#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/64/1516468.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_1516468 loop_ _publ_author_name 'Li, Chengjie' 'Ulrich, Markus' 'Liu, Xiujun' 'Wurst, Klaus' 'M\"uller, Thomas' 'Kr\"autler, Bernhard' _publ_section_title ; Blue transition metal complexes of a natural bilin-type chlorophyll catabolite ; _journal_issue 9 _journal_name_full 'Chemical Science' _journal_page_first 3388 _journal_paper_doi 10.1039/C4SC00348A _journal_volume 5 _journal_year 2014 _chemical_formula_sum 'C36 H44 K N4 O11.5' _chemical_formula_weight 755.85 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 98.948(4) _cell_angle_beta 100.210(4) _cell_angle_gamma 97.418(3) _cell_formula_units_Z 2 _cell_length_a 11.7592(8) _cell_length_b 12.7470(9) _cell_length_c 13.3933(9) _cell_measurement_reflns_used 41860 _cell_measurement_temperature 233(2) _cell_measurement_theta_max 22.5 _cell_measurement_theta_min 1.0 _cell_volume 1926.2(2) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS86 (Sheldrick, 2008)' _diffrn_ambient_temperature 233(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8392 _diffrn_reflns_theta_full 21.49 _diffrn_reflns_theta_max 21.49 _diffrn_reflns_theta_min 1.57 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_type none _exptl_crystal_colour 'light red' _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 798 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.413 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.059 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 534 _refine_ls_number_reflns 4396 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0769 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+1.9892P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1824 _refine_ls_wR_factor_ref 0.1968 _reflns_number_gt 3127 _reflns_number_total 4396 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL picc in P-1 CELL 0.71073 11.7592 12.7470 13.3933 98.948 100.210 97.418 ZERR 2.00 0.0008 0.0009 0.0009 0.004 0.004 0.003 LATT 1 SFAC C H N O K UNIT 72 88 8 23 2 L.S. 6 ACTA TEMP -40 OMIT 0 43 OMIT 1 0 1 OMIT 0 1 0 OMIT 1 1 0 OMIT 1 2 1 OMIT -1 -1 1 OMIT -2 1 0 OMIT 1 -1 1 OMIT 2 1 2 OMIT 1 -1 4 OMIT 0 -2 1 OMIT 2 -1 2 OMIT 1 -1 3 OMIT 0 -1 3 OMIT 3 -2 1 OMIT 1 0 3 OMIT 1 0 0 OMIT -1 2 0 OMIT -1 1 3 OMIT 0 0 3 OMIT 0 -2 2 OMIT -1 -2 1 OMIT 0 1 2 OMIT 1 -2 1 OMIT -2 -2 1 OMIT -3 -3 3 OMIT 1 1 3 FMAP 2 PLAN 10 BOND 0.5 BOND $H EQIV $1 -X, -Y, -Z DFIX 0.88 0.02 N21 H21N N24 H24N N22 H22N DFIX 0.83 0.02 O33 H33O HTAB N21 O125 HTAB N22 O125 HTAB N24 N23 HTAB N24 O84B HTAB O33 O82_$1 HTAB WGHT 0.087600 1.989200 FVAR 0.35937 PART 0 K125 5 -0.336194 -0.386538 0.556773 11.00000 0.07965 0.08141 = 0.05626 0.00982 0.01358 -0.01159 N21 3 -0.529422 -0.222918 0.064258 11.00000 0.04031 0.05933 = 0.03170 0.00796 0.00891 -0.00710 H21N 2 -0.531810 -0.243776 0.123426 11.00000 0.01635 N22 3 -0.242471 -0.120683 0.227037 11.00000 0.02770 0.05482 = 0.03058 0.00749 0.00434 -0.00451 H22N 2 -0.301021 -0.145294 0.255724 11.00000 0.05213 N23 3 -0.065809 0.144994 0.528565 11.00000 0.03678 0.05622 = 0.03031 -0.00252 0.00737 -0.00456 N24 3 0.098334 0.314208 0.642393 11.00000 0.04340 0.05724 = 0.03799 -0.00519 0.00922 -0.00909 H24N 2 0.082744 0.272590 0.581115 11.00000 0.05304 O33 4 -0.324601 -0.205676 -0.295873 11.00000 0.07029 0.10581 = 0.04642 -0.00087 0.02730 -0.02454 H33O 2 -0.258700 -0.176116 -0.260707 11.00000 0.14114 O82 4 0.117954 0.054776 0.208390 11.00000 0.03812 0.10365 = 0.04503 0.00479 0.01563 -0.01594 O84A 4 -0.064212 0.230122 0.294280 11.00000 0.06995 0.07359 = 0.12621 0.05073 -0.01280 -0.00329 O84B 4 0.109658 0.272279 0.400959 11.00000 0.05677 0.06568 = 0.06618 0.00077 0.00847 -0.01841 O102 4 -0.767085 -0.232601 0.097167 11.00000 0.05734 0.12738 = 0.07335 0.02891 0.02845 0.00370 O124 4 -0.493394 -0.311959 0.395782 11.00000 0.07296 0.07544 = 0.06236 0.01679 0.02110 -0.02877 O125 4 -0.436818 -0.236017 0.270103 11.00000 0.05186 0.07650 = 0.03952 0.01717 -0.00261 -0.01999 O191 4 0.267647 0.418447 0.628090 11.00000 0.06236 0.08589 = 0.05798 -0.00393 0.01789 -0.02049 C1 1 -0.616101 -0.177463 0.012195 11.00000 0.03056 0.06484 = 0.03971 0.00957 0.00056 0.00454 C2 1 -0.572182 -0.136847 -0.066452 11.00000 0.04048 0.04969 = 0.03372 0.00127 0.00423 -0.00129 C3 1 -0.456593 -0.158678 -0.060822 11.00000 0.03386 0.04517 = 0.03200 0.00468 0.00420 -0.00476 C4 1 -0.432950 -0.210704 0.021808 11.00000 0.03062 0.05071 = 0.02831 0.00112 0.00222 -0.00578 C5 1 -0.324355 -0.252412 0.063824 11.00000 0.03897 0.05198 = 0.03175 0.00301 0.00227 -0.00424 AFIX 21 H5A 2 -0.294383 -0.287957 0.005889 11.00000 -1.20000 H5B 2 -0.345094 -0.306888 0.104547 11.00000 -1.20000 AFIX 0 C6 1 -0.227964 -0.167448 0.130436 11.00000 0.03766 0.04530 = 0.03314 0.00751 -0.00075 0.00402 C7 1 -0.124299 -0.121515 0.111243 11.00000 0.02848 0.05840 = 0.03168 0.00428 0.00372 -0.00229 C8 1 -0.073460 -0.044207 0.200541 11.00000 0.02597 0.06319 = 0.03348 0.00884 0.00862 -0.00022 C9 1 -0.147900 -0.044654 0.270374 11.00000 0.02635 0.04635 = 0.03072 0.01106 -0.00538 -0.00051 C10 1 -0.104562 0.033680 0.363631 11.00000 0.02768 0.05599 = 0.03608 0.01458 -0.00050 -0.00080 C11 1 -0.140915 0.065606 0.452992 11.00000 0.03494 0.05684 = 0.03048 0.00860 0.00746 -0.00206 C12 1 -0.249744 0.033088 0.489778 11.00000 0.03297 0.05032 = 0.04472 0.01278 0.00748 -0.00088 C13 1 -0.234704 0.090672 0.587385 11.00000 0.03218 0.06039 = 0.04044 0.00235 0.00875 -0.00230 C14 1 -0.120418 0.160384 0.607464 11.00000 0.03759 0.05929 = 0.03769 0.00265 0.00766 0.00035 C15 1 -0.071440 0.237767 0.700419 11.00000 0.04225 0.07738 = 0.03105 -0.00032 0.00647 0.00094 AFIX 41 H15 2 -0.112244 0.239951 0.754849 11.00000 -1.20000 AFIX 0 C16 1 0.028882 0.307169 0.714526 11.00000 0.03545 0.05514 = 0.03455 0.00244 0.00625 0.00313 C17 1 0.086398 0.388641 0.804967 11.00000 0.05455 0.05471 = 0.03891 0.00535 0.00946 0.01413 C18 1 0.186420 0.438253 0.785012 11.00000 0.05051 0.04852 = 0.04051 -0.00101 0.00018 0.00152 C19 1 0.194738 0.392933 0.678525 11.00000 0.04779 0.05091 = 0.04780 0.00569 0.00633 -0.00217 C21 1 -0.637273 -0.083316 -0.145513 11.00000 0.05534 0.07909 = 0.05336 0.01718 0.00005 0.01127 AFIX 137 H21A 2 -0.652139 -0.129609 -0.212699 11.00000 -1.50000 H21B 2 -0.590711 -0.015429 -0.147726 11.00000 -1.50000 H21C 2 -0.711110 -0.070254 -0.127297 11.00000 -1.50000 AFIX 0 C31 1 -0.378180 -0.132489 -0.132988 11.00000 0.04646 0.05447 = 0.04222 0.00724 0.00529 -0.01274 AFIX 21 H31A 2 -0.296788 -0.115163 -0.095136 11.00000 -1.20000 H31B 2 -0.398358 -0.069092 -0.160838 11.00000 -1.20000 AFIX 0 C32 1 -0.389661 -0.225253 -0.220290 11.00000 0.06322 0.09439 = 0.05265 -0.00191 0.03083 -0.01815 AFIX 21 H32A 2 -0.365185 -0.286835 -0.191538 11.00000 -1.20000 H32B 2 -0.472480 -0.245557 -0.253752 11.00000 -1.20000 AFIX 0 C71 1 -0.071431 -0.149166 0.018228 11.00000 0.04670 0.09829 = 0.04414 0.00263 0.01312 -0.00259 AFIX 137 H71A 2 -0.118896 -0.212418 -0.027033 11.00000 -1.50000 H71B 2 0.007246 -0.163702 0.040038 11.00000 -1.50000 H71C 2 -0.068509 -0.089229 -0.018373 11.00000 -1.50000 AFIX 0 C81 1 0.031315 0.032984 0.244621 11.00000 0.02656 0.06854 = 0.03538 0.01457 0.00314 -0.00171 C82 1 0.016261 0.088035 0.350969 11.00000 0.02922 0.06221 = 0.03134 0.01496 0.00401 -0.00013 AFIX 11 H82 2 0.078041 0.073067 0.404992 11.00000 -1.20000 AFIX 0 C83 1 0.027673 0.206486 0.354636 11.00000 0.04297 0.06656 = 0.04995 0.01996 0.00856 -0.00100 C85 1 -0.060898 0.342929 0.283587 11.00000 0.13910 0.09688 = 0.24510 0.09288 -0.01122 0.01998 AFIX 31 H85A 2 -0.132754 0.350930 0.239193 11.00000 -1.50000 H85B 2 0.005340 0.365406 0.253488 11.00000 -1.50000 H85C 2 -0.053083 0.387228 0.350991 11.00000 -1.50000 AFIX 0 C101 1 -0.731491 -0.185846 0.033545 11.00000 0.04067 0.08994 = 0.05042 0.00036 0.00946 0.00426 AFIX 41 H101 2 -0.785129 -0.151823 -0.005496 11.00000 -1.20000 AFIX 0 C121 1 -0.352181 -0.046862 0.430911 11.00000 0.03188 0.06492 = 0.03934 0.00841 0.00707 -0.00501 AFIX 21 H12A 2 -0.363247 -0.040913 0.357861 11.00000 -1.20000 H12B 2 -0.422486 -0.029739 0.455506 11.00000 -1.20000 AFIX 0 C122 1 -0.339242 -0.160805 0.440773 11.00000 0.05426 0.06078 = 0.03725 0.01125 0.00110 -0.00911 AFIX 21 H12C 2 -0.345762 -0.171027 0.510683 11.00000 -1.20000 H12D 2 -0.261057 -0.173047 0.430962 11.00000 -1.20000 AFIX 0 C123 1 -0.430546 -0.243322 0.363204 11.00000 0.04977 0.06090 = 0.04868 0.02048 0.00665 -0.00451 C131 1 -0.316143 0.088256 0.661039 11.00000 0.03940 0.08860 = 0.05655 0.00038 0.01842 -0.00388 AFIX 137 H13A 2 -0.348469 0.154673 0.667788 11.00000 -1.50000 H13B 2 -0.273724 0.080704 0.727903 11.00000 -1.50000 H13C 2 -0.379161 0.027819 0.635292 11.00000 -1.50000 AFIX 0 C171 1 0.039085 0.409500 0.901086 11.00000 0.07864 0.08979 = 0.04792 -0.01354 0.01631 -0.00399 AFIX 137 H17A 2 0.103354 0.428150 0.960406 11.00000 -1.50000 H17B 2 -0.011706 0.345404 0.906935 11.00000 -1.50000 H17C 2 -0.005174 0.468517 0.898447 11.00000 -1.50000 AFIX 0 C181 1 0.274131 0.522529 0.854381 11.00000 0.07818 0.06030 = 0.05585 -0.00066 0.00671 -0.00480 AFIX 41 H18A 2 0.253840 0.553663 0.915800 11.00000 -1.20000 AFIX 0 C182 1 0.375316 0.557960 0.839862 11.00000 0.10560 0.10768 = 0.07186 -0.01346 0.01118 -0.04832 AFIX 91 H18B 2 0.399772 0.529449 0.779629 11.00000 -1.20000 H18C 2 0.425402 0.612571 0.889399 11.00000 -1.20000 AFIX 0 PART 1 O1 4 -0.599859 -0.384392 0.540735 10.50000 0.08973 0.07827 = 0.12900 0.00355 0.03427 -0.00119 C22 1 -0.697912 -0.345271 0.519673 10.50000 0.24077 0.09078 = 0.15952 0.04277 0.05822 -0.05078 O3 4 -0.495712 -0.523745 0.374596 10.50000 0.19402 0.15090 = 0.21153 -0.03560 0.12117 -0.06769 O4 4 -0.200350 -0.478406 0.759081 10.50000 0.02811 0.11796 = 0.16830 0.11901 -0.02518 -0.01941 O5 4 -0.364521 -0.516651 0.886109 10.50000 0.18120 0.01934 = 0.02963 -0.00768 0.01725 -0.01084 PART 2 O2 4 -0.358984 -0.508244 0.711842 10.50000 0.11033 0.08924 = 0.08014 0.01064 0.01129 -0.02666 C23 1 -0.297323 -0.554321 0.801809 10.50000 0.05735 0.21370 = 0.03886 0.04875 -0.02921 0.01524 O6 4 -0.678700 -0.297614 0.585952 10.50000 0.13373 0.18101 = 0.16751 0.05284 -0.04489 -0.01889 O7 4 -0.849280 -0.436108 0.459123 10.50000 0.15883 0.13022 = 0.21156 0.03844 -0.04243 0.03138 HKLF 4 REM p in P-1 REM R1 = 0.0769 for 3127 Fo > 4sig(Fo) and 0.1111 for all 4396 data REM 534 parameters refined using 4 restraints END WGHT 0.0876 1.9890 REM Highest difference peak 0.413, deepest hole -0.227, 1-sigma level 0.059 Q1 1 -0.2454 -0.4846 0.8172 11.00000 0.05 0.41 Q2 1 -0.2939 -0.4933 0.8568 11.00000 0.05 0.35 Q3 1 -0.3354 -0.5200 0.8216 11.00000 0.05 0.32 Q4 1 -0.2764 -0.5980 0.8246 11.00000 0.05 0.32 Q5 1 -0.3035 -0.5838 0.7644 11.00000 0.05 0.32 Q6 1 -0.3498 -0.5402 0.9032 11.00000 0.05 0.28 Q7 1 -0.1966 -0.5173 0.7256 11.00000 0.05 0.28 Q8 1 -0.7595 -0.3513 0.5534 11.00000 0.05 0.28 Q9 1 -0.1661 -0.4485 0.7991 11.00000 0.05 0.28 Q10 1 -0.6656 -0.4039 0.4941 11.00000 0.05 0.28 ; _cod_data_source_file c4sc00348a2.cif _cod_data_source_block PiCC _cod_depositor_comments 'Adding full bibliography for 1516468.cif.' _cod_original_formula_sum 'C36 H44 K N4 O11.50' _cod_database_code 1516468 loop_ _symmetry_equiv_pos_as_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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K125 K -0.33619(13) -0.38654(13) 0.55677(11) 0.0750(5) Uani 1 1 d . . . N21 N -0.5294(4) -0.2229(4) 0.0643(3) 0.0450(12) Uani 1 1 d D . . H21N H -0.532(3) -0.244(3) 0.123(2) 0.016(11) Uiso 1 1 d D . . N22 N -0.2425(3) -0.1207(4) 0.2270(3) 0.0389(11) Uani 1 1 d D . . H22N H -0.301(3) -0.145(4) 0.256(4) 0.052(16) Uiso 1 1 d D . . N23 N -0.0658(3) 0.1450(4) 0.5286(3) 0.0433(11) Uani 1 1 d . . . N24 N 0.0983(4) 0.3142(4) 0.6424(4) 0.0492(12) Uani 1 1 d D . . H24N H 0.083(4) 0.273(4) 0.581(2) 0.053(17) Uiso 1 1 d D . . O33 O -0.3246(4) -0.2057(4) -0.2959(3) 0.0774(14) Uani 1 1 d D . . H33O H -0.259(4) -0.176(7) -0.261(6) 0.14(4) Uiso 1 1 d D . . O82 O 0.1180(3) 0.0548(4) 0.2084(3) 0.0648(12) Uani 1 1 d . . . O84A O -0.0642(4) 0.2301(4) 0.2943(4) 0.0918(16) Uani 1 1 d . . . O84B O 0.1097(4) 0.2723(3) 0.4010(3) 0.0672(12) Uani 1 1 d . . . O102 O -0.7671(4) -0.2326(4) 0.0972(4) 0.0840(15) Uani 1 1 d . . . O124 O -0.4934(4) -0.3120(4) 0.3958(3) 0.0726(13) Uani 1 1 d . . . O125 O -0.4368(3) -0.2360(3) 0.2701(3) 0.0595(11) Uani 1 1 d . . . O191 O 0.2676(4) 0.4184(4) 0.6281(3) 0.0728(13) Uani 1 1 d . . . C1 C -0.6161(4) -0.1775(5) 0.0122(4) 0.0461(14) Uani 1 1 d . . . C2 C -0.5722(4) -0.1368(4) -0.0665(4) 0.0432(14) Uani 1 1 d . . . C3 C -0.4566(4) -0.1587(4) -0.0608(4) 0.0386(13) Uani 1 1 d . . . C4 C -0.4330(4) -0.2107(4) 0.0218(4) 0.0388(13) Uani 1 1 d . . . C5 C -0.3244(4) -0.2524(4) 0.0638(4) 0.0431(14) Uani 1 1 d . . . H5A H -0.2944 -0.2880 0.0059 0.052 Uiso 1 1 calc . . . H5B H -0.3451 -0.3069 0.1045 0.052 Uiso 1 1 calc . . . C6 C -0.2280(4) -0.1674(4) 0.1304(4) 0.0399(13) Uani 1 1 d . . . C7 C -0.1243(4) -0.1215(4) 0.1112(4) 0.0411(14) Uani 1 1 d . . . C8 C -0.0735(4) -0.0442(4) 0.2005(4) 0.0412(14) Uani 1 1 d . . . C9 C -0.1479(4) -0.0447(4) 0.2704(4) 0.0360(13) Uani 1 1 d . . . C10 C -0.1046(4) 0.0337(4) 0.3636(4) 0.0408(14) Uani 1 1 d . . . C11 C -0.1409(4) 0.0656(4) 0.4530(4) 0.0414(14) Uani 1 1 d . . . C12 C -0.2497(4) 0.0331(4) 0.4898(4) 0.0430(14) Uani 1 1 d . . . C13 C -0.2347(4) 0.0907(5) 0.5874(4) 0.0458(14) Uani 1 1 d . . . C14 C -0.1204(4) 0.1604(5) 0.6075(4) 0.0462(15) Uani 1 1 d . . . C15 C -0.0714(5) 0.2378(5) 0.7004(4) 0.0523(16) Uani 1 1 d . . . H15 H -0.1122 0.2400 0.7548 0.063 Uiso 1 1 calc . . . C16 C 0.0289(4) 0.3072(4) 0.7145(4) 0.0428(14) Uani 1 1 d . . . C17 C 0.0864(5) 0.3886(5) 0.8050(4) 0.0493(15) Uani 1 1 d . . . C18 C 0.1864(5) 0.4383(5) 0.7850(4) 0.0492(15) Uani 1 1 d . . . C19 C 0.1947(5) 0.3929(5) 0.6785(4) 0.0505(15) Uani 1 1 d . . . C21 C -0.6373(5) -0.0833(5) -0.1455(4) 0.0634(18) Uani 1 1 d . . . H21A H -0.6521 -0.1296 -0.2127 0.095 Uiso 1 1 calc R . . H21B H -0.5907 -0.0154 -0.1477 0.095 Uiso 1 1 calc R . . H21C H -0.7111 -0.0703 -0.1273 0.095 Uiso 1 1 calc R . . C31 C -0.3782(5) -0.1325(5) -0.1330(4) 0.0502(15) Uani 1 1 d . . . H31A H -0.2968 -0.1152 -0.0951 0.060 Uiso 1 1 calc . . . H31B H -0.3984 -0.0691 -0.1608 0.060 Uiso 1 1 calc . . . C32 C -0.3897(5) -0.2253(6) -0.2203(5) 0.072(2) Uani 1 1 d . . . H32A H -0.3652 -0.2868 -0.1915 0.087 Uiso 1 1 calc . . . H32B H -0.4725 -0.2456 -0.2538 0.087 Uiso 1 1 calc . . . C71 C -0.0714(5) -0.1492(6) 0.0182(4) 0.0650(18) Uani 1 1 d . . . H71A H -0.1189 -0.2124 -0.0270 0.097 Uiso 1 1 calc R . . H71B H 0.0072 -0.1637 0.0400 0.097 Uiso 1 1 calc R . . H71C H -0.0685 -0.0892 -0.0184 0.097 Uiso 1 1 calc R . . C81 C 0.0313(4) 0.0330(5) 0.2446(4) 0.0442(14) Uani 1 1 d . . . C82 C 0.0163(4) 0.0880(5) 0.3510(4) 0.0412(14) Uani 1 1 d . . . H82 H 0.0780 0.0731 0.4050 0.049 Uiso 1 1 calc . . . C83 C 0.0277(5) 0.2065(5) 0.3546(5) 0.0531(16) Uani 1 1 d . . . C85 C -0.0609(9) 0.3429(8) 0.2836(10) 0.160(5) Uani 1 1 d . . . H85A H -0.1328 0.3509 0.2392 0.240 Uiso 1 1 calc . . . H85B H 0.0053 0.3654 0.2535 0.240 Uiso 1 1 calc . . . H85C H -0.0531 0.3872 0.3510 0.240 Uiso 1 1 calc . . . C101 C -0.7315(5) -0.1858(6) 0.0335(5) 0.0622(17) Uani 1 1 d . . . H101 H -0.7851 -0.1518 -0.0055 0.075 Uiso 1 1 calc . . . C121 C -0.3522(4) -0.0469(5) 0.4309(4) 0.0467(15) Uani 1 1 d . . . H12A H -0.3632 -0.0409 0.3579 0.056 Uiso 1 1 calc . . . H12B H -0.4225 -0.0297 0.4555 0.056 Uiso 1 1 calc . . . C122 C -0.3392(5) -0.1608(5) 0.4408(4) 0.0532(16) Uani 1 1 d . . . H12C H -0.3458 -0.1710 0.5107 0.064 Uiso 1 1 calc . . . H12D H -0.2611 -0.1730 0.4310 0.064 Uiso 1 1 calc . . . C123 C -0.4305(5) -0.2433(5) 0.3632(5) 0.0536(16) Uani 1 1 d . . . C131 C -0.3161(5) 0.0883(6) 0.6610(4) 0.0631(18) Uani 1 1 d . . . H13A H -0.3485 0.1547 0.6678 0.095 Uiso 1 1 calc R . . H13B H -0.2737 0.0807 0.7279 0.095 Uiso 1 1 calc R . . H13C H -0.3792 0.0278 0.6353 0.095 Uiso 1 1 calc R . . C171 C 0.0391(6) 0.4095(6) 0.9011(5) 0.076(2) Uani 1 1 d . . . H17A H 0.1034 0.4282 0.9604 0.114 Uiso 1 1 calc R . . H17B H -0.0117 0.3454 0.9069 0.114 Uiso 1 1 calc R . . H17C H -0.0052 0.4685 0.8984 0.114 Uiso 1 1 calc R . . C181 C 0.2741(6) 0.5225(5) 0.8544(5) 0.0683(18) Uani 1 1 d . . . H18A H 0.2538 0.5537 0.9158 0.082 Uiso 1 1 calc . . . C182 C 0.3753(8) 0.5580(7) 0.8399(6) 0.105(3) Uani 1 1 d . . . H18B H 0.3998 0.5294 0.7796 0.126 Uiso 1 1 calc . . . H18C H 0.4254 0.6126 0.8894 0.126 Uiso 1 1 calc . . . O1 O -0.5999(11) -0.3844(10) 0.5407(11) 0.100(4) Uani 0.50 1 d P . 1 C22 C -0.698(4) -0.345(2) 0.520(3) 0.166(14) Uani 0.50 1 d P . 1 O3 O -0.4957(15) -0.5237(13) 0.3746(14) 0.192(8) Uani 0.50 1 d P . 1 O4 O -0.2004(6) -0.4784(8) 0.7591(9) 0.103(4) Uani 0.50 1 d P . 1 O5 O -0.3645(10) -0.5167(6) 0.8861(6) 0.081(3) Uani 0.50 1 d P A 1 O2 O -0.3590(9) -0.5082(8) 0.7118(8) 0.099(3) Uani 0.50 1 d P . 2 C23 C -0.2973(11) -0.5543(17) 0.8018(10) 0.106(6) Uani 0.50 1 d P . 2 O6 O -0.6787(18) -0.2976(19) 0.5860(17) 0.172(10) Uani 0.50 1 d P B 2 O7 O -0.8493(14) -0.4361(12) 0.4591(13) 0.175(7) Uani 0.50 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K125 0.0796(10) 0.0814(11) 0.0563(9) 0.0098(8) 0.0136(8) -0.0116(8) N21 0.040(3) 0.059(3) 0.032(3) 0.008(2) 0.009(2) -0.007(2) N22 0.028(2) 0.055(3) 0.031(3) 0.007(2) 0.004(2) -0.005(2) N23 0.037(2) 0.056(3) 0.030(3) -0.003(2) 0.007(2) -0.005(2) N24 0.043(3) 0.057(3) 0.038(3) -0.005(3) 0.009(2) -0.009(3) O33 0.070(3) 0.106(4) 0.046(3) -0.001(3) 0.027(2) -0.025(3) O82 0.038(2) 0.104(3) 0.045(2) 0.005(2) 0.0156(19) -0.016(2) O84A 0.070(3) 0.074(4) 0.126(4) 0.051(3) -0.013(3) -0.003(3) O84B 0.057(3) 0.066(3) 0.066(3) 0.001(2) 0.008(2) -0.018(2) O102 0.057(3) 0.127(4) 0.073(3) 0.029(3) 0.028(2) 0.004(3) O124 0.073(3) 0.075(3) 0.062(3) 0.017(2) 0.021(2) -0.029(2) O125 0.052(2) 0.076(3) 0.040(2) 0.017(2) -0.0026(19) -0.020(2) O191 0.062(3) 0.086(3) 0.058(3) -0.004(2) 0.018(2) -0.020(2) C1 0.031(3) 0.065(4) 0.040(3) 0.010(3) 0.001(3) 0.005(3) C2 0.040(3) 0.050(4) 0.034(3) 0.001(3) 0.004(3) -0.001(3) C3 0.034(3) 0.045(3) 0.032(3) 0.005(3) 0.004(2) -0.005(3) C4 0.031(3) 0.051(4) 0.028(3) 0.001(3) 0.002(2) -0.006(3) C5 0.039(3) 0.052(4) 0.032(3) 0.003(3) 0.002(2) -0.004(3) C6 0.038(3) 0.045(3) 0.033(3) 0.008(3) -0.001(2) 0.004(3) C7 0.028(3) 0.058(4) 0.032(3) 0.004(3) 0.004(2) -0.002(3) C8 0.026(3) 0.063(4) 0.033(3) 0.009(3) 0.009(3) 0.000(3) C9 0.026(3) 0.046(3) 0.031(3) 0.011(3) -0.005(2) -0.001(3) C10 0.028(3) 0.056(4) 0.036(3) 0.015(3) 0.000(2) -0.001(3) C11 0.035(3) 0.057(4) 0.030(3) 0.009(3) 0.007(3) -0.002(3) C12 0.033(3) 0.050(4) 0.045(4) 0.013(3) 0.007(3) -0.001(3) C13 0.032(3) 0.060(4) 0.040(3) 0.002(3) 0.009(3) -0.002(3) C14 0.038(3) 0.059(4) 0.038(3) 0.003(3) 0.008(3) 0.000(3) C15 0.042(3) 0.077(4) 0.031(3) 0.000(3) 0.006(3) 0.001(3) C16 0.035(3) 0.055(4) 0.035(3) 0.002(3) 0.006(3) 0.003(3) C17 0.055(4) 0.055(4) 0.039(3) 0.005(3) 0.009(3) 0.014(3) C18 0.051(4) 0.049(4) 0.041(4) -0.001(3) 0.000(3) 0.002(3) C19 0.048(4) 0.051(4) 0.048(4) 0.006(3) 0.006(3) -0.002(3) C21 0.055(4) 0.079(5) 0.053(4) 0.017(3) 0.000(3) 0.011(3) C31 0.046(3) 0.054(4) 0.042(3) 0.007(3) 0.005(3) -0.013(3) C32 0.063(4) 0.094(5) 0.053(4) -0.002(4) 0.031(3) -0.018(4) C71 0.047(3) 0.098(5) 0.044(4) 0.003(3) 0.013(3) -0.003(3) C81 0.027(3) 0.069(4) 0.035(3) 0.015(3) 0.003(3) -0.002(3) C82 0.029(3) 0.062(4) 0.031(3) 0.015(3) 0.004(2) 0.000(3) C83 0.043(4) 0.067(5) 0.050(4) 0.020(3) 0.009(3) -0.001(4) C85 0.139(8) 0.097(8) 0.245(14) 0.093(9) -0.011(8) 0.020(6) C101 0.041(4) 0.090(5) 0.050(4) 0.000(4) 0.009(3) 0.004(3) C121 0.032(3) 0.065(4) 0.039(3) 0.008(3) 0.007(2) -0.005(3) C122 0.054(4) 0.061(4) 0.037(3) 0.011(3) 0.001(3) -0.009(3) C123 0.050(4) 0.061(4) 0.049(4) 0.020(3) 0.007(3) -0.005(3) C131 0.039(3) 0.089(5) 0.057(4) 0.000(3) 0.018(3) -0.004(3) C171 0.079(5) 0.090(5) 0.048(4) -0.014(4) 0.016(3) -0.004(4) C181 0.078(5) 0.060(4) 0.056(4) -0.001(3) 0.007(4) -0.005(4) C182 0.106(6) 0.108(7) 0.072(5) -0.013(5) 0.011(5) -0.048(5) O1 0.090(8) 0.078(9) 0.129(10) 0.004(7) 0.034(8) -0.001(7) C22 0.24(4) 0.09(2) 0.16(3) 0.04(2) 0.06(3) -0.05(2) O3 0.194(16) 0.151(13) 0.212(17) -0.036(13) 0.121(15) -0.068(13) O4 0.028(4) 0.118(8) 0.168(10) 0.119(8) -0.025(5) -0.019(5) O5 0.181(10) 0.019(4) 0.030(4) -0.008(3) 0.017(5) -0.011(5) O2 0.110(8) 0.089(7) 0.080(7) 0.011(6) 0.011(6) -0.027(6) C23 0.057(8) 0.21(2) 0.039(8) 0.049(10) -0.029(7) 0.015(10) O6 0.134(13) 0.18(2) 0.168(19) 0.053(15) -0.045(14) -0.019(14) O7 0.159(12) 0.130(12) 0.212(17) 0.038(11) -0.042(12) 0.031(10) 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O3 K125 O191 133.6(4) 2_446 2_556 O3 K125 O33 88.3(4) 2_446 1_556 O191 K125 O33 133.22(14) 2_556 1_556 O3 K125 O84B 147.9(5) 2_446 2_556 O191 K125 O84B 76.06(12) 2_556 2_556 O33 K125 O84B 71.63(13) 1_556 2_556 O3 K125 O2 43.9(6) 2_446 . O191 K125 O2 135.5(3) 2_556 . O33 K125 O2 87.3(2) 1_556 . O84B K125 O2 108.7(2) 2_556 . O3 K125 O124 93.2(5) 2_446 . O191 K125 O124 68.07(13) 2_556 . O33 K125 O124 94.25(15) 1_556 . O84B K125 O124 112.49(12) 2_556 . O2 K125 O124 137.1(2) . . O3 K125 O1 69.5(4) 2_446 2_446 O191 K125 O1 70.1(3) 2_556 2_446 O33 K125 O1 156.6(3) 1_556 2_446 O84B K125 O1 124.1(3) 2_556 2_446 O2 K125 O1 71.6(3) . 2_446 O124 K125 O1 94.5(3) . 2_446 O3 K125 O3 74.5(5) 2_446 . O191 K125 O3 60.0(3) 2_556 . O33 K125 O3 141.5(4) 1_556 . O84B K125 O3 136.1(3) 2_556 . O2 K125 O3 102.1(4) . . O124 K125 O3 53.8(4) . . O1 K125 O3 40.7(5) 2_446 . O3 K125 O1 41.6(6) 2_446 . O191 K125 O1 114.5(3) 2_556 . O33 K125 O1 81.2(3) 1_556 . O84B K125 O1 148.7(3) 2_556 . O2 K125 O1 84.7(4) . . O124 K125 O1 53.4(3) . . O1 K125 O1 86.7(4) 2_446 . O3 K125 O1 62.9(4) . . O3 K125 O4 76.7(5) 2_446 . O191 K125 O4 121.1(2) 2_556 . O33 K125 O4 82.7(2) 1_556 . O84B K125 O4 76.11(15) 2_556 . O2 K125 O4 33.1(2) . . O124 K125 O4 169.56(18) . . O1 K125 O4 84.8(4) 2_446 . O3 K125 O4 124.5(4) . . O1 K125 O4 116.2(3) . . O3 K125 O7 105.8(6) 2_446 2_446 O191 K125 O7 66.4(3) 2_556 2_446 O33 K125 O7 129.9(3) 1_556 2_446 O84B K125 O7 71.9(3) 2_556 2_446 O2 K125 O7 73.3(4) . 2_446 O124 K125 O7 131.3(3) . 2_446 O1 K125 O7 54.3(4) 2_446 2_446 O3 K125 O7 88.4(5) . 2_446 O1 K125 O7 139.3(4) . 2_446 O4 K125 O7 55.9(4) . 2_446 O3 K125 C122 125.6(5) 2_446 . O191 K125 C122 67.92(14) 2_556 . O33 K125 C122 70.25(14) 1_556 . O84B K125 C122 71.51(13) 2_556 . O2 K125 C122 156.5(3) . . O124 K125 C122 42.71(12) . . O1 K125 C122 128.7(3) 2_446 . O3 K125 C122 91.9(4) . . O1 K125 C122 85.0(3) . . O4 K125 C122 142.83(18) . . O7 K125 C122 126.5(3) 2_446 . C4 N21 C1 109.7(4) . . C4 N21 H21N 125(3) . . C1 N21 H21N 124(3) . . C9 N22 C6 108.3(4) . . C9 N22 H22N 128(3) . . C6 N22 H22N 123(3) . . C14 N23 C11 106.0(4) . . C19 N24 C16 111.6(5) . . C19 N24 H24N 125(3) . . C16 N24 H24N 124(3) . . C32 O33 K125 112.8(4) . 1_554 C32 O33 H33O 103(6) . . K125 O33 H33O 118(7) 1_554 . C83 O84A C85 116.7(6) . . C83 O84B K125 156.9(4) . 2_556 C123 O124 K125 106.1(3) . . C19 O191 K125 147.0(4) . 2_556 N21 C1 C2 107.1(4) . . N21 C1 C101 122.5(5) . . C2 C1 C101 130.0(5) . . C1 C2 C3 107.8(5) . . C1 C2 C21 126.1(5) . . C3 C2 C21 126.0(5) . . C4 C3 C2 106.6(4) . . C4 C3 C31 127.6(5) . . C2 C3 C31 125.8(5) . . N21 C4 C3 108.8(4) . . N21 C4 C5 121.2(4) . . C3 C4 C5 130.0(4) . . C4 C5 C6 114.5(4) . . C4 C5 H5A 108.6 . . C6 C5 H5A 108.6 . . C4 C5 H5B 108.6 . . C6 C5 H5B 108.6 . . H5A C5 H5B 107.6 . . C7 C6 N22 110.2(4) . . C7 C6 C5 130.9(5) . . N22 C6 C5 118.8(4) . . C6 C7 C8 105.0(4) . . C6 C7 C71 128.5(5) . . C8 C7 C71 126.5(4) . . C9 C8 C7 109.2(4) . . C9 C8 C81 109.7(4) . . C7 C8 C81 141.1(4) . . N22 C9 C8 107.3(4) . . N22 C9 C10 139.2(4) . . C8 C9 C10 113.4(4) . . C11 C10 C9 137.0(5) . . C11 C10 C82 118.2(5) . . C9 C10 C82 104.8(4) . . C10 C11 N23 117.9(4) . . C10 C11 C12 132.6(5) . . N23 C11 C12 109.6(4) . . C13 C12 C11 105.8(4) . . C13 C12 C121 128.1(5) . . C11 C12 C121 126.0(5) . . C12 C13 C14 106.3(4) . . C12 C13 C131 128.7(5) . . C14 C13 C131 125.0(5) . . N23 C14 C15 122.8(4) . . N23 C14 C13 112.2(5) . . C15 C14 C13 124.9(5) . . C16 C15 C14 124.3(5) . . C16 C15 H15 117.8 . . C14 C15 H15 117.8 . . C15 C16 N24 124.8(5) . . C15 C16 C17 128.9(5) . . N24 C16 C17 106.2(4) . . C18 C17 C16 108.2(5) . . C18 C17 C171 127.8(5) . . C16 C17 C171 123.9(5) . . C17 C18 C181 127.5(5) . . C17 C18 C19 108.3(5) . . C181 C18 C19 124.1(5) . . O191 C19 N24 124.6(5) . . O191 C19 C18 129.8(5) . . N24 C19 C18 105.5(5) . . C2 C21 H21A 109.5 . . C2 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . C2 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C3 C31 C32 111.1(4) . . C3 C31 H31A 109.4 . . C32 C31 H31A 109.4 . . C3 C31 H31B 109.4 . . C32 C31 H31B 109.4 . . H31A C31 H31B 108.0 . . O33 C32 C31 115.2(5) . . O33 C32 H32A 108.5 . . C31 C32 H32A 108.5 . . O33 C32 H32B 108.5 . . C31 C32 H32B 108.5 . . H32A C32 H32B 107.5 . . C7 C71 H71A 109.5 . . C7 C71 H71B 109.5 . . H71A C71 H71B 109.5 . . C7 C71 H71C 109.5 . . H71A C71 H71C 109.5 . . H71B C71 H71C 109.5 . . O82 C81 C8 129.3(5) . . O82 C81 C82 123.7(5) . . C8 C81 C82 107.0(4) . . C83 C82 C81 109.3(4) . . C83 C82 C10 114.7(5) . . C81 C82 C10 105.1(4) . . C83 C82 H82 109.2 . . C81 C82 H82 109.2 . . C10 C82 H82 109.2 . . O84B C83 O84A 123.5(6) . . O84B C83 C82 125.9(6) . . O84A C83 C82 110.5(5) . . O84A C85 H85A 109.5 . . O84A C85 H85B 109.5 . . H85A C85 H85B 109.5 . . O84A C85 H85C 109.5 . . H85A C85 H85C 109.5 . . H85B C85 H85C 109.5 . . O102 C101 C1 126.4(6) . . O102 C101 H101 116.8 . . C1 C101 H101 116.8 . . C12 C121 C122 113.2(4) . . C12 C121 H12A 108.9 . . C122 C121 H12A 108.9 . . C12 C121 H12B 108.9 . . C122 C121 H12B 108.9 . . H12A C121 H12B 107.8 . . C121 C122 C123 112.8(5) . . C121 C122 K125 157.2(4) . . C123 C122 K125 78.3(3) . . C121 C122 H12C 109.0 . . C123 C122 H12C 109.0 . . K125 C122 H12C 48.4 . . C121 C122 H12D 109.0 . . C123 C122 H12D 109.0 . . K125 C122 H12D 84.2 . . H12C C122 H12D 107.8 . . O124 C123 O125 125.1(5) . . O124 C123 C122 118.8(5) . . O125 C123 C122 116.1(5) . . O124 C123 K125 53.8(3) . . O125 C123 K125 145.7(4) . . C122 C123 K125 76.5(3) . . C13 C131 H13A 109.5 . . C13 C131 H13B 109.5 . . H13A C131 H13B 109.5 . . C13 C131 H13C 109.5 . . H13A C131 H13C 109.5 . . H13B C131 H13C 109.5 . . C17 C171 H17A 109.5 . . C17 C171 H17B 109.5 . . H17A C171 H17B 109.5 . . C17 C171 H17C 109.5 . . H17A C171 H17C 109.5 . . H17B C171 H17C 109.5 . . C182 C181 C18 126.6(6) . . C182 C181 H18A 116.7 . . C18 C181 H18A 116.7 . . C181 C182 H18B 120.0 . . C181 C182 H18C 120.0 . . H18B C182 H18C 120.0 . . C22 O1 K125 104.0(16) . 2_446 C22 O1 K125 155.1(15) . . K125 O1 K125 93.3(4) 2_446 . O1 C22 K125 54.7(14) . 2_446 K125 O3 K125 105.5(5) 2_446 . C23 O2 K125 147.3(8) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 K125 O3 2.539(12) 2_446 K125 O191 2.725(4) 2_556 K125 O33 2.763(5) 1_556 K125 O84B 2.783(4) 2_556 K125 O2 2.808(10) . K125 O124 2.941(5) . K125 O1 2.949(12) 2_446 K125 O3 2.955(17) . K125 O1 3.074(13) . K125 O4 3.347(8) . K125 O7 3.347(16) 2_446 K125 C122 3.477(6) . N21 C4 1.358(6) . N21 C1 1.374(7) . N21 H21N 0.878(19) . N22 C9 1.353(6) . N22 C6 1.387(6) . N22 H22N 0.89(2) . N23 C14 1.333(6) . N23 C11 1.401(6) . N24 C19 1.374(7) . N24 C16 1.377(6) . N24 H24N 0.88(2) . O33 C32 1.406(7) . O33 K125 2.763(5) 1_554 O33 H33O 0.84(2) . O82 C81 1.223(6) . O84A C83 1.327(7) . O84A C85 1.463(10) . O84B C83 1.198(7) . O84B K125 2.783(4) 2_556 O102 C101 1.215(7) . O124 C123 1.252(6) . O125 C123 1.255(6) . O191 C19 1.224(6) . O191 K125 2.725(4) 2_556 C1 C2 1.392(7) . C1 C101 1.430(8) . C2 C3 1.414(7) . C2 C21 1.498(8) . C3 C4 1.382(7) . C3 C31 1.494(7) . C4 C5 1.498(7) . C5 C6 1.509(7) . C5 H5A 0.9800 . C5 H5B 0.9800 . C6 C7 1.367(7) . C7 C8 1.409(7) . C7 C71 1.502(7) . C8 C9 1.390(7) . C8 C81 1.443(7) . C9 C10 1.439(7) . C10 C11 1.362(7) . C10 C82 1.548(7) . C11 C12 1.484(7) . C12 C13 1.366(7) . C12 C121 1.486(7) . C13 C14 1.469(7) . C13 C131 1.493(7) . C14 C15 1.439(8) . C15 C16 1.345(7) . C15 H15 0.9400 . C16 C17 1.463(7) . C17 C18 1.352(7) . C17 C171 1.491(8) . C18 C181 1.464(8) . C18 C19 1.478(8) . C21 H21A 0.9700 . C21 H21B 0.9700 . C21 H21C 0.9700 . C31 C32 1.502(8) . C31 H31A 0.9800 . C31 H31B 0.9800 . C32 H32A 0.9800 . C32 H32B 0.9800 . C71 H71A 0.9700 . C71 H71B 0.9700 . C71 H71C 0.9700 . C81 C82 1.537(7) . C82 C83 1.491(8) . C82 H82 0.9900 . C85 H85A 0.9700 . C85 H85B 0.9700 . C85 H85C 0.9700 . C101 H101 0.9400 . C121 C122 1.503(8) . C121 H12A 0.9800 . C121 H12B 0.9800 . C122 C123 1.520(8) . C122 H12C 0.9800 . C122 H12D 0.9800 . C131 H13A 0.9700 . C131 H13B 0.9700 . C131 H13C 0.9700 . C171 H17A 0.9700 . C171 H17B 0.9700 . C171 H17C 0.9700 . C181 C182 1.276(9) . C181 H18A 0.9400 . C182 H18B 0.9400 . C182 H18C 0.9400 . O1 C22 1.32(5) . O1 K125 2.949(12) 2_446 C22 K125 3.51(4) 2_446 O3 K125 2.539(12) 2_446 O2 C23 1.531(16) . O7 K125 3.347(16) 2_446 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 N21 H21N O125 0.878(19) 2.06(3) 2.818(6) 144(3) . N22 H22N O125 0.89(2) 1.90(3) 2.753(5) 158(5) . N24 H24N N23 0.88(2) 2.16(4) 2.750(6) 124(4) . N24 H24N O84B 0.88(2) 2.49(4) 3.224(6) 142(4) . O33 H33O O82 0.84(2) 2.05(4) 2.839(6) 156(9) 2