#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:32:58 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257502 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705343.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_7705343 loop_ _publ_author_name 'Jarrah, Najmeh' 'Troyano, Javier' 'Carn\'e-S\'anchez, Arnau' 'Imaz, Inhar' 'Tangestaninejad, Shahram' 'Moghadam, Majid' 'Maspoch, Daniel' _publ_section_title ; Dynamic porous coordination polymers built-up from flexible 4,4'-dithiodibenzoate and rigid N-based ligands. ; _journal_issue 37 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 13142 _journal_page_last 13151 _journal_paper_doi 10.1039/d0dt02411b _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C19 H12 Cu N O4 S2, C3 H7 N O' _chemical_formula_sum 'C22 H19 Cu N2 O5 S2' _chemical_formula_weight 519.05 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2020-08-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-25 deposited with the CCDC. 2020-09-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 111.435(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.3747(7) _cell_length_b 13.9313(3) _cell_length_c 18.9465(7) _cell_measurement_reflns_used 18962 _cell_measurement_temperature 293 _cell_measurement_theta_max 31.2490 _cell_measurement_theta_min 1.8440 _cell_volume 5988.7(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _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 293 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.910 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -93.00 -64.00 0.50 67.87 -- -13.20 45.00 90.00 58 2 \w -50.00 54.00 0.50 67.87 -- -13.20 45.00 90.00 208 3 \w -102.00 -76.00 0.50 67.87 -- -13.20 45.00 30.00 52 4 \w -52.00 -4.00 0.50 67.87 -- -13.20 45.00 30.00 96 5 \w 26.00 52.00 0.50 67.87 -- -13.20 45.00 30.00 52 6 \w -102.00 76.00 0.50 67.87 -- -13.20 45.00 120.00 356 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC10 (RCD3): fixed-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0005458000 _diffrn_orient_matrix_UB_12 0.0444335000 _diffrn_orient_matrix_UB_13 -0.0180109000 _diffrn_orient_matrix_UB_21 0.0163800000 _diffrn_orient_matrix_UB_22 -0.0216201000 _diffrn_orient_matrix_UB_23 -0.0199598000 _diffrn_orient_matrix_UB_31 -0.0266208000 _diffrn_orient_matrix_UB_32 -0.0121940000 _diffrn_orient_matrix_UB_33 -0.0299443000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_unetI/netI 0.0319 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.910 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 35763 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.910 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.425 _diffrn_reflns_theta_min 1.876 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.52382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark blue' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.151 _exptl_crystal_description prism _exptl_crystal_F_000 2128 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.573 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.134 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 9031 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0618 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+30.9259P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1754 _refine_ls_wR_factor_ref 0.1834 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7169 _reflns_number_total 9031 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02411b2.cif _cod_data_source_block najh80c _cod_depositor_comments 'Adding full bibliography for 7705341--7705344.cif.' _cod_database_code 7705343 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula 'Cu S2 C18 H12 O4 N' _chemical_oxdiff_usercomment -173 _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 0.982 _shelx_estimated_absorpt_t_min 0.877 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 29.07 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints O1S, C2S with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints Uanis(O1S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 4.a Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16), C17(H17), C22(H22), C23(H23), C26(H26), C27(H27), C2S(H2S) 4.b Idealised Me refined as rotating group: C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC) ; _shelx_res_file ; TITL najh80c_a.res in C2/c najh80c.res created by SHELXL-2018/1 at 15:44:16 on 24-Aug-2020 REM Old TITL NAJH80C in C2/c REM SHELXT solution in C2/c REM R1 0.171, Rweak 0.006, Alpha 0.040, Orientation as input REM Formula found by SHELXT: C45 N4 O9 S4 Cu2 CELL 0.71073 24.3747 13.9313 18.9465 90 111.435 90 ZERR 8 0.0007 0.0003 0.0007 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cu N O S UNIT 176 152 8 16 40 16 DELU O1S C2S ISOR O1S L.S. 20 PLAN 20 SIZE 0.02 0.02 0.15 TEMP -173.15 BOND $H list 4 ABIN fmap 2 53 acta OMIT 1 1 3 REM REM REM WGHT 0.090200 30.925900 FVAR 0.11771 CU01 3 0.500000 0.059483 0.250000 10.50000 0.01467 0.00716 = 0.03103 0.00000 0.01252 0.00000 CU02 3 0.500000 0.247755 0.250000 10.50000 0.01549 0.00687 = 0.03419 0.00000 0.01423 0.00000 S10 6 0.155510 0.205133 0.266331 11.00000 0.01897 0.02896 = 0.04539 0.01230 0.02067 0.00596 S11 6 0.627483 0.159539 0.734260 11.00000 0.01876 0.02619 = 0.03539 -0.00383 0.01522 -0.00592 O1 5 0.415346 0.236316 0.224437 11.00000 0.01697 0.01483 = 0.05508 0.00452 0.01798 0.00155 O2 5 0.418691 0.079930 0.252876 11.00000 0.01727 0.01316 = 0.04089 0.00123 0.01542 0.00163 O19 5 0.532442 0.071981 0.360499 11.00000 0.02415 0.01078 = 0.03446 -0.00076 0.01337 0.00009 O20 5 0.512526 0.229455 0.357536 11.00000 0.03364 0.01294 = 0.03632 0.00181 0.01635 0.00072 N21 4 0.500000 0.400424 0.250000 10.50000 0.02342 0.00804 = 0.03239 0.00000 0.01593 0.00000 N28 4 0.500000 0.906102 0.250000 10.50000 0.01219 0.01204 = 0.03085 0.00000 0.01369 0.00000 C3 1 0.393369 0.160325 0.238750 11.00000 0.01473 0.01485 = 0.03815 -0.00204 0.01383 0.00147 C4 1 0.332575 0.169599 0.240159 11.00000 0.01438 0.01862 = 0.03744 0.00082 0.01398 0.00075 C5 1 0.305451 0.094167 0.261550 11.00000 0.01774 0.01639 = 0.04211 0.00419 0.01471 0.00284 AFIX 43 H5 2 0.324106 0.033147 0.271723 11.00000 -1.20000 AFIX 0 C6 1 0.251288 0.106676 0.268309 11.00000 0.02013 0.02028 = 0.04212 0.00836 0.01546 0.00124 AFIX 43 H6 2 0.233037 0.054629 0.283642 11.00000 -1.20000 AFIX 0 C7 1 0.223816 0.195102 0.252689 11.00000 0.01751 0.02383 = 0.03470 0.00463 0.01328 0.00326 C8 1 0.249122 0.271089 0.227592 11.00000 0.02526 0.02108 = 0.06435 0.01144 0.02740 0.00702 AFIX 43 H8 2 0.229363 0.330993 0.214553 11.00000 -1.20000 AFIX 0 C9 1 0.303801 0.257411 0.222048 11.00000 0.02358 0.01979 = 0.06457 0.01082 0.02704 0.00387 AFIX 43 H9 2 0.321815 0.308832 0.205633 11.00000 -1.20000 AFIX 0 C12 1 0.597967 0.162849 0.633244 11.00000 0.01875 0.02385 = 0.03255 -0.00285 0.01544 -0.00386 C13 1 0.583920 0.074404 0.597211 11.00000 0.02857 0.01803 = 0.03571 0.00235 0.01153 -0.00261 AFIX 43 H13 2 0.588773 0.017114 0.626060 11.00000 -1.20000 AFIX 0 C14 1 0.562525 0.070696 0.517874 11.00000 0.02818 0.01388 = 0.03705 0.00175 0.01026 -0.00205 AFIX 43 H14 2 0.554748 0.010290 0.492896 11.00000 -1.20000 AFIX 0 C15 1 0.552613 0.154250 0.475540 11.00000 0.02257 0.01326 = 0.03529 -0.00127 0.01546 -0.00110 C16 1 0.564489 0.242755 0.512568 11.00000 0.04803 0.01584 = 0.04072 -0.00200 0.01963 -0.00183 AFIX 43 H16 2 0.556360 0.300473 0.483882 11.00000 -1.20000 AFIX 0 C17 1 0.588097 0.246673 0.591036 11.00000 0.04701 0.01641 = 0.03814 -0.00642 0.01590 -0.00419 AFIX 43 H17 2 0.597545 0.306975 0.615975 11.00000 -1.20000 AFIX 0 C18 1 0.531235 0.151638 0.391435 11.00000 0.02014 0.01340 = 0.03166 -0.00114 0.01261 -0.00087 C22 1 0.545456 0.449786 0.297737 11.00000 0.02310 0.01054 = 0.04099 0.00313 0.01358 0.00187 AFIX 43 H22 2 0.578095 0.415222 0.331535 11.00000 -1.20000 AFIX 0 C23 1 0.547046 0.549204 0.300074 11.00000 0.02154 0.01170 = 0.03502 -0.00196 0.00898 0.00034 AFIX 43 H23 2 0.579748 0.582127 0.335311 11.00000 -1.20000 AFIX 0 C24 1 0.500000 0.599324 0.250000 10.50000 0.02802 0.00333 = 0.03211 0.00000 0.01648 0.00000 C25 1 0.500000 0.705984 0.250000 10.50000 0.01501 0.01028 = 0.03033 0.00000 0.01389 0.00000 C26 1 0.524062 0.757834 0.316965 11.00000 0.02418 0.00965 = 0.03038 0.00131 0.01336 0.00017 AFIX 43 H26 2 0.541337 0.725291 0.363992 11.00000 -1.20000 AFIX 0 C27 1 0.522713 0.857782 0.314755 11.00000 0.01871 0.00982 = 0.02971 -0.00151 0.01117 0.00008 AFIX 43 H27 2 0.538517 0.892517 0.360962 11.00000 -1.20000 AFIX 0 O1S 5 0.566676 0.525533 0.008352 11.00000 0.80902 0.09278 = 0.29633 -0.01059 0.19673 -0.00736 N3S 4 0.589689 0.391952 0.072086 11.00000 0.08200 0.12129 = 0.06212 0.03303 0.03718 0.03376 C2S 1 0.573361 0.442102 0.009225 11.00000 0.13519 0.09700 = 0.08784 0.01930 0.03107 0.02608 AFIX 43 H2S 2 0.566703 0.409703 -0.037299 11.00000 -1.20000 AFIX 0 C4S 1 0.587040 0.425790 0.139238 11.00000 0.17131 0.11846 = 0.11341 0.04579 0.10985 0.06577 AFIX 137 H4SA 2 0.576747 0.373021 0.166305 11.00000 -1.50000 H4SB 2 0.557021 0.476179 0.128343 11.00000 -1.50000 H4SC 2 0.625470 0.452193 0.170743 11.00000 -1.50000 AFIX 0 C5S 1 0.600514 0.292300 0.063009 11.00000 0.05876 0.12304 = 0.18873 -0.01318 0.02471 -0.00474 AFIX 137 H5SA 2 0.566222 0.254361 0.061408 11.00000 -1.50000 H5SB 2 0.635288 0.271127 0.105797 11.00000 -1.50000 H5SC 2 0.607425 0.283364 0.015624 11.00000 -1.50000 AFIX 0 HKLF 4 REM najh80c_a.res in C2/c REM R1 = 0.0618 for 7169 Fo > 4sig(Fo) and 0.0747 for all 9031 data REM 294 parameters refined using 7 restraints END WGHT 0.0902 30.9048 REM Highest difference peak 1.573, deepest hole -0.824, 1-sigma level 0.134 Q1 1 0.6191 0.2955 -0.0025 11.00000 0.05 1.57 Q2 1 0.6020 0.2328 -0.0015 11.00000 0.05 1.56 Q3 1 0.5172 0.2618 0.2992 11.00000 0.05 1.12 Q4 1 0.5997 0.2437 0.5531 11.00000 0.05 1.05 Q5 1 0.4815 0.0713 0.2015 11.00000 0.05 1.00 Q6 1 0.1788 0.2144 0.3201 11.00000 0.05 0.94 Q7 1 0.5832 0.2958 0.5206 11.00000 0.05 0.76 Q8 1 0.6160 0.1726 0.6832 11.00000 0.05 0.76 Q9 1 0.5969 0.0608 0.5593 11.00000 0.05 0.72 Q10 1 0.5206 0.4241 -0.0345 11.00000 0.05 0.67 Q11 1 0.6475 0.1591 0.7761 11.00000 0.05 0.66 Q12 1 0.4370 0.2404 0.2780 11.00000 0.05 0.63 Q13 1 0.5848 0.0986 0.5232 11.00000 0.05 0.62 Q14 1 0.5426 0.2352 0.3546 11.00000 0.05 0.59 Q15 1 0.6017 0.4659 0.0726 11.00000 0.05 0.56 Q16 1 0.5471 0.1597 0.4356 11.00000 0.05 0.54 Q17 1 0.3191 0.2610 0.2810 11.00000 0.05 0.50 Q18 1 0.1400 0.1874 0.2230 11.00000 0.05 0.50 Q19 1 0.5636 0.2077 0.4936 11.00000 0.05 0.46 Q20 1 0.5609 0.1166 0.4946 11.00000 0.05 0.43 ; _shelx_res_checksum 83618 _shelx_fab_file ; -35 1 13 4.0179 -0.2664 -35 1 14 -3.3107 -0.5044 -34 0 14 0.3720 0.2475 -34 0 16 -1.2497 -1.1011 -34 2 5 -1.4331 0.2661 -34 2 6 -1.9080 0.1361 -34 2 7 -1.7021 -0.1033 -34 2 8 -0.8771 -0.2356 -34 2 9 1.7198 0.0524 -34 2 10 1.1198 0.0762 -34 2 11 -1.9758 0.0235 -34 2 12 3.0796 -0.0134 -34 2 13 -3.8122 -0.1257 -34 2 14 -1.5340 -0.1149 -34 2 15 -1.0042 0.1078 -34 4 7 1.8779 -0.0415 -34 4 8 -1.8776 0.3346 -34 4 9 5.9055 -0.1438 -34 4 10 2.7024 -0.3755 -33 1 5 -3.8142 0.2162 -33 1 6 -3.4281 0.1841 -33 1 7 1.2067 -0.2730 -33 1 8 -6.4792 -0.1921 -33 1 9 2.2959 0.2271 -33 1 10 -2.4339 0.0661 -33 1 11 -3.4323 -0.1734 -33 1 12 3.5000 -0.0681 -33 1 13 -5.0067 0.2241 -33 1 14 3.4516 0.4168 -33 1 15 -1.9637 -0.6647 -33 1 16 1.4804 0.2090 -33 1 17 -1.4947 -0.5553 -33 1 18 -0.7819 -0.3846 -33 1 19 -2.4224 0.9386 -33 3 1 1.3856 0.0921 -33 3 2 -3.0838 -0.3703 -33 3 3 0.0894 0.2153 -33 3 4 -0.0926 0.2327 -33 3 5 -4.9505 -0.2336 -33 3 6 1.0321 -0.1359 -33 3 7 -0.2087 0.1762 -33 3 8 1.0070 -0.2242 -33 3 9 4.7802 0.0812 -33 3 10 2.0822 0.2701 -33 3 11 0.7998 -0.2879 -33 3 12 2.3765 -0.4969 -33 3 13 -0.7840 0.1706 -33 3 14 1.2509 0.0327 -33 3 15 1.2107 -0.0002 -33 5 5 0.0588 -0.2141 -33 5 6 -3.5353 -0.0586 -33 5 7 -0.9912 -0.1791 -33 5 8 -5.4162 -0.1686 -33 5 9 -0.5176 0.1005 -33 5 10 -3.8805 0.1597 -33 5 11 -2.2806 0.0026 -32 0 2 0.6228 0.8130 -32 0 4 0.9021 -0.1991 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-0.0622 25 3 3 4.3883 -0.1458 25 3 4 -0.6318 -0.0609 25 3 5 0.0845 0.0819 25 3 6 -1.1811 0.0046 25 3 7 -0.2376 -0.0099 25 3 8 -1.1967 -0.1243 25 3 9 -1.3527 -0.0912 25 3 10 -0.0548 -0.2568 25 5 0 -0.9945 0.0109 25 5 1 -1.4087 -0.0297 25 5 2 -1.2447 0.0156 25 5 3 -0.3530 -0.3325 25 5 4 -0.9166 0.0096 25 5 5 -1.9015 0.2194 25 5 6 -2.8123 0.0106 25 5 7 -4.0218 -0.1211 25 5 8 -0.4323 -0.0459 25 5 9 -2.5311 -1.2258 25 5 10 2.7688 0.0909 25 7 0 0.2456 -0.0871 25 7 1 0.9286 0.1439 25 7 2 -2.2850 0.0758 25 7 3 1.1173 -0.0865 25 7 4 -3.1711 0.0126 25 7 5 0.6243 -0.1354 25 7 6 -3.4370 -0.1398 25 7 7 -2.1660 -0.0088 25 7 8 -1.8286 -0.4860 25 9 0 -0.9977 -0.1271 25 9 1 3.8249 0.1219 25 9 2 0.1126 -0.2052 25 9 3 -0.5702 -0.3656 25 9 4 1.7382 0.1269 25 9 5 -0.7502 -0.1930 25 11 0 3.3122 0.2226 25 11 1 1.4676 -0.4200 25 11 2 7.2697 -0.0054 26 0 0 -1.7900 -0.5699 26 0 2 1.2286 -0.0395 26 0 4 1.3469 0.2984 26 0 6 1.1957 -0.0806 26 2 0 1.4587 -0.0962 26 2 1 1.4216 -0.0193 26 2 2 1.5329 0.0522 26 2 3 -1.0190 0.1102 26 2 4 0.0848 0.0898 26 2 5 0.1803 -0.1152 26 2 6 4.5113 -0.0079 26 2 7 1.5131 0.0106 26 2 8 3.7233 0.0114 26 2 9 -0.7358 0.3682 26 2 10 -1.4416 -0.0336 26 4 0 2.6912 -0.2667 26 4 1 0.0233 -0.1491 26 4 2 3.3336 -0.1712 26 4 3 0.9291 0.1587 26 4 4 1.1891 0.1670 26 4 5 1.1759 -0.0646 26 4 6 3.4700 -0.1484 26 4 7 2.2715 0.0284 26 4 8 7.1718 -0.6160 26 6 0 1.1018 0.0125 26 6 1 -0.3707 -0.2117 26 6 2 2.3076 -0.1615 26 6 3 0.9520 0.1351 26 6 4 -1.4629 -0.1447 26 6 5 2.4442 -0.0305 26 6 6 -2.3102 0.2048 26 6 7 1.1538 -0.6405 26 6 8 2.7432 0.8481 26 8 0 -3.6369 0.0686 26 8 1 1.9765 -0.1453 26 8 2 -2.0428 -0.0622 26 8 3 0.7722 0.0890 26 8 4 -2.2396 0.1389 26 8 5 -0.8230 0.0936 26 8 6 -0.2198 0.0557 26 10 0 6.1215 -0.6181 26 10 1 3.6629 0.0999 26 10 2 4.1423 -0.8961 26 10 3 3.4839 0.0914 27 1 0 -1.1576 -0.1646 27 1 1 -2.4009 0.2430 27 1 2 1.1208 0.1380 27 1 3 1.6384 -0.1499 27 1 4 0.8296 -0.0465 27 1 5 1.2249 0.1135 27 1 6 -0.1374 -0.0210 27 1 7 -2.6890 0.7137 27 1 8 -0.1237 0.5491 27 3 0 -0.2286 -0.1475 27 3 1 -4.2243 0.1608 27 3 2 -1.7433 0.0545 27 3 3 -0.1790 0.0530 27 3 4 -2.0319 -0.1549 27 3 5 3.7043 -0.1342 27 3 6 -0.7944 0.0177 27 3 7 0.2899 0.1512 27 3 8 -0.8872 0.3129 27 5 0 1.2173 -0.1327 27 5 1 -1.6886 -0.0782 27 5 2 1.6748 0.0405 27 5 3 -2.6915 -0.1276 27 5 4 -1.2942 0.0235 27 5 5 -0.9677 0.0945 27 5 6 -1.2217 -0.0006 27 7 0 0.0520 0.0363 27 7 1 -2.1501 -0.0788 27 7 2 2.7338 -0.0675 27 7 3 -2.1650 0.1930 27 7 4 2.3654 0.1219 27 7 5 -0.3381 0.1744 27 7 6 2.0699 0.5721 27 9 0 2.8903 0.2202 27 9 1 -1.6902 0.3049 27 9 2 0.3012 0.3640 27 9 3 -1.1703 0.7334 28 0 0 -0.6123 0.3378 28 0 2 -0.4266 -0.3082 28 0 4 -2.9150 0.3637 28 0 6 -2.5598 0.6661 28 2 0 0.3541 0.1519 28 2 1 -1.8050 -0.0440 28 2 2 3.6218 -0.0965 28 2 3 -1.1615 -0.0471 28 2 4 -0.8411 -0.0353 28 2 5 -1.1961 0.0868 28 2 6 -6.2903 0.0610 28 2 7 0.4386 -0.5293 28 4 0 0.8185 -0.0281 28 4 1 1.3730 -0.1761 28 4 2 3.1524 -0.1906 28 4 3 1.4517 0.1923 28 4 4 0.3889 0.1920 28 4 5 -0.6302 0.4272 28 4 6 -4.4842 0.7334 28 6 0 -0.8488 -0.1852 28 6 1 4.0512 -0.1451 28 6 2 -0.6440 0.4193 28 6 3 1.4000 0.0385 28 6 4 0.8086 0.5857 28 8 0 4.8258 0.1603 28 8 1 0.1742 -0.0773 28 8 2 0.6335 0.0762 28 8 3 1.8614 -0.3332 28 8 4 0.7339 -0.1130 28 10 0 -3.4301 1.0927 29 1 0 -2.2798 -0.0453 29 1 1 1.6521 -0.0008 29 1 2 -1.8020 0.1747 29 1 3 -0.2302 0.0276 29 1 4 2.4183 0.0963 29 1 5 0.3999 -1.0665 29 1 6 1.4636 -0.6338 29 3 0 0.4143 -0.0815 29 3 1 1.4843 -0.0701 29 3 2 2.4588 0.0654 29 3 3 -2.6463 0.2915 29 3 4 1.6498 0.3029 29 3 5 -3.9778 -0.0909 29 3 6 -0.3683 -0.1770 29 5 0 -2.3871 0.0866 29 5 1 1.6439 0.5848 29 5 2 -1.0025 -0.0406 29 5 3 2.0293 0.8322 29 7 0 1.0031 0.0617 29 7 1 1.3765 0.1611 29 7 2 0.0913 0.2675 29 9 0 -2.3040 -0.4098 30 0 0 -0.1941 0.7951 30 0 2 -0.3149 -0.0720 30 2 0 -1.1022 0.0059 30 2 1 2.9497 0.0348 30 2 2 -3.7685 0.0690 30 2 3 3.9950 -0.2623 30 2 4 0.6996 -0.0014 30 4 0 -2.6871 0.5460 30 4 1 -2.0971 0.0984 30 4 2 -3.5006 0.3723 30 4 3 -2.4960 -0.9078 30 6 0 -0.1017 0.7041 30 8 0 -2.4565 -0.0675 31 1 0 2.5551 -0.0550 31 1 1 -0.7070 -0.6462 31 1 2 -0.4936 -0.4042 31 3 0 0.7978 0.2193 31 3 1 0.2585 -0.2320 31 3 2 -3.1171 -0.1235 31 3 3 -0.1937 -0.1621 31 5 0 2.0334 -0.0766 31 5 1 -0.1172 -1.0313 31 5 2 -1.2416 -0.0308 32 2 0 0.8984 -0.2493 32 4 0 1.2394 -0.6671 0 0 0 0.0 0.0 ; _shelx_fab_checksum 88112 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.436 _oxdiff_exptl_absorpt_empirical_full_min 0.711 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 Cu01 Cu 0.500000 0.05948(3) 0.250000 0.01645(12) Uani 1 2 d S T P . . Cu02 Cu 0.500000 0.24775(3) 0.250000 0.01740(13) Uani 1 2 d S T P . . S10 S 0.15551(3) 0.20513(6) 0.26633(5) 0.02860(19) Uani 1 1 d . . . . . S11 S 0.62748(3) 0.15954(6) 0.73426(5) 0.02528(17) Uani 1 1 d . . . . . O1 O 0.41535(10) 0.23632(15) 0.22444(15) 0.0276(5) Uani 1 1 d . . . . . O2 O 0.41869(9) 0.07993(14) 0.25288(13) 0.0224(4) Uani 1 1 d . . . . . O19 O 0.53244(10) 0.07198(14) 0.36050(13) 0.0224(4) Uani 1 1 d . . . . . O20 O 0.51253(11) 0.22945(15) 0.35754(14) 0.0266(5) Uani 1 1 d . . . . . N21 N 0.500000 0.4004(2) 0.250000 0.0197(7) Uani 1 2 d S T P . . N28 N 0.500000 0.9061(2) 0.250000 0.0167(6) Uani 1 2 d S T P . . C3 C 0.39337(13) 0.1603(2) 0.23875(19) 0.0214(6) Uani 1 1 d . . . . . C4 C 0.33258(13) 0.1696(2) 0.24016(19) 0.0222(6) Uani 1 1 d . . . . . C5 C 0.30545(13) 0.0942(2) 0.2616(2) 0.0244(6) Uani 1 1 d . . . . . H5 H 0.324106 0.033147 0.271723 0.029 Uiso 1 1 calc R . . . . C6 C 0.25129(13) 0.1067(2) 0.2683(2) 0.0264(6) Uani 1 1 d . . . . . H6 H 0.233037 0.054629 0.283642 0.032 Uiso 1 1 calc R . . . . C7 C 0.22382(13) 0.1951(2) 0.25269(19) 0.0243(6) Uani 1 1 d . . . . . C8 C 0.24912(15) 0.2711(2) 0.2276(2) 0.0338(8) Uani 1 1 d . . . . . H8 H 0.229363 0.330993 0.214553 0.041 Uiso 1 1 calc R . . . . C9 C 0.30380(15) 0.2574(2) 0.2220(2) 0.0329(8) Uani 1 1 d . . . . . H9 H 0.321815 0.308832 0.205633 0.039 Uiso 1 1 calc R . . . . C12 C 0.59797(13) 0.1628(2) 0.63324(19) 0.0233(6) Uani 1 1 d . . . . . C13 C 0.58392(15) 0.0744(2) 0.5972(2) 0.0275(6) Uani 1 1 d . . . . . H13 H 0.588773 0.017114 0.626060 0.033 Uiso 1 1 calc R . . . . C14 C 0.56253(15) 0.0707(2) 0.5179(2) 0.0268(6) Uani 1 1 d . . . . . H14 H 0.554748 0.010290 0.492896 0.032 Uiso 1 1 calc R . . . . C15 C 0.55261(13) 0.1543(2) 0.47554(19) 0.0223(6) Uani 1 1 d . . . . . C16 C 0.56449(18) 0.2428(2) 0.5126(2) 0.0339(8) Uani 1 1 d . . . . . H16 H 0.556360 0.300473 0.483882 0.041 Uiso 1 1 calc R . . . . C17 C 0.58810(18) 0.2467(2) 0.5910(2) 0.0338(8) Uani 1 1 d . . . . . H17 H 0.597545 0.306975 0.615975 0.041 Uiso 1 1 calc R . . . . C18 C 0.53124(13) 0.1516(2) 0.39143(18) 0.0209(5) Uani 1 1 d . . . . . C22 C 0.54546(14) 0.4498(2) 0.2977(2) 0.0243(6) Uani 1 1 d . . . . . H22 H 0.578095 0.415222 0.331535 0.029 Uiso 1 1 calc R . . . . C23 C 0.54705(13) 0.5492(2) 0.30007(19) 0.0231(6) Uani 1 1 d . . . . . H23 H 0.579748 0.582127 0.335311 0.028 Uiso 1 1 calc R . . . . C24 C 0.500000 0.5993(3) 0.250000 0.0196(8) Uani 1 2 d S T P . . C25 C 0.500000 0.7060(3) 0.250000 0.0170(7) Uani 1 2 d S T P . . C26 C 0.52406(13) 0.75783(19) 0.31697(18) 0.0204(5) Uani 1 1 d . . . . . H26 H 0.541337 0.725291 0.363992 0.025 Uiso 1 1 calc R . . . . C27 C 0.52271(12) 0.85778(19) 0.31476(17) 0.0188(5) Uani 1 1 d . . . . . H27 H 0.538517 0.892517 0.360962 0.023 Uiso 1 1 calc R . . . . O1S O 0.5667(11) 0.5255(9) 0.0084(10) 0.401(14) Uani 1 1 d . U . . . N3S N 0.5897(3) 0.3920(5) 0.0721(3) 0.0854(18) Uani 1 1 d . . . . . C2S C 0.5734(4) 0.4421(7) 0.0092(5) 0.109(3) Uani 1 1 d . U . . . H2S H 0.566703 0.409703 -0.037299 0.131 Uiso 1 1 calc R . . . . C4S C 0.5870(5) 0.4258(7) 0.1392(5) 0.118(4) Uani 1 1 d . . . . . H4SA H 0.576747 0.373021 0.166305 0.177 Uiso 1 1 calc GR . . . . H4SB H 0.557021 0.476179 0.128343 0.177 Uiso 1 1 calc GR . . . . H4SC H 0.625470 0.452193 0.170743 0.177 Uiso 1 1 calc GR . . . . C5S C 0.6005(4) 0.2923(8) 0.0630(7) 0.129(4) Uani 1 1 d . . . . . H5SA H 0.566222 0.254361 0.061408 0.194 Uiso 1 1 calc GR . . . . H5SB H 0.635288 0.271127 0.105797 0.194 Uiso 1 1 calc GR . . . . H5SC H 0.607425 0.283364 0.015624 0.194 Uiso 1 1 calc GR . . . . 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 Cu01 0.0147(2) 0.0072(2) 0.0310(3) 0.000 0.01252(19) 0.000 Cu02 0.0155(2) 0.0069(2) 0.0342(3) 0.000 0.0142(2) 0.000 S10 0.0190(3) 0.0290(4) 0.0454(5) 0.0123(3) 0.0207(3) 0.0060(3) S11 0.0188(3) 0.0262(4) 0.0354(4) -0.0038(3) 0.0152(3) -0.0059(3) O1 0.0170(10) 0.0148(9) 0.0551(15) 0.0045(9) 0.0180(10) 0.0016(8) O2 0.0173(9) 0.0132(9) 0.0409(13) 0.0012(8) 0.0154(9) 0.0016(7) O19 0.0242(10) 0.0108(8) 0.0345(12) -0.0008(8) 0.0134(9) 0.0001(7) O20 0.0336(12) 0.0129(9) 0.0363(12) 0.0018(8) 0.0164(10) 0.0007(8) N21 0.0234(16) 0.0080(13) 0.0324(19) 0.000 0.0159(15) 0.000 N28 0.0122(13) 0.0120(13) 0.0308(18) 0.000 0.0137(13) 0.000 C3 0.0147(12) 0.0148(12) 0.0381(16) -0.0020(11) 0.0138(12) 0.0015(9) C4 0.0144(12) 0.0186(13) 0.0374(16) 0.0008(11) 0.0140(12) 0.0007(10) C5 0.0177(13) 0.0164(12) 0.0421(18) 0.0042(12) 0.0147(12) 0.0028(10) C6 0.0201(13) 0.0203(14) 0.0421(18) 0.0084(12) 0.0155(13) 0.0012(11) C7 0.0175(13) 0.0238(14) 0.0347(16) 0.0046(12) 0.0133(12) 0.0033(11) C8 0.0253(15) 0.0211(14) 0.064(2) 0.0114(15) 0.0274(16) 0.0070(12) C9 0.0236(15) 0.0198(14) 0.065(2) 0.0108(14) 0.0270(16) 0.0039(11) C12 0.0188(13) 0.0239(14) 0.0325(16) -0.0029(12) 0.0154(12) -0.0039(11) C13 0.0286(15) 0.0180(13) 0.0357(17) 0.0023(12) 0.0115(13) -0.0026(11) C14 0.0282(15) 0.0139(12) 0.0370(17) 0.0018(11) 0.0103(13) -0.0020(11) C15 0.0226(13) 0.0133(12) 0.0353(16) -0.0013(11) 0.0155(12) -0.0011(10) C16 0.048(2) 0.0158(13) 0.041(2) -0.0020(13) 0.0196(17) -0.0018(13) C17 0.047(2) 0.0164(14) 0.0381(19) -0.0064(13) 0.0159(16) -0.0042(13) C18 0.0201(13) 0.0134(12) 0.0317(15) -0.0011(10) 0.0126(11) -0.0009(10) C22 0.0231(14) 0.0105(11) 0.0410(18) 0.0031(11) 0.0136(13) 0.0019(10) C23 0.0215(13) 0.0117(12) 0.0350(16) -0.0020(11) 0.0090(12) 0.0003(10) C24 0.028(2) 0.0033(13) 0.032(2) 0.000 0.0165(17) 0.000 C25 0.0150(16) 0.0103(15) 0.030(2) 0.000 0.0139(15) 0.000 C26 0.0242(13) 0.0097(11) 0.0304(15) 0.0013(10) 0.0134(12) 0.0002(10) C27 0.0187(12) 0.0098(11) 0.0297(14) -0.0015(10) 0.0112(11) 0.0001(9) O1S 0.81(4) 0.093(6) 0.296(18) -0.011(9) 0.20(2) -0.007(14) N3S 0.082(4) 0.121(5) 0.062(3) 0.033(3) 0.037(3) 0.034(4) C2S 0.135(8) 0.097(6) 0.088(6) 0.019(5) 0.031(5) 0.026(6) C4S 0.171(9) 0.118(7) 0.113(6) 0.046(5) 0.110(7) 0.066(6) C5S 0.059(4) 0.123(8) 0.189(11) -0.013(7) 0.025(6) -0.005(5) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O2 Cu01 Cu02 81.90(6) . . ? O2 Cu01 Cu02 81.90(6) 2_655 . ? O2 Cu01 O2 163.81(12) 2_655 . ? O2 Cu01 N28 98.10(6) . 1_545 ? O2 Cu01 N28 98.10(6) 2_655 1_545 ? O19 Cu01 Cu02 84.89(6) . . ? O19 Cu01 Cu02 84.89(6) 2_655 . ? O19 Cu01 O2 89.97(9) . 2_655 ? O19 Cu01 O2 88.59(9) 2_655 2_655 ? O19 Cu01 O2 88.59(9) . . ? O19 Cu01 O2 89.97(9) 2_655 . ? O19 Cu01 O19 169.79(12) 2_655 . ? O19 Cu01 N28 95.11(6) 2_655 1_545 ? O19 Cu01 N28 95.11(6) . 1_545 ? N28 Cu01 Cu02 180.0 1_545 . ? O1 Cu02 Cu01 85.30(6) 2_655 . ? O1 Cu02 Cu01 85.30(6) . . ? O1 Cu02 O1 170.61(13) 2_655 . ? O1 Cu02 O20 89.00(11) 2_655 . ? O1 Cu02 O20 89.00(11) . 2_655 ? O1 Cu02 O20 89.79(11) . . ? O1 Cu02 O20 89.78(11) 2_655 2_655 ? O1 Cu02 N21 94.70(6) . . ? O1 Cu02 N21 94.70(6) 2_655 . ? O20 Cu02 Cu01 82.54(6) . . ? O20 Cu02 Cu01 82.54(6) 2_655 . ? O20 Cu02 O20 165.08(13) . 2_655 ? O20 Cu02 N21 97.46(6) . . ? O20 Cu02 N21 97.46(6) 2_655 . ? N21 Cu02 Cu01 180.0 . . ? C7 S10 S11 105.11(11) . 8_455 ? C12 S11 S10 104.96(11) . 8_556 ? C3 O1 Cu02 120.71(19) . . ? C3 O2 Cu01 121.90(18) . . ? C18 O19 Cu01 120.5(2) . . ? C18 O20 Cu02 122.1(2) . . ? C22 N21 Cu02 120.97(17) 2_655 . ? C22 N21 Cu02 120.97(17) . . ? C22 N21 C22 118.1(3) . 2_655 ? C27 N28 Cu01 120.41(17) 2_655 1_565 ? C27 N28 Cu01 120.41(17) . 1_565 ? C27 N28 C27 119.2(3) 2_655 . ? O1 C3 C4 115.6(2) . . ? O2 C3 O1 125.4(3) . . ? O2 C3 C4 119.0(3) . . ? C5 C4 C3 121.6(3) . . ? C5 C4 C9 119.4(3) . . ? C9 C4 C3 119.0(3) . . ? C4 C5 H5 119.7 . . ? C4 C5 C6 120.5(3) . . ? C6 C5 H5 119.7 . . ? C5 C6 H6 120.1 . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C6 C7 S10 116.4(2) . . ? C6 C7 C8 120.7(3) . . ? C8 C7 S10 122.9(2) . . ? C7 C8 H8 120.7 . . ? C9 C8 C7 118.6(3) . . ? C9 C8 H8 120.7 . . ? C4 C9 H9 119.5 . . ? C8 C9 C4 120.9(3) . . ? C8 C9 H9 119.5 . . ? C13 C12 S11 115.8(2) . . ? C17 C12 S11 123.9(3) . . ? C17 C12 C13 120.3(3) . . ? C12 C13 H13 120.4 . . ? C12 C13 C14 119.2(3) . . ? C14 C13 H13 120.4 . . ? C13 C14 H14 119.7 . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 C18 121.3(3) . . ? C16 C15 C18 119.2(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C12 C17 H17 119.9 . . ? C16 C17 C12 120.2(3) . . ? C16 C17 H17 119.9 . . ? O19 C18 C15 117.5(3) . . ? O20 C18 O19 126.0(3) . . ? O20 C18 C15 116.5(3) . . ? N21 C22 H22 118.6 . . ? N21 C22 C23 122.9(3) . . ? C23 C22 H22 118.6 . . ? C22 C23 H23 120.8 . . ? C24 C23 C22 118.5(3) . . ? C24 C23 H23 120.8 . . ? C23 C24 C23 119.3(3) . 2_655 ? C23 C24 C25 120.37(17) . . ? C23 C24 C25 120.37(17) 2_655 . ? C26 C25 C24 121.31(17) . . ? C26 C25 C24 121.31(17) 2_655 . ? C26 C25 C26 117.4(3) . 2_655 ? C25 C26 H26 120.2 . . ? C25 C26 C27 119.6(3) . . ? C27 C26 H26 120.2 . . ? N28 C27 C26 122.1(3) . . ? N28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C2S N3S C4S 123.7(8) . . ? C2S N3S C5S 114.5(8) . . ? C4S N3S C5S 120.9(7) . . ? O1S C2S N3S 122.4(13) . . ? O1S C2S H2S 118.8 . . ? N3S C2S H2S 118.8 . . ? N3S C4S H4SA 109.5 . . ? N3S C4S H4SB 109.5 . . ? N3S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? N3S C5S H5SA 109.5 . . ? N3S C5S H5SB 109.5 . . ? N3S C5S H5SC 109.5 . . ? H5SA C5S H5SB 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu01 Cu02 2.6229(6) . ? Cu01 O2 2.023(2) 2_655 ? Cu01 O2 2.023(2) . ? Cu01 O19 1.957(2) 2_655 ? Cu01 O19 1.957(2) . ? Cu01 N28 2.137(3) 1_545 ? Cu02 O1 1.946(2) 2_655 ? Cu02 O1 1.946(2) . ? Cu02 O20 1.963(2) . ? Cu02 O20 1.963(2) 2_655 ? Cu02 N21 2.127(3) . ? S10 S11 2.0216(11) 8_455 ? S10 C7 1.781(3) . ? S11 C12 1.782(3) . ? O1 C3 1.260(3) . ? O2 C3 1.259(3) . ? O19 C18 1.260(3) . ? O20 C18 1.258(4) . ? N21 C22 1.336(4) . ? N21 C22 1.336(4) 2_655 ? N28 C27 1.330(3) 2_655 ? N28 C27 1.330(3) . ? C3 C4 1.497(4) . ? C4 C5 1.379(4) . ? C4 C9 1.389(4) . ? C5 H5 0.9500 . ? C5 C6 1.383(4) . ? C6 H6 0.9500 . ? C6 C7 1.382(4) . ? C7 C8 1.393(4) . ? C8 H8 0.9500 . ? C8 C9 1.388(4) . ? C9 H9 0.9500 . ? C12 C13 1.389(4) . ? C12 C17 1.386(5) . ? C13 H13 0.9500 . ? C13 C14 1.400(5) . ? C14 H14 0.9500 . ? C14 C15 1.384(4) . ? C15 C16 1.396(4) . ? C15 C18 1.485(5) . ? C16 H16 0.9500 . ? C16 C17 1.385(5) . ? C17 H17 0.9500 . ? C22 H22 0.9500 . ? C22 C23 1.386(4) . ? C23 H23 0.9500 . ? C23 C24 1.381(3) . ? C24 C25 1.486(5) . ? C25 C26 1.390(4) . ? C25 C26 1.390(4) 2_655 ? C26 H26 0.9500 . ? C26 C27 1.393(4) . ? C27 H27 0.9500 . ? O1S C2S 1.173(13) . ? N3S C2S 1.311(9) . ? N3S C4S 1.380(9) . ? N3S C5S 1.435(12) . ? C2S H2S 0.9500 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? 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 0.250 -0.808 0.500 505.1 105.2 3.5DMF 2 0.250 -0.768 0.000 505.1 105.2 3.5DMF 3 0.750 -0.268 0.000 505.1 105.2 3.5DMF 4 0.750 -0.308 0.500 505.1 105.2 3.5DMF