#------------------------------------------------------------------------------ #$Date: 2019-03-14 05:34:48 +0200 (Thu, 14 Mar 2019) $ #$Revision: 214120 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/83/2108374.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108374 loop_ _publ_author_name 'Arkhipov, S. G.' 'Losev, E. A.' 'Nguyen, T. T.' 'Rychkov, D. A.' 'Boldyreva, E. V.' _publ_section_title ; A large anisotropic plasticity of L-leucinium hydrogen maleate preserved at cryogenic temperatures ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first ; ; _journal_paper_doi 10.1107/S2052520619000441 _journal_volume 75 _journal_year 2019 _chemical_absolute_configuration syn _chemical_formula_iupac 'C6 H14 N O2 +, C4 H3 O4 -' _chemical_formula_moiety 'C6 H14 N O2 +, C4 H3 O4 -' _chemical_formula_sum 'C10 H17 N O6' _chemical_formula_weight 247.24 _chemical_name_systematic ; L-Leucinium hydrogen maleate ; _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2018-10-08 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 99.653(3) _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 21.4563(9) _cell_length_b 5.67251(19) _cell_length_c 32.0779(8) _cell_measurement_reflns_used 4785 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 29.3540 _cell_measurement_theta_min 2.1340 _cell_volume 3849.0(2) _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 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 200.0 _diffrn_detector 'image plate (34 cm diameter)' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 1.000 _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 -90.00 90.00 0.50 180.00 -- 0.00 180.00 214.00 360 2 \w -20.00 90.00 0.50 180.00 -- 0.00 180.00 114.00 220 ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0162739000 _diffrn_orient_matrix_UB_12 -0.0036395000 _diffrn_orient_matrix_UB_13 -0.0211438000 _diffrn_orient_matrix_UB_21 -0.0291967000 _diffrn_orient_matrix_UB_22 0.0146174000 _diffrn_orient_matrix_UB_23 0.0073259000 _diffrn_orient_matrix_UB_31 0.0029283000 _diffrn_orient_matrix_UB_32 0.1240532000 _diffrn_orient_matrix_UB_33 -0.0014962000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_unetI/netI 0.0770 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 22918 _diffrn_reflns_point_group_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 1.925 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61905 _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_density_diffrn 1.280 _exptl_crystal_description needle _exptl_crystal_F_000 1584 _exptl_crystal_size_max 4 _exptl_crystal_size_mid 0.119 _exptl_crystal_size_min 0.062 _refine_diff_density_max 0.219 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 475 _refine_ls_number_reflns 7634 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0500 _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^)+(0.0494P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1077 _refine_ls_wR_factor_ref 0.1355 _reflns_Friedel_coverage 0.758 _reflns_Friedel_fraction_full 0.941 _reflns_Friedel_fraction_max 0.939 _reflns_number_gt 4962 _reflns_number_total 7634 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file xk5052sup1.cif _cod_data_source_block l_leu_mal_200 _cod_database_code 2108374 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula 'C10 H17 N O6' _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 0.993 _shelx_estimated_absorpt_t_min 0.676 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C21(H21), C22(H22), C43(H43), C41(H41), C23(H23), C42(H42) 2.b Secondary CH2 refined with riding coordinates: C32(H32A,H32B), C33(H33A,H33B), C31(H31A,H31B) 2.c Aromatic/amide H refined with riding coordinates: C92(H92), C91(H91), C93(H93), C83(H83), C81(H81), C82(H82) 2.d Idealised Me refined as rotating group: N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N1(H1A,H1B,H1C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C62(H62A,H62B, H62C), C52(H52A,H52B,H52C) 2.e Idealised tetrahedral OH refined as rotating group: O61(H61), O12(H12), O62(H62), O63(H63), O13(H13), O11(H11) ; _shelx_res_file ; TITL l_leu_mal_200.res created by SHELXL-2017/1 at 09:06:55 on 08-Oct-2018 CELL 0.71073 21.456325 5.672508 32.077875 90 99.6527 90 ZERR 12 0.000863 0.00019 0.000836 0 0.0034 0 LATT -7 SYMM -X,+Y,-Z SFAC C H N O UNIT 120 204 12 72 EQIV $1 1-X,-1+Y,1-Z EQIV $2 -0.5+X,-0.5+Y,+Z EQIV $3 1-X,1+Y,1-Z EQIV $4 0.5+X,-0.5+Y,+Z EQIV $5 0.5+X,-0.5+Y,1+Z EQIV $6 0.5+X,0.5+Y,1+Z EQIV $7 0.5+X,0.5+Y,+Z EQIV $8 1.5-X,-0.5+Y,1-Z EQIV $9 1-X,+Y,1-Z L.S. 4 PLAN 20 SIZE 0.062 0.119 4 TEMP -73.15 HTAB N1 O21_$8 HTAB N1 O31_$8 HTAB N1 O32_$7 HTAB N1 O42_$4 HTAB N2 O23_$2 HTAB N2 O51_$1 HTAB N2 O61_$9 HTAB N3 O22_$4 HTAB N3 O53_$5 HTAB N3 O63_$6 HTAB O11 O31 HTAB O12 O33_$3 HTAB O13 O52_$7 HTAB O61 O41 HTAB O62 O42 HTAB O63 O43 CONF BOND BOND $H fmap 2 acta SHEL 40 0.8 REM REM REM WGHT 0.049400 FVAR 0.17904 O51 4 0.500697 0.701128 0.245806 11.00000 0.06622 0.04639 = 0.02795 0.00268 -0.00411 -0.00257 O21 4 0.702950 0.551171 0.503028 11.00000 0.05305 0.04019 = 0.02765 0.00477 0.00109 -0.00575 O31 4 0.612478 0.583026 0.417945 11.00000 0.06272 0.05140 = 0.02432 0.00591 -0.00397 -0.00416 O42 4 0.280289 0.535953 0.647298 11.00000 0.06179 0.03281 = 0.02500 0.00139 0.00130 0.00304 O61 4 0.532134 0.407694 0.289181 11.00000 0.06634 0.03348 = 0.02634 -0.00013 -0.00459 -0.00068 AFIX 147 H61 2 0.546326 0.388773 0.314999 11.00000 -1.50000 AFIX 0 O52 4 0.353743 0.341717 0.776323 11.00000 0.08328 0.04616 = 0.02563 0.00459 -0.00525 -0.00410 O22 4 0.510325 0.449162 0.850336 11.00000 0.05053 0.05065 = 0.03843 -0.00892 0.01692 0.00021 N2 3 0.510342 0.149731 0.788472 11.00000 0.04444 0.03721 = 0.02666 -0.00217 0.00608 -0.00250 AFIX 137 H2A 2 0.492890 0.252547 0.768028 11.00000 -1.20000 H2B 2 0.484732 0.136189 0.808268 11.00000 -1.20000 H2C 2 0.514842 0.006163 0.776672 11.00000 -1.20000 AFIX 0 O12 4 0.609787 0.566023 0.851965 11.00000 0.06092 0.06060 = 0.04886 -0.02420 0.01551 -0.01656 AFIX 147 H12 2 0.600421 0.664945 0.869396 11.00000 -1.50000 AFIX 0 O53 4 0.414683 0.150405 -0.065708 11.00000 0.06374 0.05000 = 0.02570 0.00427 0.00225 -0.00084 O33 4 0.413499 -0.059551 0.106631 11.00000 0.07352 0.04424 = 0.02834 0.00549 0.01183 0.00751 O62 4 0.326353 0.575874 0.721734 11.00000 0.07338 0.03191 = 0.02463 0.00013 -0.00366 0.00324 AFIX 147 H62 2 0.308167 0.566022 0.696481 11.00000 -1.50000 AFIX 0 O63 4 0.426323 -0.159155 -0.024297 11.00000 0.11029 0.03834 = 0.02568 -0.00134 0.00169 0.00992 AFIX 147 H63 2 0.428168 -0.189300 0.001519 11.00000 -1.50000 AFIX 0 N3 3 0.918617 0.098602 0.896578 11.00000 0.04570 0.04004 = 0.02510 -0.00023 0.00754 0.00108 AFIX 137 H3A 2 0.951646 0.093227 0.882129 11.00000 -1.20000 H3B 2 0.912820 -0.046361 0.907461 11.00000 -1.20000 H3C 2 0.927052 0.205156 0.917988 11.00000 -1.20000 AFIX 0 O13 4 0.828343 0.465708 0.816594 11.00000 0.06148 0.06033 = 0.04051 0.02038 0.00104 0.00349 AFIX 147 H13 2 0.839954 0.578082 0.802657 11.00000 -1.50000 AFIX 0 O32 4 0.254837 0.247515 0.600959 11.00000 0.07353 0.04789 = 0.02576 -0.00424 -0.00483 0.00029 O11 4 0.642393 0.251815 0.473471 11.00000 0.06647 0.05164 = 0.02991 0.00673 -0.01168 -0.01572 AFIX 147 H11 2 0.630723 0.350461 0.454212 11.00000 -1.50000 AFIX 0 O41 4 0.579977 0.354253 0.362577 11.00000 0.05963 0.03123 = 0.03187 0.00402 0.00090 0.00090 O23 4 0.931919 0.436104 0.841693 11.00000 0.05493 0.05804 = 0.04445 0.01222 0.01572 -0.00216 O43 4 0.430778 -0.249835 0.049885 11.00000 0.14602 0.03070 = 0.03119 0.00176 0.01814 0.01276 C92 1 0.312321 0.155620 0.712532 11.00000 0.07346 0.03028 = 0.03143 0.00378 0.00563 0.00645 AFIX 43 H92 2 0.317314 0.011156 0.727708 11.00000 -1.20000 AFIX 0 C21 1 0.693713 0.202861 0.544012 11.00000 0.04175 0.03957 = 0.02576 0.00273 0.00160 -0.00150 AFIX 13 H21 2 0.695539 0.032992 0.535969 11.00000 -1.20000 AFIX 0 C102 1 0.331991 0.368470 0.738299 11.00000 0.05318 0.03350 = 0.02915 0.00381 0.00581 -0.00176 C91 1 0.545035 0.805889 0.315280 11.00000 0.06668 0.03079 = 0.03223 0.00187 -0.00754 -0.00039 AFIX 43 H91 2 0.538397 0.965513 0.306716 11.00000 -1.20000 AFIX 0 N1 3 0.756044 0.278332 0.568002 11.00000 0.04897 0.03759 = 0.02171 0.00533 0.00107 0.00299 AFIX 137 H1A 2 0.786764 0.250043 0.552228 11.00000 -1.20000 H1B 2 0.764572 0.195904 0.592637 11.00000 -1.20000 H1C 2 0.754874 0.435156 0.573797 11.00000 -1.20000 AFIX 0 C71 1 0.588567 0.558141 0.380035 11.00000 0.04466 0.03873 = 0.02591 0.00519 0.00301 0.00337 C101 1 0.524959 0.629185 0.281163 11.00000 0.05151 0.03648 = 0.03169 0.00317 0.00079 -0.00135 C93 1 0.422317 0.222627 0.007077 11.00000 0.05509 0.03358 = 0.03010 0.00041 0.00290 0.00291 AFIX 43 H93 2 0.422193 0.386034 0.000577 11.00000 -1.20000 AFIX 0 C12 1 0.560748 0.430139 0.839056 11.00000 0.05178 0.03427 = 0.02633 0.00009 0.00623 -0.00702 C22 1 0.573776 0.239043 0.808951 11.00000 0.03985 0.03358 = 0.02388 -0.00179 0.00401 -0.00197 AFIX 13 H22 2 0.596165 0.107679 0.826098 11.00000 -1.20000 AFIX 0 C83 1 0.423529 0.174197 0.048052 11.00000 0.05522 0.03032 = 0.03477 -0.00422 0.00550 -0.00082 AFIX 43 H83 2 0.425807 0.307680 0.066130 11.00000 -1.20000 AFIX 0 C73 1 0.421825 -0.058919 0.069547 11.00000 0.05629 0.03569 = 0.02856 0.00175 0.00095 -0.00003 C72 1 0.273718 0.315655 0.637559 11.00000 0.04995 0.03532 = 0.02723 0.00012 0.00299 0.00401 C81 1 0.570755 0.776788 0.355803 11.00000 0.06570 0.02944 = 0.03520 0.00009 -0.00294 -0.00315 AFIX 43 H81 2 0.578895 0.918551 0.371542 11.00000 -1.20000 AFIX 0 C103 1 0.421128 0.063829 -0.030117 11.00000 0.04926 0.03700 = 0.03293 -0.00034 0.00377 0.00464 C13 1 0.878444 0.371159 0.840718 11.00000 0.04986 0.04266 = 0.02449 0.00278 0.00962 -0.00072 C82 1 0.288722 0.134371 0.671433 11.00000 0.07347 0.02932 = 0.03135 -0.00075 0.00220 -0.00031 AFIX 43 H82 2 0.280009 -0.023161 0.662208 11.00000 -1.20000 AFIX 0 C11 1 0.681102 0.354401 0.504509 11.00000 0.04249 0.04327 = 0.02482 -0.00057 0.00631 0.00243 C32 1 0.614104 0.312701 0.776242 11.00000 0.04216 0.04865 = 0.03307 0.00104 0.00943 -0.00105 AFIX 23 H32A 2 0.592056 0.442321 0.759082 11.00000 -1.20000 H32B 2 0.654507 0.376853 0.791450 11.00000 -1.20000 AFIX 0 C43 1 0.785393 0.047254 0.919029 11.00000 0.04542 0.06126 = 0.05067 0.01848 0.01703 0.00802 AFIX 13 H43 2 0.823495 -0.023445 0.936877 11.00000 -1.20000 AFIX 0 C41 1 0.577791 0.148416 0.554265 11.00000 0.04846 0.07269 = 0.05146 0.01743 0.01509 0.00854 AFIX 13 H41 2 0.563313 0.228947 0.526605 11.00000 -1.20000 AFIX 0 C23 1 0.859971 0.170599 0.867234 11.00000 0.04634 0.03785 = 0.02349 -0.00102 0.00195 -0.00152 AFIX 13 H23 2 0.845186 0.035010 0.848201 11.00000 -1.20000 AFIX 0 C61 1 0.531742 0.213797 0.584154 11.00000 0.06432 0.10714 = 0.10624 0.02146 0.04287 0.00907 AFIX 137 H61A 2 0.545778 0.141238 0.611863 11.00000 -1.50000 H61B 2 0.489345 0.156415 0.572413 11.00000 -1.50000 H61C 2 0.530669 0.385530 0.587289 11.00000 -1.50000 AFIX 0 C63 1 0.749352 -0.147846 0.892795 11.00000 0.07476 0.04881 = 0.12511 -0.00217 0.04365 -0.01280 AFIX 137 H63A 2 0.712272 -0.080894 0.874660 11.00000 -1.50000 H63B 2 0.735642 -0.265921 0.911645 11.00000 -1.50000 H63C 2 0.776915 -0.222447 0.875175 11.00000 -1.50000 AFIX 0 C33 1 0.807234 0.238977 0.891651 11.00000 0.04241 0.04207 = 0.03018 -0.00022 0.00436 -0.00001 AFIX 23 H33A 2 0.821902 0.375210 0.909986 11.00000 -1.20000 H33B 2 0.770291 0.292010 0.871042 11.00000 -1.20000 AFIX 0 C31 1 0.643560 0.237985 0.571806 11.00000 0.05343 0.05487 = 0.03034 0.00946 0.01412 0.00689 AFIX 23 H31A 2 0.658098 0.158694 0.599205 11.00000 -1.20000 H31B 2 0.640595 0.408676 0.577604 11.00000 -1.20000 AFIX 0 C51 1 0.577108 -0.115101 0.546267 11.00000 0.06792 0.07546 = 0.15884 -0.01263 0.02626 -0.02110 AFIX 137 H51A 2 0.596810 -0.196881 0.572044 11.00000 -1.50000 H51B 2 0.600731 -0.149807 0.523362 11.00000 -1.50000 H51C 2 0.533341 -0.168929 0.538227 11.00000 -1.50000 AFIX 0 C53 1 0.744792 0.160264 0.948057 11.00000 0.07446 0.10376 = 0.06283 0.00355 0.03457 -0.00569 AFIX 137 H53A 2 0.708277 0.237379 0.931015 11.00000 -1.50000 H53B 2 0.769826 0.277581 0.966045 11.00000 -1.50000 H53C 2 0.730086 0.038716 0.965832 11.00000 -1.50000 AFIX 0 C62 1 0.674043 -0.060835 0.768833 11.00000 0.10988 0.05088 = 0.10166 0.00142 0.06405 0.01044 AFIX 137 H62A 2 0.712832 0.016923 0.782672 11.00000 -1.50000 H62B 2 0.684419 -0.175968 0.748270 11.00000 -1.50000 H62C 2 0.653998 -0.141636 0.790132 11.00000 -1.50000 AFIX 0 C42 1 0.629159 0.121318 0.746365 11.00000 0.05719 0.05616 = 0.04414 -0.01559 0.02208 -0.01058 AFIX 13 H42 2 0.588822 0.040486 0.734093 11.00000 -1.20000 AFIX 0 C52 1 0.656764 0.232767 0.710498 11.00000 0.09253 0.11126 = 0.04231 0.00397 0.03461 0.00776 AFIX 137 H52A 2 0.626828 0.348235 0.695882 11.00000 -1.50000 H52B 2 0.664718 0.110181 0.690511 11.00000 -1.50000 H52C 2 0.696573 0.311858 0.721937 11.00000 -1.50000 AFIX 0 HKLF 4 REM REM R1 = 0.0500 for 4962 Fo > 4sig(Fo) and 0.0927 for all 7634 data REM 475 parameters refined using 1 restraints END WGHT 0.0492 0.0000 REM Highest difference peak 0.219, deepest hole -0.286, 1-sigma level 0.050 Q1 1 0.4439 0.4219 -0.0114 11.00000 0.05 0.22 Q2 1 0.4776 0.2556 0.8715 11.00000 0.05 0.20 Q3 1 0.5707 0.3518 0.3390 11.00000 0.05 0.19 Q4 1 0.9918 0.3632 0.8397 11.00000 0.05 0.19 Q5 1 0.4718 -0.0357 -0.0483 11.00000 0.05 0.18 Q6 1 0.5997 0.5330 0.7694 11.00000 0.05 0.17 Q7 1 0.5871 0.1340 0.3416 11.00000 0.05 0.16 Q8 1 0.3843 -0.2682 0.0480 11.00000 0.05 0.16 Q9 1 0.4637 0.7018 0.2787 11.00000 0.05 0.16 Q10 1 0.7646 0.3978 0.9475 11.00000 0.05 0.16 Q11 1 0.7317 0.2705 0.6930 11.00000 0.05 0.15 Q12 1 0.7335 0.7583 0.5281 11.00000 0.05 0.15 Q13 1 0.5502 0.5372 0.4195 11.00000 0.05 0.15 Q14 1 0.4990 0.5568 0.5614 11.00000 0.05 0.15 Q15 1 0.5986 -0.4705 0.5165 11.00000 0.05 0.15 Q16 1 0.4471 -0.3309 0.0571 11.00000 0.05 0.15 Q17 1 0.4709 0.2672 -0.0679 11.00000 0.05 0.15 Q18 1 0.5836 0.2851 0.2722 11.00000 0.05 0.15 Q19 1 0.6271 -0.1306 0.5104 11.00000 0.05 0.15 Q20 1 0.6312 0.4598 0.3481 11.00000 0.05 0.15 ; _shelx_res_checksum 22778 _shelx_hkl_file ; 0 -6 0 10.9982 3.23096 1 0 -6 0 7.99890 3.03941 1 0 -6 0 4.06073 2.16164 2 0 -6 -1 2.85442 1.69147 1 0 -6 -1 0.40917 0.96186 1 0 -6 1 2.07447 1.85543 1 0 -6 1 1.74132 1.69324 2 0 -6 -1 1.81483 1.45051 2 0 -6 1 1.49393 1.51128 1 0 -6 -2 11.2887 3.59729 2 0 -6 -2 8.41344 3.09359 1 0 -6 -2 11.6535 3.51629 1 0 -6 2 14.1583 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0 50.3123 6.83295 2 -1 -5 0 49.2401 6.56936 2 -1 -5 0 49.5716 6.33082 1 -1 -5 -1 32.6687 4.94644 1 1 -5 1 28.2194 4.97078 2 1 -5 1 35.3297 4.78185 1 -1 -5 -1 35.0520 5.84002 2 1 -5 1 31.0363 4.53523 1 -1 -5 -1 33.1468 5.06042 1 1 -5 2 5.72406 1.98130 1 -1 -5 -2 6.63855 2.47313 2 -1 -5 -2 7.50999 2.72878 1 -1 -5 -2 6.87157 2.26816 1 1 -5 2 9.85727 2.90508 2 1 -5 2 10.0179 2.43376 1 -1 -5 -3 35.9650 5.62539 1 1 -5 3 30.4052 4.30727 1 1 -5 3 35.9408 5.72394 2 1 -5 3 38.8771 4.73252 1 -1 -5 -3 35.9182 5.63975 1 -1 -5 -3 33.8350 5.76099 2 1 -5 4 10.6704 2.19883 1 -1 -5 -4 11.6266 3.44982 1 -1 -5 -4 10.6497 3.33663 2 -1 -5 -4 12.6935 3.41306 1 1 -5 4 8.60990 2.09379 1 1 -5 4 13.2147 3.18120 2 -1 -5 -5 17.6835 4.08441 1 1 -5 5 19.8606 3.30739 1 1 -5 5 20.2119 3.37277 1 -1 -5 -5 18.4038 4.39129 2 1 -5 5 18.0708 4.01814 2 -1 -5 -5 17.2359 4.03151 1 1 -5 6 19.3700 3.07341 1 -1 -5 -6 19.6003 4.63384 2 1 -5 6 19.2559 3.16573 1 -1 -5 -6 22.4700 4.49499 1 -1 -5 -6 19.3294 4.38296 1 1 -5 6 18.0137 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30.1145 3.65998 2 -11 1 1 30.9632 3.42939 1 -11 1 1 31.7027 4.50012 2 -11 1 0 32.4428 4.60196 2 11 1 0 33.5484 4.52505 1 11 1 0 31.9435 3.75105 2 -11 1 0 29.9914 3.41772 1 -11 1 -1 48.7070 5.50888 2 11 1 1 44.5001 4.77987 2 11 1 1 44.8549 5.20675 1 -11 1 -1 45.6433 4.09162 1 -11 1 -2 9.74545 1.95942 1 11 1 2 10.3995 2.57050 1 -11 1 -2 9.77569 2.75524 2 11 1 2 7.61661 1.99942 2 11 1 3 3.78833 1.83462 1 -11 1 -3 3.14076 1.45016 2 -11 1 -3 4.96267 1.44324 1 11 1 3 3.80213 1.57723 2 -11 1 -4 11.3062 2.13939 1 -11 1 -4 10.1742 2.59287 2 11 1 4 11.0610 2.62708 2 -11 1 -5 21.0342 3.69504 2 11 1 5 23.4946 3.81381 2 -11 1 -5 22.0587 2.89954 1 -11 1 -6 96.5796 8.20949 2 -11 1 -6 83.2642 5.63279 1 11 1 6 87.2957 7.64781 2 -11 1 -6 89.9501 5.89433 1 -11 1 -7 59.2103 6.44338 2 -11 1 -7 46.0131 4.27101 1 11 1 7 49.4205 5.88804 2 -11 1 -7 51.9615 4.44186 1 -11 1 -8 101.722 6.30024 1 -11 1 -8 108.134 9.00775 2 -11 1 -8 120.591 6.59067 1 -11 1 -9 2.80539 1.85953 2 -11 1 -9 0.71071 0.62264 1 -11 1 -9 2.75859 1.41752 1 -11 1 -10 4.10711 1.40450 1 -11 1 -10 2.17416 1.44702 2 -11 1 -10 2.38328 1.20512 1 -11 1 -11 11.9269 3.13054 2 -11 1 -11 11.2124 2.20812 1 -11 1 -11 8.83437 2.02618 1 -11 1 -12 59.7501 5.42011 1 -11 1 -12 67.8715 7.78176 2 -11 1 -12 57.6623 5.02035 1 -11 1 -13 7.40082 1.94013 1 -11 1 -13 6.99343 1.99107 1 -11 1 -13 8.69375 2.92102 2 -11 1 -14 19.8507 4.13761 2 -11 1 -14 20.4795 3.36284 1 -11 1 -14 19.5197 3.06542 1 -11 1 -15 16.9021 2.82786 1 -11 1 -15 19.5528 4.38494 2 -11 1 -15 21.2979 3.37665 1 -11 1 -16 38.0366 4.46858 1 -11 1 -16 44.7255 6.49488 2 -11 1 -16 37.7378 4.66275 1 -11 1 -17 92.8948 6.97928 1 -11 1 -17 106.065 10.2881 2 -11 1 -17 106.203 8.06243 1 -11 1 -18 9.23594 2.48611 1 -11 1 -18 9.03508 2.98230 2 -11 1 -18 9.41930 2.61691 1 -11 1 -19 29.5652 4.00926 1 -11 1 -19 33.3222 6.05703 2 -11 1 -19 30.2601 4.55488 1 -11 1 -20 47.6883 5.24945 1 -11 1 -20 50.0815 7.29516 2 -11 1 -20 47.8629 5.86334 1 -11 1 -21 50.6286 5.56725 1 -11 1 -21 53.9325 7.66902 2 11 1 21 57.3176 7.87432 1 -11 1 -21 52.7056 6.30453 1 -11 1 -22 1.92144 1.11877 1 -11 1 -22 4.18916 1.86225 1 11 1 22 4.15427 2.29095 1 -11 1 -22 2.09624 1.82400 2 -11 1 -23 13.6031 3.58140 1 -11 1 -23 7.23501 2.30460 1 -11 1 -23 12.7807 4.21293 2 11 1 23 6.81367 2.75436 1 -11 1 -24 3.15377 1.80619 1 -11 1 -24 5.60371 2.86464 2 11 1 24 4.24414 2.90712 1 -11 1 -25 1.04885 1.30540 2 -11 1 -25 1.29565 0.82158 1 11 1 25-1.43547 1.79658 1 -11 1 -26 1.00879 1.20787 1 -11 1 -26 4.66864 2.78651 2 11 1 26 1.35247 1.51526 1 -11 1 -27 4.88693 2.96576 2 -11 1 -27 4.13641 2.24010 1 11 1 27 3.89746 2.59253 1 -11 1 -28 1.88510 2.13860 2 -11 1 -28 0.82287 0.93972 1 11 1 28 1.73579 2.03691 1 -11 1 -29-0.38184 2.06754 2 -11 1 -29 1.59028 1.53106 1 11 1 29-4.26416 3.33746 1 -11 1 -30 3.33844 2.14547 1 -11 1 -30 3.44255 2.92750 2 11 1 30 6.54693 3.39259 1 -11 1 -31 0.96217 1.39465 2 -11 1 -31-1.18509 1.38685 1 11 1 31 1.53689 1.57814 1 -11 1 -32 1.72774 2.57430 2 -11 1 -32 1.20937 1.85901 1 11 1 32-0.52802 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3.49025 3.00636 1 28 0 4 0.46613 2.35830 2 -28 0 -4-1.68884 3.17972 1 -28 0 -5 2.23763 3.43461 2 -28 0 -5 0.28567 2.90058 1 28 0 5 0.66249 2.29899 2 -28 0 -5-0.42309 2.64843 1 -28 0 -6-4.46541 4.41409 2 -28 0 -6 2.09664 3.15156 1 28 0 6-1.27301 2.31151 2 -28 0 -6 2.27804 3.79391 1 -28 0 -7 2.28615 2.85156 2 -28 0 -7 0.03238 1.98390 1 28 0 7 1.84641 2.60363 2 -28 0 -7-1.95351 2.55789 1 -28 0 -8-4.70464 3.10933 1 -28 2 17-10.3537 4.49819 1 28 2 -17-1.45384 4.23953 1 -28 2 16 3.06763 3.74328 2 -28 2 16-0.07180 2.31252 1 28 2 -16 2.66406 3.42441 1 -28 2 15-2.30318 4.46666 2 -28 2 15 0.41444 2.91719 1 28 2 -15-5.89802 4.38930 1 28 2 -14-1.35864 3.20653 1 -28 2 14 0.50498 2.39042 2 -28 2 14 0.03357 3.22655 1 -28 2 13 1.95738 3.33555 2 28 2 -13 0.41777 2.52106 1 -28 2 13 0.68155 2.61252 1 -28 2 12-3.31643 3.72585 2 28 2 -12-7.48302 4.44690 1 -28 2 12-0.44442 2.76843 1 -28 2 11-1.72134 2.51963 2 28 2 -11 1.37567 3.15748 1 -28 2 11 1.98703 3.47222 1 -28 2 10-2.46659 3.62840 2 -28 2 10 1.36620 2.91934 1 28 2 -10 4.44059 4.34296 1 28 2 -9-6.97139 4.93796 1 -28 2 9 2.04678 2.77921 2 -28 2 9-1.37023 3.40854 1 -28 2 8 0.34383 2.25862 2 28 2 -8 1.03649 2.31752 1 -28 2 8-0.02890 1.58000 1 -28 2 7-0.08543 2.95014 2 -28 2 7 1.03934 2.76398 1 28 2 -7 0.16461 2.33621 1 -28 2 6-1.94838 2.25719 2 28 2 -6-2.40850 2.68867 1 -28 2 6 0.02760 2.48538 1 28 2 -5-1.58819 2.72909 1 -28 2 5 3.07019 3.52321 2 -28 2 5 0.32530 2.38831 1 -28 2 4 2.28219 2.58169 2 -28 2 4 0.02665 1.74989 1 -28 2 3 5.87545 5.39637 2 -28 2 3 0.02592 1.84146 1 -28 2 2-2.75874 3.83819 2 -28 2 2 0.50407 2.43471 1 -28 2 1 4.51177 4.04347 2 -28 2 1-0.02446 2.55376 1 -28 2 0-0.36696 2.82631 2 -28 2 0-4.21110 2.75758 1 -28 2 0 0.02367 2.13894 1 -28 2 -1 1.14049 2.95360 2 -28 2 -1-3.71207 2.51096 1 -28 2 -1 0.02323 2.02503 1 -28 2 -2-0.41131 2.20400 2 -28 2 -2 0.02289 2.09908 1 -28 2 -2-0.78944 2.25156 1 -28 2 -3 0.02222 2.04153 1 -28 2 -3 6.10679 3.25093 1 -29 -1 15 7.56449 6.59863 1 29 -1 -15 0.30063 3.65264 1 -29 -1 15 10.1006 4.95608 2 29 -1 -15 1.19016 4.07360 2 -29 -1 14 6.52854 5.08285 1 -29 -1 14 1.16653 2.30071 2 29 -1 -14 0.59847 2.84584 1 29 -1 -14-0.43439 1.52312 2 -29 -1 13 3.18844 3.99384 1 -29 -1 13 0.72848 1.90250 2 29 -1 -13-4.24624 3.91551 1 29 -1 -13 0.50776 2.87411 2 -29 -1 12-0.65104 2.23387 1 -29 -1 12 0.84400 1.78905 2 29 -1 -12 1.67929 2.98421 1 29 -1 -12 0.62367 2.94817 2 -29 -1 11 0.45045 2.69036 1 -29 -1 11-2.81328 2.98699 2 29 -1 -11-0.32103 1.97264 1 29 -1 -11 0.91468 2.70834 2 -29 -1 10-2.35822 3.77540 1 -29 -1 10-0.09211 2.48210 2 29 -1 -10 2.26399 3.38788 2 29 -1 -10-1.04718 2.25236 1 -29 -1 9-2.92196 4.41012 1 -29 -1 9-0.51117 1.68295 2 29 -1 -9-2.54388 3.55452 2 29 -1 -9-0.13677 2.40260 1 29 -1 -8-0.70485 2.14681 1 -29 -1 8-0.11821 3.41803 1 -29 -1 8 1.42734 2.47683 2 29 -1 -8-0.99189 2.60033 2 -29 -1 7-0.46749 3.27114 1 -29 -1 7 0.03318 3.17210 2 29 -1 -7 0.52866 2.61342 1 29 -1 -7-1.16772 2.08337 2 -29 -1 6 0.03321 2.41802 2 -29 -1 6 1.35203 2.35273 1 29 -1 -6-0.85262 1.79146 1 29 -1 -6-0.20428 1.85304 2 -29 -1 5-1.00517 2.88727 2 -29 -1 5-0.79710 2.23143 1 29 -1 -5 0.54778 2.18854 2 29 -1 -5 0.84447 2.71911 1 -29 -1 4-0.03569 2.60579 2 -29 -1 4-0.81154 3.44371 1 29 -1 -4 3.37108 3.27239 1 29 -1 -4 9.05891 5.30743 2 29 -1 -3-0.66081 2.71775 1 -29 -1 3-0.80474 1.97937 2 -29 -1 3 1.20824 2.99353 1 29 -1 -3 0.55692 2.70650 2 -29 -1 2-0.44304 1.91494 2 -29 -1 2-0.15607 3.13592 1 29 -1 -2-1.19677 2.29114 2 29 -1 -2-0.21852 2.00306 1 -29 -1 2 1.66919 2.98411 1 -29 -1 1 0.30430 2.63357 2 -29 -1 1-0.81490 3.29416 1 29 -1 -1 2.58444 2.92600 2 -29 -1 1 6.14275 5.54471 1 -29 -1 0 3.90163 4.19219 2 -29 -1 0 2.48776 3.58654 1 29 -1 0 1.70657 3.38912 2 -29 -1 0 0.74308 2.93821 1 -29 -1 -1-2.68553 5.05627 2 -29 -1 -1-7.63383 4.15730 1 29 -1 1 1.10838 2.70893 2 -29 -1 -1-2.25662 3.57055 1 -29 1 15 5.81674 4.89337 2 29 1 -15 8.29145 5.14782 1 29 1 -15 8.08468 3.87652 2 -29 1 15 0.44530 3.68637 1 -29 1 14 3.83537 3.74804 2 29 1 -14 0.02387 2.44615 2 29 1 -14 8.61734 5.13413 1 -29 1 14 1.26575 3.83707 1 -29 1 13 1.14235 3.62394 2 29 1 -13 0.24550 2.27362 2 -29 1 13-0.17675 2.76964 1 29 1 -13 0.16478 2.37369 1 29 1 -12-3.00485 3.19129 1 -29 1 12 1.59909 2.96735 2 29 1 -12 0.02528 1.43939 2 -29 1 12-0.55498 2.72966 1 -29 1 11 2.19877 3.25215 2 29 1 -11 2.07654 3.81327 1 29 1 -11 0.02608 2.61692 2 -29 1 11 1.16905 2.48916 1 -29 1 10 1.86797 3.30034 2 29 1 -10 5.63077 3.95989 1 29 1 -10 0.16084 1.99807 2 -29 1 10-5.24620 3.32380 1 -29 1 9 3.60875 4.24508 2 29 1 -9-0.59868 3.11903 1 29 1 -9 0.63376 2.08792 2 -29 1 9 2.56267 3.96394 1 -29 1 8-3.55013 3.70276 2 29 1 -8-0.25272 1.74281 2 29 1 -8-4.12639 3.60197 1 -29 1 8 0.32391 2.61554 1 -29 1 7 2.99341 3.47583 2 29 1 -7-3.13405 3.40051 1 29 1 -7-0.40314 1.51610 2 -29 1 7 0.88726 2.72481 1 -29 1 6 1.65509 3.47472 2 29 1 -6 4.29682 3.72147 1 29 1 -6 0.20550 2.06500 2 -29 1 6 0.12456 2.17624 1 -29 1 5-0.21165 2.97818 2 29 1 -5 7.85077 4.50713 1 29 1 -5 0.92004 1.75791 2 -29 1 5 1.81285 3.33011 1 -29 1 4-1.57505 3.44769 2 29 1 -4 3.22297 2.69350 1 29 1 -4 1.25486 3.16884 2 -29 1 4-0.27504 3.05045 1 -29 1 3-0.17173 2.33363 2 29 1 -3-1.38085 2.92915 2 -29 1 3-0.94786 3.08216 1 -29 1 2 3.12630 3.77866 2 29 1 -2-0.19789 2.15832 2 -29 1 2-0.03039 3.12519 1 -29 1 1 0.27007 2.14229 1 -29 1 1 3.28436 3.81697 2 29 1 -1 0.84415 2.59533 2 -29 1 1 1.70755 2.51795 1 -29 1 0 0.88486 3.78698 1 -29 1 0-1.01424 3.29809 2 29 1 0-0.44755 2.12417 2 -29 1 0-0.39543 2.68407 1 -29 1 -1 0.02890 2.83465 1 -29 1 -1 0.95162 4.68885 2 29 1 1 0.59706 2.12946 2 -29 1 -1 4.97075 3.56935 1 0 0 0 0.00 0.00 0 TITL L_Leu_mal_200 in C2 REM C2 (#5 in standard setting) CELL 0.71073 21.456325 5.672508 32.077875 90.0000 99.6527 90.0000 ZERR 12.00 0.000863 0.000190 0.000836 0.0000 0.0034 0.0000 LATT -7 SYMM -x, y,-z SFAC C H N O UNIT 120.00 204.00 12.00 72.00 TREF HKLF 4 END ; _shelx_hkl_checksum 99557 _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 1.413 _oxdiff_exptl_absorpt_empirical_full_min 0.792 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn O51 O 0.50070(16) 0.7011(6) 0.24581(9) 0.0482(9) Uani 1 1 d . O21 O 0.70295(14) 0.5512(6) 0.50303(9) 0.0409(8) Uani 1 1 d . O31 O 0.61248(15) 0.5830(6) 0.41794(9) 0.0474(9) Uani 1 1 d . O42 O 0.28029(15) 0.5360(6) 0.64730(9) 0.0406(8) Uani 1 1 d . O61 O 0.53213(16) 0.4077(5) 0.28918(9) 0.0435(8) Uani 1 1 d . H61 H 0.546326 0.388773 0.314999 0.065 Uiso 1 1 calc GR O52 O 0.35374(17) 0.3417(6) 0.77632(10) 0.0533(9) Uani 1 1 d . O22 O 0.51033(15) 0.4492(6) 0.85034(10) 0.0454(8) Uani 1 1 d . N2 N 0.51034(16) 0.1497(7) 0.78847(11) 0.0361(9) Uani 1 1 d . H2A H 0.492890 0.252547 0.768028 0.043 Uiso 1 1 calc GR H2B H 0.484732 0.136189 0.808268 0.043 Uiso 1 1 calc GR H2C H 0.514842 0.006163 0.776672 0.043 Uiso 1 1 calc GR O12 O 0.60979(16) 0.5660(7) 0.85196(11) 0.0561(10) Uani 1 1 d . H12 H 0.600421 0.664945 0.869396 0.084 Uiso 1 1 calc GR O53 O 0.41468(16) 0.1504(6) -0.06571(9) 0.0471(8) Uani 1 1 d . O33 O 0.41350(16) -0.0596(6) 0.10663(9) 0.0483(8) Uani 1 1 d . O62 O 0.32635(17) 0.5759(6) 0.72173(9) 0.0447(8) Uani 1 1 d . H62 H 0.308167 0.566022 0.696481 0.067 Uiso 1 1 calc GR O63 O 0.4263(2) -0.1592(6) -0.02430(10) 0.0592(11) Uani 1 1 d . H63 H 0.428168 -0.189300 0.001519 0.089 Uiso 1 1 calc GR N3 N 0.91862(16) 0.0986(7) 0.89658(11) 0.0368(9) Uani 1 1 d . H3A H 0.951646 0.093227 0.882129 0.044 Uiso 1 1 calc GR H3B H 0.912820 -0.046361 0.907461 0.044 Uiso 1 1 calc GR H3C H 0.927052 0.205156 0.917988 0.044 Uiso 1 1 calc GR O13 O 0.82834(16) 0.4657(7) 0.81659(11) 0.0550(9) Uani 1 1 d . H13 H 0.839954 0.578082 0.802657 0.082 Uiso 1 1 calc GR O32 O 0.25484(16) 0.2475(6) 0.60096(9) 0.0506(9) Uani 1 1 d . O11 O 0.64239(17) 0.2518(7) 0.47347(10) 0.0516(9) Uani 1 1 d . H11 H 0.630723 0.350461 0.454212 0.077 Uiso 1 1 calc GR O41 O 0.57998(15) 0.3543(6) 0.36258(10) 0.0417(8) Uani 1 1 d . O23 O 0.93192(16) 0.4361(7) 0.84169(10) 0.0516(9) Uani 1 1 d . O43 O 0.4308(2) -0.2498(6) 0.04989(10) 0.0689(12) Uani 1 1 d . C92 C 0.3123(2) 0.1556(9) 0.71253(14) 0.0454(12) Uani 1 1 d . H92 H 0.317314 0.011156 0.727708 0.055 Uiso 1 1 calc R C21 C 0.6937(2) 0.2029(9) 0.54401(13) 0.0362(10) Uani 1 1 d . H21 H 0.695539 0.032992 0.535969 0.043 Uiso 1 1 calc R C102 C 0.3320(2) 0.3685(8) 0.73830(14) 0.0387(11) Uani 1 1 d . C91 C 0.5450(2) 0.8059(8) 0.31528(14) 0.0451(12) Uani 1 1 d . H91 H 0.538397 0.965513 0.306716 0.054 Uiso 1 1 calc R N1 N 0.75604(16) 0.2783(7) 0.56800(10) 0.0366(9) Uani 1 1 d . H1A H 0.786764 0.250043 0.552228 0.044 Uiso 1 1 calc GR H1B H 0.764572 0.195904 0.592637 0.044 Uiso 1 1 calc GR H1C H 0.754874 0.435156 0.573797 0.044 Uiso 1 1 calc GR C71 C 0.5886(2) 0.5581(9) 0.38003(13) 0.0368(10) Uani 1 1 d . C101 C 0.5250(2) 0.6292(8) 0.28116(14) 0.0406(11) Uani 1 1 d . C93 C 0.4223(2) 0.2226(9) 0.00708(13) 0.0401(11) Uani 1 1 d . H93 H 0.422193 0.386034 0.000577 0.048 Uiso 1 1 calc R C12 C 0.5607(2) 0.4301(8) 0.83906(13) 0.0375(10) Uani 1 1 d . C22 C 0.57378(19) 0.2390(8) 0.80895(13) 0.0326(9) Uani 1 1 d . H22 H 0.596165 0.107679 0.826098 0.039 Uiso 1 1 calc R C83 C 0.4235(2) 0.1742(8) 0.04805(14) 0.0403(11) Uani 1 1 d . H83 H 0.425807 0.307680 0.066130 0.048 Uiso 1 1 calc R C73 C 0.4218(2) -0.0589(9) 0.06955(14) 0.0409(11) Uani 1 1 d . C72 C 0.2737(2) 0.3157(8) 0.63756(14) 0.0379(11) Uani 1 1 d . C81 C 0.5708(2) 0.7768(9) 0.35580(15) 0.0448(12) Uani 1 1 d . H81 H 0.578895 0.918551 0.371542 0.054 Uiso 1 1 calc R C103 C 0.4211(2) 0.0638(9) -0.03012(14) 0.0401(11) Uani 1 1 d . C13 C 0.8784(2) 0.3712(9) 0.84072(13) 0.0386(11) Uani 1 1 d . C82 C 0.2887(2) 0.1344(8) 0.67143(14) 0.0455(12) Uani 1 1 d . H82 H 0.280009 -0.023161 0.662208 0.055 Uiso 1 1 calc R C11 C 0.6811(2) 0.3544(9) 0.50451(13) 0.0368(10) Uani 1 1 d . C32 C 0.6141(2) 0.3127(8) 0.77624(14) 0.0409(11) Uani 1 1 d . H32A H 0.592056 0.442321 0.759082 0.049 Uiso 1 1 calc R H32B H 0.654507 0.376853 0.791450 0.049 Uiso 1 1 calc R C43 C 0.7854(2) 0.0473(10) 0.91903(17) 0.0514(13) Uani 1 1 d . H43 H 0.823495 -0.023445 0.936877 0.062 Uiso 1 1 calc R C41 C 0.5778(2) 0.1484(11) 0.55426(18) 0.0568(15) Uani 1 1 d . H41 H 0.563313 0.228947 0.526605 0.068 Uiso 1 1 calc R C23 C 0.8600(2) 0.1706(8) 0.86723(13) 0.0363(10) Uani 1 1 d . H23 H 0.845186 0.035010 0.848201 0.044 Uiso 1 1 calc R C61 C 0.5317(3) 0.2138(15) 0.5842(2) 0.089(2) Uani 1 1 d . H61A H 0.545778 0.141238 0.611863 0.134 Uiso 1 1 calc GR H61B H 0.489345 0.156415 0.572413 0.134 Uiso 1 1 calc GR H61C H 0.530669 0.385530 0.587289 0.134 Uiso 1 1 calc GR C63 C 0.7494(3) -0.1478(11) 0.8928(2) 0.080(2) Uani 1 1 d . H63A H 0.712272 -0.080894 0.874660 0.120 Uiso 1 1 calc GR H63B H 0.735642 -0.265921 0.911645 0.120 Uiso 1 1 calc GR H63C H 0.776915 -0.222447 0.875175 0.120 Uiso 1 1 calc GR C33 C 0.8072(2) 0.2390(9) 0.89165(14) 0.0384(11) Uani 1 1 d . H33A H 0.821902 0.375210 0.909986 0.046 Uiso 1 1 calc R H33B H 0.770291 0.292010 0.871042 0.046 Uiso 1 1 calc R C31 C 0.6436(2) 0.2380(10) 0.57181(14) 0.0454(12) Uani 1 1 d . H31A H 0.658098 0.158694 0.599205 0.054 Uiso 1 1 calc R H31B H 0.640595 0.408676 0.577604 0.054 Uiso 1 1 calc R C51 C 0.5771(3) -0.1151(13) 0.5463(3) 0.100(3) Uani 1 1 d . H51A H 0.596810 -0.196881 0.572044 0.150 Uiso 1 1 calc GR H51B H 0.600731 -0.149807 0.523362 0.150 Uiso 1 1 calc GR H51C H 0.533341 -0.168929 0.538227 0.150 Uiso 1 1 calc GR C53 C 0.7448(3) 0.1603(14) 0.94806(19) 0.078(2) Uani 1 1 d . H53A H 0.708277 0.237379 0.931015 0.117 Uiso 1 1 calc GR H53B H 0.769826 0.277581 0.966045 0.117 Uiso 1 1 calc GR H53C H 0.730086 0.038716 0.965832 0.117 Uiso 1 1 calc GR C62 C 0.6740(3) -0.0608(11) 0.7688(2) 0.082(2) Uani 1 1 d . H62A H 0.712832 0.016923 0.782672 0.123 Uiso 1 1 calc GR H62B H 0.684419 -0.175968 0.748270 0.123 Uiso 1 1 calc GR H62C H 0.653998 -0.141636 0.790132 0.123 Uiso 1 1 calc GR C42 C 0.6292(2) 0.1213(10) 0.74637(16) 0.0509(14) Uani 1 1 d . H42 H 0.588822 0.040486 0.734093 0.061 Uiso 1 1 calc R C52 C 0.6568(3) 0.2328(14) 0.71050(18) 0.079(2) Uani 1 1 d . H52A H 0.626828 0.348235 0.695882 0.119 Uiso 1 1 calc GR H52B H 0.664718 0.110181 0.690511 0.119 Uiso 1 1 calc GR H52C H 0.696573 0.311858 0.721937 0.119 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 O51 0.066(2) 0.046(2) 0.0279(17) 0.0027(16) -0.0041(15) -0.0026(18) O21 0.0531(19) 0.0402(19) 0.0276(16) 0.0048(15) 0.0011(14) -0.0057(17) O31 0.063(2) 0.051(2) 0.0243(16) 0.0059(16) -0.0040(15) -0.0042(19) O42 0.062(2) 0.0328(17) 0.0250(16) 0.0014(14) 0.0013(14) 0.0030(16) O61 0.066(2) 0.0335(19) 0.0263(16) -0.0001(14) -0.0046(15) -0.0007(17) O52 0.083(2) 0.046(2) 0.0256(17) 0.0046(15) -0.0053(16) -0.0041(19) O22 0.051(2) 0.051(2) 0.0384(18) -0.0089(17) 0.0169(15) 0.0002(18) N2 0.044(2) 0.037(2) 0.0267(19) -0.0022(17) 0.0061(16) -0.0025(18) O12 0.061(2) 0.061(2) 0.049(2) -0.024(2) 0.0155(17) -0.017(2) O53 0.064(2) 0.050(2) 0.0257(17) 0.0043(15) 0.0022(14) -0.0008(18) O33 0.074(2) 0.0442(19) 0.0283(17) 0.0055(16) 0.0118(16) 0.0075(19) O62 0.073(2) 0.0319(17) 0.0246(16) 0.0001(14) -0.0037(16) 0.0032(17) O63 0.110(3) 0.038(2) 0.0257(18) -0.0013(15) 0.002(2) 0.010(2) N3 0.046(2) 0.040(2) 0.0251(19) -0.0002(17) 0.0075(16) 0.0011(19) O13 0.061(2) 0.060(2) 0.041(2) 0.0204(18) 0.0010(17) 0.003(2) O32 0.074(2) 0.048(2) 0.0258(17) -0.0042(16) -0.0048(15) 0.0003(19) O11 0.066(2) 0.052(2) 0.0299(18) 0.0067(16) -0.0117(16) -0.0157(19) O41 0.060(2) 0.0312(16) 0.0319(17) 0.0040(14) 0.0009(15) 0.0009(16) O23 0.055(2) 0.058(2) 0.044(2) 0.0122(19) 0.0157(16) -0.002(2) O43 0.146(4) 0.0307(19) 0.0312(19) 0.0018(16) 0.018(2) 0.013(2) C92 0.073(3) 0.030(2) 0.031(3) 0.004(2) 0.006(2) 0.006(2) C21 0.042(2) 0.040(3) 0.026(2) 0.003(2) 0.0016(18) -0.002(2) C102 0.053(3) 0.034(2) 0.029(2) 0.004(2) 0.006(2) -0.002(2) C91 0.067(3) 0.031(3) 0.032(3) 0.002(2) -0.008(2) 0.000(2) N1 0.049(2) 0.038(2) 0.0217(18) 0.0053(16) 0.0011(16) 0.0030(18) C71 0.045(3) 0.039(3) 0.026(2) 0.005(2) 0.0030(19) 0.003(2) C101 0.052(3) 0.036(3) 0.032(3) 0.003(2) 0.001(2) -0.001(2) C93 0.055(3) 0.034(2) 0.030(2) 0.000(2) 0.003(2) 0.003(2) C12 0.052(3) 0.034(2) 0.026(2) 0.000(2) 0.006(2) -0.007(2) C22 0.040(2) 0.034(2) 0.024(2) -0.0018(19) 0.0040(18) -0.002(2) C83 0.055(3) 0.030(2) 0.035(3) -0.004(2) 0.006(2) -0.001(2) C73 0.056(3) 0.036(2) 0.029(2) 0.002(2) 0.001(2) 0.000(2) C72 0.050(3) 0.035(3) 0.027(2) 0.0001(19) 0.003(2) 0.004(2) C81 0.066(3) 0.029(2) 0.035(3) 0.000(2) -0.003(2) -0.003(2) C103 0.049(3) 0.037(3) 0.033(3) 0.000(2) 0.004(2) 0.005(2) C13 0.050(3) 0.043(3) 0.024(2) 0.003(2) 0.010(2) -0.001(2) C82 0.073(3) 0.029(2) 0.031(3) -0.001(2) 0.002(2) 0.000(2) C11 0.042(2) 0.043(3) 0.025(2) -0.001(2) 0.0063(19) 0.002(2) C32 0.042(3) 0.049(3) 0.033(3) 0.001(2) 0.009(2) -0.001(2) C43 0.045(3) 0.061(3) 0.051(3) 0.018(3) 0.017(2) 0.008(3) C41 0.048(3) 0.073(4) 0.051(3) 0.017(3) 0.015(2) 0.009(3) C23 0.046(2) 0.038(3) 0.023(2) -0.001(2) 0.0019(18) -0.002(2) C61 0.064(4) 0.107(6) 0.106(6) 0.021(5) 0.043(4) 0.009(4) C63 0.075(4) 0.049(3) 0.125(6) -0.002(4) 0.044(4) -0.013(3) C33 0.042(2) 0.042(3) 0.030(2) 0.000(2) 0.0044(19) 0.000(2) C31 0.053(3) 0.055(3) 0.030(2) 0.009(2) 0.014(2) 0.007(3) C51 0.068(4) 0.075(5) 0.159(8) -0.013(5) 0.026(5) -0.021(4) C53 0.074(4) 0.104(6) 0.063(4) 0.004(4) 0.035(3) -0.006(4) C62 0.110(5) 0.051(4) 0.102(5) 0.001(4) 0.064(4) 0.010(4) C42 0.057(3) 0.056(3) 0.044(3) -0.016(3) 0.022(2) -0.011(3) C52 0.093(4) 0.111(6) 0.042(3) 0.004(4) 0.035(3) 0.008(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C101 O61 H61 109.5 H2A N2 H2B 109.5 H2A N2 H2C 109.5 H2B N2 H2C 109.5 C22 N2 H2A 109.5 C22 N2 H2B 109.5 C22 N2 H2C 109.5 C12 O12 H12 109.5 C102 O62 H62 109.5 C103 O63 H63 109.5 H3A N3 H3B 109.5 H3A N3 H3C 109.5 H3B N3 H3C 109.5 C23 N3 H3A 109.5 C23 N3 H3B 109.5 C23 N3 H3C 109.5 C13 O13 H13 109.5 C11 O11 H11 109.5 C102 C92 H92 114.8 C82 C92 H92 114.8 C82 C92 C102 130.4(5) N1 C21 H21 109.9 N1 C21 C11 106.7(4) N1 C21 C31 108.8(3) C11 C21 H21 109.9 C11 C21 C31 111.8(4) C31 C21 H21 109.9 O52 C102 O62 120.8(4) O52 C102 C92 118.2(4) O62 C102 C92 121.0(4) C101 C91 H91 114.6 C81 C91 H91 114.6 C81 C91 C101 130.7(4) C21 N1 H1A 109.5 C21 N1 H1B 109.5 C21 N1 H1C 109.5 H1A N1 H1B 109.5 H1A N1 H1C 109.5 H1B N1 H1C 109.5 O31 C71 O41 122.2(4) O31 C71 C81 116.5(4) O41 C71 C81 121.3(4) O51 C101 O61 121.6(4) O51 C101 C91 118.5(4) O61 C101 C91 119.9(4) C83 C93 H93 114.5 C83 C93 C103 131.0(4) C103 C93 H93 114.5 O22 C12 O12 124.5(4) O22 C12 C22 122.0(4) O12 C12 C22 113.5(4) N2 C22 C12 105.8(4) N2 C22 H22 107.9 N2 C22 C32 111.7(3) C12 C22 H22 107.9 C12 C22 C32 115.5(4) C32 C22 H22 107.9 C93 C83 H83 115.2 C93 C83 C73 129.5(4) C73 C83 H83 115.2 O33 C73 O43 122.0(5) O33 C73 C83 117.8(4) O43 C73 C83 120.2(4) O42 C72 C82 119.3(4) O32 C72 O42 122.5(4) O32 C72 C82 118.2(4) C91 C81 C71 130.1(4) C91 C81 H81 115.0 C71 C81 H81 115.0 O53 C103 O63 121.6(5) O53 C103 C93 119.1(4) O63 C103 C93 119.4(4) O13 C13 C23 111.6(4) O23 C13 O13 124.6(4) O23 C13 C23 123.8(4) C92 C82 C72 131.0(5) C92 C82 H82 114.5 C72 C82 H82 114.5 O21 C11 O11 125.0(4) O21 C11 C21 122.5(4) O11 C11 C21 112.4(4) C22 C32 H32A 108.2 C22 C32 H32B 108.2 H32A C32 H32B 107.4 C42 C32 C22 116.3(4) C42 C32 H32A 108.2 C42 C32 H32B 108.2 C63 C43 H43 108.4 C33 C43 H43 108.4 C33 C43 C63 112.2(5) C53 C43 H43 108.4 C53 C43 C63 110.8(5) C53 C43 C33 108.4(5) C61 C41 H41 107.9 C31 C41 H41 107.9 C31 C41 C61 110.1(5) C51 C41 H41 107.9 C51 C41 C61 110.8(6) C51 C41 C31 112.0(5) N3 C23 C13 106.7(4) N3 C23 H23 108.7 N3 C23 C33 111.3(3) C13 C23 H23 108.7 C13 C23 C33 112.5(4) C33 C23 H23 108.7 C41 C61 H61A 109.5 C41 C61 H61B 109.5 C41 C61 H61C 109.5 H61A C61 H61B 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 C43 C63 H63A 109.5 C43 C63 H63B 109.5 C43 C63 H63C 109.5 H63A C63 H63B 109.5 H63A C63 H63C 109.5 H63B C63 H63C 109.5 C43 C33 C23 116.1(4) C43 C33 H33A 108.3 C43 C33 H33B 108.3 C23 C33 H33A 108.3 C23 C33 H33B 108.3 H33A C33 H33B 107.4 C21 C31 H31A 108.2 C21 C31 H31B 108.2 C41 C31 C21 116.4(4) C41 C31 H31A 108.2 C41 C31 H31B 108.2 H31A C31 H31B 107.3 C41 C51 H51A 109.5 C41 C51 H51B 109.5 C41 C51 H51C 109.5 H51A C51 H51B 109.5 H51A C51 H51C 109.5 H51B C51 H51C 109.5 C43 C53 H53A 109.5 C43 C53 H53B 109.5 C43 C53 H53C 109.5 H53A C53 H53B 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 H62A C62 H62B 109.5 H62A C62 H62C 109.5 H62B C62 H62C 109.5 C42 C62 H62A 109.5 C42 C62 H62B 109.5 C42 C62 H62C 109.5 C32 C42 H42 108.3 C62 C42 C32 112.0(5) C62 C42 H42 108.3 C62 C42 C52 110.4(5) C52 C42 C32 109.4(5) C52 C42 H42 108.3 C42 C52 H52A 109.5 C42 C52 H52B 109.5 C42 C52 H52C 109.5 H52A C52 H52B 109.5 H52A C52 H52C 109.5 H52B C52 H52C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O51 C101 1.235(5) O21 C11 1.215(5) O31 C71 1.246(5) O42 C72 1.290(5) O61 H61 0.8400 O61 C101 1.287(6) O52 C102 1.240(5) O22 C12 1.202(5) N2 H2A 0.9100 N2 H2B 0.9100 N2 H2C 0.9100 N2 C22 1.497(5) O12 H12 0.8400 O12 C12 1.314(5) O53 C103 1.229(5) O33 C73 1.232(5) O62 H62 0.8400 O62 C102 1.288(6) O63 H63 0.8400 O63 C103 1.281(6) N3 H3A 0.9100 N3 H3B 0.9100 N3 H3C 0.9100 N3 C23 1.496(5) O13 H13 0.8400 O13 C13 1.328(5) O32 C72 1.238(5) O11 H11 0.8400 O11 C11 1.320(5) O41 C71 1.285(6) O23 C13 1.200(5) O43 C73 1.284(6) C92 H92 0.9500 C92 C102 1.484(7) C92 C82 1.336(6) C21 H21 1.0000 C21 N1 1.490(5) C21 C11 1.518(6) C21 C31 1.521(6) C91 H91 0.9500 C91 C101 1.493(6) C91 C81 1.335(6) N1 H1A 0.9100 N1 H1B 0.9100 N1 H1C 0.9100 C71 C81 1.480(6) C93 H93 0.9500 C93 C83 1.339(6) C93 C103 1.492(6) C12 C22 1.509(6) C22 H22 1.0000 C22 C32 1.526(6) C83 H83 0.9500 C83 C73 1.495(7) C72 C82 1.491(6) C81 H81 0.9500 C13 C23 1.513(6) C82 H82 0.9500 C32 H32A 0.9900 C32 H32B 0.9900 C32 C42 1.518(7) C43 H43 1.0000 C43 C63 1.521(8) C43 C33 1.520(7) C43 C53 1.520(8) C41 H41 1.0000 C41 C61 1.533(8) C41 C31 1.517(7) C41 C51 1.516(10) C23 H23 1.0000 C23 C33 1.530(6) C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 C63 H63A 0.9800 C63 H63B 0.9800 C63 H63C 0.9800 C33 H33A 0.9900 C33 H33B 0.9900 C31 H31A 0.9900 C31 H31B 0.9900 C51 H51A 0.9800 C51 H51B 0.9800 C51 H51C 0.9800 C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C62 H62A 0.9800 C62 H62B 0.9800 C62 H62C 0.9800 C62 C42 1.511(8) C42 H42 1.0000 C42 C52 1.517(8) C52 H52A 0.9800 C52 H52B 0.9800 C52 H52C 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 O61 H61 O41 0.84 1.59 2.425(4) 174.3 . yes N2 H2A O61 0.91 2.02 2.901(4) 161.1 2_656 yes N2 H2B O23 0.91 2.03 2.860(5) 150.5 3_445 yes N2 H2C O51 0.91 1.88 2.766(5) 163.2 2_646 yes O12 H12 O33 0.84 1.79 2.598(5) 161.0 2_666 yes O62 H62 O42 0.84 1.60 2.437(4) 174.0 . yes O63 H63 O43 0.84 1.58 2.421(5) 179.0 . yes N3 H3A O22 0.91 1.93 2.787(5) 156.4 3_545 yes N3 H3B O53 0.91 1.92 2.823(5) 170.8 3_546 yes N3 H3C O63 0.91 2.01 2.867(5) 156.8 3_556 yes O13 H13 O52 0.84 1.77 2.598(5) 170.1 3 yes O11 H11 O31 0.84 1.76 2.594(4) 172.7 . yes N1 H1A O21 0.91 2.14 2.881(5) 137.5 4_646 yes N1 H1A O31 0.91 2.41 2.994(5) 122.3 4_646 yes N1 H1B O42 0.91 1.95 2.861(4) 176.2 3_545 yes N1 H1C O32 0.91 1.97 2.865(5) 165.8 3 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 O31 C71 C81 C91 179.5(5) O42 C72 C82 C92 -4.1(9) O22 C12 C22 N2 17.2(6) O22 C12 C22 C32 141.3(4) N2 C22 C32 C42 -60.6(5) O12 C12 C22 N2 -164.3(4) O12 C12 C22 C32 -40.2(6) N3 C23 C33 C43 -60.6(5) O13 C13 C23 N3 -173.3(4) O13 C13 C23 C33 -50.9(5) O32 C72 C82 C92 176.4(5) O41 C71 C81 C91 -0.1(9) O23 C13 C23 N3 6.5(6) O23 C13 C23 C33 128.8(5) C102 C92 C82 C72 -0.4(10) N1 C21 C11 O21 -27.4(6) N1 C21 C11 O11 155.2(4) N1 C21 C31 C41 -174.3(4) C101 C91 C81 C71 0.9(10) C93 C83 C73 O33 -168.9(5) C93 C83 C73 O43 13.2(8) C12 C22 C32 C42 178.5(4) C22 C32 C42 C62 -69.5(6) C22 C32 C42 C52 167.9(4) C83 C93 C103 O53 173.9(5) C83 C93 C103 O63 -5.6(8) C81 C91 C101 O51 178.4(6) C81 C91 C101 O61 -0.4(9) C103 C93 C83 C73 -2.4(9) C13 C23 C33 C43 179.7(4) C82 C92 C102 O52 -178.8(5) C82 C92 C102 O62 1.5(9) C11 C21 C31 C41 68.2(6) C61 C41 C31 C21 -175.5(5) C63 C43 C33 C23 -70.1(5) C31 C21 C11 O21 91.4(5) C31 C21 C11 O11 -86.1(5) C51 C41 C31 C21 60.6(7) C53 C43 C33 C23 167.2(4) _cod_database_fobs_code 2108374