#------------------------------------------------------------------------------ #$Date: 2024-07-05 20:58:57 +0300 (Fri, 05 Jul 2024) $ #$Revision: 293266 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/98/7159894.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_7159894 loop_ _publ_author_name 'Gerasimova, Tatiana P.' 'Zagidullin, Almaz A.' 'Nikolaeva, Anastasiia N.' 'Fayzullin, Robert R.' 'Saitova, Aliya M.' 'Miluykov, Vasili A.' 'Grimme, Stefan' 'Katsyuba, Sergey A.' _publ_section_title ; Structural flexibility of favipiravir and its structural analogues in solutions: experimental and computational insight. ; _journal_issue 18 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 3668 _journal_page_last 3683 _journal_paper_doi 10.1039/d4ob00404c _journal_volume 22 _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety 'C7 H8 N4 O4' _chemical_formula_sum 'C7 H8 N4 O4' _chemical_formula_weight 212.17 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-02-18 deposited with the CCDC. 2024-04-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.0641(10) _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 11.6092(5) _cell_length_b 15.2706(7) _cell_length_c 15.2983(7) _cell_measurement_reflns_used 52924 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 34.95 _cell_measurement_theta_min 2.41 _cell_volume 2652.2(2) _computing_cell_refinement 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_collection 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_reduction 'APEX4 v2021.10-0 (Bruker AXS)' _computing_molecular_graphics ; WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ; _computing_publication_material ; WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 23264 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 35.022 _diffrn_reflns_theta_min 1.361 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_T_max 0.841176 _exptl_absorpt_correction_T_min 0.504965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Stalke et al., 2015) Equivalent reflections defined according to point group 2 Mean and maximum errors in direction cosine check function = 0.000 0.002 Restraint esd for equal adjacent scale factors = 0.0090 Maximum odd and even orders for spherical harmonics = 1 4 Parameter refinement for twin component 1 ------------------------------------------ 63575 single and 0 composite reflections used for parameter fitting Effective data to parameter ratio = 18.43 wR2(int) = 0.1535 (selected reflections only, before parameter refinement) wR2(int) = 0.0776 (selected reflections only, after parameter refinement) Parameter refinement for twin component 2 ------------------------------------------ 53895 single and 0 composite reflections used for parameter fitting Effective data to parameter ratio = 15.45 wR2(int) = 0.1906 (selected reflections only, before parameter refinement) wR2(int) = 0.0842 (selected reflections only, after parameter refinement) ------------------------------------------ 219897 total and 39794 unique reflections after rejecting pathological cases Reflections rejected for which |I-|/su > 3.00 Where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 216765 total and 39779 unique reflections left after |I-|/su test g = 0.0364 gave best error model; g set to 0.0364 for further calculations Statistics for singles of twin component 1 ------------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.1103 0.107 - 0.171 1.139 - 1.237 0.977 13307 9237 2 33.6 0.1332 0.063 - 0.176 1.139 - 1.229 1.008 13099 8420 3 33.6 0.0999 0.088 - 0.166 1.139 - 1.233 0.964 13394 9487 4 33.6 0.1159 0.078 - 0.149 1.139 - 1.239 0.983 13006 8922 5 33.6 0.1410 0.067 - 0.183 1.139 - 1.235 0.995 12879 8248 6 33.6 0.1195 0.090 - 0.156 1.139 - 1.229 1.015 13437 8855 7 0.0 0.2070 0.123 - 0.370 1.139 - 1.239 1.074 9691 5131 All scans 0.1330 0.063 - 0.370 1.139 - 1.239 1.002 88813 58300 Statistics for singles of twin component 2 ------------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.2150 0.017 - 0.070 1.535 - 1.897 0.977 13257 6603 2 33.6 0.1241 0.008 - 0.023 1.535 - 1.896 1.008 13013 8509 3 33.6 0.2017 0.017 - 0.063 1.554 - 1.897 0.964 13411 6993 4 33.6 0.1627 0.011 - 0.033 1.536 - 1.897 0.983 12857 7511 5 33.6 0.1587 0.009 - 0.031 1.535 - 1.897 0.995 12853 7753 6 33.6 0.2461 0.013 - 0.063 1.535 - 1.897 1.015 13351 6116 7 0.0 0.2740 0.028 - 0.069 1.535 - 1.888 1.074 9746 4280 All scans 0.1973 0.008 - 0.070 1.535 - 1.897 1.002 88488 47765 Statistics for all composite reflections ---------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.0491 0.036 - 0.116 1.286 - 1.616 0.977 5866 5179 2 33.6 0.0714 0.030 - 0.134 1.304 - 1.618 1.008 5566 4759 3 33.6 0.0475 0.048 - 0.127 1.334 - 1.605 0.964 5747 5192 4 33.6 0.0555 0.025 - 0.111 1.286 - 1.699 0.983 6100 5294 5 33.6 0.0533 0.029 - 0.133 1.308 - 1.628 0.995 6296 5410 6 33.6 0.0562 0.049 - 0.128 1.298 - 1.645 1.015 5640 4997 7 0.0 0.0579 0.067 - 0.244 1.337 - 1.574 1.074 4249 3755 All scans 0.0556 0.025 - 0.244 1.286 - 1.699 1.002 39464 34586 Statistics for all single and composite reflections --------------------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.0676 0.017 - 0.171 1.139 - 1.897 0.977 32430 21019 2 33.6 0.0888 0.008 - 0.176 1.139 - 1.896 1.008 31678 21688 3 33.6 0.0640 0.017 - 0.166 1.139 - 1.897 0.964 32552 21672 4 33.6 0.0718 0.011 - 0.149 1.139 - 1.897 0.983 31963 21727 5 33.6 0.0742 0.009 - 0.183 1.139 - 1.897 0.995 32028 21411 6 33.6 0.0762 0.013 - 0.156 1.139 - 1.897 1.015 32428 19968 7 0.0 0.0857 0.028 - 0.370 1.139 - 1.888 1.074 23686 13166 All scans 0.0759 0.008 - 0.370 1.139 - 1.897 1.002 216765 140651 su = K * Sqrt[ sigma^2(I) + (g)^2 ] where sigma(I) is estimated by SAINT Rint = 0.0749 for all 216672 observations and Rint = 0.0594 for all 110123 observations with I > 3sigma(I) HKLF 5 dataset constructed from all observations involving domain 1 31990 Corrected reflections written to file hkl Reflections merged according to point-group 2 Single reflections that also occur in composites omitted Racemic twinning not included for all components Second component not inverted relative to first Minimum and maximum apparent transmission: 0.504965 0.841176 Additional spherical absorption correction applied with mu*r = 0.0300 ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.594 _exptl_crystal_description prism _exptl_crystal_F_000 1320 _exptl_crystal_size_max 0.538 _exptl_crystal_size_mid 0.520 _exptl_crystal_size_min 0.168 _refine_diff_density_max 0.533 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.065 _refine_ls_abs_structure_details ; Flack x determined using 8143 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.1(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 866 _refine_ls_number_reflns 23264 _refine_ls_number_restraints 31 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0509 _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^)+(0.0713P)^2^+0.7419P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1269 _refine_ls_wR_factor_ref 0.1401 _reflns_Friedel_coverage 0.939 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 19754 _reflns_number_total 23264 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob00404c2.cif _cod_data_source_block zagid016 _cod_depositor_comments 'Adding full bibliography for 7159893--7159895.cif.' _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7159894 _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_min 0.932 _shelx_estimated_absorpt_t_max 0.978 _shelx_res_file ; TITL zagid016 in P2(1) shelx.res created by SHELXL-2018/3 at 10:59:26 on 18-Feb-2024 CELL 0.71073 11.60920 15.27060 15.29830 90.0000 102.0641 90.0000 ZERR 12.00 0.00050 0.00070 0.00070 0.0000 0.0010 0.0000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 84 96 48 48 MERG 0 OMIT -2 0 2 OMIT -1 1 1 OMIT -11 0 11 OMIT -1 2 1 OMIT -1 -1 -1 OMIT 1 1 1 SADI 0.01 N1A H1AA N1B H1BA N1C H1CA N1D H1DA N1E H1EA N1F H1FA SADI 0.01 N1A H1AB N1B H1BB N1C H1CB N1D H1DB N1E H1EB N1F H1FB MORE -1 HTAB N1A O3A HTAB N1A O1C HTAB N1B O3B EQIV $1 -x+1, y-1/2, -z+1 HTAB N1B O52D_$1 HTAB N1B O1D HTAB N1C O3C EQIV $2 -x+1, y-1/2, -z HTAB N1C O1F_$2 HTAB N1D O3D HTAB N1D O1A EQIV $3 -x+2, y+1/2, -z+1 HTAB N1E O52B_$3 HTAB N1E O3E HTAB N1E O1B HTAB N1F O3F HTAB N1F O1E_$3 FMAP 2 PLAN 40 SIZE 0.168 0.520 0.538 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -173.15 WGHT 0.071300 0.741900 BASF 0.28305 FVAR 0.51548 O1A 4 0.554596 0.468189 0.161860 11.00000 0.02196 0.01188 = 0.02991 -0.00514 0.00433 0.00078 O3A 4 0.413454 0.228208 0.052627 11.00000 0.01361 0.01466 = 0.01976 -0.00158 0.00009 0.00022 O51A 4 0.906823 0.321776 0.262035 11.00000 0.01944 0.02073 = 0.03913 -0.00594 -0.00320 -0.00404 O52A 4 0.920944 0.181250 0.248451 11.00000 0.01552 0.02070 = 0.02360 0.00136 0.00187 0.00487 N1A 3 0.404599 0.405910 0.063577 11.00000 0.01476 0.01243 = 0.02282 0.00024 0.00257 0.00356 H1AA 2 0.378658 0.359616 0.033624 11.00000 0.02951 H1AB 2 0.356277 0.451593 0.058748 11.00000 0.01515 N2A 3 0.683874 0.321037 0.173165 11.00000 0.01390 0.01137 = 0.01357 -0.00121 0.00432 0.00065 N3A 3 0.585955 0.160651 0.115689 11.00000 0.01385 0.00933 = 0.01474 -0.00104 0.00152 0.00042 N5A 3 0.865509 0.250764 0.235990 11.00000 0.01272 0.01822 = 0.01534 -0.00144 0.00182 0.00052 C1A 1 0.509313 0.404088 0.119157 11.00000 0.01560 0.01012 = 0.01707 0.00017 0.00683 0.00099 C2A 1 0.574359 0.317445 0.129750 11.00000 0.01267 0.00929 = 0.01413 -0.00064 0.00412 -0.00036 C3A 1 0.515380 0.235381 0.096136 11.00000 0.01442 0.01078 = 0.01143 0.00033 0.00350 0.00145 C4A 1 0.697833 0.165205 0.161947 11.00000 0.01437 0.01154 = 0.01429 0.00022 0.00251 0.00147 AFIX 43 H4A 2 0.743906 0.113724 0.176076 11.00000 -1.20000 AFIX 0 C5A 1 0.743512 0.245740 0.188090 11.00000 0.01236 0.01276 = 0.01258 -0.00095 0.00209 0.00081 C31A 1 0.536249 0.073242 0.087148 11.00000 0.02065 0.00959 = 0.01684 -0.00392 0.00260 -0.00099 AFIX 23 H31A 2 0.598628 0.035566 0.071932 11.00000 -1.20000 H31B 2 0.473069 0.079548 0.032970 11.00000 -1.20000 AFIX 0 C32A 1 0.486796 0.030487 0.160458 11.00000 0.04141 0.01630 = 0.02834 -0.00408 0.01061 -0.00996 AFIX 137 H32A 2 0.468122 -0.030903 0.144989 11.00000 -1.50000 H32B 2 0.415025 0.061227 0.167113 11.00000 -1.50000 H32C 2 0.545164 0.033406 0.216821 11.00000 -1.50000 AFIX 0 O1B 4 0.875178 0.460712 0.517351 11.00000 0.02061 0.01054 = 0.02060 -0.00390 0.00569 -0.00065 O3B 4 0.738636 0.224553 0.391665 11.00000 0.01414 0.01533 = 0.02277 -0.00305 -0.00034 -0.00067 O51B 4 1.232789 0.319112 0.597673 11.00000 0.01619 0.02128 = 0.02253 -0.00409 0.00173 -0.00506 O52B 4 1.255424 0.182905 0.564201 11.00000 0.01420 0.02078 = 0.02618 0.00071 0.00235 0.00380 N1B 3 0.717663 0.396228 0.427797 11.00000 0.01553 0.01095 = 0.02294 -0.00071 0.00370 0.00211 H1BA 2 0.693182 0.348827 0.399394 11.00000 0.02645 H1BB 2 0.671856 0.443430 0.422308 11.00000 0.01669 N2B 3 1.007749 0.316770 0.514548 11.00000 0.01307 0.01312 = 0.01195 -0.00102 0.00463 0.00021 N3B 3 0.912928 0.157420 0.450297 11.00000 0.01235 0.01102 = 0.01405 -0.00225 0.00326 0.00045 N5B 3 1.194862 0.249414 0.564077 11.00000 0.01240 0.01787 = 0.01380 0.00135 0.00337 -0.00042 C1B 1 0.828059 0.396950 0.474301 11.00000 0.01536 0.00959 = 0.01356 0.00038 0.00645 0.00023 C2B 1 0.896807 0.312815 0.474814 11.00000 0.01240 0.01039 = 0.01133 -0.00162 0.00295 -0.00022 C3B 1 0.840596 0.231651 0.435523 11.00000 0.01243 0.01195 = 0.01311 -0.00092 0.00288 0.00027 C4B 1 1.026434 0.162631 0.492526 11.00000 0.01171 0.01365 = 0.01306 -0.00041 0.00419 0.00151 AFIX 43 H4B 2 1.074571 0.111788 0.502263 11.00000 -1.20000 AFIX 0 C5B 1 1.070968 0.243067 0.521169 11.00000 0.01172 0.01338 = 0.01189 -0.00045 0.00302 0.00030 C31B 1 0.862231 0.070983 0.418620 11.00000 0.01743 0.01078 = 0.01883 -0.00658 0.00280 -0.00131 AFIX 23 H31C 2 0.926656 0.030545 0.412324 11.00000 -1.20000 H31D 2 0.809887 0.077943 0.359028 11.00000 -1.20000 AFIX 0 C32B 1 0.793205 0.031899 0.482237 11.00000 0.06176 0.02104 = 0.04958 -0.01217 0.03202 -0.02015 AFIX 137 H32D 2 0.764252 -0.026151 0.460780 11.00000 -1.50000 H32E 2 0.726266 0.069933 0.485572 11.00000 -1.50000 H32F 2 0.844213 0.026500 0.541725 11.00000 -1.50000 AFIX 0 O1C 4 0.218388 0.527225 0.080424 11.00000 0.02626 0.01081 = 0.01980 0.00220 0.00612 0.00587 O3C 4 0.094616 0.763629 -0.047137 11.00000 0.02137 0.01262 = 0.01023 -0.00013 0.00114 0.00146 O51C 4 0.220174 0.668989 0.349671 11.00000 0.02842 0.02018 = 0.01583 0.00531 0.00167 -0.00166 O52C 4 0.183913 0.808209 0.355222 11.00000 0.03014 0.02123 = 0.01475 -0.00588 0.00804 -0.00393 N1C 3 0.119833 0.586203 -0.049449 11.00000 0.02458 0.01202 = 0.01485 -0.00279 0.00359 0.00290 H1CA 2 0.075490 0.629569 -0.071886 11.00000 0.03386 H1CB 2 0.129377 0.536054 -0.077246 11.00000 0.03214 N2C 3 0.176367 0.671364 0.172317 11.00000 0.01134 0.01140 = 0.01273 0.00021 0.00270 -0.00008 N3C 3 0.123590 0.831012 0.088322 11.00000 0.01368 0.00894 = 0.01095 -0.00043 0.00162 0.00249 N5C 3 0.192853 0.740004 0.314011 11.00000 0.01501 0.01840 = 0.01107 0.00085 0.00253 -0.00254 C1C 1 0.166693 0.589447 0.037801 11.00000 0.01592 0.00927 = 0.01540 -0.00091 0.00640 0.00033 C2C 1 0.153824 0.675075 0.084725 11.00000 0.01223 0.00692 = 0.01200 -0.00013 0.00295 0.00146 C3C 1 0.122309 0.756834 0.034871 11.00000 0.01348 0.00840 = 0.01055 -0.00110 0.00234 0.00152 C4C 1 0.147470 0.826472 0.178164 11.00000 0.01384 0.01146 = 0.01071 -0.00097 0.00233 0.00114 AFIX 43 H4C 2 0.147715 0.877644 0.213517 11.00000 -1.20000 AFIX 0 C5C 1 0.171326 0.746222 0.217008 11.00000 0.01332 0.01249 = 0.01052 -0.00031 0.00299 0.00011 C31C 1 0.095652 0.917231 0.044107 11.00000 0.02330 0.00915 = 0.01457 0.00053 0.00159 0.00507 AFIX 23 H31E 2 0.074412 0.959193 0.087481 11.00000 -1.20000 H31F 2 0.026745 0.910878 -0.005972 11.00000 -1.20000 AFIX 0 C32C 1 0.198637 0.953241 0.008784 11.00000 0.03681 0.01784 = 0.05472 0.01597 0.01826 0.00485 AFIX 137 H32G 2 0.218458 0.912629 -0.035442 11.00000 -1.50000 H32H 2 0.266801 0.960130 0.058294 11.00000 -1.50000 H32I 2 0.177290 1.010264 -0.019356 11.00000 -1.50000 AFIX 0 O1D 4 0.520430 0.513110 0.424541 11.00000 0.02997 0.00915 = 0.02394 0.00196 0.00667 0.00465 O3D 4 0.455747 0.756315 0.291668 11.00000 0.02578 0.01269 = 0.01116 0.00034 0.00426 0.00136 O51D 4 0.534502 0.666010 0.688899 11.00000 0.04542 0.02084 = 0.01761 0.00770 0.00701 0.00814 O52D 4 0.518772 0.807581 0.691102 11.00000 0.02565 0.02213 = 0.01595 -0.00447 0.00579 -0.00023 N1D 3 0.467946 0.579200 0.289910 11.00000 0.02993 0.01118 = 0.01847 -0.00335 0.00808 0.00213 H1DA 2 0.436110 0.626760 0.265696 11.00000 0.03609 H1DB 2 0.485155 0.529992 0.263946 11.00000 0.03230 N2D 3 0.499402 0.663947 0.511181 11.00000 0.01215 0.01078 = 0.01419 0.00170 0.00374 0.00197 N3D 3 0.500324 0.824067 0.427145 11.00000 0.01469 0.00851 = 0.01304 0.00094 0.00377 -0.00071 N5D 3 0.520290 0.737011 0.651470 11.00000 0.01592 0.01982 = 0.01214 0.00213 0.00209 0.00243 C1D 1 0.491893 0.579171 0.378564 11.00000 0.01520 0.00960 = 0.01755 -0.00167 0.00550 0.00110 C2D 1 0.486787 0.666951 0.424149 11.00000 0.01245 0.00783 = 0.01429 0.00055 0.00336 0.00148 C3D 1 0.478361 0.749321 0.373652 11.00000 0.01491 0.00881 = 0.01314 0.00053 0.00422 0.00178 C4D 1 0.512400 0.820591 0.516118 11.00000 0.01303 0.01069 = 0.01359 -0.00056 0.00231 -0.00006 AFIX 43 H4D 2 0.523792 0.872432 0.551196 11.00000 -1.20000 AFIX 0 C5D 1 0.507889 0.740507 0.555019 11.00000 0.01472 0.01215 = 0.01155 0.00102 0.00270 0.00174 C31D 1 0.507863 0.909447 0.382823 11.00000 0.02002 0.00847 = 0.01908 0.00161 0.00558 -0.00163 AFIX 23 H31G 2 0.551215 0.901750 0.334077 11.00000 -1.20000 H31H 2 0.552865 0.951065 0.426658 11.00000 -1.20000 AFIX 0 C32D 1 0.388230 0.947343 0.344857 11.00000 0.02092 0.01767 = 0.04170 0.01304 0.00921 0.00605 AFIX 137 H32J 2 0.349765 0.912799 0.292932 11.00000 -1.50000 H32K 2 0.396841 1.008060 0.326487 11.00000 -1.50000 H32L 2 0.340165 0.945851 0.390423 11.00000 -1.50000 AFIX 0 O1E 4 0.887398 0.530705 0.761815 11.00000 0.02231 0.01036 = 0.01865 0.00105 0.00593 0.00418 O3E 4 0.775718 0.770171 0.632800 11.00000 0.02367 0.01272 = 0.01058 0.00068 0.00185 0.00256 O51E 4 0.876640 0.669884 1.028612 11.00000 0.02833 0.01864 = 0.01504 0.00417 0.00548 0.00181 O52E 4 0.844627 0.809673 1.035016 11.00000 0.02901 0.01907 = 0.01399 -0.00643 0.00611 0.00034 N1E 3 0.809149 0.594711 0.629262 11.00000 0.02260 0.01193 = 0.01380 -0.00289 0.00513 0.00027 H1EA 2 0.768858 0.639402 0.605601 11.00000 0.03124 H1EB 2 0.819964 0.544110 0.602835 11.00000 0.03622 N2E 3 0.841017 0.674252 0.851560 11.00000 0.01284 0.01028 = 0.01290 -0.00097 0.00364 -0.00018 N3E 3 0.792239 0.835074 0.768891 11.00000 0.01445 0.00858 = 0.01265 -0.00017 0.00111 0.00298 N5E 3 0.851301 0.741379 0.993065 11.00000 0.01417 0.01692 = 0.01252 -0.00092 0.00457 -0.00036 C1E 1 0.843303 0.594648 0.717562 11.00000 0.01308 0.00949 = 0.01371 -0.00231 0.00416 -0.00114 C2E 1 0.824973 0.679466 0.764233 11.00000 0.01170 0.00808 = 0.01253 -0.00022 0.00302 0.00072 C3E 1 0.796230 0.761979 0.714515 11.00000 0.01316 0.00907 = 0.01243 -0.00058 0.00239 0.00182 C4E 1 0.810876 0.828932 0.858265 11.00000 0.01164 0.01085 = 0.01193 -0.00127 0.00212 0.00238 AFIX 43 H4E 2 0.809401 0.879577 0.894078 11.00000 -1.20000 AFIX 0 C5E 1 0.831977 0.748253 0.896408 11.00000 0.01445 0.01234 = 0.00949 -0.00125 0.00322 0.00156 C31E 1 0.772228 0.923165 0.727748 11.00000 0.01952 0.00907 = 0.01711 0.00062 0.00065 0.00345 AFIX 23 H31I 2 0.727737 0.959709 0.762728 11.00000 -1.20000 H31J 2 0.724726 0.917785 0.666211 11.00000 -1.20000 AFIX 0 C32E 1 0.888192 0.966603 0.725245 11.00000 0.02547 0.01561 = 0.04226 0.01200 0.00712 0.00061 AFIX 137 H32M 2 0.926826 0.935120 0.683476 11.00000 -1.50000 H32N 2 0.938896 0.965458 0.785118 11.00000 -1.50000 H32O 2 0.874194 1.027451 0.705514 11.00000 -1.50000 AFIX 0 O1F 4 0.784345 0.967603 0.165927 11.00000 0.01977 0.01105 = 0.02746 0.00623 0.00391 0.00012 O3F 4 0.928005 0.728065 0.270067 11.00000 0.01322 0.01498 = 0.02288 0.00200 0.00017 0.00082 O51F 4 0.424066 0.821279 0.083212 11.00000 0.01857 0.01855 = 0.02855 0.00111 -0.00282 0.00504 O52F 4 0.415076 0.679801 0.091703 11.00000 0.01439 0.01980 = 0.02477 -0.00138 0.00203 -0.00466 N1F 3 0.933140 0.907225 0.266892 11.00000 0.01576 0.01123 = 0.01912 0.00175 0.00096 -0.00339 H1FA 2 0.959166 0.861497 0.298017 11.00000 0.04015 H1FB 2 0.980216 0.953740 0.271274 11.00000 0.01587 N2F 3 0.651411 0.821807 0.163985 11.00000 0.01358 0.01091 = 0.01170 0.00091 0.00427 -0.00042 N3F 3 0.759902 0.660871 0.197651 11.00000 0.01245 0.00924 = 0.01499 0.00087 0.00256 0.00041 N5F 3 0.468817 0.750093 0.104711 11.00000 0.01272 0.01631 = 0.01391 -0.00081 0.00286 -0.00083 C1F 1 0.828292 0.904500 0.211161 11.00000 0.01430 0.00849 = 0.01578 0.00104 0.00519 0.00105 C2F 1 0.763269 0.818316 0.201972 11.00000 0.01236 0.00902 = 0.01261 0.00101 0.00397 -0.00070 C3F 1 0.825866 0.735670 0.227742 11.00000 0.01280 0.01024 = 0.01261 0.00124 0.00247 -0.00092 C4F 1 0.644778 0.664934 0.159905 11.00000 0.01327 0.01159 = 0.01599 -0.00022 0.00345 -0.00144 AFIX 43 H4F 2 0.600275 0.613230 0.142751 11.00000 -1.20000 AFIX 0 C5F 1 0.593539 0.745814 0.146910 11.00000 0.01129 0.01196 = 0.01198 -0.00056 0.00189 -0.00023 C31F 1 0.819445 0.574229 0.208703 11.00000 0.02022 0.00936 = 0.01604 -0.00025 0.00465 0.00300 AFIX 23 H31K 2 0.899826 0.580369 0.197120 11.00000 -1.20000 H31L 2 0.775413 0.532865 0.164099 11.00000 -1.20000 AFIX 0 C32F 1 0.827285 0.537374 0.300802 11.00000 0.04785 0.01771 = 0.02453 0.00930 0.01641 0.01247 AFIX 137 H32P 2 0.854611 0.476563 0.302338 11.00000 -1.50000 H32Q 2 0.749411 0.539335 0.316022 11.00000 -1.50000 H32R 2 0.882947 0.572181 0.344131 11.00000 -1.50000 AFIX 0 HKLF 5 REM zagid016 in P2(1) REM wR2 = 0.1401, GooF = S = 1.044, Restrained GooF = 1.043 for all data REM R1 = 0.0509 for 19754 Fo > 4sig(Fo) and 0.0677 for all 23264 data REM 866 parameters refined using 31 restraints END WGHT 0.0713 0.7419 REM Highest difference peak 0.533, deepest hole -0.442, 1-sigma level 0.065 Q1 1 0.4841 0.7081 0.3963 11.00000 0.05 0.53 Q2 1 0.1380 0.7113 0.0607 11.00000 0.05 0.52 Q3 1 0.1551 0.7809 0.1940 11.00000 0.05 0.50 Q4 1 0.4985 0.7813 0.5319 11.00000 0.05 0.49 Q5 1 0.5006 0.7082 0.5297 11.00000 0.05 0.48 Q6 1 0.8111 0.7166 0.7376 11.00000 0.05 0.46 Q7 1 0.8774 0.2768 0.4505 11.00000 0.05 0.45 Q8 1 0.5410 0.2798 0.1113 11.00000 0.05 0.45 Q9 1 1.0572 0.2056 0.4970 11.00000 0.05 0.45 Q10 1 0.1574 0.6327 0.0677 11.00000 0.05 0.44 Q11 1 0.7182 0.2075 0.1798 11.00000 0.05 0.44 Q12 1 0.4880 0.6324 0.3992 11.00000 0.05 0.44 Q13 1 0.1631 0.7085 0.1949 11.00000 0.05 0.43 Q14 1 0.6256 0.7067 0.1430 11.00000 0.05 0.41 Q15 1 0.8243 0.7880 0.8791 11.00000 0.05 0.41 Q16 1 0.4778 0.7941 0.3967 11.00000 0.05 0.41 Q17 1 0.7950 0.7780 0.2157 11.00000 0.05 0.41 Q18 1 0.7996 0.8583 0.2112 11.00000 0.05 0.40 Q19 1 0.9588 0.3177 0.4871 11.00000 0.05 0.39 Q20 1 0.8354 0.6355 0.7353 11.00000 0.05 0.39 Q21 1 0.6404 0.1694 0.1388 11.00000 0.05 0.39 Q22 1 0.1342 0.7975 0.0672 11.00000 0.05 0.39 Q23 1 1.0360 0.2791 0.5190 11.00000 0.05 0.38 Q24 1 0.8345 0.7093 0.8672 11.00000 0.05 0.38 Q25 1 0.6214 0.7836 0.1570 11.00000 0.05 0.38 Q26 1 0.4474 0.9185 0.3771 11.00000 0.05 0.36 Q27 1 0.5057 0.7380 0.6025 11.00000 0.05 0.36 Q28 1 0.8485 0.0113 0.5020 11.00000 0.05 0.36 Q29 1 0.5474 0.3578 0.1222 11.00000 0.05 0.35 Q30 1 0.7980 0.7969 0.7414 11.00000 0.05 0.35 Q31 1 0.8784 0.7441 0.2493 11.00000 0.05 0.35 Q32 1 0.5370 0.7425 0.1257 11.00000 0.05 0.34 Q33 1 0.7104 0.2855 0.1785 11.00000 0.05 0.34 Q34 1 0.8197 0.5251 0.1678 11.00000 0.05 0.34 Q35 1 0.6048 0.7087 0.1750 11.00000 0.05 0.34 Q36 1 0.8641 0.4314 0.4831 11.00000 0.05 0.33 Q37 1 0.8755 0.1974 0.4484 11.00000 0.05 0.32 Q38 1 0.2070 0.5574 0.0587 11.00000 0.05 0.32 Q39 1 0.8116 0.2465 0.2107 11.00000 0.05 0.32 Q40 1 0.1817 0.7407 0.2722 11.00000 0.05 0.31 ; _shelx_res_checksum 1403 _shelx_hkl_file ; 1 0 0 0.16127 0.04733 1 2 0 0 4.30236 0.19526 1 4 0 0 93.0234 1.83030 1 5 0 0 76.3193 1.66860 1 -2 0 8 477.955 8.30496 -2 6 0 0 477.955 8.30496 1 7 0 0 366.630 6.27119 1 8 0 0 84.3669 16.0046 1 -3 0 12 181.055 4.53732 -2 9 0 0 181.055 4.53732 1 10 0 0 285.565 5.59504 1 11 0 0 46.8816 1.94036 1 -4 0 16 434.345 7.61511 -2 12 0 0 434.345 7.61511 1 13 0 0 14.1558 0.98782 1 14 0 0 -4.0158 1.23425 1 -5 0 20 32.8457 2.57848 -2 15 0 0 32.8457 2.57848 1 16 0 0 3.78063 1.48694 1 17 0 0 35.0200 3.86074 1 -6 0 24 4.77452 4.99911 -2 18 0 0 4.77452 4.99911 1 1 1 0 2.66629 0.14889 1 -2 -1 0 6.18801 0.24089 1 2 1 0 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0 23 24.7786 2.64083 1 -6 0 23 25.5289 2.75627 1 17 0 1 124.049 6.28593 -2 -5 0 23 124.049 6.28593 1 -4 0 23 50.9132 3.88694 1 -3 0 23 34.8011 3.30092 1 16 0 5 45.5742 3.27918 -2 -2 0 23 45.5742 3.27918 1 -1 0 23 94.4674 4.61003 1 0 0 23 68.2445 3.94461 1 15 0 9 36.1967 3.79916 -2 1 0 23 36.1967 3.79916 1 2 0 23 -0.0240 1.81270 1 10 -1 -23 0.20738 2.47245 1 -10 1 23 1.24724 2.42000 1 9 -1 -23 28.7526 3.63324 1 -9 1 23 22.2769 3.95298 1 -18 1 3 149.677 7.45452 -2 8 -1 -23 149.677 7.45452 1 18 -1 -3 140.996 7.37194 -2 -8 1 23 140.996 7.37194 1 7 -1 -23 29.0343 3.29437 1 -7 1 23 27.6928 2.88015 1 6 -1 -23 77.1960 4.67081 1 -6 1 23 84.0605 4.05157 1 17 1 1 206.964 10.0169 -2 5 -1 -23 206.964 10.0169 1 -17 -1 -1 191.834 7.92558 -2 -5 1 23 191.834 7.92558 1 4 -1 -23 7.90844 2.16213 1 -4 1 23 9.05578 2.10760 1 3 -1 -23 122.146 5.11971 1 -3 1 23 121.447 4.65739 1 16 1 5 197.611 7.39789 -2 2 -1 -23 197.611 7.39789 1 -16 -1 -5 172.015 7.80059 -2 -2 1 23 172.015 7.80059 1 1 -1 -23 29.5147 2.55802 1 -1 1 23 30.8085 2.49225 1 0 -1 -23 96.4122 4.15074 1 0 1 23 110.888 4.53503 1 15 1 9 264.332 9.39726 -2 -1 -1 -23 264.332 9.39726 1 -15 -1 -9 264.223 8.25601 -2 1 1 23 264.223 8.25601 1 -2 -1 -23 9.14793 2.11903 1 2 1 23 7.98931 2.23591 1 10 -2 -23 5.95496 2.74006 1 -10 2 23 6.58833 2.49821 1 9 -2 -23 8.65391 2.68101 1 -9 2 23 1.35659 2.27205 1 -18 2 3 6.08410 3.68157 -2 8 -2 -23 6.08410 3.68157 1 18 -2 -3 9.63512 3.25236 -2 -8 2 23 9.63512 3.25236 1 7 -2 -23 26.0833 3.22449 1 -7 2 23 20.5202 2.41067 1 6 -2 -23 19.1138 2.72493 1 -6 2 23 11.5301 2.28107 1 17 2 1 106.839 7.11445 -2 5 -2 -23 106.839 7.11445 1 -17 -2 -1 108.786 5.85803 -2 -5 2 23 108.786 5.85803 1 4 -2 -23 52.3263 3.36831 1 -4 2 23 47.4818 2.73948 1 16 2 4 37.3339 6.85633 -2 3 -2 -23 37.3339 6.85633 1 -3 2 23 22.4458 2.46111 1 16 2 5 62.0608 4.74277 -2 2 -2 -23 62.0608 4.74277 1 -16 -2 -5 50.4560 4.51382 -2 -2 2 23 50.4560 4.51382 1 1 -2 -23 29.3931 2.67223 1 -1 2 23 28.8583 2.71946 1 15 2 8 53.8322 6.75747 -2 0 -2 -23 53.8322 6.75747 1 0 2 23 49.6704 3.68636 1 15 2 9 3.61720 2.04360 -2 -1 -2 -23 3.61720 2.04360 1 -15 -2 -9 3.98539 2.55782 -2 1 2 23 3.98539 2.55782 1 -2 -2 -23 1.15897 1.58726 1 2 2 23 4.84613 2.14451 1 -18 3 4 24.7311 10.0017 -2 9 -3 -23 24.7311 10.0017 1 -9 3 23 16.2762 3.05945 1 -18 3 3 149.941 7.32702 -2 8 -3 -23 149.941 7.32702 1 18 -3 -3 130.769 5.91711 -2 -8 3 23 130.769 5.91711 1 7 -3 -23 26.7001 2.84692 1 18 -3 -2 49.4929 13.0357 -2 -7 3 23 49.4929 13.0357 1 6 -3 -23 22.0608 3.10653 1 -6 3 23 21.5832 2.49306 1 17 3 1 94.2204 5.43785 -2 5 -3 -23 94.2204 5.43785 1 -17 -3 -1 95.7170 4.80973 -2 -5 3 23 95.7170 4.80973 1 4 -3 -23 8.99010 1.84743 1 -4 3 23 9.23223 1.60278 1 16 3 4 8.63556 5.83869 -2 3 -3 -23 8.63556 5.83869 1 -3 3 23 12.1067 1.78384 1 16 3 5 16.7280 4.28400 -2 2 -3 -23 16.7280 4.28400 1 -16 -3 -5 25.0541 2.67909 -2 -2 3 23 25.0541 2.67909 1 1 -3 -23 6.29805 1.76512 1 -1 3 23 7.94530 2.00317 1 0 -3 -23 0.34280 1.44217 1 0 3 23 0.55669 1.92578 1 15 3 9 17.3344 2.32700 -2 -1 -3 -23 17.3344 2.32700 1 -15 -3 -9 20.8191 4.05938 -2 1 3 23 20.8191 4.05938 1 -2 -3 -23 6.32448 1.96745 1 2 3 23 5.18250 2.09440 1 9 -4 -23 2.56261 2.64159 1 18 -4 -4 13.0554 7.77570 -2 -9 4 23 13.0554 7.77570 1 -18 4 3 4.94644 3.56446 -2 8 -4 -23 4.94644 3.56446 1 18 -4 -3 0.82670 2.76964 -2 -8 4 23 0.82670 2.76964 1 7 -4 -23 9.80058 2.55667 1 -7 4 23 9.07109 2.38762 1 6 -4 -23 2.69368 2.56527 1 -17 -4 0 1.94168 7.33003 -2 -6 4 23 1.94168 7.33003 1 17 4 1 42.2367 3.43055 -2 5 -4 -23 42.2367 3.43055 1 -17 -4 -1 42.0094 2.78206 -2 -5 4 23 42.0094 2.78206 1 4 -4 -23 1.63343 1.63781 1 -4 4 23 3.27123 1.54662 1 16 4 4 1.15288 5.26334 -2 3 -4 -23 1.15288 5.26334 1 -3 4 23 -1.0932 1.50791 1 16 4 5 23.8861 2.95380 -2 2 -4 -23 23.8861 2.95380 1 -16 -4 -5 32.8671 2.43924 -2 -2 4 23 32.8671 2.43924 1 1 -4 -23 3.88731 1.61391 1 -1 4 23 3.55085 2.18212 1 0 -4 -23 6.10497 1.63637 1 0 4 23 5.18880 2.42432 1 15 4 9 27.3012 3.32992 -2 -1 -4 -23 27.3012 3.32992 1 -15 -4 -9 26.7274 3.58292 -2 1 4 23 26.7274 3.58292 1 -2 -4 -23 3.73020 1.70536 1 2 4 23 2.27786 2.12710 1 9 -5 -23 11.8960 3.88869 1 18 -5 -4 25.4515 8.70261 -2 -9 5 23 25.4515 8.70261 1 -18 5 3 16.1529 4.93714 -2 8 -5 -23 16.1529 4.93714 1 18 -5 -3 11.0043 2.99282 -2 -8 5 23 11.0043 2.99282 1 7 -5 -23 6.45346 2.19221 1 18 -5 -2 1.57829 8.35024 -2 -7 5 23 1.57829 8.35024 1 6 -5 -23 -0.0088 1.72162 1 -6 5 23 1.72065 1.50628 1 17 5 1 -2.4730 3.31988 -2 5 -5 -23 -2.4730 3.31988 1 -17 -5 -1 0.96692 2.26288 -2 -5 5 23 0.96692 2.26288 1 4 -5 -23 2.57671 1.57634 1 -4 5 23 7.03620 2.09932 1 16 5 4 -4.8656 4.96700 -2 3 -5 -23 -4.8656 4.96700 1 -3 5 23 -3.0391 1.33857 1 16 5 5 3.40227 2.46700 -2 2 -5 -23 3.40227 2.46700 1 -16 -5 -5 4.28754 2.29254 -2 -2 5 23 4.28754 2.29254 1 1 -5 -23 4.91121 1.77067 1 -1 5 23 11.4347 2.50992 1 0 -5 -23 2.06370 1.71419 1 0 5 23 1.86046 2.15086 1 15 5 9 9.67700 2.48890 -2 -1 -5 -23 9.67700 2.48890 1 -15 -5 -9 15.2210 3.78961 -2 1 5 23 15.2210 3.78961 1 -18 6 3 6.12964 6.45297 -2 8 -6 -23 6.12964 6.45297 1 18 -6 -3 1.61212 3.24456 -2 -8 6 23 1.61212 3.24456 1 7 -6 -23 8.22536 2.43260 1 18 -6 -2 -11.593 7.89708 -2 -7 6 23 -11.593 7.89708 1 6 -6 -23 -2.5725 1.66854 1 -17 -6 0 -0.1426 3.58073 -2 -6 6 23 -0.1426 3.58073 1 17 6 1 12.3930 5.44667 -2 5 -6 -23 12.3930 5.44667 1 -17 -6 -1 10.7088 1.90319 -2 -5 6 23 10.7088 1.90319 1 4 -6 -23 10.6837 2.00709 1 -4 6 23 14.1989 1.97440 1 16 6 4 7.70943 5.94815 -2 3 -6 -23 7.70943 5.94815 1 -3 6 23 6.08755 1.72387 1 16 6 5 12.0759 2.60734 -2 2 -6 -23 12.0759 2.60734 1 -16 -6 -5 11.0833 2.21864 -2 -2 6 23 11.0833 2.21864 1 1 -6 -23 0.44923 1.74628 1 -1 6 23 0.85978 1.62283 1 0 -6 -23 4.29998 1.80378 1 0 6 23 2.74409 2.51815 1 15 6 9 129.963 6.37536 -2 -1 -6 -23 129.963 6.37536 1 -15 -6 -9 139.028 8.65555 -2 1 6 23 139.028 8.65555 1 7 -7 -23 55.3767 4.56886 1 -7 7 23 53.8255 3.60560 1 6 -7 -23 1.31119 2.96120 1 -17 -7 0 -1.1975 7.41844 -2 -6 7 23 -1.1975 7.41844 1 17 7 1 9.83446 5.28936 -2 5 -7 -23 9.83446 5.28936 1 -17 -7 -1 5.04587 1.79216 -2 -5 7 23 5.04587 1.79216 1 4 -7 -23 2.55439 1.77743 1 -4 7 23 1.45142 1.42192 1 16 7 4 16.6200 6.51501 -2 3 -7 -23 16.6200 6.51501 1 -3 7 23 4.71077 1.67430 1 16 7 5 13.4346 3.67033 -2 2 -7 -23 13.4346 3.67033 1 -16 -7 -5 -0.2548 1.97597 -2 -2 7 23 -0.2548 1.97597 1 1 -7 -23 16.8009 2.32204 1 -1 7 23 9.96481 1.83468 1 0 -7 -23 1.69431 2.30252 1 0 7 23 -1.6709 2.80465 1 6 -8 -23 2.02859 2.56230 1 -17 -8 0 -0.4683 7.53553 -2 -6 8 23 -0.4683 7.53553 1 17 8 1 15.5055 5.69239 -2 5 -8 -23 15.5055 5.69239 1 -17 -8 -1 10.4074 2.14738 -2 -5 8 23 10.4074 2.14738 1 4 -8 -23 6.16275 1.90094 1 -4 8 23 1.84260 1.51120 1 16 8 4 -7.3705 4.35826 -2 3 -8 -23 -7.3705 4.35826 1 -16 -8 -4 2.50928 7.23456 -2 -3 8 23 2.50928 7.23456 1 16 8 5 50.2777 3.70671 -2 2 -8 -23 50.2777 3.70671 1 -16 -8 -5 38.2471 2.74986 -2 -2 8 23 38.2471 2.74986 1 1 -8 -23 8.72983 2.08482 1 -1 8 23 6.18591 2.00824 1 -8 0 24 4.83993 3.07073 1 -7 0 24 1.40942 2.66221 1 18 0 0 3.34363 2.81940 -2 -6 0 24 3.34363 2.81940 1 -5 0 24 10.8418 2.53022 1 -4 0 24 11.9867 2.48730 1 17 0 4 3.00501 2.69241 -2 -3 0 24 3.00501 2.69241 1 -2 0 24 1.99076 1.94678 1 -1 0 24 5.83750 1.76785 1 16 0 8 11.9102 7.61525 -2 0 0 24 11.9102 7.61525 1 7 -1 -24 25.9598 3.83783 1 -7 1 24 27.9414 3.28378 1 18 1 0 90.7442 5.14010 -2 6 -1 -24 90.7442 5.14010 1 -18 -1 0 88.1974 4.08429 -2 -6 1 24 88.1974 4.08429 1 5 -1 -24 13.4486 2.64069 1 -5 1 24 11.5726 2.24773 1 17 1 3 38.9285 8.48408 -2 4 -1 -24 38.9285 8.48408 1 -4 1 24 16.5847 2.46377 1 17 1 4 157.563 6.28533 -2 3 -1 -24 157.563 6.28533 1 -17 -1 -4 147.471 6.06230 -2 -3 1 24 147.471 6.06230 1 2 -1 -24 6.70868 2.16478 1 -2 1 24 8.43398 1.89776 1 1 -1 -24 10.8769 2.04698 1 -1 1 24 7.42565 2.28966 1 16 1 8 10.0003 2.63553 -2 0 -1 -24 10.0003 2.63553 1 -16 -1 -8 8.79976 7.06498 -2 0 1 24 8.79976 7.06498 1 7 -2 -24 11.9565 3.38377 1 -7 2 24 20.7910 3.19356 1 18 2 0 85.1695 4.85759 -2 6 -2 -24 85.1695 4.85759 1 -18 -2 0 82.9415 3.95494 -2 -6 2 24 82.9415 3.95494 1 5 -2 -24 34.2661 3.78578 1 -5 2 24 35.8493 3.16061 1 17 2 3 67.7149 9.59852 -2 4 -2 -24 67.7149 9.59852 1 -17 -2 -3 42.5843 8.80599 -2 -4 2 24 42.5843 8.80599 1 17 2 4 126.553 5.58044 -2 3 -2 -24 126.553 5.58044 1 -17 -2 -4 123.336 4.99332 -2 -3 2 24 123.336 4.99332 1 2 -2 -24 17.2659 2.20481 1 -2 2 24 13.8721 1.98143 1 1 -2 -24 8.04035 1.91480 1 -1 2 24 13.5057 3.19233 1 0 -2 -24 121.429 4.89749 1 0 2 24 89.3593 9.41997 1 7 -3 -24 -4.1180 2.57174 1 -7 3 24 6.45167 2.61140 1 18 3 0 8.53652 3.21051 -2 6 -3 -24 8.53652 3.21051 1 -18 -3 0 8.34045 2.68983 -2 -6 3 24 8.34045 2.68983 1 5 -3 -24 41.6810 4.06081 1 -5 3 24 41.4154 3.32168 1 17 3 3 5.38930 6.81637 -2 4 -3 -24 5.38930 6.81637 1 -17 -3 -3 16.7467 6.55696 -2 -4 3 24 16.7467 6.55696 1 17 3 4 3.26293 2.33907 -2 3 -3 -24 3.26293 2.33907 1 -17 -3 -4 2.31165 1.90507 -2 -3 3 24 2.31165 1.90507 1 2 -3 -24 21.6077 2.35318 1 -2 3 24 21.1044 2.30646 1 16 3 7 5.04242 5.34237 -2 1 -3 -24 5.04242 5.34237 1 -1 3 24 1.90729 2.18480 1 18 4 0 7.74278 5.74988 -2 6 -4 -24 7.74278 5.74988 1 -18 -4 0 7.75105 2.59844 -2 -6 4 24 7.75105 2.59844 1 5 -4 -24 1.02724 2.25178 1 -5 4 24 1.42262 1.95998 1 17 4 3 -0.0321 6.14489 -2 4 -4 -24 -0.0321 6.14489 1 -17 -4 -3 0.00264 3.88612 -2 -4 4 24 0.00264 3.88612 1 17 4 4 42.4249 3.49918 -2 3 -4 -24 42.4249 3.49918 1 -17 -4 -4 42.2014 2.99823 -2 -3 4 24 42.2014 2.99823 1 2 -4 -24 -0.4713 1.60568 1 -2 4 24 3.45811 1.82259 1 16 4 7 28.0768 6.50494 -2 1 -4 -24 28.0768 6.50494 1 -1 4 24 21.6120 3.99003 1 5 -5 -24 3.23887 1.88829 1 -5 5 24 1.84731 1.57674 1 17 5 3 -1.9346 6.08336 -2 4 -5 -24 -1.9346 6.08336 1 -4 5 24 3.96706 1.59083 1 17 5 4 1.41917 2.61274 -2 3 -5 -24 1.41917 2.61274 1 -17 -5 -4 -1.4538 2.21462 -2 -3 5 24 -1.4538 2.21462 1 2 -5 -24 8.00849 1.93384 1 -2 5 24 5.72173 2.02531 1 0 0 0 0.00 0.00 0 _chemical_formula_moiety 'C7 H8 N4 O4' _exptl_crystal_description prism _exptl_crystal_colour colorless _cell_measurement_reflns_used 52924 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 34.95 _exptl_absorpt_correction_T_min 0.504965 _exptl_absorpt_correction_T_max 0.841176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ) SADABS-2016/2 (Stalke et al., 2015) Equivalent reflections defined according to point group 2 Mean and maximum errors in direction cosine check function = 0.000 0.002 Restraint esd for equal adjacent scale factors = 0.0090 Maximum odd and even orders for spherical harmonics = 1 4 Parameter refinement for twin component 1 ------------------------------------------ 63575 single and 0 composite reflections used for parameter fitting Effective data to parameter ratio = 18.43 wR2(int) = 0.1535 (selected reflections only, before parameter refinement) wR2(int) = 0.0776 (selected reflections only, after parameter refinement) Parameter refinement for twin component 2 ------------------------------------------ 53895 single and 0 composite reflections used for parameter fitting Effective data to parameter ratio = 15.45 wR2(int) = 0.1906 (selected reflections only, before parameter refinement) wR2(int) = 0.0842 (selected reflections only, after parameter refinement) ------------------------------------------ 219897 total and 39794 unique reflections after rejecting pathological cases Reflections rejected for which |I-|/su > 3.00 Where: su^2 = sigma(I)^2 + ( 0.04000 )^2 (sigma(I) from SAINT) 216765 total and 39779 unique reflections left after |I-|/su test g = 0.0364 gave best error model; g set to 0.0364 for further calculations Statistics for singles of twin component 1 ------------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.1103 0.107 - 0.171 1.139 - 1.237 0.977 13307 9237 2 33.6 0.1332 0.063 - 0.176 1.139 - 1.229 1.008 13099 8420 3 33.6 0.0999 0.088 - 0.166 1.139 - 1.233 0.964 13394 9487 4 33.6 0.1159 0.078 - 0.149 1.139 - 1.239 0.983 13006 8922 5 33.6 0.1410 0.067 - 0.183 1.139 - 1.235 0.995 12879 8248 6 33.6 0.1195 0.090 - 0.156 1.139 - 1.229 1.015 13437 8855 7 0.0 0.2070 0.123 - 0.370 1.139 - 1.239 1.074 9691 5131 All scans 0.1330 0.063 - 0.370 1.139 - 1.239 1.002 88813 58300 Statistics for singles of twin component 2 ------------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.2150 0.017 - 0.070 1.535 - 1.897 0.977 13257 6603 2 33.6 0.1241 0.008 - 0.023 1.535 - 1.896 1.008 13013 8509 3 33.6 0.2017 0.017 - 0.063 1.554 - 1.897 0.964 13411 6993 4 33.6 0.1627 0.011 - 0.033 1.536 - 1.897 0.983 12857 7511 5 33.6 0.1587 0.009 - 0.031 1.535 - 1.897 0.995 12853 7753 6 33.6 0.2461 0.013 - 0.063 1.535 - 1.897 1.015 13351 6116 7 0.0 0.2740 0.028 - 0.069 1.535 - 1.888 1.074 9746 4280 All scans 0.1973 0.008 - 0.070 1.535 - 1.897 1.002 88488 47765 Statistics for all composite reflections ---------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.0491 0.036 - 0.116 1.286 - 1.616 0.977 5866 5179 2 33.6 0.0714 0.030 - 0.134 1.304 - 1.618 1.008 5566 4759 3 33.6 0.0475 0.048 - 0.127 1.334 - 1.605 0.964 5747 5192 4 33.6 0.0555 0.025 - 0.111 1.286 - 1.699 0.983 6100 5294 5 33.6 0.0533 0.029 - 0.133 1.308 - 1.628 0.995 6296 5410 6 33.6 0.0562 0.049 - 0.128 1.298 - 1.645 1.015 5640 4997 7 0.0 0.0579 0.067 - 0.244 1.337 - 1.574 1.074 4249 3755 All scans 0.0556 0.025 - 0.244 1.286 - 1.699 1.002 39464 34586 Statistics for all single and composite reflections --------------------------------------------------- Scan 2-theta R(int) Incid. factors Diffr. factors K Total I>2sig(I) 1 33.6 0.0676 0.017 - 0.171 1.139 - 1.897 0.977 32430 21019 2 33.6 0.0888 0.008 - 0.176 1.139 - 1.896 1.008 31678 21688 3 33.6 0.0640 0.017 - 0.166 1.139 - 1.897 0.964 32552 21672 4 33.6 0.0718 0.011 - 0.149 1.139 - 1.897 0.983 31963 21727 5 33.6 0.0742 0.009 - 0.183 1.139 - 1.897 0.995 32028 21411 6 33.6 0.0762 0.013 - 0.156 1.139 - 1.897 1.015 32428 19968 7 0.0 0.0857 0.028 - 0.370 1.139 - 1.888 1.074 23686 13166 All scans 0.0759 0.008 - 0.370 1.139 - 1.897 1.002 216765 140651 su = K * Sqrt[ sigma^2(I) + (g)^2 ] where sigma(I) is estimated by SAINT Rint = 0.0749 for all 216672 observations and Rint = 0.0594 for all 110123 observations with I > 3sigma(I) HKLF 5 dataset constructed from all observations involving domain 1 31990 Corrected reflections written to file hkl Reflections merged according to point-group 2 Single reflections that also occur in composites omitted Racemic twinning not included for all components Second component not inverted relative to first Minimum and maximum apparent transmission: 0.504965 0.841176 Additional spherical absorption correction applied with mu*r = 0.0300 ) loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -4.00 1.00 2.00 0.2140 -3.00 1.00 3.00 0.1860 -3.00 2.00 3.00 0.1780 -3.00 3.00 4.00 0.1750 -2.00 0.00 3.00 0.1980 -1.00 0.00 3.00 0.2670 -1.00 -4.00 1.00 0.1060 -1.00 -4.00 0.00 0.1090 -1.00 -4.00 -1.00 0.1170 -1.00 -3.00 -3.00 0.1510 -1.00 -1.00 -2.00 0.1800 -1.00 -1.00 0.00 0.1950 -1.00 -1.00 1.00 0.1760 -1.00 -1.00 2.00 0.2030 0.00 1.00 -3.00 0.1700 0.00 1.00 0.00 0.0840 0.00 -1.00 0.00 0.0490 0.00 -4.00 -1.00 0.0790 0.00 -1.00 -2.00 0.1700 1.00 -4.00 1.00 0.1190 1.00 0.00 -3.00 0.2710 1.00 -4.00 0.00 0.0970 2.00 -1.00 1.00 0.1730 2.00 -2.00 1.00 0.1610 3.00 -3.00 -1.00 0.2320 3.00 4.00 1.00 0.1780 4.00 3.00 2.00 0.1620 _chemical_absolute_configuration ad _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_type MoK\a _diffrn_measurement_device 'four-circle diffractometer' _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD plate' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \f scans' _computing_data_collection 'APEX4 v2021.10-0 (Bruker AXS)' _computing_cell_refinement 'APEX4 v2021.10-0 (Bruker AXS)' _computing_data_reduction 'APEX4 v2021.10-0 (Bruker AXS)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_molecular_graphics ) WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ) _computing_publication_material ) WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); Olex2 (Dolomanov et al., 2009) ) _refine_special_details ) Refined as a 2-component twin. Component 2 rotated by -179.96\% around [1.00 0.00 -1.00] (reciprocal) or [1.00 0.00 -0.50] (direct). Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ) CELL 0.71073 11.60920 15.27060 15.29830 90.0000 102.0641 90.0000 ZERR 12.00 0.00050 0.00070 0.00070 0.0000 0.0010 0.0000 LATT -1 SYMM - X, 1/2 + Y, - Z ; _shelx_hkl_checksum 70187 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 O1A O 0.55460(18) 0.46819(12) 0.16186(15) 0.0214(4) Uani 1 1 d . . . . . O3A O 0.41345(16) 0.22821(12) 0.05263(13) 0.0165(3) Uani 1 1 d . . . . . O51A O 0.90682(19) 0.32178(15) 0.26203(17) 0.0278(4) Uani 1 1 d . . . . . O52A O 0.92094(17) 0.18125(13) 0.24845(14) 0.0203(4) Uani 1 1 d . . . . . N1A N 0.40460(19) 0.40591(14) 0.06358(15) 0.0169(4) Uani 1 1 d D . . . . H1AA H 0.379(3) 0.3596(18) 0.034(2) 0.030(10) Uiso 1 1 d D . . . . H1AB H 0.356(3) 0.4516(16) 0.059(2) 0.015(8) Uiso 1 1 d D . . . . N2A N 0.68387(18) 0.32104(13) 0.17316(14) 0.0127(3) Uani 1 1 d . . . . . N3A N 0.58595(17) 0.16065(13) 0.11569(13) 0.0129(3) Uani 1 1 d . . . . . N5A N 0.86551(19) 0.25076(15) 0.23599(14) 0.0156(4) Uani 1 1 d . . . . . C1A C 0.5093(2) 0.40409(15) 0.11916(16) 0.0138(4) Uani 1 1 d . . . . . C2A C 0.5744(2) 0.31745(14) 0.12975(15) 0.0118(4) Uani 1 1 d . . . . . C3A C 0.5154(2) 0.23538(15) 0.09614(15) 0.0121(4) Uani 1 1 d . . . . . C4A C 0.6978(2) 0.16520(15) 0.16195(15) 0.0135(4) Uani 1 1 d . . . . . H4A H 0.743906 0.113724 0.176076 0.016 Uiso 1 1 calc R U . . . C5A C 0.7435(2) 0.24574(16) 0.18809(15) 0.0126(4) Uani 1 1 d . . . . . C31A C 0.5362(2) 0.07324(14) 0.08715(16) 0.0159(4) Uani 1 1 d . . . . . H31A H 0.598628 0.035566 0.071932 0.019 Uiso 1 1 calc R U . . . H31B H 0.473069 0.079548 0.032970 0.019 Uiso 1 1 calc R U . . . C32A C 0.4868(3) 0.03049(17) 0.1605(2) 0.0282(6) Uani 1 1 d . . . . . H32A H 0.468122 -0.030903 0.144989 0.042 Uiso 1 1 calc R U . . . H32B H 0.415025 0.061227 0.167113 0.042 Uiso 1 1 calc R U . . . H32C H 0.545164 0.033406 0.216821 0.042 Uiso 1 1 calc R U . . . O1B O 0.87518(17) 0.46071(11) 0.51735(13) 0.0170(3) Uani 1 1 d . . . . . O3B O 0.73864(17) 0.22455(12) 0.39167(14) 0.0180(3) Uani 1 1 d . . . . . O51B O 1.23279(17) 0.31911(14) 0.59767(14) 0.0203(4) Uani 1 1 d . . . . . O52B O 1.25542(17) 0.18290(13) 0.56420(14) 0.0207(4) Uani 1 1 d . . . . . N1B N 0.71766(18) 0.39623(13) 0.42780(15) 0.0165(4) Uani 1 1 d D . . . . H1BA H 0.693(3) 0.3488(17) 0.399(2) 0.026(9) Uiso 1 1 d D . . . . H1BB H 0.672(3) 0.4434(15) 0.422(2) 0.017(8) Uiso 1 1 d D . . . . N2B N 1.00775(18) 0.31677(13) 0.51455(13) 0.0124(3) Uani 1 1 d . . . . . N3B N 0.91293(17) 0.15742(13) 0.45030(13) 0.0124(3) Uani 1 1 d . . . . . N5B N 1.19486(19) 0.24941(15) 0.56408(14) 0.0146(3) Uani 1 1 d . . . . . C1B C 0.8281(2) 0.39695(14) 0.47430(15) 0.0123(4) Uani 1 1 d . . . . . C2B C 0.8968(2) 0.31281(14) 0.47481(15) 0.0113(3) Uani 1 1 d . . . . . C3B C 0.8406(2) 0.23165(15) 0.43552(15) 0.0125(4) Uani 1 1 d . . . . . C4B C 1.02643(19) 0.16263(16) 0.49253(15) 0.0126(4) Uani 1 1 d . . . . . H4B H 1.074571 0.111788 0.502263 0.015 Uiso 1 1 calc R U . . . C5B C 1.0710(2) 0.24307(16) 0.52117(15) 0.0123(4) Uani 1 1 d . . . . . C31B C 0.8622(2) 0.07098(14) 0.41862(16) 0.0158(4) Uani 1 1 d . . . . . H31C H 0.926656 0.030545 0.412324 0.019 Uiso 1 1 calc R U . . . H31D H 0.809887 0.077943 0.359028 0.019 Uiso 1 1 calc R U . . . C32B C 0.7932(4) 0.0319(2) 0.4822(3) 0.0412(9) Uani 1 1 d . . . . . H32D H 0.764252 -0.026151 0.460780 0.062 Uiso 1 1 calc R U . . . H32E H 0.726266 0.069933 0.485572 0.062 Uiso 1 1 calc R U . . . H32F H 0.844213 0.026500 0.541725 0.062 Uiso 1 1 calc R U . . . O1C O 0.21839(18) 0.52722(12) 0.08042(13) 0.0188(3) Uani 1 1 d . . . . . O3C O 0.09462(17) 0.76363(11) -0.04714(12) 0.0151(3) Uani 1 1 d . . . . . O51C O 0.22017(19) 0.66899(14) 0.34967(13) 0.0219(4) Uani 1 1 d . . . . . O52C O 0.1839(2) 0.80821(14) 0.35522(13) 0.0216(4) Uani 1 1 d . . . . . N1C N 0.1198(2) 0.58620(14) -0.04945(14) 0.0172(4) Uani 1 1 d D . . . . H1CA H 0.075(3) 0.630(2) -0.072(3) 0.034(11) Uiso 1 1 d D . . . . H1CB H 0.129(4) 0.5361(17) -0.077(3) 0.032(11) Uiso 1 1 d D . . . . N2C N 0.17637(17) 0.67136(13) 0.17232(13) 0.0118(3) Uani 1 1 d . . . . . N3C N 0.12359(17) 0.83101(12) 0.08832(12) 0.0113(3) Uani 1 1 d . . . . . N5C N 0.19285(19) 0.74000(15) 0.31401(14) 0.0149(3) Uani 1 1 d . . . . . C1C C 0.1667(2) 0.58945(14) 0.03780(16) 0.0131(4) Uani 1 1 d . . . . . C2C C 0.15382(19) 0.67507(13) 0.08473(15) 0.0103(3) Uani 1 1 d . . . . . C3C C 0.1223(2) 0.75683(14) 0.03487(15) 0.0108(3) Uani 1 1 d . . . . . C4C C 0.14747(19) 0.82647(15) 0.17816(15) 0.0120(4) Uani 1 1 d . . . . . H4C H 0.147715 0.877644 0.213517 0.014 Uiso 1 1 calc R U . . . C5C C 0.1713(2) 0.74622(15) 0.21701(15) 0.0120(4) Uani 1 1 d . . . . . C31C C 0.0957(2) 0.91723(14) 0.04411(15) 0.0160(4) Uani 1 1 d . . . . . H31E H 0.074412 0.959193 0.087481 0.019 Uiso 1 1 calc R U . . . H31F H 0.026745 0.910878 -0.005972 0.019 Uiso 1 1 calc R U . . . C32C C 0.1986(3) 0.95324(19) 0.0088(3) 0.0352(7) Uani 1 1 d . . . . . H32G H 0.218458 0.912629 -0.035442 0.053 Uiso 1 1 calc R U . . . H32H H 0.266801 0.960130 0.058294 0.053 Uiso 1 1 calc R U . . . H32I H 0.177290 1.010264 -0.019356 0.053 Uiso 1 1 calc R U . . . O1D O 0.52043(19) 0.51311(12) 0.42454(13) 0.0209(4) Uani 1 1 d . . . . . O3D O 0.45575(18) 0.75631(12) 0.29167(12) 0.0165(3) Uani 1 1 d . . . . . O51D O 0.5345(2) 0.66601(15) 0.68890(15) 0.0279(5) Uani 1 1 d . . . . . O52D O 0.51877(19) 0.80758(14) 0.69110(13) 0.0210(4) Uani 1 1 d . . . . . N1D N 0.4679(2) 0.57920(14) 0.28991(15) 0.0194(4) Uani 1 1 d D . . . . H1DA H 0.436(4) 0.6268(19) 0.266(3) 0.036(12) Uiso 1 1 d D . . . . H1DB H 0.485(4) 0.5300(17) 0.264(3) 0.032(11) Uiso 1 1 d D . . . . N2D N 0.49940(18) 0.66395(13) 0.51118(14) 0.0122(3) Uani 1 1 d . . . . . N3D N 0.50032(17) 0.82407(12) 0.42715(12) 0.0120(3) Uani 1 1 d . . . . . N5D N 0.52029(19) 0.73701(15) 0.65147(14) 0.0161(4) Uani 1 1 d . . . . . C1D C 0.4919(2) 0.57917(14) 0.37856(16) 0.0138(4) Uani 1 1 d . . . . . C2D C 0.48679(19) 0.66695(14) 0.42415(15) 0.0114(4) Uani 1 1 d . . . . . C3D C 0.4784(2) 0.74932(14) 0.37365(15) 0.0121(4) Uani 1 1 d . . . . . C4D C 0.51240(19) 0.82059(15) 0.51612(15) 0.0125(3) Uani 1 1 d . . . . . H4D H 0.523792 0.872432 0.551196 0.015 Uiso 1 1 calc R U . . . C5D C 0.5079(2) 0.74051(15) 0.55502(15) 0.0128(4) Uani 1 1 d . . . . . C31D C 0.5079(2) 0.90945(14) 0.38282(15) 0.0156(4) Uani 1 1 d . . . . . H31G H 0.551215 0.901750 0.334077 0.019 Uiso 1 1 calc R U . . . H31H H 0.552865 0.951065 0.426658 0.019 Uiso 1 1 calc R U . . . C32D C 0.3882(2) 0.94734(17) 0.3449(2) 0.0264(5) Uani 1 1 d . . . . . H32J H 0.349765 0.912799 0.292932 0.040 Uiso 1 1 calc R U . . . H32K H 0.396841 1.008060 0.326487 0.040 Uiso 1 1 calc R U . . . H32L H 0.340165 0.945851 0.390423 0.040 Uiso 1 1 calc R U . . . O1E O 0.88740(17) 0.53071(11) 0.76181(13) 0.0169(3) Uani 1 1 d . . . . . O3E O 0.77572(17) 0.77017(11) 0.63280(12) 0.0159(3) Uani 1 1 d . . . . . O51E O 0.87664(19) 0.66988(14) 1.02861(13) 0.0205(4) Uani 1 1 d . . . . . O52E O 0.84463(19) 0.80967(13) 1.03502(13) 0.0205(4) Uani 1 1 d . . . . . N1E N 0.8091(2) 0.59471(14) 0.62926(14) 0.0159(4) Uani 1 1 d D . . . . H1EA H 0.769(3) 0.6394(19) 0.606(3) 0.031(11) Uiso 1 1 d D . . . . H1EB H 0.820(4) 0.5441(17) 0.603(3) 0.036(11) Uiso 1 1 d D . . . . N2E N 0.84102(18) 0.67425(12) 0.85156(13) 0.0119(3) Uani 1 1 d . . . . . N3E N 0.79224(17) 0.83507(12) 0.76889(13) 0.0121(3) Uani 1 1 d . . . . . N5E N 0.85130(18) 0.74138(15) 0.99306(14) 0.0143(3) Uani 1 1 d . . . . . C1E C 0.8433(2) 0.59465(14) 0.71756(15) 0.0119(4) Uani 1 1 d . . . . . C2E C 0.8250(2) 0.67947(13) 0.76423(15) 0.0107(3) Uani 1 1 d . . . . . C3E C 0.7962(2) 0.76198(14) 0.71451(15) 0.0116(4) Uani 1 1 d . . . . . C4E C 0.81088(19) 0.82893(14) 0.85826(15) 0.0115(3) Uani 1 1 d . . . . . H4E H 0.809401 0.879577 0.894078 0.014 Uiso 1 1 calc R U . . . C5E C 0.8320(2) 0.74825(15) 0.89641(14) 0.0120(4) Uani 1 1 d . . . . . C31E C 0.7722(2) 0.92317(14) 0.72775(16) 0.0157(4) Uani 1 1 d . . . . . H31I H 0.727737 0.959709 0.762728 0.019 Uiso 1 1 calc R U . . . H31J H 0.724726 0.917785 0.666211 0.019 Uiso 1 1 calc R U . . . C32E C 0.8882(3) 0.96660(17) 0.7252(2) 0.0278(6) Uani 1 1 d . . . . . H32M H 0.926826 0.935120 0.683476 0.042 Uiso 1 1 calc R U . . . H32N H 0.938896 0.965458 0.785118 0.042 Uiso 1 1 calc R U . . . H32O H 0.874194 1.027451 0.705514 0.042 Uiso 1 1 calc R U . . . O1F O 0.78435(18) 0.96760(12) 0.16593(14) 0.0196(4) Uani 1 1 d . . . . . O3F O 0.92801(16) 0.72806(12) 0.27007(13) 0.0176(3) Uani 1 1 d . . . . . O51F O 0.42407(18) 0.82128(14) 0.08321(15) 0.0230(4) Uani 1 1 d . . . . . O52F O 0.41508(17) 0.67980(13) 0.09170(14) 0.0200(4) Uani 1 1 d . . . . . N1F N 0.93314(19) 0.90722(13) 0.26689(15) 0.0158(4) Uani 1 1 d D . . . . H1FA H 0.959(4) 0.861(2) 0.298(3) 0.040(12) Uiso 1 1 d D . . . . H1FB H 0.980(3) 0.9537(16) 0.271(2) 0.016(8) Uiso 1 1 d D . . . . N2F N 0.65141(17) 0.82181(13) 0.16398(13) 0.0118(3) Uani 1 1 d . . . . . N3F N 0.75990(17) 0.66087(13) 0.19765(13) 0.0123(3) Uani 1 1 d . . . . . N5F N 0.46882(19) 0.75009(15) 0.10471(14) 0.0143(3) Uani 1 1 d . . . . . C1F C 0.8283(2) 0.90450(14) 0.21116(16) 0.0126(4) Uani 1 1 d . . . . . C2F C 0.76327(19) 0.81832(14) 0.20197(15) 0.0111(3) Uani 1 1 d . . . . . C3F C 0.8259(2) 0.73567(15) 0.22774(15) 0.0119(4) Uani 1 1 d . . . . . C4F C 0.6448(2) 0.66493(15) 0.15991(16) 0.0136(4) Uani 1 1 d . . . . . H4F H 0.600275 0.613230 0.142751 0.016 Uiso 1 1 calc R U . . . C5F C 0.5935(2) 0.74581(15) 0.14691(15) 0.0118(3) Uani 1 1 d . . . . . C31F C 0.8194(2) 0.57423(14) 0.20870(15) 0.0151(4) Uani 1 1 d . . . . . H31K H 0.899826 0.580369 0.197120 0.018 Uiso 1 1 calc R U . . . H31L H 0.775413 0.532865 0.164099 0.018 Uiso 1 1 calc R U . . . C32F C 0.8273(3) 0.53737(18) 0.30080(18) 0.0287(6) Uani 1 1 d . . . . . H32P H 0.854611 0.476563 0.302338 0.043 Uiso 1 1 calc R U . . . H32Q H 0.749411 0.539335 0.316022 0.043 Uiso 1 1 calc R U . . . H32R H 0.882947 0.572181 0.344131 0.043 Uiso 1 1 calc R 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 O1A 0.0220(9) 0.0119(7) 0.0299(10) -0.0051(7) 0.0043(7) 0.0008(6) O3A 0.0136(7) 0.0147(7) 0.0198(8) -0.0016(6) 0.0001(6) 0.0002(6) O51A 0.0194(9) 0.0207(9) 0.0391(12) -0.0059(9) -0.0032(8) -0.0040(8) O52A 0.0155(8) 0.0207(9) 0.0236(9) 0.0014(7) 0.0019(7) 0.0049(7) N1A 0.0148(9) 0.0124(8) 0.0228(10) 0.0002(7) 0.0026(7) 0.0036(7) N2A 0.0139(8) 0.0114(7) 0.0136(8) -0.0012(6) 0.0043(6) 0.0006(7) N3A 0.0139(8) 0.0093(7) 0.0147(8) -0.0010(6) 0.0015(6) 0.0004(6) N5A 0.0127(8) 0.0182(9) 0.0153(8) -0.0014(7) 0.0018(7) 0.0005(7) C1A 0.0156(9) 0.0101(8) 0.0171(9) 0.0002(7) 0.0068(8) 0.0010(7) C2A 0.0127(9) 0.0093(8) 0.0141(9) -0.0006(7) 0.0041(7) -0.0004(7) C3A 0.0144(9) 0.0108(8) 0.0114(8) 0.0003(7) 0.0035(7) 0.0015(7) C4A 0.0144(9) 0.0115(8) 0.0143(9) 0.0002(7) 0.0025(7) 0.0015(7) C5A 0.0124(9) 0.0128(8) 0.0126(8) -0.0010(7) 0.0021(7) 0.0008(7) C31A 0.0207(10) 0.0096(8) 0.0168(9) -0.0039(7) 0.0026(8) -0.0010(7) C32A 0.0414(16) 0.0163(10) 0.0283(13) -0.0041(9) 0.0106(12) -0.0100(10) O1B 0.0206(8) 0.0105(7) 0.0206(8) -0.0039(6) 0.0057(6) -0.0006(6) O3B 0.0141(8) 0.0153(7) 0.0228(8) -0.0030(6) -0.0003(6) -0.0007(6) O51B 0.0162(8) 0.0213(8) 0.0225(9) -0.0041(7) 0.0017(6) -0.0051(7) O52B 0.0142(8) 0.0208(8) 0.0262(9) 0.0007(7) 0.0024(7) 0.0038(6) N1B 0.0155(8) 0.0109(7) 0.0229(9) -0.0007(7) 0.0037(7) 0.0021(6) N2B 0.0131(8) 0.0131(7) 0.0120(7) -0.0010(6) 0.0046(6) 0.0002(6) N3B 0.0123(7) 0.0110(7) 0.0141(8) -0.0023(6) 0.0033(6) 0.0005(6) N5B 0.0124(8) 0.0179(9) 0.0138(8) 0.0013(7) 0.0034(6) -0.0004(7) C1B 0.0154(9) 0.0096(8) 0.0136(9) 0.0004(7) 0.0065(7) 0.0002(7) C2B 0.0124(8) 0.0104(8) 0.0113(8) -0.0016(6) 0.0029(7) -0.0002(7) C3B 0.0124(9) 0.0120(8) 0.0131(8) -0.0009(7) 0.0029(7) 0.0003(7) C4B 0.0117(8) 0.0137(8) 0.0131(8) -0.0004(7) 0.0042(7) 0.0015(7) C5B 0.0117(8) 0.0134(8) 0.0119(8) -0.0004(7) 0.0030(7) 0.0003(7) C31B 0.0174(10) 0.0108(8) 0.0188(10) -0.0066(7) 0.0028(8) -0.0013(7) C32B 0.062(2) 0.0210(12) 0.0496(19) -0.0122(13) 0.0320(18) -0.0202(14) O1C 0.0263(9) 0.0108(7) 0.0198(8) 0.0022(6) 0.0061(7) 0.0059(6) O3C 0.0214(8) 0.0126(7) 0.0102(7) -0.0001(5) 0.0011(6) 0.0015(6) O51C 0.0284(10) 0.0202(8) 0.0158(8) 0.0053(7) 0.0017(7) -0.0017(7) O52C 0.0301(10) 0.0212(9) 0.0147(8) -0.0059(7) 0.0080(7) -0.0039(7) N1C 0.0246(10) 0.0120(8) 0.0148(8) -0.0028(7) 0.0036(7) 0.0029(7) N2C 0.0113(7) 0.0114(7) 0.0127(7) 0.0002(6) 0.0027(6) -0.0001(6) N3C 0.0137(8) 0.0089(7) 0.0110(7) -0.0004(6) 0.0016(6) 0.0025(6) N5C 0.0150(8) 0.0184(9) 0.0111(7) 0.0009(7) 0.0025(6) -0.0025(7) C1C 0.0159(9) 0.0093(8) 0.0154(9) -0.0009(7) 0.0064(7) 0.0003(7) C2C 0.0122(8) 0.0069(8) 0.0120(8) -0.0001(6) 0.0029(7) 0.0015(6) C3C 0.0135(9) 0.0084(8) 0.0106(8) -0.0011(6) 0.0023(7) 0.0015(6) C4C 0.0138(9) 0.0115(8) 0.0107(8) -0.0010(7) 0.0023(7) 0.0011(7) C5C 0.0133(9) 0.0125(8) 0.0105(8) -0.0003(7) 0.0030(7) 0.0001(7) C31C 0.0233(11) 0.0092(8) 0.0146(9) 0.0005(7) 0.0016(8) 0.0051(7) C32C 0.0368(16) 0.0178(11) 0.055(2) 0.0160(12) 0.0183(14) 0.0048(11) O1D 0.0300(10) 0.0092(6) 0.0239(9) 0.0020(6) 0.0067(7) 0.0047(6) O3D 0.0258(9) 0.0127(7) 0.0112(7) 0.0003(5) 0.0043(6) 0.0014(6) O51D 0.0454(13) 0.0208(9) 0.0176(8) 0.0077(7) 0.0070(8) 0.0081(9) O52D 0.0257(9) 0.0221(9) 0.0159(8) -0.0045(7) 0.0058(7) -0.0002(7) N1D 0.0299(11) 0.0112(8) 0.0185(9) -0.0033(7) 0.0081(8) 0.0021(7) N2D 0.0122(7) 0.0108(7) 0.0142(8) 0.0017(6) 0.0037(6) 0.0020(6) N3D 0.0147(8) 0.0085(7) 0.0130(7) 0.0009(6) 0.0038(6) -0.0007(6) N5D 0.0159(9) 0.0198(9) 0.0121(8) 0.0021(7) 0.0021(7) 0.0024(7) C1D 0.0152(9) 0.0096(8) 0.0176(10) -0.0017(7) 0.0055(8) 0.0011(7) C2D 0.0125(8) 0.0078(8) 0.0143(8) 0.0005(7) 0.0034(7) 0.0015(7) C3D 0.0149(9) 0.0088(8) 0.0131(8) 0.0005(7) 0.0042(7) 0.0018(7) C4D 0.0130(9) 0.0107(7) 0.0136(8) -0.0006(7) 0.0023(7) -0.0001(7) C5D 0.0147(9) 0.0122(8) 0.0116(8) 0.0010(7) 0.0027(7) 0.0017(7) C31D 0.0200(10) 0.0085(7) 0.0191(9) 0.0016(7) 0.0056(8) -0.0016(7) C32D 0.0209(11) 0.0177(10) 0.0417(15) 0.0130(10) 0.0092(11) 0.0061(8) O1E 0.0223(8) 0.0104(7) 0.0187(8) 0.0010(6) 0.0059(6) 0.0042(6) O3E 0.0237(9) 0.0127(7) 0.0106(7) 0.0007(5) 0.0018(6) 0.0026(6) O51E 0.0283(9) 0.0186(8) 0.0150(8) 0.0042(7) 0.0055(7) 0.0018(7) O52E 0.0290(10) 0.0191(8) 0.0140(7) -0.0064(6) 0.0061(7) 0.0003(7) N1E 0.0226(9) 0.0119(7) 0.0138(8) -0.0029(6) 0.0051(7) 0.0003(7) N2E 0.0128(7) 0.0103(7) 0.0129(7) -0.0010(6) 0.0036(6) -0.0002(6) N3E 0.0144(8) 0.0086(7) 0.0127(7) -0.0002(6) 0.0011(6) 0.0030(6) N5E 0.0142(8) 0.0169(8) 0.0125(8) -0.0009(7) 0.0046(6) -0.0004(7) C1E 0.0131(8) 0.0095(8) 0.0137(9) -0.0023(6) 0.0042(7) -0.0011(7) C2E 0.0117(8) 0.0081(8) 0.0125(8) -0.0002(6) 0.0030(7) 0.0007(6) C3E 0.0132(9) 0.0091(8) 0.0124(8) -0.0006(6) 0.0024(7) 0.0018(7) C4E 0.0116(8) 0.0108(8) 0.0119(8) -0.0013(7) 0.0021(6) 0.0024(7) C5E 0.0144(9) 0.0123(8) 0.0095(8) -0.0012(7) 0.0032(7) 0.0016(7) C31E 0.0195(10) 0.0091(8) 0.0171(9) 0.0006(7) 0.0007(8) 0.0035(7) C32E 0.0255(12) 0.0156(10) 0.0423(16) 0.0120(10) 0.0071(11) 0.0006(9) O1F 0.0198(8) 0.0111(7) 0.0275(9) 0.0062(6) 0.0039(7) 0.0001(6) O3F 0.0132(7) 0.0150(7) 0.0229(8) 0.0020(6) 0.0002(6) 0.0008(6) O51F 0.0186(8) 0.0185(8) 0.0285(10) 0.0011(8) -0.0028(7) 0.0050(7) O52F 0.0144(8) 0.0198(9) 0.0248(9) -0.0014(7) 0.0020(7) -0.0047(6) N1F 0.0158(8) 0.0112(8) 0.0191(9) 0.0018(7) 0.0010(7) -0.0034(7) N2F 0.0136(8) 0.0109(7) 0.0117(7) 0.0009(6) 0.0043(6) -0.0004(6) N3F 0.0125(7) 0.0092(6) 0.0150(8) 0.0009(6) 0.0026(6) 0.0004(6) N5F 0.0127(8) 0.0163(8) 0.0139(8) -0.0008(7) 0.0029(6) -0.0008(7) C1F 0.0143(9) 0.0085(7) 0.0158(9) 0.0010(7) 0.0052(7) 0.0010(7) C2F 0.0124(8) 0.0090(8) 0.0126(8) 0.0010(7) 0.0040(7) -0.0007(7) C3F 0.0128(9) 0.0102(8) 0.0126(8) 0.0012(7) 0.0025(7) -0.0009(7) C4F 0.0133(9) 0.0116(8) 0.0160(9) -0.0002(7) 0.0035(7) -0.0014(7) C5F 0.0113(8) 0.0120(8) 0.0120(8) -0.0006(7) 0.0019(7) -0.0002(7) C31F 0.0202(10) 0.0094(7) 0.0160(9) -0.0002(7) 0.0047(8) 0.0030(7) C32F 0.0479(17) 0.0177(10) 0.0245(12) 0.0093(9) 0.0164(12) 0.0125(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1A N1A H1AA 120(3) . . ? C1A N1A H1AB 123(2) . . ? H1AA N1A H1AB 117(3) . . ? C2A N2A C5A 117.7(2) . . ? C4A N3A C3A 121.9(2) . . ? C4A N3A C31A 118.36(19) . . ? C3A N3A C31A 119.75(19) . . ? O51A N5A O52A 123.9(2) . . ? O51A N5A C5A 119.1(2) . . ? O52A N5A C5A 117.0(2) . . ? O1A C1A N1A 123.6(2) . . ? O1A C1A C2A 119.3(2) . . ? N1A C1A C2A 117.1(2) . . ? N2A C2A C3A 123.1(2) . . ? N2A C2A C1A 115.3(2) . . ? C3A C2A C1A 121.48(19) . . ? O3A C3A N3A 119.6(2) . . ? O3A C3A C2A 126.0(2) . . ? N3A C3A C2A 114.30(19) . . ? N3A C4A C5A 118.3(2) . . ? N3A C4A H4A 120.9 . . ? C5A C4A H4A 120.9 . . ? N2A C5A C4A 124.7(2) . . ? N2A C5A N5A 117.1(2) . . ? C4A C5A N5A 118.2(2) . . ? N3A C31A C32A 110.80(19) . . ? N3A C31A H31A 109.5 . . ? C32A C31A H31A 109.5 . . ? N3A C31A H31B 109.5 . . ? C32A C31A H31B 109.5 . . ? H31A C31A H31B 108.1 . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C1B N1B H1BA 117(3) . . ? C1B N1B H1BB 122(2) . . ? H1BA N1B H1BB 120(3) . . ? C2B N2B C5B 118.0(2) . . ? C4B N3B C3B 121.6(2) . . ? C4B N3B C31B 119.46(19) . . ? C3B N3B C31B 118.91(18) . . ? O51B N5B O52B 124.1(2) . . ? O51B N5B C5B 118.9(2) . . ? O52B N5B C5B 117.1(2) . . ? O1B C1B N1B 124.1(2) . . ? O1B C1B C2B 119.5(2) . . ? N1B C1B C2B 116.40(19) . . ? N2B C2B C3B 122.7(2) . . ? N2B C2B C1B 115.56(19) . . ? C3B C2B C1B 121.73(19) . . ? O3B C3B N3B 119.3(2) . . ? O3B C3B C2B 126.0(2) . . ? N3B C3B C2B 114.62(19) . . ? N3B C4B C5B 118.3(2) . . ? N3B C4B H4B 120.8 . . ? C5B C4B H4B 120.8 . . ? N2B C5B C4B 124.5(2) . . ? N2B C5B N5B 117.0(2) . . ? C4B C5B N5B 118.4(2) . . ? N3B C31B C32B 111.7(2) . . ? N3B C31B H31C 109.3 . . ? C32B C31B H31C 109.3 . . ? N3B C31B H31D 109.3 . . ? C32B C31B H31D 109.3 . . ? H31C C31B H31D 107.9 . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C1C N1C H1CA 117(3) . . ? C1C N1C H1CB 116(3) . . ? H1CA N1C H1CB 126(4) . . ? C2C N2C C5C 117.64(19) . . ? C4C N3C C3C 122.10(19) . . ? C4C N3C C31C 119.32(18) . . ? C3C N3C C31C 118.58(17) . . ? O51C N5C O52C 124.2(2) . . ? O51C N5C C5C 119.0(2) . . ? O52C N5C C5C 116.8(2) . . ? O1C C1C N1C 123.5(2) . . ? O1C C1C C2C 120.0(2) . . ? N1C C1C C2C 116.5(2) . . ? N2C C2C C3C 122.82(19) . . ? N2C C2C C1C 115.38(19) . . ? C3C C2C C1C 121.77(19) . . ? O3C C3C N3C 119.8(2) . . ? O3C C3C C2C 125.7(2) . . ? N3C C3C C2C 114.50(18) . . ? N3C C4C C5C 118.1(2) . . ? N3C C4C H4C 121.0 . . ? C5C C4C H4C 121.0 . . ? N2C C5C C4C 124.8(2) . . ? N2C C5C N5C 116.6(2) . . ? C4C C5C N5C 118.6(2) . . ? N3C C31C C32C 111.8(2) . . ? N3C C31C H31E 109.3 . . ? C32C C31C H31E 109.3 . . ? N3C C31C H31F 109.3 . . ? C32C C31C H31F 109.3 . . ? H31E C31C H31F 107.9 . . ? C31C C32C H32G 109.5 . . ? C31C C32C H32H 109.5 . . ? H32G C32C H32H 109.5 . . ? C31C C32C H32I 109.5 . . ? H32G C32C H32I 109.5 . . ? H32H C32C H32I 109.5 . . ? C1D N1D H1DA 115(3) . . ? C1D N1D H1DB 116(3) . . ? H1DA N1D H1DB 129(4) . . ? C2D N2D C5D 117.3(2) . . ? C4D N3D C3D 122.03(18) . . ? C4D N3D C31D 119.77(18) . . ? C3D N3D C31D 118.19(18) . . ? O51D N5D O52D 123.9(2) . . ? O51D N5D C5D 118.9(2) . . ? O52D N5D C5D 117.2(2) . . ? O1D C1D N1D 123.8(2) . . ? O1D C1D C2D 119.4(2) . . ? N1D C1D C2D 116.7(2) . . ? N2D C2D C3D 123.1(2) . . ? N2D C2D C1D 115.4(2) . . ? C3D C2D C1D 121.29(19) . . ? O3D C3D N3D 120.0(2) . . ? O3D C3D C2D 125.9(2) . . ? N3D C3D C2D 114.07(19) . . ? N3D C4D C5D 118.2(2) . . ? N3D C4D H4D 120.9 . . ? C5D C4D H4D 120.9 . . ? N2D C5D C4D 124.6(2) . . ? N2D C5D N5D 117.2(2) . . ? C4D C5D N5D 118.1(2) . . ? N3D C31D C32D 112.17(19) . . ? N3D C31D H31G 109.2 . . ? C32D C31D H31G 109.2 . . ? N3D C31D H31H 109.2 . . ? C32D C31D H31H 109.2 . . ? H31G C31D H31H 107.9 . . ? C31D C32D H32J 109.5 . . ? C31D C32D H32K 109.5 . . ? H32J C32D H32K 109.5 . . ? C31D C32D H32L 109.5 . . ? H32J C32D H32L 109.5 . . ? H32K C32D H32L 109.5 . . ? C1E N1E H1EA 117(3) . . ? C1E N1E H1EB 115(3) . . ? H1EA N1E H1EB 128(4) . . ? C2E N2E C5E 117.47(19) . . ? C4E N3E C3E 122.13(18) . . ? C4E N3E C31E 118.26(18) . . ? C3E N3E C31E 119.56(18) . . ? O51E N5E O52E 123.8(2) . . ? O51E N5E C5E 119.1(2) . . ? O52E N5E C5E 117.1(2) . . ? O1E C1E N1E 124.0(2) . . ? O1E C1E C2E 120.0(2) . . ? N1E C1E C2E 116.0(2) . . ? N2E C2E C3E 123.10(19) . . ? N2E C2E C1E 115.08(19) . . ? C3E C2E C1E 121.78(19) . . ? O3E C3E N3E 120.0(2) . . ? O3E C3E C2E 125.9(2) . . ? N3E C3E C2E 114.05(19) . . ? N3E C4E C5E 118.39(19) . . ? N3E C4E H4E 120.8 . . ? C5E C4E H4E 120.8 . . ? N2E C5E C4E 124.8(2) . . ? N2E C5E N5E 116.7(2) . . ? C4E C5E N5E 118.5(2) . . ? N3E C31E C32E 110.38(19) . . ? N3E C31E H31I 109.6 . . ? C32E C31E H31I 109.6 . . ? N3E C31E H31J 109.6 . . ? C32E C31E H31J 109.6 . . ? H31I C31E H31J 108.1 . . ? C31E C32E H32M 109.5 . . ? C31E C32E H32N 109.5 . . ? H32M C32E H32N 109.5 . . ? C31E C32E H32O 109.5 . . ? H32M C32E H32O 109.5 . . ? H32N C32E H32O 109.5 . . ? C1F N1F H1FA 120(3) . . ? C1F N1F H1FB 123(2) . . ? H1FA N1F H1FB 118(4) . . ? C2F N2F C5F 117.5(2) . . ? C4F N3F C3F 122.11(19) . . ? C4F N3F C31F 119.20(19) . . ? C3F N3F C31F 118.69(18) . . ? O51F N5F O52F 123.9(2) . . ? O51F N5F C5F 119.1(2) . . ? O52F N5F C5F 116.9(2) . . ? O1F C1F N1F 123.4(2) . . ? O1F C1F C2F 119.3(2) . . ? N1F C1F C2F 117.32(19) . . ? N2F C2F C3F 122.9(2) . . ? N2F C2F C1F 115.9(2) . . ? C3F C2F C1F 120.97(19) . . ? O3F C3F N3F 119.8(2) . . ? O3F C3F C2F 126.2(2) . . ? N3F C3F C2F 114.04(19) . . ? N3F C4F C5F 117.9(2) . . ? N3F C4F H4F 121.0 . . ? C5F C4F H4F 121.0 . . ? N2F C5F C4F 124.7(2) . . ? N2F C5F N5F 117.3(2) . . ? C4F C5F N5F 117.8(2) . . ? N3F C31F C32F 112.08(19) . . ? N3F C31F H31K 109.2 . . ? C32F C31F H31K 109.2 . . ? N3F C31F H31L 109.2 . . ? C32F C31F H31L 109.2 . . ? H31K C31F H31L 107.9 . . ? C31F C32F H32P 109.5 . . ? C31F C32F H32Q 109.5 . . ? H32P C32F H32Q 109.5 . . ? C31F C32F H32R 109.5 . . ? H32P C32F H32R 109.5 . . ? H32Q C32F H32R 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 O1A C1A 1.232(3) . ? O3A C3A 1.235(3) . ? O51A N5A 1.219(3) . ? O52A N5A 1.235(3) . ? N1A C1A 1.330(3) . ? N1A H1AA 0.862(19) . ? N1A H1AB 0.889(17) . ? N2A C2A 1.307(3) . ? N2A C5A 1.337(3) . ? N3A C4A 1.345(3) . ? N3A C3A 1.400(3) . ? N3A C31A 1.483(3) . ? N5A C5A 1.454(3) . ? C1A C2A 1.515(3) . ? C2A C3A 1.469(3) . ? C4A C5A 1.366(3) . ? C4A H4A 0.9500 . ? C31A C32A 1.511(4) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? O1B C1B 1.237(3) . ? O3B C3B 1.237(3) . ? O51B N5B 1.223(3) . ? O52B N5B 1.235(3) . ? N1B C1B 1.330(3) . ? N1B H1BA 0.861(19) . ? N1B H1BB 0.889(17) . ? N2B C2B 1.306(3) . ? N2B C5B 1.336(3) . ? N3B C4B 1.343(3) . ? N3B C3B 1.401(3) . ? N3B C31B 1.485(3) . ? N5B C5B 1.454(3) . ? C1B C2B 1.512(3) . ? C2B C3B 1.469(3) . ? C4B C5B 1.369(3) . ? C4B H4B 0.9500 . ? C31B C32B 1.507(4) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? O1C C1C 1.235(3) . ? O3C C3C 1.233(3) . ? O51C N5C 1.226(3) . ? O52C N5C 1.233(3) . ? N1C C1C 1.333(3) . ? N1C H1CA 0.865(19) . ? N1C H1CB 0.894(18) . ? N2C C2C 1.312(3) . ? N2C C5C 1.340(3) . ? N3C C4C 1.346(3) . ? N3C C3C 1.395(3) . ? N3C C31C 1.485(3) . ? N5C C5C 1.456(3) . ? C1C C2C 1.514(3) . ? C2C C3C 1.469(3) . ? C4C C5C 1.365(3) . ? C4C H4C 0.9500 . ? C31C C32C 1.515(4) . ? C31C H31E 0.9900 . ? C31C H31F 0.9900 . ? C32C H32G 0.9800 . ? C32C H32H 0.9800 . ? C32C H32I 0.9800 . ? O1D C1D 1.235(3) . ? O3D C3D 1.231(3) . ? O51D N5D 1.221(3) . ? O52D N5D 1.238(3) . ? N1D C1D 1.326(3) . ? N1D H1DA 0.863(19) . ? N1D H1DB 0.892(18) . ? N2D C2D 1.309(3) . ? N2D C5D 1.341(3) . ? N3D C4D 1.340(3) . ? N3D C3D 1.397(3) . ? N3D C31D 1.481(3) . ? N5D C5D 1.453(3) . ? C1D C2D 1.518(3) . ? C2D C3D 1.469(3) . ? C4D C5D 1.366(3) . ? C4D H4D 0.9500 . ? C31D C32D 1.505(3) . ? C31D H31G 0.9900 . ? C31D H31H 0.9900 . ? C32D H32J 0.9800 . ? C32D H32K 0.9800 . ? C32D H32L 0.9800 . ? O1E C1E 1.237(3) . ? O3E C3E 1.229(3) . ? O51E N5E 1.228(3) . ? O52E N5E 1.235(3) . ? N1E C1E 1.326(3) . ? N1E H1EA 0.863(19) . ? N1E H1EB 0.893(18) . ? N2E C2E 1.312(3) . ? N2E C5E 1.337(3) . ? N3E C4E 1.342(3) . ? N3E C3E 1.399(3) . ? N3E C31E 1.483(3) . ? N5E C5E 1.452(3) . ? C1E C2E 1.515(3) . ? C2E C3E 1.474(3) . ? C4E C5E 1.363(3) . ? C4E H4E 0.9500 . ? C31E C32E 1.508(4) . ? C31E H31I 0.9900 . ? C31E H31J 0.9900 . ? C32E H32M 0.9800 . ? C32E H32N 0.9800 . ? C32E H32O 0.9800 . ? O1F C1F 1.233(3) . ? O3F C3F 1.232(3) . ? O51F N5F 1.220(3) . ? O52F N5F 1.237(3) . ? N1F C1F 1.333(3) . ? N1F H1FA 0.863(19) . ? N1F H1FB 0.890(17) . ? N2F C2F 1.308(3) . ? N2F C5F 1.339(3) . ? N3F C4F 1.342(3) . ? N3F C3F 1.398(3) . ? N3F C31F 1.486(3) . ? N5F C5F 1.458(3) . ? C1F C2F 1.509(3) . ? C2F C3F 1.469(3) . ? C4F C5F 1.367(3) . ? C4F H4F 0.9500 . ? C31F C32F 1.502(3) . ? C31F H31K 0.9900 . ? C31F H31L 0.9900 . ? C32F H32P 0.9800 . ? C32F H32Q 0.9800 . ? C32F H32R 0.9800 . ? 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 N1A H1AA O3A 0.862(19) 2.06(3) 2.722(3) 134(4) . yes N1A H1AB O1C 0.889(17) 2.06(2) 2.899(3) 158(3) . yes N1B H1BA O3B 0.861(19) 1.98(3) 2.701(3) 141(3) . yes N1B H1BA O52D 0.861(19) 2.64(3) 3.254(3) 130(3) 2_646 yes N1B H1BB O1D 0.889(17) 2.06(2) 2.895(3) 156(3) . yes N1C H1CA O3C 0.865(19) 2.09(3) 2.726(3) 130(4) . yes N1C H1CB O1F 0.894(18) 2.12(3) 2.919(3) 148(4) 2_645 yes N1D H1DA O3D 0.863(19) 2.02(3) 2.709(3) 136(4) . yes N1D H1DB O1A 0.892(18) 2.12(3) 2.924(3) 149(4) . yes N1E H1EA O52B 0.863(19) 2.64(4) 3.195(3) 123(3) 2_756 yes N1E H1EA O3E 0.863(19) 2.04(3) 2.710(3) 134(4) . yes N1E H1EB O1B 0.893(18) 2.02(2) 2.873(3) 159(4) . yes N1F H1FA O3F 0.863(19) 2.10(4) 2.737(3) 130(4) . yes N1F H1FB O1E 0.890(17) 2.08(2) 2.911(3) 155(3) 2_756 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 C5A N2A C2A C3A -0.8(3) . . . . ? C5A N2A C2A C1A 176.9(2) . . . . ? O1A C1A C2A N2A -10.8(3) . . . . ? N1A C1A C2A N2A 169.5(2) . . . . ? O1A C1A C2A C3A 166.9(2) . . . . ? N1A C1A C2A C3A -12.8(3) . . . . ? C4A N3A C3A O3A 179.2(2) . . . . ? C31A N3A C3A O3A -2.4(3) . . . . ? C4A N3A C3A C2A 0.4(3) . . . . ? C31A N3A C3A C2A 178.73(19) . . . . ? N2A C2A C3A O3A -177.8(2) . . . . ? C1A C2A C3A O3A 4.6(4) . . . . ? N2A C2A C3A N3A 0.9(3) . . . . ? C1A C2A C3A N3A -176.60(19) . . . . ? C3A N3A C4A C5A -1.7(3) . . . . ? C31A N3A C4A C5A 179.9(2) . . . . ? C2A N2A C5A C4A -0.7(4) . . . . ? C2A N2A C5A N5A 179.6(2) . . . . ? N3A C4A C5A N2A 1.9(4) . . . . ? N3A C4A C5A N5A -178.4(2) . . . . ? O51A N5A C5A N2A 1.8(3) . . . . ? O52A N5A C5A N2A -178.9(2) . . . . ? O51A N5A C5A C4A -178.0(2) . . . . ? O52A N5A C5A C4A 1.4(3) . . . . ? C4A N3A C31A C32A 85.7(3) . . . . ? C3A N3A C31A C32A -92.7(3) . . . . ? C5B N2B C2B C3B -1.7(3) . . . . ? C5B N2B C2B C1B 176.43(19) . . . . ? O1B C1B C2B N2B -6.8(3) . . . . ? N1B C1B C2B N2B 174.6(2) . . . . ? O1B C1B C2B C3B 171.3(2) . . . . ? N1B C1B C2B C3B -7.3(3) . . . . ? C4B N3B C3B O3B 175.7(2) . . . . ? C31B N3B C3B O3B -4.5(3) . . . . ? C4B N3B C3B C2B -3.8(3) . . . . ? C31B N3B C3B C2B 175.97(19) . . . . ? N2B C2B C3B O3B -174.6(2) . . . . ? C1B C2B C3B O3B 7.4(4) . . . . ? N2B C2B C3B N3B 4.8(3) . . . . ? C1B C2B C3B N3B -173.13(19) . . . . ? C3B N3B C4B C5B -0.1(3) . . . . ? C31B N3B C4B C5B -179.9(2) . . . . ? C2B N2B C5B C4B -2.9(3) . . . . ? C2B N2B C5B N5B 178.80(19) . . . . ? N3B C4B C5B N2B 3.9(3) . . . . ? N3B C4B C5B N5B -177.85(19) . . . . ? O51B N5B C5B N2B 5.5(3) . . . . ? O52B N5B C5B N2B -174.6(2) . . . . ? O51B N5B C5B C4B -172.9(2) . . . . ? O52B N5B C5B C4B 7.0(3) . . . . ? C4B N3B C31B C32B 99.4(3) . . . . ? C3B N3B C31B C32B -80.4(3) . . . . ? C5C N2C C2C C3C -0.8(3) . . . . ? C5C N2C C2C C1C 177.09(19) . . . . ? O1C C1C C2C N2C -14.4(3) . . . . ? N1C C1C C2C N2C 165.5(2) . . . . ? O1C C1C C2C C3C 163.5(2) . . . . ? N1C C1C C2C C3C -16.6(3) . . . . ? C4C N3C C3C O3C 176.6(2) . . . . ? C31C N3C C3C O3C -2.3(3) . . . . ? C4C N3C C3C C2C -2.4(3) . . . . ? C31C N3C C3C C2C 178.6(2) . . . . ? N2C C2C C3C O3C -176.2(2) . . . . ? C1C C2C C3C O3C 6.0(4) . . . . ? N2C C2C C3C N3C 2.8(3) . . . . ? C1C C2C C3C N3C -174.95(19) . . . . ? C3C N3C C4C C5C 0.2(3) . . . . ? C31C N3C C4C C5C 179.1(2) . . . . ? C2C N2C C5C C4C -1.8(3) . . . . ? C2C N2C C5C N5C 178.04(19) . . . . ? N3C C4C C5C N2C 2.2(4) . . . . ? N3C C4C C5C N5C -177.7(2) . . . . ? O51C N5C C5C N2C 3.8(3) . . . . ? O52C N5C C5C N2C -177.3(2) . . . . ? O51C N5C C5C C4C -176.4(2) . . . . ? O52C N5C C5C C4C 2.5(3) . . . . ? C4C N3C C31C C32C 103.7(3) . . . . ? C3C N3C C31C C32C -77.3(3) . . . . ? C5D N2D C2D C3D -1.8(3) . . . . ? C5D N2D C2D C1D 173.2(2) . . . . ? O1D C1D C2D N2D -8.2(3) . . . . ? N1D C1D C2D N2D 173.6(2) . . . . ? O1D C1D C2D C3D 166.8(2) . . . . ? N1D C1D C2D C3D -11.4(3) . . . . ? C4D N3D C3D O3D 172.5(2) . . . . ? C31D N3D C3D O3D -6.3(3) . . . . ? C4D N3D C3D C2D -8.3(3) . . . . ? C31D N3D C3D C2D 172.92(19) . . . . ? N2D C2D C3D O3D -172.9(2) . . . . ? C1D C2D C3D O3D 12.5(4) . . . . ? N2D C2D C3D N3D 7.9(3) . . . . ? C1D C2D C3D N3D -166.7(2) . . . . ? C3D N3D C4D C5D 2.9(3) . . . . ? C31D N3D C4D C5D -178.4(2) . . . . ? C2D N2D C5D C4D -4.7(3) . . . . ? C2D N2D C5D N5D 179.2(2) . . . . ? N3D C4D C5D N2D 4.3(4) . . . . ? N3D C4D C5D N5D -179.6(2) . . . . ? O51D N5D C5D N2D 7.4(3) . . . . ? O52D N5D C5D N2D -174.4(2) . . . . ? O51D N5D C5D C4D -169.0(2) . . . . ? O52D N5D C5D C4D 9.2(3) . . . . ? C4D N3D C31D C32D -98.0(3) . . . . ? C3D N3D C31D C32D 80.8(3) . . . . ? C5E N2E C2E C3E -0.9(3) . . . . ? C5E N2E C2E C1E 176.6(2) . . . . ? O1E C1E C2E N2E -10.4(3) . . . . ? N1E C1E C2E N2E 169.4(2) . . . . ? O1E C1E C2E C3E 167.1(2) . . . . ? N1E C1E C2E C3E -13.1(3) . . . . ? C4E N3E C3E O3E 178.2(2) . . . . ? C31E N3E C3E O3E -4.7(3) . . . . ? C4E N3E C3E C2E -1.3(3) . . . . ? C31E N3E C3E C2E 175.9(2) . . . . ? N2E C2E C3E O3E -176.9(2) . . . . ? C1E C2E C3E O3E 5.8(4) . . . . ? N2E C2E C3E N3E 2.5(3) . . . . ? C1E C2E C3E N3E -174.84(19) . . . . ? C3E N3E C4E C5E -1.3(3) . . . . ? C31E N3E C4E C5E -178.5(2) . . . . ? C2E N2E C5E C4E -2.1(4) . . . . ? C2E N2E C5E N5E -179.3(2) . . . . ? N3E C4E C5E N2E 3.2(4) . . . . ? N3E C4E C5E N5E -179.6(2) . . . . ? O51E N5E C5E N2E 1.3(3) . . . . ? O52E N5E C5E N2E 179.1(2) . . . . ? O51E N5E C5E C4E -176.1(2) . . . . ? O52E N5E C5E C4E 1.6(3) . . . . ? C4E N3E C31E C32E 85.6(3) . . . . ? C3E N3E C31E C32E -91.6(3) . . . . ? C5F N2F C2F C3F -1.3(3) . . . . ? C5F N2F C2F C1F 173.7(2) . . . . ? O1F C1F C2F N2F -17.0(3) . . . . ? N1F C1F C2F N2F 164.9(2) . . . . ? O1F C1F C2F C3F 158.2(2) . . . . ? N1F C1F C2F C3F -20.0(3) . . . . ? C4F N3F C3F O3F 172.6(2) . . . . ? C31F N3F C3F O3F -6.9(3) . . . . ? C4F N3F C3F C2F -8.9(3) . . . . ? C31F N3F C3F C2F 171.58(19) . . . . ? N2F C2F C3F O3F -173.7(2) . . . . ? C1F C2F C3F O3F 11.6(4) . . . . ? N2F C2F C3F N3F 8.0(3) . . . . ? C1F C2F C3F N3F -166.7(2) . . . . ? C3F N3F C4F C5F 3.4(3) . . . . ? C31F N3F C4F C5F -177.1(2) . . . . ? C2F N2F C5F C4F -5.3(3) . . . . ? C2F N2F C5F N5F 179.89(19) . . . . ? N3F C4F C5F N2F 4.4(3) . . . . ? N3F C4F C5F N5F 179.1(2) . . . . ? O51F N5F C5F N2F 3.3(3) . . . . ? O52F N5F C5F N2F -177.8(2) . . . . ? O51F N5F C5F C4F -171.9(2) . . . . ? O52F N5F C5F C4F 7.1(3) . . . . ? C4F N3F C31F C32F -96.9(3) . . . . ? C3F N3F C31F C32F 82.6(3) . . . . ?