#------------------------------------------------------------------------------ #$Date: 2023-11-02 04:27:17 +0200 (Thu, 02 Nov 2023) $ #$Revision: 287240 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247652.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_7247652 loop_ _publ_author_name 'Zamora-Moreno, Julio' 'Salom\'on-Flores, Mar\'ia K.' 'Valdes-Garc\'ia, Josue' 'Pinz\'on-Vanegas, Cristian' 'Mart\'inez-Otero, Diego' 'Barroso-Flores, Joaqu\'in' 'Villamil-Ramos, Ra\'ul' 'Romero-Solano, Miguel \'A.' 'Dorazco-Gonz\'alez, Alejandro' _publ_section_title ; Water-soluble fluorescent chemosensor for sorbitol based on a dicationic diboronic receptor. Crystal structure and spectroscopic studies ; _journal_issue 46 _journal_name_full 'RSC Advances' _journal_page_first 32185 _journal_page_last 32198 _journal_paper_doi 10.1039/D3RA06198A _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'C39 H33 B2 N5 O6, O4 S, 3(C2 H6 O S), 3.201(H2 O)' _chemical_formula_sum 'C45 H57.41 B2 N5 O16.21 S4' _chemical_formula_weight 1077.52 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2023-07-12 deposited with the CCDC. 2023-10-25 downloaded from the CCDC. ; _cell_angle_alpha 95.8776(14) _cell_angle_beta 100.6117(14) _cell_angle_gamma 102.3371(14) _cell_formula_units_Z 2 _cell_length_a 11.5675(8) _cell_length_b 14.3355(10) _cell_length_c 15.8991(11) _cell_measurement_reflns_used 9927 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.64 _cell_volume 2503.8(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirrors _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 107739 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.445 _diffrn_reflns_theta_min 1.824 _diffrn_source 'Incoatec ImuS' _exptl_absorpt_coefficient_mu 0.265 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.7016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.429 _exptl_crystal_description Prism _exptl_crystal_F_000 1132 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.303 _exptl_crystal_size_mid 0.267 _exptl_crystal_size_min 0.261 _refine_diff_density_max 0.711 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 745 _refine_ls_number_reflns 11433 _refine_ls_number_restraints 146 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0396 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+2.2470P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1044 _refine_ls_wR_factor_ref 0.1105 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9952 _reflns_number_total 11433 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra06198a2.cif _cod_data_source_block 125DGA23_0m _cod_database_code 7247652 _shelx_shelxl_version_number 2019/3 _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 0.924 _shelx_estimated_absorpt_t_max 0.934 _shelx_res_file ; TITL 125DGA23_0m in P-1 125DGA23_0m.res created by SHELXL-2019/3 at 15:31:13 on 12-Jul-2023 CELL 0.71073 11.56750 14.33550 15.89910 95.8776 100.6117 102.3371 ZERR 2.00 0.00080 0.00100 0.00110 0.0014 0.0014 0.0014 LATT 1 SFAC C H N O S B UNIT 90 114.823 10 32.4115 8 4 TEMP 0.000 SIZE 0.261 0.267 0.303 L.S. 10 BOND $H LIST 4 conf acta HTAB O2 S1 HTAB O2 O7 HTAB O3 S1 HTAB O3 O10 HTAB O5 S1 HTAB O5 O10 HTAB O6 S1 HTAB O6 O8 HTAB N2 N1 EQIV $1 x, y-1, z HTAB N2 O11_$1 HTAB N4 O11_$1 HTAB O11 O9 HTAB O11 O12 HTAB O12 S2 HTAB O12 O15 HTAB O12 S2A HTAB O12 O15A HTAB O12 S3 HTAB O12 O16 HTAB O13 O12 HTAB O13 S4 HTAB O13 O17 HTAB O14 O7 EQIV $2 -x+1, -y+1, -z HTAB O14 O7_$2 HTAB O14 O14_$2 FMAP 2 PLAN 10 omit -1 0 1 WGHT 0.053900 2.247000 FVAR 0.08969 0.95048 0.71356 0.48682 S1 5 0.641256 0.686243 0.201827 11.00000 0.02543 0.01617 = 0.01709 0.00289 0.00860 0.00672 O7 4 0.640120 0.626565 0.120150 11.00000 0.03092 0.02587 = 0.02022 -0.00401 0.00283 0.01182 O8 4 0.537271 0.644249 0.238849 11.00000 0.02730 0.02190 = 0.03047 0.01240 0.01202 0.00866 O9 4 0.634852 0.784468 0.186003 11.00000 0.03340 0.01735 = 0.02057 0.00505 0.01182 0.00623 O10 4 0.755583 0.690808 0.264238 11.00000 0.02754 0.02508 = 0.01943 0.00139 0.00754 0.00440 S3 5 0.608694 1.174679 -0.048307 11.00000 0.02163 0.02257 = 0.02096 0.00403 0.00474 0.00316 O16 4 0.716458 1.154500 0.011608 11.00000 0.02772 0.03285 = 0.02843 0.01197 0.00568 0.01055 C42 1 0.553410 1.258359 0.014891 11.00000 0.02920 0.04262 = 0.01937 0.00205 0.00742 0.01312 AFIX 137 H42A 2 0.490560 1.278893 -0.021514 11.00000 -1.50000 H42B 2 0.618377 1.313351 0.040698 11.00000 -1.50000 H42C 2 0.521511 1.227915 0.059538 11.00000 -1.50000 AFIX 0 C43 1 0.672739 1.255038 -0.114876 11.00000 0.02207 0.02744 = 0.02022 0.00483 0.00535 0.00459 AFIX 137 H43A 2 0.714725 1.222554 -0.150713 11.00000 -1.50000 H43B 2 0.728562 1.310245 -0.079049 11.00000 -1.50000 H43C 2 0.609462 1.275643 -0.150759 11.00000 -1.50000 AFIX 0 S4 5 0.297089 1.220541 0.258836 11.00000 0.02394 0.02121 = 0.03417 -0.00506 0.00201 0.00409 O17 4 0.403397 1.195767 0.314800 11.00000 0.03472 0.02367 = 0.03322 0.00887 0.00889 0.01294 C44 1 0.245110 1.303573 0.324296 11.00000 0.04501 0.03806 = 0.05082 0.00851 0.02009 0.02458 AFIX 137 H44A 2 0.309721 1.359722 0.347167 11.00000 -1.50000 H44B 2 0.218827 1.273802 0.371113 11.00000 -1.50000 H44C 2 0.178641 1.322150 0.290048 11.00000 -1.50000 AFIX 0 C45 1 0.358532 1.303832 0.194355 11.00000 0.05369 0.07489 = 0.03594 0.03079 0.01414 0.03394 AFIX 137 H45A 2 0.396457 1.272221 0.154796 11.00000 -1.50000 H45B 2 0.417528 1.356756 0.230921 11.00000 -1.50000 H45C 2 0.294907 1.327656 0.162404 11.00000 -1.50000 AFIX 0 simu 0.001 s2 > c41a rigu s2 > c41a part 1 21.0 S2 5 0.794375 1.307336 0.340601 21.00000 0.03076 0.03163 = 0.02252 0.00611 0.00460 0.00873 O15 4 0.839834 1.226169 0.302203 21.00000 0.04035 0.04316 = 0.03575 0.00199 -0.00061 0.02137 C40 1 0.678130 1.325706 0.259189 21.00000 0.02993 0.03552 = 0.03417 0.00049 0.00047 0.01298 AFIX 137 H40A 2 0.708157 1.334563 0.207437 21.00000 -1.50000 H40B 2 0.652419 1.382057 0.278593 21.00000 -1.50000 H40C 2 0.610766 1.270462 0.247382 21.00000 -1.50000 AFIX 0 C41 1 0.903373 1.416710 0.341577 21.00000 0.03333 0.04301 = 0.03968 0.00990 -0.00041 0.00266 AFIX 137 H41A 2 0.927132 1.416144 0.286804 21.00000 -1.50000 H41B 2 0.973097 1.421993 0.386757 21.00000 -1.50000 H41C 2 0.868462 1.470767 0.351694 21.00000 -1.50000 AFIX 0 part 2 -21.0 same s2 > c41 S2A 5 0.847594 1.331197 0.267292 -21.00000 0.03332 0.03644 = 0.02952 0.00523 0.00281 0.01010 O15A 4 0.886108 1.246796 0.283424 -21.00000 0.03472 0.03703 = 0.02946 0.00474 0.00281 0.01317 C40A 1 0.694798 1.328609 0.236951 -21.00000 0.03128 0.03451 = 0.02847 0.00415 0.00275 0.01066 AFIX 33 H40D 2 0.685497 1.392231 0.228742 -21.00000 -1.50000 H40E 2 0.660173 1.285147 0.183889 -21.00000 -1.50000 H40F 2 0.654210 1.307017 0.281439 -21.00000 -1.50000 AFIX 0 C41A 1 0.893222 1.410380 0.370471 -21.00000 0.03234 0.03729 = 0.03021 0.00715 0.00264 0.00723 AFIX 33 H41D 2 0.869349 1.469813 0.363811 -21.00000 -1.50000 H41E 2 0.854866 1.379583 0.412396 -21.00000 -1.50000 H41F 2 0.979555 1.423580 0.389715 -21.00000 -1.50000 AFIX 0 part 0 O1 4 1.143838 -0.150534 0.221788 11.00000 0.02207 0.02141 = 0.01693 0.00506 0.01048 0.01017 dfix 0.84 0.01 o2 h2a O2 4 0.772776 0.487177 0.124709 11.00000 0.02363 0.01995 = 0.03222 0.00018 0.00570 0.00568 H2A 2 0.726810 0.524766 0.129260 11.00000 -1.50000 dfix 0.84 0.01 o3 h3a O3 4 0.927269 0.627788 0.195593 11.00000 0.02706 0.02227 = 0.02404 -0.00235 0.00794 0.00300 H3A 2 0.873093 0.646973 0.216491 11.00000 -1.50000 O4 4 0.866791 -0.127819 0.576822 11.00000 0.03915 0.04035 = 0.01923 0.01464 0.01744 0.02507 dfix 0.84 0.01 o5 h5 O5 4 0.739306 0.616384 0.412522 11.00000 0.03403 0.02989 = 0.02402 0.01020 0.00180 -0.00448 H5 2 0.737199 0.642915 0.367738 11.00000 -1.50000 dfix 0.84 0.01 o6 h6 O6 4 0.554799 0.504737 0.336324 11.00000 0.03083 0.01999 = 0.02349 0.00840 0.00031 0.00435 H6 2 0.548398 0.543561 0.300792 11.00000 -1.50000 N1 3 0.974397 -0.120679 0.382997 11.00000 0.01217 0.01591 = 0.01201 0.00156 0.00361 0.00321 dfix 0.86 0.01 n2 h2n N2 3 1.024517 -0.045473 0.242952 11.00000 0.01509 0.01953 = 0.01382 0.00602 0.00909 0.00649 H2N 2 0.976296 -0.032350 0.273866 11.00000 -1.50000 N3 3 1.079851 0.196329 -0.008305 11.00000 0.01868 0.01485 = 0.01406 0.00396 0.00288 0.00256 dfix 0.86 0.01 n4 h4n N4 3 0.817884 -0.047446 0.463017 11.00000 0.01601 0.01865 = 0.01147 0.00239 0.00679 0.00638 H4N 2 0.827471 -0.040741 0.411949 11.00000 -1.50000 N5 3 0.515960 0.168458 0.583861 11.00000 0.01468 0.01376 = 0.01838 -0.00038 0.00482 0.00269 C1 1 1.042514 -0.162705 0.339167 11.00000 0.01140 0.01566 = 0.01079 0.00109 0.00252 0.00214 C2 1 1.087301 -0.240902 0.363170 11.00000 0.01502 0.01873 = 0.01423 0.00105 0.00397 0.00590 AFIX 43 H2 2 1.132255 -0.269289 0.329822 11.00000 -1.20000 AFIX 0 C3 1 1.063361 -0.275535 0.437970 11.00000 0.02190 0.02000 = 0.01748 0.00628 0.00496 0.00952 AFIX 43 H3 2 1.092669 -0.327308 0.456170 11.00000 -1.20000 AFIX 0 C4 1 0.994918 -0.231573 0.485158 11.00000 0.02029 0.02256 = 0.01567 0.00732 0.00702 0.00783 AFIX 43 H4 2 0.978592 -0.252421 0.536177 11.00000 -1.20000 AFIX 0 C5 1 0.951298 -0.155678 0.454478 11.00000 0.01322 0.01720 = 0.01364 0.00237 0.00442 0.00374 C6 1 1.075330 -0.119871 0.261659 11.00000 0.01262 0.01535 = 0.01155 0.00079 0.00250 0.00170 C7 1 1.045904 0.013613 0.180107 11.00000 0.01341 0.01529 = 0.01372 0.00362 0.00419 0.00251 C8 1 0.984258 0.089340 0.175777 11.00000 0.01497 0.01941 = 0.02050 0.00511 0.00860 0.00521 AFIX 43 H8 2 0.936310 0.098050 0.215516 11.00000 -1.20000 AFIX 0 C9 1 0.993401 0.149680 0.114948 11.00000 0.01486 0.01708 = 0.02032 0.00454 0.00599 0.00533 AFIX 43 H9 2 0.950101 0.197384 0.112163 11.00000 -1.20000 AFIX 0 C10 1 1.069417 0.138850 0.056236 11.00000 0.01508 0.01479 = 0.01249 0.00316 0.00325 0.00073 C11 1 1.159168 0.190231 -0.058663 11.00000 0.02436 0.01815 = 0.01360 0.00363 0.00554 0.00036 AFIX 43 H11 2 1.165784 0.230892 -0.100403 11.00000 -1.20000 AFIX 0 C12 1 1.232269 0.124741 -0.050482 11.00000 0.02308 0.02230 = 0.01497 0.00270 0.00978 0.00273 AFIX 43 H12 2 1.288973 0.123485 -0.084884 11.00000 -1.20000 AFIX 0 C13 1 1.220029 0.062161 0.008633 11.00000 0.01938 0.01899 = 0.01490 0.00129 0.00723 0.00425 AFIX 43 H13 2 1.265669 0.016062 0.012700 11.00000 -1.20000 AFIX 0 C14 1 1.137689 0.067982 0.063435 11.00000 0.01435 0.01531 = 0.01143 -0.00004 0.00367 0.00089 C15 1 1.123046 0.003948 0.124873 11.00000 0.01464 0.01521 = 0.01318 0.00210 0.00451 0.00418 AFIX 43 H15 2 1.165256 -0.044440 0.127991 11.00000 -1.20000 AFIX 0 C16 1 0.999891 0.264128 -0.023997 11.00000 0.02228 0.01716 = 0.01588 0.00465 0.00094 0.00548 AFIX 23 H16A 2 0.918787 0.232750 -0.019248 11.00000 -1.20000 H16B 2 0.995760 0.278726 -0.082563 11.00000 -1.20000 AFIX 0 C17 1 1.042764 0.357559 0.038473 11.00000 0.02263 0.01459 = 0.01438 0.00609 -0.00027 0.00419 C18 1 0.957731 0.397750 0.070900 11.00000 0.01998 0.01814 = 0.01497 0.00585 0.00104 0.00275 AFIX 43 H18 2 0.877170 0.363514 0.057977 11.00000 -1.20000 AFIX 0 C19 1 0.990124 0.488528 0.122579 11.00000 0.02452 0.01773 = 0.01365 0.00620 0.00170 0.00433 C20 1 1.112923 0.535634 0.143993 11.00000 0.02639 0.01593 = 0.01809 0.00376 -0.00086 0.00368 AFIX 43 H20 2 1.137325 0.595029 0.179603 11.00000 -1.20000 AFIX 0 C21 1 1.199327 0.495800 0.113327 11.00000 0.02059 0.01716 = 0.02975 0.00574 -0.00240 0.00248 AFIX 43 H21 2 1.280724 0.527795 0.129282 11.00000 -1.20000 AFIX 0 C22 1 1.163673 0.407784 0.058602 11.00000 0.02119 0.01786 = 0.02604 0.00814 0.00120 0.00694 AFIX 43 H22 2 1.220731 0.382584 0.035511 11.00000 -1.20000 AFIX 0 C23 1 0.874939 -0.109194 0.504493 11.00000 0.01696 0.02031 = 0.01628 0.00401 0.00733 0.00607 C24 1 0.743497 0.005521 0.496713 11.00000 0.01186 0.01490 = 0.01399 -0.00078 0.00346 0.00237 C25 1 0.703482 0.074294 0.447665 11.00000 0.01663 0.01720 = 0.01263 0.00194 0.00542 0.00297 AFIX 43 H25 2 0.728447 0.082907 0.396049 11.00000 -1.20000 AFIX 0 C26 1 0.474917 0.242921 0.535731 11.00000 0.01603 0.01703 = 0.02273 0.00267 0.00432 0.00601 AFIX 23 H26A 2 0.409024 0.261081 0.558099 11.00000 -1.20000 H26B 2 0.444354 0.215906 0.475204 11.00000 -1.20000 AFIX 0 C27 1 0.707356 -0.006932 0.573870 11.00000 0.01566 0.01713 = 0.01287 0.00152 0.00462 0.00430 AFIX 43 H27 2 0.732887 -0.051916 0.606454 11.00000 -1.20000 AFIX 0 C28 1 0.631740 0.048702 0.603018 11.00000 0.01343 0.01624 = 0.01314 -0.00054 0.00379 0.00156 C29 1 0.594838 0.037128 0.682131 11.00000 0.01837 0.02173 = 0.01377 0.00179 0.00513 0.00446 AFIX 43 H29 2 0.622044 -0.006262 0.715951 11.00000 -1.20000 AFIX 0 C30 1 0.481587 0.155632 0.658317 11.00000 0.01617 0.01873 = 0.01835 -0.00360 0.00651 0.00294 AFIX 43 H30 2 0.430904 0.191923 0.676951 11.00000 -1.20000 AFIX 0 C31 1 0.519157 0.089770 0.708833 11.00000 0.01917 0.02343 = 0.01440 -0.00098 0.00717 0.00335 AFIX 43 H31 2 0.493191 0.081563 0.760162 11.00000 -1.20000 AFIX 0 C32 1 0.591725 0.116262 0.553240 11.00000 0.01310 0.01358 = 0.01510 -0.00203 0.00427 0.00129 C33 1 0.628925 0.128351 0.474497 11.00000 0.01660 0.01601 = 0.01573 0.00255 0.00380 0.00389 AFIX 43 H33 2 0.603077 0.172599 0.441121 11.00000 -1.20000 AFIX 0 C34 1 0.575898 0.331993 0.543146 11.00000 0.01732 0.01482 = 0.02005 -0.00057 0.00621 0.00633 C35 1 0.572794 0.385872 0.475430 11.00000 0.01939 0.01850 = 0.01808 -0.00039 0.00251 0.00605 AFIX 43 H35 2 0.510871 0.364768 0.426442 11.00000 -1.20000 AFIX 0 C36 1 0.660174 0.470984 0.478829 11.00000 0.02140 0.01753 = 0.01825 0.00065 0.00511 0.00639 C37 1 0.754572 0.498414 0.551829 11.00000 0.02033 0.01779 = 0.02257 0.00016 0.00382 0.00186 AFIX 43 H37 2 0.816011 0.553088 0.554561 11.00000 -1.20000 AFIX 0 C38 1 0.758516 0.445627 0.620468 11.00000 0.02328 0.02209 = 0.01994 0.00104 -0.00130 0.00301 AFIX 43 H38 2 0.821685 0.465494 0.668796 11.00000 -1.20000 AFIX 0 C39 1 0.668196 0.363265 0.616904 11.00000 0.02365 0.01918 = 0.01877 0.00328 0.00359 0.00627 AFIX 43 H39 2 0.669254 0.329056 0.663571 11.00000 -1.20000 AFIX 0 B1 6 0.650760 0.535185 0.404080 11.00000 0.02467 0.01814 = 0.02025 0.00244 0.00672 0.00624 B2 6 0.889994 0.537349 0.149741 11.00000 0.02656 0.01844 = 0.01517 0.00564 0.00470 0.00510 dfix 0.84 0.01 o11 h11a dfix 0.84 0.01 o11 h11b O11 4 0.778387 0.960368 0.273581 11.00000 0.01764 0.02048 = 0.01666 0.00445 0.00431 0.00563 H11A 2 0.744337 0.903756 0.252715 11.00000 -1.50000 H11B 2 0.748190 0.993765 0.240218 11.00000 -1.50000 dfix 0.84 0.01 o12 h12a dfix 0.84 0.01 o12 h12b O12 4 0.692705 1.091064 0.169309 11.00000 0.03890 0.03667 = 0.02938 0.01050 0.00900 0.02060 H12A 2 0.730743 1.139125 0.207201 11.00000 -1.50000 H12B 2 0.695609 1.106109 0.119516 11.00000 -1.50000 dfix 0.84 0.01 o13 h13a dfix 0.84 0.01 o13 h13b part 1 31.0 O13 4 0.450872 1.088745 0.161959 31.00000 0.02398 0.03963 = 0.02975 0.00787 0.01008 0.01202 H13A 2 0.523328 1.084342 0.167920 31.00000 -1.50000 H13B 2 0.455983 1.122793 0.209457 31.00000 -1.50000 part 1 41.0 dfix 0.84 0.01 o14 h14a dfix 0.84 0.01 o14 h14b O14 4 0.452599 0.449534 0.063472 41.00000 0.03102 0.03629 = 0.02655 -0.00227 0.00622 -0.00045 H14A 2 0.498575 0.505195 0.073725 41.00000 -1.50000 H14B 2 0.454027 0.435760 0.011100 41.00000 -1.50000 part 0 HKLF 4 REM 125DGA23_0m in P-1 REM wR2 = 0.1105, GooF = S = 1.029, Restrained GooF = 1.057 for all data REM R1 = 0.0396 for 9952 Fo > 4sig(Fo) and 0.0467 for all 11433 data REM 745 parameters refined using 146 restraints END WGHT 0.0539 2.2472 REM Highest difference peak 0.711, deepest hole -0.647, 1-sigma level 0.061 Q1 1 0.7074 0.7151 0.2361 11.00000 0.05 0.71 Q2 1 0.9068 1.3833 0.2966 11.00000 0.05 0.62 Q3 1 1.0570 -0.1394 0.3007 11.00000 0.05 0.48 Q4 1 0.6554 0.5025 0.4424 11.00000 0.05 0.47 Q5 1 0.8823 1.3569 0.3555 11.00000 0.05 0.46 Q6 1 1.1330 0.0473 0.0993 11.00000 0.05 0.44 Q7 1 1.1009 0.1014 0.0575 11.00000 0.05 0.44 Q8 1 0.3196 1.2615 0.2210 11.00000 0.05 0.42 Q9 1 0.6162 0.0846 0.5805 11.00000 0.05 0.41 Q10 1 1.0072 0.0442 0.1688 11.00000 0.05 0.40 ; _shelx_res_checksum 26530 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.64126(4) 0.68624(3) 0.20183(3) 0.01871(9) Uani 1 1 d . . . . . O7 O 0.64012(12) 0.62656(9) 0.12015(8) 0.0258(3) Uani 1 1 d . . . . . O8 O 0.53727(12) 0.64425(9) 0.23885(9) 0.0247(3) Uani 1 1 d . . . . . O9 O 0.63485(12) 0.78447(8) 0.18600(8) 0.0228(3) Uani 1 1 d . . . . . O10 O 0.75558(12) 0.69081(9) 0.26424(8) 0.0241(3) Uani 1 1 d . . . . . S3 S 0.60869(4) 1.17468(3) -0.04831(3) 0.02195(10) Uani 1 1 d . . . . . O16 O 0.71646(12) 1.15450(10) 0.01161(9) 0.0286(3) Uani 1 1 d . . . . . C42 C 0.55341(18) 1.25836(16) 0.01489(12) 0.0296(4) Uani 1 1 d . . . . . H42A H 0.490560 1.278893 -0.021514 0.044 Uiso 1 1 calc R U . . . H42B H 0.618377 1.313351 0.040698 0.044 Uiso 1 1 calc R U . . . H42C H 0.521511 1.227915 0.059538 0.044 Uiso 1 1 calc R U . . . C43 C 0.67274(16) 1.25504(13) -0.11488(11) 0.0232(3) Uani 1 1 d . . . . . H43A H 0.714725 1.222554 -0.150713 0.035 Uiso 1 1 calc R U . . . H43B H 0.728562 1.310245 -0.079049 0.035 Uiso 1 1 calc R U . . . H43C H 0.609462 1.275643 -0.150759 0.035 Uiso 1 1 calc R U . . . S4 S 0.29709(4) 1.22054(3) 0.25884(3) 0.02785(11) Uani 1 1 d . . . . . O17 O 0.40340(13) 1.19577(9) 0.31480(9) 0.0291(3) Uani 1 1 d . . . . . C44 C 0.2451(2) 1.30357(17) 0.32430(16) 0.0409(5) Uani 1 1 d . . . . . H44A H 0.309721 1.359722 0.347167 0.061 Uiso 1 1 calc R U . . . H44B H 0.218827 1.273802 0.371113 0.061 Uiso 1 1 calc R U . . . H44C H 0.178641 1.322150 0.290048 0.061 Uiso 1 1 calc R U . . . C45 C 0.3585(2) 1.3038(2) 0.19435(16) 0.0497(6) Uani 1 1 d . . . . . H45A H 0.396457 1.272221 0.154796 0.075 Uiso 1 1 calc R U . . . H45B H 0.417528 1.356756 0.230921 0.075 Uiso 1 1 calc R U . . . H45C H 0.294907 1.327656 0.162404 0.075 Uiso 1 1 calc R U . . . S2 S 0.79438(5) 1.30734(4) 0.34060(3) 0.02809(13) Uani 0.9505(13) 1 d D U P A 1 O15 O 0.83983(17) 1.22617(13) 0.30220(11) 0.0394(4) Uani 0.9505(13) 1 d D U P A 1 C40 C 0.6781(2) 1.3257(2) 0.25919(15) 0.0336(5) Uani 0.9505(13) 1 d D U P A 1 H40A H 0.708157 1.334563 0.207437 0.050 Uiso 0.9505(13) 1 calc R U P A 1 H40B H 0.652419 1.382057 0.278593 0.050 Uiso 0.9505(13) 1 calc R U P A 1 H40C H 0.610766 1.270462 0.247382 0.050 Uiso 0.9505(13) 1 calc R U P A 1 C41 C 0.9034(2) 1.41671(19) 0.34158(18) 0.0405(5) Uani 0.9505(13) 1 d D U P A 1 H41A H 0.927132 1.416144 0.286804 0.061 Uiso 0.9505(13) 1 calc R U P A 1 H41B H 0.973097 1.421993 0.386757 0.061 Uiso 0.9505(13) 1 calc R U P A 1 H41C H 0.868462 1.470767 0.351694 0.061 Uiso 0.9505(13) 1 calc R U P A 1 S2A S 0.8476(9) 1.3312(8) 0.2673(7) 0.0333(5) Uani 0.0495(13) 1 d D U P A 2 O15A O 0.886(3) 1.2468(17) 0.283(2) 0.0336(8) Uani 0.0495(13) 1 d D U P A 2 C40A C 0.695(2) 1.329(4) 0.237(3) 0.0315(8) Uani 0.0495(13) 1 d D U P A 2 H40D H 0.685497 1.392231 0.228742 0.047 Uiso 0.0495(13) 1 calc R U P A 2 H40E H 0.660173 1.285147 0.183889 0.047 Uiso 0.0495(13) 1 calc R U P A 2 H40F H 0.654210 1.307017 0.281439 0.047 Uiso 0.0495(13) 1 calc R U P A 2 C41A C 0.893(4) 1.410(3) 0.370(2) 0.0338(8) Uani 0.0495(13) 1 d D U P A 2 H41D H 0.869349 1.469813 0.363811 0.051 Uiso 0.0495(13) 1 calc R U P A 2 H41E H 0.854866 1.379583 0.412396 0.051 Uiso 0.0495(13) 1 calc R U P A 2 H41F H 0.979555 1.423580 0.389715 0.051 Uiso 0.0495(13) 1 calc R U P A 2 O1 O 1.14384(11) -0.15053(8) 0.22179(7) 0.0184(2) Uani 1 1 d . . . . . O2 O 0.77278(12) 0.48718(9) 0.12471(9) 0.0255(3) Uani 1 1 d D . . . . H2A H 0.7268(19) 0.5248(15) 0.1293(16) 0.038 Uiso 1 1 d D U . . . O3 O 0.92727(12) 0.62779(9) 0.19559(8) 0.0250(3) Uani 1 1 d D . . . . H3A H 0.8731(17) 0.6470(17) 0.2165(15) 0.037 Uiso 1 1 d D U . . . O4 O 0.86679(13) -0.12782(10) 0.57682(8) 0.0283(3) Uani 1 1 d . . . . . O5 O 0.73931(13) 0.61638(10) 0.41252(9) 0.0313(3) Uani 1 1 d D . . . . H5 H 0.737(2) 0.6429(18) 0.3677(11) 0.047 Uiso 1 1 d D U . . . O6 O 0.55480(12) 0.50474(9) 0.33632(8) 0.0254(3) Uani 1 1 d D . . . . H6 H 0.548(2) 0.5436(15) 0.3008(13) 0.038 Uiso 1 1 d D U . . . N1 N 0.97440(11) -0.12068(9) 0.38300(8) 0.0133(2) Uani 1 1 d . . . . . N2 N 1.02452(12) -0.04547(10) 0.24295(8) 0.0147(3) Uani 1 1 d D . . . . H2N H 0.9763(16) -0.0324(15) 0.2739(12) 0.022 Uiso 1 1 d D U . . . N3 N 1.07985(12) 0.19633(9) -0.00831(8) 0.0160(3) Uani 1 1 d . . . . . N4 N 0.81788(12) -0.04745(10) 0.46302(8) 0.0145(3) Uani 1 1 d D . . . . H4N H 0.8275(19) -0.0407(15) 0.4119(8) 0.022 Uiso 1 1 d D U . . . N5 N 0.51596(12) 0.16846(9) 0.58386(9) 0.0157(3) Uani 1 1 d . . . . . C1 C 1.04251(13) -0.16270(11) 0.33917(9) 0.0128(3) Uani 1 1 d . . . . . C2 C 1.08730(14) -0.24090(11) 0.36317(10) 0.0157(3) Uani 1 1 d . . . . . H2 H 1.132255 -0.269289 0.329822 0.019 Uiso 1 1 calc R U . . . C3 C 1.06336(15) -0.27554(12) 0.43797(10) 0.0187(3) Uani 1 1 d . . . . . H3 H 1.092669 -0.327308 0.456170 0.022 Uiso 1 1 calc R U . . . C4 C 0.99492(15) -0.23157(12) 0.48516(10) 0.0183(3) Uani 1 1 d . . . . . H4 H 0.978592 -0.252421 0.536177 0.022 Uiso 1 1 calc R U . . . C5 C 0.95130(14) -0.15568(11) 0.45448(10) 0.0145(3) Uani 1 1 d . . . . . C6 C 1.07533(13) -0.11987(11) 0.26166(9) 0.0135(3) Uani 1 1 d . . . . . C7 C 1.04590(13) 0.01361(11) 0.18011(10) 0.0140(3) Uani 1 1 d . . . . . C8 C 0.98426(14) 0.08934(12) 0.17578(11) 0.0173(3) Uani 1 1 d . . . . . H8 H 0.936310 0.098050 0.215516 0.021 Uiso 1 1 calc R U . . . C9 C 0.99340(14) 0.14968(11) 0.11495(10) 0.0168(3) Uani 1 1 d . . . . . H9 H 0.950101 0.197384 0.112163 0.020 Uiso 1 1 calc R U . . . C10 C 1.06942(14) 0.13885(11) 0.05624(10) 0.0144(3) Uani 1 1 d . . . . . C11 C 1.15917(15) 0.19023(12) -0.05866(10) 0.0191(3) Uani 1 1 d . . . . . H11 H 1.165784 0.230892 -0.100403 0.023 Uiso 1 1 calc R U . . . C12 C 1.23227(15) 0.12474(12) -0.05048(10) 0.0198(3) Uani 1 1 d . . . . . H12 H 1.288973 0.123485 -0.084884 0.024 Uiso 1 1 calc R U . . . C13 C 1.22003(15) 0.06216(12) 0.00863(10) 0.0174(3) Uani 1 1 d . . . . . H13 H 1.265669 0.016062 0.012700 0.021 Uiso 1 1 calc R U . . . C14 C 1.13769(14) 0.06798(11) 0.06344(10) 0.0141(3) Uani 1 1 d . . . . . C15 C 1.12305(14) 0.00395(11) 0.12487(10) 0.0140(3) Uani 1 1 d . . . . . H15 H 1.165256 -0.044440 0.127991 0.017 Uiso 1 1 calc R U . . . C16 C 0.99989(15) 0.26413(11) -0.02400(10) 0.0186(3) Uani 1 1 d . . . . . H16A H 0.918787 0.232750 -0.019248 0.022 Uiso 1 1 calc R U . . . H16B H 0.995760 0.278726 -0.082563 0.022 Uiso 1 1 calc R U . . . C17 C 1.04276(15) 0.35756(11) 0.03847(10) 0.0175(3) Uani 1 1 d . . . . . C18 C 0.95773(15) 0.39775(12) 0.07090(10) 0.0181(3) Uani 1 1 d . . . . . H18 H 0.877170 0.363514 0.057977 0.022 Uiso 1 1 calc R U . . . C19 C 0.99012(15) 0.48853(12) 0.12258(10) 0.0188(3) Uani 1 1 d . . . . . C20 C 1.11292(16) 0.53563(12) 0.14399(11) 0.0210(3) Uani 1 1 d . . . . . H20 H 1.137325 0.595029 0.179603 0.025 Uiso 1 1 calc R U . . . C21 C 1.19933(16) 0.49580(12) 0.11333(12) 0.0237(4) Uani 1 1 d . . . . . H21 H 1.280724 0.527795 0.129282 0.028 Uiso 1 1 calc R U . . . C22 C 1.16367(16) 0.40778(12) 0.05860(11) 0.0215(3) Uani 1 1 d . . . . . H22 H 1.220731 0.382584 0.035511 0.026 Uiso 1 1 calc R U . . . C23 C 0.87494(14) -0.10919(12) 0.50449(10) 0.0170(3) Uani 1 1 d . . . . . C24 C 0.74350(13) 0.00552(11) 0.49671(10) 0.0138(3) Uani 1 1 d . . . . . C25 C 0.70348(14) 0.07429(11) 0.44766(10) 0.0154(3) Uani 1 1 d . . . . . H25 H 0.728447 0.082907 0.396049 0.018 Uiso 1 1 calc R U . . . C26 C 0.47492(14) 0.24292(11) 0.53573(11) 0.0183(3) Uani 1 1 d . . . . . H26A H 0.409024 0.261081 0.558099 0.022 Uiso 1 1 calc R U . . . H26B H 0.444354 0.215906 0.475204 0.022 Uiso 1 1 calc R U . . . C27 C 0.70736(14) -0.00693(11) 0.57387(10) 0.0150(3) Uani 1 1 d . . . . . H27 H 0.732887 -0.051916 0.606454 0.018 Uiso 1 1 calc R U . . . C28 C 0.63174(13) 0.04870(11) 0.60302(10) 0.0146(3) Uani 1 1 d . . . . . C29 C 0.59484(14) 0.03713(12) 0.68213(10) 0.0178(3) Uani 1 1 d . . . . . H29 H 0.622044 -0.006262 0.715951 0.021 Uiso 1 1 calc R U . . . C30 C 0.48159(14) 0.15563(12) 0.65832(10) 0.0180(3) Uani 1 1 d . . . . . H30 H 0.430904 0.191923 0.676951 0.022 Uiso 1 1 calc R U . . . C31 C 0.51916(15) 0.08977(12) 0.70883(10) 0.0191(3) Uani 1 1 d . . . . . H31 H 0.493191 0.081563 0.760162 0.023 Uiso 1 1 calc R U . . . C32 C 0.59173(13) 0.11626(11) 0.55324(10) 0.0143(3) Uani 1 1 d . . . . . C33 C 0.62892(14) 0.12835(11) 0.47450(10) 0.0160(3) Uani 1 1 d . . . . . H33 H 0.603077 0.172599 0.441121 0.019 Uiso 1 1 calc R U . . . C34 C 0.57590(14) 0.33199(11) 0.54315(11) 0.0169(3) Uani 1 1 d . . . . . C35 C 0.57279(15) 0.38587(12) 0.47543(11) 0.0188(3) Uani 1 1 d . . . . . H35 H 0.510871 0.364768 0.426442 0.023 Uiso 1 1 calc R U . . . C36 C 0.66017(15) 0.47098(12) 0.47883(11) 0.0188(3) Uani 1 1 d . . . . . C37 C 0.75457(15) 0.49841(12) 0.55183(11) 0.0209(3) Uani 1 1 d . . . . . H37 H 0.816011 0.553088 0.554561 0.025 Uiso 1 1 calc R U . . . C38 C 0.75852(16) 0.44563(13) 0.62047(11) 0.0231(3) Uani 1 1 d . . . . . H38 H 0.821685 0.465494 0.668796 0.028 Uiso 1 1 calc R U . . . C39 C 0.66820(16) 0.36326(12) 0.61690(11) 0.0204(3) Uani 1 1 d . . . . . H39 H 0.669254 0.329056 0.663571 0.025 Uiso 1 1 calc R U . . . B1 B 0.65076(18) 0.53519(14) 0.40408(12) 0.0206(4) Uani 1 1 d . . . . . B2 B 0.88999(18) 0.53735(14) 0.14974(12) 0.0198(4) Uani 1 1 d . . . . . O11 O 0.77839(10) 0.96037(9) 0.27358(7) 0.0179(2) Uani 1 1 d D . . . . H11A H 0.7443(18) 0.9038(8) 0.2527(14) 0.027 Uiso 1 1 d D U . . . H11B H 0.7482(19) 0.9938(14) 0.2402(12) 0.027 Uiso 1 1 d D U . . . O12 O 0.69270(14) 1.09106(11) 0.16931(9) 0.0325(3) Uani 1 1 d D . . . . H12A H 0.731(2) 1.1391(14) 0.2072(14) 0.049 Uiso 1 1 d D U . . . H12B H 0.696(3) 1.106(2) 0.1195(10) 0.049 Uiso 1 1 d D U . . . O13 O 0.45087(17) 1.08874(15) 0.16196(13) 0.0297(6) Uani 0.714(5) 1 d D . P B 1 H13A H 0.5233(14) 1.084(3) 0.168(2) 0.044 Uiso 0.714(5) 1 d D U P B 1 H13B H 0.456(3) 1.123(2) 0.2095(13) 0.044 Uiso 0.714(5) 1 d D U P B 1 O14 O 0.4526(3) 0.4495(2) 0.06347(19) 0.0331(10) Uani 0.487(5) 1 d D . P C 1 H14A H 0.499(4) 0.5052(18) 0.074(4) 0.050 Uiso 0.487(5) 1 d D U P C 1 H14B H 0.454(5) 0.436(4) 0.0111(12) 0.050 Uiso 0.487(5) 1 d D U P C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0254(2) 0.01617(19) 0.01709(19) 0.00289(14) 0.00860(15) 0.00672(15) O7 0.0309(7) 0.0259(6) 0.0202(6) -0.0040(5) 0.0028(5) 0.0118(5) O8 0.0273(6) 0.0219(6) 0.0305(7) 0.0124(5) 0.0120(5) 0.0087(5) O9 0.0334(7) 0.0174(6) 0.0206(6) 0.0051(5) 0.0118(5) 0.0062(5) O10 0.0275(6) 0.0251(6) 0.0194(6) 0.0014(5) 0.0075(5) 0.0044(5) S3 0.0216(2) 0.0226(2) 0.0210(2) 0.00403(16) 0.00474(16) 0.00316(16) O16 0.0277(7) 0.0328(7) 0.0284(7) 0.0120(6) 0.0057(5) 0.0106(6) C42 0.0292(9) 0.0426(11) 0.0194(8) 0.0021(8) 0.0074(7) 0.0131(8) C43 0.0221(8) 0.0274(9) 0.0202(8) 0.0048(7) 0.0053(6) 0.0046(7) S4 0.0239(2) 0.0212(2) 0.0342(3) -0.00506(18) 0.00201(18) 0.00409(17) O17 0.0347(7) 0.0237(6) 0.0332(7) 0.0089(5) 0.0089(6) 0.0129(6) C44 0.0450(13) 0.0381(12) 0.0508(13) 0.0085(10) 0.0201(10) 0.0246(10) C45 0.0537(15) 0.0749(18) 0.0359(12) 0.0308(12) 0.0141(11) 0.0339(13) S2 0.0308(3) 0.0316(3) 0.0225(2) 0.00611(18) 0.00460(18) 0.00873(19) O15 0.0404(8) 0.0432(8) 0.0357(7) 0.0020(6) -0.0006(6) 0.0214(6) C40 0.0299(8) 0.0355(8) 0.0342(9) 0.0005(8) 0.0005(7) 0.0130(7) C41 0.0333(9) 0.0430(9) 0.0397(9) 0.0099(8) -0.0004(8) 0.0027(8) S2A 0.0333(7) 0.0364(7) 0.0295(7) 0.0052(7) 0.0028(7) 0.0101(7) O15A 0.0347(13) 0.0370(13) 0.0295(13) 0.0047(12) 0.0028(12) 0.0132(12) C40A 0.0313(13) 0.0345(13) 0.0285(13) 0.0042(13) 0.0028(12) 0.0107(12) C41A 0.0323(13) 0.0373(13) 0.0302(13) 0.0072(13) 0.0026(13) 0.0072(12) O1 0.0221(6) 0.0214(6) 0.0169(5) 0.0051(4) 0.0105(4) 0.0102(5) O2 0.0236(6) 0.0200(6) 0.0322(7) 0.0002(5) 0.0057(5) 0.0057(5) O3 0.0271(7) 0.0223(6) 0.0240(6) -0.0023(5) 0.0079(5) 0.0030(5) O4 0.0391(8) 0.0404(8) 0.0192(6) 0.0146(5) 0.0174(5) 0.0251(6) O5 0.0340(7) 0.0299(7) 0.0240(7) 0.0102(5) 0.0018(6) -0.0045(6) O6 0.0308(7) 0.0200(6) 0.0235(6) 0.0084(5) 0.0003(5) 0.0043(5) N1 0.0122(6) 0.0159(6) 0.0120(6) 0.0016(5) 0.0036(5) 0.0032(5) N2 0.0151(6) 0.0195(6) 0.0138(6) 0.0060(5) 0.0091(5) 0.0065(5) N3 0.0187(6) 0.0149(6) 0.0141(6) 0.0040(5) 0.0029(5) 0.0026(5) N4 0.0160(6) 0.0187(6) 0.0115(6) 0.0024(5) 0.0068(5) 0.0064(5) N5 0.0147(6) 0.0138(6) 0.0184(6) -0.0004(5) 0.0048(5) 0.0027(5) C1 0.0114(7) 0.0157(7) 0.0108(7) 0.0011(5) 0.0025(5) 0.0021(5) C2 0.0150(7) 0.0187(7) 0.0142(7) 0.0010(6) 0.0040(6) 0.0059(6) C3 0.0219(8) 0.0200(8) 0.0175(8) 0.0063(6) 0.0050(6) 0.0095(6) C4 0.0203(8) 0.0226(8) 0.0157(7) 0.0073(6) 0.0070(6) 0.0078(6) C5 0.0132(7) 0.0172(7) 0.0136(7) 0.0024(6) 0.0044(5) 0.0037(6) C6 0.0126(7) 0.0153(7) 0.0115(7) 0.0008(5) 0.0025(5) 0.0017(5) C7 0.0134(7) 0.0153(7) 0.0137(7) 0.0036(5) 0.0042(5) 0.0025(5) C8 0.0150(7) 0.0194(8) 0.0205(8) 0.0051(6) 0.0086(6) 0.0052(6) C9 0.0149(7) 0.0171(7) 0.0203(8) 0.0045(6) 0.0060(6) 0.0053(6) C10 0.0151(7) 0.0148(7) 0.0125(7) 0.0032(5) 0.0032(5) 0.0007(6) C11 0.0244(8) 0.0181(7) 0.0136(7) 0.0036(6) 0.0055(6) 0.0004(6) C12 0.0231(8) 0.0223(8) 0.0150(7) 0.0027(6) 0.0098(6) 0.0027(6) C13 0.0194(7) 0.0190(7) 0.0149(7) 0.0013(6) 0.0072(6) 0.0043(6) C14 0.0144(7) 0.0153(7) 0.0114(7) 0.0000(5) 0.0037(5) 0.0009(5) C15 0.0146(7) 0.0152(7) 0.0132(7) 0.0021(5) 0.0045(5) 0.0042(5) C16 0.0223(8) 0.0172(7) 0.0159(7) 0.0046(6) 0.0009(6) 0.0055(6) C17 0.0226(8) 0.0146(7) 0.0144(7) 0.0061(6) -0.0003(6) 0.0042(6) C18 0.0200(8) 0.0181(7) 0.0150(7) 0.0059(6) 0.0010(6) 0.0027(6) C19 0.0245(8) 0.0177(7) 0.0137(7) 0.0062(6) 0.0017(6) 0.0043(6) C20 0.0264(9) 0.0159(7) 0.0181(8) 0.0038(6) -0.0009(6) 0.0037(6) C21 0.0206(8) 0.0172(8) 0.0297(9) 0.0057(7) -0.0024(7) 0.0025(6) C22 0.0212(8) 0.0179(8) 0.0260(9) 0.0081(6) 0.0012(7) 0.0069(6) C23 0.0170(7) 0.0203(8) 0.0163(7) 0.0040(6) 0.0073(6) 0.0061(6) C24 0.0119(7) 0.0149(7) 0.0140(7) -0.0008(5) 0.0035(5) 0.0024(5) C25 0.0166(7) 0.0172(7) 0.0126(7) 0.0019(6) 0.0054(6) 0.0030(6) C26 0.0160(7) 0.0170(7) 0.0227(8) 0.0027(6) 0.0043(6) 0.0060(6) C27 0.0157(7) 0.0171(7) 0.0129(7) 0.0015(6) 0.0046(5) 0.0043(6) C28 0.0134(7) 0.0162(7) 0.0131(7) -0.0005(6) 0.0038(5) 0.0016(6) C29 0.0184(8) 0.0217(8) 0.0138(7) 0.0018(6) 0.0051(6) 0.0045(6) C30 0.0162(7) 0.0187(7) 0.0184(8) -0.0036(6) 0.0065(6) 0.0029(6) C31 0.0192(8) 0.0234(8) 0.0144(7) -0.0010(6) 0.0072(6) 0.0033(6) C32 0.0131(7) 0.0136(7) 0.0151(7) -0.0020(5) 0.0043(5) 0.0013(5) C33 0.0166(7) 0.0160(7) 0.0157(7) 0.0025(6) 0.0038(6) 0.0039(6) C34 0.0173(7) 0.0148(7) 0.0201(8) -0.0006(6) 0.0062(6) 0.0063(6) C35 0.0194(8) 0.0185(8) 0.0181(8) -0.0004(6) 0.0025(6) 0.0061(6) C36 0.0214(8) 0.0175(7) 0.0183(8) 0.0007(6) 0.0051(6) 0.0064(6) C37 0.0203(8) 0.0178(8) 0.0226(8) 0.0002(6) 0.0038(6) 0.0019(6) C38 0.0233(8) 0.0221(8) 0.0199(8) 0.0010(6) -0.0013(6) 0.0030(7) C39 0.0237(8) 0.0192(8) 0.0188(8) 0.0033(6) 0.0036(6) 0.0063(6) B1 0.0247(9) 0.0181(8) 0.0203(9) 0.0024(7) 0.0067(7) 0.0062(7) B2 0.0266(9) 0.0184(8) 0.0152(8) 0.0056(7) 0.0047(7) 0.0051(7) O11 0.0176(6) 0.0205(6) 0.0167(6) 0.0044(4) 0.0043(4) 0.0056(5) O12 0.0389(8) 0.0367(8) 0.0294(7) 0.0105(6) 0.0090(6) 0.0206(7) O13 0.0240(10) 0.0396(12) 0.0297(11) 0.0079(8) 0.0101(8) 0.0120(8) O14 0.0310(17) 0.0363(18) 0.0266(16) -0.0023(12) 0.0062(12) -0.0004(12) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 S1 O8 108.88(7) . . ? O9 S1 O7 109.92(7) . . ? O8 S1 O7 110.68(8) . . ? O9 S1 O10 109.23(8) . . ? O8 S1 O10 109.33(7) . . ? O7 S1 O10 108.78(7) . . ? O16 S3 C43 105.18(8) . . ? O16 S3 C42 106.09(9) . . ? C43 S3 C42 97.94(9) . . ? S3 C42 H42A 109.5 . . ? S3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? S3 C43 H43A 109.5 . . ? S3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? S3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O17 S4 C45 106.34(10) . . ? O17 S4 C44 107.44(10) . . ? C45 S4 C44 96.44(12) . . ? S4 C44 H44A 109.5 . . ? S4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? S4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? S4 C45 H45A 109.5 . . ? S4 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S4 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O15 S2 C40 106.47(11) . . ? O15 S2 C41 107.27(12) . . ? C40 S2 C41 97.47(12) . . ? S2 C40 H40A 109.5 . . ? S2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? S2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? S2 C41 H41A 109.5 . . ? S2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O15A S2A C40A 121(2) . . ? O15A S2A C41A 105.3(17) . . ? C40A S2A C41A 102.6(17) . . ? S2A C40A H40D 109.5 . . ? S2A C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? S2A C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? S2A C41A H41D 109.5 . . ? S2A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? S2A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? B2 O2 H2A 109.7(17) . . ? B2 O3 H3A 114.2(17) . . ? B1 O5 H5 113.9(19) . . ? B1 O6 H6 114.9(18) . . ? C5 N1 C1 117.13(13) . . ? C6 N2 C7 127.19(13) . . ? C6 N2 H2N 116.3(14) . . ? C7 N2 H2N 116.5(14) . . ? C11 N3 C10 120.91(14) . . ? C11 N3 C16 118.88(13) . . ? C10 N3 C16 120.19(13) . . ? C23 N4 C24 125.78(13) . . ? C23 N4 H4N 117.4(14) . . ? C24 N4 H4N 116.8(14) . . ? C30 N5 C32 121.27(14) . . ? C30 N5 C26 118.28(13) . . ? C32 N5 C26 120.41(13) . . ? N1 C1 C2 123.55(14) . . ? N1 C1 C6 117.46(13) . . ? C2 C1 C6 118.95(13) . . ? C3 C2 C1 118.43(14) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 118.77(15) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 118.46(14) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 123.61(14) . . ? N1 C5 C23 117.78(14) . . ? C4 C5 C23 118.60(14) . . ? O1 C6 N2 124.93(14) . . ? O1 C6 C1 121.09(14) . . ? N2 C6 C1 113.96(13) . . ? C15 C7 N2 124.54(14) . . ? C15 C7 C8 119.38(14) . . ? N2 C7 C8 116.07(13) . . ? C9 C8 C7 121.90(14) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 119.29(14) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N3 C10 C9 121.85(14) . . ? N3 C10 C14 118.69(14) . . ? C9 C10 C14 119.47(14) . . ? N3 C11 C12 121.86(15) . . ? N3 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C13 C12 C11 119.47(15) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 119.68(15) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C10 119.17(14) . . ? C13 C14 C15 120.79(14) . . ? C10 C14 C15 120.04(14) . . ? C7 C15 C14 119.73(14) . . ? C7 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? N3 C16 C17 113.15(13) . . ? N3 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? N3 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C22 119.37(15) . . ? C18 C17 C16 119.00(15) . . ? C22 C17 C16 121.43(15) . . ? C17 C18 C19 121.81(15) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 117.35(16) . . ? C20 C19 B2 121.92(15) . . ? C18 C19 B2 120.61(15) . . ? C21 C20 C19 121.54(16) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.78(16) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C17 C22 C21 120.03(16) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? O4 C23 N4 124.55(14) . . ? O4 C23 C5 120.30(14) . . ? N4 C23 C5 115.15(13) . . ? C27 C24 N4 123.32(14) . . ? C27 C24 C25 119.36(14) . . ? N4 C24 C25 117.32(13) . . ? C33 C25 C24 121.62(14) . . ? C33 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? N5 C26 C34 112.07(13) . . ? N5 C26 H26A 109.2 . . ? C34 C26 H26A 109.2 . . ? N5 C26 H26B 109.2 . . ? C34 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C24 C27 C28 119.87(14) . . ? C24 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C32 120.20(14) . . ? C27 C28 C29 120.41(14) . . ? C32 C28 C29 119.38(14) . . ? C31 C29 C28 119.97(15) . . ? C31 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? N5 C30 C31 122.02(15) . . ? N5 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C29 C31 C30 119.13(15) . . ? C29 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? N5 C32 C28 118.22(14) . . ? N5 C32 C33 122.27(14) . . ? C28 C32 C33 119.51(14) . . ? C25 C33 C32 119.43(14) . . ? C25 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C39 119.47(15) . . ? C35 C34 C26 118.39(15) . . ? C39 C34 C26 122.09(15) . . ? C34 C35 C36 121.79(15) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C37 C36 C35 117.55(15) . . ? C37 C36 B1 121.19(15) . . ? C35 C36 B1 121.25(15) . . ? C38 C37 C36 121.30(16) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C39 C38 C37 120.01(16) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 119.78(16) . . ? C38 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? O5 B1 O6 125.02(17) . . ? O5 B1 C36 117.38(16) . . ? O6 B1 C36 117.59(15) . . ? O2 B2 O3 124.51(17) . . ? O2 B2 C19 117.97(15) . . ? O3 B2 C19 117.51(16) . . ? H11A O11 H11B 105(2) . . ? H12A O12 H12B 109(3) . . ? H13A O13 H13B 99(4) . . ? H14A O14 H14B 99(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O9 1.4703(12) . ? S1 O8 1.4763(13) . ? S1 O7 1.4764(12) . ? S1 O10 1.4847(14) . ? S3 O16 1.5226(14) . ? S3 C43 1.7804(18) . ? S3 C42 1.7819(19) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? S4 O17 1.5094(14) . ? S4 C45 1.772(3) . ? S4 C44 1.773(2) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? S2 O15 1.4958(17) . ? S2 C40 1.770(2) . ? S2 C41 1.786(2) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? S2A O15A 1.407(17) . ? S2A C40A 1.736(18) . ? S2A C41A 1.817(18) . ? C40A H40D 0.9600 . ? C40A H40E 0.9600 . ? C40A H40F 0.9600 . ? C41A H41D 0.9600 . ? C41A H41E 0.9600 . ? C41A H41F 0.9600 . ? O1 C6 1.2247(19) . ? O2 B2 1.357(2) . ? O2 H2A 0.841(10) . ? O3 B2 1.360(2) . ? O3 H3A 0.843(10) . ? O4 C23 1.223(2) . ? O5 B1 1.353(2) . ? O5 H5 0.840(10) . ? O6 B1 1.356(2) . ? O6 H6 0.837(10) . ? N1 C5 1.336(2) . ? N1 C1 1.3374(19) . ? N2 C6 1.356(2) . ? N2 C7 1.3971(19) . ? N2 H2N 0.846(9) . ? N3 C11 1.335(2) . ? N3 C10 1.3867(19) . ? N3 C16 1.487(2) . ? N4 C23 1.365(2) . ? N4 C24 1.4034(19) . ? N4 H4N 0.852(9) . ? N5 C30 1.334(2) . ? N5 C32 1.3884(19) . ? N5 C26 1.483(2) . ? C1 C2 1.391(2) . ? C1 C6 1.506(2) . ? C2 C3 1.386(2) . ? C2 H2 0.9300 . ? C3 C4 1.386(2) . ? C3 H3 0.9300 . ? C4 C5 1.389(2) . ? C4 H4 0.9300 . ? C5 C23 1.503(2) . ? C7 C15 1.380(2) . ? C7 C8 1.421(2) . ? C8 C9 1.366(2) . ? C8 H8 0.9300 . ? C9 C10 1.414(2) . ? C9 H9 0.9300 . ? C10 C14 1.415(2) . ? C11 C12 1.392(2) . ? C11 H11 0.9300 . ? C12 C13 1.370(2) . ? C12 H12 0.9300 . ? C13 C14 1.414(2) . ? C13 H13 0.9300 . ? C14 C15 1.415(2) . ? C15 H15 0.9300 . ? C16 C17 1.513(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.390(2) . ? C17 C22 1.391(2) . ? C18 C19 1.403(2) . ? C18 H18 0.9300 . ? C19 C20 1.398(2) . ? C19 B2 1.577(3) . ? C20 C21 1.389(3) . ? C20 H20 0.9300 . ? C21 C22 1.393(2) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C24 C27 1.383(2) . ? C24 C25 1.419(2) . ? C25 C33 1.371(2) . ? C25 H25 0.9300 . ? C26 C34 1.513(2) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.410(2) . ? C27 H27 0.9300 . ? C28 C32 1.411(2) . ? C28 C29 1.415(2) . ? C29 C31 1.367(2) . ? C29 H29 0.9300 . ? C30 C31 1.388(2) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.412(2) . ? C33 H33 0.9300 . ? C34 C35 1.387(2) . ? C34 C39 1.394(2) . ? C35 C36 1.397(2) . ? C35 H35 0.9300 . ? C36 C37 1.397(2) . ? C36 B1 1.578(3) . ? C37 C38 1.390(2) . ? C37 H37 0.9300 . ? C38 C39 1.388(2) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? O11 H11A 0.827(10) . ? O11 H11B 0.829(9) . ? O12 H12A 0.848(10) . ? O12 H12B 0.846(10) . ? O13 H13A 0.843(10) . ? O13 H13B 0.841(10) . ? O14 H14A 0.840(10) . ? O14 H14B 0.840(10) . ? 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 _geom_hbond_publ_flag O2 H2A S1 0.841(10) 2.919(13) 3.7131(13) 158(2) . yes O2 H2A O7 0.841(10) 1.942(11) 2.7662(18) 166(2) . yes O3 H3A S1 0.843(10) 2.829(14) 3.5981(14) 153(2) . yes O3 H3A O10 0.843(10) 1.862(10) 2.7045(18) 179(3) . yes O5 H5 S1 0.840(10) 2.851(14) 3.6447(14) 158(2) . yes O5 H5 O10 0.840(10) 1.877(11) 2.7064(18) 169(3) . yes O6 H6 S1 0.837(10) 2.856(14) 3.6274(13) 154(2) . yes O6 H6 O8 0.837(10) 1.842(11) 2.6712(17) 170(2) . yes N2 H2N N1 0.846(9) 2.25(2) 2.6751(18) 111.2(16) . yes N2 H2N O11 0.846(9) 2.268(15) 2.9924(17) 143.7(19) 1_545 yes N4 H4N O11 0.852(9) 2.171(12) 2.9794(17) 158.4(19) 1_545 yes O11 H11A O9 0.827(10) 1.965(11) 2.7739(17) 166(2) . yes O11 H11B O12 0.829(9) 2.017(10) 2.8400(18) 172(2) . yes O12 H12A S2^a 0.848(10) 2.911(12) 3.7343(16) 164(2) . yes O12 H12A O15^a 0.848(10) 1.916(12) 2.746(2) 166(3) . yes O12 H12A S2A^b 0.848(10) 2.778(18) 3.567(11) 156(3) . yes O12 H12A O15A^b 0.848(10) 2.17(3) 2.97(3) 157(3) . yes O12 H12B S3 0.846(10) 3.011(14) 3.8027(15) 157(2) . yes O12 H12B O16 0.846(10) 1.951(11) 2.793(2) 173(3) . yes O13^a H13A^a O12 0.843(10) 1.937(12) 2.771(2) 170(4) . yes O13^a H13B^a S4 0.841(10) 2.71(3) 3.310(2) 129(3) . yes O13^a H13B^a O17 0.841(10) 2.135(16) 2.941(2) 160(4) . yes O14^a H14A^a O7 0.840(10) 2.080(18) 2.901(3) 165(6) . yes O14^a H14B^a O7 0.840(10) 2.17(3) 2.925(3) 150(5) 2_665 yes O14^a H14B^a O14^a 0.840(10) 2.32(5) 2.847(6) 121(5) 2_665 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 1.4(2) . . . . ? C5 N1 C1 C6 -176.35(13) . . . . ? N1 C1 C2 C3 -2.0(2) . . . . ? C6 C1 C2 C3 175.66(14) . . . . ? C1 C2 C3 C4 0.7(2) . . . . ? C2 C3 C4 C5 1.2(2) . . . . ? C1 N1 C5 C4 0.6(2) . . . . ? C1 N1 C5 C23 179.96(13) . . . . ? C3 C4 C5 N1 -1.9(2) . . . . ? C3 C4 C5 C23 178.76(15) . . . . ? C7 N2 C6 O1 -4.6(3) . . . . ? C7 N2 C6 C1 174.12(14) . . . . ? N1 C1 C6 O1 175.20(14) . . . . ? C2 C1 C6 O1 -2.6(2) . . . . ? N1 C1 C6 N2 -3.60(19) . . . . ? C2 C1 C6 N2 178.56(14) . . . . ? C6 N2 C7 C15 1.1(3) . . . . ? C6 N2 C7 C8 -177.61(15) . . . . ? C15 C7 C8 C9 4.0(2) . . . . ? N2 C7 C8 C9 -177.25(15) . . . . ? C7 C8 C9 C10 -2.1(2) . . . . ? C11 N3 C10 C9 174.64(15) . . . . ? C16 N3 C10 C9 -7.1(2) . . . . ? C11 N3 C10 C14 -4.9(2) . . . . ? C16 N3 C10 C14 173.37(13) . . . . ? C8 C9 C10 N3 178.29(15) . . . . ? C8 C9 C10 C14 -2.1(2) . . . . ? C10 N3 C11 C12 1.7(2) . . . . ? C16 N3 C11 C12 -176.60(15) . . . . ? N3 C11 C12 C13 2.4(3) . . . . ? C11 C12 C13 C14 -3.1(2) . . . . ? C12 C13 C14 C10 -0.2(2) . . . . ? C12 C13 C14 C15 179.79(15) . . . . ? N3 C10 C14 C13 4.1(2) . . . . ? C9 C10 C14 C13 -175.47(14) . . . . ? N3 C10 C14 C15 -175.82(14) . . . . ? C9 C10 C14 C15 4.6(2) . . . . ? N2 C7 C15 C14 179.91(14) . . . . ? C8 C7 C15 C14 -1.4(2) . . . . ? C13 C14 C15 C7 177.30(14) . . . . ? C10 C14 C15 C7 -2.8(2) . . . . ? C11 N3 C16 C17 -100.75(17) . . . . ? C10 N3 C16 C17 80.90(18) . . . . ? N3 C16 C17 C18 -139.86(15) . . . . ? N3 C16 C17 C22 45.4(2) . . . . ? C22 C17 C18 C19 0.9(2) . . . . ? C16 C17 C18 C19 -173.97(14) . . . . ? C17 C18 C19 C20 -3.0(2) . . . . ? C17 C18 C19 B2 173.12(14) . . . . ? C18 C19 C20 C21 1.9(2) . . . . ? B2 C19 C20 C21 -174.16(15) . . . . ? C19 C20 C21 C22 1.2(3) . . . . ? C18 C17 C22 C21 2.3(2) . . . . ? C16 C17 C22 C21 177.11(15) . . . . ? C20 C21 C22 C17 -3.4(3) . . . . ? C24 N4 C23 O4 1.3(3) . . . . ? C24 N4 C23 C5 -178.96(14) . . . . ? N1 C5 C23 O4 -168.49(16) . . . . ? C4 C5 C23 O4 10.9(2) . . . . ? N1 C5 C23 N4 11.8(2) . . . . ? C4 C5 C23 N4 -168.85(15) . . . . ? C23 N4 C24 C27 -7.7(2) . . . . ? C23 N4 C24 C25 172.94(15) . . . . ? C27 C24 C25 C33 -0.5(2) . . . . ? N4 C24 C25 C33 178.89(14) . . . . ? C30 N5 C26 C34 105.65(16) . . . . ? C32 N5 C26 C34 -72.09(18) . . . . ? N4 C24 C27 C28 -179.54(14) . . . . ? C25 C24 C27 C28 -0.2(2) . . . . ? C24 C27 C28 C32 0.7(2) . . . . ? C24 C27 C28 C29 -179.55(14) . . . . ? C27 C28 C29 C31 -178.44(15) . . . . ? C32 C28 C29 C31 1.3(2) . . . . ? C32 N5 C30 C31 -0.1(2) . . . . ? C26 N5 C30 C31 -177.85(15) . . . . ? C28 C29 C31 C30 -1.3(2) . . . . ? N5 C30 C31 C29 0.8(2) . . . . ? C30 N5 C32 C28 0.1(2) . . . . ? C26 N5 C32 C28 177.75(13) . . . . ? C30 N5 C32 C33 179.76(15) . . . . ? C26 N5 C32 C33 -2.6(2) . . . . ? C27 C28 C32 N5 179.09(14) . . . . ? C29 C28 C32 N5 -0.7(2) . . . . ? C27 C28 C32 C33 -0.6(2) . . . . ? C29 C28 C32 C33 179.66(14) . . . . ? C24 C25 C33 C32 0.6(2) . . . . ? N5 C32 C33 C25 -179.74(14) . . . . ? C28 C32 C33 C25 -0.1(2) . . . . ? N5 C26 C34 C35 150.70(14) . . . . ? N5 C26 C34 C39 -32.0(2) . . . . ? C39 C34 C35 C36 0.2(2) . . . . ? C26 C34 C35 C36 177.55(14) . . . . ? C34 C35 C36 C37 2.6(2) . . . . ? C34 C35 C36 B1 -175.90(15) . . . . ? C35 C36 C37 C38 -3.0(2) . . . . ? B1 C36 C37 C38 175.45(16) . . . . ? C36 C37 C38 C39 0.7(3) . . . . ? C37 C38 C39 C34 2.1(3) . . . . ? C35 C34 C39 C38 -2.6(2) . . . . ? C26 C34 C39 C38 -179.82(15) . . . . ? C37 C36 B1 O5 1.7(2) . . . . ? C35 C36 B1 O5 -179.95(16) . . . . ? C37 C36 B1 O6 -178.45(16) . . . . ? C35 C36 B1 O6 -0.1(2) . . . . ? C20 C19 B2 O2 178.68(15) . . . . ? C18 C19 B2 O2 2.7(2) . . . . ? C20 C19 B2 O3 -0.3(2) . . . . ? C18 C19 B2 O3 -176.22(15) . . . . ?