#------------------------------------------------------------------------------ #$Date: 2020-08-21 04:43:26 +0300 (Fri, 21 Aug 2020) $ #$Revision: 255505 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705228.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_7705228 loop_ _publ_author_name 'Li, Meng-Hua' 'Lv, Shu-Li' 'You, Ming-Hua' 'Lin, Mei-Jin' _publ_section_title ; Three-component D-A hybrid heterostructures with enhanced photochromic, photomodulated luminescent and selectively anion-sensing properties ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02390F _journal_year 2020 _chemical_formula_moiety 'C14 H20 N2 O8 Sm, C6 Co N6, 0.5(H O), 2(H2 O)' _chemical_formula_sum 'C20 H24.5 Co N8 O10.5 Sm' _chemical_formula_weight 754.25 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-07-30 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139) ; _audit_update_record ; 2020-07-30 deposited with the CCDC. 2020-08-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 130.659(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 31.267(2) _cell_length_b 11.4024(6) _cell_length_c 21.1252(14) _cell_measurement_reflns_used 9044 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 26.35 _cell_measurement_theta_min 2.54 _cell_volume 5713.4(6) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 33182 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.542 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 2.682 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6473 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0671 before and 0.0487 after correction. The Ratio of minimum to maximum transmission is 0.8684. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light white' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary white _exptl_crystal_density_diffrn 1.754 _exptl_crystal_description block _exptl_crystal_F_000 2988 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.814 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 395 _refine_ls_number_reflns 5042 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0283 _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^)+(0.0280P)^2^+31.3009P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.0692 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4576 _reflns_number_total 5042 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02390f2.cif _cod_data_source_block c2 _cod_original_formula_sum 'C20 H24.50 Co N8 O10.50 Sm' _cod_database_code 7705228 _shelx_shelxl_version_number 2017/1 _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 0.757 _shelx_estimated_absorpt_t_min 0.616 _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 O(H) groups, All O(H,H) groups 2. Restrained distances Sm1-H8a \\sim Sm1-H8b with sigma of 0.02 Sm1-H7a \\sim Sm1-H7b with sigma of 0.02 3. Others Fixed Sof: H6(0.5) 4.a Free rotating group: O8(H8a,H8b), O7(H7a,H7b), O6(H6), O5(H5a,H5b) 4.b Rotating group: O11(H11a,H11b) 4.c Secondary CH2 refined with riding coordinates: C19(H19a,H19b), C8(H8c,H8d) 4.d Aromatic/amide H refined with riding coordinates: C17(H17), C13(H13), C10(H10), C18(H18), C12(H12), C9(H9), C16(H16), C15(H15) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL c2_a.res in C2/c c2.res created by SHELXL-2017/1 at 16:02:55 on 29-Jul-2020 REM Old TITL C2 in C2/c REM SHELXT solution in C2/c REM R1 0.104, Rweak 0.003, Alpha 0.047, Orientation as input REM Formula found by SHELXT: C42 N19 O17 Fe2 Sm2 CELL 0.71073 31.2667 11.4024 21.1252 90 130.659 90 ZERR 8 0.0021 0.0006 0.0014 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Co N O Sm UNIT 160 196 8 64 84 8 SADI Sm1 H8a Sm1 H8b SADI Sm1 H7a Sm1 H7b L.S. 5 PLAN 19 SIZE 0.2 0.15 0.11 TEMP 23 CONF FREE H10a Sm1 FREE H10a H10b FREE H9a H9b list 4 MORE -1 BOND $H ABIN fmap 2 53 acta SHEL 999 0.84 REM REM REM WGHT 0.028000 31.300900 FVAR 0.15705 SM1 6 0.423541 0.551447 0.489864 11.00000 0.02337 0.01952 = 0.02675 -0.00402 0.01282 -0.00127 CO1 3 0.638457 0.974871 0.787008 11.00000 0.03696 0.02311 = 0.02587 -0.00173 0.02297 -0.00001 O3 5 0.603754 0.544436 0.635285 11.00000 0.03128 0.04102 = 0.02881 -0.00390 0.01593 0.00443 AFIX 6 O8 5 0.341655 0.669280 0.382453 11.00000 0.02533 0.03025 = 0.04490 0.00742 0.02095 0.00243 H8A 2 0.345315 0.737026 0.369671 11.00000 -1.50000 H8B 2 0.312394 0.674420 0.377092 11.00000 -1.50000 AFIX 0 O4 5 0.520374 0.582029 0.599640 11.00000 0.02354 0.04558 = 0.04913 -0.02031 0.00837 0.00498 O2 5 0.965026 0.139031 1.034239 11.00000 0.03332 0.02450 = 0.05220 -0.00226 0.02834 -0.00250 O1 5 1.048289 0.175388 1.069098 11.00000 0.02921 0.03483 = 0.05858 -0.01044 0.02599 -0.00144 O10 5 0.338527 0.438189 0.428631 11.00000 0.04573 0.04147 = 0.06377 -0.00149 0.04093 -0.00700 N7 4 0.935700 0.362216 1.012484 11.00000 0.02549 0.02175 = 0.02424 -0.00006 0.01405 0.00018 AFIX 6 O7 5 0.431578 0.739137 0.552026 11.00000 0.03332 0.04427 = 0.07688 -0.03409 0.03231 -0.01019 H7A 2 0.460620 0.782441 0.577049 11.00000 -1.50000 H7B 2 0.419591 0.750639 0.577811 11.00000 -1.50000 AFIX 0 N8 4 0.654529 0.499173 0.796649 11.00000 0.02665 0.03407 = 0.03224 0.00267 0.01937 0.00501 AFIX 6 O6 5 0.500000 1.356130 0.750000 10.50000 0.04494 0.02776 = 0.07405 0.00000 0.03636 0.00000 H6 2 0.524157 1.310324 0.756808 10.50000 -1.50000 AFIX 0 C3 1 0.643827 1.065930 0.717411 11.00000 0.02166 0.02322 = 0.02620 -0.00066 0.01381 0.00057 O9 5 0.268094 0.401992 0.265682 11.00000 0.03003 0.06316 = 0.05795 -0.00809 0.02225 -0.00255 N5 4 0.647698 1.120498 0.676064 11.00000 0.02748 0.03353 = 0.03620 0.00710 0.01899 0.00128 N1 4 0.529154 0.871048 0.633069 11.00000 0.05673 0.04127 = 0.04380 -0.01263 0.03662 -0.01826 C11 1 0.765404 0.432880 0.893274 11.00000 0.03169 0.02601 = 0.02196 0.00292 0.01845 0.00400 C20 1 1.002695 0.204372 1.050578 11.00000 0.02708 0.02527 = 0.03128 -0.00315 0.01657 -0.00160 C7 1 0.571723 0.555904 0.650647 11.00000 0.02627 0.02604 = 0.03482 -0.00953 0.01079 0.00266 O11 5 0.428658 0.506637 0.605876 11.00000 0.08812 0.08991 = 0.06346 0.00547 0.05944 0.02325 AFIX 7 H11A 2 0.427664 0.429568 0.611274 11.00000 -1.50000 H11B 2 0.398094 0.531292 0.597085 11.00000 -1.50000 AFIX 0 C17 1 0.894552 0.337933 0.931047 11.00000 0.03167 0.03450 = 0.02428 -0.00118 0.02090 0.00046 AFIX 43 H17 2 0.903702 0.306647 0.900534 11.00000 -1.20000 AFIX 0 C6 1 0.632706 0.877258 0.854206 11.00000 0.06279 0.03214 = 0.03629 -0.00483 0.03762 -0.00069 AFIX 6 O5 5 0.848866 1.150867 1.084740 11.00000 0.06807 0.05119 = 0.08826 -0.02530 0.05242 -0.01192 H5A 2 0.862090 1.214728 1.112008 11.00000 -1.50000 H5B 2 0.824232 1.165794 1.032900 11.00000 -1.50000 AFIX 0 C14 1 0.825179 0.404736 0.937333 11.00000 0.03092 0.01917 = 0.02296 0.00131 0.01666 0.00318 C13 1 0.667319 0.397361 0.780713 11.00000 0.03418 0.03060 = 0.03690 -0.00431 0.02309 -0.00536 AFIX 43 H13 2 0.638705 0.350099 0.737146 11.00000 -1.20000 AFIX 0 C2 1 0.595126 1.096824 0.780477 11.00000 0.03803 0.03458 = 0.03397 -0.00931 0.02650 -0.00505 C19 1 0.994024 0.335470 1.049982 11.00000 0.02669 0.02723 = 0.03233 -0.00139 0.01789 -0.00211 AFIX 23 H19A 2 1.019746 0.365038 1.106718 11.00000 -1.20000 H19B 2 1.002522 0.374656 1.018554 11.00000 -1.20000 AFIX 0 C10 1 0.750597 0.534145 0.911597 11.00000 0.03303 0.03425 = 0.02553 -0.00239 0.01630 0.00607 AFIX 43 H10 2 0.778275 0.580435 0.956945 11.00000 -1.20000 AFIX 0 C18 1 0.839317 0.358868 0.892680 11.00000 0.02872 0.03142 = 0.01827 0.00073 0.01437 0.00003 AFIX 43 H18 2 0.811189 0.342094 0.836251 11.00000 -1.20000 AFIX 0 C1 1 0.571534 0.906838 0.691421 11.00000 0.04985 0.02341 = 0.03334 -0.00778 0.03204 -0.01022 N6 4 0.570550 1.176409 0.775404 11.00000 0.05794 0.05187 = 0.05798 -0.00857 0.04155 0.00867 N2 4 0.628868 0.816618 0.893592 11.00000 0.09405 0.04248 = 0.05111 -0.00236 0.05832 -0.00744 C8 1 0.595058 0.537586 0.739793 11.00000 0.02978 0.04735 = 0.04407 -0.00215 0.02593 0.00382 AFIX 23 H8C 2 0.592048 0.610418 0.760376 11.00000 -1.20000 H8D 2 0.572438 0.479128 0.739608 11.00000 -1.20000 AFIX 0 C12 1 0.722343 0.362734 0.828339 11.00000 0.03230 0.02401 = 0.03326 0.00031 0.02187 0.00168 AFIX 43 H12 2 0.730942 0.291816 0.817149 11.00000 -1.20000 AFIX 0 C9 1 0.694755 0.565468 0.862243 11.00000 0.03705 0.03332 = 0.03040 -0.00103 0.02171 0.00658 AFIX 43 H9 2 0.684762 0.633200 0.874416 11.00000 -1.20000 AFIX 0 C5 1 0.686726 0.862554 0.795850 11.00000 0.05698 0.03935 = 0.03066 0.01142 0.03241 0.01290 N3 4 0.718248 0.797657 0.802883 11.00000 0.07500 0.05815 = 0.05262 0.02312 0.04820 0.03043 C4 1 0.703234 1.051269 0.881952 11.00000 0.05406 0.05043 = 0.03594 0.00451 0.03193 0.00253 C16 1 0.923264 0.403389 1.057917 11.00000 0.03090 0.04342 = 0.02143 -0.00755 0.01048 0.00741 AFIX 43 H16 2 0.952043 0.416940 1.114661 11.00000 -1.20000 AFIX 0 C15 1 0.868286 0.426002 1.021664 11.00000 0.03828 0.04809 = 0.02277 -0.00626 0.01650 0.01300 AFIX 43 H15 2 0.860059 0.455527 1.053714 11.00000 -1.20000 AFIX 0 N4 4 0.742258 1.101356 0.938792 11.00000 0.07626 0.09359 = 0.02971 -0.01094 0.02078 -0.03144 H10A 2 0.350031 0.448631 0.466253 11.00000 0.01467 H10B 2 0.324573 0.395519 0.439958 11.00000 0.22142 H9A 2 0.276466 0.391128 0.307946 11.00000 0.01008 H9B 2 0.232302 0.401487 0.239553 11.00000 0.08484 HKLF 4 REM c2_a.res in C2/c REM R1 = 0.0283 for 4576 Fo > 4sig(Fo) and 0.0329 for all 5042 data REM 395 parameters refined using 2 restraints END WGHT 0.0280 31.2970 REM Highest difference peak 1.814, deepest hole -0.536, 1-sigma level 0.088 Q1 1 0.4003 0.5590 0.5015 11.00000 0.05 1.81 Q2 1 0.6776 0.7553 0.7687 11.00000 0.05 0.99 Q3 1 0.4407 0.5225 0.4610 11.00000 0.05 0.83 Q4 1 0.5999 0.9574 0.7459 11.00000 0.05 0.64 Q5 1 0.4587 0.5407 0.6375 11.00000 0.05 0.58 Q6 1 0.6584 0.9924 0.7780 11.00000 0.05 0.56 Q7 1 0.2790 0.3448 0.2454 11.00000 0.05 0.45 Q8 1 0.6455 0.8352 0.7548 11.00000 0.05 0.44 Q9 1 0.6604 1.1383 0.7184 11.00000 0.05 0.41 Q10 1 1.0397 0.2130 1.0225 11.00000 0.05 0.41 Q11 1 0.8402 1.1951 1.0374 11.00000 0.05 0.41 Q12 1 0.4398 0.5028 0.5738 11.00000 0.05 0.40 Q13 1 0.6408 0.9814 0.7451 11.00000 0.05 0.39 Q14 1 0.4614 0.4406 0.6599 11.00000 0.05 0.35 Q15 1 0.4619 0.7084 0.6101 11.00000 0.05 0.34 Q16 1 0.3112 0.4229 0.3586 11.00000 0.05 0.34 Q17 1 0.6565 0.9562 0.8403 11.00000 0.05 0.32 Q18 1 0.5012 0.8974 0.6002 11.00000 0.05 0.30 Q19 1 0.5157 0.5367 0.6222 11.00000 0.05 0.30 ; _shelx_res_checksum 6970 _shelx_fab_file ; -37 1 15 -0.2589 -0.0434 -37 1 16 0.5005 -0.3459 -37 1 17 -0.2979 -0.0037 -36 0 12 -1.6582 0.0634 -36 0 14 0.0813 -0.0538 -36 0 16 -1.5950 0.5091 -36 0 18 -2.6954 0.0752 -36 0 20 -0.3670 0.0578 -36 2 12 0.2640 0.0445 -36 2 13 -1.0322 0.2845 -36 2 14 -0.6948 -0.1251 -36 2 15 -0.8367 0.0135 -36 2 16 -1.7640 0.4203 -36 2 17 -0.7193 -0.3168 -36 2 18 1.0393 0.2989 -36 2 19 0.7369 0.0175 -35 1 10 -0.7473 0.0926 -35 1 11 0.3802 -0.0881 -35 1 12 -0.8343 0.4642 -35 1 13 -0.4236 -0.3011 -35 1 14 -1.7589 0.7055 -35 1 15 -0.3389 -0.2364 -35 1 16 -0.0548 0.1961 -35 1 17 2.1322 0.0157 -35 1 18 -0.8956 0.3137 -35 1 19 -0.8881 -0.1673 -35 1 20 0.3665 0.2529 -35 1 21 2.4203 -0.1867 -35 3 11 -0.5005 0.1464 -35 3 12 0.6144 -0.1787 -35 3 13 1.5607 0.1229 -35 3 14 0.8358 0.5703 -35 3 15 1.6512 -0.5170 -35 3 16 1.3890 0.4967 -35 3 17 1.7448 -0.3720 -35 3 18 0.0421 0.2969 -35 3 19 1.1912 -0.4700 -35 3 20 0.7497 0.4833 -34 0 8 0.4012 0.1732 -34 0 10 -0.6254 0.2746 -34 0 12 -0.9760 0.1603 -34 0 14 -0.1527 -0.2642 -34 0 16 1.2943 0.1216 -34 0 18 -0.4262 -0.0887 -34 0 20 2.9177 -0.1741 -34 0 22 0.2978 0.2278 -34 2 8 -0.2027 0.5140 -34 2 9 0.6490 0.1787 -34 2 10 -0.3744 0.3445 -34 2 11 0.9986 -0.4878 -34 2 12 0.3430 0.7175 -34 2 13 1.7535 -0.2775 -34 2 14 2.0544 0.1859 -34 2 15 1.1692 -0.1805 -34 2 16 -0.5899 0.1205 -34 2 17 0.9522 -0.2573 -34 2 18 2.4836 0.1738 -34 2 19 1.0181 0.0094 -34 2 20 -1.2964 0.1606 -34 2 21 0.7787 -0.2578 -34 2 22 0.1812 0.1694 -34 4 10 0.7887 0.0374 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18 4 7 0.7964 0.3625 18 6 0 1.5064 0.0213 18 6 1 -0.5273 -0.1060 18 6 2 -2.7762 0.2747 18 6 3 -0.1422 0.1654 18 6 4 0.4856 0.1301 18 6 5 0.2620 -0.1097 18 6 6 -0.4452 0.0360 18 8 0 -0.6424 -0.0643 18 8 1 1.6186 0.1002 18 8 2 0.3338 0.0640 18 8 3 -0.8169 -0.0792 18 8 4 -0.2295 -0.0391 18 10 0 -0.8162 0.0940 18 10 1 -0.6722 0.0141 19 1 0 2.0433 0.1474 19 1 1 3.4952 0.2225 19 1 2 -1.2449 -0.0232 19 1 3 -1.8312 -0.3901 19 1 4 2.1358 0.1045 19 1 5 2.2947 -0.0547 19 1 6 -0.9354 0.3424 19 1 7 -0.6938 -0.0297 19 3 0 -3.3282 -0.1176 19 3 1 -0.3565 -0.0251 19 3 2 1.9756 0.0886 19 3 3 -0.3946 0.1602 19 3 4 -1.8004 0.0711 19 3 5 0.0071 0.2268 19 3 6 1.0503 0.0385 19 3 7 0.0831 0.2882 19 5 0 0.1158 0.1144 19 5 1 -2.6975 0.1753 19 5 2 -0.5754 -0.0077 19 5 3 0.9158 0.0700 19 5 4 0.5212 -0.1746 19 5 5 -1.6185 0.3190 19 5 6 -0.6166 -0.1249 19 7 0 1.0717 0.1489 19 7 1 1.5776 -0.1444 19 7 2 -0.8280 -0.2629 19 7 3 -0.6010 -0.2690 19 7 4 0.0268 0.0305 19 9 0 -1.0543 -0.0928 19 9 1 0.5010 -0.0157 19 9 2 1.1080 -0.2043 20 0 0 4.4800 0.4064 20 0 2 -1.9831 -0.4245 20 0 4 2.4714 0.1702 20 0 6 -0.3954 0.2083 20 2 0 -1.9991 -0.1771 20 2 1 2.0138 0.0373 20 2 2 0.7877 0.2875 20 2 3 -2.4918 -0.0506 20 2 4 -1.4452 0.3175 20 2 5 1.4968 -0.1407 20 2 6 0.5721 0.1902 20 2 7 -0.9344 0.2149 20 4 0 -1.5505 0.0640 20 4 1 -1.5130 -0.0128 20 4 2 0.9721 0.0112 20 4 3 0.6725 -0.0403 20 4 4 -1.4961 0.0192 20 4 5 -0.9339 -0.0197 20 4 6 0.0322 -0.2334 20 6 0 2.4802 -0.1892 20 6 1 -0.4282 -0.2209 20 6 2 -1.0880 -0.1592 20 6 3 -0.2977 0.2097 20 6 4 0.7714 -0.3273 20 8 0 -0.1998 -0.1025 20 8 1 1.5126 -0.0239 20 8 2 0.5325 0.1995 21 1 0 1.3046 0.0776 21 1 1 1.6063 0.3255 21 1 2 -1.8916 -0.0634 21 1 3 -2.2014 0.1937 21 1 4 1.3641 -0.0182 21 1 5 0.5391 -0.0614 21 1 6 -1.0772 0.1677 21 3 0 -2.2446 0.0591 21 3 1 0.0870 -0.0788 21 3 2 1.4672 0.0244 21 3 3 -0.3256 -0.2353 21 3 4 -1.4593 0.1532 21 3 5 -0.2206 -0.2410 21 5 0 0.4009 -0.0862 21 5 1 -1.4347 -0.0492 21 5 2 -0.2296 -0.0208 21 5 3 1.4927 -0.2817 21 5 4 0.0403 -0.1850 21 7 0 1.3668 0.1827 21 7 1 1.1971 0.1933 21 7 2 0.1959 -0.2636 21 7 3 0.1406 0.0275 21 9 0 -0.9357 0.2246 22 0 0 1.8897 0.2862 22 0 2 -2.3982 -0.0463 22 0 4 0.2563 -0.3114 22 2 0 -1.0299 -0.1537 22 2 1 2.0699 0.0364 22 2 2 0.9665 -0.2098 22 2 3 -1.9747 0.0266 22 2 4 -0.8422 -0.0496 22 2 5 0.7591 -0.0985 22 4 0 -0.8757 -0.0721 22 4 1 -0.5826 -0.0982 22 4 2 1.2674 0.0246 22 4 3 0.6055 -0.3264 22 4 4 -0.4596 0.0846 22 6 0 1.8807 -0.0661 22 6 1 0.3024 -0.0951 22 6 2 -0.7993 0.2329 22 6 3 0.9236 0.2650 22 8 0 -0.5084 -0.1381 23 1 0 1.2967 -0.0255 23 1 1 1.8876 -0.0875 23 1 2 -1.6866 -0.2303 23 1 3 -0.6875 0.3428 23 1 4 1.0418 -0.1205 23 3 0 -1.3948 0.0195 23 3 1 0.4034 0.0723 23 3 2 1.3188 -0.2991 23 3 3 0.1884 0.0463 23 3 4 -0.2403 -0.0385 23 5 0 0.2980 0.1234 23 5 1 -1.0960 0.0802 23 5 2 0.7769 0.3331 23 5 3 0.9018 0.0495 23 7 0 -0.1183 0.2170 23 7 1 0.3435 0.1675 24 0 0 2.1129 -0.0251 24 0 2 -0.4434 0.5434 24 0 4 0.8528 -0.3284 24 2 0 -0.7963 -0.0483 24 2 1 2.0324 0.0012 24 2 2 0.8568 -0.2347 24 2 3 -0.9936 0.0028 24 4 0 -0.8374 -0.0743 24 4 1 0.1689 0.3475 24 4 2 0.8305 0.0281 24 6 0 0.9524 0.0729 24 6 1 -1.3442 -0.2344 25 1 0 1.6840 0.2113 25 1 1 0.7441 -0.6366 25 1 2 -1.0504 0.0061 25 1 3 -0.6248 0.5255 25 3 0 -0.8478 0.2264 25 3 1 0.0760 0.1192 25 3 2 0.9278 -0.0728 25 5 0 -1.3145 -0.1020 25 5 1 -1.0668 0.0743 26 0 0 0.7005 -0.6887 26 0 2 -0.3881 0.6780 26 2 0 -0.4487 0.3343 26 2 1 1.3000 -0.0237 26 4 0 -0.8022 -0.0541 27 1 0 0.9838 0.1612 27 1 1 0.4991 -0.5928 27 3 0 -1.2087 0.3587 28 0 0 0.3853 -0.9321 0 0 0 0.0 0.0 ; _shelx_fab_checksum 26398 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 Sm1 Sm 0.42354(2) 0.55145(2) 0.48986(2) 0.02586(7) Uani 1 1 d D . . . . Co1 Co 0.63846(2) 0.97487(4) 0.78701(3) 0.02676(12) Uani 1 1 d . . . . . O3 O 0.60375(12) 0.5444(2) 0.63528(16) 0.0365(6) Uani 1 1 d . . . . . O8 O 0.34165(11) 0.6693(2) 0.38245(18) 0.0349(6) Uani 1 1 d G . . . . H8A H 0.345315 0.737026 0.369671 0.052 Uiso 1 1 d DG U . . . H8B H 0.312394 0.674420 0.377092 0.052 Uiso 1 1 d DG U . . . O4 O 0.52037(12) 0.5820(3) 0.5996(2) 0.0510(9) Uani 1 1 d . . . . . O2 O 0.96503(11) 0.1390(2) 1.03424(18) 0.0363(6) Uani 1 1 d . . . . . O1 O 1.04829(11) 0.1754(3) 1.06910(19) 0.0428(7) Uani 1 1 d . . . . . O10 O 0.33853(18) 0.4382(3) 0.4286(3) 0.0463(9) Uani 1 1 d . . . . . N7 N 0.93570(12) 0.3622(3) 1.01248(18) 0.0254(6) Uani 1 1 d . . . . . O7 O 0.43158(13) 0.7391(3) 0.5520(2) 0.0542(9) Uani 1 1 d G . . . . H7A H 0.460620 0.782441 0.577049 0.081 Uiso 1 1 d DG U . . . H7B H 0.419591 0.750639 0.577811 0.081 Uiso 1 1 d DG U . . . N8 N 0.65453(13) 0.4992(3) 0.7966(2) 0.0309(7) Uani 1 1 d . . . . . O6 O 0.500000 1.3561(4) 0.750000 0.0507(12) Uani 1 2 d GS T P . . H6 H 0.524157 1.310324 0.756808 0.076 Uiso 0.5 1 d G U P . . C3 C 0.64383(15) 1.0659(3) 0.7174(2) 0.0250(8) Uani 1 1 d . . . . . O9 O 0.26809(15) 0.4020(3) 0.2657(3) 0.0552(9) Uani 1 1 d . . . . . N5 N 0.64770(13) 1.1205(3) 0.6761(2) 0.0337(7) Uani 1 1 d . . . . . N1 N 0.52915(17) 0.8710(3) 0.6331(2) 0.0443(9) Uani 1 1 d . . . . . C11 C 0.76540(16) 0.4329(3) 0.8933(2) 0.0258(8) Uani 1 1 d . . . . . C20 C 1.00269(16) 0.2044(3) 1.0506(2) 0.0297(8) Uani 1 1 d . . . . . C7 C 0.57172(16) 0.5559(3) 0.6506(3) 0.0359(10) Uani 1 1 d . . . . . O11 O 0.42866(18) 0.5066(4) 0.6059(2) 0.0729(11) Uani 1 1 d . . . . . H11A H 0.427664 0.429568 0.611274 0.109 Uiso 1 1 d R U . . . H11B H 0.398094 0.531292 0.597085 0.109 Uiso 1 1 d R U . . . C17 C 0.89455(15) 0.3379(3) 0.9310(2) 0.0281(8) Uani 1 1 d . . . . . H17 H 0.903702 0.306647 0.900534 0.034 Uiso 1 1 calc R U . . . C6 C 0.6327(2) 0.8773(4) 0.8542(3) 0.0397(10) Uani 1 1 d . . . . . O5 O 0.84887(17) 1.1509(3) 1.0847(3) 0.0681(11) Uani 1 1 d G . . . . H5A H 0.862090 1.214728 1.112008 0.102 Uiso 1 1 d G U . . . H5B H 0.824232 1.165794 1.032900 0.102 Uiso 1 1 d G U . . . C14 C 0.82518(15) 0.4047(3) 0.9373(2) 0.0250(8) Uani 1 1 d . . . . . C13 C 0.66732(17) 0.3974(3) 0.7807(3) 0.0339(9) Uani 1 1 d . . . . . H13 H 0.638705 0.350099 0.737146 0.041 Uiso 1 1 calc R U . . . C2 C 0.59513(17) 1.0968(4) 0.7805(2) 0.0332(9) Uani 1 1 d . . . . . C19 C 0.99402(15) 0.3355(3) 1.0500(2) 0.0298(8) Uani 1 1 d . . . . . H19A H 1.019746 0.365038 1.106718 0.036 Uiso 1 1 calc R U . . . H19B H 1.002522 0.374656 1.018554 0.036 Uiso 1 1 calc R U . . . C10 C 0.75060(17) 0.5341(3) 0.9116(2) 0.0330(9) Uani 1 1 d . . . . . H10 H 0.778275 0.580435 0.956945 0.040 Uiso 1 1 calc R U . . . C18 C 0.83932(15) 0.3589(3) 0.8927(2) 0.0268(8) Uani 1 1 d . . . . . H18 H 0.811189 0.342094 0.836251 0.032 Uiso 1 1 calc R U . . . C1 C 0.57153(18) 0.9068(3) 0.6914(2) 0.0318(9) Uani 1 1 d . . . . . N6 N 0.57055(18) 1.1764(4) 0.7754(3) 0.0531(10) Uani 1 1 d . . . . . N2 N 0.6289(2) 0.8166(3) 0.8936(3) 0.0542(11) Uani 1 1 d . . . . . C8 C 0.59506(17) 0.5376(4) 0.7398(3) 0.0390(10) Uani 1 1 d . . . . . H8C H 0.592048 0.610418 0.760376 0.047 Uiso 1 1 calc R U . . . H8D H 0.572438 0.479128 0.739608 0.047 Uiso 1 1 calc R U . . . C12 C 0.72234(16) 0.3627(3) 0.8283(2) 0.0295(8) Uani 1 1 d . . . . . H12 H 0.730942 0.291816 0.817149 0.035 Uiso 1 1 calc R U . . . C9 C 0.69475(17) 0.5655(4) 0.8622(2) 0.0338(9) Uani 1 1 d . . . . . H9 H 0.684762 0.633200 0.874416 0.041 Uiso 1 1 calc R U . . . C5 C 0.6867(2) 0.8626(4) 0.7958(2) 0.0394(10) Uani 1 1 d . . . . . N3 N 0.71825(19) 0.7977(4) 0.8029(3) 0.0569(11) Uani 1 1 d . . . . . C4 C 0.7032(2) 1.0513(4) 0.8820(3) 0.0448(11) Uani 1 1 d . . . . . C16 C 0.92326(17) 0.4034(4) 1.0579(2) 0.0369(10) Uani 1 1 d . . . . . H16 H 0.952043 0.416940 1.114661 0.044 Uiso 1 1 calc R U . . . C15 C 0.86829(17) 0.4260(4) 1.0217(2) 0.0389(10) Uani 1 1 d . . . . . H15 H 0.860059 0.455527 1.053714 0.047 Uiso 1 1 calc R U . . . N4 N 0.7423(2) 1.1014(5) 0.9388(3) 0.0769(15) Uani 1 1 d . . . . . H10A H 0.350(2) 0.449(4) 0.466(3) 0.015(15) Uiso 1 1 d . . . . . H10B H 0.325(5) 0.396(11) 0.440(8) 0.22(6) Uiso 1 1 d . . . . . H9A H 0.2765(16) 0.391(3) 0.308(2) 0.010(11) Uiso 1 1 d . . . . . H9B H 0.232(3) 0.401(6) 0.240(4) 0.08(2) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02337(11) 0.01952(11) 0.02675(11) -0.00402(7) 0.01282(9) -0.00127(7) Co1 0.0370(3) 0.0231(3) 0.0259(3) -0.00173(19) 0.0230(2) 0.0000(2) O3 0.0313(15) 0.0410(16) 0.0288(14) -0.0039(12) 0.0159(13) 0.0044(12) O8 0.0253(14) 0.0302(15) 0.0449(16) 0.0074(12) 0.0209(13) 0.0024(11) O4 0.0235(15) 0.0456(18) 0.0491(18) -0.0203(15) 0.0084(14) 0.0050(13) O2 0.0333(15) 0.0245(14) 0.0522(17) -0.0023(12) 0.0283(14) -0.0025(12) O1 0.0292(15) 0.0348(16) 0.0586(19) -0.0104(14) 0.0260(15) -0.0014(12) O10 0.046(2) 0.041(2) 0.064(3) -0.0015(19) 0.041(2) -0.0070(16) N7 0.0255(16) 0.0217(15) 0.0242(15) -0.0001(12) 0.0141(14) 0.0002(12) O7 0.0333(17) 0.0443(19) 0.077(2) -0.0341(17) 0.0323(17) -0.0102(14) N8 0.0267(16) 0.0341(18) 0.0322(17) 0.0027(14) 0.0194(15) 0.0050(14) O6 0.045(3) 0.028(2) 0.074(3) 0.000 0.036(3) 0.000 C3 0.0217(18) 0.0232(18) 0.0262(18) -0.0007(15) 0.0138(16) 0.0006(14) O9 0.0300(19) 0.063(2) 0.058(3) -0.008(2) 0.0222(19) -0.0026(16) N5 0.0275(17) 0.0335(18) 0.0362(18) 0.0071(15) 0.0190(16) 0.0013(14) N1 0.057(2) 0.041(2) 0.044(2) -0.0126(17) 0.037(2) -0.0183(19) C11 0.0317(19) 0.0260(18) 0.0220(17) 0.0029(14) 0.0185(16) 0.0040(15) C20 0.027(2) 0.0253(19) 0.031(2) -0.0032(15) 0.0166(17) -0.0016(16) C7 0.026(2) 0.026(2) 0.035(2) -0.0095(16) 0.0108(19) 0.0027(16) O11 0.088(3) 0.090(3) 0.063(2) 0.005(2) 0.059(2) 0.023(2) C17 0.032(2) 0.035(2) 0.0243(18) -0.0012(16) 0.0209(17) 0.0005(16) C6 0.063(3) 0.032(2) 0.036(2) -0.0048(18) 0.038(2) -0.001(2) O5 0.068(3) 0.051(2) 0.088(3) -0.025(2) 0.052(2) -0.0119(19) C14 0.0309(19) 0.0192(17) 0.0230(18) 0.0013(14) 0.0167(16) 0.0032(15) C13 0.034(2) 0.031(2) 0.037(2) -0.0043(17) 0.0231(19) -0.0054(17) C2 0.038(2) 0.035(2) 0.034(2) -0.0093(17) 0.0265(19) -0.0050(18) C19 0.0267(19) 0.027(2) 0.032(2) -0.0014(16) 0.0179(17) -0.0021(15) C10 0.033(2) 0.034(2) 0.0255(19) -0.0024(16) 0.0163(18) 0.0061(17) C18 0.0287(19) 0.031(2) 0.0183(17) 0.0007(15) 0.0144(16) 0.0000(15) C1 0.050(3) 0.0234(19) 0.033(2) -0.0078(16) 0.032(2) -0.0102(18) N6 0.058(3) 0.052(2) 0.058(3) -0.009(2) 0.042(2) 0.009(2) N2 0.094(3) 0.042(2) 0.051(2) -0.0024(19) 0.058(3) -0.007(2) C8 0.030(2) 0.047(3) 0.044(2) -0.0021(19) 0.026(2) 0.0038(18) C12 0.032(2) 0.0240(19) 0.033(2) 0.0003(16) 0.0219(18) 0.0017(16) C9 0.037(2) 0.033(2) 0.030(2) -0.0010(17) 0.0217(19) 0.0066(17) C5 0.057(3) 0.039(2) 0.031(2) 0.0114(18) 0.032(2) 0.013(2) N3 0.075(3) 0.058(3) 0.053(2) 0.023(2) 0.048(2) 0.030(2) C4 0.054(3) 0.050(3) 0.036(2) 0.005(2) 0.032(2) 0.003(2) C16 0.031(2) 0.043(2) 0.0214(18) -0.0075(17) 0.0105(17) 0.0074(18) C15 0.038(2) 0.048(3) 0.0228(19) -0.0063(18) 0.0165(18) 0.0130(19) N4 0.076(3) 0.094(4) 0.030(2) -0.011(2) 0.021(2) -0.031(3) 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' Co Co 0.3494 0.9721 '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' Sm Sm -0.1638 3.4418 '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 O3 Sm1 H10A 86.7(11) 5_666 . ? O8 Sm1 O3 79.91(9) . 5_666 ? O8 Sm1 H10A 77.7(12) . . ? O4 Sm1 O3 116.84(10) . 5_666 ? O4 Sm1 O8 137.21(10) . . ? O4 Sm1 O2 74.11(10) . 8_455 ? O4 Sm1 O1 75.64(12) . 4_656 ? O4 Sm1 O10 149.57(14) . . ? O4 Sm1 O7 73.95(10) . . ? O4 Sm1 O11 80.69(14) . . ? O4 Sm1 H10A 138.1(11) . . ? O2 Sm1 O3 74.64(10) 8_455 5_666 ? O2 Sm1 O8 147.14(9) 8_455 . ? O2 Sm1 O1 116.79(10) 8_455 4_656 ? O2 Sm1 O10 81.47(11) 8_455 . ? O2 Sm1 O7 138.49(12) 8_455 . ? O2 Sm1 O11 75.40(12) 8_455 . ? O2 Sm1 H10A 80.4(12) 8_455 . ? O1 Sm1 O3 71.91(10) 4_656 5_666 ? O1 Sm1 O8 73.15(9) 4_656 . ? O1 Sm1 O10 132.83(13) 4_656 . ? O1 Sm1 O7 79.55(12) 4_656 . ? O1 Sm1 O11 148.35(14) 4_656 . ? O1 Sm1 H10A 146.2(11) 4_656 . ? O10 Sm1 O3 72.36(13) . 5_666 ? O10 Sm1 O8 71.14(11) . . ? O10 Sm1 O7 116.47(12) . . ? O10 Sm1 H10A 15.1(11) . . ? O7 Sm1 O3 144.74(12) . 5_666 ? O7 Sm1 O8 72.21(11) . . ? O7 Sm1 H10A 107.4(11) . . ? O11 Sm1 O3 138.76(13) . 5_666 ? O11 Sm1 O8 113.45(12) . . ? O11 Sm1 O10 75.72(16) . . ? O11 Sm1 O7 73.88(14) . . ? O11 Sm1 H10A 60.8(11) . . ? C3 Co1 C6 177.40(16) . . ? C2 Co1 C3 87.81(16) . . ? C2 Co1 C6 94.21(18) . . ? C2 Co1 C1 88.96(17) . . ? C2 Co1 C5 174.89(19) . . ? C2 Co1 C4 87.70(19) . . ? C1 Co1 C3 89.54(15) . . ? C1 Co1 C6 88.85(18) . . ? C1 Co1 C5 94.84(19) . . ? C1 Co1 C4 176.61(19) . . ? C5 Co1 C3 88.81(16) . . ? C5 Co1 C6 89.28(18) . . ? C5 Co1 C4 88.5(2) . . ? C4 Co1 C3 89.74(17) . . ? C4 Co1 C6 91.99(19) . . ? C7 O3 Sm1 123.8(2) . 5_666 ? Sm1 O8 H8A 121.3 . . ? Sm1 O8 H8B 123.4 . . ? H8A O8 H8B 104.6 . . ? C7 O4 Sm1 156.6(3) . . ? C20 O2 Sm1 146.4(3) . 8_556 ? C20 O1 Sm1 136.2(3) . 4_646 ? Sm1 O10 H10A 73(5) . . ? Sm1 O10 H10B 143(10) . . ? H10A O10 H10B 73(10) . . ? C17 N7 C19 117.6(3) . . ? C16 N7 C17 120.6(3) . . ? C16 N7 C19 121.7(3) . . ? Sm1 O7 H7A 122.6 . . ? Sm1 O7 H7B 123.2 . . ? H7A O7 H7B 104.5 . . ? C13 N8 C8 118.4(3) . . ? C13 N8 C9 121.0(3) . . ? C9 N8 C8 120.6(3) . . ? H6 O6 H6 104.2 . 2_656 ? N5 C3 Co1 179.2(3) . . ? H9A O9 H9B 93(5) . . ? C10 C11 C14 121.2(3) . . ? C12 C11 C14 120.7(3) . . ? C12 C11 C10 118.0(3) . . ? O2 C20 O1 127.7(4) . . ? O2 C20 C19 117.3(3) . . ? O1 C20 C19 115.0(3) . . ? O3 C7 O4 126.7(4) . . ? O3 C7 C8 119.2(3) . . ? O4 C7 C8 114.1(4) . . ? Sm1 O11 H11A 110.9 . . ? Sm1 O11 H11B 111.7 . . ? H11A O11 H11B 102.5 . . ? N7 C17 H17 119.7 . . ? N7 C17 C18 120.5(3) . . ? C18 C17 H17 119.7 . . ? N2 C6 Co1 178.6(4) . . ? H5A O5 H5B 109.5 . . ? C18 C14 C11 119.2(3) . . ? C18 C14 C15 118.0(3) . . ? C15 C14 C11 122.8(3) . . ? N8 C13 H13 119.9 . . ? N8 C13 C12 120.2(4) . . ? C12 C13 H13 119.9 . . ? N6 C2 Co1 175.2(4) . . ? N7 C19 C20 111.1(3) . . ? N7 C19 H19A 109.4 . . ? N7 C19 H19B 109.4 . . ? C20 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C11 C10 H10 120.2 . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C17 C18 C14 120.3(3) . . ? C17 C18 H18 119.9 . . ? C14 C18 H18 119.9 . . ? N1 C1 Co1 176.0(4) . . ? N8 C8 C7 112.3(3) . . ? N8 C8 H8C 109.1 . . ? N8 C8 H8D 109.1 . . ? C7 C8 H8C 109.1 . . ? C7 C8 H8D 109.1 . . ? H8C C8 H8D 107.9 . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H12 119.8 . . ? N8 C9 C10 120.6(4) . . ? N8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? N3 C5 Co1 176.8(4) . . ? N4 C4 Co1 177.9(5) . . ? N7 C16 H16 119.7 . . ? N7 C16 C15 120.6(3) . . ? C15 C16 H16 119.7 . . ? C14 C15 H15 120.0 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H15 120.0 . . ? 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 Sm1 O3 2.444(3) 5_666 ? Sm1 O8 2.437(3) . ? Sm1 O4 2.349(3) . ? Sm1 O2 2.386(3) 8_455 ? Sm1 O1 2.399(3) 4_656 ? Sm1 O10 2.434(4) . ? Sm1 O7 2.437(3) . ? Sm1 O11 2.405(4) . ? Sm1 H10A 2.33(5) . ? Co1 C3 1.895(4) . ? Co1 C6 1.902(4) . ? Co1 C2 1.883(4) . ? Co1 C1 1.885(4) . ? Co1 C5 1.893(4) . ? Co1 C4 1.895(5) . ? O3 C7 1.245(5) . ? O8 H8A 0.8503 . ? O8 H8B 0.8475 . ? O4 C7 1.254(5) . ? O2 C20 1.238(5) . ? O1 C20 1.252(5) . ? O10 H10A 0.63(4) . ? O10 H10B 0.79(13) . ? N7 C17 1.344(5) . ? N7 C19 1.471(5) . ? N7 C16 1.334(5) . ? O7 H7A 0.8499 . ? O7 H7B 0.8488 . ? N8 C13 1.340(5) . ? N8 C8 1.477(5) . ? N8 C9 1.343(5) . ? O6 H6 0.85(11) 2_656 ? O6 H6 0.8499 . ? C3 N5 1.141(5) . ? O9 H9A 0.76(4) . ? O9 H9B 0.87(7) . ? N1 C1 1.146(5) . ? C11 C14 1.482(5) . ? C11 C10 1.390(5) . ? C11 C12 1.388(5) . ? C20 C19 1.518(5) . ? C7 C8 1.527(6) . ? O11 H11A 0.8893 . ? O11 H11B 0.8919 . ? C17 H17 0.9300 . ? C17 C18 1.368(5) . ? C6 N2 1.147(5) . ? O5 H5A 0.8501 . ? O5 H5B 0.8499 . ? C14 C18 1.379(5) . ? C14 C15 1.386(5) . ? C13 H13 0.9300 . ? C13 C12 1.368(5) . ? C2 N6 1.148(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C10 H10 0.9300 . ? C10 C9 1.375(6) . ? C18 H18 0.9300 . ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? C12 H12 0.9300 . ? C9 H9 0.9300 . ? C5 N3 1.162(6) . ? C4 N4 1.161(6) . ? C16 H16 0.9300 . ? C16 C15 1.376(6) . ? C15 H15 0.9300 . ? 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 Sm1 O3 C7 O4 -40.7(6) 5_666 . . . ? Sm1 O3 C7 C8 139.4(3) 5_666 . . . ? Sm1 O4 C7 O3 74.8(10) . . . . ? Sm1 O4 C7 C8 -105.4(8) . . . . ? Sm1 O2 C20 O1 -21.0(8) 8_556 . . . ? Sm1 O2 C20 C19 160.2(3) 8_556 . . . ? Sm1 O1 C20 O2 52.2(6) 4_646 . . . ? Sm1 O1 C20 C19 -129.0(3) 4_646 . . . ? O3 C7 C8 N8 -4.0(5) . . . . ? O4 C7 C8 N8 176.1(3) . . . . ? O2 C20 C19 N7 -11.9(5) . . . . ? O1 C20 C19 N7 169.2(3) . . . . ? N7 C17 C18 C14 -0.3(6) . . . . ? N7 C16 C15 C14 0.7(7) . . . . ? N8 C13 C12 C11 -0.3(6) . . . . ? C11 C14 C18 C17 176.6(3) . . . . ? C11 C14 C15 C16 -176.7(4) . . . . ? C11 C10 C9 N8 0.0(6) . . . . ? C17 N7 C19 C20 -65.5(4) . . . . ? C17 N7 C16 C15 -2.5(6) . . . . ? C14 C11 C10 C9 171.4(4) . . . . ? C14 C11 C12 C13 -171.3(3) . . . . ? C13 N8 C8 C7 -61.2(5) . . . . ? C13 N8 C9 C10 4.2(6) . . . . ? C19 N7 C17 C18 178.9(3) . . . . ? C19 N7 C16 C15 -179.0(4) . . . . ? C10 C11 C14 C18 -139.3(4) . . . . ? C10 C11 C14 C15 38.5(6) . . . . ? C10 C11 C12 C13 4.3(6) . . . . ? C18 C14 C15 C16 1.2(6) . . . . ? C8 N8 C13 C12 175.3(4) . . . . ? C8 N8 C9 C10 -175.2(4) . . . . ? C12 C11 C14 C18 36.1(5) . . . . ? C12 C11 C14 C15 -146.0(4) . . . . ? C12 C11 C10 C9 -4.2(6) . . . . ? C9 N8 C13 C12 -4.1(6) . . . . ? C9 N8 C8 C7 118.2(4) . . . . ? C16 N7 C17 C18 2.3(6) . . . . ? C16 N7 C19 C20 111.1(4) . . . . ? C15 C14 C18 C17 -1.4(6) . . . . ? 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 0.000 0.292 0.750 49.2 8.7 ? 2 0.000 0.708 0.250 49.2 8.6 ? 3 0.250 0.250 0.000 42.6 3.4 ? 4 0.250 0.750 0.500 42.6 3.4 ? 5 0.500 0.208 0.250 49.2 8.6 ? 6 0.500 0.792 0.750 49.2 8.7 ? 7 0.750 0.250 0.500 42.6 3.4 ? 8 0.750 0.750 0.000 42.6 3.4 ?