 -16 0 0 153.368 13.4079 2 16 0 0 153.248 11.9576 2 17 0 0 0.00872 3.85374 2 -17 0 0 2.60004 5.10658 2 19 0 0 2.17067 4.41500 2 -19 0 0 5.84634 5.56959 2 -20 0 0 11.6820 6.20504 2 20 0 0 5.20699 4.60382 2 -21 0 0 3.12296 5.90214 2 21 0 0 0.24494 4.37056 2 -22 0 0 15.7313 7.11392 2 22 0 0 17.9840 6.27194 2 23 0 0 3.82359 4.19333 2 -23 0 0 0.41542 5.37171 2 -24 0 0 20.2827 8.15975 2 24 0 0 20.8495 9.47933 2 0 -1 0 1.13520 0.99690 4 0 -1 0 1.75028 1.20991 5 0 -1 0 2.48412 1.06648 3 0 1 0 1.15901 1.16151 4 1 -1 0 471.172 18.9850 3 -1 -1 0 440.181 18.4327 4 1 -1 0 490.536 18.3218 6 -1 -1 0 442.959 19.6081 5 1 1 0 440.210 18.5040 4 1 1 0 440.117 19.0769 5 -1 1 0 486.993 19.0331 3 -2 -1 0 2797.78 116.076 1 2 1 0 2807.55 116.603 1 -2 1 0 2811.39 118.367 1 -3 -1 0 5145.97 211.599 1 3 1 0 5071.62 213.630 1 -3 1 0 5174.34 209.103 1 4 -1 0 15.1418 2.42659 2 -4 -1 0 15.5483 1.89351 2 -4 -1 0 11.8007 3.83172 2 4 -1 0 15.6053 2.66215 2 4 -1 0 12.3779 2.66749 3 4 1 0 16.3811 2.07534 2 -4 1 0 14.4389 2.47053 3 -4 1 0 13.6094 2.24036 6 -4 1 0 14.6773 2.18434 2 5 -1 0 13.3595 2.89572 2 -5 -1 0 15.5292 2.16483 2 -5 -1 0 13.7864 2.95192 2 5 -1 0 14.0972 2.70139 2 5 -1 0 14.0887 2.94013 3 -5 1 0 13.1855 2.75966 2 -5 1 0 11.9726 2.49663 6 -5 1 0 14.2127 2.46300 2 5 1 0 15.8523 1.96767 2 5 1 0 13.3155 2.39819 2 -5 1 0 12.0872 2.53878 3 6 -1 0 144.386 8.12817 2 6 -1 0 130.100 8.28972 2 -6 1 0 137.992 8.22510 2 -7 -1 0 433.015 20.3172 2 -7 -1 0 456.914 21.3457 2 7 -1 0 443.374 21.3305 2 7 -1 0 457.549 20.6741 2 -7 1 0 436.915 21.0654 3 -7 1 0 469.788 21.0336 2 -7 1 0 451.187 21.0928 6 -7 1 0 455.052 20.5405 2 7 1 0 449.563 20.6769 2 7 1 0 456.404 19.8599 2 8 -1 0 88.0499 7.20754 2 -8 -1 0 93.0548 7.36733 2 -8 -1 0 86.3560 6.43024 2 8 -1 0 92.9173 6.83329 2 -8 1 0 91.4060 7.11011 2 -8 1 0 88.6189 6.81089 3 -8 1 0 95.4177 7.08856 6 8 1 0 89.6568 6.63916 2 -8 1 0 92.7836 6.53616 2 8 1 0 94.7308 6.12784 2 9 -1 0 89.5214 6.81604 2 -9 -1 0 65.8736 6.76148 2 9 -1 0 82.0359 7.07217 2 9 1 0 74.4670 5.76317 2 -9 1 0 92.2173 7.29681 2 9 1 0 85.4050 6.62756 2 10 -1 0 358.080 18.3586 2 -10 -1 0 343.329 17.8018 2 -10 -1 0 360.890 18.8896 2 10 -1 0 332.017 18.6533 2 -10 1 0 360.512 18.4320 6 10 1 0 365.704 16.8249 2 -10 1 0 353.988 17.8382 2 -10 1 0 344.457 18.7166 2 -10 1 0 342.602 18.4384 3 11 -1 0 38.6620 5.00435 2 -11 1 0 56.8007 5.97776 6 -11 1 0 44.9840 5.06238 2 -11 1 0 54.2047 6.06501 2 11 1 0 40.3246 5.01941 2 11 1 0 37.7905 4.51672 2 12 -1 0 7.90132 3.68158 2 -12 1 0 8.76212 3.35812 6 12 1 0 9.35785 3.73148 2 -12 1 0 8.34261 3.74554 2 -13 -1 0 35.6675 6.44711 2 13 -1 0 54.5536 6.33829 2 -13 1 0 41.9592 6.57058 2 13 1 0 49.6241 5.53050 2 -14 -1 0 11.5646 5.13216 2 14 -1 0 12.5351 4.42114 2 -14 1 0 22.8624 5.82742 2 14 1 0 13.5636 4.07165 2 15 -1 0 17.0558 5.51408 2 -15 -1 0 20.0131 6.28018 2 -15 1 0 18.8075 6.15543 2 15 1 0 17.6701 4.90649 2 -16 -1 0 2.87449 4.33240 2 16 -1 0 0.89579 3.27761 2 16 1 0 -3.8682 2.41614 2 -16 1 0 -3.1463 3.55834 2 17 -1 0 -2.2086 3.07587 2 -17 -1 0 5.48740 4.54809 2 17 1 0 6.04442 3.84729 2 -17 1 0 5.28552 5.08385 2 18 -1 0 2.83285 3.93902 2 -18 -1 0 2.23162 4.99777 2 18 1 0 4.46730 3.78169 2 -18 1 0 11.4007 5.58286 2 -19 -1 0 4.32203 5.67579 2 19 -1 0 6.60779 4.78822 2 -19 1 0 0.22100 4.59933 2 19 1 0 3.30749 4.01539 2 -20 -1 0 14.2866 7.42370 2 20 -1 0 13.4092 6.09578 2 -20 1 0 0.73481 5.24183 2 20 1 0 11.3122 5.08936 2 -21 -1 0 -0.9059 5.41608 2 21 -1 0 3.46269 4.56068 2 21 1 0 4.60564 4.62911 2 -21 1 0 9.69482 6.45454 2 -22 -1 0 5.04698 5.80110 2 22 -1 0 3.18688 4.27407 2 22 1 0 -0.3097 3.94277 2 -22 1 0 0.35902 5.59231 2 23 -1 0 5.02913 4.66302 2 23 1 0 0.88771 4.64030 2 -23 1 0 3.79963 4.65408 2 -24 -1 0 7.94045 6.88005 2 24 -1 0 9.30317 4.86297 2 24 1 0 7.62433 4.50321 2 -24 1 0 7.77937 10.3681 2 0 -2 0 61.6414 4.46259 3 0 -2 0 67.6174 4.64286 4 0 -2 0 62.1490 4.77605 5 1 -2 0 782.633 30.2808 6 -1 -2 0 705.012 31.2530 5 -1 -2 0 708.049 30.6177 4 1 -2 0 732.702 31.4196 4 1 -2 0 810.574 31.3143 3 1 2 0 751.199 31.0289 4 1 2 0 728.345 31.5247 5 2 -2 0 2.70684 1.66600 3 -2 -2 0 -0.4522 1.13819 5 -2 -2 0 0.92471 1.04749 4 2 -2 0 1.10308 0.84503 6 -2 2 0 -0.0602 1.33323 3 2 2 0 -0.0914 1.16365 4 2 2 0 0.26784 1.49029 5 -3 -2 0 374.897 18.2236 5 -3 -2 0 385.352 16.4296 2 3 -2 0 433.395 18.7265 3 -3 -2 0 392.039 17.5290 4 3 -2 0 410.268 17.0886 2 3 -2 0 462.963 17.2940 6 -3 -2 0 394.617 16.1559 2 3 -2 0 449.743 16.8878 2 3 2 0 384.228 18.6285 5 -3 2 0 411.213 18.5147 3 3 2 0 391.984 17.8185 4 -3 2 0 429.173 17.0216 6 4 -2 0 41.6522 3.19850 2 -4 -2 0 33.0909 2.67788 4 -4 -2 0 34.9012 2.78730 2 4 -2 0 33.6003 3.22601 2 4 -2 0 28.1516 3.55838 3 -4 -2 0 31.1471 3.10472 5 -4 -2 0 34.7187 2.26795 2 4 -2 0 37.0132 3.06845 6 4 2 0 30.6657 3.43180 5 -4 2 0 36.0674 3.82708 3 -4 2 0 36.7758 2.70590 6 4 2 0 33.7427 2.98496 4 -5 -2 0 117.689 6.67837 2 5 -2 0 113.814 6.58269 2 -5 -2 0 110.892 5.72240 2 5 -2 0 116.705 7.53254 3 5 -2 0 109.935 6.46873 6 -5 -2 0 106.190 5.95595 4 5 -2 0 108.164 6.83524 2 -5 2 0 115.807 5.64551 2 5 2 0 106.252 6.81347 5 -5 2 0 110.621 5.40319 2 5 2 0 110.797 6.07664 4 -5 2 0 111.554 7.43682 3 5 2 0 111.823 4.73101 7 -5 2 0 108.997 6.00164 6 -6 -2 0 177.706 9.23454 2 -6 -2 0 141.168 7.85178 2 6 2 0 176.324 9.10051 5 6 2 0 151.828 7.02151 7 6 2 0 147.699 7.97414 4 7 -2 0 14.1121 3.09605 2 -7 -2 0 13.8105 2.39370 2 7 -2 0 14.7297 3.33530 2 -7 -2 0 16.7664 3.42184 2 7 -2 0 14.0225 3.53166 3 -7 2 0 17.4300 2.86158 2 7 2 0 14.2630 1.92163 7 -7 2 0 18.1923 2.50505 2 7 2 0 14.1369 2.33723 4 7 2 0 15.4684 2.69443 5 -7 2 0 12.9501 3.75123 3 -7 2 0 14.1109 2.72193 6 8 -2 0 2.45409 1.97767 3 8 -2 0 -1.6606 3.14664 2 -8 -2 0 5.27640 2.62164 2 -8 -2 0 1.21088 1.41364 2 8 -2 0 4.10950 2.20152 2 -8 2 0 4.84413 2.49928 3 8 2 0 3.50695 1.66581 4 -8 2 0 8.95561 2.23761 2 8 2 0 0.72631 1.50296 5 -8 2 0 3.86026 2.05754 2 8 2 0 3.04446 1.42457 2 8 2 0 1.15829 1.01924 2 8 2 0 2.21962 1.32546 7 9 -2 0 44.9824 4.88420 2 -9 -2 0 40.2569 5.07786 2 -9 -2 0 34.4508 3.94156 2 9 -2 0 43.0359 5.07128 2 9 2 0 34.4772 3.72472 4 -9 2 0 47.1981 5.08445 3 9 2 0 30.6108 3.42329 7 9 2 0 38.5030 4.21366 5 -9 2 0 50.6273 4.88431 2 9 2 0 37.3886 3.70232 2 9 2 0 35.4149 3.14084 2 -10 -2 0 107.396 7.76389 2 -10 -2 0 99.1311 8.78281 2 10 -2 0 117.635 8.68853 2 -10 2 0 118.175 7.96205 6 -10 2 0 111.996 10.5984 2 -10 2 0 113.917 8.31552 2 10 2 0 118.258 6.76978 2 10 2 0 118.226 7.30270 4 10 2 0 102.760 7.00703 7 10 2 0 107.036 7.26664 2 10 2 0 117.183 7.76659 5 11 -2 0 21.6548 4.28272 2 11 2 0 16.3572 3.00510 7 11 2 0 11.1837 3.20562 5 11 2 0 9.00400 2.77812 4 11 2 0 11.1378 2.49564 2 11 2 0 8.35769 2.90153 2 12 -2 0 3.44799 3.15615 2 -12 -2 0 3.10931 3.41700 2 -12 2 0 1.51932 2.42529 6 12 2 0 -0.4535 1.85289 4 12 2 0 1.77216 1.85991 2 -12 2 0 4.85178 4.97684 2 -12 2 0 2.56006 2.84222 2 12 2 0 0.73309 1.79022 7 12 2 0 -0.5516 3.35228 2 -13 -2 0 30.7535 6.78947 2 13 -2 0 27.4903 5.40752 2 13 2 0 23.2156 4.74870 4 13 2 0 23.3550 4.04001 7 -13 2 0 36.1061 5.64044 2 13 2 0 26.4903 4.60699 2 13 2 0 27.3189 3.93029 2 -14 -2 0 20.7982 5.99080 2 14 -2 0 25.1044 5.68071 2 14 2 0 15.0414 3.89207 4 14 2 0 19.6605 4.33240 7 -14 2 0 24.5926 5.90483 2 14 2 0 21.1191 5.39027 2 15 -2 0 -0.3062 3.20527 2 -15 -2 0 4.06776 4.57554 2 15 2 0 3.09997 3.12219 4 15 2 0 7.27694 3.10828 7 15 2 0 2.90448 2.59017 2 -15 2 0 2.79742 3.56431 2 -16 -2 0 2.61996 4.32990 2 16 -2 0 1.84484 3.70894 2 16 2 0 1.25535 2.60443 2 -16 2 0 1.45661 3.59175 2 16 2 0 2.87488 3.20819 4 -17 -2 0 -0.0723 4.44345 2 17 2 0 -1.2529 2.94431 4 -17 2 0 2.30980 4.09357 2 17 2 0 1.57354 2.83458 2 -18 -2 0 13.2673 6.70569 2 18 -2 0 14.2124 5.25723 2 18 2 0 12.7625 4.59157 4 18 2 0 13.9087 4.23922 2 -18 2 0 12.7120 5.26640 2 19 -2 0 3.15953 4.12020 2 -19 -2 0 1.94058 4.91278 2 19 2 0 1.16655 3.37855 4 19 2 0 0.58331 2.83695 2 20 -2 0 -2.6088 3.90938 2 -20 -2 0 6.67299 5.66597 2 -20 2 0 1.38476 4.59856 2 20 2 0 0.00517 2.95514 2 20 2 0 -2.7778 3.27155 4 -21 -2 0 -1.2797 5.54854 2 21 -2 0 2.53559 4.51021 2 -21 2 0 5.31454 5.14201 2 21 2 0 -1.1533 3.72608 4 -22 -2 0 32.2252 9.48734 2 22 -2 0 37.5859 7.59178 2 22 2 0 27.7359 5.90449 4 -22 2 0 29.3999 7.99795 2 22 2 0 26.7324 5.44582 2 23 -2 0 21.4996 6.75058 2 -23 -2 0 21.4965 8.68707 2 -23 2 0 22.0973 7.32876 2 23 2 0 22.0917 6.14271 4 23 2 0 25.4319 5.44524 2 0 -3 0 3.55947 2.43913 5 0 -3 0 3.34070 2.00231 4 0 -3 0 3.07826 2.06074 3 1 -3 0 230.310 11.8684 4 1 -3 0 221.464 11.7945 3 -1 -3 0 225.173 11.6707 3 -1 -3 0 216.244 11.3185 4 1 -3 0 220.141 10.6705 6 -1 -3 0 208.460 12.1311 5 -2 -3 0 611.068 28.4653 5 2 -3 0 614.043 27.0183 3 -2 -3 0 584.466 26.0144 4 2 -3 0 649.372 25.4900 6 2 -3 0 658.820 27.6979 4 2 3 0 567.903 26.5556 4 2 3 0 575.286 27.4714 5 3 -3 0 19.5250 2.60825 6 -3 -3 0 18.5416 1.44110 7 3 -3 0 20.3238 1.70184 2 -3 -3 0 17.3869 2.44565 4 3 -3 0 24.7386 3.67038 3 3 -3 0 19.1310 1.91039 2 -3 3 0 16.5783 3.15054 3 3 3 0 18.1902 3.52960 5 3 3 0 19.0805 3.05734 4 -4 -3 0 1.57114 0.64654 2 -4 -3 0 1.82618 1.26534 4 -4 -3 0 1.66509 0.89532 2 4 -3 0 0.24556 1.90800 3 4 -3 0 2.22930 1.44189 2 4 -3 0 0.59536 1.18987 2 -4 -3 0 3.33472 1.80706 5 4 3 0 1.50595 1.66284 4 4 3 0 2.77439 2.50308 5 -4 3 0 1.93098 1.91265 3 5 -3 0 49.7129 4.20832 2 5 -3 0 48.2295 3.85258 2 -5 -3 0 53.8779 3.84495 4 -5 -3 0 54.1366 4.61189 5 5 -3 0 47.6044 3.95232 6 5 -3 0 45.7280 5.03795 3 -5 -3 0 51.6966 3.08854 2 -5 3 0 53.0264 5.06512 3 -5 3 0 50.5587 3.54562 6 5 3 0 61.2940 5.43067 5 5 3 0 56.8373 4.47721 4 -6 -3 0 32.4532 3.08921 4 -6 -3 0 32.7790 3.61011 5 6 -3 0 25.4611 4.20057 3 6 -3 0 31.7624 3.39295 6 -6 -3 0 39.4955 3.70189 2 6 -3 0 30.6233 3.45231 2 -6 -3 0 33.4248 2.70253 2 6 -3 0 26.1386 3.51697 2 6 3 0 44.1499 4.82973 5 6 3 0 39.1094 3.73844 4 -6 3 0 29.0843 2.76098 6 -6 3 0 28.9924 4.04274 3 7 -3 0 12.1207 3.10538 2 7 -3 0 16.9804 3.71571 3 7 -3 0 15.8669 3.62217 2 -7 -3 0 15.1027 2.14667 2 -7 -3 0 12.0128 2.18531 4 -7 -3 0 19.4829 3.29558 2 7 3 0 12.5954 2.79727 4 -7 3 0 13.0570 2.21769 6 7 3 0 20.9675 3.56468 5 -7 3 0 19.3812 4.43486 3 8 -3 0 0.92069 2.00610 2 8 -3 0 2.91871 2.52413 3 8 -3 0 0.87250 2.16427 2 -8 -3 0 0.12038 1.36613 2 -8 -3 0 4.15570 2.48080 2 8 3 0 3.21640 1.82044 4 -8 3 0 2.25669 1.36452 2 -8 3 0 -0.0918 1.19052 6 -8 3 0 1.02048 0.95451 2 8 3 0 -0.2731 2.42514 5 9 -3 0 11.6490 3.69595 3 -9 -3 0 14.2408 2.65448 2 -9 -3 0 19.5818 4.03586 2 9 -3 0 10.4203 3.21202 2 9 -3 0 19.0336 3.77522 2 9 3 0 6.99760 3.18289 5 9 3 0 14.9536 2.80725 4 -9 3 0 17.1346 2.45876 2 10 -3 0 13.1667 5.44049 2 -10 -3 0 7.14668 2.55093 2 10 -3 0 14.2044 4.22970 3 -10 -3 0 8.79735 3.62079 2 10 3 0 10.0280 3.52223 5 -10 3 0 17.6519 3.15612 6 -10 3 0 16.1186 2.64745 2 -10 3 0 14.3727 2.78803 2 10 3 0 9.77200 2.74149 4 11 -3 0 39.3024 5.53671 2 11 -3 0 40.1739 5.90889 3 -11 -3 0 42.9858 9.46604 2 11 3 0 43.0429 2.55369 2 11 3 0 41.9288 2.70846 2 -11 3 0 39.1622 4.62229 6 -11 3 0 41.3773 4.50787 2 11 3 0 39.1582 5.29063 5 11 3 0 36.1105 3.26137 7 -11 3 0 36.5989 4.12530 2 11 3 0 36.1976 4.31917 4 12 -3 0 64.8617 7.29312 2 -12 -3 0 60.8127 7.65256 2 -12 3 0 72.3467 6.55007 6 -12 3 0 69.3505 6.04829 2 12 3 0 58.3050 4.80747 2 12 3 0 56.1662 5.63695 4 12 3 0 62.6033 4.13654 2 12 3 0 57.6203 6.83088 5 12 3 0 61.0915 4.55479 7 -13 -3 0 8.31177 4.74603 2 13 -3 0 11.3765 4.49571 2 -13 3 0 11.9155 3.18777 2 -13 3 0 14.3996 3.78436 2 13 3 0 7.40931 2.25807 2 13 3 0 11.3043 2.18950 2 13 3 0 9.94026 2.46671 7 13 3 0 14.7811 4.30901 5 -13 3 0 11.7102 3.51201 6 -14 -3 0 2.76215 4.31422 2 14 -3 0 4.79793 3.70718 2 14 3 0 1.80413 1.65112 2 14 3 0 8.32091 3.78044 5 14 3 0 4.19824 2.17395 7 -14 3 0 0.37792 3.64670 2 -14 3 0 -0.2312 2.35173 6 14 3 0 4.73654 2.05240 2 14 3 0 2.24658 2.52900 4 -15 -3 0 4.13324 4.51988 2 15 -3 0 2.96467 4.21365 2 -15 3 0 6.37418 3.53472 2 15 3 0 6.80513 2.62436 2 15 3 0 2.90323 3.06713 4 15 3 0 4.64313 2.59199 7 15 3 0 6.69063 2.18339 2 15 3 0 4.81309 3.54373 5 16 -3 0 26.3341 8.63360 2 -16 -3 0 34.9036 7.85465 2 16 3 0 34.0422 7.52390 7 -16 3 0 32.2263 6.30989 2 16 3 0 22.5490 6.14454 5 16 3 0 33.7980 4.09676 2 16 3 0 33.6334 5.31534 4 -17 -3 0 3.39058 6.26956 2 17 -3 0 -1.4102 4.05081 2 17 3 0 5.60671 2.68637 2 17 3 0 6.08737 3.65267 4 17 3 0 2.97324 3.13035 2 -17 3 0 4.82125 4.02081 2 17 3 0 -1.6058 3.17999 5 17 3 0 4.63216 3.41832 7 -18 -3 0 62.8326 10.4298 2 18 -3 0 61.4945 9.52553 2 18 3 0 55.0683 7.27871 2 -18 3 0 54.1370 8.02751 2 18 3 0 54.0067 7.20030 4 18 3 0 55.9044 8.42000 5 19 -3 0 -3.3014 3.72671 2 -19 -3 0 1.27756 5.37898 2 19 3 0 1.11824 2.62285 2 19 3 0 0.39094 3.69699 4 -19 3 0 -1.2990 3.88294 2 19 3 0 0.01677 4.17488 5 -20 -3 0 15.1875 7.40020 2 20 -3 0 8.26740 5.43056 2 -20 3 0 -0.5946 4.60433 2 20 3 0 2.02761 4.83919 5 20 3 0 5.84353 2.97283 2 -21 -3 0 -2.9083 4.69103 2 21 -3 0 2.57444 4.53593 2 -21 3 0 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6 5 -4 0 25.2726 2.99043 2 5 -4 0 26.3803 4.59968 3 5 4 0 28.5961 4.12055 4 5 4 0 33.2987 5.06414 5 6 -4 0 218.826 10.6075 6 6 -4 0 203.190 12.9002 3 6 -4 0 232.091 11.0094 2 -6 -4 0 202.271 9.54020 2 6 -4 0 207.139 11.3288 2 -6 -4 0 196.917 10.6241 4 -6 -4 0 196.784 10.5881 2 6 4 0 196.768 12.9724 5 6 4 0 197.167 11.7411 4 7 -4 0 19.0786 3.45163 2 -7 -4 0 18.2388 3.29499 4 7 -4 0 22.2015 3.28264 6 -7 -4 0 24.0876 2.65915 2 7 -4 0 23.4295 4.63428 3 -7 -4 0 24.9365 3.70873 2 7 4 0 28.4670 4.95931 5 7 4 0 24.7188 3.93038 4 -8 -4 0 108.778 8.15004 2 -8 -4 0 102.538 7.95881 4 -8 -4 0 106.086 6.78396 2 8 -4 0 116.546 8.12678 2 8 -4 0 115.302 9.51609 3 8 -4 0 108.765 8.47891 2 8 4 0 114.224 9.34943 5 8 4 0 119.227 8.05593 4 9 -4 0 483.591 25.5406 3 9 -4 0 518.043 24.0512 2 -9 -4 0 507.278 24.4195 2 -9 -4 0 467.127 22.4463 2 9 4 0 492.209 23.3066 4 -9 4 0 501.095 21.6539 6 9 4 0 474.107 25.1681 5 10 -4 0 7.72475 3.57202 2 10 -4 0 6.76546 3.85709 3 -10 -4 0 7.91976 3.73472 2 10 4 0 3.79862 2.78595 4 10 4 0 8.69983 4.13012 5 -10 4 0 8.14067 2.30305 6 11 -4 0 17.4765 4.99236 2 11 -4 0 17.1978 5.00085 3 -11 -4 0 15.0139 5.15581 2 11 4 0 13.2909 4.62124 5 -11 4 0 21.9811 3.25999 6 11 4 0 15.0252 3.94235 4 12 -4 0 141.301 11.2146 2 -12 -4 0 140.389 12.0059 2 12 -4 0 136.325 12.0706 3 12 4 0 132.202 13.7114 4 12 4 0 132.474 11.3731 5 -12 4 0 150.154 8.75229 6 -13 -4 0 142.193 12.1655 2 13 -4 0 125.277 10.9287 2 13 4 0 145.870 11.6717 5 -13 4 0 128.721 11.3630 6 -13 4 0 123.763 7.30159 2 13 4 0 131.217 9.47065 4 -14 -4 0 21.5657 6.62366 2 14 -4 0 15.6051 5.22431 2 -14 4 0 11.2012 3.31399 6 -14 4 0 17.7859 2.82718 2 14 4 0 11.2238 4.71338 5 14 4 0 14.7980 4.31010 4 -15 -4 0 63.7087 9.09872 2 15 -4 0 58.3626 8.47508 2 -15 4 0 58.4839 5.10496 2 -15 4 0 55.9725 5.24612 2 15 4 0 58.5999 7.85049 5 15 4 0 65.7706 6.60930 4 -15 4 0 54.9871 6.74269 6 16 -4 0 28.9603 6.88012 2 -16 -4 0 34.2581 9.54739 2 -16 4 0 23.9155 6.75695 2 -16 4 0 27.6263 4.21607 2 16 4 0 24.1712 5.48682 4 16 4 0 24.3812 6.60746 5 17 -4 0 27.9395 7.36081 2 -17 -4 0 32.5065 8.65548 2 -17 4 0 29.8159 6.12759 2 17 4 0 30.3961 5.77446 4 17 4 0 26.0058 6.96589 5 -18 -4 0 38.9284 8.81103 2 18 -4 0 34.8427 7.26856 2 18 4 0 41.3873 7.81737 5 18 4 0 34.0246 6.36234 4 19 -4 0 3.26343 4.28890 2 -19 -4 0 9.01249 5.83465 2 -19 4 0 0.87261 2.94489 2 19 4 0 4.82625 4.39179 5 19 4 0 5.44519 3.90496 4 20 -4 0 6.51354 6.39293 2 -20 -4 0 12.4227 5.85175 2 20 4 0 11.7592 6.69564 5 -20 4 0 7.26771 4.83040 2 20 4 0 7.89408 5.99136 4 21 -4 0 14.0784 4.69795 2 21 4 0 10.0700 6.56972 4 21 4 0 6.54084 7.02029 5 -21 4 0 12.6446 5.88543 2 0 -5 0 -1.0781 1.67243 6 0 -5 0 2.07954 2.87134 3 1 -5 0 8.31130 2.49212 6 -1 -5 0 3.86082 3.42182 3 1 -5 0 6.39283 3.53991 3 -1 -5 0 3.79519 2.09666 7 -2 -5 0 22.4557 4.58687 4 2 -5 0 25.4462 3.57715 6 -2 -5 0 25.1722 5.03840 3 2 -5 0 27.4632 5.31533 3 2 -5 0 28.3106 1.87335 2 -2 -5 0 23.3244 3.01931 7 -3 -5 0 12.0359 1.93507 7 3 -5 0 8.40129 2.51446 6 -3 -5 0 8.45253 2.78401 4 3 -5 0 13.4416 4.11959 3 -3 -5 0 8.73233 1.49104 7 3 -5 0 9.12587 2.14593 2 -3 -5 0 10.0587 3.83430 3 -4 -5 0 8.00901 1.61737 2 4 -5 0 8.14212 2.46899 6 4 -5 0 15.8769 4.41253 3 -4 -5 0 10.1567 1.93754 2 -4 -5 0 8.72029 2.77264 4 4 -5 0 11.3419 2.63170 2 4 -5 0 12.6995 2.22230 2 5 -5 0 9.79056 2.47565 2 5 -5 0 1.75659 3.15597 3 -5 -5 0 9.40042 1.62830 2 5 -5 0 8.47222 2.70244 2 -5 -5 0 10.9634 3.03060 4 5 -5 0 6.58653 2.23177 6 5 5 0 4.07674 3.34256 4 6 -5 0 361.732 18.5339 2 6 -5 0 400.773 16.9270 6 -6 -5 0 337.462 17.7356 4 6 -5 0 386.697 20.4789 3 6 -5 0 397.234 17.2446 2 -6 -5 0 350.203 17.3709 2 -6 -5 0 347.611 16.1118 2 6 5 0 332.554 21.4170 5 6 5 0 346.961 19.4438 4 -7 -5 0 133.725 7.75616 2 7 -5 0 152.795 8.42983 6 7 -5 0 135.890 9.73142 2 -7 -5 0 136.178 8.86086 2 7 -5 0 147.015 9.01393 2 -7 -5 0 134.215 8.89944 4 7 -5 0 134.826 11.4519 3 7 5 0 139.546 11.6471 5 7 5 0 135.798 10.2689 4 -8 -5 0 59.9843 5.53615 4 8 -5 0 65.7996 6.27570 2 -8 -5 0 67.4500 6.40179 2 8 -5 0 68.1923 8.13503 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5.37750 3.77497 2 1 2 34 1.86949 6.05899 4 1 2 34 0.47716 4.64346 7 -1 2 -34 5.79994 5.46456 6 2 0 -35 -1.3491 4.96537 6 2 0 -35 2.48838 4.42446 3 -2 0 35 -1.8034 1.94057 4 2 0 -35 -0.5067 2.56314 2 -2 0 35 -1.1587 2.32773 7 1 0 -35 1.56384 3.22596 6 -1 0 35 -0.4690 2.47893 7 1 0 -35 0.47551 2.10307 3 -1 0 35 -0.3990 2.43332 2 -1 0 35 -0.4589 2.28217 4 1 0 -35 -1.9469 2.10991 2 0 0 35 6.99886 5.60982 7 0 0 35 0.69680 5.22583 2 0 0 35 10.3374 5.78934 4 0 0 -35 9.69429 7.15310 6 0 0 -35 9.09494 5.32069 3 0 0 -35 10.7079 5.51033 2 -1 0 -35 0.97860 3.08432 6 1 0 35 -0.7955 2.57401 4 1 0 35 4.96836 3.15752 7 -1 0 -35 -1.5887 2.06476 3 -1 0 -35 3.81084 3.11065 2 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 14974 _shelx_res_file ; TITL m22168=HSY30=I : space group P21/c m22168.res created by SHELXL-2019/2 at 14:32:43 on 06-Aug-2022 CELL 0.71073 27.0910 6.2408 18.6851 90.000 90.975 90.000 ZERR 4 0.0029 0.0005 0.0021 0.000 0.003 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 144 172 4 24 TEMP -183 SIZE 0.24 0.14 0.03 REM FORM plate REM COLR colourless REM All crystals tried (about a half dozen in total) were twinned by REM pseudo-merohedry, typically with refined minor component volume REM fraction of about 0.4, as determined by the BASF parameter. A REM small number of the plate-like crystals were thick enough that REM it proved possible to cut along the twin plane, thereby separating REM the twin components. Data was collected from such a separated REM individual. The TWIN model was retained for the final model because, REM in spite of the very low occupancy fraction of 0.191%, its standard REM uncertainty, at 0.02%, is about one tenth as large. Even with such REM a tiny residual minor twin component, the refinement statistics are REM marginally better with TWIN/BASF included. REM REM The two largest difference map peaks are only about 0.5 and 0.4 REM electrons per cubic angstrom and are in positions that suggest a REM third, much lower occupancy, disorder component. This was not REM modelled due to the necessarily very low occupancy that it would REM require. TWIN -1 0 0 0 -1 0 0 0 1 L.S. 10 BOND $H ACTA LIST 4 CONF REM Specific hydrogen-bonds: HTAB N1 O4 HTAB N1' O4 EQIV $1 x, y-1, z HTAB C7 O2_$1 EQIV $2 x, -y+5/2, z+1/2 HTAB C8 O6_$2 HTAB C34 O5_$1 EQIV $3 x, y+1, z HTAB C35 O3_$3 HTAB O5 O3_$3 REM C-H...pi close contacts - dummy atoms for Cg1, Cg2, Cg3 are at the REM end of the atom list: EQIV $4 1-x, -y, -z RTAB D2CG C31 C21_$4 C22_$4 C23_$4 C24_$4 C25_$4 C26_$4 RTAB D2CG H31 C21_$4 C22_$4 C23_$4 C24_$4 C25_$4 C26_$4 HTAB C31 Cg1_$4 EQIV $5 1-x, 1-y, -z RTAB D2CG C23 C27_$5 C28_$5 C29_$5 C30_$5 C31_$5 C32_$5 RTAB D2CG H23 C27_$5 C28_$5 C29_$5 C30_$5 C31_$5 C32_$5 HTAB C23 Cg2_$5 EQIV $6 1-x, -1/2+y, -1/2-z RTAB D2CG C25 C21_$6 C22_$6 C23_$6 C24_$6 C25_$6 C26_$6 RTAB D2CG H25 C21_$6 C22_$6 C23_$6 C24_$6 C25_$6 C26_$6 HTAB C25 Cg3_$6 REM Excluded 'hydrogen bond' suggestions: REM HTAB N1 O3 REM HTAB C3' O4 REM HTAB C5 O3 REM EQIV $7 x, -y+3/2, z+1/2 REM C6 O6_$7 REM HTAB C6' O6_$7 REM Generic short-form potential hydrogen bond command: HTAB REM Instructions for planes and dihedrals, torsions etc. MPLA C7 C8 C9 C10 O2 C11 C12 C13 C14 C15 C16 MPLA C33 O3 O4 MPLA C36 O5 O6 MPLA C21 C22 C23 C24 C25 C26 MPLA C27 C28 C29 C30 C31 C32 MPLA C21' C22' C23' C24' C25' C26' MPLA C27' C28' C29' C30' C31' C32' RTAB tors C10 C9 C8 C7 RTAB tors C1 O1 C4 C5 RTAB tors C1' O1' C4' C5' RTAB tors C4 O1 C1 C27 RTAB tors C4' O1' C1' C27' REM Numbers to be quoted in manuscript: REM Disorder occupancies are 0.729(4) and 0.271(4) REM Distance N1...O4 = 2.697(11) \%A REM RMS deviation from mean plane of (C7-C16) = 0.0814 \%A REM Largest deviation is for C7 at 0.1879(13) \%A REM Torsion for C10-C9-C8-C7 = -168.02(14)\% REM Hydrogenfumarate COO-/COOH dihedral = 23.51(14)\% REM Torsion C1-O1-C4-C5 = 177.4(3)\% major vs 85.8(11)\% minor REM Torsion C4-O1-C1-C27 = 175.6(3)\% major vs 68.67(11)\% minor REM Phenyl rings dihedral = 73.41(18)\% major, 73.3(6)\% minor REM COO- distances C33-O3, C33-O4 = 1.2638(18), 1.2503(18) \%A REM COOH distances C36-O5, C36-O6 = 1.3197(19), 1.211(2) \%A REM Strong H-bond O5-H5O...O3#3 = 2.5402(17)\%A, long O-H of 1.04(2) \%A REM Weak H-bond C35-H35...O3#O3 = 3.1450(19)\%A REM Weak H-bond C34-H34...O5##1 = 3.208(2)\%A REM Weak H-bond C8-H8B...O6#2 = 3.325(2) \%A REM Probably won't quote these explicitly, just point them out in the REM H-bonding table: REM C31-H31...CG1#4 = 3.534(6) \%A REM C23-H23...CG2#5 = 3.624(4) \%A REM C25-H25...CG3#6 = 3.532(4) \%A FMAP 2 PLAN 5 REM The standard uncertainty of the EXTI parameter is 0.00039, which makes REM the EXTI parameter a little over 4.5 sigma, therefore it is retained. WGHT 0.033300 1.537000 EXTI 0.001691 BASF 0.00186 FVAR 0.38146 0.72898 C7 1 0.208486 0.716967 -0.167515 11.00000 0.02795 0.03083 = 0.03018 0.00523 0.00253 -0.00442 AFIX 23 H7A 2 0.185362 0.615042 -0.190991 11.00000 -1.20000 H7B 2 0.208016 0.689703 -0.115336 11.00000 -1.20000 AFIX 0 C8 1 0.191169 0.943503 -0.182089 11.00000 0.03124 0.02788 = 0.02305 -0.00131 -0.00023 -0.00657 AFIX 23 H8A 2 0.190854 0.969760 -0.234348 11.00000 -1.20000 H8B 2 0.214680 1.045616 -0.159546 11.00000 -1.20000 AFIX 0 C9 1 0.140016 0.983250 -0.153372 11.00000 0.02988 0.03011 = 0.02289 0.00082 0.00067 -0.00602 AFIX 23 H9A 2 0.118220 0.862657 -0.167570 11.00000 -1.20000 H9B 2 0.141905 0.986853 -0.100427 11.00000 -1.20000 AFIX 0 C10 1 0.117518 1.190034 -0.180146 11.00000 0.03294 0.02712 = 0.02116 -0.00150 -0.00321 -0.00904 C11 1 0.067227 1.251825 -0.155881 11.00000 0.03026 0.02649 = 0.02145 0.00082 -0.00288 -0.00610 C12 1 0.044941 1.436068 -0.183293 11.00000 0.04032 0.03001 = 0.03080 0.00608 0.00156 -0.00328 AFIX 43 H12 2 0.061969 1.520883 -0.217124 11.00000 -1.20000 AFIX 0 C13 1 -0.001501 1.497312 -0.162064 11.00000 0.04036 0.03239 = 0.03134 0.00950 -0.00279 0.00378 AFIX 43 H13 2 -0.015849 1.623305 -0.181951 11.00000 -1.20000 AFIX 0 C14 1 -0.028008 1.379356 -0.112181 11.00000 0.02978 0.02952 = 0.02408 -0.00040 -0.00630 -0.00337 C15 1 -0.005375 1.195725 -0.085346 11.00000 0.03179 0.03260 = 0.03990 0.01353 0.00273 -0.00048 AFIX 43 H15 2 -0.022282 1.111001 -0.051361 11.00000 -1.20000 AFIX 0 C16 1 0.041113 1.132613 -0.106700 11.00000 0.03232 0.03097 = 0.03835 0.01116 0.00073 0.00211 AFIX 43 H16 2 0.055326 1.005624 -0.087336 11.00000 -1.20000 AFIX 0 C17 1 -0.080647 1.440770 -0.092094 11.00000 0.03066 0.02851 = 0.02956 0.00155 -0.00399 0.00168 C18 1 -0.087514 1.683186 -0.091499 11.00000 0.04636 0.03350 = 0.06593 -0.00179 0.00492 0.00495 AFIX 137 H18A 2 -0.082349 1.740047 -0.139684 11.00000 -1.50000 H18B 2 -0.063553 1.747785 -0.058064 11.00000 -1.50000 H18C 2 -0.121055 1.717576 -0.076368 11.00000 -1.50000 AFIX 0 C19 1 -0.115374 1.341870 -0.148775 11.00000 0.03070 0.05313 = 0.04048 -0.00383 -0.00762 0.00179 AFIX 137 H19A 2 -0.107029 1.397234 -0.196135 11.00000 -1.50000 H19B 2 -0.149580 1.379546 -0.138061 11.00000 -1.50000 H19C 2 -0.111696 1.185656 -0.148334 11.00000 -1.50000 AFIX 0 C20 1 -0.094526 1.354293 -0.018635 11.00000 0.03958 0.05566 = 0.03247 0.00683 0.00253 0.01252 AFIX 137 H20A 2 -0.127537 1.405422 -0.006443 11.00000 -1.50000 H20B 2 -0.070520 1.404689 0.017402 11.00000 -1.50000 H20C 2 -0.094425 1.197298 -0.019745 11.00000 -1.50000 AFIX 0 O2 4 0.139519 1.304332 -0.221886 11.00000 0.03812 0.03188 = 0.03153 0.00500 0.00382 -0.00745 REM The spherical-atom scattering factor approximation imposes an REM accuracy (note: not 'precision') limit on light-atom coordinates REM of about 0.02\%A: SADI 0.020 C6 N1 C6 N1' SADI 0.020 C3 O1 C3' O1' SADI 0.020 C2 C3 C2 C3' C4 C3 C4 C3' SAME 0.020 N1' > C32' REM Mild flatness restraint for overlapping phenyl rings: FLAT C27 > C32 FLAT C27' > C32' REM Rigid-body restraints on Uij for disordered groups: RIGU N1 > C32 RIGU N1' > C32' REM Pairwise similarity restraints for overlapping and/or closely REM proximate disordered atoms: SIMU 0.005 N1 N1' SIMU 0.005 C1 C1' SIMU 0.005 C2 C2' SIMU 0.005 C3 C3' SIMU 0.005 C4 C4' SIMU 0.005 C5 C5' SIMU 0.005 C6 C6' SIMU 0.005 C21 C27' SIMU 0.005 C27 C21' SIMU 0.005 C28 C22' SIMU 0.005 C29 C23' SIMU 0.005 C30 C24' SIMU 0.005 C31 C25' SIMU 0.005 C32 C26' PART 1 N1 3 0.260843 0.677174 -0.195002 21.00000 0.02447 0.02508 = 0.01253 0.00048 -0.00065 -0.00171 AFIX 14 H1N 2 0.264603 0.758329 -0.237631 21.00000 -1.20000 AFIX 0 O1 4 0.367654 0.363945 -0.140954 21.00000 0.03513 0.03867 = 0.02459 0.00737 -0.00802 0.00981 C1 1 0.406925 0.405285 -0.089428 21.00000 0.03309 0.04141 = 0.02059 -0.00270 -0.00700 0.01474 AFIX 13 H1 2 0.401014 0.548461 -0.067124 21.00000 -1.20000 AFIX 0 C2 1 0.299021 0.753520 -0.141422 21.00000 0.03989 0.02560 = 0.02396 0.00028 -0.01056 -0.00391 AFIX 23 H2A 2 0.297565 0.664873 -0.097570 21.00000 -1.20000 H2B 2 0.292141 0.904014 -0.128130 21.00000 -1.20000 AFIX 0 C3 1 0.349955 0.737613 -0.173192 21.00000 0.02799 0.02900 = 0.04353 0.01047 -0.01416 0.00066 AFIX 23 H3A 2 0.374828 0.782540 -0.136773 21.00000 -1.20000 H3B 2 0.352040 0.837638 -0.214153 21.00000 -1.20000 AFIX 0 C4 1 0.362295 0.510988 -0.198713 21.00000 0.03189 0.03531 = 0.02850 0.00981 -0.00264 0.00419 AFIX 13 H4 2 0.393500 0.514544 -0.226516 21.00000 -1.20000 AFIX 0 C5 1 0.320704 0.425983 -0.245922 21.00000 0.03298 0.03275 = 0.02042 0.00119 -0.00636 0.00655 AFIX 23 H5A 2 0.327102 0.273168 -0.256541 21.00000 -1.20000 H5B 2 0.320539 0.504963 -0.291875 21.00000 -1.20000 AFIX 0 C6 1 0.270138 0.445900 -0.212698 21.00000 0.03783 0.02087 = 0.01641 0.00183 -0.00461 -0.00121 AFIX 23 H6A 2 0.244433 0.393366 -0.246661 21.00000 -1.20000 H6B 2 0.268802 0.358040 -0.168659 21.00000 -1.20000 AFIX 0 C21 1 0.457739 0.406842 -0.122252 21.00000 0.03611 0.03538 = 0.01596 0.00316 -0.00430 0.01126 C22 1 0.492103 0.560907 -0.102503 21.00000 0.03964 0.03708 = 0.02420 0.00025 0.00194 0.00608 AFIX 43 H22 2 0.483326 0.665914 -0.068179 21.00000 -1.20000 AFIX 0 C23 1 0.538884 0.566801 -0.131207 21.00000 0.04099 0.03682 = 0.02748 -0.00521 0.00517 0.00450 AFIX 43 H23 2 0.561954 0.673858 -0.116928 21.00000 -1.20000 AFIX 0 C24 1 0.551231 0.412935 -0.181216 21.00000 0.04116 0.03696 = 0.02280 0.00094 0.00373 0.00868 AFIX 43 H24 2 0.583134 0.413880 -0.201546 21.00000 -1.20000 AFIX 0 C25 1 0.517268 0.257461 -0.201779 21.00000 0.03264 0.04082 = 0.02471 -0.00415 0.00170 0.00824 AFIX 43 H25 2 0.526049 0.152763 -0.236204 21.00000 -1.20000 AFIX 0 C26 1 0.470693 0.253669 -0.172539 21.00000 0.02973 0.03826 = 0.02377 -0.00218 -0.00125 0.00354 AFIX 43 H26 2 0.447625 0.146595 -0.186809 21.00000 -1.20000 AFIX 0 C27 1 0.400341 0.235168 -0.032988 21.00000 0.02926 0.05311 = 0.02279 0.00461 -0.00667 0.00999 C28 1 0.354382 0.219410 0.001671 21.00000 0.03178 0.09203 = 0.07042 0.05382 0.01811 0.02819 AFIX 43 H28 2 0.328738 0.316813 -0.010989 21.00000 -1.20000 AFIX 0 C29 1 0.345929 0.067816 0.052849 21.00000 0.03660 0.07887 = 0.05264 0.03726 0.01383 0.02207 AFIX 43 H29 2 0.315266 0.065145 0.076755 21.00000 -1.20000 AFIX 0 C30 1 0.382009 -0.081902 0.069901 21.00000 0.03728 0.05822 = 0.03376 0.01737 0.00231 0.01900 AFIX 43 H30 2 0.376530 -0.184382 0.106513 21.00000 -1.20000 AFIX 0 C31 1 0.425642 -0.081764 0.033798 21.00000 0.03030 0.04173 = 0.02870 0.00404 -0.00214 0.01113 AFIX 43 H31 2 0.450309 -0.185406 0.044800 21.00000 -1.20000 AFIX 0 C32 1 0.433638 0.070979 -0.019070 21.00000 0.03238 0.04239 = 0.02927 0.00070 0.00101 0.00857 AFIX 43 H32 2 0.462801 0.062460 -0.046450 21.00000 -1.20000 AFIX 0 PART 2 N1' 3 0.257421 0.700990 -0.186026 -21.00000 0.03233 0.02228 = 0.01147 0.00461 0.00385 0.00064 AFIX 13 H1N' 2 0.259455 0.772729 -0.233740 -21.00000 -1.20000 AFIX 0 O1' 4 0.368307 0.474308 -0.121274 -21.00000 0.04882 0.04014 = 0.02977 0.00647 -0.00268 0.01451 C1' 1 0.402240 0.295150 -0.123370 -21.00000 0.03368 0.04061 = 0.02805 0.00510 -0.00785 0.01097 AFIX 13 H1' 2 0.391924 0.195831 -0.162870 -21.00000 -1.20000 AFIX 0 C2' 1 0.296146 0.808193 -0.140373 -21.00000 0.03787 0.02680 = 0.02464 0.00089 -0.01263 -0.00147 AFIX 23 H2'1 2 0.298622 0.734598 -0.093513 -21.00000 -1.20000 H2'2 2 0.286471 0.958811 -0.131678 -21.00000 -1.20000 AFIX 0 C3' 1 0.346183 0.803005 -0.176310 -21.00000 0.02877 0.02613 = 0.03984 0.01305 -0.00865 0.00201 AFIX 23 H3'1 2 0.344118 0.882281 -0.222156 -21.00000 -1.20000 H3'2 2 0.371053 0.874878 -0.145181 -21.00000 -1.20000 AFIX 0 C4' 1 0.362139 0.576126 -0.190207 -21.00000 0.02889 0.03707 = 0.02621 0.01064 -0.00675 0.00153 AFIX 13 H4' 2 0.393715 0.573293 -0.217142 -21.00000 -1.20000 AFIX 0 C5' 1 0.321775 0.451618 -0.230452 -21.00000 0.03683 0.03477 = 0.02514 0.00161 -0.01055 0.01042 AFIX 23 H5'1 2 0.320513 0.501750 -0.280718 -21.00000 -1.20000 H5'2 2 0.330949 0.298078 -0.230940 -21.00000 -1.20000 AFIX 0 C6' 1 0.270957 0.472682 -0.199535 -21.00000 0.03257 0.02391 = 0.01648 0.00103 -0.00871 0.00050 AFIX 23 H6'1 2 0.246455 0.408576 -0.233113 -21.00000 -1.20000 H6'2 2 0.269747 0.391902 -0.154000 -21.00000 -1.20000 AFIX 0 C21' 1 0.394167 0.182104 -0.049566 -21.00000 0.02476 0.05253 = 0.02663 0.01546 -0.00938 0.00445 C22' 1 0.364204 0.278445 0.005017 -21.00000 0.04795 0.09339 = 0.05984 0.04719 0.01721 0.03740 AFIX 43 H22' 2 0.352840 0.422012 0.000961 -21.00000 -1.20000 AFIX 0 C23' 1 0.352702 0.151938 0.063793 -21.00000 0.04066 0.07651 = 0.05406 0.02976 0.01272 0.03006 AFIX 43 H23' 2 0.329001 0.198259 0.097343 -21.00000 -1.20000 AFIX 0 C24' 1 0.376249 -0.040370 0.072180 -21.00000 0.03025 0.06579 = 0.03609 0.01694 0.00552 0.01745 AFIX 43 H24' 2 0.366492 -0.136032 0.108873 -21.00000 -1.20000 AFIX 0 C25' 1 0.414268 -0.095836 0.027299 -21.00000 0.02241 0.04419 = 0.03227 0.00562 -0.00341 0.00529 AFIX 43 H25' 2 0.432588 -0.222590 0.037098 -21.00000 -1.20000 AFIX 0 C26' 1 0.426379 0.025999 -0.030824 -21.00000 0.03394 0.04716 = 0.02999 0.00422 -0.00319 0.00670 AFIX 43 H26' 2 0.455824 0.001951 -0.056525 -21.00000 -1.20000 AFIX 0 C27' 1 0.454154 0.368421 -0.135454 -21.00000 0.03169 0.03343 = 0.01911 0.00441 -0.00713 0.00647 C28' 1 0.473837 0.545725 -0.099813 -21.00000 0.03006 0.04674 = 0.03474 -0.00028 -0.00442 0.00341 AFIX 43 H28' 2 0.453933 0.622240 -0.067147 -21.00000 -1.20000 AFIX 0 C29' 1 0.521028 0.611676 -0.110824 -21.00000 0.02736 0.04374 = 0.04400 -0.01273 -0.00257 0.00087 AFIX 43 H29' 2 0.533659 0.733207 -0.085975 -21.00000 -1.20000 AFIX 0 C30' 1 0.550169 0.503830 -0.157376 -21.00000 0.03659 0.03899 = 0.04329 0.00310 0.00076 0.00529 AFIX 43 H30' 2 0.582673 0.556029 -0.164371 -21.00000 -1.20000 AFIX 0 C31' 1 0.535536 0.323105 -0.195181 -21.00000 0.04667 0.04186 = 0.03407 0.00196 0.00604 -0.00394 AFIX 43 H31' 2 0.556234 0.246170 -0.226675 -21.00000 -1.20000 AFIX 0 C32' 1 0.486861 0.267921 -0.181441 -21.00000 0.03909 0.03460 = 0.02556 0.00232 0.00435 0.00470 AFIX 43 H32' 2 0.474349 0.146602 -0.206531 -21.00000 -1.20000 AFIX 0 PART 0 REM Fumarate anion C33 1 0.254923 0.836659 -0.365239 11.00000 0.02611 0.01850 = 0.01730 0.00017 -0.00033 0.00329 C34 1 0.244318 0.966568 -0.430832 11.00000 0.03166 0.02145 = 0.01390 -0.00024 0.00114 -0.00148 AFIX 43 H34 2 0.244724 0.896818 -0.476010 11.00000 -1.20000 AFIX 0 C35 1 0.234442 1.172873 -0.429115 11.00000 0.02771 0.01928 = 0.01712 0.00012 -0.00246 -0.00231 AFIX 43 H35 2 0.235790 1.247094 -0.384736 11.00000 -1.20000 AFIX 0 C36 1 0.221192 1.291387 -0.495774 11.00000 0.03793 0.01857 = 0.02149 0.00233 -0.00602 -0.00137 O3 4 0.242965 0.641039 -0.367850 11.00000 0.05330 0.01439 = 0.02306 0.00278 -0.00982 -0.00017 O4 4 0.273046 0.927036 -0.311161 11.00000 0.03847 0.02314 = 0.01787 0.00091 -0.00418 -0.00372 O5 4 0.214553 1.499915 -0.489232 11.00000 0.06764 0.01556 = 0.02677 0.00097 -0.01858 0.00208 H5O 2 0.224489 1.545287 -0.437180 11.00000 -1.50000 O6 4 0.216373 1.203671 -0.553266 11.00000 0.07692 0.02333 = 0.01786 -0.00002 -0.01129 0.00101 REM Dummy 'Cg' atoms to calculate C-H...pi interactions. Here the occupancies REM the scattering factors and displacement parameters are irrelevant, so set REM to values that are obviously fake but cannot cause any harm. REM Cg1 is Cg(C21-C26) REM Cg2 is Cg(C27-C32) REM Cg3 is Cg(C21-C26) AFIX 1 CG1 2 0.504650 0.409770 -0.151920 10.00000 10.99999 CG2 2 0.390320 0.071620 0.017690 10.00000 10.99999 CG3 2 0.504650 0.409770 -0.151920 10.00000 10.99999 AFIX 0 HKLF 4 1 0 0 1 0 -1 0 1 0 0 REM m22168=HSY30=I : space group P21/c REM wR2 = 0.1137, GooF = S = 1.030, Restrained GooF = 1.019 for all data REM R1 = 0.0469 for 5164 Fo > 4sig(Fo) and 0.0731 for all 7224 data REM 578 parameters refined using 445 restraints END WGHT 0.0333 1.5370 REM Instructions for potential hydrogen bonds HTAB C7 O2_$1 HTAB C8 O6_$2 HTAB N1 O3 HTAB N1 O4 HTAB C5 O3 EQIV $7 x, -y+3/2, z+1/2 HTAB C6 O6_$7 HTAB N1' O4 HTAB C3' O4 HTAB C6' O6_$7 HTAB C34 O5_$1 HTAB C35 O3_$3 HTAB O5 O3_$3 REM Highest difference peak 0.520, deepest hole -0.189, 1-sigma level 0.039 Q1 1 0.3967 0.4269 -0.1655 11.00000 0.05 0.52 Q2 1 0.3393 0.4732 -0.1474 11.00000 0.05 0.42 Q3 1 0.3318 0.7027 -0.1367 11.00000 0.05 0.31 Q4 1 0.3894 0.3510 0.0150 11.00000 0.05 0.18 Q5 1 0.4152 0.3169 -0.0518 11.00000 0.05 0.18 ; _shelx_res_checksum 91371 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_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 _atom_site_disorder_assembly _atom_site_disorder_group C C7 0.20849(6) 0.7170(3) -0.16752(10) 0.0296(4) Uani d 1 . . H H7A 0.185362 0.615042 -0.190991 0.036 Uiso calc 1 A 1 H H7B 0.208016 0.689703 -0.115336 0.036 Uiso calc 1 A 1 C C8 0.19117(6) 0.9435(3) -0.18209(9) 0.0274(4) Uani d 1 . . H H8A 0.190854 0.969760 -0.234348 0.033 Uiso calc 1 . . H H8B 0.214680 1.045616 -0.159546 0.033 Uiso calc 1 . . C C9 0.14002(6) 0.9833(3) -0.15337(9) 0.0276(4) Uani d 1 . . H H9A 0.118220 0.862657 -0.167570 0.033 Uiso calc 1 . . H H9B 0.141905 0.986853 -0.100427 0.033 Uiso calc 1 . . C C10 0.11752(6) 1.1900(3) -0.18015(9) 0.0271(4) Uani d 1 . . C C11 0.06723(6) 1.2518(3) -0.15588(9) 0.0261(4) Uani d 1 . . C C12 0.04494(7) 1.4361(3) -0.18329(10) 0.0337(4) Uani d 1 . . H H12 0.061969 1.520883 -0.217124 0.040 Uiso calc 1 . . C C13 -0.00150(7) 1.4973(3) -0.16206(10) 0.0347(4) Uani d 1 . . H H13 -0.015849 1.623305 -0.181951 0.042 Uiso calc 1 . . C C14 -0.02801(6) 1.3794(3) -0.11218(9) 0.0279(4) Uani d 1 . . C C15 -0.00537(6) 1.1957(3) -0.08535(11) 0.0347(4) Uani d 1 . . H H15 -0.022282 1.111001 -0.051361 0.042 Uiso calc 1 . . C C16 0.04111(6) 1.1326(3) -0.10670(10) 0.0339(4) Uani d 1 . . H H16 0.055326 1.005624 -0.087336 0.041 Uiso calc 1 . . C C17 -0.08065(6) 1.4408(3) -0.09209(10) 0.0296(4) Uani d 1 . . C C18 -0.08751(8) 1.6832(3) -0.09150(13) 0.0486(5) Uani d 1 . . H H18A -0.082349 1.740047 -0.139684 0.073 Uiso calc 1 . . H H18B -0.063553 1.747785 -0.058064 0.073 Uiso calc 1 . . H H18C -0.121055 1.717576 -0.076368 0.073 Uiso calc 1 . . C C19 -0.11537(7) 1.3419(3) -0.14877(11) 0.0415(5) Uani d 1 . . H H19A -0.107029 1.397234 -0.196135 0.062 Uiso calc 1 . . H H19B -0.149580 1.379546 -0.138061 0.062 Uiso calc 1 . . H H19C -0.111696 1.185656 -0.148334 0.062 Uiso calc 1 . . C C20 -0.09453(7) 1.3543(3) -0.01864(10) 0.0426(5) Uani d 1 . . H H20A -0.127537 1.405422 -0.006443 0.064 Uiso calc 1 . . H H20B -0.070520 1.404689 0.017402 0.064 Uiso calc 1 . . H H20C -0.094425 1.197298 -0.019745 0.064 Uiso calc 1 . . O O2 0.13952(4) 1.30433(19) -0.22189(7) 0.0338(3) Uani d 1 . . N N1 0.2608(3) 0.6772(14) -0.1950(5) 0.0207(10) Uani d 0.729(4) B 1 H H1N 0.2646(3) 0.758(3) -0.2376(12) 0.025 Uiso calc 0.729(4) B 1 O O1 0.36765(7) 0.3639(4) -0.14095(11) 0.0329(5) Uani d 0.729(4) B 1 C C1 0.40693(8) 0.4053(5) -0.08943(14) 0.0318(6) Uani d 0.729(4) B 1 H H1 0.401014 0.548461 -0.067124 0.038 Uiso calc 0.729(4) B 1 C C2 0.2990(2) 0.7535(8) -0.1414(4) 0.0299(10) Uani d 0.729(4) B 1 H H2A 0.297565 0.664873 -0.097570 0.036 Uiso calc 0.729(4) B 1 H H2B 0.292141 0.904014 -0.128130 0.036 Uiso calc 0.729(4) B 1 C C3 0.34996(19) 0.7376(6) -0.1732(3) 0.0337(9) Uani d 0.729(4) B 1 H H3A 0.374828 0.782540 -0.136773 0.040 Uiso calc 0.729(4) B 1 H H3B 0.352040 0.837638 -0.214153 0.040 Uiso calc 0.729(4) B 1 C C4 0.3623(2) 0.5110(6) -0.1987(2) 0.0319(10) Uani d 0.729(4) B 1 H H4 0.393500 0.514544 -0.226516 0.038 Uiso calc 0.729(4) B 1 C C5 0.3207(2) 0.4260(11) -0.2459(3) 0.0288(9) Uani d 0.729(4) B 1 H H5A 0.327102 0.273168 -0.256541 0.035 Uiso calc 0.729(4) B 1 H H5B 0.320539 0.504963 -0.291875 0.035 Uiso calc 0.729(4) B 1 C C6 0.2701(3) 0.4459(13) -0.2127(4) 0.0251(10) Uani d 0.729(4) B 1 H H6A 0.244433 0.393366 -0.246661 0.030 Uiso calc 0.729(4) B 1 H H6B 0.268802 0.358040 -0.168659 0.030 Uiso calc 0.729(4) B 1 C C21 0.45774(19) 0.4068(10) -0.1223(3) 0.0292(10) Uani d 0.729(4) B 1 C C22 0.49210(17) 0.5609(7) -0.1025(2) 0.0336(9) Uani d 0.729(4) B 1 H H22 0.483326 0.665914 -0.068179 0.040 Uiso calc 0.729(4) B 1 C C23 0.53888(16) 0.5668(6) -0.1312(2) 0.0350(9) Uani d 0.729(4) B 1 H H23 0.561954 0.673858 -0.116928 0.042 Uiso calc 0.729(4) B 1 C C24 0.55123(14) 0.4129(7) -0.18122(19) 0.0336(9) Uani d 0.729(4) B 1 H H24 0.583134 0.413880 -0.201546 0.040 Uiso calc 0.729(4) B 1 C C25 0.51727(14) 0.2575(6) -0.20178(19) 0.0327(8) Uani d 0.729(4) B 1 H H25 0.526049 0.152763 -0.236204 0.039 Uiso calc 0.729(4) B 1 C C26 0.47069(15) 0.2537(8) -0.1725(3) 0.0306(9) Uani d 0.729(4) B 1 H H26 0.447625 0.146595 -0.186809 0.037 Uiso calc 0.729(4) B 1 C C27 0.40034(17) 0.2352(7) -0.0330(2) 0.0351(10) Uani d 0.729(4) B 1 C C28 0.3544(2) 0.2194(9) 0.0017(3) 0.0645(16) Uani d 0.729(4) B 1 H H28 0.328738 0.316813 -0.010989 0.077 Uiso calc 0.729(4) B 1 C C29 0.3459(2) 0.0678(7) 0.0528(3) 0.0559(15) Uani d 0.729(4) B 1 H H29 0.315266 0.065145 0.076755 0.067 Uiso calc 0.729(4) B 1 C C30 0.3820(3) -0.0819(13) 0.0699(5) 0.0431(11) Uani d 0.729(4) B 1 H H30 0.376530 -0.184382 0.106513 0.052 Uiso calc 0.729(4) B 1 C C31 0.4256(2) -0.0818(12) 0.0338(4) 0.0336(12) Uani d 0.729(4) B 1 H H31 0.450309 -0.185406 0.044800 0.040 Uiso calc 0.729(4) B 1 C C32 0.4336(2) 0.0710(8) -0.0191(3) 0.0347(12) Uani d 0.729(4) B 1 H H32 0.462801 0.062460 -0.046450 0.042 Uiso calc 0.729(4) B 1 N N1' 0.2574(7) 0.701(4) -0.1860(14) 0.022(2) Uani d 0.271(4) B 2 H H1N' 0.259455 0.772729 -0.233740 0.026 Uiso calc 0.271(4) B 2 O O1' 0.3683(2) 0.4743(11) -0.1213(3) 0.0396(15) Uani d 0.271(4) B 2 C C1' 0.4022(2) 0.2951(12) -0.1234(4) 0.0342(15) Uani d 0.271(4) B 2 H H1' 0.391924 0.195831 -0.162870 0.041 Uiso calc 0.271(4) B 2 C C2' 0.2961(6) 0.808(2) -0.1404(12) 0.030(2) Uani d 0.271(4) B 2 H H2'1 0.298622 0.734598 -0.093513 0.036 Uiso calc 0.271(4) B 2 H H2'2 0.286471 0.958811 -0.131678 0.036 Uiso calc 0.271(4) B 2 C C3' 0.3462(5) 0.8030(17) -0.1763(9) 0.0317(19) Uani d 0.271(4) B 2 H H3'1 0.344118 0.882281 -0.222156 0.038 Uiso calc 0.271(4) B 2 H H3'2 0.371053 0.874878 -0.145181 0.038 Uiso calc 0.271(4) B 2 C C4' 0.3621(5) 0.5761(19) -0.1902(7) 0.031(2) Uani d 0.271(4) B 2 H H4' 0.393715 0.573293 -0.217142 0.037 Uiso calc 0.271(4) B 2 C C5' 0.3218(6) 0.452(3) -0.2305(9) 0.032(2) Uani d 0.271(4) B 2 H H5'1 0.320513 0.501750 -0.280718 0.039 Uiso calc 0.271(4) B 2 H H5'2 0.330949 0.298078 -0.230940 0.039 Uiso calc 0.271(4) B 2 C C6' 0.2710(7) 0.473(4) -0.1995(12) 0.024(2) Uani d 0.271(4) B 2 H H6'1 0.246455 0.408576 -0.233113 0.029 Uiso calc 0.271(4) B 2 H H6'2 0.269747 0.391902 -0.154000 0.029 Uiso calc 0.271(4) B 2 C C21' 0.3942(5) 0.182(2) -0.0496(6) 0.035(2) Uani d 0.271(4) B 2 C C22' 0.3642(7) 0.278(3) 0.0050(9) 0.067(3) Uani d 0.271(4) B 2 H H22' 0.352840 0.422012 0.000961 0.080 Uiso calc 0.271(4) B 2 C C23' 0.3527(6) 0.152(2) 0.0638(9) 0.057(3) Uani d 0.271(4) B 2 H H23' 0.329001 0.198259 0.097343 0.068 Uiso calc 0.271(4) B 2 C C24' 0.3762(9) -0.040(4) 0.0722(14) 0.044(2) Uani d 0.271(4) B 2 H H24' 0.366492 -0.136032 0.108873 0.053 Uiso calc 0.271(4) B 2 C C25' 0.4143(6) -0.096(4) 0.0273(11) 0.033(3) Uani d 0.271(4) B 2 H H25' 0.432588 -0.222590 0.037098 0.040 Uiso calc 0.271(4) B 2 C C26' 0.4264(6) 0.026(2) -0.0308(9) 0.037(3) Uani d 0.271(4) B 2 H H26' 0.455824 0.001951 -0.056525 0.044 Uiso calc 0.271(4) B 2 C C27' 0.4542(5) 0.368(3) -0.1355(9) 0.028(2) Uani d 0.271(4) B 2 C C28' 0.4738(4) 0.546(2) -0.0998(8) 0.037(3) Uani d 0.271(4) B 2 H H28' 0.453933 0.622240 -0.067147 0.045 Uiso calc 0.271(4) B 2 C C29' 0.5210(4) 0.6117(17) -0.1108(6) 0.038(2) Uani d 0.271(4) B 2 H H29' 0.533659 0.733207 -0.085975 0.046 Uiso calc 0.271(4) B 2 C C30' 0.5502(4) 0.5038(19) -0.1574(7) 0.040(3) Uani d 0.271(4) B 2 H H30' 0.582673 0.556029 -0.164371 0.048 Uiso calc 0.271(4) B 2 C C31' 0.5355(4) 0.3231(19) -0.1952(6) 0.041(3) Uani d 0.271(4) B 2 H H31' 0.556234 0.246170 -0.226675 0.049 Uiso calc 0.271(4) B 2 C C32' 0.4869(4) 0.268(2) -0.1814(7) 0.033(3) Uani d 0.271(4) B 2 H H32' 0.474349 0.146602 -0.206531 0.040 Uiso calc 0.271(4) B 2 C C33 0.25492(5) 0.8367(2) -0.36524(8) 0.0206(3) Uani d 1 . . C C34 0.24432(6) 0.9666(2) -0.43083(8) 0.0223(3) Uani d 1 . . H H34 0.244724 0.896818 -0.476010 0.027 Uiso calc 1 . . C C35 0.23444(5) 1.1729(2) -0.42912(9) 0.0214(3) Uani d 1 . . H H35 0.235790 1.247094 -0.384736 0.026 Uiso calc 1 . . C C36 0.22119(6) 1.2914(3) -0.49577(9) 0.0261(4) Uani d 1 . . O O3 0.24297(4) 0.64104(17) -0.36785(6) 0.0304(3) Uani d 1 . . O O4 0.27305(4) 0.92704(17) -0.31116(6) 0.0265(3) Uani d 1 . . O O5 0.21455(5) 1.49991(18) -0.48923(7) 0.0369(3) Uani d 1 . . H H5O 0.2245(8) 1.545(3) -0.4372(13) 0.055 Uiso d 1 . . O O6 0.21637(5) 1.20367(19) -0.55327(7) 0.0395(3) 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 C7 0.0280(8) 0.0308(9) 0.0302(10) -0.0044(7) 0.0025(7) 0.0052(8) C8 0.0312(8) 0.0279(9) 0.0230(9) -0.0066(7) -0.0002(7) -0.0013(7) C9 0.0299(8) 0.0301(9) 0.0229(9) -0.0060(7) 0.0007(7) 0.0008(7) C10 0.0329(8) 0.0271(9) 0.0212(9) -0.0090(7) -0.0032(7) -0.0015(7) C11 0.0303(8) 0.0265(9) 0.0215(9) -0.0061(7) -0.0029(7) 0.0008(7) C12 0.0403(10) 0.0300(9) 0.0308(10) -0.0033(8) 0.0016(8) 0.0061(8) C13 0.0404(10) 0.0324(10) 0.0313(11) 0.0038(8) -0.0028(8) 0.0095(8) C14 0.0298(8) 0.0295(9) 0.0241(9) -0.0034(7) -0.0063(7) -0.0004(7) C15 0.0318(9) 0.0326(10) 0.0399(12) -0.0005(7) 0.0027(8) 0.0135(8) C16 0.0323(9) 0.0310(10) 0.0384(11) 0.0021(7) 0.0007(8) 0.0112(8) C17 0.0307(8) 0.0285(9) 0.0296(10) 0.0017(7) -0.0040(7) 0.0015(7) C18 0.0464(11) 0.0335(11) 0.0659(16) 0.0049(9) 0.0049(10) -0.0018(10) C19 0.0307(9) 0.0531(13) 0.0405(12) 0.0018(9) -0.0076(8) -0.0038(10) C20 0.0396(10) 0.0557(13) 0.0325(12) 0.0125(9) 0.0025(8) 0.0068(9) O2 0.0381(7) 0.0319(7) 0.0315(7) -0.0075(5) 0.0038(5) 0.0050(6) N1 0.0245(14) 0.025(2) 0.013(2) -0.0017(12) -0.0006(14) 0.0005(14) O1 0.0351(10) 0.0387(13) 0.0246(11) 0.0098(10) -0.0080(8) 0.0074(9) C1 0.0331(12) 0.0414(15) 0.0206(13) 0.0147(11) -0.0070(10) -0.0027(11) C2 0.0399(15) 0.026(3) 0.0240(14) -0.0039(17) -0.0106(12) 0.0003(19) C3 0.0280(14) 0.029(2) 0.0435(17) 0.0007(17) -0.0142(12) 0.010(2) C4 0.0319(13) 0.035(2) 0.0285(17) 0.0042(17) -0.0026(12) 0.0098(16) C5 0.0330(13) 0.033(2) 0.020(2) 0.0066(13) -0.0064(14) 0.0012(15) C6 0.0378(14) 0.021(2) 0.016(3) -0.0012(13) -0.0046(15) 0.0018(15) C21 0.0361(15) 0.035(2) 0.016(2) 0.0113(14) -0.0043(14) 0.0032(15) C22 0.040(3) 0.0371(18) 0.0242(16) 0.0061(19) 0.002(2) 0.0003(13) C23 0.041(2) 0.037(2) 0.027(2) 0.0045(18) 0.0052(16) -0.0052(16) C24 0.0412(17) 0.037(3) 0.023(2) 0.0087(17) 0.0037(14) 0.0009(17) C25 0.0326(19) 0.041(2) 0.0247(15) 0.0082(15) 0.0017(15) -0.0042(14) C26 0.0297(19) 0.0383(18) 0.0238(19) 0.0035(16) -0.0013(15) -0.0022(14) C27 0.0293(16) 0.053(2) 0.0228(18) 0.0100(16) -0.0067(14) 0.0046(15) C28 0.032(2) 0.092(4) 0.070(2) 0.028(2) 0.0181(18) 0.054(3) C29 0.0366(19) 0.079(3) 0.053(3) 0.022(2) 0.0138(18) 0.037(3) C30 0.037(3) 0.058(3) 0.0338(17) 0.0190(17) 0.0023(15) 0.017(2) C31 0.030(3) 0.0417(18) 0.0287(18) 0.011(2) -0.0021(19) 0.0040(15) C32 0.032(2) 0.042(2) 0.029(2) 0.0086(17) 0.0010(16) 0.0007(17) N1' 0.032(3) 0.022(4) 0.011(5) 0.001(3) 0.004(3) 0.005(3) O1' 0.049(3) 0.040(3) 0.030(3) 0.015(3) -0.003(2) 0.006(2) C1' 0.034(3) 0.041(3) 0.028(3) 0.011(2) -0.008(2) 0.005(2) C2' 0.038(3) 0.027(5) 0.025(3) -0.001(3) -0.013(3) 0.001(4) C3' 0.029(3) 0.026(4) 0.040(3) 0.002(3) -0.009(3) 0.013(4) C4' 0.029(3) 0.037(4) 0.026(3) 0.002(3) -0.007(3) 0.011(3) C5' 0.037(3) 0.035(4) 0.025(5) 0.010(3) -0.011(3) 0.002(3) C6' 0.033(3) 0.024(4) 0.016(5) 0.001(3) -0.009(3) 0.001(3) C21' 0.025(3) 0.053(4) 0.027(4) 0.004(3) -0.009(3) 0.015(3) C22' 0.048(5) 0.093(5) 0.060(4) 0.037(4) 0.017(4) 0.047(4) C23' 0.041(4) 0.077(5) 0.054(4) 0.030(4) 0.013(4) 0.030(4) C24' 0.030(4) 0.066(5) 0.036(3) 0.017(3) 0.006(3) 0.017(4) C25' 0.022(5) 0.044(4) 0.032(4) 0.005(4) -0.003(4) 0.006(3) C26' 0.034(4) 0.047(5) 0.030(4) 0.007(4) -0.003(3) 0.004(4) C27' 0.032(3) 0.033(4) 0.019(4) 0.006(3) -0.007(3) 0.004(3) C28' 0.030(5) 0.047(5) 0.035(5) 0.003(4) -0.004(4) 0.000(4) C29' 0.027(5) 0.044(5) 0.044(6) 0.001(4) -0.003(4) -0.013(4) C30' 0.037(4) 0.039(7) 0.043(8) 0.005(4) 0.001(4) 0.003(4) C31' 0.047(6) 0.042(7) 0.034(6) -0.004(4) 0.006(5) 0.002(4) C32' 0.039(6) 0.035(4) 0.026(5) 0.005(4) 0.004(4) 0.002(3) C33 0.0261(7) 0.0185(8) 0.0173(8) 0.0033(6) -0.0003(6) 0.0002(6) C34 0.0317(8) 0.0215(8) 0.0139(8) -0.0015(6) 0.0011(6) -0.0002(6) C35 0.0277(8) 0.0193(8) 0.0171(8) -0.0023(6) -0.0025(6) 0.0001(6) C36 0.0379(9) 0.0186(8) 0.0215(9) -0.0014(7) -0.0060(7) 0.0023(7) O3 0.0533(7) 0.0144(6) 0.0231(7) -0.0002(5) -0.0098(5) 0.0028(5) O4 0.0385(6) 0.0231(6) 0.0179(6) -0.0037(5) -0.0042(5) 0.0009(5) O5 0.0676(9) 0.0156(6) 0.0268(7) 0.0021(6) -0.0186(6) 0.0010(5) O6 0.0769(9) 0.0233(6) 0.0179(7) 0.0010(6) -0.0113(6) 0.0000(5) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1' C7 C8 . . 108.6(11) ? C8 C7 N1 . . 112.1(4) ? C8 C7 H7A . . 109.2 ? N1 C7 H7A . . 109.2 ? C8 C7 H7B . . 109.2 ? N1 C7 H7B . . 109.2 ? H7A C7 H7B . . 107.9 ? C7 C8 C9 . . 111.84(13) ? C7 C8 H8A . . 109.2 ? C9 C8 H8A . . 109.2 ? C7 C8 H8B . . 109.2 ? C9 C8 H8B . . 109.2 ? H8A C8 H8B . . 107.9 ? C10 C9 C8 . . 112.92(14) ? C10 C9 H9A . . 109.0 ? C8 C9 H9A . . 109.0 ? C10 C9 H9B . . 109.0 ? C8 C9 H9B . . 109.0 ? H9A C9 H9B . . 107.8 ? O2 C10 C11 . . 120.08(16) ? O2 C10 C9 . . 120.87(15) ? C11 C10 C9 . . 119.04(14) ? C16 C11 C12 . . 117.66(16) ? C16 C11 C10 . . 122.76(15) ? C12 C11 C10 . . 119.57(15) ? C13 C12 C11 . . 120.99(17) ? C13 C12 H12 . . 119.5 ? C11 C12 H12 . . 119.5 ? C12 C13 C14 . . 121.86(17) ? C12 C13 H13 . . 119.1 ? C14 C13 H13 . . 119.1 ? C15 C14 C13 . . 116.55(16) ? C15 C14 C17 . . 121.72(16) ? C13 C14 C17 . . 121.60(15) ? C16 C15 C14 . . 121.91(17) ? C16 C15 H15 . . 119.0 ? C14 C15 H15 . . 119.0 ? C15 C16 C11 . . 121.02(16) ? C15 C16 H16 . . 119.5 ? C11 C16 H16 . . 119.5 ? C18 C17 C20 . . 108.19(17) ? C18 C17 C14 . . 111.40(15) ? C20 C17 C14 . . 112.13(14) ? C18 C17 C19 . . 109.32(16) ? C20 C17 C19 . . 108.70(16) ? C14 C17 C19 . . 107.04(15) ? C17 C18 H18A . . 109.5 ? C17 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? C17 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? C17 C19 H19A . . 109.5 ? C17 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C17 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? C17 C20 H20A . . 109.5 ? C17 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? C17 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? C6 N1 C2 . . 109.6(5) ? C6 N1 C7 . . 112.8(6) ? C2 N1 C7 . . 110.8(5) ? C6 N1 H1N . . 107.8 ? C2 N1 H1N . . 107.8 ? C7 N1 H1N . . 107.8 ? C4 O1 C1 . . 117.0(3) ? O1 C1 C27 . . 104.2(2) ? O1 C1 C21 . . 113.2(3) ? C27 C1 C21 . . 114.0(3) ? O1 C1 H1 . . 108.4 ? C27 C1 H1 . . 108.4 ? C21 C1 H1 . . 108.4 ? N1 C2 C3 . . 109.8(5) ? N1 C2 H2A . . 109.7 ? C3 C2 H2A . . 109.7 ? N1 C2 H2B . . 109.7 ? C3 C2 H2B . . 109.7 ? H2A C2 H2B . . 108.2 ? C2 C3 C4 . . 112.8(3) ? C2 C3 H3A . . 109.0 ? C4 C3 H3A . . 109.0 ? C2 C3 H3B . . 109.0 ? C4 C3 H3B . . 109.0 ? H3A C3 H3B . . 107.8 ? O1 C4 C5 . . 106.3(4) ? O1 C4 C3 . . 112.3(3) ? C5 C4 C3 . . 109.9(4) ? O1 C4 H4 . . 109.4 ? C5 C4 H4 . . 109.4 ? C3 C4 H4 . . 109.4 ? C4 C5 C6 . . 113.6(4) ? C4 C5 H5A . . 108.8 ? C6 C5 H5A . . 108.8 ? C4 C5 H5B . . 108.8 ? C6 C5 H5B . . 108.8 ? H5A C5 H5B . . 107.7 ? N1 C6 C5 . . 108.9(5) ? N1 C6 H6A . . 109.9 ? C5 C6 H6A . . 109.9 ? N1 C6 H6B . . 109.9 ? C5 C6 H6B . . 109.9 ? H6A C6 H6B . . 108.3 ? C22 C21 C26 . . 118.8(4) ? C22 C21 C1 . . 120.5(4) ? C26 C21 C1 . . 120.7(4) ? C21 C22 C23 . . 122.1(4) ? C21 C22 H22 . . 119.0 ? C23 C22 H22 . . 119.0 ? C24 C23 C22 . . 118.4(3) ? C24 C23 H23 . . 120.8 ? C22 C23 H23 . . 120.8 ? C23 C24 C25 . . 120.4(4) ? C23 C24 H24 . . 119.8 ? C25 C24 H24 . . 119.8 ? C26 C25 C24 . . 120.5(4) ? C26 C25 H25 . . 119.7 ? C24 C25 H25 . . 119.7 ? C25 C26 C21 . . 119.8(4) ? C25 C26 H26 . . 120.1 ? C21 C26 H26 . . 120.1 ? C32 C27 C28 . . 115.9(5) ? C32 C27 C1 . . 124.5(4) ? C28 C27 C1 . . 118.9(4) ? C29 C28 C27 . . 121.8(5) ? C29 C28 H28 . . 119.1 ? C27 C28 H28 . . 119.1 ? C28 C29 C30 . . 120.1(5) ? C28 C29 H29 . . 119.9 ? C30 C29 H29 . . 119.9 ? C31 C30 C29 . . 119.8(6) ? C31 C30 H30 . . 120.1 ? C29 C30 H30 . . 120.1 ? C30 C31 C32 . . 119.7(6) ? C30 C31 H31 . . 120.2 ? C32 C31 H31 . . 120.2 ? C27 C32 C31 . . 122.0(5) ? C27 C32 H32 . . 119.0 ? C31 C32 H32 . . 119.0 ? C7 N1' C6' . . 110.6(17) ? C7 N1' C2' . . 119.4(16) ? C6' N1' C2' . . 110.5(13) ? C7 N1' H1N' . . 105.0 ? C6' N1' H1N' . . 105.0 ? C2' N1' H1N' . . 105.0 ? C4' O1' C1' . . 112.3(7) ? O1' C1' C27' . . 111.5(9) ? O1' C1' C21' . . 103.0(7) ? C27' C1' C21' . . 114.5(9) ? O1' C1' H1' . . 109.2 ? C27' C1' H1' . . 109.2 ? C21' C1' H1' . . 109.2 ? N1' C2' C3' . . 111.1(14) ? N1' C2' H2'1 . . 109.4 ? C3' C2' H2'1 . . 109.4 ? N1' C2' H2'2 . . 109.4 ? C3' C2' H2'2 . . 109.4 ? H2'1 C2' H2'2 . . 108.0 ? C4' C3' C2' . . 110.9(10) ? C4' C3' H3'1 . . 109.5 ? C2' C3' H3'1 . . 109.5 ? C4' C3' H3'2 . . 109.5 ? C2' C3' H3'2 . . 109.5 ? H3'1 C3' H3'2 . . 108.0 ? O1' C4' C3' . . 106.8(9) ? O1' C4' C5' . . 106.6(11) ? C3' C4' C5' . . 111.0(11) ? O1' C4' H4' . . 110.8 ? C3' C4' H4' . . 110.8 ? C5' C4' H4' . . 110.8 ? C6' C5' C4' . . 114.7(11) ? C6' C5' H5'1 . . 108.6 ? C4' C5' H5'1 . . 108.6 ? C6' C5' H5'2 . . 108.6 ? C4' C5' H5'2 . . 108.6 ? H5'1 C5' H5'2 . . 107.6 ? N1' C6' C5' . . 112.1(15) ? N1' C6' H6'1 . . 109.2 ? C5' C6' H6'1 . . 109.2 ? N1' C6' H6'2 . . 109.2 ? C5' C6' H6'2 . . 109.2 ? H6'1 C6' H6'2 . . 107.9 ? C26' C21' C22' . . 119.0(13) ? C26' C21' C1' . . 117.0(11) ? C22' C21' C1' . . 121.5(11) ? C23' C22' C21' . . 117.2(14) ? C23' C22' H22' . . 121.4 ? C21' C22' H22' . . 121.4 ? C24' C23' C22' . . 118.6(14) ? C24' C23' H23' . . 120.7 ? C22' C23' H23' . . 120.7 ? C23' C24' C25' . . 120.1(17) ? C23' C24' H24' . . 120.0 ? C25' C24' H24' . . 120.0 ? C26' C25' C24' . . 122.2(17) ? C26' C25' H25' . . 118.9 ? C24' C25' H25' . . 118.9 ? C21' C26' C25' . . 116.3(15) ? C21' C26' H26' . . 121.8 ? C25' C26' H26' . . 121.8 ? C28' C27' C32' . . 114.2(11) ? C28' C27' C1' . . 121.5(11) ? C32' C27' C1' . . 124.3(11) ? C29' C28' C27' . . 121.4(13) ? C29' C28' H28' . . 119.3 ? C27' C28' H28' . . 119.3 ? C28' C29' C30' . . 120.2(12) ? C28' C29' H29' . . 119.9 ? C30' C29' H29' . . 119.9 ? C29' C30' C31' . . 124.3(10) ? C29' C30' H30' . . 117.8 ? C31' C30' H30' . . 117.8 ? C30' C31' C32' . . 111.8(10) ? C30' C31' H31' . . 124.1 ? C32' C31' H31' . . 124.1 ? C31' C32' C27' . . 128.1(11) ? C31' C32' H32' . . 116.0 ? C27' C32' H32' . . 116.0 ? O4 C33 O3 . . 124.32(14) ? O4 C33 C34 . . 119.06(14) ? O3 C33 C34 . . 116.56(14) ? C35 C34 C33 . . 123.21(15) ? C35 C34 H34 . . 118.4 ? C33 C34 H34 . . 118.4 ? C34 C35 C36 . . 120.84(15) ? C34 C35 H35 . . 119.6 ? C36 C35 H35 . . 119.6 ? O6 C36 O5 . . 121.01(15) ? O6 C36 C35 . . 122.62(15) ? O5 C36 C35 . . 116.37(14) ? C36 O5 H5O . . 108.7(12) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C7 N1' . 1.38(2) ? C7 C8 . 1.513(2) ? C7 N1 . 1.537(8) ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C8 C9 . 1.515(2) ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? C9 C10 . 1.509(2) ? C9 H9A . 0.9900 ? C9 H9B . 0.9900 ? C10 O2 . 1.220(2) ? C10 C11 . 1.494(2) ? C11 C16 . 1.386(2) ? C11 C12 . 1.392(2) ? C12 C13 . 1.380(2) ? C12 H12 . 0.9500 ? C13 C14 . 1.396(2) ? C13 H13 . 0.9500 ? C14 C15 . 1.389(2) ? C14 C17 . 1.530(2) ? C15 C16 . 1.385(2) ? C15 H15 . 0.9500 ? C16 H16 . 0.9500 ? C17 C18 . 1.524(3) ? C17 C20 . 1.528(3) ? C17 C19 . 1.534(2) ? C18 H18A . 0.9800 ? C18 H18B . 0.9800 ? C18 H18C . 0.9800 ? C19 H19A . 0.9800 ? C19 H19B . 0.9800 ? C19 H19C . 0.9800 ? C20 H20A . 0.9800 ? C20 H20B . 0.9800 ? C20 H20C . 0.9800 ? N1 C6 . 1.503(5) ? N1 C2 . 1.505(6) ? N1 H1N . 0.95(2) ? O1 C4 . 1.422(4) ? O1 C1 . 1.446(3) ? C1 C27 . 1.509(5) ? C1 C21 . 1.517(5) ? C1 H1 . 1.0000 ? C2 C3 . 1.515(5) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C3 C4 . 1.531(4) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 C5 . 1.515(5) ? C4 H4 . 1.0000 ? C5 C6 . 1.519(5) ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C6 H6A . 0.9900 ? C6 H6B . 0.9900 ? C21 C22 . 1.384(6) ? C21 C26 . 1.390(6) ? C22 C23 . 1.385(5) ? C22 H22 . 0.9500 ? C23 C24 . 1.385(4) ? C23 H23 . 0.9500 ? C24 C25 . 1.387(5) ? C24 H24 . 0.9500 ? C25 C26 . 1.384(4) ? C25 H25 . 0.9500 ? C26 H26 . 0.9500 ? C27 C32 . 1.387(6) ? C27 C28 . 1.417(6) ? C28 C29 . 1.367(6) ? C28 H28 . 0.9500 ? C29 C30 . 1.385(6) ? C29 H29 . 0.9500 ? C30 C31 . 1.371(7) ? C30 H30 . 0.9500 ? C31 C32 . 1.392(6) ? C31 H31 . 0.9500 ? C32 H32 . 0.9500 ? N1' C6' . 1.494(14) ? N1' C2' . 1.498(14) ? N1' H1N' . 1.0000 ? O1' C4' . 1.443(11) ? O1' C1' . 1.448(9) ? C1' C27' . 1.500(13) ? C1' C21' . 1.568(12) ? C1' H1' . 1.0000 ? C2' C3' . 1.523(13) ? C2' H2'1 . 0.9900 ? C2' H2'2 . 0.9900 ? C3' C4' . 1.504(10) ? C3' H3'1 . 0.9900 ? C3' H3'2 . 0.9900 ? C4' C5' . 1.529(12) ? C4' H4' . 1.0000 ? C5' C6' . 1.508(14) ? C5' H5'1 . 0.9900 ? C5' H5'2 . 0.9900 ? C6' H6'1 . 0.9900 ? C6' H6'2 . 0.9900 ? C21' C26' . 1.350(15) ? C21' C22' . 1.445(16) ? C22' C23' . 1.392(15) ? C22' H22' . 0.9500 ? C23' C24' . 1.367(15) ? C23' H23' . 0.9500 ? C24' C25' . 1.383(16) ? C24' H24' . 0.9500 ? C25' C26' . 1.370(16) ? C25' H25' . 0.9500 ? C26' H26' . 0.9500 ? C27' C28' . 1.393(14) ? C27' C32' . 1.394(14) ? C28' C29' . 1.362(10) ? C28' H28' . 0.9500 ? C29' C30' . 1.362(11) ? C29' H29' . 0.9500 ? C30' C31' . 1.385(12) ? C30' H30' . 0.9500 ? C31' C32' . 1.391(11) ? C31' H31' . 0.9500 ? C32' H32' . 0.9500 ? C33 O4 . 1.2503(18) ? C33 O3 . 1.2638(18) ? C33 C34 . 1.493(2) ? C34 C35 . 1.316(2) ? C34 H34 . 0.9500 ? C35 C36 . 1.487(2) ? C35 H35 . 0.9500 ? C36 O6 . 1.211(2) ? C36 O5 . 1.3197(19) ? O5 H5O . 1.04(2) ? 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 _geom_hbond_publ_flag N1 H1N O4 . 0.95 1.75 2.697(11) 175 yes N1' H1N' O4 . 1.00 1.78 2.77(3) 169 yes O5 H5O O3 1_565 1.04(2) 1.50(2) 2.5402(17) 171(2) yes C7 H7A O2 1_545 0.99 2.37 3.330(2) 164 yes C8 H8B O6 4_586 0.99 2.53 3.325(2) 137 yes C34 H34 O5 1_545 0.95 2.62 3.208(2) 121 yes C35 H35 O3 1_565 0.95 2.49 3.1450(19) 127 yes C31 H31 Cg1 3_655 0.95 2.72 3.534(6) 145 yes C25 H25 Cg1 2_644 0.95 2.70 3.532(4) 146 yes C23 H23 Cg2 3_665 0.95 2.75 3.624(4) 154 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1' C7 C8 C9 . . . . -171.8(10) ? N1 C7 C8 C9 . . . . -178.7(3) ? C7 C8 C9 C10 . . . . -168.02(14) ? C8 C9 C10 O2 . . . . 1.6(2) ? C8 C9 C10 C11 . . . . -179.52(14) ? O2 C10 C11 C16 . . . . -177.72(17) ? C9 C10 C11 C16 . . . . 3.4(2) ? O2 C10 C11 C12 . . . . 2.4(2) ? C9 C10 C11 C12 . . . . -176.43(16) ? C16 C11 C12 C13 . . . . 0.0(3) ? C10 C11 C12 C13 . . . . 179.89(16) ? C11 C12 C13 C14 . . . . 0.4(3) ? C12 C13 C14 C15 . . . . -0.5(3) ? C12 C13 C14 C17 . . . . -176.41(16) ? C13 C14 C15 C16 . . . . 0.1(3) ? C17 C14 C15 C16 . . . . 176.04(17) ? C14 C15 C16 C11 . . . . 0.3(3) ? C12 C11 C16 C15 . . . . -0.4(3) ? C10 C11 C16 C15 . . . . 179.75(16) ? C15 C14 C17 C18 . . . . 148.79(18) ? C13 C14 C17 C18 . . . . -35.5(2) ? C15 C14 C17 C20 . . . . 27.4(2) ? C13 C14 C17 C20 . . . . -156.94(17) ? C15 C14 C17 C19 . . . . -91.8(2) ? C13 C14 C17 C19 . . . . 83.9(2) ? C8 C7 N1 C6 . . . . -153.5(5) ? C8 C7 N1 C2 . . . . 83.3(7) ? C4 O1 C1 C27 . . . . 175.6(3) ? C4 O1 C1 C21 . . . . -60.0(4) ? C6 N1 C2 C3 . . . . 61.7(8) ? C7 N1 C2 C3 . . . . -173.2(5) ? N1 C2 C3 C4 . . . . -56.4(7) ? C1 O1 C4 C5 . . . . 177.4(3) ? C1 O1 C4 C3 . . . . -62.3(4) ? C2 C3 C4 O1 . . . . -67.9(6) ? C2 C3 C4 C5 . . . . 50.2(6) ? O1 C4 C5 C6 . . . . 70.8(6) ? C3 C4 C5 C6 . . . . -51.0(7) ? C2 N1 C6 C5 . . . . -61.5(8) ? C7 N1 C6 C5 . . . . 174.6(6) ? C4 C5 C6 N1 . . . . 57.3(8) ? O1 C1 C21 C22 . . . . 137.7(4) ? C27 C1 C21 C22 . . . . -103.5(5) ? O1 C1 C21 C26 . . . . -42.5(6) ? C27 C1 C21 C26 . . . . 76.4(6) ? C26 C21 C22 C23 . . . . -0.1(7) ? C1 C21 C22 C23 . . . . 179.8(5) ? C21 C22 C23 C24 . . . . 0.0(6) ? C22 C23 C24 C25 . . . . 0.1(5) ? C23 C24 C25 C26 . . . . -0.1(5) ? C24 C25 C26 C21 . . . . 0.1(6) ? C22 C21 C26 C25 . . . . 0.0(7) ? C1 C21 C26 C25 . . . . -179.9(5) ? O1 C1 C27 C32 . . . . 113.8(4) ? C21 C1 C27 C32 . . . . -10.1(5) ? O1 C1 C27 C28 . . . . -56.4(4) ? C21 C1 C27 C28 . . . . 179.7(4) ? C32 C27 C28 C29 . . . . 8.4(7) ? C1 C27 C28 C29 . . . . 179.5(5) ? C27 C28 C29 C30 . . . . -2.9(9) ? C28 C29 C30 C31 . . . . -2.0(12) ? C29 C30 C31 C32 . . . . 0.9(13) ? C28 C27 C32 C31 . . . . -9.5(8) ? C1 C27 C32 C31 . . . . 180.0(5) ? C30 C31 C32 C27 . . . . 5.1(10) ? C8 C7 N1' C6' . . . . -158.4(14) ? C8 C7 N1' C2' . . . . 72(2) ? C4' O1' C1' C27' . . . . 68.7(11) ? C4' O1' C1' C21' . . . . -168.0(8) ? C7 N1' C2' C3' . . . . -170.6(18) ? C6' N1' C2' C3' . . . . 60(2) ? N1' C2' C3' C4' . . . . -59.2(19) ? C1' O1' C4' C3' . . . . -155.5(9) ? C1' O1' C4' C5' . . . . 85.8(11) ? C2' C3' C4' O1' . . . . -63.7(15) ? C2' C3' C4' C5' . . . . 52.2(16) ? O1' C4' C5' C6' . . . . 67.7(18) ? C3' C4' C5' C6' . . . . -48(2) ? C7 N1' C6' C5' . . . . 171.5(18) ? C2' N1' C6' C5' . . . . -54(2) ? C4' C5' C6' N1' . . . . 49(2) ? O1' C1' C21' C26' . . . . -170.1(11) ? C27' C1' C21' C26' . . . . -48.9(15) ? O1' C1' C21' C22' . . . . -8.3(15) ? C27' C1' C21' C22' . . . . 112.9(15) ? C26' C21' C22' C23' . . . . -29(2) ? C1' C21' C22' C23' . . . . 170.0(13) ? C21' C22' C23' C24' . . . . 10(3) ? C22' C23' C24' C25' . . . . 7(4) ? C23' C24' C25' C26' . . . . -7(4) ? C22' C21' C26' C25' . . . . 28(2) ? C1' C21' C26' C25' . . . . -169.2(14) ? C24' C25' C26' C21' . . . . -11(3) ? O1' C1' C27' C28' . . . . 43.1(15) ? C21' C1' C27' C28' . . . . -73.4(15) ? O1' C1' C27' C32' . . . . -137.7(14) ? C21' C1' C27' C32' . . . . 105.9(16) ? C32' C27' C28' C29' . . . . 0.6(15) ? C1' C27' C28' C29' . . . . 179.9(15) ? C27' C28' C29' C30' . . . . -0.1(14) ? C28' C29' C30' C31' . . . . -1.2(17) ? C29' C30' C31' C32' . . . . 1.7(17) ? C30' C31' C32' C27' . . . . -1(2) ? C28' C27' C32' C31' . . . . 0(2) ? C1' C27' C32' C31' . . . . -179.2(14) ? O4 C33 C34 C35 . . . . -27.3(2) ? O3 C33 C34 C35 . . . . 150.19(16) ? C33 C34 C35 C36 . . . . -176.29(14) ? C34 C35 C36 O6 . . . . 3.9(3) ? C34 C35 C36 O5 . . . . -176.43(15) ? _cod_database_fobs_code 2244148