#------------------------------------------------------------------------------ #$Date: 2016-03-13 15:25:55 +0200 (Sun, 13 Mar 2016) $ #$Revision: 178180 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/27/1542792.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_1542792 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 'C31 H28 N2 O9' _chemical_formula_weight 572.55 _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _cell_angle_alpha 97.351(7) _cell_angle_beta 95.446(7) _cell_angle_gamma 115.237(8) _cell_formula_units_Z 2 _cell_length_a 10.1899(9) _cell_length_b 11.6532(11) _cell_length_c 13.0214(12) _cell_measurement_temperature 150(2) _cell_volume 1367.8(2) _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 14650 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.483 _diffrn_reflns_theta_min 3.200 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.390 _exptl_crystal_description Plate _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.280 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 407 _refine_ls_number_reflns 6248 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0511 _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^)+(0.0598P)^2^+0.4848P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1199 _refine_ls_wR_factor_ref 0.1323 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4498 _reflns_number_total 6248 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file lc5063.cif _cod_data_source_block QDP_I _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_database_code 1542792 _publcif_datablock.id {2ca2c0b0-c370-46ca-aa86-b0c8e7d68c41} _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 0.950 _shelx_estimated_absorpt_t_max 0.985 _shelxl_version_number 2013-2 _shelx_res_file ; TITL datam in P-1 CELL 0.71073 10.1899 11.6532 13.0214 97.351 95.446 115.237 ZERR 2.00 0.0009 0.0011 0.0012 0.007 0.007 0.008 LATT 1 SFAC C H N O UNIT 62 56 4 18 MERG 2 FMAP 2 PLAN 20 SIZE 0.150 0.250 0.500 ACTA BOND $H L.S. 10 TEMP -123.00 WGHT 0.059800 0.484800 FVAR 0.47225 O4 4 0.353282 0.054755 0.090771 11.00000 0.03483 0.04884 = 0.01451 0.00725 0.00427 0.03386 O7 4 0.113202 0.143864 -0.068810 11.00000 0.02478 0.03097 = 0.01142 0.00490 0.00447 0.01979 O3 4 0.408492 0.000318 -0.103650 11.00000 0.03301 0.04148 = 0.01732 0.00507 0.00425 0.02956 O1 4 0.039377 0.156834 -0.430799 11.00000 0.03796 0.04658 = 0.01487 0.01067 0.00780 0.03394 O5 4 0.178831 0.164018 0.396590 11.00000 0.03526 0.04867 = 0.01317 0.00871 0.00638 0.03115 O6 4 -0.008142 0.273777 0.381638 11.00000 0.03912 0.04604 = 0.01538 0.00637 0.00808 0.03443 O2 4 0.376858 0.010718 -0.304706 11.00000 0.03942 0.05328 = 0.01695 0.00754 0.00748 0.03872 C9 1 0.182472 0.124302 0.018433 11.00000 0.02020 0.02174 = 0.01352 0.00393 0.00178 0.01142 C2 1 0.072939 0.151906 -0.246887 11.00000 0.02494 0.02695 = 0.01735 0.00537 0.00558 0.01921 AFIX 43 H2 2 0.004189 0.184865 -0.233837 11.00000 -1.20000 AFIX 0 C6 1 0.247336 0.074372 -0.181983 11.00000 0.02102 0.02282 = 0.01443 0.00241 0.00262 0.01289 C10 1 0.133917 0.163092 0.113665 11.00000 0.01967 0.02006 = 0.01551 0.00309 0.00416 0.01078 C7 1 0.316748 0.046061 -0.095012 11.00000 0.01982 0.02146 = 0.01778 0.00233 0.00192 0.01271 C4 1 0.207033 0.084201 -0.366805 11.00000 0.03038 0.03258 = 0.01324 0.00580 0.00771 0.02156 AFIX 43 H4 2 0.227728 0.071631 -0.435834 11.00000 -1.20000 AFIX 0 N1 3 0.159949 0.759598 0.394553 11.00000 0.04267 0.05142 = 0.02283 0.01125 0.01005 0.03709 C8 1 0.281775 0.075599 0.006760 11.00000 0.02313 0.02431 = 0.01355 0.00451 0.00176 0.01402 C11 1 0.179515 0.144311 0.213277 11.00000 0.01940 0.02387 = 0.01791 0.00459 0.00387 0.01463 AFIX 43 H11 2 0.243696 0.104876 0.220097 11.00000 -1.20000 AFIX 0 C1 1 0.145055 0.122496 -0.166639 11.00000 0.02000 0.02087 = 0.01305 0.00311 0.00538 0.01166 N2 3 0.795571 0.368591 0.348047 11.00000 0.03443 0.04025 = 0.02879 0.00938 0.01030 0.02782 C14 1 -0.010132 0.258054 0.194310 11.00000 0.02667 0.03048 = 0.01901 0.00800 0.00571 0.02100 AFIX 43 H14 2 -0.074627 0.297205 0.187686 11.00000 -1.20000 AFIX 0 C12 1 0.131400 0.182921 0.300971 11.00000 0.02149 0.02451 = 0.01393 0.00554 0.00272 0.01299 C24 1 0.237288 0.602849 0.323096 11.00000 0.03122 0.03662 = 0.03258 0.00173 0.00284 0.02261 AFIX 43 H24 2 0.215162 0.526644 0.274173 11.00000 -1.20000 AFIX 0 C17 1 0.568244 0.357956 0.268647 11.00000 0.02620 0.03223 = 0.03638 0.00029 0.00248 0.01547 AFIX 43 H17 2 0.482958 0.314577 0.216134 11.00000 -1.20000 AFIX 0 C22 1 0.483394 0.617734 0.394640 11.00000 0.02421 0.03276 = 0.03108 0.00648 0.00424 0.01827 C5 1 0.277384 0.056052 -0.285621 11.00000 0.02501 0.02633 = 0.01671 0.00180 0.00467 0.01800 C21 1 0.475951 0.515445 0.331487 11.00000 0.02613 0.03341 = 0.03092 0.00161 0.00064 0.01874 C23 1 0.371927 0.665564 0.391257 11.00000 0.02733 0.03112 = 0.02474 0.00823 0.00763 0.01936 C18 1 0.587928 0.467804 0.338358 11.00000 0.02515 0.02712 = 0.03006 0.00586 0.00649 0.01660 C3 1 0.104304 0.131672 -0.347402 11.00000 0.02597 0.02770 = 0.01444 0.00530 0.00329 0.01755 C13 1 0.035512 0.240010 0.292422 11.00000 0.02393 0.02281 = 0.01581 0.00432 0.00581 0.01365 C19 1 0.716287 0.526587 0.412777 11.00000 0.03049 0.03344 = 0.02554 0.00054 0.00369 0.02094 AFIX 43 H19 2 0.735581 0.601861 0.461882 11.00000 -1.20000 AFIX 0 C15 1 0.037466 0.219558 0.106384 11.00000 0.02638 0.03005 = 0.01503 0.00754 0.00417 0.01820 AFIX 43 H15 2 0.004153 0.231620 0.039810 11.00000 -1.20000 AFIX 0 C27 1 0.396620 0.777363 0.460326 11.00000 0.03109 0.03536 = 0.02824 0.00153 0.00256 0.02057 AFIX 43 H27 2 0.486852 0.823965 0.507769 11.00000 -1.20000 AFIX 0 C16 1 0.673072 0.312714 0.276338 11.00000 0.03462 0.03177 = 0.03512 0.00233 0.00978 0.02079 AFIX 43 H16 2 0.657317 0.237864 0.228089 11.00000 -1.20000 AFIX 0 C20 1 0.814569 0.474591 0.414395 11.00000 0.02925 0.04308 = 0.02534 0.00454 0.00339 0.02409 AFIX 43 H20 2 0.901370 0.516258 0.465663 11.00000 -1.20000 AFIX 0 C26 1 0.289056 0.819876 0.459304 11.00000 0.04718 0.04295 = 0.02702 0.00477 0.00796 0.03370 AFIX 43 H26 2 0.307893 0.895982 0.507166 11.00000 -1.20000 AFIX 0 C25 1 0.136912 0.652898 0.327693 11.00000 0.03117 0.04879 = 0.02855 0.00634 0.00371 0.02692 AFIX 43 H25 2 0.046032 0.609115 0.280656 11.00000 -1.20000 AFIX 0 O9 4 0.363826 0.545004 0.083660 11.00000 0.05216 0.08402 = 0.06031 0.03333 -0.00799 0.01708 O8 4 0.196416 0.605357 -0.064068 11.00000 0.08672 0.07763 = 0.06482 0.03042 -0.00152 0.04682 C28 1 0.384933 0.671394 0.086109 11.00000 0.05561 0.05918 = 0.06056 0.00036 0.00808 0.00198 AFIX 23 H28A 2 0.463792 0.714647 0.045659 11.00000 -1.20000 H28B 2 0.417426 0.718771 0.159651 11.00000 -1.20000 AFIX 0 C29 1 0.249210 0.677122 0.041708 11.00000 0.08193 0.07447 = 0.09457 0.02287 0.02600 0.03938 AFIX 23 H29A 2 0.172621 0.640888 0.085636 11.00000 -1.20000 H29B 2 0.269655 0.768236 0.042224 11.00000 -1.20000 AFIX 0 C31 1 0.317246 0.477549 -0.022225 11.00000 0.07623 0.03861 = 0.09146 0.00469 -0.03656 0.01668 AFIX 23 H31A 2 0.298931 0.386645 -0.024536 11.00000 -1.20000 H31B 2 0.396029 0.517343 -0.063699 11.00000 -1.20000 AFIX 0 C30 1 0.182496 0.481292 -0.068614 11.00000 0.09497 0.05888 = 0.09728 0.00810 -0.04819 0.02475 AFIX 23 H30A 2 0.155119 0.436892 -0.142956 11.00000 -1.20000 H30B 2 0.101651 0.433202 -0.031340 11.00000 -1.20000 AFIX 0 H22 2 0.567780 0.667367 0.449653 11.00000 0.03041 H21 2 0.395281 0.468820 0.276996 11.00000 0.04128 H6O 2 -0.073078 0.306174 0.366954 11.00000 0.05580 H5O 2 0.118160 0.167949 0.441250 11.00000 0.05900 H4O 2 0.417224 0.030460 0.068216 11.00000 0.05366 H1O 2 -0.031386 0.188226 -0.413703 11.00000 0.06273 H2O 2 0.407345 -0.000482 -0.244349 11.00000 0.05258 HKLF 4 REM datam in P-1 REM R1 = 0.0511 for 4498 Fo > 4sig(Fo) and 0.0773 for all 6248 data REM 407 parameters refined using 0 restraints END WGHT 0.0575 0.5026 REM Highest difference peak 0.280, deepest hole -0.226, 1-sigma level 0.048 Q1 1 0.2777 0.0838 -0.2264 11.00000 0.05 0.28 Q2 1 0.3137 0.0877 -0.0430 11.00000 0.05 0.28 Q3 1 0.2143 0.0830 0.0174 11.00000 0.05 0.26 Q4 1 0.2042 0.1003 -0.1769 11.00000 0.05 0.26 Q5 1 0.2638 0.1327 0.0150 11.00000 0.05 0.25 Q6 1 0.3122 0.7202 -0.0166 11.00000 0.05 0.25 Q7 1 0.2941 0.6272 0.3701 11.00000 0.05 0.24 Q8 1 0.0850 0.2141 0.2999 11.00000 0.05 0.24 Q9 1 0.4428 0.6558 0.3764 11.00000 0.05 0.23 Q10 1 0.2954 0.0840 -0.1361 11.00000 0.05 0.23 Q11 1 0.0845 0.0908 -0.2252 11.00000 0.05 0.23 Q12 1 0.0429 0.2771 0.2483 11.00000 0.05 0.22 Q13 1 0.2364 0.4807 0.0598 11.00000 0.05 0.22 Q14 1 0.2787 0.1151 -0.3179 11.00000 0.05 0.21 Q15 1 0.0648 0.1126 -0.3005 11.00000 0.05 0.21 Q16 1 0.3105 0.7672 0.4765 11.00000 0.05 0.21 Q17 1 0.1349 0.1224 0.0658 11.00000 0.05 0.20 Q18 1 0.1138 0.8080 0.3895 11.00000 0.05 0.20 Q19 1 0.1924 0.0284 -0.3315 11.00000 0.05 0.20 Q20 1 0.8106 0.3069 0.3487 11.00000 0.05 0.20 ; _shelx_res_checksum 54970 _shelx_hkl_file ; 0 0 2 103.53 1.19 0 0 -2 100.38 1.28 0 0 -2 93.21 1.20 0 0 3 2182.85 21.17 0 0 -3 2218.14 22.57 0 0 -3 2219.94 21.32 0 0 4 968.28 11.81 0 0 -4 943.77 11.55 0 0 -4 947.53 12.26 0 0 5 92.78 2.19 0 0 -5 102.69 2.31 0 0 -5 92.85 1.95 0 0 6 496.38 8.51 0 0 6 515.97 8.32 0 0 -6 531.84 9.32 0 0 7 30.05 1.19 0 0 7 28.58 1.31 0 0 -7 38.01 1.58 0 0 8 85.89 2.73 0 0 8 89.50 2.55 0 0 -8 87.47 2.87 0 0 9 -0.10 0.77 0 0 9 1.22 0.73 0 0 -9 0.08 0.93 0 0 10 258.04 6.58 0 0 10 252.47 6.93 0 0 -10 245.99 6.96 0 0 11 65.16 3.44 0 0 11 67.57 3.11 0 0 -11 67.62 3.14 0 0 12 13.37 1.48 0 0 12 15.61 1.73 0 0 -12 16.80 1.81 0 0 13 6.43 1.61 0 0 13 10.47 1.64 0 0 -13 7.20 1.61 0 0 14 22.00 2.76 0 0 14 22.56 2.14 0 0 -14 21.39 2.82 0 0 15 -0.38 1.32 0 0 15 1.59 1.43 0 0 -15 1.58 1.41 0 0 -16 11.24 2.31 0 1 -16 0.41 1.29 0 -1 16 -0.52 1.31 0 1 -15 37.46 2.89 0 -1 15 36.96 3.73 0 1 -14 -0.52 1.12 0 -1 14 0.07 0.91 0 -1 14 -0.99 1.21 0 1 -13 -0.34 1.10 0 -1 13 2.73 1.49 0 -1 13 1.93 0.92 0 1 -12 2.63 1.09 0 -1 12 -0.43 1.16 0 -1 12 1.85 1.06 0 1 -11 564.32 14.44 0 -1 11 577.73 13.60 0 -1 11 584.12 15.41 0 1 -10 109.97 3.85 0 -1 10 111.57 3.51 0 -1 10 110.76 4.09 0 1 -9 14.42 1.30 0 1 -9 16.87 1.38 0 -1 9 14.15 1.43 0 1 -8 54.97 2.09 0 1 -8 56.95 1.91 0 -1 8 63.46 2.35 0 1 -7 7.20 0.83 0 1 -7 9.00 0.85 0 -1 7 7.49 0.92 0 1 -6 0.08 0.37 0 1 -6 -0.44 0.52 0 -1 6 -0.18 0.45 0 1 -5 201.20 3.52 0 1 -5 196.95 3.51 0 -1 5 202.72 3.79 0 1 -4 206.53 3.18 0 1 -4 206.90 3.13 0 -1 4 212.11 3.66 0 1 -3 2512.51 23.81 0 1 -3 2502.83 23.80 0 -1 3 2506.75 26.30 0 1 -2 7.64 0.29 0 1 -2 7.53 0.28 0 -1 2 10.16 0.41 0 1 2 334.37 3.99 0 1 2 341.63 3.16 0 -1 -2 350.07 4.16 0 1 3 2.18 0.46 0 1 3 2.14 0.35 0 -1 -3 2.20 0.41 0 1 4 27.60 0.77 0 1 4 30.48 0.96 0 -1 -4 31.58 1.06 0 1 5 2.76 0.41 0 1 5 1.88 0.48 0 -1 -5 3.41 0.58 0 1 6 4.46 0.58 0 1 6 4.92 0.63 0 -1 -6 4.82 0.76 0 1 7 178.18 3.80 0 1 7 183.75 4.15 0 -1 -7 174.39 4.35 0 1 8 -0.40 0.57 0 1 8 1.37 0.53 0 -1 -8 -0.60 0.68 0 1 9 29.06 1.84 0 1 9 35.18 1.71 0 -1 -9 31.57 1.99 0 1 10 54.69 2.45 0 1 10 52.26 2.33 0 -1 -10 58.24 2.83 0 1 11 6.01 1.38 0 1 11 6.29 1.34 0 -1 -11 5.15 1.37 0 1 12 64.51 3.40 0 1 12 58.53 3.40 0 -1 -12 68.33 3.56 0 1 13 41.84 2.99 0 1 13 42.87 3.07 0 -1 -13 41.03 2.85 0 1 14 3.38 1.46 0 1 14 1.57 1.62 0 -1 -14 5.07 1.55 0 1 15 85.45 5.10 0 -1 -15 96.98 5.16 0 -1 -16 2.42 1.77 0 2 -16 9.25 2.28 0 -2 16 7.63 2.30 0 2 -15 9.74 1.80 0 -2 15 10.97 2.05 0 2 -14 34.55 2.55 0 -2 14 33.09 2.69 0 -2 14 30.81 3.45 0 2 -13 25.00 2.19 0 -2 13 31.72 2.55 0 -2 13 25.39 1.90 0 2 -12 23.71 1.99 0 -2 12 26.85 2.25 0 2 -11 313.07 8.29 0 2 -11 297.23 7.68 0 -2 11 313.06 9.90 0 2 -10 201.77 5.49 0 2 -10 187.71 5.25 0 -2 10 213.85 6.40 0 2 -9 3.97 0.77 0 2 -9 3.68 0.85 0 -2 9 3.67 1.14 0 2 -8 22.06 1.31 0 2 -8 21.81 1.23 0 -2 8 23.71 1.61 0 2 -7 114.83 2.76 0 2 -7 116.93 2.91 0 -2 7 114.14 3.30 0 2 -6 17.51 0.98 0 2 -6 15.45 0.80 0 -2 6 15.28 1.05 0 2 -5 505.88 7.23 0 2 -5 530.22 7.96 0 -2 5 514.83 8.54 0 2 -4 4.47 0.39 0 2 -4 5.96 0.46 0 -2 4 5.35 0.66 0 2 -3 641.73 7.11 0 2 -3 641.14 7.94 0 -2 3 648.48 8.58 0 2 -2 255.21 3.32 0 2 -2 249.68 2.69 0 -2 2 261.80 3.58 0 2 -1 277.84 3.52 0 -2 1 281.28 3.01 0 -2 1 269.64 3.15 0 2 0 27.71 0.76 0 -2 0 29.72 0.60 0 -2 0 26.44 0.52 0 2 1 1255.01 13.69 0 -2 -1 1204.32 8.81 0 -2 -1 1227.66 12.61 0 2 2 0.76 0.47 0 2 2 1.45 0.25 0 -2 -2 1.01 0.41 0 2 3 1.32 0.30 0 2 3 1.31 0.49 0 -2 -3 1.44 0.48 0 2 4 133.74 2.78 0 2 4 128.53 2.20 0 -2 -4 134.89 2.88 0 2 5 157.75 2.93 0 2 5 163.08 3.59 0 -2 -5 163.96 3.69 0 2 6 1.16 0.56 0 2 6 0.19 0.46 0 -2 -6 0.04 0.64 0 2 7 16.49 1.18 0 2 7 17.61 1.08 0 -2 -7 19.83 1.40 0 2 8 47.89 2.04 0 2 8 40.05 1.68 0 -2 -8 50.23 2.29 0 2 9 171.37 5.08 0 2 9 159.66 4.66 0 -2 -9 178.02 5.39 0 2 10 74.98 3.58 0 2 10 71.22 2.98 0 -2 -10 78.92 3.65 0 2 11 168.21 5.48 0 2 11 180.87 6.03 0 -2 -11 178.57 6.29 0 2 12 235.87 7.79 0 2 12 220.08 7.48 0 -2 -12 243.47 8.19 0 2 13 59.85 3.62 0 2 13 72.34 3.72 0 -2 -13 70.20 4.08 0 2 14 5.11 1.60 0 -2 -14 -2.67 1.77 0 2 15 4.94 2.03 0 -2 -15 5.44 1.81 0 3 -16 19.03 2.46 0 -3 16 17.70 2.99 0 3 -15 3.46 1.50 0 -3 15 5.99 2.27 0 3 -14 20.30 2.39 0 -3 14 14.68 1.72 0 -3 14 16.19 2.43 0 3 -13 10.21 1.48 0 3 -13 6.74 1.85 0 -3 13 7.56 1.84 0 3 -12 35.64 2.25 0 3 -12 25.40 1.80 0 -3 12 33.22 2.47 0 3 -11 11.63 1.57 0 3 -11 13.33 1.29 0 -3 11 11.11 1.79 0 3 -10 151.61 4.62 0 3 -10 144.49 4.31 0 -3 10 149.51 5.16 0 3 -9 4.10 0.82 0 3 -9 5.15 1.02 0 -3 9 4.61 1.19 0 3 -8 3.90 0.92 0 3 -8 5.64 0.74 0 -3 8 5.01 1.13 0 3 -7 11.90 0.81 0 3 -7 11.12 0.85 0 -3 7 12.78 1.27 0 3 -6 45.07 1.35 0 3 -6 49.29 1.53 0 -3 6 44.82 1.91 0 3 -5 21.51 0.88 0 3 -5 19.11 0.91 0 -3 5 19.95 1.17 0 3 -4 52.43 1.21 0 3 -4 50.12 1.41 0 -3 4 52.34 1.71 0 3 -3 199.68 3.46 0 3 -3 203.43 2.88 0 -3 3 208.79 3.62 0 3 -2 187.05 3.18 0 -3 2 189.05 2.81 0 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6.65 2.05 0 4 -13 2.76 1.27 0 4 -13 3.79 1.36 0 -4 13 6.47 1.66 0 4 -12 17.98 1.57 0 4 -12 17.39 1.64 0 -4 12 15.13 2.17 0 4 -11 54.00 2.77 0 4 -11 53.60 2.47 0 -4 11 48.12 3.24 0 4 -10 115.70 3.62 0 4 -10 121.56 4.15 0 -4 10 111.35 4.50 0 4 -9 27.39 1.83 0 4 -9 25.90 1.43 0 -4 9 31.86 2.22 0 4 -8 29.98 1.75 0 4 -8 34.21 1.62 0 -4 8 32.60 2.13 0 4 -7 37.36 1.53 0 4 -7 39.56 1.51 0 -4 7 38.84 2.09 0 4 -6 33.75 1.44 0 4 -6 35.17 1.19 0 -4 6 39.91 1.90 0 4 -5 12.24 0.89 0 4 -5 13.17 0.66 0 -4 5 13.68 1.19 0 4 -4 114.07 2.67 0 4 -4 106.65 2.01 0 -4 4 104.42 2.69 0 4 -3 5.11 0.62 0 -4 3 3.61 0.50 0 -4 3 2.36 0.79 0 4 -2 0.58 0.49 0 -4 2 -0.01 0.38 0 -4 2 0.40 0.40 0 4 -1 49.06 1.62 0 -4 1 46.46 1.17 0 -4 1 46.01 1.19 0 4 0 27.37 1.21 0 -4 0 26.33 0.82 0 -4 0 26.18 0.91 0 4 1 26.97 1.27 0 -4 -1 26.31 1.01 0 -4 -1 24.57 0.71 0 4 2 3.94 0.78 0 -4 -2 5.38 0.62 0 -4 -2 4.15 0.31 0 4 3 21.83 1.19 0 -4 -3 27.10 1.20 0 -4 -3 21.03 0.57 0 4 4 0.80 0.70 0 4 4 -0.23 0.27 0 -4 -4 -0.48 0.54 0 4 5 385.44 8.56 0 4 5 368.89 5.91 0 -4 -5 406.51 8.58 0 4 6 14.99 1.63 0 4 6 12.12 0.76 0 -4 -6 14.81 1.32 0 4 7 10.00 0.83 0 4 7 13.61 1.60 0 -4 -7 9.41 1.36 0 4 8 0.80 0.55 0 4 8 0.03 0.90 0 -4 -8 1.64 0.98 0 4 9 10.87 1.09 0 4 9 11.78 1.61 0 -4 -9 12.32 1.72 0 4 10 95.47 4.23 0 -4 -10 95.49 4.36 0 4 11 37.69 3.10 0 -4 -11 35.81 2.85 0 4 12 24.06 2.65 0 -4 -12 14.84 2.46 0 4 13 -0.51 1.44 0 -4 -13 0.07 1.38 0 4 14 8.70 2.06 0 -4 -14 12.81 2.83 0 5 -16 1.27 1.46 0 -5 16 -1.28 2.05 0 5 -15 15.32 2.34 0 -5 15 12.51 2.56 0 5 -14 15.60 1.87 0 -5 14 12.48 2.40 0 5 -13 9.35 1.41 0 5 -13 9.86 1.43 0 -5 13 11.24 2.05 0 5 -12 35.11 2.36 0 5 -12 30.91 2.11 0 -5 12 33.84 2.94 0 5 -11 157.39 4.80 0 5 -11 157.70 5.45 0 -5 11 147.15 5.82 0 5 -10 20.17 1.45 0 5 -10 15.12 1.59 0 -5 10 18.93 2.21 0 5 -9 11.17 1.14 0 5 -9 12.61 1.27 0 -5 9 10.83 1.81 0 5 -8 50.18 2.04 0 5 -8 50.87 1.96 0 -5 8 49.35 2.76 0 5 -7 39.36 1.75 0 5 -7 39.91 1.60 0 -5 7 37.41 2.27 0 5 -6 30.08 1.12 0 5 -6 30.63 1.62 0 -5 6 32.33 1.88 0 5 -5 344.24 5.97 0 5 -5 350.79 7.40 0 -5 5 348.71 7.84 0 5 -4 10.31 0.92 0 5 -4 10.64 0.60 0 -5 4 11.42 1.03 0 5 -3 -0.11 0.57 0 -5 3 0.97 0.55 0 -5 3 0.30 0.47 0 5 -2 3.83 0.89 0 -5 2 6.08 0.79 0 -5 2 6.41 0.67 0 5 -1 35.79 1.72 0 -5 1 39.59 1.34 0 -5 1 35.21 1.30 0 5 0 16.50 1.15 0 -5 0 12.64 0.64 0 -5 0 13.40 0.82 0 5 1 40.04 1.82 0 -5 -1 39.15 1.39 0 -5 -1 39.02 1.04 0 5 2 0.48 0.80 0 -5 -2 1.94 0.62 0 -5 -2 1.53 0.35 0 5 3 97.57 3.17 0 -5 -3 98.20 2.87 0 -5 -3 93.46 1.65 0 5 4 1.15 0.88 0 -5 -4 2.28 0.76 0 -5 -4 1.47 0.30 0 5 5 221.75 5.99 0 -5 -5 209.08 3.23 0 -5 -5 240.07 6.07 0 5 6 52.51 1.64 0 5 6 62.22 2.78 0 -5 -6 65.21 2.71 0 5 7 2.87 1.07 0 -5 -7 0.56 1.07 0 5 8 4.03 1.19 0 -5 -8 3.19 1.26 0 5 9 26.91 2.17 0 -5 -9 26.36 2.27 0 5 10 10.49 1.70 0 -5 -10 14.77 1.98 0 5 11 16.92 2.02 0 -5 -11 14.40 2.29 0 5 12 6.89 1.73 0 -5 -12 8.17 2.03 0 5 13 1.12 1.52 0 -5 -13 3.38 1.72 0 5 14 16.47 2.76 0 -5 -14 26.42 3.02 0 6 -16 28.92 3.51 0 -6 16 39.75 3.94 0 6 -15 6.78 1.65 0 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100.88 3.80 0 -6 -4 93.90 1.86 0 -6 -4 99.28 3.48 0 6 5 61.73 3.11 0 -6 -5 63.56 2.95 0 6 6 73.18 3.92 0 -6 -6 71.98 3.21 0 6 7 6.61 1.57 0 -6 -7 5.55 1.45 0 6 8 -0.08 1.17 0 -6 -8 -2.17 1.17 0 6 9 12.95 2.00 0 -6 -9 16.55 2.07 0 6 10 0.18 1.14 0 -6 -10 -0.90 1.25 0 6 11 1.28 1.90 0 -6 -11 2.89 1.59 0 6 12 -0.31 1.41 0 -6 -12 1.78 1.57 0 6 13 3.80 1.89 0 -6 -13 3.95 2.12 0 -7 15 11.51 3.20 0 7 -14 -0.05 0.94 0 -7 14 1.14 1.58 0 7 -13 10.43 1.83 0 7 -13 10.25 1.75 0 -7 13 9.15 2.21 0 7 -12 9.97 1.39 0 7 -12 9.51 1.89 0 -7 12 20.62 2.27 0 7 -11 17.43 1.70 0 7 -11 16.91 1.72 0 -7 11 17.07 2.80 0 7 -10 0.50 1.14 0 7 -10 3.22 0.81 0 -7 10 0.95 1.43 0 7 -9 1.81 0.73 0 7 -9 3.31 1.25 0 -7 9 3.64 1.45 0 7 -8 -0.13 0.55 0 7 -8 -0.20 0.84 0 -7 8 -0.17 1.08 0 7 -7 36.39 1.52 0 7 -7 35.63 2.06 0 -7 7 35.29 2.49 0 7 -6 41.07 2.29 0 7 -6 38.64 1.69 0 -7 6 43.93 2.98 0 7 -5 76.33 3.02 0 7 -5 74.82 2.33 0 -7 5 75.71 3.08 0 7 -4 28.62 2.16 0 -7 4 30.24 1.77 0 -7 4 25.51 1.32 0 7 -3 77.67 3.07 0 -7 3 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1.86 2.09 -5 10 -12 8.40 2.24 5 -10 13 12.05 2.92 -5 10 -13 15.42 2.86 5 -9 -12 3.31 1.80 5 -9 -11 1.01 1.74 5 -9 -10 0.24 1.41 -5 9 10 2.57 1.31 -5 9 10 2.57 1.32 5 -9 -9 2.66 1.27 -5 9 9 -0.09 1.26 -5 9 9 1.36 1.17 5 -9 -8 9.85 1.58 -5 9 8 9.22 1.95 -5 9 8 7.52 1.58 5 -9 -7 15.20 1.80 -5 9 7 17.12 2.26 -5 9 7 14.83 1.86 5 -9 -6 227.31 7.41 -5 9 6 233.45 7.82 -5 9 6 230.20 7.74 5 -9 -5 22.71 1.69 -5 9 5 24.06 2.09 -5 9 5 27.94 2.24 5 -9 -4 17.76 1.53 5 -9 -4 16.58 1.37 -5 9 4 14.44 1.90 5 -9 -3 2.66 1.29 5 -9 -3 3.13 0.76 -5 9 3 5.52 1.35 5 -9 -2 193.41 5.71 5 -9 -2 171.50 4.07 -5 9 2 187.15 6.40 5 -9 -1 100.54 3.64 5 -9 -1 90.72 2.46 -5 9 1 104.40 4.27 5 -9 0 17.83 1.52 -5 9 0 16.05 2.47 5 -9 1 19.94 1.73 -5 9 -1 18.28 1.96 5 -9 2 30.08 2.07 -5 9 -2 28.39 2.38 5 -9 3 10.89 1.59 -5 9 -3 11.17 1.80 5 -9 4 44.18 3.09 -5 9 -4 49.62 3.33 5 -9 5 159.14 5.97 -5 9 -5 167.52 7.33 5 -9 6 30.99 2.44 -5 9 -6 29.54 2.78 5 -9 7 101.80 4.74 -5 9 -7 106.38 5.13 5 -9 8 3.58 1.61 -5 9 -8 2.82 1.60 5 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0 -4 1.91 1.43 -11 0 4 -1.14 1.59 11 0 -3 2.04 1.62 -11 0 3 3.04 1.78 -11 0 2 9.51 1.85 -11 0 2 9.93 2.34 11 0 -1 1.12 1.25 -11 0 1 0.03 1.59 11 0 0 0.19 1.27 -11 0 0 1.49 1.52 11 0 1 1.89 1.66 -11 0 -1 3.12 1.77 11 0 2 0.22 1.47 -11 0 -2 -0.78 1.51 11 0 3 13.63 2.73 -11 0 -3 12.58 2.76 11 1 -7 3.48 2.10 -11 -1 7 5.86 2.33 11 1 -6 71.68 4.82 -11 -1 6 56.81 4.84 11 1 -5 12.78 2.33 -11 -1 5 9.99 2.45 11 1 -4 7.94 2.26 -11 -1 4 8.45 2.41 -11 -1 2 -1.14 1.77 -11 -1 1 7.45 2.36 11 1 0 -0.61 1.61 -11 -1 0 -3.48 1.92 11 1 1 1.83 1.56 -11 -1 -1 0.68 1.84 11 1 2 3.24 2.01 -11 -1 -2 3.61 2.18 11 2 -5 8.69 2.36 11 2 -4 -2.61 1.89 -11 -2 3 -0.83 1.80 -11 -2 2 0.68 1.74 -11 -2 1 0.19 1.61 12 -11 -3 1.56 1.78 12 -11 -2 15.48 2.48 -12 11 2 10.85 2.84 12 -11 -1 3.70 1.64 -12 11 1 -2.40 1.99 12 -11 0 5.94 1.97 -12 11 0 4.99 2.07 12 -11 1 17.05 2.70 -12 11 -1 15.49 3.54 12 -11 2 14.93 2.34 -12 11 -2 5.51 2.69 -12 10 5 11.05 2.94 -12 10 4 3.86 2.26 12 -10 -3 17.70 2.70 12 -10 -2 -1.23 1.44 -12 10 2 2.21 1.34 12 -10 -1 0.08 1.25 -12 10 1 -0.09 1.25 12 -10 0 9.02 2.15 -12 10 0 9.11 2.33 12 -10 1 -0.50 1.25 -12 10 -1 0.72 1.71 12 -10 2 30.23 3.22 -12 10 -2 27.19 3.39 12 -10 3 2.41 2.07 -12 10 -3 5.35 2.20 12 -10 4 9.49 2.50 -12 10 -4 8.57 2.59 -12 9 6 -1.24 1.95 -12 9 5 20.75 3.45 -12 9 4 2.60 2.08 -12 9 3 5.09 2.21 12 -9 -2 1.35 1.72 -12 9 2 3.35 1.45 12 -9 -1 0.80 1.57 -12 9 1 1.56 1.42 12 -9 0 -2.18 1.42 -12 9 0 0.02 1.47 12 -9 1 1.35 1.36 -12 9 -1 -0.44 1.41 12 -9 2 26.04 3.08 -12 9 -2 31.37 3.16 12 -9 3 2.69 1.79 -12 9 -3 5.32 2.04 12 -9 4 0.93 1.65 -12 9 -4 1.64 1.84 12 -9 5 3.07 3.03 -12 9 -5 88.11 4.31 12 -8 -7 0.85 1.27 -12 8 7 1.80 2.11 -12 8 6 27.80 3.93 -12 8 5 8.60 2.66 -12 8 4 -0.85 1.70 -12 8 3 36.76 3.78 -12 8 2 11.09 2.39 -12 8 2 16.81 2.72 12 -8 -1 6.35 1.80 -12 8 1 4.96 1.77 12 -8 0 4.24 1.67 -12 8 0 6.32 1.81 12 -8 1 5.59 2.09 -12 8 -1 2.69 1.76 12 -8 2 3.45 2.06 -12 8 -2 4.62 1.85 12 -8 3 23.24 3.19 -12 8 -3 23.21 3.10 12 -8 4 7.92 2.00 -12 8 -4 7.24 2.22 12 -8 5 39.18 3.52 -12 8 -5 40.29 4.12 12 -7 -8 16.09 2.65 -12 7 8 28.09 3.41 12 -7 -7 4.01 2.15 -12 7 7 7.90 2.40 12 -7 -6 3.38 1.89 -12 7 6 5.99 2.37 12 -7 -5 7.05 2.00 -12 7 5 6.57 2.92 12 -7 -4 15.74 2.36 -12 7 4 18.94 3.08 12 -7 -3 15.51 2.18 -12 7 3 18.49 2.88 -12 7 2 0.55 1.02 -12 7 2 -0.48 1.40 12 -7 -1 -0.40 0.79 -12 7 1 0.59 1.11 12 -7 0 10.18 1.95 -12 7 0 8.55 2.32 12 -7 1 1.85 1.32 -12 7 -1 0.16 1.40 12 -7 2 34.11 2.96 -12 7 -2 30.27 3.33 12 -7 3 45.49 4.15 -12 7 -3 57.79 4.12 12 -7 4 -1.82 1.39 -12 7 -4 0.18 2.06 12 -7 5 -1.72 1.24 -12 7 -5 2.38 1.65 12 -6 -8 27.44 3.11 -12 6 8 28.50 3.99 12 -6 -7 -0.61 1.25 -12 6 7 0.88 1.74 12 -6 -6 5.72 1.78 -12 6 6 8.90 2.57 12 -6 -5 2.67 1.53 -12 6 5 5.79 2.01 12 -6 -4 0.83 1.52 -12 6 4 1.82 1.79 12 -6 -3 1.33 1.12 -12 6 3 -0.58 1.98 12 -6 -2 13.11 2.13 -12 6 2 9.16 2.42 12 -6 -1 42.76 2.79 -12 6 1 43.86 3.60 -12 6 1 42.92 3.60 12 -6 0 7.25 1.70 -12 6 0 4.65 2.04 12 -6 1 8.16 2.10 -12 6 -1 9.57 1.90 12 -6 2 9.24 1.84 -12 6 -2 12.43 2.75 12 -6 3 10.60 1.88 -12 6 -3 12.83 2.89 12 -6 4 13.03 1.98 -12 6 -4 10.62 2.99 -12 6 -5 0.45 2.06 12 -5 -8 17.06 3.45 -12 5 8 22.65 3.54 12 -5 -7 1.23 1.93 -12 5 7 1.16 1.97 12 -5 -6 1.55 1.65 -12 5 6 2.55 1.96 12 -5 -5 0.86 1.30 -12 5 5 0.13 1.75 12 -5 -4 1.63 1.33 -12 5 4 -0.24 1.73 12 -5 -3 10.67 1.80 -12 5 3 10.10 2.98 12 -5 -2 -0.09 1.05 -12 5 2 -0.84 1.40 12 -5 -1 1.86 1.52 -12 5 1 0.93 1.51 12 -5 0 4.65 1.54 12 -5 0 4.31 1.40 -12 5 0 7.67 1.71 12 -5 1 0.81 1.18 12 -5 1 -1.03 1.10 -12 5 -1 0.95 1.19 12 -5 2 1.16 1.17 -12 5 -2 1.00 1.49 12 -5 3 9.99 2.10 -12 5 -3 10.92 2.42 -12 5 -4 0.01 1.72 -12 5 -5 12.26 3.41 12 -4 -8 10.25 2.82 -12 4 8 5.80 2.72 12 -4 -7 2.68 1.62 -12 4 7 0.05 1.95 12 -4 -6 2.42 1.62 -12 4 6 1.34 1.92 12 -4 -5 1.40 1.39 -12 4 5 -0.73 1.95 12 -4 -4 1.29 1.33 -12 4 4 0.41 1.62 12 -4 -3 16.61 2.27 -12 4 3 16.09 3.25 12 -4 -2 17.17 2.26 -12 4 2 18.32 2.51 12 -4 -1 -0.21 0.99 12 -4 -1 0.65 1.00 -12 4 1 -0.93 1.19 12 -4 0 4.87 1.87 12 -4 0 4.54 1.58 12 -4 1 13.80 2.06 12 -4 1 6.40 1.24 12 -4 1 17.34 2.11 12 -4 2 1.88 1.13 12 -4 2 -0.86 1.37 -12 4 -2 1.18 1.32 12 -4 3 3.20 1.76 -12 4 -3 1.64 1.79 12 -4 4 18.65 2.93 12 -3 -8 19.10 3.16 -12 3 8 24.17 3.48 12 -3 -7 4.79 1.92 -12 3 7 0.41 2.09 12 -3 -6 3.52 1.92 -12 3 6 4.78 2.24 12 -3 -5 5.01 2.99 -12 3 5 35.10 3.52 12 -3 -4 0.41 1.44 -12 3 4 3.25 2.11 12 -3 -3 10.95 2.55 -12 3 3 9.54 2.18 12 -3 -2 17.80 2.28 -12 3 2 19.39 2.59 12 -3 -1 -0.77 1.64 -12 3 1 -1.34 1.39 12 -3 0 5.21 1.21 12 -3 0 10.61 2.33 -12 3 0 10.61 1.79 12 -3 1 10.59 2.07 -12 3 -1 9.39 2.17 12 -3 2 4.71 2.21 -12 3 -2 1.79 2.02 12 -3 3 1.85 1.99 -12 3 -3 -0.04 1.70 12 -2 -7 9.42 2.48 12 -2 -6 11.40 2.28 -12 2 6 8.06 2.46 12 -2 -5 9.20 2.23 -12 2 5 10.88 2.44 12 -2 -4 3.12 1.71 -12 2 4 1.04 1.69 12 -2 -3 -0.65 1.41 -12 2 3 -0.28 1.80 12 -2 -2 49.80 3.88 -12 2 2 45.96 4.30 12 -2 -1 16.24 2.28 -12 2 1 14.63 2.22 12 -2 0 9.55 2.29 -12 2 0 6.86 2.69 12 -2 1 -0.47 1.39 -12 2 -1 1.02 1.42 12 -2 2 9.07 2.00 -12 2 -2 1.19 1.90 12 -1 -6 11.27 2.46 -12 1 6 8.31 2.59 12 -1 -5 2.63 2.06 -12 1 5 0.45 2.08 12 -1 -4 0.20 1.48 -12 1 4 -1.46 1.50 12 -1 -3 2.23 1.63 -12 1 3 0.88 1.90 12 -1 -2 16.43 3.06 -12 1 1 9.34 2.96 -12 1 0 2.62 1.85 12 -1 1 2.59 2.57 -12 1 -1 8.41 2.22 -13 8 3 20.61 3.44 13 -8 -2 8.76 2.14 13 -8 -1 -0.73 1.44 13 -8 0 1.23 1.56 -13 8 0 2.38 1.60 13 -8 1 27.28 3.01 -13 8 -1 23.68 3.27 -13 7 4 14.58 2.98 -13 7 3 5.04 2.31 -13 7 2 -1.10 1.85 13 -7 -1 -0.81 1.47 13 -7 0 1.33 1.92 -13 7 0 2.74 1.62 13 -7 1 1.34 1.49 -13 7 -1 1.20 1.52 13 -6 -4 0.12 1.30 -13 6 4 0.24 1.56 -13 6 3 3.16 2.19 -13 6 2 0.52 1.57 13 -6 -1 2.88 1.61 13 -6 0 0.05 1.18 13 -6 1 3.19 1.55 -13 6 -1 2.82 2.16 13 -5 -4 16.73 2.59 -13 5 4 15.66 3.13 13 -5 -3 1.46 1.69 -13 5 3 7.61 2.06 13 -5 -2 3.92 1.70 -13 5 2 3.62 2.05 -13 5 1 11.28 2.29 13 -5 0 26.11 2.66 13 -4 -3 7.40 2.12 -13 4 3 7.67 2.85 13 -4 -2 0.81 1.64 -13 4 2 5.76 1.92 13 -4 -1 20.07 2.81 -13 4 1 15.75 2.74 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 10147 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 O4 O 0.35328(15) 0.05476(13) 0.09077(9) 0.0271(3) Uani 1 1 d . . O7 O 0.11320(12) 0.14386(11) -0.06881(8) 0.0195(3) Uani 1 1 d . . O3 O 0.40849(14) 0.00032(13) -0.10365(9) 0.0260(3) Uani 1 1 d . . O1 O 0.03938(15) 0.15683(13) -0.43080(9) 0.0270(3) Uani 1 1 d . . O5 O 0.17883(15) 0.16402(14) 0.39659(9) 0.0274(3) Uani 1 1 d . . O6 O -0.00814(15) 0.27378(13) 0.38164(9) 0.0276(3) Uani 1 1 d . . O2 O 0.37686(15) 0.01072(14) -0.30471(10) 0.0298(3) Uani 1 1 d . . C9 C 0.18247(18) 0.12430(16) 0.01843(12) 0.0177(3) Uani 1 1 d . . C2 C 0.07294(19) 0.15191(16) -0.24689(12) 0.0201(4) Uani 1 1 d . . H2 H 0.0042 0.1849 -0.2338 0.024 Uiso 1 1 calc R U C6 C 0.24734(18) 0.07437(16) -0.18198(12) 0.0184(3) Uani 1 1 d . . C10 C 0.13392(18) 0.16309(16) 0.11366(12) 0.0176(3) Uani 1 1 d . . C7 C 0.31675(18) 0.04606(16) -0.09501(13) 0.0186(3) Uani 1 1 d . . C4 C 0.20703(19) 0.08420(17) -0.36681(13) 0.0222(4) Uani 1 1 d . . H4 H 0.2277 0.0716 -0.4358 0.027 Uiso 1 1 calc R U N1 N 0.15995(19) 0.75960(17) 0.39455(12) 0.0324(4) Uani 1 1 d . . C8 C 0.28177(18) 0.07560(16) 0.00676(12) 0.0191(4) Uani 1 1 d . . C11 C 0.17951(18) 0.14431(16) 0.21328(12) 0.0185(3) Uani 1 1 d . . H11 H 0.2437 0.1049 0.2201 0.022 Uiso 1 1 calc R U C1 C 0.14506(18) 0.12250(16) -0.16664(12) 0.0169(3) Uani 1 1 d . . N2 N 0.79557(18) 0.36859(16) 0.34805(12) 0.0298(4) Uani 1 1 d . . C14 C -0.01013(19) 0.25805(17) 0.19431(13) 0.0219(4) Uani 1 1 d . . H14 H -0.0746 0.2972 0.1877 0.026 Uiso 1 1 calc R U C12 C 0.13140(18) 0.18292(17) 0.30097(12) 0.0188(3) Uani 1 1 d . . C24 C 0.2373(2) 0.6028(2) 0.32310(15) 0.0314(4) Uani 1 1 d . . H24 H 0.2152 0.5266 0.2742 0.038 Uiso 1 1 calc R U C17 C 0.5682(2) 0.35796(19) 0.26865(16) 0.0315(4) Uani 1 1 d . . H17 H 0.4830 0.3146 0.2161 0.038 Uiso 1 1 calc R U C22 C 0.4834(2) 0.61773(19) 0.39464(15) 0.0273(4) Uani 1 1 d . . C5 C 0.27738(19) 0.05605(17) -0.28562(13) 0.0204(4) Uani 1 1 d . . C21 C 0.4760(2) 0.5154(2) 0.33149(16) 0.0289(4) Uani 1 1 d . . C23 C 0.3719(2) 0.66556(18) 0.39126(14) 0.0249(4) Uani 1 1 d . . C18 C 0.5879(2) 0.46780(18) 0.33836(15) 0.0255(4) Uani 1 1 d . . C3 C 0.10430(19) 0.13167(17) -0.34740(13) 0.0206(4) Uani 1 1 d . . C13 C 0.03551(19) 0.24001(16) 0.29242(13) 0.0194(4) Uani 1 1 d . . C19 C 0.7163(2) 0.52659(19) 0.41278(14) 0.0280(4) Uani 1 1 d . . H19 H 0.7356 0.6019 0.4619 0.034 Uiso 1 1 calc R U C15 C 0.03747(19) 0.21956(17) 0.10638(13) 0.0214(4) Uani 1 1 d . . H15 H 0.0042 0.2316 0.0398 0.026 Uiso 1 1 calc R U C27 C 0.3966(2) 0.77736(19) 0.46033(15) 0.0301(4) Uani 1 1 d . . H27 H 0.4869 0.8240 0.5078 0.036 Uiso 1 1 calc R U C16 C 0.6731(2) 0.31271(19) 0.27634(16) 0.0318(4) Uani 1 1 d . . H16 H 0.6573 0.2379 0.2281 0.038 Uiso 1 1 calc R U C20 C 0.8146(2) 0.4746(2) 0.41439(15) 0.0299(4) Uani 1 1 d . . H20 H 0.9014 0.5163 0.4657 0.036 Uiso 1 1 calc R U C26 C 0.2891(2) 0.8199(2) 0.45930(15) 0.0342(5) Uani 1 1 d . . H26 H 0.3079 0.8960 0.5072 0.041 Uiso 1 1 calc R U C25 C 0.1369(2) 0.6529(2) 0.32769(15) 0.0331(5) Uani 1 1 d . . H25 H 0.0460 0.6091 0.2807 0.040 Uiso 1 1 calc R U O9 O 0.3638(2) 0.5450(2) 0.08366(15) 0.0695(6) Uani 1 1 d . . O8 O 0.1964(2) 0.6054(2) -0.06407(16) 0.0720(6) Uani 1 1 d . . C28 C 0.3849(3) 0.6714(3) 0.0861(2) 0.0681(8) Uani 1 1 d . . H28A H 0.4638 0.7146 0.0457 0.082 Uiso 1 1 calc R U H28B H 0.4174 0.7188 0.1597 0.082 Uiso 1 1 calc R U C29 C 0.2492(4) 0.6771(3) 0.0417(3) 0.0805(10) Uani 1 1 d . . H29A H 0.1726 0.6409 0.0856 0.097 Uiso 1 1 calc R U H29B H 0.2697 0.7682 0.0422 0.097 Uiso 1 1 calc R U C31 C 0.3172(3) 0.4775(3) -0.0222(3) 0.0763(10) Uani 1 1 d . . H31A H 0.2989 0.3866 -0.0245 0.092 Uiso 1 1 calc R U H31B H 0.3960 0.5173 -0.0637 0.092 Uiso 1 1 calc R U C30 C 0.1825(4) 0.4813(3) -0.0686(3) 0.0924(12) Uani 1 1 d . . H30A H 0.1551 0.4369 -0.1430 0.111 Uiso 1 1 calc R U H30B H 0.1017 0.4332 -0.0313 0.111 Uiso 1 1 calc R U H22 H 0.568(2) 0.6674(19) 0.4497(16) 0.030(5) Uiso 1 1 d . . H21 H 0.395(3) 0.469(2) 0.2770(17) 0.041(6) Uiso 1 1 d . . H6O H -0.073(3) 0.306(2) 0.3670(19) 0.056(7) Uiso 1 1 d . . H5O H 0.118(3) 0.168(2) 0.441(2) 0.059(8) Uiso 1 1 d . . H4O H 0.417(3) 0.030(2) 0.0682(19) 0.054(7) Uiso 1 1 d . . H1O H -0.031(3) 0.188(2) -0.414(2) 0.063(8) Uiso 1 1 d . . H2O H 0.407(3) 0.000(2) -0.244(2) 0.053(7) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O4 0.0348(7) 0.0488(8) 0.0145(6) 0.0073(6) 0.0043(5) 0.0339(7) O7 0.0248(6) 0.0310(7) 0.0114(5) 0.0049(5) 0.0045(5) 0.0198(6) O3 0.0330(7) 0.0415(8) 0.0173(6) 0.0051(5) 0.0042(5) 0.0296(7) O1 0.0380(8) 0.0466(8) 0.0149(6) 0.0107(6) 0.0078(5) 0.0339(7) O5 0.0353(7) 0.0487(8) 0.0132(6) 0.0087(6) 0.0064(5) 0.0311(7) O6 0.0391(8) 0.0460(8) 0.0154(6) 0.0064(6) 0.0081(5) 0.0344(7) O2 0.0394(8) 0.0533(9) 0.0170(6) 0.0075(6) 0.0075(6) 0.0387(7) C9 0.0202(8) 0.0217(9) 0.0135(8) 0.0039(6) 0.0018(6) 0.0114(7) C2 0.0249(9) 0.0269(9) 0.0174(8) 0.0054(7) 0.0056(7) 0.0192(8) C6 0.0210(8) 0.0228(9) 0.0144(8) 0.0024(7) 0.0026(6) 0.0129(7) C10 0.0197(8) 0.0201(8) 0.0155(8) 0.0031(7) 0.0042(6) 0.0108(7) C7 0.0198(8) 0.0215(9) 0.0178(8) 0.0023(7) 0.0019(7) 0.0127(7) C4 0.0304(9) 0.0326(10) 0.0132(8) 0.0058(7) 0.0077(7) 0.0216(8) N1 0.0427(10) 0.0514(11) 0.0228(8) 0.0113(8) 0.0101(7) 0.0371(9) C8 0.0231(9) 0.0243(9) 0.0136(8) 0.0045(7) 0.0018(7) 0.0140(8) C11 0.0194(8) 0.0239(9) 0.0179(8) 0.0046(7) 0.0039(7) 0.0146(7) C1 0.0200(8) 0.0209(8) 0.0131(7) 0.0031(6) 0.0054(6) 0.0117(7) N2 0.0344(9) 0.0402(10) 0.0288(8) 0.0094(7) 0.0103(7) 0.0278(8) C14 0.0267(9) 0.0305(10) 0.0190(8) 0.0080(7) 0.0057(7) 0.0210(8) C12 0.0215(8) 0.0245(9) 0.0139(8) 0.0055(7) 0.0027(7) 0.0130(7) C24 0.0312(10) 0.0366(11) 0.0326(10) 0.0017(9) 0.0028(8) 0.0226(9) C17 0.0262(10) 0.0322(11) 0.0364(11) 0.0003(9) 0.0025(8) 0.0155(9) C22 0.0242(9) 0.0328(11) 0.0311(10) 0.0065(8) 0.0042(8) 0.0183(9) C5 0.0250(9) 0.0263(9) 0.0167(8) 0.0018(7) 0.0047(7) 0.0180(8) C21 0.0261(10) 0.0334(11) 0.0309(10) 0.0016(9) 0.0006(8) 0.0187(9) C23 0.0273(9) 0.0311(10) 0.0247(9) 0.0082(8) 0.0076(8) 0.0194(9) C18 0.0251(9) 0.0271(10) 0.0301(10) 0.0059(8) 0.0065(8) 0.0166(8) C3 0.0260(9) 0.0277(9) 0.0144(8) 0.0053(7) 0.0033(7) 0.0176(8) C13 0.0239(9) 0.0228(9) 0.0158(8) 0.0043(7) 0.0058(7) 0.0137(8) C19 0.0305(10) 0.0334(11) 0.0255(9) 0.0005(8) 0.0037(8) 0.0209(9) C15 0.0264(9) 0.0300(10) 0.0150(8) 0.0075(7) 0.0042(7) 0.0182(8) C27 0.0311(10) 0.0354(11) 0.0282(10) 0.0015(8) 0.0026(8) 0.0206(9) C16 0.0346(11) 0.0318(11) 0.0351(11) 0.0023(9) 0.0098(9) 0.0208(9) C20 0.0293(10) 0.0431(12) 0.0253(9) 0.0045(8) 0.0034(8) 0.0241(9) C26 0.0472(12) 0.0430(12) 0.0270(10) 0.0048(9) 0.0080(9) 0.0337(11) C25 0.0312(10) 0.0488(13) 0.0285(10) 0.0063(9) 0.0037(8) 0.0269(10) O9 0.0522(11) 0.0840(15) 0.0603(12) 0.0333(11) -0.0080(9) 0.0171(11) O8 0.0867(15) 0.0776(14) 0.0648(13) 0.0304(11) -0.0015(11) 0.0468(13) C28 0.0556(17) 0.0592(19) 0.0606(18) 0.0004(15) 0.0081(14) 0.0020(15) C29 0.082(2) 0.074(2) 0.095(3) 0.023(2) 0.026(2) 0.039(2) C31 0.076(2) 0.0386(15) 0.091(2) 0.0047(15) -0.0366(18) 0.0167(15) C30 0.095(3) 0.059(2) 0.097(3) 0.0081(18) -0.048(2) 0.0248(19) 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 C8 O4 H4O 107.7(16) C1 O7 C9 122.44(12) C3 O1 H1O 113.4(15) C12 O5 H5O 109.1(16) C13 O6 H6O 110.1(16) C5 O2 H2O 104.6(16) C8 C9 O7 119.29(14) C8 C9 C10 130.01(15) O7 C9 C10 110.70(13) C1 C2 C3 117.83(14) C1 C2 H2 121.1 C3 C2 H2 121.1 C1 C6 C5 117.40(14) C1 C6 C7 119.67(14) C5 C6 C7 122.93(14) C15 C10 C11 118.18(14) C15 C10 C9 119.38(14) C11 C10 C9 122.43(14) O3 C7 C6 122.96(15) O3 C7 C8 119.92(14) C6 C7 C8 117.09(14) C5 C4 C3 119.74(15) C5 C4 H4 120.1 C3 C4 H4 120.1 C26 N1 C25 116.86(16) O4 C8 C9 121.44(15) O4 C8 C7 117.31(14) C9 C8 C7 121.24(14) C12 C11 C10 120.42(14) C12 C11 H11 119.8 C10 C11 H11 119.8 O7 C1 C2 116.76(13) O7 C1 C6 120.13(14) C2 C1 C6 123.11(14) C16 N2 C20 116.59(15) C15 C14 C13 120.57(15) C15 C14 H14 119.7 C13 C14 H14 119.7 O5 C12 C11 118.81(14) O5 C12 C13 120.51(14) C11 C12 C13 120.68(14) C25 C24 C23 119.20(18) C25 C24 H24 120.4 C23 C24 H24 120.4 C16 C17 C18 119.77(18) C16 C17 H17 120.1 C18 C17 H17 120.1 C21 C22 C23 125.88(18) C21 C22 H22 120.1(12) C23 C22 H22 114.0(12) O2 C5 C4 119.50(15) O2 C5 C6 119.82(14) C4 C5 C6 120.68(14) C22 C21 C18 124.69(19) C22 C21 H21 120.0(13) C18 C21 H21 115.3(13) C27 C23 C24 116.99(16) C27 C23 C22 119.76(17) C24 C23 C22 123.23(17) C19 C18 C17 116.75(16) C19 C18 C21 123.20(17) C17 C18 C21 120.04(17) O1 C3 C2 122.31(14) O1 C3 C4 116.45(15) C2 C3 C4 121.24(15) O6 C13 C14 123.78(15) O6 C13 C12 117.20(14) C14 C13 C12 119.01(15) C20 C19 C18 119.36(17) C20 C19 H19 120.3 C18 C19 H19 120.3 C14 C15 C10 121.13(15) C14 C15 H15 119.4 C10 C15 H15 119.4 C26 C27 C23 119.60(18) C26 C27 H27 120.2 C23 C27 H27 120.2 N2 C16 C17 123.46(18) N2 C16 H16 118.3 C17 C16 H16 118.3 N2 C20 C19 124.07(18) N2 C20 H20 118.0 C19 C20 H20 118.0 N1 C26 C27 123.46(18) N1 C26 H26 118.3 C27 C26 H26 118.3 N1 C25 C24 123.88(19) N1 C25 H25 118.1 C24 C25 H25 118.1 C28 O9 C31 108.9(2) C30 O8 C29 110.7(2) O9 C28 C29 112.0(2) O9 C28 H28A 109.2 C29 C28 H28A 109.2 O9 C28 H28B 109.2 C29 C28 H28B 109.2 H28A C28 H28B 107.9 O8 C29 C28 110.5(3) O8 C29 H29A 109.5 C28 C29 H29A 109.5 O8 C29 H29B 109.5 C28 C29 H29B 109.5 H29A C29 H29B 108.1 O9 C31 C30 110.7(3) O9 C31 H31A 109.5 C30 C31 H31A 109.5 O9 C31 H31B 109.5 C30 C31 H31B 109.5 H31A C31 H31B 108.1 O8 C30 C31 113.3(3) O8 C30 H30A 108.9 C31 C30 H30A 108.9 O8 C30 H30B 108.9 C31 C30 H30B 108.9 H30A C30 H30B 107.7 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O4 C8 1.3617(19) O4 H4O 0.87(3) O7 C1 1.3625(18) O7 C9 1.3755(18) O3 C7 1.2650(19) O1 C3 1.347(2) O1 H1O 0.97(3) O5 C12 1.3708(19) O5 H5O 0.90(3) O6 C13 1.3538(19) O6 H6O 0.91(3) O2 C5 1.3561(19) O2 H2O 0.86(3) C9 C8 1.366(2) C9 C10 1.466(2) C2 C1 1.382(2) C2 C3 1.391(2) C2 H2 0.9500 C6 C1 1.396(2) C6 C5 1.422(2) C6 C7 1.426(2) C10 C15 1.399(2) C10 C11 1.411(2) C7 C8 1.442(2) C4 C5 1.373(2) C4 C3 1.405(2) C4 H4 0.9500 N1 C26 1.336(3) N1 C25 1.340(3) C11 C12 1.382(2) C11 H11 0.9500 N2 C16 1.336(3) N2 C20 1.342(2) C14 C15 1.381(2) C14 C13 1.390(2) C14 H14 0.9500 C12 C13 1.401(2) C24 C25 1.379(3) C24 C23 1.397(3) C24 H24 0.9500 C17 C16 1.379(3) C17 C18 1.397(3) C17 H17 0.9500 C22 C21 1.328(3) C22 C23 1.463(2) C22 H22 0.97(2) C21 C18 1.467(2) C21 H21 0.94(2) C23 C27 1.395(3) C18 C19 1.394(3) C19 C20 1.374(2) C19 H19 0.9500 C15 H15 0.9500 C27 C26 1.382(3) C27 H27 0.9500 C16 H16 0.9500 C20 H20 0.9500 C26 H26 0.9500 C25 H25 0.9500 O9 C28 1.390(3) O9 C31 1.423(3) O8 C30 1.384(4) O8 C29 1.438(4) C28 C29 1.479(4) C28 H28A 0.9900 C28 H28B 0.9900 C29 H29A 0.9900 C29 H29B 0.9900 C31 C30 1.467(4) C31 H31A 0.9900 C31 H31B 0.9900 C30 H30A 0.9900 C30 H30B 0.9900