#------------------------------------------------------------------------------ #$Date: 2024-02-04 13:41:47 +0200 (Sun, 04 Feb 2024) $ #$Revision: 289457 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247826.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_7247826 loop_ _publ_author_name 'Zhang, Menglei' 'Li, Zhongkui' 'Zhu, Yanhong' 'Yan, Li' 'Zhong, Xue' 'Zhang, Yijie' 'Li, Ziyao' 'Bai, Yixiang' 'Li, Hui' _publ_section_title ; Mimic uracil--uracil base pairing: self-assembly and single crystal structure ; _journal_issue 3 _journal_name_full CrystEngComm _journal_page_first 261 _journal_page_last 267 _journal_paper_doi 10.1039/D3CE01056B _journal_volume 26 _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety 'C27 H29 Cd N8 O11 P, 3(H2 O)' _chemical_formula_sum 'C27 H35 Cd N8 O14 P' _chemical_formula_weight 839.00 _space_group_crystal_system orthorhombic _space_group_IT_number 20 _space_group_name_Hall 'C 2c 2' _space_group_name_H-M_alt 'C 2 2 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2023-06-26 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-08-16 deposited with the CCDC. 2023-12-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.7744(4) _cell_length_b 25.5061(11) _cell_length_c 31.6431(12) _cell_measurement_reflns_used 9861 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 27.03 _cell_measurement_theta_min 2.42 _cell_volume 8695.9(6) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_unetI/netI 0.0454 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 49298 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.134 _diffrn_reflns_theta_min 1.287 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.5337 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0757 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.7159. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.282 _exptl_crystal_description plate _exptl_crystal_F_000 3424 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.990 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.073 _refine_ls_abs_structure_details ; Flack x determined using 2894 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.000(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 486 _refine_ls_number_reflns 9610 _refine_ls_number_restraints 118 _refine_ls_restrained_S_all 1.032 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0407 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+5.6080P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.0994 _reflns_Friedel_coverage 0.829 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 7596 _reflns_number_total 9610 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01056b2.cif _cod_data_source_block 00 _cod_depositor_comments 'Adding full bibliography for 7247822--7247826.cif.' _cod_database_code 7247826 _shelx_shelxl_version_number 2018/3 _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_max 0.976 _shelx_estimated_absorpt_t_min 0.859 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 2. Restrained distances H13b-O5 1.95 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains N2, N6, N9, N10, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: N6(0.5) N9(0.5) C14(0.5) H14(0.5) C13(0.5) H13(0.5) N2(0.5) C17(0.5) H17(0.5) C16(0.5) H16(0.5) C15(0.5) C18(0.5) H18(0.5) C21(0.5) C20(0.5) H20(0.5) C19(0.5) H19(0.5) N10(0.5) C23(0.5) H23(0.5) C22(0.5) H22(0.5) C24(0.5) H24(0.5) 6.a Free rotating group: O13(H13a,H13b), O14(H14a,H14b), O12(H12a,H12b) 6.b Rotating group: O1(H1a,H1b), O3(H3a,H3b) 6.c Ternary CH refined with riding coordinates: C26(H26), C27(H27), C28(H28), C29(H29) 6.d Aromatic/amide H refined with riding coordinates: C2(H2), C1(H1), C5(H5), C4(H4), C6(H6), C7(H7), C8(H8a), C10(H10), C11(H11), C12(H12), C25(H25), N8(H8b), C32(H32), C33(H33), C14(H14), C13(H13), C17(H17), C16(H16), C18(H18), C20(H20), C19(H19), C23(H23), C22(H22), C24(H24) 6.e Fitted hexagon refined as free rotating group: C2(C1,N1,C5,C4,C3), C7(C8,C9,C10,C11,N5), C30(N8,C31,C32,C33,N7), C14(C13,N2, C17,C16,C15), C21(C20,C19,N10,C23,C22) 6.f Idealised tetrahedral OH refined as rotating group: O8(H8), O9(H9) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 00_c.res in C222(1) 00.res created by SHELXL-2018/3 at 17:02:47 on 04-May-2022 REM Old TITL 00_c.res in C222(1) REM SHELXT solution in C222(1) REM R1 0.143, Rweak 0.018, Alpha 0.141, Orientation as input REM Flack x = 0.083 ( 0.010 ) from Parsons' quotients REM Formula found by SHELXT: C31 Cd N9 O16 P CELL 0.71073 10.7744 25.5061 31.6431 90 90 90 ZERR 8 0.0004 0.0011 0.0012 0 0 0 LATT -7 SYMM -X,-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM +X,-Y,-Z SFAC C H Cd N O P UNIT 216 280 8 64 112 8 EQIV $1 -0.5+X,1.5-Y,1-Z EQIV $2 -X,+Y,1.5-Z RIGU N2 N6 N9 N10 C13 C14 C15 C16 C17 C18 C19 C20 C21 C22 C23 C24 DFIX 1.95 H13b O5 ISOR 0.01 0.02 O14 L.S. 5 PLAN 20 SIZE 0.24 0.26 0.04 TEMP 23 CONF HTAB O3 O5 HTAB O8 O5_$1 HTAB O9 O14_$1 HTAB N8 O10_$2 LIST 4 MORE -1 BOND $H HTAB ABIN fmap 2 acta OMIT 0 2 1 REM REM REM WGHT 0.049600 5.608000 FVAR 0.11089 CD1 3 0.265554 0.500000 0.500000 10.50000 0.02839 0.03411 = 0.01985 0.00092 0.00000 0.00000 CD2 3 0.592575 0.500000 0.500000 10.50000 0.02881 0.03864 = 0.01590 -0.00066 0.00000 0.00000 P1 6 0.434469 0.617913 0.495185 11.00000 0.03546 0.02325 = 0.02448 0.00009 0.00214 -0.00165 O1 5 0.104177 0.439129 0.498191 11.00000 0.07271 0.09591 = 0.04645 0.01744 -0.02529 -0.04661 AFIX 7 H1A 2 0.048532 0.443986 0.475600 11.00000 -1.50000 H1B 2 0.050571 0.442651 0.521130 11.00000 -1.50000 AFIX 0 O2 5 0.429137 0.558221 0.499074 11.00000 0.03202 0.02215 = 0.04020 0.00199 -0.00167 -0.00121 O3 5 0.747107 0.563336 0.494649 11.00000 0.04259 0.05512 = 0.03819 0.00257 0.00249 -0.00793 AFIX 7 H3A 2 0.717046 0.594667 0.499727 11.00000 -1.50000 H3B 2 0.803273 0.559338 0.514591 11.00000 -1.50000 AFIX 0 O4 5 0.348704 0.641046 0.463194 11.00000 0.06495 0.04241 = 0.05540 0.01049 -0.02064 0.00223 O5 5 0.567011 0.636404 0.490353 11.00000 0.04363 0.03762 = 0.04681 -0.00082 0.01256 -0.00586 O6 5 0.390423 0.636575 0.541567 11.00000 0.05129 0.02171 = 0.04472 0.00360 0.01935 0.00954 O7 5 0.200011 0.677812 0.595594 11.00000 0.04999 0.03023 = 0.03845 -0.00030 0.00319 0.00551 O8 5 0.083213 0.770492 0.548711 11.00000 0.05944 0.03807 = 0.06165 0.01425 -0.00445 0.01432 AFIX 147 H8 2 0.080998 0.797080 0.534162 11.00000 -1.50000 AFIX 0 O9 5 0.160184 0.812548 0.625749 11.00000 0.10686 0.04705 = 0.06120 -0.01390 0.01045 0.02530 AFIX 147 H9 2 0.091393 0.815825 0.614982 11.00000 -1.50000 AFIX 0 O10 5 0.008199 0.711618 0.695070 11.00000 0.03774 0.07314 = 0.03297 0.00160 0.00832 0.00497 O11 5 0.316419 0.667443 0.784261 11.00000 0.05239 0.20751 = 0.03652 -0.00177 -0.01793 0.00420 N3 4 0.170410 0.466239 0.270809 11.00000 0.05952 0.07678 = 0.01639 0.00315 -0.00441 -0.00366 N4 4 0.156237 0.478287 0.227518 11.00000 0.05749 0.07891 = 0.02067 -0.00239 -0.00583 -0.00730 AFIX 66 C2 1 0.229579 0.549455 0.361511 11.00000 0.10215 0.03972 = 0.02474 0.00186 -0.01719 -0.01000 AFIX 43 H2 2 0.226895 0.581393 0.347361 11.00000 -1.20000 AFIX 65 C1 1 0.246836 0.548285 0.405034 11.00000 0.08872 0.04374 = 0.04295 -0.00285 -0.00400 0.01010 AFIX 43 H1 2 0.255696 0.579440 0.420002 11.00000 -1.20000 AFIX 65 N1 4 0.250848 0.500552 0.426184 11.00000 0.03445 0.04246 = 0.02761 0.01042 -0.00142 0.00394 C5 1 0.237604 0.453987 0.403812 11.00000 0.04656 0.04476 = 0.02579 -0.00931 -0.00934 0.01609 AFIX 43 H5 2 0.240289 0.422050 0.417963 11.00000 -1.20000 AFIX 65 C4 1 0.220348 0.455156 0.360289 11.00000 0.04772 0.04554 = 0.04091 -0.01196 0.00003 0.00779 AFIX 43 H4 2 0.211487 0.424002 0.345321 11.00000 -1.20000 AFIX 65 C3 1 0.216335 0.502890 0.339139 11.00000 0.03737 0.04869 = 0.02663 0.00727 -0.00311 -0.00413 AFIX 0 C6 1 0.195270 0.506264 0.292864 11.00000 0.06117 0.05991 = 0.02430 -0.00445 -0.00149 -0.01862 AFIX 43 H6 2 0.200502 0.538777 0.279682 11.00000 -1.20000 AFIX 66 C7 1 0.091656 0.490602 0.094401 11.00000 0.06740 0.07233 = 0.03535 0.00666 -0.00059 0.00946 AFIX 43 H7 2 0.092064 0.522336 0.079928 11.00000 -1.20000 AFIX 65 C8 1 0.109719 0.489780 0.137890 11.00000 0.05040 0.05258 = 0.03836 -0.00882 -0.00286 -0.00181 AFIX 43 H8A 2 0.122212 0.520964 0.152514 11.00000 -1.20000 AFIX 65 C9 1 0.109110 0.442350 0.159522 11.00000 0.03903 0.05904 = 0.02297 -0.00295 -0.00164 -0.00127 C10 1 0.090437 0.395742 0.137664 11.00000 0.04801 0.03944 = 0.04073 -0.00440 0.00432 -0.00924 AFIX 43 H10 2 0.090030 0.364008 0.152137 11.00000 -1.20000 AFIX 65 C11 1 0.072374 0.396563 0.094175 11.00000 0.05869 0.06850 = 0.03209 -0.00158 0.01306 -0.00264 AFIX 43 H11 2 0.059881 0.365379 0.079550 11.00000 -1.20000 AFIX 65 N5 4 0.072983 0.443993 0.072542 11.00000 0.06354 0.05963 = 0.02889 -0.01014 0.00102 -0.00387 AFIX 0 C12 1 0.126501 0.439276 0.205953 11.00000 0.05248 0.05064 = 0.02918 0.00379 0.00191 -0.00620 AFIX 43 H12 2 0.114877 0.407251 0.219436 11.00000 -1.20000 AFIX 0 C25 1 0.370684 0.691483 0.548763 11.00000 0.04369 0.02710 = 0.05922 -0.00259 0.02357 -0.00007 AFIX 43 H25 2 0.432689 0.716836 0.548094 11.00000 -1.20000 AFIX 0 C26 1 0.236280 0.702388 0.557513 11.00000 0.04013 0.03276 = 0.02193 0.00294 -0.00384 -0.00021 AFIX 13 H26 2 0.186613 0.687875 0.534355 11.00000 -1.20000 AFIX 0 C27 1 0.206873 0.760861 0.561649 11.00000 0.04041 0.02831 = 0.04810 0.00465 0.00901 0.00393 AFIX 13 H27 2 0.266600 0.782722 0.546316 11.00000 -1.20000 AFIX 0 C28 1 0.216993 0.768056 0.609933 11.00000 0.07140 0.02115 = 0.04502 -0.01223 0.00863 0.00211 AFIX 13 H28 2 0.304998 0.768847 0.617732 11.00000 -1.20000 AFIX 0 C29 1 0.161136 0.717245 0.625584 11.00000 0.04150 0.03523 = 0.03425 0.00638 0.01178 0.01547 AFIX 13 H29 2 0.070413 0.719978 0.625328 11.00000 -1.20000 AFIX 66 C30 1 0.121984 0.704346 0.701154 11.00000 0.03738 0.04778 = 0.03815 0.00031 0.00758 -0.00115 N8 4 0.165214 0.692720 0.741467 11.00000 0.03786 0.09833 = 0.02386 0.00456 0.00912 -0.00647 AFIX 43 H8B 2 0.115786 0.694523 0.762757 11.00000 -1.20000 AFIX 65 C31 1 0.288334 0.678182 0.747369 11.00000 0.03962 0.13246 = 0.05517 0.03210 0.00508 0.00986 C32 1 0.368224 0.675268 0.712958 11.00000 0.04602 0.19797 = 0.02595 0.00615 0.01104 0.02258 AFIX 43 H32 2 0.450599 0.665541 0.716907 11.00000 -1.20000 AFIX 65 C33 1 0.324996 0.686894 0.672645 11.00000 0.04623 0.09103 = 0.05575 0.01178 0.00858 0.02618 AFIX 43 H33 2 0.378448 0.684944 0.649622 11.00000 -1.20000 AFIX 65 N7 4 0.201877 0.701432 0.666742 11.00000 0.04101 0.06983 = 0.02574 -0.00848 0.00296 0.00081 AFIX 0 PART -1 N6 4 0.517498 0.515033 0.730237 10.50000 0.03494 0.08281 = 0.01850 -0.00660 -0.00003 -0.00726 N9 4 0.509178 0.501085 0.772449 10.50000 0.04841 0.08544 = 0.01952 -0.00042 -0.00260 0.02983 AFIX 66 C14 1 0.592191 0.443824 0.636203 10.50000 0.07026 0.03873 = 0.03698 -0.00668 0.00074 -0.00445 AFIX 43 H14 2 0.600561 0.411353 0.649266 10.50000 -1.20000 AFIX 65 C13 1 0.603795 0.447946 0.592580 10.50000 0.04134 0.04259 = 0.03321 -0.01013 0.01308 0.00467 AFIX 43 H13 2 0.619929 0.418232 0.576456 10.50000 -1.20000 AFIX 65 N2 4 0.591285 0.496477 0.573057 10.50000 0.01893 0.05596 = 0.01554 -0.00160 -0.00530 -0.00401 C17 1 0.567171 0.540887 0.597156 10.50000 0.05463 0.04772 = 0.01835 0.00765 0.00207 -0.00038 AFIX 43 H17 2 0.558800 0.573357 0.584094 10.50000 -1.20000 AFIX 65 C16 1 0.555566 0.536766 0.640779 10.50000 0.07323 0.04606 = 0.01938 0.00036 0.00060 0.00972 AFIX 43 H16 2 0.539432 0.566479 0.656903 10.50000 -1.20000 AFIX 65 C15 1 0.568076 0.488235 0.660303 10.50000 0.03665 0.03860 = 0.02500 -0.00763 -0.00053 -0.00773 AFIX 0 C18 1 0.547375 0.480060 0.706425 10.50000 0.06860 0.07192 = 0.03325 0.00291 0.01314 0.00147 AFIX 43 H18 2 0.557896 0.446541 0.717423 10.50000 -1.20000 AFIX 66 C21 1 0.442851 0.526972 0.841502 10.50000 0.04244 0.04958 = 0.02145 -0.00561 -0.00966 0.00512 C20 1 0.417566 0.569391 0.867701 10.50000 0.04134 0.04775 = 0.02468 -0.00059 -0.00406 0.00795 AFIX 43 H20 2 0.412276 0.602982 0.856411 10.50000 -1.20000 AFIX 65 C19 1 0.400189 0.561606 0.910773 10.50000 0.06604 0.04204 = 0.02304 -0.00638 0.00303 0.01268 AFIX 43 H19 2 0.383272 0.589987 0.928301 10.50000 -1.20000 AFIX 65 N10 4 0.408096 0.511401 0.927646 10.50000 0.06850 0.03782 = 0.03549 -0.00188 0.00436 0.01403 C23 1 0.433381 0.468982 0.901448 10.50000 0.04754 0.03374 = 0.02229 -0.00290 -0.00577 0.02578 AFIX 43 H23 2 0.438671 0.435392 0.912737 10.50000 -1.20000 AFIX 65 C22 1 0.450758 0.476767 0.858376 10.50000 0.02905 0.05519 = 0.02848 0.00490 0.00146 0.01524 AFIX 43 H22 2 0.467675 0.448385 0.840847 10.50000 -1.20000 AFIX 0 C24 1 0.458800 0.534987 0.795738 10.50000 0.03445 0.07035 = 0.01551 0.00349 -0.00208 0.01386 AFIX 43 H24 2 0.430794 0.566052 0.783661 10.50000 -1.20000 AFIX 6 PART 0 O13 5 0.693896 0.690137 0.555194 11.00000 0.07719 0.12382 = 0.08211 -0.01448 -0.01201 -0.02238 H13A 2 0.769877 0.697089 0.550669 11.00000 -1.50000 H13B 2 0.672193 0.671403 0.534261 11.00000 -1.50000 AFIX 6 O14 5 0.414557 0.668750 0.383001 11.00000 0.17277 0.23665 = 0.08941 0.03990 -0.04145 -0.12973 H14A 2 0.386251 0.699830 0.381785 11.00000 -1.50000 H14B 2 0.395234 0.658187 0.407613 11.00000 -1.50000 AFIX 6 O12 5 -0.079027 0.695102 0.518729 11.00000 0.09035 0.07559 = 0.11742 0.02782 -0.01210 -0.00634 H12A 2 -0.051084 0.675578 0.499084 11.00000 -1.50000 H12B 2 -0.033760 0.722348 0.517734 11.00000 -1.50000 AFIX 0 HKLF 4 REM 00_c.res in C222(1) REM wR2 = 0.0994, GooF = S = 1.032, Restrained GooF = 1.032 for all data REM R1 = 0.0407 for 7596 Fo > 4sig(Fo) and 0.0601 for all 9610 data REM 486 parameters refined using 118 restraints END WGHT 0.0496 5.6078 REM Instructions for potential hydrogen bonds EQIV $5 -x, y, -z+1/2 HTAB O1 N5_$5 HTAB O3 O5 EQIV $3 -x+1, -y+1, z+1/2 HTAB O3 N5_$3 HTAB O8 O5_$1 HTAB O9 O8 HTAB O9 O14_$1 HTAB C1 O4 EQIV $4 x, -y+1, -z+1 HTAB C5 O6_$4 HTAB C5 O7_$4 EQIV $6 -x, -y+1, z-1/2 HTAB C10 O10_$6 HTAB C11 O12_$6 HTAB N8 O10_$2 EQIV $7 -x+1, y, -z+3/2 HTAB C32 O11_$7 HTAB C13 O5_$4 REM Highest difference peak 0.990, deepest hole -0.954, 1-sigma level 0.073 Q1 1 0.2620 0.4989 0.5297 11.00000 0.05 0.99 Q2 1 0.6085 0.4990 0.5300 11.00000 0.05 0.73 Q3 1 0.2490 0.5324 0.4093 11.00000 0.05 0.65 Q4 1 -0.0652 0.4995 0.5096 11.00000 0.05 0.61 Q5 1 0.2471 0.4701 0.4077 11.00000 0.05 0.58 Q6 1 0.4241 0.6194 0.5210 11.00000 0.05 0.54 Q7 1 0.0982 0.4738 0.0915 11.00000 0.05 0.48 Q8 1 0.4767 0.5000 0.5000 10.50000 0.05 0.44 Q9 1 0.4207 0.6481 0.8691 11.00000 0.05 0.42 Q10 1 0.3810 0.5000 0.5000 10.50000 0.05 0.40 Q11 1 0.2491 0.4803 0.4993 11.00000 0.05 0.37 Q12 1 0.1023 0.5306 0.0907 11.00000 0.05 0.36 Q13 1 0.4225 0.5244 0.9161 11.00000 0.05 0.35 Q14 1 0.3651 0.5815 0.4999 11.00000 0.05 0.34 Q15 1 0.1784 0.4579 0.5021 11.00000 0.05 0.34 Q16 1 0.7030 0.5000 0.5000 10.50000 0.05 0.33 Q17 1 0.0588 0.4093 0.5029 11.00000 0.05 0.32 Q18 1 0.5041 0.5420 0.4987 11.00000 0.05 0.31 Q19 1 0.4276 0.4776 0.9178 11.00000 0.05 0.31 Q20 1 0.6307 0.5000 0.5000 10.50000 0.05 0.29 ; _shelx_res_checksum 61238 _shelx_fab_file ; -13 -9 -7 2.5344 -0.7140 -13 -9 -6 -1.7286 0.0610 -13 -9 -5 -1.7560 1.2107 -13 -9 -4 2.3236 1.9683 -13 -9 -3 0.6727 4.5992 -13 -9 -2 -2.4366 -3.4817 -13 -9 -1 0.1986 -6.1164 -13 -7 -10 0.0308 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12 2 6 -0.7887 2.3112 12 2 7 -2.2200 -2.2941 12 2 8 -0.8013 -0.0205 12 2 9 1.1683 -2.5829 12 2 10 1.9349 0.7589 12 2 11 -0.9866 -0.3625 12 2 12 2.4305 2.6428 12 2 13 2.5170 -0.6926 12 2 14 -2.5195 0.9925 12 2 15 0.2985 1.0264 12 2 16 -1.1142 1.3219 12 2 17 -0.4581 0.2256 12 2 18 -1.0880 -2.8939 12 2 19 1.0087 -1.3149 12 4 0 -0.2752 -0.0692 12 4 1 -0.6476 1.5115 12 4 2 -0.6381 -2.6967 12 4 3 -1.3993 -0.2658 12 4 4 -0.3003 -1.2874 12 4 5 0.1251 -1.9094 12 4 6 -2.1320 -3.5779 12 4 7 0.8938 2.3936 12 4 8 2.4133 -0.0221 12 4 9 1.0815 2.6603 12 4 10 -0.6007 0.1288 12 4 11 -1.4129 -0.2479 12 4 12 -0.4782 -0.9373 12 4 13 -1.4458 -2.4102 12 4 14 0.5842 0.8121 12 4 15 -0.9038 -1.3720 12 4 16 0.3796 -0.6692 12 4 17 1.0063 -2.4669 12 4 18 2.4900 2.5752 12 4 19 1.6432 1.1867 12 6 0 -0.3919 -0.0780 12 6 1 -0.1289 -1.6775 12 6 2 -0.8698 0.6664 12 6 3 -0.0185 -0.4278 12 6 4 -1.1566 2.2784 12 6 5 -1.8282 0.3497 12 6 6 1.8433 2.3425 12 6 7 4.3539 -0.4440 12 6 8 2.3048 -3.2856 12 6 9 -1.4239 -0.7705 12 6 10 -3.2235 -2.5323 12 6 11 0.0838 1.0917 12 6 12 1.0360 -0.7846 12 6 13 2.5108 3.0555 12 6 14 1.0491 0.9137 12 6 15 0.6744 -1.2000 12 6 16 1.8951 0.2893 12 6 17 0.2127 1.3308 12 6 18 -2.2183 -1.0940 12 8 0 -0.2551 0.0819 12 8 1 2.2826 0.3418 12 8 2 0.2551 -2.6406 12 8 3 1.0994 1.5263 12 8 4 1.2713 -0.5075 12 8 5 1.7335 -1.7370 12 8 6 4.2275 0.6534 12 8 7 -1.3012 -2.9874 12 8 8 -4.8468 3.2099 12 8 9 -1.8074 1.4167 12 8 10 0.8672 1.0701 12 8 11 1.6911 1.3478 12 8 12 3.1388 0.1869 12 8 13 -1.3254 0.9987 12 8 14 -3.6807 -4.0497 12 8 15 -0.0418 1.3472 12 8 16 -1.4876 0.8094 12 8 17 -2.4626 -0.6702 12 10 0 2.0913 0.1277 12 10 1 -1.9833 -1.3029 12 10 2 -0.8653 3.3834 12 10 3 -0.0475 1.9537 12 10 4 -0.0000 -1.2609 12 10 5 0.7911 0.8368 12 10 6 -4.8487 -0.5718 12 10 7 -2.9815 0.8237 12 10 8 2.2284 1.8631 12 10 9 0.2022 -2.2742 12 10 10 0.8524 0.2708 12 10 11 2.7135 -1.6700 12 10 12 -2.3477 0.1998 12 10 13 -3.1358 -4.0044 12 10 14 1.4966 1.5096 12 10 15 0.9004 2.2973 12 12 0 -0.8621 -0.0009 12 12 1 0.0417 1.3489 12 12 2 1.0966 -0.3237 12 12 3 0.8612 -2.0455 12 12 4 -1.6569 -1.1621 12 12 5 -1.8184 1.7899 12 12 6 3.3449 -1.8518 12 12 7 4.7664 0.5593 12 12 8 -0.6004 -2.3104 12 12 9 -0.8795 -1.7755 12 12 10 1.4207 1.6038 12 12 11 -2.0311 1.0565 12 12 12 -1.9773 0.0048 12 12 13 0.6932 2.7876 12 14 0 0.5443 -0.1709 12 14 1 0.7012 -0.4155 12 14 2 0.4393 -0.8265 12 14 3 -1.3076 -0.7421 12 14 4 0.9350 1.3558 12 14 5 2.0513 -1.9339 12 14 6 -0.8485 0.3595 12 14 7 -4.4358 2.2070 12 14 8 -3.4055 0.7082 12 14 9 0.9324 4.4251 12 14 10 0.0035 -0.0801 12 16 0 -1.2583 -0.2636 12 16 1 -1.1453 -0.7135 12 16 2 -1.0069 0.7580 12 16 3 -0.2530 1.6687 13 1 0 1.1456 -0.1431 13 1 1 -1.3942 1.6516 13 1 2 -2.7088 -1.3045 13 1 3 1.8401 1.9133 13 1 4 0.1109 -3.0510 13 1 5 0.5788 -0.7087 13 1 6 0.5012 -3.2181 13 1 7 0.3559 -1.6124 13 1 8 -0.0053 0.2273 13 1 9 0.4403 0.2137 13 1 10 0.1908 -0.3403 13 1 11 4.3374 1.0235 13 1 12 2.3672 -0.8170 13 1 13 -5.6885 -2.3244 13 3 0 -0.1077 0.1150 13 3 1 -2.0496 -1.2062 13 3 2 0.0939 -0.3282 13 3 3 1.7943 -3.9380 13 3 4 0.6829 -0.9873 13 3 5 1.4092 1.3908 13 3 6 1.5295 2.2866 13 3 7 0.6546 2.6577 13 3 8 -0.5996 -0.4070 13 3 9 0.0583 -1.2410 13 3 10 0.3756 -0.2936 13 3 11 -1.8656 -0.2034 13 3 12 -5.1404 -1.9091 13 3 13 2.5404 4.0385 13 5 0 -0.0373 0.0717 13 5 1 -0.0405 0.0459 13 5 2 3.6494 -1.9664 13 5 3 2.4946 0.8863 13 5 4 -1.1809 3.3323 13 5 5 -0.7327 0.0797 13 5 6 -0.3999 -2.4747 13 5 7 -2.6109 -3.2028 13 5 8 -1.0098 0.6096 13 5 9 -0.1996 1.4297 13 5 10 0.1094 3.0723 13 5 11 -0.6602 0.4343 13 5 12 2.0845 1.1395 13 7 0 -1.0170 0.0046 13 7 1 0.3751 -4.0286 13 7 2 0.4838 2.1218 13 7 3 -4.7984 4.8319 13 7 4 -1.3663 -0.5413 13 7 5 2.1166 -0.5860 13 7 6 -1.7046 0.8852 13 7 7 -1.5421 3.0822 13 7 8 0.3590 1.6554 13 7 9 0.6807 0.0651 13 7 10 0.0308 -1.4553 13 9 0 0.3771 -0.1050 13 9 1 0.1986 6.1164 13 9 2 -2.4366 3.4817 13 9 3 0.6727 -4.5992 13 9 4 2.3236 -1.9683 13 9 5 -1.7560 -1.2107 13 9 6 -1.7286 -0.0610 13 9 7 2.5344 0.7140 13 11 0 -1.9717 -0.2435 0 0 0 0.0 0.0 ; _shelx_fab_checksum 79484 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -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 Cd1 Cd 0.26555(4) 0.500000 0.500000 0.02745(13) Uani 1 2 d S T P . . Cd2 Cd 0.59258(4) 0.500000 0.500000 0.02778(13) Uani 1 2 d S T P . . P1 P 0.43447(13) 0.61791(4) 0.49518(4) 0.0277(3) Uani 1 1 d . . . . . O1 O 0.1042(4) 0.43913(18) 0.49819(18) 0.0717(15) Uani 1 1 d . . . . . H1A H 0.048532 0.443986 0.475600 0.108 Uiso 1 1 d R U . . . H1B H 0.050571 0.442651 0.521130 0.108 Uiso 1 1 d R U . . . O2 O 0.4291(3) 0.55822(10) 0.49907(14) 0.0315(6) Uani 1 1 d . . . . . O3 O 0.7471(4) 0.56334(16) 0.49465(16) 0.0453(11) Uani 1 1 d . . . . . H3A H 0.717046 0.594667 0.499727 0.068 Uiso 1 1 d R U . . . H3B H 0.803273 0.559338 0.514591 0.068 Uiso 1 1 d R U . . . O4 O 0.3487(5) 0.64105(18) 0.46319(16) 0.0543(14) Uani 1 1 d . . . . . O5 O 0.5670(4) 0.63640(14) 0.49035(11) 0.0427(10) Uani 1 1 d D . . . . O6 O 0.3904(4) 0.63657(15) 0.54157(13) 0.0392(11) Uani 1 1 d . . . . . O7 O 0.2000(4) 0.67781(14) 0.59559(12) 0.0396(9) Uani 1 1 d . . . . . O8 O 0.0832(4) 0.77049(16) 0.54871(14) 0.0531(12) Uani 1 1 d . . . . . H8 H 0.080998 0.797080 0.534162 0.080 Uiso 1 1 calc R U . . . O9 O 0.1602(6) 0.81255(18) 0.62575(17) 0.0717(16) Uani 1 1 d . . . . . H9 H 0.091393 0.815825 0.614982 0.108 Uiso 1 1 calc R U . . . O10 O 0.0082(4) 0.71162(17) 0.69507(12) 0.0479(11) Uani 1 1 d . . . . . O11 O 0.3164(5) 0.6674(3) 0.78426(15) 0.099(2) Uani 1 1 d . . . . . N3 N 0.1704(5) 0.4662(2) 0.27081(14) 0.0509(14) Uani 1 1 d . . . . . N4 N 0.1562(5) 0.4783(2) 0.22752(14) 0.0524(15) Uani 1 1 d . . . . . C2 C 0.2296(5) 0.54946(15) 0.36151(12) 0.056(2) Uani 1 1 d G . . . . H2 H 0.226895 0.581393 0.347361 0.067 Uiso 1 1 calc R U . . . C1 C 0.2468(5) 0.54829(15) 0.40503(12) 0.058(3) Uani 1 1 d G . . . . H1 H 0.255696 0.579440 0.420002 0.070 Uiso 1 1 calc R U . . . N1 N 0.2508(3) 0.50055(19) 0.42618(6) 0.0348(9) Uani 1 1 d G . . . . C5 C 0.2376(5) 0.45399(15) 0.40381(12) 0.0390(18) Uani 1 1 d G . . . . H5 H 0.240289 0.422050 0.417963 0.047 Uiso 1 1 calc R U . . . C4 C 0.2203(5) 0.45516(16) 0.36029(12) 0.0447(18) Uani 1 1 d G . . . . H4 H 0.211487 0.424002 0.345321 0.054 Uiso 1 1 calc R U . . . C3 C 0.2163(3) 0.5029(2) 0.33914(6) 0.0376(11) Uani 1 1 d G . . . . C6 C 0.1953(6) 0.5063(3) 0.29286(16) 0.0485(16) Uani 1 1 d . . . . . H6 H 0.200502 0.538777 0.279682 0.058 Uiso 1 1 calc R U . . . C7 C 0.0917(4) 0.49060(12) 0.09440(10) 0.0584(19) Uani 1 1 d G . . . . H7 H 0.092064 0.522336 0.079928 0.070 Uiso 1 1 calc R U . . . C8 C 0.1097(4) 0.48978(12) 0.13789(10) 0.0471(17) Uani 1 1 d G . . . . H8A H 0.122212 0.520964 0.152514 0.057 Uiso 1 1 calc R U . . . C9 C 0.1091(4) 0.44235(15) 0.15952(7) 0.0403(14) Uani 1 1 d G . . . . C10 C 0.0904(4) 0.39574(12) 0.13766(10) 0.0427(15) Uani 1 1 d G . . . . H10 H 0.090030 0.364008 0.152137 0.051 Uiso 1 1 calc R U . . . C11 C 0.0724(4) 0.39656(12) 0.09417(10) 0.0531(16) Uani 1 1 d G . . . . H11 H 0.059881 0.365379 0.079550 0.064 Uiso 1 1 calc R U . . . N5 N 0.0730(4) 0.44399(15) 0.07254(7) 0.0507(13) Uani 1 1 d G . . . . C12 C 0.1265(6) 0.4393(3) 0.20595(18) 0.0441(15) Uani 1 1 d . . . . . H12 H 0.114877 0.407251 0.219436 0.053 Uiso 1 1 calc R U . . . C25 C 0.3707(6) 0.6915(2) 0.5488(2) 0.0433(16) Uani 1 1 d . . . . . H25 H 0.432689 0.716836 0.548094 0.052 Uiso 1 1 calc R U . . . C26 C 0.2363(5) 0.7024(2) 0.55751(17) 0.0316(12) Uani 1 1 d . . . . . H26 H 0.186613 0.687875 0.534355 0.038 Uiso 1 1 calc R U . . . C27 C 0.2069(6) 0.7609(2) 0.56165(19) 0.0389(13) Uani 1 1 d . . . . . H27 H 0.266600 0.782722 0.546316 0.047 Uiso 1 1 calc R U . . . C28 C 0.2170(7) 0.7681(2) 0.60993(19) 0.0459(15) Uani 1 1 d . . . . . H28 H 0.304998 0.768847 0.617732 0.055 Uiso 1 1 calc R U . . . C29 C 0.1611(6) 0.7172(2) 0.62558(17) 0.0370(14) Uani 1 1 d . . . . . H29 H 0.070413 0.719978 0.625328 0.044 Uiso 1 1 calc R U . . . C30 C 0.1220(3) 0.70435(16) 0.70115(10) 0.0411(14) Uani 1 1 d G . . . . N8 N 0.1652(3) 0.69272(17) 0.74147(9) 0.0534(15) Uani 1 1 d G . . . . H8B H 0.115786 0.694523 0.762757 0.064 Uiso 1 1 calc R U . . . C31 C 0.2883(4) 0.6782(2) 0.74737(9) 0.076(2) Uani 1 1 d G . . . . C32 C 0.3682(3) 0.6753(2) 0.71296(12) 0.090(3) Uani 1 1 d G . . . . H32 H 0.450599 0.665541 0.716907 0.108 Uiso 1 1 calc R U . . . C33 C 0.3250(3) 0.68689(19) 0.67264(10) 0.064(2) Uani 1 1 d G . . . . H33 H 0.378448 0.684944 0.649622 0.077 Uiso 1 1 calc R U . . . N7 N 0.2019(3) 0.70143(16) 0.66674(8) 0.0455(13) Uani 1 1 d G . . . . N6 N 0.517(3) 0.5150(11) 0.7302(9) 0.045(5) Uani 0.5 1 d . . P A -1 N9 N 0.509(3) 0.5011(12) 0.7724(9) 0.051(5) Uani 0.5 1 d . . P A -1 C14 C 0.5922(11) 0.4438(3) 0.6362(3) 0.049(4) Uani 0.5 1 d G . P A -1 H14 H 0.600561 0.411353 0.649266 0.058 Uiso 0.5 1 calc R U P A -1 C13 C 0.6038(11) 0.4479(3) 0.5926(2) 0.039(4) Uani 0.5 1 d G . P A -1 H13 H 0.619929 0.418232 0.576456 0.047 Uiso 0.5 1 calc R U P A -1 N2 N 0.5913(11) 0.4965(4) 0.57306(17) 0.030(3) Uani 0.5 1 d G . P A -1 C17 C 0.5672(12) 0.5409(3) 0.5972(2) 0.040(4) Uani 0.5 1 d G . P A -1 H17 H 0.558800 0.573357 0.584094 0.048 Uiso 0.5 1 calc R U P A -1 C16 C 0.5556(13) 0.5368(3) 0.6408(2) 0.046(4) Uani 0.5 1 d G . P A -1 H16 H 0.539432 0.566479 0.656903 0.055 Uiso 0.5 1 calc R U P A -1 C15 C 0.5681(12) 0.4882(4) 0.66030(17) 0.033(3) Uani 0.5 1 d G . P A -1 C18 C 0.5474(18) 0.4801(6) 0.7064(4) 0.058(4) Uani 0.5 1 d . . P A -1 H18 H 0.557896 0.446541 0.717423 0.070 Uiso 0.5 1 calc R U P A -1 C21 C 0.4429(12) 0.5270(4) 0.84150(17) 0.038(3) Uani 0.5 1 d G . P A -1 C20 C 0.4176(11) 0.5694(3) 0.8677(2) 0.038(3) Uani 0.5 1 d G . P A -1 H20 H 0.412276 0.602982 0.856411 0.046 Uiso 0.5 1 calc R U P A -1 C19 C 0.4002(13) 0.5616(3) 0.9108(2) 0.044(5) Uani 0.5 1 d G . P A -1 H19 H 0.383272 0.589987 0.928301 0.052 Uiso 0.5 1 calc R U P A -1 N10 N 0.4081(15) 0.5114(4) 0.92765(18) 0.047(5) Uani 0.5 1 d G . P A -1 C23 C 0.4334(13) 0.4690(3) 0.9014(2) 0.035(3) Uani 0.5 1 d G . P A -1 H23 H 0.438671 0.435392 0.912737 0.041 Uiso 0.5 1 calc R U P A -1 C22 C 0.4508(11) 0.4768(3) 0.8584(2) 0.038(3) Uani 0.5 1 d G . P A -1 H22 H 0.467675 0.448385 0.840847 0.045 Uiso 0.5 1 calc R U P A -1 C24 C 0.4588(12) 0.5350(6) 0.7957(3) 0.040(3) Uani 0.5 1 d . . P A -1 H24 H 0.430794 0.566052 0.783661 0.048 Uiso 0.5 1 calc R U P A -1 O13 O 0.6939(6) 0.6901(3) 0.5552(2) 0.094(2) Uani 1 1 d G . . . . H13A H 0.769877 0.697089 0.550669 0.142 Uiso 1 1 d G U . . . H13B H 0.672193 0.671403 0.534261 0.142 Uiso 1 1 d DG U . . . O14 O 0.4146(10) 0.6687(4) 0.3830(2) 0.166(4) Uani 1 1 d G U . . . H14A H 0.386251 0.699830 0.381785 0.249 Uiso 1 1 d G U . . . H14B H 0.395234 0.658187 0.407613 0.249 Uiso 1 1 d G U . . . O12 O -0.0790(7) 0.6951(2) 0.5187(2) 0.0945(19) Uani 1 1 d G . . . . H12A H -0.051084 0.675578 0.499084 0.142 Uiso 1 1 d G U . . . H12B H -0.033760 0.722348 0.517734 0.142 Uiso 1 1 d G U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0284(2) 0.0341(3) 0.0198(2) 0.0009(4) 0.000 0.000 Cd2 0.0288(3) 0.0386(3) 0.01590(19) -0.0007(3) 0.000 0.000 P1 0.0355(6) 0.0232(5) 0.0245(7) 0.0001(6) 0.0021(8) -0.0017(5) O1 0.073(3) 0.096(3) 0.046(2) 0.017(4) -0.025(4) -0.047(3) O2 0.0320(15) 0.0221(14) 0.0402(16) 0.002(2) -0.002(4) -0.0012(13) O3 0.043(2) 0.055(2) 0.038(3) 0.003(2) 0.002(2) -0.0079(17) O4 0.065(3) 0.042(3) 0.055(3) 0.010(2) -0.021(3) 0.002(2) O5 0.044(2) 0.038(2) 0.047(3) -0.0008(16) 0.013(2) -0.0059(18) O6 0.051(3) 0.0217(19) 0.045(2) 0.0036(17) 0.019(2) 0.0095(18) O7 0.050(3) 0.030(2) 0.038(2) -0.0003(18) 0.0032(19) 0.0055(19) O8 0.059(3) 0.038(2) 0.062(3) 0.014(2) -0.004(2) 0.014(2) O9 0.107(5) 0.047(3) 0.061(3) -0.014(2) 0.010(3) 0.025(3) O10 0.038(2) 0.073(3) 0.033(2) 0.002(2) 0.0083(18) 0.005(2) O11 0.052(3) 0.208(7) 0.037(3) -0.002(4) -0.018(2) 0.004(4) N3 0.060(4) 0.077(4) 0.016(2) 0.003(2) -0.004(2) -0.004(3) N4 0.057(4) 0.079(4) 0.021(2) -0.002(2) -0.006(2) -0.007(3) C2 0.102(7) 0.040(4) 0.025(3) 0.002(3) -0.017(4) -0.010(4) C1 0.089(8) 0.044(5) 0.043(4) -0.003(4) -0.004(4) 0.010(5) N1 0.034(2) 0.042(2) 0.028(2) 0.010(3) -0.0014(14) 0.004(4) C5 0.047(5) 0.045(4) 0.026(3) -0.009(3) -0.009(3) 0.016(4) C4 0.048(5) 0.046(4) 0.041(4) -0.012(3) 0.000(3) 0.008(4) C3 0.037(3) 0.049(3) 0.027(2) 0.007(3) -0.0031(19) -0.004(4) C6 0.061(4) 0.060(5) 0.024(2) -0.004(3) -0.001(2) -0.019(4) C7 0.067(5) 0.072(5) 0.035(3) 0.007(3) -0.001(3) 0.009(4) C8 0.050(3) 0.053(5) 0.038(3) -0.009(3) -0.003(2) -0.002(3) C9 0.039(3) 0.059(4) 0.023(3) -0.003(3) -0.002(2) -0.001(3) C10 0.048(4) 0.039(3) 0.041(3) -0.004(3) 0.004(3) -0.009(3) C11 0.059(4) 0.068(4) 0.032(3) -0.002(3) 0.013(3) -0.003(4) N5 0.064(4) 0.060(3) 0.029(2) -0.010(2) 0.001(3) -0.004(3) C12 0.052(4) 0.051(4) 0.029(3) 0.004(3) 0.002(3) -0.006(3) C25 0.044(4) 0.027(3) 0.059(4) -0.003(3) 0.024(3) 0.000(3) C26 0.040(3) 0.033(3) 0.022(3) 0.003(2) -0.004(2) 0.000(3) C27 0.040(3) 0.028(3) 0.048(3) 0.005(3) 0.009(3) 0.004(3) C28 0.071(4) 0.021(3) 0.045(4) -0.012(3) 0.009(3) 0.002(3) C29 0.042(3) 0.035(3) 0.034(3) 0.006(2) 0.012(2) 0.015(3) C30 0.037(3) 0.048(4) 0.038(3) 0.000(3) 0.008(3) -0.001(3) N8 0.038(3) 0.098(5) 0.024(3) 0.005(3) 0.009(2) -0.006(3) C31 0.040(4) 0.132(7) 0.055(5) 0.032(5) 0.005(4) 0.010(5) C32 0.046(4) 0.198(10) 0.026(3) 0.006(5) 0.011(3) 0.023(6) C33 0.046(4) 0.091(6) 0.056(4) 0.012(4) 0.009(3) 0.026(4) N7 0.041(3) 0.070(4) 0.026(2) -0.008(2) 0.003(2) 0.001(3) N6 0.035(12) 0.083(13) 0.018(5) -0.007(7) 0.000(7) -0.007(9) N9 0.048(13) 0.085(14) 0.020(5) 0.000(8) -0.003(7) 0.030(9) C14 0.070(12) 0.039(7) 0.037(6) -0.007(5) 0.001(7) -0.004(7) C13 0.041(11) 0.043(8) 0.033(6) -0.010(5) 0.013(6) 0.005(6) N2 0.019(7) 0.056(7) 0.016(6) -0.002(5) -0.005(5) -0.004(7) C17 0.055(11) 0.048(8) 0.018(5) 0.008(5) 0.002(7) 0.000(8) C16 0.073(13) 0.046(7) 0.019(6) 0.000(5) 0.001(7) 0.010(8) C15 0.037(6) 0.039(7) 0.025(5) -0.008(4) -0.001(5) -0.008(6) C18 0.069(12) 0.072(8) 0.033(6) 0.003(5) 0.013(7) 0.001(8) C21 0.042(8) 0.050(7) 0.021(5) -0.006(5) -0.010(6) 0.005(7) C20 0.041(7) 0.048(6) 0.025(5) -0.001(5) -0.004(5) 0.008(7) C19 0.066(13) 0.042(7) 0.023(5) -0.006(5) 0.003(6) 0.013(7) N10 0.069(15) 0.038(6) 0.035(9) -0.002(4) 0.004(9) 0.014(6) C23 0.048(10) 0.034(7) 0.022(5) -0.003(5) -0.006(6) 0.026(7) C22 0.029(8) 0.055(7) 0.028(6) 0.005(5) 0.001(6) 0.015(6) C24 0.034(8) 0.070(9) 0.016(5) 0.003(5) -0.002(5) 0.014(6) O13 0.077(5) 0.124(6) 0.082(4) -0.014(4) -0.012(4) -0.022(4) O14 0.173(8) 0.237(9) 0.089(5) 0.040(6) -0.041(5) -0.130(8) O12 0.090(5) 0.076(4) 0.117(5) 0.028(3) -0.012(4) -0.006(4) 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' Cd Cd -0.8075 1.2024 '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' P P 0.1023 0.0942 '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 O1 Cd1 O1 83.6(3) 4_566 . ? O1 Cd1 N1 88.28(17) 4_566 . ? O1 Cd1 N1 88.3(4) . 4_566 ? O1 Cd1 N1 85.93(17) . . ? O1 Cd1 N1 85.9(4) 4_566 4_566 ? O2 Cd1 O1 177.30(18) . . ? O2 Cd1 O1 98.14(15) 4_566 . ? O2 Cd1 O1 98.14(15) . 4_566 ? O2 Cd1 O1 177.31(18) 4_566 4_566 ? O2 Cd1 O2 80.24(15) 4_566 . ? O2 Cd1 N1 92.02(15) . . ? O2 Cd1 N1 92.0(3) 4_566 4_566 ? O2 Cd1 N1 93.92(15) 4_566 . ? O2 Cd1 N1 93.9(4) . 4_566 ? N1 Cd1 N1 172.2(3) 4_566 . ? O2 Cd2 O2 80.29(14) . 4_566 ? O2 Cd2 O3 95.66(13) 4_566 4_566 ? O2 Cd2 O3 174.73(16) . 4_566 ? O2 Cd2 O3 95.66(13) . . ? O2 Cd2 O3 174.73(16) 4_566 . ? O2 Cd2 N2 87.6(3) 4_566 . ? O2 Cd2 N2 91.9(3) . . ? O3 Cd2 O3 88.6(2) 4_566 . ? N2 Cd2 O3 84.5(3) . 4_566 ? N2 Cd2 O3 96.0(3) . . ? O2 P1 O6 102.1(2) . . ? O4 P1 O2 115.2(3) . . ? O4 P1 O5 113.1(3) . . ? O4 P1 O6 108.5(3) . . ? O5 P1 O2 110.8(2) . . ? O5 P1 O6 106.1(2) . . ? Cd1 O1 H1A 114.0 . . ? Cd1 O1 H1B 112.3 . . ? H1A O1 H1B 100.6 . . ? Cd2 O2 Cd1 99.73(10) . . ? P1 O2 Cd1 132.18(18) . . ? P1 O2 Cd2 127.91(18) . . ? Cd2 O3 H3A 110.8 . . ? Cd2 O3 H3B 111.1 . . ? H3A O3 H3B 103.2 . . ? C25 O6 P1 118.4(4) . . ? C26 O7 C29 109.4(4) . . ? C27 O8 H8 109.5 . . ? C28 O9 H9 109.5 . . ? C6 N3 N4 112.5(6) . . ? C12 N4 N3 112.6(5) . . ? C1 C2 H2 120.0 . . ? C1 C2 C3 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C1 H1 120.0 . . ? N1 C1 C2 120.0 . . ? N1 C1 H1 120.0 . . ? C1 N1 Cd1 119.2(2) . . ? C5 N1 Cd1 120.7(2) . . ? C5 N1 C1 120.0 . . ? N1 C5 H5 120.0 . . ? N1 C5 C4 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C2 C3 C6 117.9(5) . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 122.0(5) . . ? N3 C6 C3 122.0(6) . . ? N3 C6 H6 119.0 . . ? C3 C6 H6 119.0 . . ? C8 C7 H7 120.0 . . ? C8 C7 N5 120.0 . . ? N5 C7 H7 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C12 122.2(3) . . ? C10 C9 C8 120.0 . . ? C10 C9 C12 117.8(3) . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 H11 120.0 . . ? N5 C11 C10 120.0 . . ? N5 C11 H11 120.0 . . ? C11 N5 C7 120.0 . . ? N4 C12 C9 122.1(5) . . ? N4 C12 H12 118.9 . . ? C9 C12 H12 118.9 . . ? O6 C25 H25 124.7 . . ? O6 C25 C26 110.7(5) . . ? C26 C25 H25 124.7 . . ? O7 C26 C25 110.0(5) . . ? O7 C26 H26 108.6 . . ? O7 C26 C27 107.6(4) . . ? C25 C26 H26 108.6 . . ? C25 C26 C27 113.3(5) . . ? C27 C26 H26 108.6 . . ? O8 C27 C26 109.8(5) . . ? O8 C27 H27 112.1 . . ? O8 C27 C28 109.4(5) . . ? C26 C27 H27 112.1 . . ? C26 C27 C28 100.7(4) . . ? C28 C27 H27 112.1 . . ? O9 C28 C27 115.1(5) . . ? O9 C28 H28 108.7 . . ? O9 C28 C29 114.1(6) . . ? C27 C28 H28 108.7 . . ? C29 C28 C27 101.2(5) . . ? C29 C28 H28 108.7 . . ? O7 C29 C28 105.4(4) . . ? O7 C29 H29 109.5 . . ? C28 C29 H29 109.5 . . ? N7 C29 O7 108.2(4) . . ? N7 C29 C28 114.7(5) . . ? N7 C29 H29 109.5 . . ? O10 C30 N8 120.0(3) . . ? O10 C30 N7 119.5(3) . . ? N8 C30 N7 120.0 . . ? C30 N8 H8B 120.0 . . ? C30 N8 C31 120.0 . . ? C31 N8 H8B 120.0 . . ? O11 C31 N8 114.8(4) . . ? O11 C31 C32 125.2(4) . . ? C32 C31 N8 120.0 . . ? C31 C32 H32 120.0 . . ? C31 C32 C33 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 H33 120.0 . . ? N7 C33 C32 120.0 . . ? N7 C33 H33 120.0 . . ? C30 N7 C29 120.5(3) . . ? C33 N7 C29 119.3(3) . . ? C33 N7 C30 120.0 . . ? C18 N6 N9 115(3) . . ? C24 N9 N6 115(3) . . ? C13 C14 H14 120.0 . . ? C13 C14 C15 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C13 H13 120.0 . . ? N2 C13 C14 120.0 . . ? N2 C13 H13 120.0 . . ? C13 N2 Cd2 118.6(5) . . ? C13 N2 C17 120.0 . . ? C17 N2 Cd2 121.2(5) . . ? N2 C17 H17 120.0 . . ? N2 C17 C16 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C14 C15 C18 116.8(9) . . ? C16 C15 C14 120.0 . . ? C16 C15 C18 123.0(9) . . ? N6 C18 C15 123.1(19) . . ? N6 C18 H18 118.5 . . ? C15 C18 H18 118.5 . . ? C20 C21 C22 120.0 . . ? C20 C21 C24 120.1(8) . . ? C22 C21 C24 119.9(8) . . ? C21 C20 H20 120.0 . . ? C19 C20 C21 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C19 H19 120.0 . . ? C20 C19 N10 120.0 . . ? N10 C19 H19 120.0 . . ? C23 N10 C19 120.0 . . ? N10 C23 H23 120.0 . . ? N10 C23 C22 120.0 . . ? C22 C23 H23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? N9 C24 C21 122.0(15) . . ? N9 C24 H24 119.0 . . ? C21 C24 H24 119.0 . . ? H13A O13 H13B 104.5 . . ? H14A O14 H14B 104.4 . . ? H12A O12 H12B 104.4 . . ? 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 Cd1 O1 2.332(4) . ? Cd1 O1 2.332(4) 4_566 ? Cd1 O2 2.305(3) 4_566 ? Cd1 O2 2.305(3) . ? Cd1 N1 2.341(2) 4_566 ? Cd1 N1 2.341(2) . ? Cd2 O2 2.304(3) . ? Cd2 O2 2.304(3) 4_566 ? Cd2 O3 2.326(4) . ? Cd2 O3 2.326(4) 4_566 ? Cd2 N2 2.314(6) . ? P1 O2 1.529(3) . ? P1 O4 1.492(5) . ? P1 O5 1.512(4) . ? P1 O6 1.614(4) . ? O1 H1A 0.9412 . ? O1 H1B 0.9319 . ? O3 H3A 0.8771 . ? O3 H3B 0.8802 . ? O6 C25 1.435(7) . ? O7 C26 1.413(6) . ? O7 C29 1.445(6) . ? O8 H8 0.8200 . ? O8 C27 1.415(7) . ? O9 H9 0.8200 . ? O9 C28 1.383(7) . ? O10 C30 1.255(5) . ? O11 C31 1.237(5) . ? N3 N4 1.412(6) . ? N3 C6 1.265(8) . ? N4 C12 1.248(7) . ? C2 H2 0.9300 . ? C2 C1 1.3900 . ? C2 C3 1.3900 . ? C1 H1 0.9300 . ? C1 N1 1.3900 . ? N1 C5 1.3900 . ? C5 H5 0.9300 . ? C5 C4 1.3900 . ? C4 H4 0.9300 . ? C4 C3 1.3900 . ? C3 C6 1.484(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C7 C8 1.3900 . ? C7 N5 1.3900 . ? C8 H8A 0.9300 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C9 C12 1.483(6) . ? C10 H10 0.9300 . ? C10 C11 1.3900 . ? C11 H11 0.9300 . ? C11 N5 1.3900 . ? C12 H12 0.9300 . ? C25 H25 0.9300 . ? C25 C26 1.500(8) . ? C26 H26 0.9800 . ? C26 C27 1.530(8) . ? C27 H27 0.9800 . ? C27 C28 1.543(8) . ? C28 H28 0.9800 . ? C28 C29 1.512(8) . ? C29 H29 0.9800 . ? C29 N7 1.432(6) . ? C30 N8 1.3900 . ? C30 N7 1.3900 . ? N8 H8B 0.8600 . ? N8 C31 1.3900 . ? C31 C32 1.3900 . ? C32 H32 0.9300 . ? C32 C33 1.3900 . ? C33 H33 0.9300 . ? C33 N7 1.3900 . ? N6 N9 1.385(17) . ? N6 C18 1.21(3) . ? N9 C24 1.26(3) . ? C14 H14 0.9300 . ? C14 C13 1.3900 . ? C14 C15 1.3900 . ? C13 H13 0.9300 . ? C13 N2 1.3900 . ? N2 C17 1.3900 . ? C17 H17 0.9300 . ? C17 C16 1.3900 . ? C16 H16 0.9300 . ? C16 C15 1.3900 . ? C15 C18 1.491(15) . ? C18 H18 0.9300 . ? C21 C20 1.3900 . ? C21 C22 1.3900 . ? C21 C24 1.473(12) . ? C20 H20 0.9300 . ? C20 C19 1.3900 . ? C19 H19 0.9300 . ? C19 N10 1.3900 . ? N10 C23 1.3900 . ? C23 H23 0.9300 . ? C23 C22 1.3900 . ? C22 H22 0.9300 . ? C24 H24 0.9300 . ? O13 H13A 0.8498 . ? O13 H13B 0.8496 . ? O14 H14A 0.8502 . ? O14 H14B 0.8500 . ? O12 H12A 0.8515 . ? O12 H12B 0.8496 . ? 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 O3 H3A O5 0.88 1.96 2.694(6) 140.6 . yes O8 H8 O5 0.82 1.87 2.683(5) 170.0 8_466 yes O9 H9 O14 0.82 1.95 2.703(12) 153.1 8_466 yes N8 H8B O10 0.86 1.94 2.785(5) 168.1 3_556 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 Cd1 N1 C5 C4 175.5(2) . . . . ? Cd2 N2 C17 C16 174.0(8) . . . . ? P1 O6 C25 C26 114.3(5) . . . . ? O2 P1 O6 C25 -173.3(4) . . . . ? O4 P1 O2 Cd1 -42.3(4) . . . . ? O4 P1 O2 Cd2 131.8(3) . . . . ? O4 P1 O6 C25 -51.3(5) . . . . ? O5 P1 O2 Cd1 -172.3(3) . . . . ? O5 P1 O2 Cd2 1.8(4) . . . . ? O5 P1 O6 C25 70.6(5) . . . . ? O6 P1 O2 Cd1 75.0(4) . . . . ? O6 P1 O2 Cd2 -110.8(3) . . . . ? O6 C25 C26 O7 64.6(6) . . . . ? O6 C25 C26 C27 -174.9(5) . . . . ? O7 C26 C27 O8 -87.5(5) . . . . ? O7 C26 C27 C28 27.8(6) . . . . ? O7 C29 N7 C30 -134.4(4) . . . . ? O7 C29 N7 C33 50.5(6) . . . . ? O8 C27 C28 O9 -45.8(7) . . . . ? O8 C27 C28 C29 77.8(6) . . . . ? O9 C28 C29 O7 160.3(5) . . . . ? O9 C28 C29 N7 -80.8(7) . . . . ? O10 C30 N8 C31 171.9(5) . . . . ? O10 C30 N7 C29 13.0(5) . . . . ? O10 C30 N7 C33 -171.9(5) . . . . ? O11 C31 C32 C33 178.1(7) . . . . ? N3 N4 C12 C9 -178.7(5) . . . . ? N4 N3 C6 C3 -178.9(5) . . . . ? C2 C1 N1 Cd1 -175.60(19) . . . . ? C2 C1 N1 C5 0.0 . . . . ? C2 C3 C6 N3 -173.1(6) . . . . ? C1 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C6 178.6(4) . . . . ? C1 N1 C5 C4 0.0 . . . . ? N1 C5 C4 C3 0.0 . . . . ? C5 C4 C3 C2 0.0 . . . . ? C5 C4 C3 C6 -178.6(4) . . . . ? C4 C3 C6 N3 5.5(8) . . . . ? C3 C2 C1 N1 0.0 . . . . ? C6 N3 N4 C12 -177.1(6) . . . . ? C7 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C12 -179.3(4) . . . . ? C8 C7 N5 C11 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C8 C9 C12 N4 -8.1(8) . . . . ? C9 C10 C11 N5 0.0 . . . . ? C10 C9 C12 N4 172.6(5) . . . . ? C10 C11 N5 C7 0.0 . . . . ? N5 C7 C8 C9 0.0 . . . . ? C12 C9 C10 C11 179.3(4) . . . . ? C25 C26 C27 O8 150.7(5) . . . . ? C25 C26 C27 C28 -94.0(6) . . . . ? C26 O7 C29 C28 -19.5(6) . . . . ? C26 O7 C29 N7 -142.6(4) . . . . ? C26 C27 C28 O9 -161.4(6) . . . . ? C26 C27 C28 C29 -37.9(6) . . . . ? C27 C28 C29 O7 36.1(6) . . . . ? C27 C28 C29 N7 154.9(5) . . . . ? C28 C29 N7 C30 108.3(5) . . . . ? C28 C29 N7 C33 -66.9(5) . . . . ? C29 O7 C26 C25 118.0(5) . . . . ? C29 O7 C26 C27 -5.9(6) . . . . ? C30 N8 C31 O11 -178.3(6) . . . . ? C30 N8 C31 C32 0.0 . . . . ? N8 C30 N7 C29 -175.1(5) . . . . ? N8 C30 N7 C33 0.0 . . . . ? N8 C31 C32 C33 0.0 . . . . ? C31 C32 C33 N7 0.0 . . . . ? C32 C33 N7 C29 175.1(4) . . . . ? C32 C33 N7 C30 0.0 . . . . ? N7 C30 N8 C31 0.0 . . . . ? N6 N9 C24 C21 -179.6(14) . . . . ? N9 N6 C18 C15 -176.5(15) . . . . ? C14 C13 N2 Cd2 -174.2(8) . . . . ? C14 C13 N2 C17 0.0 . . . . ? C14 C15 C18 N6 -174.9(19) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C13 C14 C15 C18 175.5(13) . . . . ? C13 N2 C17 C16 0.0 . . . . ? N2 C17 C16 C15 0.0 . . . . ? C17 C16 C15 C14 0.0 . . . . ? C17 C16 C15 C18 -175.2(14) . . . . ? C16 C15 C18 N6 0(3) . . . . ? C15 C14 C13 N2 0.0 . . . . ? C18 N6 N9 C24 -169(3) . . . . ? C21 C20 C19 N10 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C20 C21 C24 N9 163(2) . . . . ? C20 C19 N10 C23 0.0 . . . . ? C19 N10 C23 C22 0.0 . . . . ? N10 C23 C22 C21 0.0 . . . . ? C22 C21 C20 C19 0.0 . . . . ? C22 C21 C24 N9 -18(3) . . . . ? C24 C21 C20 C19 178.8(13) . . . . ? C24 C21 C22 C23 -178.8(12) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.713 0.172 0.250 541.1 158.3 ? 2 0.200 0.328 0.750 541.1 158.3 ? 3 -0.793 0.672 0.250 541.1 158.3 ? 4 -0.767 0.828 0.750 541.1 158.3 ?