#------------------------------------------------------------------------------ #$Date: 2016-03-13 15:25:55 +0200 (Sun, 13 Mar 2016) $ #$Revision: 178180 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/27/1542796.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1542796 loop_ _publ_author_name 'Dubey, Ritesh' 'Desiraju, Gautam R.' _publ_section_title ; Combinatorial selection of molecular conformations and supramolecular synthons in quercetin cocrystal landscapes: a route to ternary solids ; _journal_issue 4 _journal_name_full IUCrJ _journal_page_first 402 _journal_page_last 408 _journal_paper_doi 10.1107/S2052252515009884 _journal_volume 2 _journal_year 2015 _chemical_formula_sum 'C27 H20 N2 O7' _chemical_formula_weight 484.45 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 101.912(7) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 21.831(5) _cell_length_b 12.904(3) _cell_length_c 15.876(4) _cell_measurement_temperature 150(2) _cell_volume 4376.1(18) _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_unetI/netI 0.0606 _diffrn_reflns_laue_measured_fraction_full 0.997 _diffrn_reflns_laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 18633 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 3.041 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_crystal_colour Yellow-Red _exptl_crystal_density_diffrn 1.471 _exptl_crystal_description Plate _exptl_crystal_F_000 2016 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.274 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef 0.0006(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 5006 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0545 _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^)+(0.0666P)^2^+1.7713P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1287 _refine_ls_wR_factor_ref 0.1497 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3202 _reflns_number_total 5006 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lc5063.cif _cod_data_source_block QDP_V _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /usr/data/users/saulius/automatic-downloads/current/IUCr/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4287 2015-11-16 14:04:37Z antanas ; _cod_original_cell_volume 4376.0(17) _cod_database_code 1542796 _publcif_datablock.id {8ef442f8-28b7-40d5-a54e-858a26e8f417} _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 0.968 _shelx_estimated_absorpt_t_max 0.987 _shelxl_version_number 2013-2 _shelx_res_file ; TITL datam in C2/c CELL 0.71073 21.8314 12.9036 15.8758 90.000 101.912 90.000 ZERR 8.00 0.0049 0.0030 0.0036 0.000 0.007 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O UNIT 216 160 16 56 MERG 2 EQIV $1 -x+1/2, y+1/2, -z+1/2 HTAB O1 N1_$1 HTAB O4 O3 EQIV $2 -x, y, -z-1/2 HTAB O4 O5_$2 EQIV $3 x-1/2, -y+3/2, z-1/2 HTAB O5 O2_$3 EQIV $4 -x-1/2, -y+1/2, -z HTAB O6 N2_$4 HTAB O2 O3 HTAB C4 N1_$1 HTAB C11 O4 EQIV $5 -x+1/2, -y+1/2, -z HTAB C20 O3_$5 EQIV $6 -x, -y+1, -z HTAB C24 O4_$6 FMAP 2 PLAN 20 SIZE 0.120 0.200 0.300 ACTA HTAB 2.00000 BOND $H L.S. 10 TEMP -123.00 WGHT 0.066600 1.771300 EXTI 0.000582 FVAR 0.14982 H21 2 0.037876 0.064872 0.095017 11.00000 0.04779 H22 2 0.053091 -0.151641 0.130425 11.00000 0.04729 H1O 2 0.165439 0.532012 0.361762 11.00000 0.04901 H4O 2 0.095161 0.736101 -0.147576 11.00000 0.05277 H5O 2 -0.194043 0.767006 -0.292149 11.00000 0.08837 H6O 2 -0.271932 0.637934 -0.179964 11.00000 0.07904 H2O 2 0.225734 0.684886 0.063389 11.00000 0.09348 MOLE 1 O7 4 0.016942 0.618461 0.054733 11.00000 0.01633 0.04066 = 0.02416 0.00639 0.00377 0.00026 O4 4 0.059300 0.726760 -0.135542 11.00000 0.01664 0.06006 = 0.02764 0.01094 0.00515 -0.00042 O3 4 0.172435 0.712067 -0.027825 11.00000 0.01877 0.04509 = 0.03012 0.00411 0.00683 -0.00270 O2 4 0.239359 0.666651 0.124248 11.00000 0.01716 0.04663 = 0.02858 0.00306 0.00438 -0.00398 O6 4 -0.239272 0.673393 -0.206291 11.00000 0.01374 0.05111 = 0.03390 0.00590 0.00232 -0.00223 O1 4 0.128483 0.531770 0.329791 11.00000 0.02396 0.05595 = 0.02594 0.00938 0.00362 -0.00149 O5 4 -0.149121 0.759197 -0.274122 11.00000 0.01821 0.05173 = 0.02621 0.00788 0.00515 0.00367 C9 1 0.011341 0.657079 -0.027361 11.00000 0.02179 0.02879 = 0.02254 0.00203 0.00554 0.00093 C6 1 0.127976 0.645229 0.084878 11.00000 0.01836 0.02453 = 0.02571 -0.00107 0.00497 0.00107 C8 1 0.063573 0.687924 -0.055245 11.00000 0.02033 0.03101 = 0.02442 0.00148 0.00531 0.00191 C10 1 -0.053910 0.660144 -0.073384 11.00000 0.01670 0.02835 = 0.02449 -0.00212 0.00436 0.00124 C7 1 0.125269 0.682964 -0.000285 11.00000 0.01953 0.02694 = 0.02485 -0.00290 0.00656 0.00231 C4 1 0.186370 0.598734 0.227716 11.00000 0.01731 0.03567 = 0.02565 0.00049 0.00174 0.00051 AFIX 43 H4 2 0.224881 0.594242 0.268353 11.00000 -1.20000 AFIX 0 C11 1 -0.071483 0.706040 -0.154613 11.00000 0.01852 0.03094 = 0.02579 0.00120 0.00798 -0.00015 AFIX 43 H11 2 -0.040384 0.734928 -0.181542 11.00000 -1.20000 AFIX 0 C14 1 -0.163299 0.619619 -0.078704 11.00000 0.01939 0.03190 = 0.02816 0.00049 0.00861 -0.00173 AFIX 43 H14 2 -0.194537 0.589493 -0.052721 11.00000 -1.20000 AFIX 0 C2 1 0.073649 0.573382 0.191428 11.00000 0.01888 0.03649 = 0.02761 0.00091 0.00683 -0.00005 AFIX 43 H2 2 0.035876 0.551166 0.206621 11.00000 -1.20000 AFIX 0 C5 1 0.184765 0.636114 0.146282 11.00000 0.01867 0.02651 = 0.02664 -0.00295 0.00485 -0.00226 C15 1 -0.101030 0.617312 -0.035647 11.00000 0.02406 0.02930 = 0.02507 0.00057 0.00684 -0.00144 AFIX 43 H15 2 -0.090212 0.586511 0.019790 11.00000 -1.20000 AFIX 0 C12 1 -0.133408 0.709722 -0.195860 11.00000 0.01901 0.03035 = 0.02172 0.00124 0.00411 0.00247 C3 1 0.130201 0.567256 0.249983 11.00000 0.02637 0.02984 = 0.02585 0.00088 0.00731 0.00172 C13 1 -0.180289 0.665339 -0.159039 11.00000 0.01467 0.03109 = 0.02775 -0.00332 0.00462 0.00035 C1 1 0.073556 0.612432 0.110750 11.00000 0.01606 0.02778 = 0.02658 -0.00102 0.00207 0.00170 MOLE 2 N1 3 0.250116 0.022411 0.076180 11.00000 0.02513 0.03545 = 0.02675 -0.00089 0.00733 0.00004 N2 3 -0.158748 -0.103123 0.157545 11.00000 0.02121 0.04433 = 0.03604 0.00343 0.00748 -0.00166 C18 1 0.125055 0.005612 0.093706 11.00000 0.02225 0.03287 = 0.02577 -0.00259 0.00530 -0.00131 C20 1 0.227405 -0.065455 0.102786 11.00000 0.02636 0.03398 = 0.03557 0.00139 0.00677 0.00308 AFIX 43 H20 2 0.254741 -0.123258 0.115088 11.00000 -1.20000 AFIX 0 C21 1 0.059775 0.001523 0.104284 11.00000 0.02456 0.03622 = 0.03727 0.00163 0.00690 0.00242 C23 1 -0.034296 -0.085967 0.137393 11.00000 0.02270 0.03715 = 0.02905 -0.00010 0.00625 -0.00191 C19 1 0.166689 -0.076742 0.113314 11.00000 0.03069 0.03270 = 0.03830 0.00191 0.01145 -0.00059 AFIX 43 H19 2 0.153345 -0.140298 0.133815 11.00000 -1.20000 AFIX 0 C16 1 0.209714 0.101270 0.056838 11.00000 0.02743 0.03247 = 0.02875 0.00066 0.00741 -0.00468 AFIX 43 H16 2 0.224465 0.164103 0.036969 11.00000 -1.20000 AFIX 0 C17 1 0.148144 0.096348 0.064131 11.00000 0.02642 0.03307 = 0.02678 0.00080 0.00474 0.00244 AFIX 43 H17 2 0.121444 0.154505 0.049089 11.00000 -1.20000 AFIX 0 C22 1 0.030738 -0.081703 0.125974 11.00000 0.02629 0.03630 = 0.03747 -0.00037 0.01011 0.00048 C27 1 -0.061671 -0.181597 0.145457 11.00000 0.02887 0.03616 = 0.04497 0.00482 0.01208 0.00385 AFIX 43 H27 2 -0.038225 -0.243447 0.144472 11.00000 -1.20000 AFIX 0 C24 1 -0.071448 0.001283 0.140325 11.00000 0.03031 0.03156 = 0.04620 -0.00405 0.01153 -0.00334 AFIX 43 H24 2 -0.054995 0.068632 0.135292 11.00000 -1.20000 AFIX 0 C26 1 -0.122903 -0.186524 0.154888 11.00000 0.02926 0.03388 = 0.04974 0.00803 0.01062 -0.00337 AFIX 43 H26 2 -0.140657 -0.252911 0.159779 11.00000 -1.20000 AFIX 0 C25 1 -0.132500 -0.010867 0.150624 11.00000 0.02533 0.03968 = 0.04562 -0.00278 0.01001 0.00135 AFIX 43 H25 2 -0.156977 0.049549 0.152883 11.00000 -1.20000 AFIX 0 HKLF 4 REM datam in C2/c REM R1 = 0.0545 for 3202 Fo > 4sig(Fo) and 0.0992 for all 5006 data REM 354 parameters refined using 0 restraints END WGHT 0.0641 1.9513 REM Instructions for potential hydrogen bonds HTAB O1 N1_$1 HTAB O4 O3 HTAB O4 O5_$2 HTAB O5 O2_$3 HTAB O6 N2_$4 HTAB O2 O3 HTAB C4 N1_$1 HTAB C11 O4 HTAB C20 O3_$5 HTAB C24 O4_$6 REM Highest difference peak 0.274, deepest hole -0.323, 1-sigma level 0.058 Q1 1 0.1769 0.0931 0.0686 11.00000 0.05 0.27 Q2 1 0.0971 0.0021 0.0986 11.00000 0.05 0.24 Q3 1 -0.0025 -0.0833 0.1244 11.00000 0.05 0.24 Q4 1 0.0866 0.5638 0.3339 11.00000 0.05 0.24 Q5 1 0.2894 0.0301 0.0727 11.00000 0.05 0.23 Q6 1 0.0945 0.6834 -0.0292 11.00000 0.05 0.22 Q7 1 0.1494 0.5965 0.2201 11.00000 0.05 0.21 Q8 1 0.1582 0.5724 0.2344 11.00000 0.05 0.21 Q9 1 0.1628 -0.2429 0.1487 11.00000 0.05 0.20 Q10 1 0.1317 0.5700 0.2820 11.00000 0.05 0.19 Q11 1 -0.2303 0.7819 -0.1848 11.00000 0.05 0.19 Q12 1 0.0426 -0.1629 0.0824 11.00000 0.05 0.19 Q13 1 0.0000 0.4317 0.2500 10.50000 0.05 0.19 Q14 1 0.1345 0.0556 0.0770 11.00000 0.05 0.19 Q15 1 0.0274 0.5019 0.2879 11.00000 0.05 0.19 Q16 1 0.0253 0.6943 -0.0490 11.00000 0.05 0.19 Q17 1 0.0980 -0.0439 0.0235 11.00000 0.05 0.19 Q18 1 -0.0273 0.6451 -0.0536 11.00000 0.05 0.18 Q19 1 0.2727 0.0024 0.0300 11.00000 0.05 0.18 Q20 1 -0.0726 -0.1631 0.1890 11.00000 0.05 0.18 ; _shelx_res_checksum 41782 _shelx_hkl_file ; 0 0 3 0.46 0.38 0 0 -3 -0.16 0.25 0 0 -3 0.38 0.34 0 0 4 2909.09 31.56 0 0 -4 2909.64 27.93 0 0 5 -0.24 0.55 0 0 -5 0.25 0.46 0 0 6 12.48 1.42 0 0 -6 10.49 1.15 0 0 7 0.76 0.98 0 0 -7 -0.91 0.74 0 0 -8 8.32 1.44 0 0 -9 0.96 0.90 0 0 -9 1.19 0.69 0 0 10 262.63 8.08 0 0 -10 224.02 5.41 0 0 -10 233.42 7.13 0 0 11 1.40 1.13 0 0 -11 -0.50 0.63 0 0 12 4.89 2.15 0 0 -12 7.41 1.93 0 0 -12 3.69 1.11 0 0 13 -1.03 1.42 0 0 -13 -0.05 0.84 0 0 -13 -0.36 1.24 0 0 14 48.29 4.38 0 0 -14 53.59 4.29 0 0 15 -2.15 2.47 0 0 -15 3.04 1.92 0 0 16 2.35 2.60 0 0 -16 4.21 2.23 0 0 17 -0.23 2.95 0 0 -17 -2.67 2.41 0 0 18 0.04 2.26 0 0 -18 1.22 2.28 0 0 19 5.88 3.33 0 0 -19 0.77 2.62 0 0 20 2.69 3.82 0 0 -20 1.91 3.11 0 2 0 0.30 0.38 0 2 0 1.50 0.17 0 2 -1 112.46 2.10 0 2 -1 113.76 1.61 0 -2 -1 113.86 2.02 0 -2 2 2.37 0.26 0 2 2 4.34 0.73 0 2 -2 3.22 0.51 0 2 -2 3.53 0.70 0 -2 -2 3.08 0.61 0 -2 3 118.79 2.91 0 2 3 114.33 2.76 0 2 -3 120.84 2.67 0 -2 -3 124.32 2.89 0 2 4 556.72 9.18 0 -2 4 526.62 8.82 0 -2 -4 533.39 8.40 0 2 -4 555.99 8.50 0 -2 5 490.37 8.81 0 2 5 489.11 9.07 0 -2 -5 486.73 6.39 0 2 -5 487.25 8.39 0 2 6 311.77 6.97 0 2 -6 308.89 6.77 0 -2 -6 317.58 6.35 0 -2 -6 298.84 5.21 0 2 7 167.93 5.29 0 -2 -7 169.88 4.70 0 -2 8 3.89 1.61 0 2 8 6.38 1.54 0 2 -8 4.40 1.25 0 -2 -8 4.67 1.24 0 2 9 56.64 3.46 0 -2 9 56.73 3.39 0 -2 -9 57.00 2.69 0 2 -9 56.73 3.22 0 -2 10 10.68 2.09 0 2 10 13.32 2.26 0 2 -10 14.60 2.00 0 -2 -10 12.82 1.62 0 2 11 19.20 3.03 0 -2 11 26.53 2.68 0 -2 -11 24.31 2.26 0 -2 -11 22.30 2.12 0 2 -11 23.79 2.83 0 -2 12 66.08 4.24 0 2 -12 65.60 4.35 0 -2 -12 54.78 3.56 0 -2 13 4.33 2.34 0 2 13 2.14 2.39 0 2 -13 6.02 2.26 0 -2 -13 0.92 1.56 0 -2 14 43.00 4.50 0 -2 -14 24.12 3.04 0 2 -14 38.44 3.87 0 -2 -14 37.77 3.65 0 2 15 60.88 5.25 0 -2 15 69.35 5.98 0 -2 -15 50.79 4.26 0 2 -15 64.33 5.64 0 -2 16 2.62 2.81 0 2 16 -1.18 2.83 0 2 -16 4.21 2.32 0 -2 -16 3.71 2.03 0 -2 17 1.59 2.25 0 2 17 0.81 2.29 0 -2 -17 0.16 1.67 0 2 -17 -1.76 1.97 0 2 18 3.87 3.33 0 -2 18 6.97 3.45 0 2 -18 -0.50 2.62 0 2 19 5.65 4.18 0 -2 19 11.30 3.32 0 2 -19 -0.44 3.05 0 -2 -19 -0.37 2.77 0 2 20 -3.04 3.67 0 -4 0 471.09 7.60 0 4 0 474.29 8.20 0 -4 1 1029.23 13.28 0 4 1 1085.91 15.66 0 4 -1 1047.47 15.41 0 -4 -1 1087.39 15.37 0 4 2 410.30 7.67 0 -4 -2 415.02 7.66 0 4 -2 411.20 6.16 0 4 -2 410.95 7.68 0 4 3 42.90 1.93 0 4 -3 40.13 1.67 0 -4 -3 43.83 2.00 0 4 -3 38.82 1.97 0 4 4 2.23 0.96 0 -4 4 0.74 0.87 0 -4 -4 2.89 1.04 0 -4 5 148.06 4.73 0 4 5 159.40 4.97 0 -4 -5 141.32 4.62 0 -4 6 89.77 3.49 0 4 6 95.74 4.14 0 -4 -6 91.07 2.10 0 4 -6 82.07 3.40 0 -4 -6 86.34 3.91 0 4 7 629.42 14.20 0 -4 7 647.97 14.20 0 -4 -7 625.26 13.87 0 4 -7 630.55 13.25 0 4 8 47.31 3.01 0 -4 8 50.80 2.91 0 4 -8 44.89 2.75 0 -4 -8 41.66 1.78 0 -4 -8 49.61 2.99 0 -4 9 4.40 1.46 0 4 -9 1.33 1.43 0 -4 -9 1.83 1.54 0 4 10 43.37 3.39 0 -4 10 44.16 3.73 0 -4 -10 33.87 2.12 0 4 -10 41.25 3.11 0 -4 -10 40.55 2.90 0 -4 11 72.88 4.83 0 4 11 59.40 4.79 0 -4 -11 56.20 2.87 0 -4 -11 63.22 4.30 0 4 -11 68.16 4.15 0 -4 12 15.78 2.98 0 4 12 8.83 3.26 0 -4 -12 13.69 2.50 0 4 -12 14.85 3.09 0 -4 -12 10.67 1.79 0 -4 13 0.29 1.96 0 4 13 0.21 1.88 0 -4 -13 1.39 1.37 0 -4 14 0.55 1.99 0 -4 -14 2.14 1.71 0 4 -14 2.01 1.95 0 -4 -14 0.18 1.31 0 4 15 11.19 3.51 0 -4 15 7.70 2.77 0 4 -15 7.84 3.30 0 -4 16 10.79 3.26 0 4 16 14.24 3.73 0 -4 -16 1.78 2.77 0 4 -16 10.80 3.19 0 -4 -16 6.43 2.22 0 4 17 3.71 2.81 0 -4 17 3.54 3.03 0 4 -17 2.91 2.96 0 -4 -17 -0.67 2.01 0 -4 18 1.94 3.30 0 4 18 1.59 3.63 0 4 -18 2.44 3.03 0 -4 19 4.52 3.36 0 4 -19 1.47 3.73 0 -6 0 39.97 2.22 0 6 0 38.23 2.67 0 6 1 91.52 3.62 0 -6 1 94.23 3.43 0 -6 -1 96.52 3.93 0 6 -1 94.89 3.78 0 6 2 121.54 4.61 0 -6 -2 123.77 4.56 0 6 -2 124.11 4.40 0 6 -2 115.64 3.27 0 -6 3 134.41 3.61 0 6 3 141.51 4.90 0 6 -3 135.84 5.13 0 6 -3 135.45 3.94 0 -6 -3 138.26 5.27 0 6 4 98.94 3.95 0 -6 4 86.22 2.49 0 6 -4 89.97 3.28 0 6 -4 85.46 4.08 0 -6 -5 7.58 1.73 0 6 -5 3.58 1.11 0 -6 6 70.71 1.88 0 -6 6 80.16 4.15 0 6 -6 72.19 3.42 0 -6 -6 75.76 4.14 0 6 7 6.31 2.13 0 -6 7 4.61 1.70 0 6 -7 8.02 1.53 0 6 8 22.40 2.99 0 -6 8 19.71 2.64 0 -6 -8 14.24 2.68 0 6 -8 15.41 2.44 0 6 9 30.65 3.54 0 -6 9 26.59 3.00 0 6 -9 24.37 2.74 0 -6 -9 29.18 3.47 0 6 10 14.08 2.74 0 -6 -10 3.32 2.00 0 6 -10 2.77 2.13 0 6 11 10.74 2.87 0 -6 11 6.96 2.67 0 6 -11 7.82 2.44 0 6 12 36.18 4.29 0 -6 12 43.76 4.32 0 6 -12 38.63 3.89 0 -6 -12 34.39 3.95 0 6 13 49.17 5.74 0 -6 13 46.13 4.79 0 6 -13 50.91 5.37 0 -6 -13 45.37 4.86 0 6 14 17.35 3.78 0 -6 14 18.63 3.63 0 -6 -14 17.58 3.65 0 6 -14 18.02 4.48 0 6 15 -0.62 2.05 0 6 -15 2.45 1.72 0 -6 -15 -1.79 1.62 0 6 16 18.04 4.88 0 6 17 1.97 3.15 0 -6 17 1.29 3.02 0 6 -17 2.54 3.21 0 -6 -17 -0.60 2.46 0 6 18 7.07 4.22 0 -6 18 5.65 3.69 0 6 -18 4.19 3.60 0 8 0 2.69 0.67 0 -8 0 5.56 1.46 0 8 0 2.38 1.49 0 8 1 39.43 2.72 0 -8 1 39.49 2.59 0 8 1 33.39 1.24 0 -8 -1 38.62 2.94 0 8 -1 36.83 1.77 0 -8 2 36.09 2.36 0 8 2 34.64 3.13 0 8 -2 32.79 1.94 0 8 -2 33.97 2.84 0 -8 3 122.21 4.26 0 8 3 127.41 5.46 0 8 -3 127.69 4.19 0 8 -3 119.15 5.32 0 -8 -3 121.79 5.31 0 -8 4 20.33 1.80 0 8 4 21.86 2.77 0 8 -4 20.57 2.01 0 -8 -4 22.30 2.66 0 8 -4 20.28 2.61 0 8 5 251.58 8.62 0 -8 5 223.28 5.85 0 -8 -5 232.00 9.16 0 8 -5 246.29 9.17 0 8 -5 253.39 7.53 0 -8 6 76.20 2.84 0 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2.60 -25 7 6 -3.00 2.59 25 7 -5 1.61 2.11 25 -7 -5 -0.93 2.69 -25 -7 5 2.77 2.97 -25 7 5 0.60 3.22 25 7 -4 3.32 3.06 25 -7 -4 2.26 3.06 -25 -7 4 2.67 4.20 -25 7 4 6.76 3.46 25 7 -3 -1.78 1.71 25 -7 -3 2.96 2.19 -25 -7 3 -0.14 2.56 -25 7 3 0.42 2.28 25 7 -2 0.26 2.05 25 -7 -2 0.22 2.31 -25 -7 2 1.05 3.12 -25 7 2 -0.52 2.28 25 7 -1 0.29 2.21 25 -7 -1 -0.86 2.28 -25 -7 1 -2.17 2.93 -25 7 1 0.50 2.51 25 7 0 4.63 3.05 25 -7 0 2.78 3.37 -25 7 0 4.54 3.51 -26 0 11 1.48 2.76 26 0 -10 14.65 3.61 -26 0 10 21.39 4.89 -26 0 8 23.42 5.16 26 0 -7 4.08 2.81 26 0 -6 5.12 2.67 -26 0 6 3.05 3.34 26 0 -5 -0.87 2.28 -26 0 5 -1.50 2.85 26 0 -4 16.09 4.29 -26 0 4 20.29 5.01 26 0 -3 0.29 2.45 -26 0 3 -2.13 2.81 -26 0 2 39.91 6.54 26 0 -1 1.91 2.80 -26 0 1 0.24 3.54 26 0 0 38.95 5.07 -26 0 0 33.88 7.23 26 0 1 -0.62 1.86 -26 0 -1 1.24 2.71 -26 0 -2 46.88 7.39 26 0 3 -1.59 2.60 -26 0 -3 -0.69 3.11 -26 0 -4 20.53 6.07 26 2 -11 10.81 3.70 26 -2 -11 11.95 3.83 -26 -2 11 6.64 4.38 -26 2 11 10.03 3.74 26 2 -10 0.23 2.43 26 -2 -10 1.74 2.54 -26 -2 10 1.65 3.02 -26 2 10 -0.03 3.19 26 2 -9 -4.06 2.45 26 -2 -9 -0.86 2.71 -26 -2 9 -0.47 3.17 -26 2 9 0.82 3.30 26 2 -8 7.91 3.81 26 -2 -8 11.35 3.28 -26 2 8 10.15 3.81 26 2 -7 25.92 4.83 26 -2 -7 21.76 3.92 -26 2 7 22.57 5.09 26 2 -6 1.13 3.12 -26 2 6 7.54 3.71 26 2 -5 -1.43 2.25 26 -2 -5 0.79 2.23 -26 -2 5 4.41 2.74 -26 2 5 -0.06 3.09 26 2 -4 -1.93 2.07 26 -2 -4 -1.59 2.08 -26 -2 4 3.47 2.47 26 2 -3 7.40 3.41 26 -2 -3 10.68 3.67 -26 -2 3 4.42 4.33 -26 2 3 6.53 3.76 26 2 -2 0.42 2.14 -26 2 2 1.30 3.14 26 2 -1 1.05 2.78 26 -2 -1 4.95 2.56 -26 -2 1 -1.59 3.34 -26 2 1 0.51 3.33 26 2 0 5.22 3.40 26 -2 0 4.97 3.08 -26 -2 0 0.99 3.87 -26 2 0 6.12 3.79 26 2 1 4.80 3.17 26 -2 1 5.72 3.31 -26 -2 -1 2.29 4.15 -26 2 -1 11.95 4.35 26 2 2 13.06 3.68 26 -2 2 9.44 4.14 -26 -2 -2 12.52 5.15 -26 2 -2 14.54 5.08 26 2 3 -1.41 2.43 26 -2 3 2.94 2.67 -26 -2 -3 2.18 3.68 26 4 -10 9.99 3.10 26 -4 -10 3.84 3.35 -26 -4 10 1.77 3.76 -26 4 10 4.51 4.18 26 4 -9 2.63 2.82 26 -4 -9 2.87 2.89 -26 4 9 3.15 3.59 26 4 -8 -0.34 2.43 -26 -4 8 0.24 2.83 -26 4 8 -0.98 2.82 26 4 -7 11.32 3.27 26 -4 -7 9.34 3.34 -26 -4 7 8.39 4.79 26 -4 -6 5.96 3.04 -26 -4 6 1.58 3.67 -26 4 6 7.37 3.39 26 4 -5 -1.03 2.46 26 -4 -5 -0.11 2.15 -26 -4 5 2.27 2.95 -26 4 5 -3.14 3.02 26 4 -4 12.67 3.11 26 -4 -4 3.39 3.12 -26 -4 4 3.53 4.39 -26 4 4 5.96 3.77 26 4 -3 26.96 4.72 26 -4 -3 20.35 4.10 -26 -4 3 19.40 5.45 -26 4 3 16.69 4.78 26 4 -2 8.06 3.28 26 -4 -2 14.17 3.78 -26 -4 2 10.49 5.13 -26 4 2 14.67 4.75 26 4 -1 0.36 2.03 26 -4 -1 1.12 2.02 -26 -4 1 -1.48 2.97 -26 4 1 -2.03 2.77 26 4 0 7.95 3.45 26 -4 0 8.36 3.84 -26 -4 0 0.48 4.96 26 4 1 31.35 4.83 26 -4 1 37.08 5.74 -26 -4 -1 36.25 7.65 26 4 2 0.27 2.32 26 -4 2 0.69 2.63 -26 -4 -2 1.04 3.38 -26 4 -2 2.86 3.40 26 -6 -7 1.87 3.07 -26 -6 7 2.42 3.88 -26 6 7 6.26 3.97 26 6 -6 5.57 3.06 26 -6 -6 -1.27 2.87 -26 -6 6 -0.21 3.85 -26 6 6 5.13 3.28 26 6 -5 5.30 2.80 26 -6 -5 4.91 3.48 -26 -6 5 5.73 4.31 -26 6 5 8.09 4.34 26 6 -4 22.51 4.60 26 -6 -4 22.45 4.85 -26 -6 4 21.56 5.39 -26 6 4 26.35 5.76 26 6 -3 4.30 2.53 26 -6 -3 0.29 3.14 -26 -6 3 0.73 4.18 26 6 -2 17.12 3.96 26 -6 -2 13.58 3.65 -26 -6 2 -0.85 4.66 -26 6 2 5.78 4.08 26 6 -1 3.04 2.49 26 -6 -1 -1.95 2.73 -26 6 1 -0.18 2.95 -27 -1 10 -0.92 2.73 -27 1 10 -0.57 3.07 27 1 -9 12.68 3.92 27 -1 -9 10.30 3.74 -27 -1 9 5.08 4.35 -27 1 9 0.79 4.41 27 1 -8 -0.46 2.88 27 -1 -8 1.93 2.73 -27 -1 8 1.84 3.45 -27 1 8 2.52 3.42 27 1 -7 2.86 2.37 27 -1 -7 0.69 2.57 -27 -1 7 -0.19 3.22 -27 1 7 -1.43 3.21 27 1 -6 14.01 3.73 27 -1 -6 11.83 3.46 -27 -1 6 4.74 4.89 -27 1 6 5.86 4.89 27 -1 -5 -1.58 2.11 27 1 -5 0.40 2.25 -27 -1 5 -2.54 2.95 -27 1 5 2.65 2.47 27 1 -4 -0.09 2.51 27 -1 -4 0.96 2.69 -27 -1 4 3.24 2.85 -27 1 4 -1.76 3.33 27 -1 -3 -3.16 2.85 -27 -1 3 0.70 3.51 -27 1 3 6.33 3.05 27 1 -2 4.16 2.97 27 -1 -2 2.28 2.76 -27 -1 2 1.45 3.73 -27 1 2 2.71 3.55 27 1 -1 0.46 2.45 27 -1 -1 1.48 2.27 -27 1 1 0.65 2.91 -27 -1 1 -2.20 2.87 27 -1 0 8.94 3.73 -27 -1 0 1.20 4.38 -27 1 0 8.98 4.38 27 -1 1 0.11 2.50 -27 -1 -1 3.30 3.32 -27 1 -1 -1.43 2.53 -27 3 9 3.91 3.95 27 3 -8 2.47 2.76 27 -3 -8 -2.60 2.73 -27 3 8 4.19 3.39 27 3 -7 1.36 2.83 27 -3 -7 1.92 2.61 -27 3 7 -0.50 2.94 27 3 -6 23.65 4.27 27 -3 -6 25.22 4.80 -27 3 6 14.19 5.24 27 3 -5 0.53 2.38 27 -3 -5 1.06 2.39 -27 -3 5 -2.48 2.75 -27 3 5 1.90 3.04 27 -3 -4 1.70 2.79 -27 -3 4 1.10 3.23 -27 3 4 -0.25 3.05 27 3 -3 20.02 4.68 27 -3 -3 23.31 4.40 -27 3 3 20.81 5.35 27 3 -2 13.53 3.49 27 -3 -2 6.08 4.05 -27 -3 2 10.24 5.09 -27 3 2 12.86 5.12 27 3 -1 0.08 2.29 27 -3 -1 -2.33 2.29 -27 -3 1 1.27 3.47 -27 3 1 -0.01 3.22 27 3 0 31.01 5.30 27 -3 0 31.45 5.27 -27 -3 0 36.90 7.59 -27 3 0 25.98 6.42 -27 -5 5 3.39 2.86 -27 5 5 -2.81 3.34 -27 -5 4 -1.59 3.36 -27 5 4 2.07 2.71 -27 -5 3 12.76 5.14 -27 5 3 13.45 4.54 28 0 -7 -1.00 2.99 28 0 -6 0.52 2.31 28 0 -5 0.29 1.88 -28 0 5 -0.72 2.74 28 0 -4 3.00 3.48 -28 0 4 2.58 3.61 28 0 -3 0.64 2.74 -28 0 3 4.41 4.05 28 0 -2 9.77 4.05 -28 0 2 4.55 4.87 28 2 -6 12.95 4.60 28 -2 -6 10.91 3.87 -28 -2 6 5.65 5.24 -28 2 6 17.60 4.60 28 2 -5 11.66 4.10 28 -2 -5 6.92 4.54 -28 -2 5 8.80 4.70 -28 2 5 30.13 5.01 28 -2 -4 23.38 5.32 -28 -2 4 23.14 5.94 -28 2 4 25.97 6.55 28 -2 -3 6.35 3.45 -28 2 3 4.73 4.12 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 70907 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 H21 H 0.0379(13) 0.065(2) 0.0950(17) 0.048(8) Uiso 1 1 d . . H22 H 0.0531(13) -0.152(2) 0.1304(17) 0.047(8) Uiso 1 1 d . . H1O H 0.1654(14) 0.532(2) 0.3618(18) 0.049(9) Uiso 1 1 d . . H4O H 0.0952(14) 0.736(2) -0.1476(19) 0.053(9) Uiso 1 1 d . . H5O H -0.1940(18) 0.767(3) -0.292(2) 0.088(12) Uiso 1 1 d . . H6O H -0.2719(16) 0.638(3) -0.180(2) 0.079(11) Uiso 1 1 d . . H2O H 0.2257(17) 0.685(3) 0.063(3) 0.093(13) Uiso 1 1 d . . O7 O 0.01694(7) 0.61846(13) 0.05473(10) 0.0271(4) Uani 1 1 d . . O4 O 0.05930(8) 0.72676(14) -0.13554(11) 0.0347(5) Uani 1 1 d . . O3 O 0.17244(7) 0.71207(13) -0.02782(10) 0.0311(4) Uani 1 1 d . . O2 O 0.23936(7) 0.66665(14) 0.12425(11) 0.0308(4) Uani 1 1 d . . O6 O -0.23927(7) 0.67339(14) -0.20629(11) 0.0333(4) Uani 1 1 d . . O1 O 0.12848(8) 0.53177(15) 0.32979(11) 0.0355(5) Uani 1 1 d . . O5 O -0.14912(7) 0.75920(14) -0.27412(10) 0.0320(4) Uani 1 1 d . . C9 C 0.01134(10) 0.65708(18) -0.02736(14) 0.0242(5) Uani 1 1 d . . C6 C 0.12798(10) 0.64523(17) 0.08488(15) 0.0228(5) Uani 1 1 d . . C8 C 0.06357(10) 0.68792(18) -0.05524(15) 0.0252(5) Uani 1 1 d . . C10 C -0.05391(10) 0.66014(18) -0.07338(14) 0.0232(5) Uani 1 1 d . . C7 C 0.12527(10) 0.68296(17) -0.00028(15) 0.0235(5) Uani 1 1 d . . C4 C 0.18637(10) 0.59873(18) 0.22772(14) 0.0266(5) Uani 1 1 d . . H4 H 0.2249 0.5942 0.2684 0.032 Uiso 1 1 calc R U C11 C -0.07148(10) 0.70604(18) -0.15461(14) 0.0246(5) Uani 1 1 d . . H11 H -0.0404 0.7349 -0.1815 0.030 Uiso 1 1 calc R U C14 C -0.16330(10) 0.61962(18) -0.07870(15) 0.0259(5) Uani 1 1 d . . H14 H -0.1945 0.5895 -0.0527 0.031 Uiso 1 1 calc R U C2 C 0.07365(10) 0.57338(19) 0.19143(15) 0.0274(5) Uani 1 1 d . . H2 H 0.0359 0.5512 0.2066 0.033 Uiso 1 1 calc R U C5 C 0.18477(10) 0.63611(18) 0.14628(15) 0.0239(5) Uani 1 1 d . . C15 C -0.10103(10) 0.61731(18) -0.03565(15) 0.0259(5) Uani 1 1 d . . H15 H -0.0902 0.5865 0.0198 0.031 Uiso 1 1 calc R U C12 C -0.13341(10) 0.70972(18) -0.19586(14) 0.0237(5) Uani 1 1 d . . C3 C 0.13020(11) 0.56726(18) 0.24998(15) 0.0271(5) Uani 1 1 d . . C13 C -0.18029(10) 0.66534(18) -0.15904(15) 0.0245(5) Uani 1 1 d . . C1 C 0.07356(10) 0.61243(18) 0.11075(14) 0.0238(5) Uani 1 1 d . . N1 N 0.25012(9) 0.02241(16) 0.07618(12) 0.0288(5) Uani 1 1 d . . N2 N -0.15875(9) -0.10312(17) 0.15754(13) 0.0336(5) Uani 1 1 d . . C18 C 0.12506(10) 0.00561(19) 0.09371(15) 0.0269(5) Uani 1 1 d . . C20 C 0.22740(11) -0.0655(2) 0.10279(16) 0.0319(6) Uani 1 1 d . . H20 H 0.2547 -0.1233 0.1151 0.038 Uiso 1 1 calc R U C21 C 0.05978(11) 0.0015(2) 0.10428(17) 0.0326(6) Uani 1 1 d . . C23 C -0.03430(11) -0.08597(19) 0.13739(15) 0.0295(6) Uani 1 1 d . . C19 C 0.16669(11) -0.0767(2) 0.11331(16) 0.0333(6) Uani 1 1 d . . H19 H 0.1533 -0.1403 0.1338 0.040 Uiso 1 1 calc R U C16 C 0.20971(11) 0.10127(19) 0.05684(15) 0.0293(6) Uani 1 1 d . . H16 H 0.2245 0.1641 0.0370 0.035 Uiso 1 1 calc R U C17 C 0.14814(11) 0.09635(19) 0.06413(15) 0.0289(5) Uani 1 1 d . . H17 H 0.1214 0.1545 0.0491 0.035 Uiso 1 1 calc R U C22 C 0.03074(11) -0.0817(2) 0.12597(17) 0.0328(6) Uani 1 1 d . . C27 C -0.06167(11) -0.1816(2) 0.14546(17) 0.0360(6) Uani 1 1 d . . H27 H -0.0382 -0.2434 0.1445 0.043 Uiso 1 1 calc R U C24 C -0.07145(11) 0.0013(2) 0.14033(17) 0.0355(6) Uani 1 1 d . . H24 H -0.0550 0.0686 0.1353 0.043 Uiso 1 1 calc R U C26 C -0.12290(11) -0.1865(2) 0.15489(18) 0.0373(6) Uani 1 1 d . . H26 H -0.1407 -0.2529 0.1598 0.045 Uiso 1 1 calc R U C25 C -0.13250(11) -0.0109(2) 0.15062(17) 0.0365(6) Uani 1 1 d . . H25 H -0.1570 0.0495 0.1529 0.044 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O7 0.0163(8) 0.0407(10) 0.0242(9) 0.0064(8) 0.0038(6) 0.0003(7) O4 0.0166(9) 0.0601(12) 0.0276(9) 0.0109(9) 0.0052(7) -0.0004(8) O3 0.0188(8) 0.0451(11) 0.0301(9) 0.0041(8) 0.0068(7) -0.0027(7) O2 0.0172(8) 0.0466(11) 0.0286(10) 0.0031(8) 0.0044(7) -0.0040(7) O6 0.0137(8) 0.0511(12) 0.0339(10) 0.0059(9) 0.0023(7) -0.0022(7) O1 0.0240(9) 0.0559(13) 0.0259(10) 0.0094(9) 0.0036(7) -0.0015(8) O5 0.0182(9) 0.0517(11) 0.0262(9) 0.0079(8) 0.0052(7) 0.0037(7) C9 0.0218(11) 0.0288(13) 0.0225(12) 0.0020(10) 0.0055(9) 0.0009(9) C6 0.0184(11) 0.0245(13) 0.0257(12) -0.0011(10) 0.0050(9) 0.0011(9) C8 0.0203(11) 0.0310(13) 0.0244(12) 0.0015(10) 0.0053(9) 0.0019(9) C10 0.0167(11) 0.0284(13) 0.0245(12) -0.0021(10) 0.0044(9) 0.0012(9) C7 0.0195(11) 0.0269(13) 0.0249(12) -0.0029(10) 0.0066(9) 0.0023(9) C4 0.0173(11) 0.0357(14) 0.0256(12) 0.0005(11) 0.0017(9) 0.0005(9) C11 0.0185(11) 0.0309(13) 0.0258(12) 0.0012(10) 0.0080(9) -0.0002(9) C14 0.0194(11) 0.0319(13) 0.0282(13) 0.0005(11) 0.0086(9) -0.0017(9) C2 0.0189(11) 0.0365(14) 0.0276(13) 0.0009(11) 0.0068(9) 0.0000(10) C5 0.0187(11) 0.0265(13) 0.0266(13) -0.0030(10) 0.0049(9) -0.0023(9) C15 0.0241(12) 0.0293(13) 0.0251(12) 0.0006(11) 0.0068(9) -0.0014(10) C12 0.0190(11) 0.0304(13) 0.0217(12) 0.0012(10) 0.0041(9) 0.0025(9) C3 0.0264(12) 0.0298(13) 0.0258(13) 0.0009(11) 0.0073(9) 0.0017(10) C13 0.0147(10) 0.0311(13) 0.0277(13) -0.0033(10) 0.0046(9) 0.0003(9) C1 0.0161(11) 0.0278(13) 0.0266(12) -0.0010(10) 0.0021(9) 0.0017(9) N1 0.0251(10) 0.0355(12) 0.0267(11) -0.0009(9) 0.0073(8) 0.0000(9) N2 0.0212(11) 0.0443(14) 0.0360(12) 0.0034(10) 0.0075(9) -0.0017(9) C18 0.0222(12) 0.0329(14) 0.0258(12) -0.0026(11) 0.0053(9) -0.0013(10) C20 0.0264(13) 0.0340(14) 0.0356(14) 0.0014(12) 0.0068(10) 0.0031(10) C21 0.0246(13) 0.0362(15) 0.0373(15) 0.0016(12) 0.0069(11) 0.0024(11) C23 0.0227(12) 0.0372(15) 0.0290(13) -0.0001(11) 0.0063(10) -0.0019(10) C19 0.0307(13) 0.0327(14) 0.0383(15) 0.0019(12) 0.0115(11) -0.0006(11) C16 0.0274(13) 0.0325(14) 0.0287(13) 0.0007(11) 0.0074(10) -0.0047(10) C17 0.0264(12) 0.0331(14) 0.0268(13) 0.0008(11) 0.0047(10) 0.0024(10) C22 0.0263(13) 0.0363(15) 0.0375(15) -0.0004(12) 0.0101(11) 0.0005(11) C27 0.0289(13) 0.0362(15) 0.0450(16) 0.0048(13) 0.0121(11) 0.0038(11) C24 0.0303(14) 0.0316(14) 0.0462(16) -0.0040(12) 0.0115(11) -0.0033(11) C26 0.0293(14) 0.0339(15) 0.0497(17) 0.0080(13) 0.0106(12) -0.0034(11) C25 0.0253(13) 0.0397(16) 0.0456(16) -0.0028(13) 0.0100(11) 0.0013(11) 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 C1 O7 C9 121.85(17) C8 O4 H4O 112(2) C5 O2 H2O 103(2) C13 O6 H6O 114.1(19) C3 O1 H1O 110.3(19) C12 O5 H5O 111(2) C8 C9 O7 119.71(19) C8 C9 C10 128.6(2) O7 C9 C10 111.72(18) C1 C6 C5 116.7(2) C1 C6 C7 120.62(19) C5 C6 C7 122.70(19) O4 C8 C9 120.9(2) O4 C8 C7 117.28(19) C9 C8 C7 121.8(2) C11 C10 C15 118.3(2) C11 C10 C9 121.74(19) C15 C10 C9 120.0(2) O3 C7 C6 123.7(2) O3 C7 C8 120.3(2) C6 C7 C8 115.96(19) C5 C4 C3 119.0(2) C5 C4 H4 120.5 C3 C4 H4 120.5 C12 C11 C10 120.6(2) C12 C11 H11 119.7 C10 C11 H11 119.7 C13 C14 C15 120.7(2) C13 C14 H14 119.6 C15 C14 H14 119.6 C1 C2 C3 118.4(2) C1 C2 H2 120.8 C3 C2 H2 120.8 O2 C5 C4 119.2(2) O2 C5 C6 119.1(2) C4 C5 C6 121.7(2) C14 C15 C10 120.6(2) C14 C15 H15 119.7 C10 C15 H15 119.7 O5 C12 C11 118.89(19) O5 C12 C13 119.92(19) C11 C12 C13 121.2(2) O1 C3 C2 117.0(2) O1 C3 C4 121.8(2) C2 C3 C4 121.2(2) O6 C13 C14 125.91(19) O6 C13 C12 115.5(2) C14 C13 C12 118.6(2) O7 C1 C2 116.97(19) O7 C1 C6 120.0(2) C2 C1 C6 123.1(2) C16 N1 C20 116.5(2) C25 N2 C26 116.8(2) C19 C18 C17 116.9(2) C19 C18 C21 123.4(2) C17 C18 C21 119.7(2) N1 C20 C19 123.7(2) N1 C20 H20 118.1 C19 C20 H20 118.1 C22 C21 C18 125.8(2) C22 C21 H21 119.2(17) C18 C21 H21 115.0(17) C27 C23 C24 116.8(2) C27 C23 C22 119.3(2) C24 C23 C22 123.9(2) C20 C19 C18 119.5(2) C20 C19 H19 120.2 C18 C19 H19 120.2 N1 C16 C17 123.7(2) N1 C16 H16 118.2 C17 C16 H16 118.2 C16 C17 C18 119.7(2) C16 C17 H17 120.2 C18 C17 H17 120.2 C21 C22 C23 126.0(2) C21 C22 H22 119.0(15) C23 C22 H22 114.7(15) C26 C27 C23 119.8(2) C26 C27 H27 120.1 C23 C27 H27 120.1 C25 C24 C23 119.6(2) C25 C24 H24 120.2 C23 C24 H24 120.2 N2 C26 C27 123.7(2) N2 C26 H26 118.2 C27 C26 H26 118.2 N2 C25 C24 123.4(2) N2 C25 H25 118.3 C24 C25 H25 118.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O7 C1 1.368(2) O7 C9 1.377(3) O4 C8 1.355(3) O4 H4O 0.85(3) O3 C7 1.256(3) O2 C5 1.368(3) O2 H2O 0.98(4) O6 C13 1.354(3) O6 H6O 1.01(4) O1 C3 1.355(3) O1 H1O 0.86(3) O5 C12 1.376(3) O5 H5O 0.97(4) C9 C8 1.365(3) C9 C10 1.461(3) C6 C1 1.400(3) C6 C5 1.415(3) C6 C7 1.427(3) C8 C7 1.447(3) C10 C11 1.399(3) C10 C15 1.406(3) C4 C5 1.374(3) C4 C3 1.404(3) C4 H4 0.9500 C11 C12 1.376(3) C11 H11 0.9500 C14 C13 1.385(3) C14 C15 1.390(3) C14 H14 0.9500 C2 C1 1.376(3) C2 C3 1.386(3) C2 H2 0.9500 C15 H15 0.9500 C12 C13 1.401(3) N1 C16 1.340(3) N1 C20 1.340(3) N2 C25 1.335(3) N2 C26 1.336(3) C18 C19 1.391(3) C18 C17 1.394(3) C18 C21 1.470(3) C20 C19 1.378(3) C20 H20 0.9500 C21 C22 1.328(4) C21 H21 0.94(3) C23 C27 1.388(3) C23 C24 1.394(3) C23 C22 1.469(3) C19 H19 0.9500 C16 C17 1.374(3) C16 H16 0.9500 C17 H17 0.9500 C22 H22 1.02(3) C27 C26 1.377(3) C27 H27 0.9500 C24 C25 1.385(3) C24 H24 0.9500 C26 H26 0.9500 C25 H25 0.9500 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O N1 0.86(3) 1.91(3) 2.763(3) 174(3) 4 O4 H4O O3 0.85(3) 2.29(3) 2.705(2) 110(2) . O4 H4O O5 0.85(3) 1.90(3) 2.690(2) 153(3) 2_554 O5 H5O O2 0.97(4) 1.95(4) 2.797(2) 144(3) 8_465 O6 H6O N2 1.01(4) 1.69(4) 2.663(2) 162(3) 7_455 O2 H2O O3 0.98(4) 1.70(4) 2.617(2) 155(3) . C4 H4 N1 0.95 2.59 3.287(3) 130.7 4 C11 H11 O4 0.95 2.15 2.821(3) 126.5 . C20 H20 O3 0.95 2.58 3.294(3) 131.9 7 C24 H24 O4 0.95 2.64 3.521(3) 154.1 5_565