#------------------------------------------------------------------------------ #$Date: 2020-05-14 03:24:22 +0300 (Thu, 14 May 2020) $ #$Revision: 252037 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240512.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_7240512 loop_ _publ_author_name 'Liu, Mei' 'Shi, Lulu' 'Li, Hui' _publ_section_title ; A cucurbit[6]uril-based supramolecular assembly as a highly sensitive and quickly responsive luminescent sensor for the detection of fluoroquinolones antibiotics in simulated wastewater ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00603C _journal_year 2020 _chemical_formula_moiety '2(C12 H8 O6 S2), C39 H63 N25 Na4 O23, 2(H2 O)' _chemical_formula_sum 'C63 H83 N25 Na4 O37 S4' _chemical_formula_weight 2002.74 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-05-10 _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-05-10 deposited with the CCDC. 2020-05-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.691(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.2749(9) _cell_length_b 24.769(2) _cell_length_c 14.9058(12) _cell_measurement_reflns_used 9867 _cell_measurement_temperature 273 _cell_measurement_theta_max 28.40 _cell_measurement_theta_min 2.84 _cell_volume 4158.1(6) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 47673 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.010 _diffrn_reflns_theta_max 25.010 _diffrn_reflns_theta_min 2.736 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_T_max 0.7856 _exptl_absorpt_correction_T_min 0.5612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Bruker;sadabs;2018 _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.600 _exptl_crystal_description block _exptl_crystal_F_000 2080 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.151 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.101 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 681 _refine_ls_number_reflns 7338 _refine_ls_number_restraints 825 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0927 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+14.5232P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2203 _refine_ls_wR_factor_ref 0.2325 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6257 _reflns_number_total 7338 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; mo_20190721_shilulu_liumei_2_0.res created by SHELXL-2014/7 TITL mo_20190721_shilulu_liumei_2_0_a.res in P2(1)/n REM Old TITL mo_20190721_shilulu_liumei_2_0 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.238, Rweak 0.034, Alpha 0.061, Orientation as input REM Formula found by SHELXT: C70 N33 O26 S4 CELL 0.71073 11.2749 24.7692 14.9058 90 92.691 90 ZERR 2 0.0009 0.002 0.0012 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Na O S UNIT 126 166 50 8 74 8 DFIX 1.2 0.01 O3 C0AA DFIX 2.5 0.01 C0AA C1AA DFIX 2.3 0.01 O3 N0AA DFIX 1.5 0.01 N0AA C0AA N0AA C1AA DFIX 2.5 0.01 C2AA C1AA DFIX 2.5 0.01 C0AA C2AA DFIX 1.48 0.01 N0AA C2AA N0AA C1AA DFIX 1.48 0.01 N0AA C0AA DFIX 0.84 O10 H10b O10 H10a DFIX 1.46 H10b H10a DFIX 2.4 H10b Na2 DFIX 2.5 H10a Na2 DFIX 2.3 Na2 O10 SADI S002 O15 S002 O19 S002 O20 S002 O18 S002 O17 S002 O16 FLAT 0.01 C1AA C2AA N0AA C0AA O3 DELU SIMU SIMU 0.01 0.02 2 C0AA O3 N0AA C1AA C2AA RIGU 0.01 0.01 O3 C0AA N0AA C1AA C2AA ISOR 0.005 0.01 O15 O20 O18 O17 O16 O19 ISOR 0.005 0.01 Na3 Na2 O15 ISOR 0.001 0.002 O15 ISOR 0.01 0.02 O3 N0AA C0AA C2AA C1AA L.S. 50 0 132 PLAN 5 SIZE 0.19 0.12 0.08 TEMP 0 damp 600 list 4 fmap 2 acta OMIT 0 50.02 REM REM REM WGHT 0.113000 14.523201 FVAR 0.42200 S1 6 0.928792 0.803857 -0.073559 11.00000 0.03282 0.04135 = 0.02034 0.00933 0.00428 -0.00085 S002 6 0.950057 0.633373 0.579979 11.00000 0.08059 0.04902 = 0.02602 0.01610 -0.01200 -0.00688 NA1 4 0.206886 0.617473 -0.149777 11.00000 0.05187 0.05242 = 0.03766 -0.00118 -0.00439 -0.01241 O5 5 0.178335 0.619456 0.003708 11.00000 0.03455 0.04101 = 0.02905 0.00351 -0.00759 -0.00336 O7 5 0.878318 0.523083 0.006170 11.00000 0.03947 0.03724 = 0.02669 0.00327 -0.00739 0.00533 O8 5 0.785968 0.613939 0.147788 11.00000 0.03387 0.04356 = 0.03382 0.00341 -0.00276 0.00530 O4 5 0.387985 0.660694 -0.130029 11.00000 0.03087 0.04833 = 0.03376 0.00057 -0.00659 -0.00123 O9 5 0.567202 0.560777 0.279240 11.00000 0.03026 0.04917 = 0.05158 0.00077 -0.00886 0.00214 O6 5 0.514570 0.573175 -0.288373 11.00000 0.03300 0.05913 = 0.04466 -0.00472 -0.01350 0.00879 N4 3 0.206480 0.590100 0.149305 11.00000 0.02314 0.02818 = 0.02584 -0.00164 -0.00513 -0.00368 N2 3 0.472644 0.632867 0.210862 11.00000 0.02398 0.03478 = 0.02756 -0.00378 -0.00191 -0.00336 N12 3 0.828813 0.506334 -0.142884 11.00000 0.02322 0.02559 = 0.02406 0.00163 -0.00271 0.00258 N9 3 0.827245 0.590720 -0.092810 11.00000 0.02939 0.02477 = 0.02400 0.00062 -0.00182 0.00220 N5 3 0.465706 0.690136 0.006347 11.00000 0.02483 0.03043 = 0.02922 -0.00081 -0.00003 0.00048 N10 3 0.673891 0.609935 -0.207401 11.00000 0.02829 0.03427 = 0.02677 0.00048 -0.00280 0.00741 N8 3 0.750293 0.655370 0.011436 11.00000 0.02567 0.03016 = 0.02813 -0.00017 0.00009 0.00290 N1 3 0.364056 0.564722 0.258723 11.00000 0.02652 0.02974 = 0.02445 -0.00218 -0.00420 -0.00185 N3 3 0.313269 0.658654 0.104321 11.00000 0.02666 0.03062 = 0.02627 -0.00077 -0.00110 -0.00346 N6 3 0.624048 0.668320 0.117484 11.00000 0.02635 0.03770 = 0.02572 -0.00239 0.00021 -0.00137 N7 3 0.588308 0.670983 -0.100822 11.00000 0.02584 0.03071 = 0.02576 -0.00064 -0.00213 0.00155 N11 3 0.693259 0.529379 -0.268282 11.00000 0.02925 0.02956 = 0.02521 0.00054 -0.00549 0.00110 O2 5 0.089991 0.541881 -0.158728 11.00000 0.07310 0.07048 = 0.04332 0.00991 -0.00189 -0.02584 AFIX 7 H2A 2 0.107630 0.517484 -0.114197 11.00000 -1.50000 H2B 2 0.104776 0.521882 -0.207984 11.00000 -1.50000 AFIX 0 O1 5 0.084099 0.690217 -0.195151 11.00000 0.06682 0.07290 = 0.04707 -0.00433 -0.00943 0.01209 AFIX 7 H1A 2 0.015547 0.689871 -0.168039 11.00000 -1.50000 H1B 2 0.060796 0.687315 -0.252774 11.00000 -1.50000 AFIX 0 C2 1 0.228998 0.621841 0.077975 11.00000 0.02349 0.02401 = 0.02566 -0.00212 0.00001 0.00422 C28 1 0.929993 0.776877 0.036821 11.00000 0.02761 0.03101 = 0.01688 0.00178 -0.00043 -0.00251 C22 1 0.937001 0.708962 0.300846 11.00000 0.02913 0.02212 = 0.01872 -0.00369 -0.00380 -0.00152 C25 1 0.932414 0.732581 0.209214 11.00000 0.02698 0.02339 = 0.01733 -0.00291 -0.00205 -0.00440 C13 1 0.848156 0.538144 -0.068780 11.00000 0.01681 0.03145 = 0.02454 0.00217 -0.00079 0.00031 O21 5 0.842858 0.846198 -0.078423 11.00000 0.10726 0.08557 = 0.04453 0.02674 0.01627 0.04734 C27 1 0.843120 0.790848 0.095106 11.00000 0.02806 0.03083 = 0.02230 0.00168 -0.00183 0.00654 AFIX 43 H27 2 0.783290 0.814828 0.076821 11.00000 -1.20000 AFIX 0 C11 1 0.726679 0.642456 0.097469 11.00000 0.02441 0.02667 = 0.02813 -0.00419 -0.00318 -0.00292 C1 1 0.120045 0.547043 0.146069 11.00000 0.01975 0.02882 = 0.02967 -0.00063 -0.00142 0.00033 AFIX 23 H1C 2 0.072716 0.549573 0.198594 11.00000 -1.20000 H1D 2 0.067153 0.552029 0.093505 11.00000 -1.20000 AFIX 0 C26 1 0.845414 0.769060 0.180720 11.00000 0.02601 0.03237 = 0.01891 -0.00177 0.00344 0.00475 AFIX 43 H26 2 0.787451 0.779104 0.219846 11.00000 -1.20000 AFIX 0 O22 5 0.894792 0.759553 -0.132294 11.00000 0.14718 0.06612 = 0.02879 0.00433 -0.00504 -0.03113 C4 1 0.277147 0.604524 0.229002 11.00000 0.02481 0.03000 = 0.01959 -0.00506 0.00332 -0.00005 AFIX 13 H4 2 0.227104 0.615376 0.277897 11.00000 -1.20000 AFIX 0 C15 1 0.796531 0.596702 -0.186879 11.00000 0.02595 0.02759 = 0.02096 0.00243 0.00448 -0.00132 AFIX 13 H15 2 0.850370 0.621539 -0.216022 11.00000 -1.20000 AFIX 0 C21 1 0.833476 0.703190 0.348080 11.00000 0.02833 0.03203 = 0.02464 0.00234 -0.00531 -0.00530 AFIX 43 H21 2 0.761527 0.715182 0.322279 11.00000 -1.20000 AFIX 0 C12 1 0.853153 0.635285 -0.032184 11.00000 0.01774 0.03108 = 0.03168 -0.00245 -0.00118 -0.00107 AFIX 23 H12A 2 0.911904 0.623695 0.013414 11.00000 -1.20000 H12B 2 0.887574 0.664523 -0.065573 11.00000 -1.20000 AFIX 0 C9 1 0.471975 0.672627 -0.080100 11.00000 0.03051 0.02036 = 0.03249 0.00503 -0.00052 0.00220 C3 1 0.352648 0.652142 0.197074 11.00000 0.02772 0.02680 = 0.02134 -0.00738 0.00142 -0.00010 AFIX 13 H3 2 0.339100 0.684921 0.231961 11.00000 -1.20000 AFIX 0 C14 1 0.807323 0.538480 -0.222838 11.00000 0.02680 0.03020 = 0.02026 0.00005 0.00567 -0.00023 AFIX 13 H14 2 0.872238 0.535158 -0.263965 11.00000 -1.20000 AFIX 0 C5 1 0.477447 0.583798 0.252466 11.00000 0.02855 0.03458 = 0.02267 -0.00760 -0.00436 -0.00039 C10 1 0.665976 0.692990 -0.029655 11.00000 0.02290 0.02406 = 0.03123 0.00127 0.00116 -0.00103 AFIX 13 H10 2 0.705009 0.726147 -0.048690 11.00000 -1.20000 AFIX 0 C16 1 0.615673 0.570867 -0.257478 11.00000 0.02989 0.03706 = 0.02080 0.00551 -0.00109 0.00426 C6 1 0.576244 0.666561 0.206007 11.00000 0.02864 0.03813 = 0.02497 -0.01018 -0.00213 -0.00823 AFIX 23 H6A 2 0.637205 0.653341 0.248552 11.00000 -1.20000 H6B 2 0.555986 0.702962 0.223772 11.00000 -1.20000 AFIX 0 O23 5 1.045146 0.821632 -0.086878 11.00000 0.04991 0.15091 = 0.05352 0.04627 0.00771 -0.01625 C18 1 0.663310 0.480417 -0.316046 11.00000 0.03594 0.03856 = 0.01660 0.00020 -0.00371 -0.00460 AFIX 23 H18A 2 0.729275 0.470453 -0.352128 11.00000 -1.20000 H18B 2 0.595303 0.487333 -0.356702 11.00000 -1.20000 AFIX 0 O11 5 0.841393 0.539082 0.290899 11.00000 0.06639 0.07824 = 0.10261 0.02931 -0.00178 0.01026 PART 1 AFIX 3 H11A 2 0.818463 0.552022 0.240179 10.50000 -1.50000 H11B 2 0.890603 0.514492 0.278459 10.50000 -1.50000 AFIX 3 PART 0 PART 2 H11C 2 0.830973 0.562782 0.250049 10.50000 -1.50000 H11D 2 0.898703 0.519972 0.273749 10.50000 -1.50000 AFIX 0 PART 0 C19 1 0.943278 0.661925 0.470751 11.00000 0.05068 0.03083 = 0.02037 0.00181 -0.00722 -0.00509 C17 1 0.623580 0.662553 -0.191872 11.00000 0.03558 0.03150 = 0.02555 0.00811 0.00042 0.00843 AFIX 23 H17A 2 0.554728 0.667441 -0.232560 11.00000 -1.20000 H17B 2 0.681426 0.689867 -0.206076 11.00000 -1.20000 AFIX 0 C7 1 0.354163 0.701226 0.046640 11.00000 0.02628 0.02611 = 0.03495 0.00387 0.00065 0.00477 AFIX 23 H7A 2 0.294014 0.707535 -0.000878 11.00000 -1.20000 H7B 2 0.362409 0.734183 0.081528 11.00000 -1.20000 AFIX 0 C24 1 1.046589 0.668365 0.425886 11.00000 0.03764 0.03788 = 0.03250 0.00395 -0.01181 0.00636 AFIX 43 H24 2 1.118638 0.656950 0.452307 11.00000 -1.20000 AFIX 0 C23 1 1.042991 0.691689 0.342008 11.00000 0.03115 0.03431 = 0.02851 0.00087 -0.00040 0.00260 AFIX 43 H23 2 1.113145 0.695941 0.312358 11.00000 -1.20000 AFIX 0 C30 1 1.017826 0.718438 0.148724 11.00000 0.03317 0.04196 = 0.03119 0.00535 0.00281 0.01756 AFIX 43 H30 2 1.076564 0.693703 0.166094 11.00000 -1.20000 AFIX 0 C20 1 0.836301 0.679923 0.432606 11.00000 0.03676 0.03802 = 0.02411 0.00276 -0.00069 -0.00746 AFIX 43 H20 2 0.766899 0.676430 0.463447 11.00000 -1.20000 AFIX 0 C8 1 0.580212 0.704111 0.046825 11.00000 0.02797 0.02451 = 0.03332 -0.00298 0.00338 -0.00290 AFIX 13 H8 2 0.583170 0.741963 0.065937 11.00000 -1.20000 AFIX 0 C29 1 1.016960 0.740435 0.063474 11.00000 0.03173 0.05367 = 0.02445 0.00469 0.00908 0.01131 AFIX 43 H29 2 1.074956 0.730655 0.024201 11.00000 -1.20000 AFIX 0 O10 5 0.750322 0.404666 0.296977 11.00000 0.08683 0.08117 = 0.08302 -0.00499 0.03247 -0.01640 PART 1 NA3 4 0.672752 0.498190 0.362379 10.50000 0.06888 0.08152 = 0.08770 0.05280 0.02920 0.03449 PART 0 AFIX 6 O13 5 0.947198 0.471306 0.599168 11.00000 0.10570 0.08530 = 0.08785 -0.00505 0.02567 0.00191 H13A 2 0.904630 0.462387 0.552973 11.00000 -1.50000 H13B 2 0.963649 0.504722 0.596520 11.00000 -1.50000 AFIX 0 PART 1 O19 5 0.998809 0.674350 0.635796 10.75000 0.17031 0.09066 = 0.03725 0.01188 -0.03033 -0.04013 O15 5 1.017353 0.585322 0.575689 10.75000 0.10322 0.08995 = 0.09197 0.00830 0.00132 0.00669 O17 5 0.831527 0.620053 0.600885 10.75000 0.09902 0.16996 = 0.05839 0.05891 0.00707 -0.01466 O14 5 0.636128 0.572846 0.493115 10.50000 0.08450 0.06308 = 0.07142 0.03880 -0.01909 -0.00847 AFIX 7 H14A 2 0.563002 0.571385 0.509244 10.50000 -1.50000 H14B 2 0.677497 0.564528 0.541955 10.50000 -1.50000 AFIX 0 PART 0 PART 2 O12 5 0.612448 0.440462 0.462599 10.50000 0.11368 0.11154 = 0.04118 0.00210 -0.01890 0.00397 AFIX 7 H12C 2 0.583484 0.465040 0.495046 10.50000 -1.50000 H12D 2 0.677047 0.431501 0.490654 10.50000 -1.50000 AFIX 0 PART 0 O3 5 0.360012 0.536072 -0.125786 10.50000 0.08460 0.07070 = 0.09663 0.00753 0.00864 0.00741 PART 2 O20 5 1.071651 0.610083 0.588216 10.25000 0.05603 0.09466 = 0.05044 0.04407 -0.01592 0.00412 O16 5 0.883970 0.585782 0.577146 10.25000 0.07712 0.04532 = 0.04486 0.02059 -0.00588 -0.01345 O18 5 0.920774 0.673283 0.641575 10.25000 0.10098 0.06586 = 0.03653 0.00367 0.00119 -0.00012 NA2 4 0.662029 0.483000 0.296274 10.50000 0.04256 0.04739 = 0.10353 0.00244 -0.00585 0.01020 PART 0 PART -1 N0AA 3 0.484053 0.500620 9.987370 10.50000 0.08291 0.03748 = 0.06883 0.00200 0.02610 -0.00543 PART 0 C0AA 1 0.392857 0.497191 -0.084872 10.50000 0.09065 0.06502 = 0.09159 0.00199 0.00692 -0.00672 AFIX 43 H0AA 2 0.359476 0.463799 -0.099382 10.50000 -1.20000 AFIX 0 PART -1 C1AA 1 0.536616 0.553171 0.010858 10.50000 0.12542 0.07259 = 0.13101 0.00283 -0.03108 -0.01553 AFIX 33 H1AA 2 0.501402 0.580525 -0.027459 10.50000 -1.50000 H1AB 2 0.522254 0.561456 0.072321 10.50000 -1.50000 H1AC 2 0.620618 0.551950 0.003096 10.50000 -1.50000 AFIX 0 C2AA 1 0.524112 0.453575 0.036707 10.50000 0.17401 0.07392 = 0.13373 0.02393 -0.02059 -0.00592 AFIX 3 H2AA 2 0.583832 0.463875 0.081457 10.50000 -1.50000 H2AB 2 0.458392 0.437375 0.065307 10.50000 -1.50000 H2AC 2 0.556972 0.428085 -0.003823 10.50000 -1.50000 AFIX 0 PART 0 H10A 2 0.808259 0.409520 0.334135 11.00000 0.48633 H10B 2 0.690586 0.387493 0.313737 11.00000 0.26396 HKLF 4 REM mo_20190721_shilulu_liumei_2_0_a.res in P2(1)/n REM R1 = 0.0927 for 6257 Fo > 4sig(Fo) and 0.1138 for all 7338 data REM 681 parameters refined using 825 restraints END WGHT 0.1131 14.4357 REM Highest difference peak 1.151, deepest hole -0.757, 1-sigma level 0.101 Q1 1 0.6465 0.4791 0.4449 11.00000 0.05 1.15 Q2 1 1.0333 0.7817 -0.1143 11.00000 0.05 1.09 Q3 1 1.0719 0.6489 0.6203 11.00000 0.05 1.07 Q4 1 0.8225 0.7897 -0.1188 11.00000 0.05 0.91 Q5 1 0.7003 0.5115 0.4108 11.00000 0.05 0.80 REM The information below was added by Olex2. REM REM R1 = 0.0927 for 6257 Fo > 4sig(Fo) and 0.1138 for all 60148 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.15, deepest hole -0.76 REM Mean Shift 0, Max Shift 0.046. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1138 REM R1_gt = 0.0927 REM wR_ref = 0.2325 REM GOOF = 1.076 REM Shift_max = 0.046 REM Shift_mean = 0 REM Reflections_all = 60148 REM Reflections_gt = 6257 REM Parameters = n/a REM Hole = -0.76 REM Peak = 1.15 REM Flack = n/a ; _cod_data_source_file d0ce00603c2.cif _cod_data_source_block mo_20190721_shilulu_liumei_2_0 _cod_original_cell_volume 4158.2(6) _cod_database_code 7240512 _shelx_shelxl_version_number 2014/7 _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_max 0.981 _shelx_estimated_absorpt_t_min 0.955 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups, All O(H,H,H,H) groups 2. Restrained distances O3-C0AA 1.2 with sigma of 0.01 C0AA-C1AA 2.5 with sigma of 0.01 O3-N0AA 2.3 with sigma of 0.01 N0AA-C0AA = N0AA-C1AA 1.5 with sigma of 0.01 C2AA-C1AA 2.5 with sigma of 0.01 C0AA-C2AA 2.5 with sigma of 0.01 N0AA-C2AA = N0AA-C1AA 1.48 with sigma of 0.01 N0AA-C0AA 1.48 with sigma of 0.01 O10-H10B = O10-H10A 0.84 with sigma of 0.02 H10B-H10A 1.46 with sigma of 0.02 H10B-Na2 2.4 with sigma of 0.02 H10A-Na2 2.5 with sigma of 0.02 Na2-O10 2.3 with sigma of 0.02 S002-O15 \\sim S002-O19 \\sim S002-O20 \\sim S002-O18 \\sim S002-O17 \\sim S002-O16 with sigma of 0.02 3. Restrained planarity C1AA, C2AA, N0AA, C0AA, O3 with sigma of 0.01 4. Rigid bond restraints All non-hydrogen atoms with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C0AA \\sim O3 \\sim N0AA \\sim C1AA \\sim C2AA: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O15) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(Na3) \\sim Ueq, Uanis(Na2) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(O15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O3) \\sim Ueq, Uanis(N0AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 6. Rigid body (RIGU) restrains O3, C0AA, N0AA, C1AA, C2AA with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 7. Others Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) H11D(0.5) Na3(0.5) O19(0.75) O15(0.75) O17(0.75) O14(0.5) H14A(0.5) H14B(0.5) O12(0.5) H12C(0.5) H12D(0.5) O3(0.5) O20(0.25) O16(0.25) O18(0.25) Na2(0.5) N0AA(0.5) C0AA(0.5) H0AA(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) Fixed Z: N0AA(-0.01263) 8.a Riding coordinates: O11(H11A,H11B), O11(H11C,H11D), C2AA(H2AA,H2AB,H2AC) 8.b Free rotating group: O13(H13A,H13B) 8.c Rotating group: O2(H2A,H2B), O1(H1A,H1B), O14(H14A,H14B), O12(H12C,H12D) 8.d Ternary CH refined with riding coordinates: C4(H4), C15(H15), C3(H3), C14(H14), C10(H10), C8(H8) 8.e Secondary CH2 refined with riding coordinates: C1(H1C,H1D), C12(H12A,H12B), C6(H6A,H6B), C18(H18A,H18B), C17(H17A,H17B), C7(H7A,H7B) 8.f Me refined with riding coordinates: C1AA(H1AA,H1AB,H1AC) 8.g Aromatic/amide H refined with riding coordinates: C27(H27), C26(H26), C21(H21), C24(H24), C23(H23), C30(H30), C20(H20), C29(H29), C0AA(H0AA) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.92879(8) 0.80386(4) -0.07356(6) 0.0314(2) Uani 1 1 d . U . . . S002 S 0.95006(12) 0.63337(5) 0.57998(7) 0.0523(3) Uani 1 1 d D U . . . Na1 Na 0.20689(15) 0.61747(7) -0.14978(11) 0.0475(4) Uani 1 1 d . U . . . O5 O 0.1783(2) 0.61946(10) 0.00371(16) 0.0352(6) Uani 1 1 d . U . . . O7 O 0.8783(2) 0.52308(10) 0.00617(16) 0.0347(6) Uani 1 1 d . U . . . O8 O 0.7860(2) 0.61394(11) 0.14779(17) 0.0372(6) Uani 1 1 d . U . . . O4 O 0.3880(2) 0.66069(11) -0.13003(17) 0.0379(6) Uani 1 1 d . U . . . O9 O 0.5672(2) 0.56078(12) 0.2792(2) 0.0440(7) Uani 1 1 d . U . . . O6 O 0.5146(2) 0.57318(12) -0.28837(19) 0.0461(7) Uani 1 1 d . U . . . N4 N 0.2065(2) 0.59010(11) 0.14930(18) 0.0259(6) Uani 1 1 d . U . . . N2 N 0.4726(3) 0.63287(12) 0.21086(19) 0.0289(7) Uani 1 1 d . U . . . N12 N 0.8288(2) 0.50633(11) -0.14288(18) 0.0244(6) Uani 1 1 d . U . . . N9 N 0.8272(2) 0.59072(11) -0.09281(18) 0.0262(6) Uani 1 1 d . U . . . N5 N 0.4657(2) 0.69014(11) 0.00635(19) 0.0282(7) Uani 1 1 d . U . . . N10 N 0.6739(3) 0.60993(12) -0.20740(19) 0.0299(7) Uani 1 1 d . U . . . N8 N 0.7503(3) 0.65537(11) 0.01144(19) 0.0280(7) Uani 1 1 d . U . . . N1 N 0.3641(3) 0.56472(11) 0.25872(19) 0.0271(6) Uani 1 1 d . U . . . N3 N 0.3133(3) 0.65865(11) 0.10432(19) 0.0279(7) Uani 1 1 d . U . . . N6 N 0.6240(3) 0.66832(12) 0.11748(19) 0.0300(7) Uani 1 1 d . U . . . N7 N 0.5883(2) 0.67098(11) -0.10082(19) 0.0275(7) Uani 1 1 d . U . . . N11 N 0.6933(3) 0.52938(11) -0.26828(19) 0.0282(7) Uani 1 1 d . U . . . O2 O 0.0900(3) 0.54188(14) -0.1587(2) 0.0624(9) Uani 1 1 d . U . . . H2A H 0.1076 0.5175 -0.1142 0.094 Uiso 1 1 d GR . . . . H2B H 0.1048 0.5219 -0.2080 0.094 Uiso 1 1 d GR . . . . O1 O 0.0841(3) 0.69022(14) -0.1952(2) 0.0626(9) Uani 1 1 d . U . . . H1A H 0.0155 0.6899 -0.1680 0.094 Uiso 1 1 d GR . . . . H1B H 0.0608 0.6873 -0.2528 0.094 Uiso 1 1 d GR . . . . C2 C 0.2290(3) 0.62184(13) 0.0780(2) 0.0244(7) Uani 1 1 d . U . . . C28 C 0.9300(3) 0.77688(13) 0.0368(2) 0.0252(7) Uani 1 1 d . U . . . C22 C 0.9370(3) 0.70896(12) 0.3008(2) 0.0235(7) Uani 1 1 d . U . . . C25 C 0.9324(3) 0.73258(12) 0.2092(2) 0.0227(7) Uani 1 1 d . U . . . C13 C 0.8482(3) 0.53814(13) -0.0688(2) 0.0243(7) Uani 1 1 d . U . . . O21 O 0.8429(4) 0.84620(15) -0.0784(2) 0.0787(11) Uani 1 1 d . U . . . C27 C 0.8431(3) 0.79085(14) 0.0951(2) 0.0272(8) Uani 1 1 d . U . . . H27 H 0.7833 0.8148 0.0768 0.033 Uiso 1 1 calc R . . . . C11 C 0.7267(3) 0.64246(13) 0.0975(2) 0.0265(8) Uani 1 1 d . U . . . C1 C 0.1200(3) 0.54704(13) 0.1461(2) 0.0262(8) Uani 1 1 d . U . . . H1C H 0.0727 0.5496 0.1986 0.031 Uiso 1 1 calc R . . . . H1D H 0.0672 0.5520 0.0935 0.031 Uiso 1 1 calc R . . . . C26 C 0.8454(3) 0.76906(13) 0.1807(2) 0.0257(7) Uani 1 1 d . U . . . H26 H 0.7875 0.7791 0.2198 0.031 Uiso 1 1 calc R . . . . O22 O 0.8948(4) 0.75955(15) -0.1323(2) 0.0810(12) Uani 1 1 d . U . . . C4 C 0.2771(3) 0.60452(13) 0.2290(2) 0.0247(7) Uani 1 1 d . U . . . H4 H 0.2271 0.6154 0.2779 0.030 Uiso 1 1 calc R . . . . C15 C 0.7965(3) 0.59670(13) -0.1869(2) 0.0247(7) Uani 1 1 d . U . . . H15 H 0.8504 0.6215 -0.2160 0.030 Uiso 1 1 calc R . . . . C21 C 0.8335(3) 0.70319(14) 0.3481(2) 0.0285(8) Uani 1 1 d . U . . . H21 H 0.7615 0.7152 0.3223 0.034 Uiso 1 1 calc R . . . . C12 C 0.8532(3) 0.63529(14) -0.0322(2) 0.0269(8) Uani 1 1 d . U . . . H12A H 0.9119 0.6237 0.0134 0.032 Uiso 1 1 calc R . . . . H12B H 0.8876 0.6645 -0.0656 0.032 Uiso 1 1 calc R . . . . C9 C 0.4720(3) 0.67263(13) -0.0801(2) 0.0278(8) Uani 1 1 d . U . . . C3 C 0.3526(3) 0.65214(13) 0.1971(2) 0.0253(7) Uani 1 1 d . U . . . H3 H 0.3391 0.6849 0.2320 0.030 Uiso 1 1 calc R . . . . C14 C 0.8073(3) 0.53848(13) -0.2228(2) 0.0256(7) Uani 1 1 d . U . . . H14 H 0.8722 0.5352 -0.2640 0.031 Uiso 1 1 calc R . . . . C5 C 0.4774(3) 0.58380(14) 0.2525(2) 0.0288(8) Uani 1 1 d . U . . . C10 C 0.6660(3) 0.69299(13) -0.0297(2) 0.0261(7) Uani 1 1 d . U . . . H10 H 0.7050 0.7261 -0.0487 0.031 Uiso 1 1 calc R . . . . C16 C 0.6157(3) 0.57087(14) -0.2575(2) 0.0293(8) Uani 1 1 d . U . . . C6 C 0.5762(3) 0.66656(15) 0.2060(2) 0.0307(8) Uani 1 1 d . U . . . H6A H 0.6372 0.6533 0.2486 0.037 Uiso 1 1 calc R . . . . H6B H 0.5560 0.7030 0.2238 0.037 Uiso 1 1 calc R . . . . O23 O 1.0451(3) 0.8216(2) -0.0869(2) 0.0846(12) Uani 1 1 d . U . . . C18 C 0.6633(3) 0.48042(14) -0.3160(2) 0.0305(8) Uani 1 1 d . U . . . H18A H 0.7293 0.4705 -0.3521 0.037 Uiso 1 1 calc R . . . . H18B H 0.5953 0.4873 -0.3567 0.037 Uiso 1 1 calc R . . . . O11 O 0.8414(3) 0.53908(16) 0.2909(3) 0.0826(12) Uani 1 1 d . U . . . H11A H 0.8185 0.5520 0.2402 0.124 Uiso 0.5 1 d R . P A 1 H11B H 0.8906 0.5145 0.2785 0.124 Uiso 0.5 1 d R . P A 1 H11C H 0.8310 0.5628 0.2500 0.124 Uiso 0.5 1 d R . P B 2 H11D H 0.8987 0.5200 0.2737 0.124 Uiso 0.5 1 d R . P B 2 C19 C 0.9433(4) 0.66193(14) 0.4708(2) 0.0342(9) Uani 1 1 d . U . . . C17 C 0.6236(3) 0.66255(14) -0.1919(2) 0.0309(8) Uani 1 1 d . U . . . H17A H 0.5547 0.6674 -0.2326 0.037 Uiso 1 1 calc R . . . . H17B H 0.6814 0.6899 -0.2061 0.037 Uiso 1 1 calc R . . . . C7 C 0.3542(3) 0.70123(13) 0.0466(2) 0.0291(8) Uani 1 1 d . U . . . H7A H 0.2940 0.7075 -0.0009 0.035 Uiso 1 1 calc R . . . . H7B H 0.3624 0.7342 0.0815 0.035 Uiso 1 1 calc R . . . . C24 C 1.0466(4) 0.66836(15) 0.4259(3) 0.0364(9) Uani 1 1 d . U . . . H24 H 1.1186 0.6570 0.4523 0.044 Uiso 1 1 calc R . . . . C23 C 1.0430(3) 0.69169(14) 0.3420(2) 0.0314(8) Uani 1 1 d . U . . . H23 H 1.1131 0.6959 0.3124 0.038 Uiso 1 1 calc R . . . . C30 C 1.0178(3) 0.71844(15) 0.1487(2) 0.0354(9) Uani 1 1 d . U . . . H30 H 1.0766 0.6937 0.1661 0.042 Uiso 1 1 calc R . . . . C20 C 0.8363(3) 0.67992(15) 0.4326(2) 0.0330(8) Uani 1 1 d . U . . . H20 H 0.7669 0.6764 0.4634 0.040 Uiso 1 1 calc R . . . . C8 C 0.5802(3) 0.70411(13) 0.0468(2) 0.0285(8) Uani 1 1 d . U . . . H8 H 0.5832 0.7420 0.0659 0.034 Uiso 1 1 calc R . . . . C29 C 1.0170(3) 0.74043(16) 0.0635(2) 0.0364(9) Uani 1 1 d . U . . . H29 H 1.0750 0.7307 0.0242 0.044 Uiso 1 1 calc R . . . . O10 O 0.7503(4) 0.40467(17) 0.2970(3) 0.0828(11) Uani 1 1 d D U . . . Na3 Na 0.6728(4) 0.49819(18) 0.3624(3) 0.0786(11) Uani 0.5 1 d . U P C 1 O13 O 0.9472(4) 0.47131(19) 0.5992(3) 0.0923(14) Uani 1 1 d . U . . . H13A H 0.9046 0.4624 0.5530 0.138 Uiso 1 1 d G . . . . H13B H 0.9636 0.5047 0.5965 0.138 Uiso 1 1 d G . . . . O19 O 0.9988(7) 0.6744(2) 0.6358(3) 0.1005(19) Uani 0.75 1 d D U P D 1 O15 O 1.0174(6) 0.5853(2) 0.5757(4) 0.0951(13) Uani 0.75 1 d D U P D 1 O17 O 0.8315(5) 0.6201(3) 0.6009(4) 0.1090(19) Uani 0.75 1 d D U P D 1 O14 O 0.6361(7) 0.5728(3) 0.4931(5) 0.0737(19) Uani 0.5 1 d . U P C 1 H14A H 0.5630 0.5714 0.5092 0.111 Uiso 0.5 1 d GR . P C 1 H14B H 0.6775 0.5645 0.5420 0.111 Uiso 0.5 1 d GR . P C 1 O12 O 0.6124(9) 0.4405(4) 0.4626(5) 0.090(3) Uani 0.5 1 d . U P C 2 H12C H 0.5835 0.4650 0.4950 0.134 Uiso 0.5 1 d GR . P C 2 H12D H 0.6770 0.4315 0.4907 0.134 Uiso 0.5 1 d GR . P C 2 O3 O 0.3600(5) 0.5361(3) -0.1258(4) 0.0838(19) Uani 0.5 1 d D U P E . O20 O 1.0717(9) 0.6101(6) 0.5882(9) 0.068(3) Uani 0.25 1 d D U P D 2 O16 O 0.8840(11) 0.5858(4) 0.5771(8) 0.056(3) Uani 0.25 1 d D U P D 2 O18 O 0.9208(15) 0.6733(5) 0.6416(8) 0.068(3) Uani 0.25 1 d D U P D 2 Na2 Na 0.6620(3) 0.48300(14) 0.2963(3) 0.0648(10) Uani 0.5 1 d D U P C 2 N0AA N 0.48405(16) 0.5006(2) -0.0126 0.0624(16) Uani 0.5 1 d D U P E -1 C0AA C 0.3929(4) 0.4972(3) -0.0849(3) 0.082(2) Uani 0.5 1 d D U P . . H0AA H 0.3595 0.4638 -0.0994 0.099 Uiso 0.5 1 calc R . P E . C1AA C 0.5366(5) 0.5532(2) 0.0109(4) 0.111(4) Uani 0.5 1 d D U P E -1 H1AA H 0.5014 0.5805 -0.0275 0.166 Uiso 0.5 1 calc R . P E -1 H1AB H 0.5223 0.5615 0.0723 0.166 Uiso 0.5 1 calc R . P E -1 H1AC H 0.6206 0.5520 0.0031 0.166 Uiso 0.5 1 calc R . P E -1 C2AA C 0.5241(4) 0.4536(2) 0.0367(3) 0.128(4) Uani 0.5 1 d D U P E -1 H2AA H 0.5838 0.4639 0.0815 0.192 Uiso 0.5 1 d R . P E -1 H2AB H 0.4584 0.4374 0.0653 0.192 Uiso 0.5 1 d R . P E -1 H2AC H 0.5570 0.4281 -0.0038 0.192 Uiso 0.5 1 d R . P E -1 H10A H 0.8083(14) 0.4095(9) 0.334(2) 0.49(14) Uiso 1 1 d D . . . . H10B H 0.6906(14) 0.3875(6) 0.314(3) 0.26(6) Uiso 1 1 d 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 S1 0.0328(5) 0.0413(5) 0.0203(4) 0.0093(4) 0.0043(3) -0.0008(4) S002 0.0806(8) 0.0490(6) 0.0260(5) 0.0161(4) -0.0120(5) -0.0069(6) Na1 0.0519(9) 0.0524(9) 0.0377(8) -0.0012(7) -0.0044(7) -0.0124(8) O5 0.0346(13) 0.0410(13) 0.0291(12) 0.0035(11) -0.0076(10) -0.0034(11) O7 0.0395(14) 0.0372(13) 0.0267(12) 0.0033(11) -0.0074(11) 0.0053(11) O8 0.0339(14) 0.0436(14) 0.0338(13) 0.0034(12) -0.0028(11) 0.0053(11) O4 0.0309(13) 0.0483(14) 0.0338(13) 0.0006(12) -0.0066(11) -0.0012(12) O9 0.0303(14) 0.0492(15) 0.0516(16) 0.0008(13) -0.0089(12) 0.0021(12) O6 0.0330(14) 0.0591(17) 0.0447(15) -0.0047(14) -0.0135(12) 0.0088(13) N4 0.0231(14) 0.0282(13) 0.0258(14) -0.0016(12) -0.0051(11) -0.0037(11) N2 0.0240(14) 0.0348(14) 0.0276(14) -0.0038(12) -0.0019(12) -0.0034(12) N12 0.0232(14) 0.0256(12) 0.0241(13) 0.0016(11) -0.0027(11) 0.0026(11) N9 0.0294(15) 0.0248(12) 0.0240(13) 0.0006(11) -0.0018(11) 0.0022(12) N5 0.0248(14) 0.0304(14) 0.0292(14) -0.0008(12) 0.0000(11) 0.0005(12) N10 0.0283(15) 0.0343(14) 0.0268(14) 0.0005(12) -0.0028(12) 0.0074(12) N8 0.0257(14) 0.0302(14) 0.0281(14) -0.0002(12) 0.0001(11) 0.0029(12) N1 0.0265(14) 0.0297(13) 0.0245(14) -0.0022(12) -0.0042(11) -0.0019(12) N3 0.0267(14) 0.0306(14) 0.0263(14) -0.0008(12) -0.0011(11) -0.0035(12) N6 0.0263(15) 0.0377(15) 0.0257(14) -0.0024(12) 0.0002(11) -0.0014(12) N7 0.0258(14) 0.0307(14) 0.0258(14) -0.0006(12) -0.0021(11) 0.0016(12) N11 0.0292(15) 0.0296(13) 0.0252(14) 0.0005(12) -0.0055(12) 0.0011(12) O2 0.073(2) 0.0705(19) 0.0433(17) 0.0099(15) -0.0019(16) -0.0258(16) O1 0.067(2) 0.073(2) 0.0471(17) -0.0043(16) -0.0094(16) 0.0121(17) C2 0.0235(16) 0.0240(14) 0.0257(15) -0.0021(13) 0.0000(13) 0.0042(13) C28 0.0276(17) 0.0310(16) 0.0169(14) 0.0018(13) -0.0004(13) -0.0025(14) C22 0.0291(17) 0.0221(14) 0.0187(15) -0.0037(12) -0.0038(13) -0.0015(13) C25 0.0270(16) 0.0234(14) 0.0173(14) -0.0029(12) -0.0021(12) -0.0044(13) C13 0.0168(15) 0.0314(15) 0.0245(16) 0.0022(13) -0.0008(13) 0.0003(13) O21 0.107(3) 0.086(2) 0.0445(18) 0.0267(17) 0.0163(18) 0.047(2) C27 0.0281(17) 0.0308(16) 0.0223(16) 0.0017(14) -0.0018(13) 0.0065(14) C11 0.0244(17) 0.0267(15) 0.0281(16) -0.0042(14) -0.0032(13) -0.0029(13) C1 0.0197(16) 0.0288(15) 0.0297(17) -0.0006(14) -0.0014(13) 0.0003(13) C26 0.0260(16) 0.0324(16) 0.0189(15) -0.0018(13) 0.0034(13) 0.0047(14) O22 0.147(3) 0.066(2) 0.0288(15) 0.0043(15) -0.0050(19) -0.031(2) C4 0.0248(16) 0.0300(15) 0.0196(15) -0.0051(13) 0.0033(12) -0.0001(13) C15 0.0259(16) 0.0276(15) 0.0210(15) 0.0024(13) 0.0045(13) -0.0013(13) C21 0.0283(17) 0.0320(16) 0.0246(16) 0.0023(14) -0.0053(14) -0.0053(14) C12 0.0177(16) 0.0311(16) 0.0317(17) -0.0024(14) -0.0012(13) -0.0011(13) C9 0.0305(17) 0.0204(14) 0.0325(17) 0.0050(14) -0.0005(14) 0.0022(13) C3 0.0277(16) 0.0268(15) 0.0213(15) -0.0074(13) 0.0014(13) -0.0001(13) C14 0.0268(16) 0.0302(15) 0.0203(15) 0.0001(13) 0.0057(13) -0.0002(13) C5 0.0285(17) 0.0346(16) 0.0227(16) -0.0076(14) -0.0044(14) -0.0004(14) C10 0.0229(16) 0.0241(15) 0.0312(16) 0.0013(13) 0.0012(13) -0.0010(13) C16 0.0299(17) 0.0371(17) 0.0208(16) 0.0055(14) -0.0011(14) 0.0043(14) C6 0.0286(17) 0.0381(17) 0.0250(16) -0.0102(15) -0.0021(14) -0.0082(15) O23 0.0499(18) 0.151(3) 0.0535(19) 0.046(2) 0.0077(15) -0.016(2) C18 0.0359(19) 0.0386(17) 0.0166(15) 0.0002(14) -0.0037(14) -0.0046(16) O11 0.066(2) 0.078(2) 0.103(3) 0.029(2) -0.002(2) 0.0103(19) C19 0.051(2) 0.0308(17) 0.0204(15) 0.0018(14) -0.0072(15) -0.0051(16) C17 0.0356(19) 0.0315(16) 0.0255(16) 0.0081(14) 0.0004(14) 0.0084(15) C7 0.0263(17) 0.0261(15) 0.0350(18) 0.0039(14) 0.0007(14) 0.0048(13) C24 0.038(2) 0.0379(19) 0.0325(18) 0.0040(16) -0.0118(16) 0.0064(16) C23 0.0311(18) 0.0343(17) 0.0285(17) 0.0009(15) -0.0004(14) 0.0026(15) C30 0.0332(19) 0.0420(19) 0.0312(18) 0.0054(16) 0.0028(15) 0.0176(16) C20 0.0368(19) 0.0380(18) 0.0241(16) 0.0028(15) -0.0007(15) -0.0075(16) C8 0.0280(17) 0.0245(15) 0.0333(17) -0.0030(14) 0.0034(14) -0.0029(13) C29 0.0317(18) 0.054(2) 0.0245(17) 0.0047(16) 0.0091(14) 0.0113(16) O10 0.087(3) 0.081(2) 0.083(2) -0.005(2) 0.032(2) -0.016(2) Na3 0.069(2) 0.082(2) 0.088(2) 0.0528(17) 0.0292(18) 0.0345(17) O13 0.106(3) 0.085(3) 0.088(3) -0.005(2) 0.026(2) 0.002(3) O19 0.170(5) 0.091(3) 0.037(2) 0.012(2) -0.030(3) -0.040(3) O15 0.1032(19) 0.0900(18) 0.0920(19) 0.0083(15) 0.0013(15) 0.0067(15) O17 0.099(3) 0.170(5) 0.058(3) 0.059(3) 0.007(3) -0.015(3) O14 0.085(5) 0.063(4) 0.071(4) 0.039(3) -0.019(3) -0.008(4) O12 0.114(6) 0.112(6) 0.041(3) 0.002(3) -0.019(3) 0.004(5) O3 0.085(4) 0.071(3) 0.097(4) 0.008(3) 0.009(3) 0.007(3) O20 0.056(4) 0.095(6) 0.050(5) 0.044(5) -0.016(4) 0.004(4) O16 0.077(5) 0.045(4) 0.045(5) 0.021(4) -0.006(5) -0.013(4) O18 0.101(7) 0.066(5) 0.037(5) 0.004(4) 0.001(5) 0.000(5) Na2 0.0426(18) 0.0474(17) 0.104(3) 0.0024(18) -0.0059(18) 0.0102(14) N0AA 0.083(4) 0.037(2) 0.069(3) 0.002(2) 0.026(3) -0.005(3) C0AA 0.091(4) 0.065(4) 0.092(4) 0.002(3) 0.007(3) -0.007(3) C1AA 0.125(8) 0.073(5) 0.131(9) 0.003(6) -0.031(7) -0.016(5) C2AA 0.174(10) 0.074(5) 0.134(8) 0.024(6) -0.021(7) -0.006(6) 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' Na Na 0.0362 0.0249 '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' 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 O21 S1 C28 107.41(18) . . ? O21 S1 O22 111.5(3) . . ? O22 S1 C28 105.43(17) . . ? O23 S1 C28 106.38(18) . . ? O23 S1 O21 113.5(3) . . ? O23 S1 O22 112.0(3) . . ? O19 S002 C19 104.7(3) . . ? O19 S002 O15 116.0(4) . . ? O19 S002 O17 112.4(4) . . ? O15 S002 C19 107.1(3) . . ? O15 S002 O17 109.0(4) . . ? O17 S002 C19 107.0(3) . . ? O20 S002 C19 103.3(5) . . ? O16 S002 C19 108.0(5) . . ? O16 S002 O20 99.4(8) . . ? O16 S002 O18 118.4(9) . . ? O18 S002 C19 108.6(5) . . ? O18 S002 O20 117.7(9) . . ? O5 Na1 O1 99.20(12) . . ? O5 Na1 O10 166.90(15) . 3_665 ? O5 Na1 O3 90.15(14) . . ? O5 Na1 Na2 132.71(11) . 3_665 ? O4 Na1 O5 91.56(11) . . ? O4 Na1 O1 100.73(13) . . ? O4 Na1 O10 90.47(14) . 3_665 ? O4 Na1 O3 76.75(16) . . ? O4 Na1 Na2 90.68(10) . 3_665 ? O2 Na1 O5 88.21(12) . . ? O2 Na1 O4 152.68(14) . . ? O2 Na1 O1 106.27(14) . . ? O2 Na1 O10 84.08(14) . 3_665 ? O2 Na1 O3 75.93(17) . . ? O2 Na1 Na2 69.96(12) . 3_665 ? O1 Na1 O3 170.41(16) . . ? O1 Na1 Na2 126.64(12) . 3_665 ? O10 Na1 O1 93.13(15) 3_665 . ? O10 Na1 O3 77.72(17) 3_665 . ? O10 Na1 Na2 34.30(13) 3_665 3_665 ? O3 Na1 Na2 44.81(14) . 3_665 ? C2 O5 Na1 144.2(2) . . ? C9 O4 Na1 148.2(2) . . ? C5 O9 Na3 154.6(3) . . ? C5 O9 Na2 147.0(3) . . ? C16 O6 Na3 139.8(3) . 3_665 ? C16 O6 Na2 138.3(3) . 3_665 ? C2 N4 C1 123.6(3) . . ? C2 N4 C4 112.7(3) . . ? C4 N4 C1 123.8(3) . . ? C5 N2 C3 112.2(3) . . ? C5 N2 C6 121.6(3) . . ? C6 N2 C3 124.0(3) . . ? C13 N12 C1 120.4(3) . 3_665 ? C13 N12 C14 111.3(3) . . ? C1 N12 C14 122.0(3) 3_665 . ? C13 N9 C15 112.6(3) . . ? C13 N9 C12 122.4(3) . . ? C15 N9 C12 124.3(3) . . ? C9 N5 C7 122.5(3) . . ? C9 N5 C8 112.7(3) . . ? C8 N5 C7 124.1(3) . . ? C15 N10 C17 123.5(3) . . ? C16 N10 C15 112.7(3) . . ? C16 N10 C17 122.9(3) . . ? C11 N8 C12 122.7(3) . . ? C11 N8 C10 113.4(3) . . ? C12 N8 C10 123.8(3) . . ? C4 N1 C18 123.2(3) . 3_665 ? C5 N1 C4 111.4(3) . . ? C5 N1 C18 122.1(3) . 3_665 ? C2 N3 C3 112.4(3) . . ? C2 N3 C7 123.6(3) . . ? C3 N3 C7 123.9(3) . . ? C11 N6 C6 122.6(3) . . ? C11 N6 C8 113.1(3) . . ? C8 N6 C6 123.5(3) . . ? C9 N7 C10 112.2(3) . . ? C9 N7 C17 121.8(3) . . ? C17 N7 C10 123.9(3) . . ? C16 N11 C14 112.9(3) . . ? C16 N11 C18 123.8(3) . . ? C18 N11 C14 123.2(3) . . ? O5 C2 N4 125.8(3) . . ? O5 C2 N3 125.7(3) . . ? N4 C2 N3 108.4(3) . . ? C27 C28 S1 120.9(3) . . ? C29 C28 S1 119.2(3) . . ? C29 C28 C27 119.9(3) . . ? C21 C22 C25 120.6(3) . . ? C23 C22 C25 121.4(3) . . ? C23 C22 C21 117.9(3) . . ? C26 C25 C22 122.2(3) . . ? C26 C25 C30 117.8(3) . . ? C30 C25 C22 120.0(3) . . ? O7 C13 N12 126.5(3) . . ? O7 C13 N9 124.9(3) . . ? N12 C13 N9 108.6(3) . . ? C28 C27 C26 119.9(3) . . ? O8 C11 N8 126.5(3) . . ? O8 C11 N6 126.0(3) . . ? N8 C11 N6 107.5(3) . . ? N12 C1 N4 114.0(3) 3_665 . ? C27 C26 C25 121.3(3) . . ? N4 C4 N1 115.1(3) . . ? N4 C4 C3 103.1(3) . . ? N1 C4 C3 103.9(3) . . ? N9 C15 N10 114.6(3) . . ? N9 C15 C14 102.9(3) . . ? N10 C15 C14 103.3(3) . . ? C20 C21 C22 121.1(3) . . ? N8 C12 N9 113.6(3) . . ? O4 C9 N5 125.7(3) . . ? O4 C9 N7 125.9(3) . . ? N7 C9 N5 108.5(3) . . ? N2 C3 N3 114.8(3) . . ? N2 C3 C4 103.3(3) . . ? N3 C3 C4 103.4(3) . . ? N12 C14 C15 104.0(3) . . ? N11 C14 N12 114.4(3) . . ? N11 C14 C15 103.0(3) . . ? O9 C5 N2 125.7(3) . . ? O9 C5 N1 125.6(3) . . ? N2 C5 N1 108.7(3) . . ? N8 C10 N7 115.5(3) . . ? N8 C10 C8 102.9(3) . . ? N7 C10 C8 103.2(3) . . ? O6 C16 N10 126.3(3) . . ? O6 C16 N11 126.0(3) . . ? N11 C16 N10 107.6(3) . . ? N2 C6 N6 113.6(3) . . ? N11 C18 N1 114.2(3) . 3_665 ? C24 C19 S002 119.4(3) . . ? C24 C19 C20 120.2(3) . . ? C20 C19 S002 120.3(3) . . ? N10 C17 N7 114.1(3) . . ? N5 C7 N3 114.5(3) . . ? C23 C24 C19 120.0(3) . . ? C24 C23 C22 121.3(3) . . ? C29 C30 C25 121.3(3) . . ? C19 C20 C21 119.4(3) . . ? N5 C8 N6 115.2(3) . . ? N5 C8 C10 103.1(3) . . ? N6 C8 C10 102.9(3) . . ? C28 C29 C30 119.8(3) . . ? Na1 O10 Na3 129.2(2) 3_665 . ? Na2 O10 Na1 108.6(2) . 3_665 ? O9 Na3 O6 81.79(17) . 3_665 ? O9 Na3 O11 83.01(17) . . ? O9 Na3 O10 124.1(2) . . ? O9 Na3 O14 80.5(2) . . ? O11 Na3 O6 130.4(2) . 3_665 ? O11 Na3 O10 85.73(19) . . ? O11 Na3 O14 100.2(3) . . ? O10 Na3 O6 65.34(15) . 3_665 ? O10 Na3 O14 155.3(2) . . ? O14 Na3 O6 123.1(2) . 3_665 ? Na2 O3 Na1 88.54(18) 3_665 . ? C0AA O3 Na1 149.8(4) . . ? C0AA O3 Na2 111.7(4) . 3_665 ? O9 Na2 Na1 136.8(2) . 3_665 ? O9 Na2 O6 95.89(17) . 3_665 ? O9 Na2 O11 84.15(17) . . ? O9 Na2 O12 108.5(3) . . ? O9 Na2 O3 91.3(2) . 3_665 ? O6 Na2 Na1 86.26(13) 3_665 3_665 ? O6 Na2 O11 175.3(3) 3_665 . ? O6 Na2 O12 68.1(2) 3_665 . ? O6 Na2 O3 78.9(2) 3_665 3_665 ? O11 Na2 Na1 90.51(16) . 3_665 ? O11 Na2 O12 116.4(3) . . ? O11 Na2 O3 96.5(2) . 3_665 ? O10 Na2 Na1 37.10(14) . 3_665 ? O10 Na2 O9 173.5(3) . . ? O10 Na2 O6 82.15(18) . 3_665 ? O10 Na2 O11 97.3(2) . . ? O10 Na2 O12 76.6(3) . . ? O10 Na2 O3 82.2(2) . 3_665 ? O12 Na2 Na1 112.2(2) . 3_665 ? O3 Na2 Na1 46.65(14) 3_665 3_665 ? O3 Na2 O12 142.6(3) 3_665 . ? C0AA N0AA C1AA 119.5(4) . . ? C2AA N0AA C0AA 121.6(4) . . ? C2AA N0AA C1AA 118.9(3) . . ? O3 C0AA N0AA 121.6(6) . . ? 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 C28 1.775(3) . ? S1 O21 1.427(4) . ? S1 O22 1.444(4) . ? S1 O23 1.407(4) . ? S002 C19 1.773(4) . ? S002 O19 1.408(5) . ? S002 O15 1.415(6) . ? S002 O17 1.425(6) . ? S002 O20 1.487(10) . ? S002 O16 1.394(9) . ? S002 O18 1.399(10) . ? Na1 O5 2.326(3) . ? Na1 O4 2.312(3) . ? Na1 O2 2.290(4) . ? Na1 O1 2.352(4) . ? Na1 O10 2.334(4) 3_665 ? Na1 O3 2.668(6) . ? Na1 Na2 3.667(5) 3_665 ? O5 C2 1.223(4) . ? O7 C13 1.211(4) . ? O8 C11 1.209(4) . ? O4 C9 1.213(4) . ? O9 C5 1.213(4) . ? O9 Na3 2.284(5) . ? O9 Na2 2.212(5) . ? O6 C16 1.211(4) . ? O6 Na3 2.930(6) 3_665 ? O6 Na2 2.428(5) 3_665 ? N4 C2 1.356(4) . ? N4 C1 1.444(4) . ? N4 C4 1.444(4) . ? N2 C3 1.440(4) . ? N2 C5 1.364(5) . ? N2 C6 1.440(4) . ? N12 C13 1.366(4) . ? N12 C1 1.444(4) 3_665 ? N12 C14 1.444(4) . ? N9 C13 1.368(4) . ? N9 C15 1.436(4) . ? N9 C12 1.448(4) . ? N5 C9 1.365(5) . ? N5 C7 1.445(4) . ? N5 C8 1.441(5) . ? N10 C15 1.440(4) . ? N10 C16 1.371(5) . ? N10 C17 1.444(4) . ? N8 C11 1.360(5) . ? N8 C12 1.444(4) . ? N8 C10 1.447(4) . ? N1 C4 1.445(4) . ? N1 C5 1.370(5) . ? N1 C18 1.449(4) 3_665 ? N3 C2 1.361(4) . ? N3 C3 1.441(4) . ? N3 C7 1.449(4) . ? N6 C11 1.368(4) . ? N6 C6 1.449(4) . ? N6 C8 1.446(5) . ? N7 C9 1.362(5) . ? N7 C10 1.450(4) . ? N7 C17 1.447(4) . ? N11 C14 1.443(4) . ? N11 C16 1.364(5) . ? N11 C18 1.438(4) . ? C28 C27 1.383(5) . ? C28 C29 1.377(5) . ? C22 C25 1.485(4) . ? C22 C21 1.398(5) . ? C22 C23 1.385(5) . ? C25 C26 1.386(5) . ? C25 C30 1.395(5) . ? C27 C26 1.385(5) . ? C1 N12 1.444(4) 3_665 ? C4 C3 1.543(5) . ? C15 C14 1.545(5) . ? C21 C20 1.384(5) . ? C10 C8 1.554(5) . ? C18 N1 1.449(4) 3_665 ? O11 Na3 2.443(6) . ? O11 Na2 2.458(6) . ? C19 C24 1.379(6) . ? C19 C20 1.383(5) . ? C24 C23 1.376(5) . ? C30 C29 1.382(5) . ? O10 Na1 2.334(4) 3_665 ? O10 Na3 2.676(6) . ? O10 Na2 2.181(5) . ? Na3 O6 2.930(6) 3_665 ? Na3 O14 2.732(9) . ? O12 Na2 2.775(9) . ? O3 Na2 2.585(7) 3_665 ? O3 C0AA 1.190(7) . ? Na2 Na1 3.667(5) 3_665 ? Na2 O6 2.427(5) 3_665 ? Na2 O3 2.585(7) 3_665 ? N0AA C0AA 1.456(4) . ? N0AA C1AA 1.466(5) . ? N0AA C2AA 1.439(6) . ?