#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:07:21 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247605 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125644.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_7125644 loop_ _publ_author_name 'Cho, Jihee' 'Verwilst, Peter' 'Kang, Minjung' 'Pan, Jia-Lin' 'Sharma, Amit' 'Hong, Chang Seop' 'Kim, Jong Seung' 'Kim, Sanghee' _publ_section_title ; Crown ether-appended calix[2]triazolium[2]arene as a macrocyclic receptor for the recognition of the H2PO4- anion. ; _journal_issue 7 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1038 _journal_page_last 1041 _journal_paper_doi 10.1039/c9cc08906c _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C36 H48 N6 O5' _chemical_formula_sum 'C36 H48 N6 O5' _chemical_formula_weight 644.80 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2018-06-01 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-05-17 deposited with the CCDC. 2019-12-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.795(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4230(3) _cell_length_b 20.3482(7) _cell_length_c 17.1498(7) _cell_measurement_reflns_used 4862 _cell_measurement_temperature 292.8(3) _cell_measurement_theta_max 73.0560 _cell_measurement_theta_min 3.4370 _cell_volume 3482.1(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment air _diffrn_ambient_temperature 292.8(3) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2262 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.968 _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 -66.00 11.00 1.00 3.45 -- -41.49 38.00-120.00 77 2 \w -100.00 -42.00 1.00 3.45 -- -41.49 -38.00 30.00 58 3 \w 15.00 49.00 1.00 3.45 -- 41.49 57.00 -60.00 34 4 \w 23.00 60.00 1.00 3.45 -- 41.49-125.00 0.00 37 5 \w 67.00 115.00 1.00 3.45 -- 41.49 57.00 -60.00 48 6 \w 78.00 142.00 1.00 13.80 -- 106.19 30.00-180.00 64 7 \w 82.00 177.00 1.00 13.80 -- 106.19 45.00 30.00 95 8 \w 61.00 154.00 1.00 13.80 -- 106.19 -15.00-180.00 93 9 \w 53.00 118.00 1.00 13.80 -- 106.19 -30.00 0.00 65 10 \w 34.00 127.00 1.00 13.80 -- 106.19 -61.00-120.00 93 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0281364000 _diffrn_orient_matrix_UB_12 -0.0460990000 _diffrn_orient_matrix_UB_13 0.0742790000 _diffrn_orient_matrix_UB_21 0.1289369000 _diffrn_orient_matrix_UB_22 0.0387085000 _diffrn_orient_matrix_UB_23 0.0410082000 _diffrn_orient_matrix_UB_31 -0.0798024000 _diffrn_orient_matrix_UB_32 0.0460082000 _diffrn_orient_matrix_UB_33 0.0401136000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 13883 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.700 _diffrn_reflns_theta_min 3.459 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_correction_T_min 0.980 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic light white' _exptl_crystal_density_diffrn 1.230 _exptl_crystal_description irregular _exptl_crystal_F_000 1384 _exptl_crystal_size_max 0.436 _exptl_crystal_size_mid 0.311 _exptl_crystal_size_min 0.155 _refine_diff_density_max 0.437 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 497 _refine_ls_number_reflns 6803 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0728 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1344P)^2^+1.0817P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2120 _refine_ls_wR_factor_ref 0.2348 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5139 _reflns_number_total 6803 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc08906c2.cif _cod_data_source_block exp_1235 _cod_depositor_comments 'Adding full bibliography for 7125644--7125647.cif.' _cod_database_code 7125644 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula 'c36 h48 n6 o5' _chemical_oxdiff_usercomment CJH-8-176 _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. ; _reflns_odcompleteness_completeness 99.83 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(O32B)=Sof(H30A)=Sof(H30B)=Sof(H33C)=Sof(H33D)=Sof(H31C)=Sof(H31D)= Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)= Sof(H46F)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C27B)=Sof(H27C)= Sof(H27D)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(O29B)=1-FVAR(1) Sof(O32A)=Sof(H30C)=Sof(H30D)=Sof(H33A)=Sof(H33B)=Sof(H31A)=Sof(H31B)= Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46A)=Sof(H46A)=Sof(H46B)= Sof(H46C)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C27A)=Sof(H27A)= Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(O29A)=FVAR(1) 3.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C4(H4A,H4B), C20(H20A,H20B), C14(H14A,H14B), C37(H37A,H37B), C36(H36A,H36B), C30(H30C,H30D), C30(H30A,H30B), C34(H34A,H34B), C33(H33A,H33B), C33(H33C,H33D), C31(H31A,H31B), C31(H31C,H31D), C27A(H27A,H27B), C27B(H27C, H27D), C28A(H28A,H28B), C28B(H28C,H28D) 3.b Aromatic/amide H refined with riding coordinates: C18(H18), C12(H12), C8(H8), C6(H6), C16(H16), C2(H2) 3.c Idealised Me refined as rotating group: C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45A(H45A,H45B, H45C), C45B(H45D,H45E,H45F), C46A(H46A,H46B,H46C), C46B(H46D,H46E,H46F), C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F) ; _shelx_res_file ; TITL exp_1235_a.res in P2(1)/c exp_1235.res created by SHELXL-2017/1 at 10:42:57 on 01-Jun-2018 REM Old TITL exp_1235 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.242, Rweak 0.105, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C43 N2 O2 CELL 1.54184 10.423 20.3482 17.1498 90 106.795 90 ZERR 4 0.0003 0.0007 0.0007 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 144 192 24 20 L.S. 4 PLAN 20 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.134400 1.081700 FVAR 3.03833 0.65530 O38 4 0.307730 0.901282 0.504692 11.00000 0.05082 0.05696 = 0.06026 -0.00025 0.00401 -0.00859 O26 4 0.053967 0.745412 0.421654 11.00000 0.05365 0.07401 = 0.05890 0.00952 0.01807 -0.00728 N11 3 0.483047 0.766027 0.555348 11.00000 0.04307 0.06195 = 0.06075 -0.00065 0.02001 0.00499 N1 3 -0.081824 0.843811 0.531045 11.00000 0.03994 0.05529 = 0.07682 0.00215 0.01083 0.00570 C13 1 0.345457 0.684914 0.520420 11.00000 0.04246 0.04684 = 0.05927 -0.00452 0.02237 0.00484 C3 1 0.057597 0.922166 0.580413 11.00000 0.03141 0.04561 = 0.06942 -0.00426 0.00648 0.00910 N24 3 0.538371 0.714303 0.600199 11.00000 0.05514 0.06456 = 0.07574 0.00403 0.00815 0.01239 N23 3 0.455286 0.664592 0.579243 11.00000 0.07073 0.05755 = 0.08326 0.00797 0.01988 0.01055 C25 1 0.027103 0.706866 0.481540 11.00000 0.04528 0.04972 = 0.04950 -0.00466 0.01221 -0.00922 O35 4 0.483838 0.917273 0.400611 11.00000 0.09736 0.11055 = 0.07539 0.00609 0.01827 -0.01033 C39 1 0.366625 0.906247 0.587851 11.00000 0.03714 0.04440 = 0.05874 -0.00085 0.00650 -0.00627 C9 1 0.487447 0.873734 0.621332 11.00000 0.03463 0.04928 = 0.06082 -0.00131 0.01396 -0.00627 C18 1 -0.109019 0.681855 0.568521 11.00000 0.03681 0.05082 = 0.05306 -0.00530 0.00960 -0.00762 AFIX 43 H18 2 -0.180630 0.692407 0.588317 11.00000 -1.20000 AFIX 0 C19 1 -0.078063 0.723282 0.512099 11.00000 0.03356 0.04897 = 0.05275 -0.00221 0.00527 -0.00482 C12 1 0.362576 0.748727 0.504468 11.00000 0.04096 0.05725 = 0.06528 0.00137 0.01209 0.00321 AFIX 43 H12 2 0.303687 0.775318 0.466355 11.00000 -1.20000 AFIX 0 C8 1 0.549152 0.879357 0.704831 11.00000 0.03501 0.05193 = 0.06138 0.00155 0.01091 -0.00153 AFIX 43 H8 2 0.630892 0.858434 0.727094 11.00000 -1.20000 AFIX 0 C5 1 0.304446 0.940030 0.637168 11.00000 0.03847 0.03993 = 0.07297 -0.00602 0.00678 -0.00158 C6 1 0.368700 0.943737 0.720639 11.00000 0.04511 0.04657 = 0.07145 -0.01051 0.01554 -0.00014 AFIX 43 H6 2 0.326861 0.966188 0.753770 11.00000 -1.20000 AFIX 0 C7 1 0.493398 0.914967 0.756095 11.00000 0.04436 0.04674 = 0.05990 -0.00115 0.01319 -0.00486 C15 1 0.108971 0.653186 0.511895 11.00000 0.04511 0.04630 = 0.06452 -0.01179 0.01621 -0.00465 C16 1 0.074627 0.613281 0.567685 11.00000 0.05005 0.04135 = 0.06971 -0.00068 0.01101 -0.00063 AFIX 43 H16 2 0.127607 0.576702 0.587322 11.00000 -1.20000 AFIX 0 C17 1 -0.036046 0.625225 0.596100 11.00000 0.04143 0.05050 = 0.05515 -0.00261 0.00734 -0.01059 C10 1 0.548422 0.830980 0.569673 11.00000 0.03718 0.06327 = 0.06442 -0.00190 0.01824 -0.00564 AFIX 23 H10A 2 0.539166 0.852436 0.517828 11.00000 -1.20000 H10B 2 0.643288 0.825349 0.596716 11.00000 -1.20000 AFIX 0 C2 1 0.029135 0.874004 0.523656 11.00000 0.04382 0.05876 = 0.07141 -0.00652 0.01644 -0.00415 AFIX 43 H2 2 0.076591 0.863780 0.486921 11.00000 -1.20000 AFIX 0 N22 3 -0.035266 0.920346 0.621058 11.00000 0.06587 0.08976 = 0.12430 -0.03975 0.04068 -0.00297 N21 3 -0.120136 0.872919 0.591062 11.00000 0.05998 0.09201 = 0.12315 -0.03427 0.04546 -0.00853 C4 1 0.167630 0.970886 0.602284 11.00000 0.04577 0.04608 = 0.09071 -0.01152 0.00470 0.00495 AFIX 23 H4A 2 0.151223 1.001300 0.641897 11.00000 -1.20000 H4B 2 0.167395 0.995884 0.554083 11.00000 -1.20000 AFIX 0 C20 1 -0.155500 0.786834 0.487248 11.00000 0.03329 0.05711 = 0.06994 0.00387 0.00491 -0.00281 AFIX 23 H20A 2 -0.172513 0.793382 0.429117 11.00000 -1.20000 H20B 2 -0.241320 0.783459 0.498440 11.00000 -1.20000 AFIX 0 C44 1 0.566512 0.921988 0.847003 11.00000 0.05454 0.06659 = 0.06125 -0.00677 0.01102 -0.00270 C40 1 -0.074124 0.576658 0.654191 11.00000 0.05754 0.05855 = 0.06641 0.00898 0.00952 -0.01058 C14 1 0.232651 0.639504 0.484386 11.00000 0.05713 0.05352 = 0.08782 -0.01881 0.03047 -0.00302 AFIX 23 H14A 2 0.262040 0.594778 0.499066 11.00000 -1.20000 H14B 2 0.208718 0.642922 0.425514 11.00000 -1.20000 AFIX 0 C37 1 0.316818 0.958514 0.456734 11.00000 0.09226 0.06094 = 0.07849 0.01024 0.01107 0.00257 AFIX 23 H37A 2 0.384520 0.988204 0.488783 11.00000 -1.20000 H37B 2 0.231645 0.981491 0.441532 11.00000 -1.20000 AFIX 0 PART 1 O32A 4 0.368787 0.818074 0.276166 21.00000 0.11208 0.08570 = 0.08749 -0.02310 0.03409 -0.00119 PART 0 PART 2 O32B 4 0.395365 0.785692 0.309687 -21.00000 0.10461 0.18833 = 0.07568 0.01444 0.02371 -0.00749 PART 0 C36 1 0.352484 0.938500 0.381805 11.00000 0.10189 0.09102 = 0.06055 0.01491 0.00933 -0.01169 AFIX 23 H36A 2 0.293262 0.903453 0.354596 11.00000 -1.20000 H36B 2 0.339964 0.975525 0.344732 11.00000 -1.20000 AFIX 0 C41 1 -0.195334 0.600839 0.680845 11.00000 0.07610 0.09453 = 0.10657 0.02903 0.03772 -0.00307 AFIX 137 H41A 2 -0.173093 0.641554 0.709896 11.00000 -1.50000 H41B 2 -0.217783 0.568585 0.715611 11.00000 -1.50000 H41C 2 -0.270539 0.607422 0.633612 11.00000 -1.50000 AFIX 0 C42 1 0.043946 0.568843 0.730969 11.00000 0.07804 0.10420 = 0.08373 0.02477 0.00804 -0.00717 AFIX 137 H42A 2 0.119947 0.551932 0.716468 11.00000 -1.50000 H42B 2 0.019930 0.538888 0.767678 11.00000 -1.50000 H42C 2 0.066106 0.610800 0.756972 11.00000 -1.50000 AFIX 0 C43 1 -0.108280 0.511054 0.612240 11.00000 0.13610 0.06858 = 0.10438 0.00167 0.02884 -0.04241 AFIX 137 H43A 2 -0.185406 0.515771 0.565705 11.00000 -1.50000 H43B 2 -0.127410 0.479890 0.649407 11.00000 -1.50000 H43C 2 -0.033748 0.495775 0.594927 11.00000 -1.50000 AFIX 0 C30 1 0.200137 0.736419 0.223192 11.00000 0.14742 0.11148 = 0.06753 -0.01671 0.02510 0.00499 PART 2 AFIX 23 H30C 2 0.143523 0.758141 0.175174 21.00000 -1.20000 H30D 2 0.200051 0.689816 0.211279 21.00000 -1.20000 AFIX 23 PART 0 PART 1 H30A 2 0.184456 0.705808 0.178052 -21.00000 -1.20000 H30B 2 0.139249 0.773049 0.205077 -21.00000 -1.20000 AFIX 0 PART 0 C34 1 0.524654 0.897940 0.332112 11.00000 0.14218 0.11318 = 0.09806 0.00636 0.06041 -0.01803 AFIX 23 H34A 2 0.618894 0.908376 0.342405 11.00000 -1.20000 H34B 2 0.475110 0.923579 0.285429 11.00000 -1.20000 AFIX 0 C33 1 0.505228 0.828527 0.311680 11.00000 0.10430 0.15922 = 0.10706 -0.02031 0.03858 -0.02002 PART 1 AFIX 23 H33A 2 0.554920 0.816367 0.273985 21.00000 -1.20000 H33B 2 0.537102 0.801965 0.360428 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H33C 2 0.516694 0.825127 0.257673 -21.00000 -1.20000 H33D 2 0.582710 0.806981 0.347941 -21.00000 -1.20000 AFIX 0 PART 0 C31 1 0.330831 0.760355 0.238548 11.00000 0.15009 0.14092 = 0.11407 -0.03114 0.07964 -0.03307 PART 1 AFIX 23 H31A 2 0.389985 0.727087 0.270302 21.00000 -1.20000 H31B 2 0.349675 0.762710 0.186440 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H31C 2 0.385215 0.724498 0.228406 -21.00000 -1.20000 H31D 2 0.328961 0.793693 0.197807 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C45A 1 0.585840 0.851954 0.889378 21.00000 0.08757 0.08676 = 0.06632 0.01367 0.00314 0.00844 AFIX 137 H45A 2 0.499716 0.832664 0.884185 21.00000 -1.50000 H45B 2 0.633673 0.856702 0.946019 21.00000 -1.50000 H45C 2 0.635830 0.824102 0.863584 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C45B 1 0.693832 0.886968 0.868671 -21.00000 0.12708 0.19259 = 0.06213 -0.00945 -0.02014 0.08318 AFIX 137 H45D 2 0.677430 0.840506 0.863950 -21.00000 -1.50000 H45E 2 0.743314 0.897431 0.923733 -21.00000 -1.50000 H45F 2 0.744659 0.899888 0.832609 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C46A 1 0.707049 0.949490 0.857809 21.00000 0.06817 0.12859 = 0.07530 -0.02216 0.00526 -0.03796 AFIX 137 H46A 2 0.754655 0.921290 0.830860 21.00000 -1.50000 H46B 2 0.754373 0.951728 0.914785 21.00000 -1.50000 H46C 2 0.700386 0.992724 0.834571 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C46B 1 0.586652 0.999032 0.862493 -21.00000 0.12916 0.07660 = 0.07317 -0.00842 -0.00632 -0.02183 AFIX 137 H46D 2 0.646562 1.015569 0.833854 -21.00000 -1.50000 H46E 2 0.623852 1.007090 0.919756 -21.00000 -1.50000 H46F 2 0.501675 1.020843 0.843198 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C47A 1 0.495285 0.963499 0.894789 21.00000 0.08820 0.11305 = 0.06615 -0.02243 0.01220 0.01965 AFIX 137 H47A 2 0.490478 1.008140 0.876050 21.00000 -1.50000 H47B 2 0.543855 0.961886 0.951601 21.00000 -1.50000 H47C 2 0.406316 0.946819 0.887046 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C47B 1 0.476148 0.900014 0.891726 -21.00000 0.18603 0.23611 = 0.04715 0.00547 0.02077 -0.12006 AFIX 137 H47D 2 0.392620 0.923130 0.872664 -21.00000 -1.50000 H47E 2 0.515231 0.908645 0.948704 -21.00000 -1.50000 H47F 2 0.460627 0.853686 0.883488 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C27A 1 -0.033527 0.744451 0.342525 21.00000 0.08565 0.13466 = 0.05789 0.01252 0.00969 -0.02714 AFIX 23 H27A 2 -0.040941 0.787936 0.318455 21.00000 -1.20000 H27B 2 -0.122001 0.730110 0.343100 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C27B 1 -0.011627 0.706985 0.341540 -21.00000 0.06061 0.05974 = 0.04771 -0.00270 0.01976 -0.01282 AFIX 23 H27C 2 0.015412 0.661227 0.348297 -21.00000 -1.20000 H27D 2 -0.108449 0.708905 0.329041 -21.00000 -1.20000 AFIX 0 C28A 1 0.029012 0.735038 0.276959 21.00000 0.10484 0.10908 = 0.06113 0.00255 0.01124 0.02113 AFIX 23 H28A 2 -0.001481 0.706227 0.230183 21.00000 -1.20000 H28B 2 -0.018312 0.776367 0.262623 21.00000 -1.20000 AFIX 0 PART 0 PART 1 C28B 1 0.024612 0.697440 0.295340 -21.00000 0.08444 0.13906 = 0.05303 -0.01411 -0.00433 -0.01335 AFIX 23 H28C 2 -0.035433 0.696909 0.240319 -21.00000 -1.20000 H28D 2 0.019441 0.654192 0.318031 -21.00000 -1.20000 AFIX 0 PART 0 PART 2 O29A 4 0.145527 0.745516 0.286947 21.00000 0.11065 0.18773 = 0.07890 -0.03271 0.05210 -0.06231 PART 0 PART 1 O29B 4 0.163807 0.704303 0.287862 -21.00000 0.10094 0.12992 = 0.06545 -0.00093 0.01430 0.04399 HKLF 4 REM exp_1235_a.res in P2(1)/c REM R1 = 0.0728 for 5139 Fo > 4sig(Fo) and 0.0901 for all 6803 data REM 497 parameters refined using 0 restraints END WGHT 0.1344 1.0817 REM Highest difference peak 0.437, deepest hole -0.339, 1-sigma level 0.060 Q1 1 -0.2283 0.5498 0.6067 11.00000 0.05 0.44 Q2 1 0.0182 0.5125 0.6668 11.00000 0.05 0.40 Q3 1 0.6717 0.7830 0.2785 11.00000 0.05 0.39 Q4 1 0.3813 0.8899 0.3646 11.00000 0.05 0.35 Q5 1 -0.0743 0.6028 0.7230 11.00000 0.05 0.35 Q6 1 0.0412 0.9260 0.6015 11.00000 0.05 0.31 Q7 1 0.0910 0.9421 0.5817 11.00000 0.05 0.30 Q8 1 0.4225 0.8729 0.2719 11.00000 0.05 0.30 Q9 1 0.3048 0.6743 0.5042 11.00000 0.05 0.26 Q10 1 0.4241 0.8915 0.6062 11.00000 0.05 0.24 Q11 1 0.3416 0.7037 0.5212 11.00000 0.05 0.23 Q12 1 0.3655 0.6775 0.5521 11.00000 0.05 0.23 Q13 1 0.2428 0.9546 0.6202 11.00000 0.05 0.21 Q14 1 0.5010 0.8803 0.6442 11.00000 0.05 0.21 Q15 1 0.4032 0.9238 0.7258 11.00000 0.05 0.19 Q16 1 0.2953 0.8464 0.2366 11.00000 0.05 0.19 Q17 1 0.2866 0.8076 0.2373 11.00000 0.05 0.18 Q18 1 0.1005 0.7757 0.4219 11.00000 0.05 0.18 Q19 1 0.2597 0.7035 0.2582 11.00000 0.05 0.17 Q20 1 0.3119 0.9276 0.6811 11.00000 0.05 0.17 ; _shelx_res_checksum 78942 _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 1.625 _oxdiff_exptl_absorpt_empirical_full_min 0.565 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O38 O 0.30773(18) 0.90128(9) 0.50469(11) 0.0585(5) Uani 1 1 d . . . . O26 O 0.05397(19) 0.74541(10) 0.42165(11) 0.0618(5) Uani 1 1 d . . . . N11 N 0.4830(2) 0.76603(11) 0.55535(13) 0.0542(5) Uani 1 1 d . . . . N1 N -0.0818(2) 0.84381(11) 0.53105(14) 0.0586(5) Uani 1 1 d . . . . C13 C 0.3455(2) 0.68491(11) 0.52042(15) 0.0479(5) Uani 1 1 d . . . . C3 C 0.0576(2) 0.92217(11) 0.58041(16) 0.0505(6) Uani 1 1 d . . . . N24 N 0.5384(2) 0.71430(12) 0.60020(16) 0.0674(6) Uani 1 1 d . . . . N23 N 0.4553(3) 0.66459(12) 0.57924(17) 0.0710(7) Uani 1 1 d . . . . C25 C 0.0271(2) 0.70687(12) 0.48154(14) 0.0485(5) Uani 1 1 d . . . . O35 O 0.4838(3) 0.91727(15) 0.40061(16) 0.0958(8) Uani 1 1 d . . . . C39 C 0.3666(2) 0.90625(11) 0.58785(15) 0.0483(5) Uani 1 1 d . . . . C9 C 0.4874(2) 0.87373(11) 0.62133(15) 0.0482(5) Uani 1 1 d . . . . C18 C -0.1090(2) 0.68186(11) 0.56852(14) 0.0476(5) Uani 1 1 d . . . . H18 H -0.180630 0.692407 0.588317 0.057 Uiso 1 1 calc R . . . C19 C -0.0781(2) 0.72328(11) 0.51210(14) 0.0466(5) Uani 1 1 d . . . . C12 C 0.3626(2) 0.74873(13) 0.50447(17) 0.0552(6) Uani 1 1 d . . . . H12 H 0.303687 0.775318 0.466355 0.066 Uiso 1 1 calc R . . . C8 C 0.5492(2) 0.87936(12) 0.70483(15) 0.0501(5) Uani 1 1 d . . . . H8 H 0.630892 0.858434 0.727094 0.060 Uiso 1 1 calc R . . . C5 C 0.3044(2) 0.94003(11) 0.63717(17) 0.0524(6) Uani 1 1 d . . . . C6 C 0.3687(2) 0.94374(12) 0.72064(17) 0.0546(6) Uani 1 1 d . . . . H6 H 0.326861 0.966188 0.753770 0.066 Uiso 1 1 calc R . . . C7 C 0.4934(2) 0.91497(12) 0.75610(16) 0.0507(5) Uani 1 1 d . . . . C15 C 0.1090(2) 0.65319(12) 0.51189(16) 0.0519(6) Uani 1 1 d . . . . C16 C 0.0746(3) 0.61328(12) 0.56768(17) 0.0550(6) Uani 1 1 d . . . . H16 H 0.127607 0.576702 0.587322 0.066 Uiso 1 1 calc R . . . C17 C -0.0360(2) 0.62523(12) 0.59610(15) 0.0504(5) Uani 1 1 d . . . . C10 C 0.5484(2) 0.83098(13) 0.56967(16) 0.0542(6) Uani 1 1 d . . . . H10A H 0.539166 0.852436 0.517828 0.065 Uiso 1 1 calc R . . . H10B H 0.643288 0.825349 0.596716 0.065 Uiso 1 1 calc R . . . C2 C 0.0291(2) 0.87400(13) 0.52366(17) 0.0580(6) Uani 1 1 d . . . . H2 H 0.076591 0.863780 0.486921 0.070 Uiso 1 1 calc R . . . N22 N -0.0353(3) 0.92035(16) 0.6211(2) 0.0905(9) Uani 1 1 d . . . . N21 N -0.1201(3) 0.87292(16) 0.5911(2) 0.0877(9) Uani 1 1 d . . . . C4 C 0.1676(3) 0.97089(13) 0.6023(2) 0.0640(7) Uani 1 1 d . . . . H4A H 0.151223 1.001300 0.641897 0.077 Uiso 1 1 calc R . . . H4B H 0.167395 0.995884 0.554083 0.077 Uiso 1 1 calc R . . . C20 C -0.1555(2) 0.78683(13) 0.48725(17) 0.0555(6) Uani 1 1 d . . . . H20A H -0.172513 0.793382 0.429117 0.067 Uiso 1 1 calc R . . . H20B H -0.241320 0.783459 0.498440 0.067 Uiso 1 1 calc R . . . C44 C 0.5665(3) 0.92199(15) 0.84700(17) 0.0620(7) Uani 1 1 d . . . . C40 C -0.0741(3) 0.57666(14) 0.65419(18) 0.0626(7) Uani 1 1 d . . . . C14 C 0.2327(3) 0.63950(14) 0.4844(2) 0.0642(7) Uani 1 1 d . . . . H14A H 0.262040 0.594778 0.499066 0.077 Uiso 1 1 calc R . . . H14B H 0.208718 0.642922 0.425514 0.077 Uiso 1 1 calc R . . . C37 C 0.3168(4) 0.95851(16) 0.4567(2) 0.0801(9) Uani 1 1 d . . . . H37A H 0.384520 0.988204 0.488783 0.096 Uiso 1 1 calc R . . . H37B H 0.231645 0.981491 0.441532 0.096 Uiso 1 1 calc R . . . O32A O 0.3688(6) 0.8181(3) 0.2762(4) 0.0940(15) Uani 0.655(7) 1 d . P A 1 O32B O 0.3954(13) 0.7857(9) 0.3097(7) 0.123(4) Uani 0.345(7) 1 d . P A 2 C36 C 0.3525(4) 0.9385(2) 0.3818(2) 0.0875(10) Uani 1 1 d . . . . H36A H 0.293262 0.903453 0.354596 0.105 Uiso 1 1 calc R . . . H36B H 0.339964 0.975525 0.344732 0.105 Uiso 1 1 calc R . . . C41 C -0.1953(4) 0.6008(2) 0.6808(3) 0.0900(11) Uani 1 1 d . . . . H41A H -0.173093 0.641554 0.709896 0.135 Uiso 1 1 calc GR . . . H41B H -0.217783 0.568585 0.715611 0.135 Uiso 1 1 calc GR . . . H41C H -0.270539 0.607422 0.633612 0.135 Uiso 1 1 calc GR . . . C42 C 0.0439(4) 0.5688(2) 0.7310(2) 0.0919(11) Uani 1 1 d . . . . H42A H 0.119947 0.551932 0.716468 0.138 Uiso 1 1 calc GR . . . H42B H 0.019930 0.538888 0.767678 0.138 Uiso 1 1 calc GR . . . H42C H 0.066106 0.610800 0.756972 0.138 Uiso 1 1 calc GR . . . C43 C -0.1083(5) 0.51105(18) 0.6122(3) 0.1043(14) Uani 1 1 d . . . . H43A H -0.185406 0.515771 0.565705 0.156 Uiso 1 1 calc GR . . . H43B H -0.127410 0.479890 0.649407 0.156 Uiso 1 1 calc GR . . . H43C H -0.033748 0.495775 0.594927 0.156 Uiso 1 1 calc GR . . . C30 C 0.2001(6) 0.7364(2) 0.2232(2) 0.1101(15) Uani 1 1 d . . . . H30C H 0.143523 0.758141 0.175174 0.132 Uiso 0.655(7) 1 calc R P A 2 H30D H 0.200051 0.689816 0.211279 0.132 Uiso 0.655(7) 1 calc R P A 2 H30A H 0.184456 0.705808 0.178052 0.132 Uiso 0.345(7) 1 calc R P A 1 H30B H 0.139249 0.773049 0.205077 0.132 Uiso 0.345(7) 1 calc R P A 1 C34 C 0.5247(6) 0.8979(2) 0.3321(3) 0.1124(15) Uani 1 1 d . . . . H34A H 0.618894 0.908376 0.342405 0.135 Uiso 1 1 calc R . . . H34B H 0.475110 0.923579 0.285429 0.135 Uiso 1 1 calc R . . . C33 C 0.5052(5) 0.8285(3) 0.3117(3) 0.1218(17) Uani 1 1 d . . . . H33A H 0.554920 0.816367 0.273985 0.146 Uiso 0.655(7) 1 calc R P A 1 H33B H 0.537102 0.801965 0.360428 0.146 Uiso 0.655(7) 1 calc R P A 1 H33C H 0.516694 0.825127 0.257673 0.146 Uiso 0.345(7) 1 calc R P A 2 H33D H 0.582710 0.806981 0.347941 0.146 Uiso 0.345(7) 1 calc R P A 2 C31 C 0.3308(7) 0.7604(3) 0.2385(4) 0.1263(19) Uani 1 1 d . . . . H31A H 0.389985 0.727087 0.270302 0.152 Uiso 0.655(7) 1 calc R P A 1 H31B H 0.349675 0.762710 0.186440 0.152 Uiso 0.655(7) 1 calc R P A 1 H31C H 0.385215 0.724498 0.228406 0.152 Uiso 0.345(7) 1 calc R P A 2 H31D H 0.328961 0.793693 0.197807 0.152 Uiso 0.345(7) 1 calc R P A 2 C45A C 0.5858(7) 0.8520(3) 0.8894(3) 0.0842(17) Uani 0.655(7) 1 d . P A 1 H45A H 0.499716 0.832664 0.884185 0.126 Uiso 0.655(7) 1 calc GR P A 1 H45B H 0.633673 0.856702 0.946019 0.126 Uiso 0.655(7) 1 calc GR P A 1 H45C H 0.635830 0.824102 0.863584 0.126 Uiso 0.655(7) 1 calc GR P A 1 C45B C 0.6938(18) 0.8870(11) 0.8687(7) 0.137(9) Uani 0.345(7) 1 d . P A 2 H45D H 0.677430 0.840506 0.863950 0.206 Uiso 0.345(7) 1 calc GR P A 2 H45E H 0.743314 0.897431 0.923733 0.206 Uiso 0.345(7) 1 calc GR P A 2 H45F H 0.744659 0.899888 0.832609 0.206 Uiso 0.345(7) 1 calc GR P A 2 C46A C 0.7070(6) 0.9495(4) 0.8578(4) 0.094(2) Uani 0.655(7) 1 d . P A 1 H46A H 0.754655 0.921290 0.830860 0.141 Uiso 0.655(7) 1 calc GR P A 1 H46B H 0.754373 0.951728 0.914785 0.141 Uiso 0.655(7) 1 calc GR P A 1 H46C H 0.700386 0.992724 0.834571 0.141 Uiso 0.655(7) 1 calc GR P A 1 C46B C 0.5867(15) 0.9990(5) 0.8625(7) 0.100(5) Uani 0.345(7) 1 d . P A 2 H46D H 0.646562 1.015569 0.833854 0.151 Uiso 0.345(7) 1 calc GR P A 2 H46E H 0.623852 1.007090 0.919756 0.151 Uiso 0.345(7) 1 calc GR P A 2 H46F H 0.501675 1.020843 0.843198 0.151 Uiso 0.345(7) 1 calc GR P A 2 C47A C 0.4953(7) 0.9635(4) 0.8948(3) 0.091(2) Uani 0.655(7) 1 d . P A 1 H47A H 0.490478 1.008140 0.876050 0.137 Uiso 0.655(7) 1 calc GR P A 1 H47B H 0.543855 0.961886 0.951601 0.137 Uiso 0.655(7) 1 calc GR P A 1 H47C H 0.406316 0.946819 0.887046 0.137 Uiso 0.655(7) 1 calc GR P A 1 C47B C 0.476(2) 0.9000(12) 0.8917(7) 0.159(11) Uani 0.345(7) 1 d . P A 2 H47D H 0.392620 0.923130 0.872664 0.239 Uiso 0.345(7) 1 calc GR P A 2 H47E H 0.515231 0.908645 0.948704 0.239 Uiso 0.345(7) 1 calc GR P A 2 H47F H 0.460627 0.853686 0.883488 0.239 Uiso 0.345(7) 1 calc GR P A 2 C27A C -0.0335(8) 0.7445(6) 0.3425(4) 0.095(2) Uani 0.655(7) 1 d . P A 1 H27A H -0.040941 0.787936 0.318455 0.114 Uiso 0.655(7) 1 calc R P A 1 H27B H -0.122001 0.730110 0.343100 0.114 Uiso 0.655(7) 1 calc R P A 1 C27B C -0.0116(11) 0.7070(6) 0.3415(6) 0.055(2) Uani 0.345(7) 1 d . P A 2 H27C H 0.015412 0.661227 0.348297 0.066 Uiso 0.345(7) 1 calc R P A 2 H27D H -0.108449 0.708905 0.329041 0.066 Uiso 0.345(7) 1 calc R P A 2 C28A C 0.0290(10) 0.7350(5) 0.2770(5) 0.094(3) Uani 0.655(7) 1 d . P A 2 H28A H -0.001481 0.706227 0.230183 0.113 Uiso 0.655(7) 1 calc R P A 2 H28B H -0.018312 0.776367 0.262623 0.113 Uiso 0.655(7) 1 calc R P A 2 C28B C 0.0246(16) 0.6974(11) 0.2953(10) 0.097(5) Uani 0.345(7) 1 d . P A 1 H28C H -0.035433 0.696909 0.240319 0.117 Uiso 0.345(7) 1 calc R P A 1 H28D H 0.019441 0.654192 0.318031 0.117 Uiso 0.345(7) 1 calc R P A 1 O29A O 0.1455(8) 0.7455(5) 0.2869(4) 0.121(3) Uani 0.655(7) 1 d . P A 2 O29B O 0.1638(13) 0.7043(7) 0.2879(7) 0.101(4) Uani 0.345(7) 1 d . P A 1 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 O38 0.0508(10) 0.0570(10) 0.0603(10) -0.0002(8) 0.0040(8) -0.0086(8) O26 0.0536(10) 0.0740(12) 0.0589(10) 0.0095(9) 0.0181(8) -0.0073(8) N11 0.0431(10) 0.0619(12) 0.0608(12) -0.0006(9) 0.0200(9) 0.0050(9) N1 0.0399(10) 0.0553(12) 0.0768(14) 0.0021(10) 0.0108(10) 0.0057(9) C13 0.0425(12) 0.0468(12) 0.0593(13) -0.0045(10) 0.0224(10) 0.0048(9) C3 0.0314(10) 0.0456(11) 0.0694(15) -0.0043(10) 0.0065(10) 0.0091(8) N24 0.0551(13) 0.0646(14) 0.0757(15) 0.0040(11) 0.0081(11) 0.0124(11) N23 0.0707(16) 0.0575(13) 0.0833(16) 0.0080(12) 0.0199(13) 0.0105(11) C25 0.0453(12) 0.0497(12) 0.0495(12) -0.0047(9) 0.0122(10) -0.0092(9) O35 0.0974(19) 0.111(2) 0.0754(15) 0.0061(13) 0.0183(14) -0.0103(15) C39 0.0371(11) 0.0444(11) 0.0587(13) -0.0009(9) 0.0065(10) -0.0063(8) C9 0.0346(10) 0.0493(12) 0.0608(14) -0.0013(10) 0.0140(10) -0.0063(9) C18 0.0368(11) 0.0508(12) 0.0531(12) -0.0053(10) 0.0096(9) -0.0076(9) C19 0.0336(10) 0.0490(12) 0.0527(12) -0.0022(9) 0.0053(9) -0.0048(8) C12 0.0410(12) 0.0573(14) 0.0653(15) 0.0014(11) 0.0121(11) 0.0032(10) C8 0.0350(11) 0.0519(12) 0.0614(14) 0.0016(10) 0.0109(10) -0.0015(9) C5 0.0385(11) 0.0399(11) 0.0730(16) -0.0060(10) 0.0068(11) -0.0016(9) C6 0.0451(12) 0.0466(12) 0.0714(16) -0.0105(11) 0.0155(11) -0.0001(10) C7 0.0444(12) 0.0467(12) 0.0599(14) -0.0011(10) 0.0132(10) -0.0049(9) C15 0.0451(12) 0.0463(12) 0.0645(14) -0.0118(10) 0.0162(11) -0.0046(9) C16 0.0500(13) 0.0413(11) 0.0697(15) -0.0007(10) 0.0110(11) -0.0006(10) C17 0.0414(12) 0.0505(12) 0.0551(13) -0.0026(10) 0.0073(10) -0.0106(9) C10 0.0372(11) 0.0633(14) 0.0644(15) -0.0019(11) 0.0182(10) -0.0056(10) C2 0.0438(13) 0.0588(14) 0.0714(16) -0.0065(12) 0.0164(11) -0.0041(10) N22 0.0659(16) 0.090(2) 0.124(3) -0.0398(18) 0.0407(17) -0.0030(14) N21 0.0600(15) 0.092(2) 0.123(2) -0.0343(18) 0.0455(16) -0.0085(14) C4 0.0458(13) 0.0461(13) 0.0907(19) -0.0115(12) 0.0047(13) 0.0049(10) C20 0.0333(11) 0.0571(14) 0.0699(15) 0.0039(11) 0.0049(10) -0.0028(10) C44 0.0545(15) 0.0666(16) 0.0613(15) -0.0068(12) 0.0110(12) -0.0027(12) C40 0.0575(15) 0.0586(15) 0.0664(16) 0.0090(12) 0.0095(12) -0.0106(12) C14 0.0571(15) 0.0535(14) 0.0878(19) -0.0188(13) 0.0305(14) -0.0030(11) C37 0.092(2) 0.0609(17) 0.078(2) 0.0102(15) 0.0111(17) 0.0026(16) O32A 0.112(4) 0.086(3) 0.087(3) -0.023(2) 0.034(3) -0.001(3) O32B 0.105(7) 0.188(13) 0.076(6) 0.014(7) 0.024(5) -0.007(8) C36 0.102(3) 0.091(2) 0.0606(18) 0.0149(16) 0.0093(17) -0.012(2) C41 0.076(2) 0.095(2) 0.107(3) 0.029(2) 0.038(2) -0.0031(18) C42 0.078(2) 0.104(3) 0.084(2) 0.025(2) 0.0080(18) -0.007(2) C43 0.136(4) 0.069(2) 0.104(3) 0.0017(19) 0.029(3) -0.042(2) C30 0.147(5) 0.111(3) 0.068(2) -0.017(2) 0.025(2) 0.005(3) C34 0.142(4) 0.113(3) 0.098(3) 0.006(3) 0.060(3) -0.018(3) C33 0.104(4) 0.159(5) 0.107(3) -0.020(3) 0.039(3) -0.020(3) C31 0.150(5) 0.141(4) 0.114(4) -0.031(3) 0.080(4) -0.033(4) C45A 0.088(4) 0.087(4) 0.066(3) 0.014(2) 0.003(3) 0.008(3) C45B 0.127(13) 0.19(2) 0.062(6) -0.009(9) -0.020(7) 0.083(15) C46A 0.068(3) 0.129(6) 0.075(3) -0.022(4) 0.005(3) -0.038(4) C46B 0.129(11) 0.077(6) 0.073(6) -0.008(5) -0.006(6) -0.022(7) C47A 0.088(4) 0.113(5) 0.066(3) -0.022(3) 0.012(3) 0.020(4) C47B 0.186(18) 0.24(3) 0.047(6) 0.005(9) 0.021(8) -0.120(18) C27A 0.086(4) 0.135(7) 0.058(3) 0.013(4) 0.010(3) -0.027(5) C27B 0.061(5) 0.060(5) 0.048(5) -0.003(4) 0.020(4) -0.013(4) C28A 0.105(6) 0.109(6) 0.061(4) 0.003(4) 0.011(3) 0.021(5) C28B 0.084(9) 0.139(15) 0.053(7) -0.014(8) -0.004(6) -0.013(10) O29A 0.111(5) 0.188(7) 0.079(3) -0.033(4) 0.052(3) -0.062(5) O29B 0.101(7) 0.130(9) 0.065(5) -0.001(6) 0.014(4) 0.044(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 -8 7 0.1355 3 -3 8 0.1286 4 0 7 0.1085 -6 0 -2 0.1586 -3 -6 -7 0.1128 -5 -7 -3 0.0567 -5 -9 0 0.0667 6 7 -2 0.0818 3 11 -2 0.0836 -5 -7 5 0.1146 -4 -11 2 0.0722 6 7 -5 0.1190 -3 -12 4 0.1042 -3 -6 9 0.1319 -1 11 -5 0.1609 -1 -1 11 0.1538 -1 0 -10 0.1612 -2 -7 -7 0.1169 1 10 6 0.0954 6 5 1 0.0983 0 12 5 0.1239 2 11 3 0.0965 -3 -11 -2 0.0754 -5 -9 0 0.0627 3 12 -1 0.0828 -3 -12 2 0.0762 1 13 -1 0.1146 5 -8 -7 0.2249 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C39 O38 C37 116.4(2) C25 O26 C27A 119.8(4) C25 O26 C27B 103.8(4) N24 N11 C12 109.5(2) N24 N11 C10 120.6(2) C12 N11 C10 129.7(2) C2 N1 C20 130.3(2) N21 N1 C2 108.9(2) N21 N1 C20 120.8(2) N23 C13 C14 121.2(2) C12 C13 N23 108.2(2) C12 C13 C14 130.6(2) C2 C3 C4 131.3(3) N22 C3 C2 108.2(2) N22 C3 C4 120.5(2) N23 N24 N11 108.0(2) N24 N23 C13 108.5(2) O26 C25 C19 119.7(2) O26 C25 C15 119.3(2) C19 C25 C15 121.0(2) C36 O35 C34 114.1(3) O38 C39 C9 118.0(2) O38 C39 C5 121.2(2) C5 C39 C9 120.7(2) C39 C9 C8 118.6(2) C39 C9 C10 121.1(2) C8 C9 C10 120.2(2) C19 C18 H18 119.1 C17 C18 H18 119.1 C17 C18 C19 121.8(2) C25 C19 C18 119.0(2) C25 C19 C20 120.9(2) C18 C19 C20 120.0(2) N11 C12 H12 127.1 C13 C12 N11 105.8(2) C13 C12 H12 127.1 C9 C8 H8 118.7 C7 C8 C9 122.6(2) C7 C8 H8 118.7 C39 C5 C6 118.8(2) C39 C5 C4 121.1(2) C6 C5 C4 120.0(2) C5 C6 H6 118.8 C7 C6 C5 122.3(2) C7 C6 H6 118.8 C8 C7 C6 116.8(2) C8 C7 C44 121.1(2) C6 C7 C44 122.1(2) C25 C15 C14 120.7(2) C16 C15 C25 117.9(2) C16 C15 C14 121.4(2) C15 C16 H16 118.5 C15 C16 C17 123.1(2) C17 C16 H16 118.5 C18 C17 C16 116.9(2) C18 C17 C40 122.5(2) C16 C17 C40 120.6(2) N11 C10 C9 111.24(19) N11 C10 H10A 109.4 N11 C10 H10B 109.4 C9 C10 H10A 109.4 C9 C10 H10B 109.4 H10A C10 H10B 108.0 N1 C2 C3 106.2(2) N1 C2 H2 126.9 C3 C2 H2 126.9 N21 N22 C3 108.8(3) N22 N21 N1 108.0(2) C3 C4 C5 113.3(2) C3 C4 H4A 108.9 C3 C4 H4B 108.9 C5 C4 H4A 108.9 C5 C4 H4B 108.9 H4A C4 H4B 107.7 N1 C20 C19 111.78(18) N1 C20 H20A 109.3 N1 C20 H20B 109.3 C19 C20 H20A 109.3 C19 C20 H20B 109.3 H20A C20 H20B 107.9 C7 C44 C45A 110.0(3) C7 C44 C46B 105.3(4) C45B C44 C7 111.3(5) C45B C44 C46B 111.9(11) C46A C44 C7 109.6(3) C46A C44 C45A 106.4(4) C47A C44 C7 115.2(3) C47A C44 C45A 105.7(4) C47A C44 C46A 109.5(4) C47B C44 C7 107.6(6) C47B C44 C45B 113.5(14) C47B C44 C46B 106.9(12) C17 C40 C41 112.0(2) C42 C40 C17 109.3(2) C42 C40 C41 107.6(3) C43 C40 C17 109.3(3) C43 C40 C41 108.8(3) C43 C40 C42 109.8(3) C13 C14 C15 113.4(2) C13 C14 H14A 108.9 C13 C14 H14B 108.9 C15 C14 H14A 108.9 C15 C14 H14B 108.9 H14A C14 H14B 107.7 O38 C37 H37A 109.6 O38 C37 H37B 109.6 O38 C37 C36 110.1(3) H37A C37 H37B 108.2 C36 C37 H37A 109.6 C36 C37 H37B 109.6 C31 O32A C33 117.7(5) C31 O32B C33 116.8(9) O35 C36 C37 111.1(3) O35 C36 H36A 109.4 O35 C36 H36B 109.4 C37 C36 H36A 109.4 C37 C36 H36B 109.4 H36A C36 H36B 108.0 C40 C41 H41A 109.5 C40 C41 H41B 109.5 C40 C41 H41C 109.5 H41A C41 H41B 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C40 C42 H42A 109.5 C40 C42 H42B 109.5 C40 C42 H42C 109.5 H42A C42 H42B 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C40 C43 H43A 109.5 C40 C43 H43B 109.5 C40 C43 H43C 109.5 H43A C43 H43B 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 H30C C30 H30D 107.7 H30A C30 H30B 107.1 C31 C30 H30C 108.8 C31 C30 H30D 108.8 C31 C30 H30A 107.7 C31 C30 H30B 107.7 C31 C30 O29B 118.4(7) O29A C30 H30C 108.8 O29A C30 H30D 108.8 O29A C30 C31 113.9(4) O29B C30 H30A 107.7 O29B C30 H30B 107.7 O35 C34 H34A 108.6 O35 C34 H34B 108.6 O35 C34 C33 114.5(4) H34A C34 H34B 107.6 C33 C34 H34A 108.6 C33 C34 H34B 108.6 O32A C33 C34 107.9(5) O32A C33 H33A 110.1 O32A C33 H33B 110.1 O32B C33 C34 130.6(8) O32B C33 H33C 104.6 O32B C33 H33D 104.6 C34 C33 H33A 110.1 C34 C33 H33B 110.1 C34 C33 H33C 104.6 C34 C33 H33D 104.6 H33A C33 H33B 108.4 H33C C33 H33D 105.7 O32A C31 C30 122.1(5) O32A C31 H31A 106.8 O32A C31 H31B 106.8 O32B C31 C30 121.3(7) O32B C31 H31C 107.0 O32B C31 H31D 107.0 C30 C31 H31A 106.8 C30 C31 H31B 106.8 C30 C31 H31C 107.0 C30 C31 H31D 107.0 H31A C31 H31B 106.7 H31C C31 H31D 106.7 C44 C45A H45A 109.5 C44 C45A H45B 109.5 C44 C45A H45C 109.5 H45A C45A H45B 109.5 H45A C45A H45C 109.5 H45B C45A H45C 109.5 C44 C45B H45D 109.5 C44 C45B H45E 109.5 C44 C45B H45F 109.5 H45D C45B H45E 109.5 H45D C45B H45F 109.5 H45E C45B H45F 109.5 C44 C46A H46A 109.5 C44 C46A H46B 109.5 C44 C46A H46C 109.5 H46A C46A H46B 109.5 H46A C46A H46C 109.5 H46B C46A H46C 109.5 C44 C46B H46D 109.5 C44 C46B H46E 109.5 C44 C46B H46F 109.5 H46D C46B H46E 109.5 H46D C46B H46F 109.5 H46E C46B H46F 109.5 C44 C47A H47A 109.5 C44 C47A H47B 109.5 C44 C47A H47C 109.5 H47A C47A H47B 109.5 H47A C47A H47C 109.5 H47B C47A H47C 109.5 C44 C47B H47D 109.5 C44 C47B H47E 109.5 C44 C47B H47F 109.5 H47D C47B H47E 109.5 H47D C47B H47F 109.5 H47E C47B H47F 109.5 O26 C27A H27A 110.4 O26 C27A H27B 110.5 O26 C27A C28B 106.4(9) H27A C27A H27B 108.6 C28B C27A H27A 110.4 C28B C27A H27B 110.4 O26 C27B H27C 109.8 O26 C27B H27D 109.8 H27C C27B H27D 108.2 C28A C27B O26 109.5(7) C28A C27B H27C 109.8 C28A C27B H27D 109.8 C27B C28A H28A 107.6 C27B C28A H28B 107.6 H28A C28A H28B 107.1 O29A C28A C27B 118.8(8) O29A C28A H28A 107.6 O29A C28A H28B 107.6 C27A C28B H28C 106.6 C27A C28B H28D 106.6 C27A C28B O29B 122.8(13) H28C C28B H28D 106.6 O29B C28B H28C 106.6 O29B C28B H28D 106.6 C28A O29A C30 119.7(7) C30 O29B C28B 126.1(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O38 C39 1.384(3) O38 C37 1.445(4) O26 C25 1.384(3) O26 C27A 1.399(7) O26 C27B 1.557(11) N11 N24 1.333(3) N11 C12 1.352(3) N11 C10 1.475(3) N1 C2 1.348(3) N1 N21 1.344(4) N1 C20 1.471(3) C13 N23 1.353(4) C13 C12 1.349(4) C13 C14 1.483(4) C3 C2 1.352(4) C3 N22 1.347(4) C3 C4 1.480(3) N24 N23 1.312(4) C25 C19 1.386(3) C25 C15 1.391(3) O35 C36 1.382(5) O35 C34 1.416(5) C39 C9 1.391(3) C39 C5 1.387(4) C9 C8 1.395(3) C9 C10 1.507(3) C18 H18 0.9300 C18 C19 1.390(3) C18 C17 1.386(3) C19 C20 1.519(3) C12 H12 0.9300 C8 H8 0.9300 C8 C7 1.390(3) C5 C6 1.396(4) C5 C4 1.514(3) C6 H6 0.9300 C6 C7 1.395(3) C7 C44 1.531(4) C15 C16 1.379(4) C15 C14 1.521(4) C16 H16 0.9300 C16 C17 1.397(4) C17 C40 1.535(4) C10 H10A 0.9700 C10 H10B 0.9700 C2 H2 0.9300 N22 N21 1.310(4) C4 H4A 0.9700 C4 H4B 0.9700 C20 H20A 0.9700 C20 H20B 0.9700 C44 C45A 1.586(6) C44 C45B 1.457(13) C44 C46A 1.529(6) C44 C46B 1.594(11) C44 C47A 1.513(6) C44 C47B 1.447(15) C40 C41 1.543(5) C40 C42 1.529(5) C40 C43 1.509(5) C14 H14A 0.9700 C14 H14B 0.9700 C37 H37A 0.9700 C37 H37B 0.9700 C37 C36 1.494(5) O32A C33 1.392(8) O32A C31 1.343(7) O32B C33 1.432(15) O32B C31 1.316(12) C36 H36A 0.9700 C36 H36B 0.9700 C41 H41A 0.9600 C41 H41B 0.9600 C41 H41C 0.9600 C42 H42A 0.9600 C42 H42B 0.9600 C42 H42C 0.9600 C43 H43A 0.9600 C43 H43B 0.9600 C43 H43C 0.9600 C30 H30C 0.9700 C30 H30D 0.9700 C30 H30A 0.9700 C30 H30B 0.9700 C30 C31 1.398(7) C30 O29A 1.383(7) C30 O29B 1.429(14) C34 H34A 0.9700 C34 H34B 0.9700 C34 C33 1.455(7) C33 H33A 0.9700 C33 H33B 0.9700 C33 H33C 0.9700 C33 H33D 0.9700 C31 H31A 0.9700 C31 H31B 0.9700 C31 H31C 0.9700 C31 H31D 0.9700 C45A H45A 0.9600 C45A H45B 0.9600 C45A H45C 0.9600 C45B H45D 0.9600 C45B H45E 0.9600 C45B H45F 0.9600 C46A H46A 0.9600 C46A H46B 0.9600 C46A H46C 0.9600 C46B H46D 0.9600 C46B H46E 0.9600 C46B H46F 0.9600 C47A H47A 0.9600 C47A H47B 0.9600 C47A H47C 0.9600 C47B H47D 0.9600 C47B H47E 0.9600 C47B H47F 0.9600 C27A H27A 0.9700 C27A H27B 0.9700 C27A C28B 1.490(19) C27B H27C 0.9700 C27B H27D 0.9700 C27B C28A 1.415(14) C28A H28A 0.9700 C28A H28B 0.9700 C28A O29A 1.196(11) C28B H28C 0.9700 C28B H28D 0.9700 C28B O29B 1.50(2) loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2.3467 -7.8152 6.6521 0.9204 0.2728 -0.2800 2.6214 -2.8879 8.3055 0.8238 0.5668 -0.0089 3.8278 0.3692 6.9691 0.6083 0.7936 -0.0089 -6.1475 0.2522 -1.5510 -0.2998 -0.8465 0.4400 -2.7763 -6.2002 -7.0038 -0.3125 -0.8852 -0.3447 -4.6386 -7.1158 -3.0024 -0.0255 -0.9967 -0.0777 -4.9401 -8.6578 0.3280 0.2845 -0.9586 0.0091 5.7096 6.9449 -1.6022 -0.2785 0.9393 -0.2004 3.3328 11.4792 -1.6221 -0.5559 0.8075 0.1971 -5.4957 -7.1546 4.9025 0.5393 -0.7845 0.3061 -3.5304 -11.2494 1.8905 0.5597 -0.8131 -0.1600 5.5695 6.8826 -5.0380 -0.5348 0.7779 -0.3299 -2.5579 -11.5910 4.3318 0.7841 -0.6008 -0.1554 -3.4307 -6.4157 9.2146 0.8837 -0.3128 0.3482 -1.3088 10.6379 -5.3565 -0.9251 0.0234 0.3790 -1.2319 -1.1630 11.0201 0.8375 0.2481 0.4869 -0.7359 -0.3174 -10.2397 -0.7667 -0.5271 -0.3666 -2.3258 -6.6476 -7.3332 -0.3037 -0.8579 -0.4144 0.7497 10.1862 6.3045 0.0198 0.7495 0.6617 5.8686 4.6261 0.9829 0.0249 0.9761 -0.2161 -0.4923 11.7122 5.0755 -0.1768 0.5980 0.7817 2.3549 11.3934 2.7575 -0.2541 0.8577 0.4469 -2.6228 -11.2414 -2.4905 0.2594 -0.8754 -0.4078 -4.7254 -9.0256 0.0156 0.2843 -0.9580 -0.0375 2.9303 11.8833 -1.0810 -0.5457 0.7935 0.2695 -3.2616 -11.5568 1.5213 0.5540 -0.8055 -0.2104 0.5950 13.0797 -1.3588 -0.6872 0.5273 0.4998 4.5646 -7.9294 -6.7528 -0.0076 0.0047 -1.0000