#------------------------------------------------------------------------------ #$Date: 2024-09-12 04:06:16 +0300 (Thu, 12 Sep 2024) $ #$Revision: 294728 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249333.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_7249333 loop_ _publ_author_name 'Poungsripong, Peeranuch' 'Boonprab, Theerapoom' 'Harding, Phimphaka' 'Murray, Keith S.' 'Phonsri, Wasinee' 'Zhang, Ningjin' 'Kitchen, Jonathan A.' 'Harding, David J.' _publ_section_title ; Synthesis, mixed-spin-state structure and Langmuir-Blodgett deposition of amphiphilic Fe(iii) quinolylsalicylaldiminate complexes. ; _journal_issue 39 _journal_name_full 'RSC advances' _journal_page_first 28716 _journal_page_last 28723 _journal_paper_doi 10.1039/d4ra06111j _journal_volume 14 _journal_year 2024 _chemical_formula_moiety 'C28 H36 N2 O2, 0.5(H2 O)' _chemical_formula_sum 'C28 H37 N2 O2.5' _chemical_formula_weight 441.59 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2019-10-29 _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-05-21 deposited with the CCDC. 2024-09-04 downloaded from the CCDC. ; _cell_angle_alpha 87.836(2) _cell_angle_beta 79.244(2) _cell_angle_gamma 74.869(3) _cell_formula_units_Z 4 _cell_length_a 11.2840(4) _cell_length_b 12.1389(4) _cell_length_c 19.1724(5) _cell_measurement_reflns_used 10861 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 30.4340 _cell_measurement_theta_min 2.0260 _cell_volume 2490.40(14) _computing_cell_refinement 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _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 N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 28.5714 _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -58.00 66.00 1.00 30.00 -- -22.90 57.00 90.00 124 2 \w -58.00 66.00 1.00 30.00 -- -22.90 57.00 0.00 124 3 \w -112.00 15.00 1.00 30.00 -- -22.90 -72.00 60.00 127 4 \w -112.00 15.00 1.00 30.00 -- -22.90 -72.00-120.00 127 5 \w -112.00 15.00 1.00 30.00 -- -22.90 -72.00 120.00 127 6 \w -61.00 66.00 1.00 30.00 -- -22.90 72.00 30.00 127 7 \w -112.00 15.00 1.00 30.00 -- -22.90 -72.00-180.00 127 8 \w -61.00 -36.00 1.00 30.00 -- -22.90 72.00-180.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC12 (RCD3): Kappa single' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen MicroLoop' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0418750000 _diffrn_orient_matrix_UB_12 0.0512882000 _diffrn_orient_matrix_UB_13 -0.0082886000 _diffrn_orient_matrix_UB_21 -0.0140913000 _diffrn_orient_matrix_UB_22 0.0169342000 _diffrn_orient_matrix_UB_23 0.0362525000 _diffrn_orient_matrix_UB_31 0.0493494000 _diffrn_orient_matrix_UB_32 0.0273349000 _diffrn_orient_matrix_UB_33 -0.0059440000 _diffrn_radiation_collimation 0.2 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_unetI/netI 0.0495 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 45828 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 1.902 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_current 55.0 _diffrn_source_power 2.475 _diffrn_source_target Mo _diffrn_source_type 'Rigaku (Mo) X-ray Source' _diffrn_source_voltage 45.0 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.178 _exptl_crystal_description plate _exptl_crystal_F_000 956 _exptl_crystal_size_max 0.055 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.291 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.039 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 639 _refine_ls_number_reflns 10166 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0568 _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^)+(0.0716P)^2^+0.3709P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1323 _refine_ls_wR_factor_ref 0.1580 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6046 _reflns_number_total 10166 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ra06111j2.cif _cod_data_source_block njz_pe_longchain _cod_original_formula_sum 'C28 H37 N2 O2.50' _cod_database_code 7249333 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula 'C H N O ' _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 0.999 _shelx_estimated_absorpt_t_min 0.996 _reflns_odcompleteness_completeness 99.98 _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 C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Restrained distances C131-C130 1.55 with sigma of 0.01 C128-C127 1.55 with sigma of 0.01 3. Others Fixed Sof: H12K(0.65) H12L(0.65) H12M(0.35) H12N(0.35) C126(0.65) H12O(0.65) H12P(0.65) C127(0.65) H12Q(0.65) H12R(0.65) C128(0.65) H12S(0.65) H12T(0.65) H12U(0.65) C129(0.35) H12V(0.35) H12W(0.35) C130(0.35) H13A(0.35) H13B(0.35) C131(0.35) H13C(0.35) H13D(0.35) H13E(0.35) O200(0.5) H20C(0.5) H20D(0.5) O201(0.5) H20E(0.5) H20F(0.5) 4.a Free rotating group: O200(H20C,H20D), O201(H20E,H20F) 4.b Secondary CH2 refined with riding coordinates: C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A, H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C117(H11A,H11B), C118(H11C,H11D), C119(H11E, H11F), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L), C125(H12M,H12N), C126(H12O,H12P), C127(H12Q, H12R), C129(H12V,H12W), C130(H13A,H13B) 4.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2A), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C13(H13), C15(H15), C16(H16), C101(H101), C102(H10A), C103(H103), C105(H105), C106(H106), C107(H107), C110(H110), C113(H113), C115(H115), C116(H116) 4.d Idealised Me refined as rotating group: C28(H28A,H28B,H28C), C128(H12S,H12T,H12U), C131(H13C,H13D,H13E) ; _shelx_res_file ; TITL njz_pe_longchain_a.res in P-1 njz_pe_longchain.res created by SHELXL-2018/1 at 15:15:30 on 29-Oct-2019 REM Old TITL NJZ_PE_longchain in P-1 REM SHELXT solution in P-1 REM R1 0.233, Rweak 0.010, Alpha 0.057, Orientation as input REM Formula found by SHELXT: C57 N4 O4 CELL 0.71073 11.284 12.1389 19.1724 87.836 79.244 74.869 ZERR 4 0.0004 0.0004 0.0005 0.002 0.002 0.003 LATT 1 SFAC C H N O UNIT 112 148 8 10 EQIV $1 1+X,+Y,+Z DFIX 1.55 0.01 C131 C130 DFIX 1.55 0.01 C128 C127 L.S. 10 PLAN 20 SIZE 0.015 0.05 0.055 TEMP -173 HTAB N2 O1 HTAB N102 O101 HTAB O200 O101_$1 BOND $H LIST 4 CONF WPDB HTAB fmap 2 acta OMIT 0 1 0 OMIT 0 0 2 OMIT 1 -2 8 OMIT 0 -1 1 OMIT 0 1 1 OMIT 0 0 3 REM REM REM WGHT 0.071600 0.370900 FVAR 0.30490 O1 4 0.852499 0.368342 0.744772 11.00000 0.04186 0.04425 = 0.03675 0.00730 -0.00862 -0.01261 O2 4 0.728114 0.744193 0.654704 11.00000 0.04074 0.04079 = 0.04194 0.00946 -0.01288 -0.01168 N1 3 0.966941 0.128898 0.839125 11.00000 0.05983 0.05321 = 0.03978 0.00137 0.00102 -0.01460 N2 3 1.022017 0.329238 0.823653 11.00000 0.03725 0.04894 = 0.02965 0.00545 -0.00669 -0.00682 H2 2 0.960627 0.306643 0.799795 11.00000 0.07262 C1 1 0.938251 0.030475 0.845640 11.00000 0.07309 0.05944 = 0.04884 0.00283 0.00610 -0.02174 AFIX 43 H1 2 0.875211 0.020399 0.821729 11.00000 -1.20000 AFIX 0 C2 1 0.994721 -0.061065 0.885705 11.00000 0.09313 0.05525 = 0.05273 0.00315 0.01679 -0.01870 AFIX 43 H2A 2 0.970393 -0.130592 0.888581 11.00000 -1.20000 AFIX 0 C3 1 1.084992 -0.047543 0.920207 11.00000 0.08837 0.05509 = 0.04032 0.01113 0.01202 0.00496 AFIX 43 H3 2 1.124170 -0.108121 0.947722 11.00000 -1.20000 AFIX 0 C4 1 1.120957 0.056204 0.915389 11.00000 0.06591 0.05600 = 0.02932 0.00652 0.00565 0.00245 C5 1 1.213485 0.078556 0.949162 11.00000 0.07254 0.07130 = 0.03739 0.00884 -0.01188 0.01271 AFIX 43 H5 2 1.256591 0.021359 0.977277 11.00000 -1.20000 AFIX 0 C6 1 1.241251 0.181145 0.941737 11.00000 0.06201 0.07705 = 0.04748 -0.00037 -0.02063 0.00483 AFIX 43 H6 2 1.303507 0.194691 0.965011 11.00000 -1.20000 AFIX 0 C7 1 1.179672 0.268097 0.900211 11.00000 0.05437 0.05984 = 0.04258 0.00078 -0.01494 -0.00387 AFIX 43 H7 2 1.200360 0.339358 0.895715 11.00000 -1.20000 AFIX 0 C8 1 1.089814 0.249172 0.866388 11.00000 0.04592 0.05163 = 0.02943 0.00209 -0.00408 -0.00334 C9 1 1.058223 0.143056 0.873631 11.00000 0.05445 0.05243 = 0.02718 0.00303 0.00061 -0.00300 C10 1 1.027874 0.435422 0.811467 11.00000 0.03587 0.04877 = 0.03459 0.00044 -0.00407 -0.01152 AFIX 43 H10 2 1.085386 0.463076 0.831732 11.00000 -1.20000 AFIX 0 C11 1 0.953009 0.508745 0.770016 11.00000 0.03269 0.04494 = 0.02905 0.00428 -0.00290 -0.01016 C12 1 0.864515 0.470153 0.737196 11.00000 0.03292 0.04262 = 0.02596 0.00125 0.00110 -0.00892 C13 1 0.789657 0.551616 0.696761 11.00000 0.03410 0.04362 = 0.02851 0.00325 -0.00433 -0.01140 AFIX 43 H13 2 0.732267 0.528806 0.673643 11.00000 -1.20000 AFIX 0 C14 1 0.799022 0.661377 0.690731 11.00000 0.03263 0.04329 = 0.02913 0.00564 -0.00172 -0.00945 C15 1 0.885016 0.699134 0.723521 11.00000 0.04325 0.04204 = 0.04212 0.00570 -0.00836 -0.01524 AFIX 43 H15 2 0.890434 0.775944 0.718863 11.00000 -1.20000 AFIX 0 C16 1 0.958863 0.624166 0.761379 11.00000 0.03663 0.05040 = 0.03918 0.00243 -0.00701 -0.01715 AFIX 43 H16 2 1.016544 0.649463 0.782909 11.00000 -1.20000 AFIX 0 C17 1 0.637151 0.711752 0.622073 11.00000 0.03831 0.04094 = 0.03368 0.00417 -0.00810 -0.01162 AFIX 23 H17A 2 0.579262 0.681618 0.658346 11.00000 -1.20000 H17B 2 0.679430 0.651210 0.585922 11.00000 -1.20000 AFIX 0 C18 1 0.565365 0.815426 0.587630 11.00000 0.04148 0.03753 = 0.03419 0.00314 -0.00690 -0.00962 AFIX 23 H18A 2 0.624197 0.846006 0.552253 11.00000 -1.20000 H18B 2 0.523190 0.875363 0.624178 11.00000 -1.20000 AFIX 0 C19 1 0.468439 0.786251 0.551195 11.00000 0.04421 0.03572 = 0.03278 0.00544 -0.00773 -0.01129 AFIX 23 H19A 2 0.410300 0.755453 0.586910 11.00000 -1.20000 H19B 2 0.511303 0.725510 0.515258 11.00000 -1.20000 AFIX 0 C20 1 0.392973 0.887646 0.514944 11.00000 0.04306 0.03261 = 0.03256 0.00426 -0.00680 -0.00994 AFIX 23 H20A 2 0.351454 0.949085 0.550621 11.00000 -1.20000 H20B 2 0.450809 0.917397 0.478418 11.00000 -1.20000 AFIX 0 C21 1 0.294596 0.858241 0.480097 11.00000 0.04715 0.03485 = 0.03149 0.00458 -0.01009 -0.01303 AFIX 23 H21A 2 0.237354 0.827931 0.516684 11.00000 -1.20000 H21B 2 0.336438 0.796874 0.444417 11.00000 -1.20000 AFIX 0 C22 1 0.217819 0.958103 0.443926 11.00000 0.04650 0.03476 = 0.03336 0.00427 -0.01049 -0.01335 AFIX 23 H22A 2 0.177741 1.020375 0.479235 11.00000 -1.20000 H22B 2 0.274646 0.987018 0.406318 11.00000 -1.20000 AFIX 0 C23 1 0.117276 0.928432 0.411032 11.00000 0.04997 0.03505 = 0.03101 0.00583 -0.01159 -0.01491 AFIX 23 H23A 2 0.157093 0.865444 0.376183 11.00000 -1.20000 H23B 2 0.059552 0.900714 0.448727 11.00000 -1.20000 AFIX 0 C24 1 0.042314 1.028369 0.374071 11.00000 0.05250 0.03813 = 0.03576 0.00677 -0.01540 -0.01581 AFIX 23 H24A 2 0.099930 1.053951 0.335264 11.00000 -1.20000 H24B 2 0.005858 1.092396 0.408527 11.00000 -1.20000 AFIX 0 C25 1 -0.062434 1.002457 0.343201 11.00000 0.05203 0.03608 = 0.03061 0.00593 -0.01086 -0.01508 AFIX 23 H25A 2 -0.119033 0.974925 0.381651 11.00000 -1.20000 H25B 2 -0.025968 0.940127 0.307567 11.00000 -1.20000 AFIX 0 C26 1 -0.138830 1.104946 0.308174 11.00000 0.05013 0.03775 = 0.03214 0.00547 -0.01206 -0.01545 AFIX 23 H26A 2 -0.177485 1.166399 0.344187 11.00000 -1.20000 H26B 2 -0.081834 1.133992 0.270736 11.00000 -1.20000 AFIX 0 C27 1 -0.240937 1.078128 0.275350 11.00000 0.04705 0.03828 = 0.03195 0.00517 -0.00923 -0.01480 AFIX 23 H27A 2 -0.298362 1.049641 0.312825 11.00000 -1.20000 H27B 2 -0.202425 1.016366 0.239524 11.00000 -1.20000 AFIX 0 C28 1 -0.316243 1.180553 0.240068 11.00000 0.05457 0.05040 = 0.03836 0.00770 -0.01205 -0.01511 AFIX 137 H28A 2 -0.356372 1.241524 0.275412 11.00000 -1.50000 H28B 2 -0.380296 1.157842 0.220092 11.00000 -1.50000 H28C 2 -0.260461 1.208122 0.202023 11.00000 -1.50000 AFIX 0 O101 4 -0.294016 0.491443 0.187255 11.00000 0.04643 0.06143 = 0.03451 -0.00418 0.00229 -0.01404 O102 4 -0.311205 0.458322 0.437941 11.00000 0.04128 0.05904 = 0.03310 -0.00590 -0.00299 -0.02132 N101 3 -0.354399 0.595098 0.014767 11.00000 0.05347 0.09721 = 0.04358 -0.01513 0.00701 -0.01360 N102 3 -0.498705 0.599088 0.143484 11.00000 0.04370 0.04985 = 0.03829 0.00101 -0.00258 -0.01432 H102 2 -0.413696 0.564431 0.133982 11.00000 0.07145 C101 1 -0.283767 0.593115 -0.048441 11.00000 0.06216 0.14572 = 0.04885 -0.01915 0.01191 -0.01179 AFIX 43 H101 2 -0.195892 0.566936 -0.051581 11.00000 -1.20000 AFIX 0 C102 1 -0.328793 0.626814 -0.111424 11.00000 0.07626 0.09407 = 0.04391 -0.00386 0.01531 -0.00416 AFIX 43 H10A 2 -0.272621 0.622967 -0.155387 11.00000 -1.20000 AFIX 0 C103 1 -0.451332 0.664229 -0.108630 11.00000 0.07452 0.05586 = 0.04163 0.00938 0.00450 0.00484 AFIX 43 H103 2 -0.483987 0.686975 -0.150667 11.00000 -1.20000 AFIX 0 C104 1 -0.532578 0.669750 -0.042197 11.00000 0.06201 0.05064 = 0.04118 0.01249 0.00294 0.00373 C105 1 -0.662097 0.709879 -0.034138 11.00000 0.06928 0.12996 = 0.04486 0.03552 -0.00335 0.01245 AFIX 43 H105 2 -0.699651 0.733091 -0.074535 11.00000 -1.20000 AFIX 0 C106 1 -0.735478 0.715872 0.032235 11.00000 0.05666 0.17789 = 0.04765 0.04499 0.00126 0.01513 AFIX 43 H106 2 -0.823344 0.745489 0.037236 11.00000 -1.20000 AFIX 0 C107 1 -0.683597 0.679396 0.092294 11.00000 0.05342 0.11625 = 0.04206 0.02713 0.00122 -0.00572 AFIX 43 H107 2 -0.735983 0.683041 0.137566 11.00000 -1.20000 AFIX 0 C108 1 -0.558143 0.638698 0.085907 11.00000 0.05000 0.05004 = 0.03870 0.00907 0.00003 -0.01082 C109 1 -0.479504 0.634067 0.017926 11.00000 0.05541 0.04171 = 0.04190 0.00273 0.00283 -0.00800 C110 1 -0.551532 0.606369 0.211490 11.00000 0.04175 0.04554 = 0.04223 -0.00513 0.00180 -0.01923 AFIX 43 H110 2 -0.638262 0.642348 0.223741 11.00000 -1.20000 AFIX 0 C111 1 -0.486873 0.564202 0.265834 11.00000 0.04037 0.04357 = 0.03657 -0.00527 -0.00264 -0.01972 C112 1 -0.355079 0.505835 0.251308 11.00000 0.04428 0.04259 = 0.03645 -0.00688 0.00164 -0.02090 C113 1 -0.296503 0.467530 0.310515 11.00000 0.03948 0.04521 = 0.03731 -0.00510 -0.00093 -0.01872 AFIX 43 H113 2 -0.210730 0.427278 0.302773 11.00000 -1.20000 AFIX 0 C114 1 -0.361886 0.487790 0.378577 11.00000 0.04203 0.04227 = 0.03786 -0.00440 -0.00517 -0.02304 C115 1 -0.491751 0.544009 0.392803 11.00000 0.04356 0.05344 = 0.03415 -0.00959 0.00051 -0.02336 AFIX 43 H115 2 -0.536241 0.555413 0.440283 11.00000 -1.20000 AFIX 0 C116 1 -0.550676 0.580843 0.337848 11.00000 0.03852 0.04916 = 0.04188 -0.00936 0.00118 -0.02089 AFIX 43 H116 2 -0.637090 0.618937 0.347360 11.00000 -1.20000 AFIX 0 C117 1 -0.178625 0.407388 0.428826 11.00000 0.04182 0.04474 = 0.03665 -0.00453 -0.00029 -0.01990 AFIX 23 H11A 2 -0.132524 0.456084 0.398480 11.00000 -1.20000 H11B 2 -0.157438 0.331400 0.405741 11.00000 -1.20000 AFIX 0 C118 1 -0.143245 0.396011 0.501358 11.00000 0.04890 0.04341 = 0.03700 -0.00377 -0.00223 -0.02357 AFIX 23 H11C 2 -0.192307 0.349358 0.531465 11.00000 -1.20000 H11D 2 -0.165268 0.472650 0.523682 11.00000 -1.20000 AFIX 0 C119 1 -0.005038 0.341282 0.498744 11.00000 0.04763 0.04092 = 0.03483 -0.00262 0.00004 -0.02134 AFIX 23 H11E 2 0.044134 0.386721 0.467588 11.00000 -1.20000 H11F 2 0.016542 0.263759 0.477694 11.00000 -1.20000 AFIX 0 C120 1 0.030952 0.332948 0.572078 11.00000 0.04723 0.04496 = 0.03425 -0.00508 -0.00092 -0.02310 AFIX 23 H12A 2 0.010198 0.410834 0.592494 11.00000 -1.20000 H12B 2 -0.020306 0.289329 0.603309 11.00000 -1.20000 AFIX 0 C121 1 0.167662 0.276624 0.572488 11.00000 0.04817 0.04429 = 0.03327 -0.00214 0.00075 -0.02031 AFIX 23 H12C 2 0.219004 0.322543 0.543508 11.00000 -1.20000 H12D 2 0.189809 0.200195 0.549873 11.00000 -1.20000 AFIX 0 C122 1 0.200148 0.263572 0.646653 11.00000 0.05163 0.04652 = 0.03471 -0.00240 -0.00019 -0.02584 AFIX 23 H12E 2 0.181391 0.340292 0.668442 11.00000 -1.20000 H12F 2 0.146132 0.220590 0.676237 11.00000 -1.20000 AFIX 0 C123 1 0.335886 0.202647 0.647560 11.00000 0.05372 0.04526 = 0.03627 0.00015 -0.00197 -0.02446 AFIX 23 H12G 2 0.389709 0.248430 0.620746 11.00000 -1.20000 H12H 2 0.356277 0.128096 0.622807 11.00000 -1.20000 AFIX 0 C124 1 0.366251 0.182543 0.721980 11.00000 0.07052 0.04549 = 0.03414 0.00108 -0.00562 -0.02925 AFIX 23 H12I 2 0.351584 0.257337 0.745525 11.00000 -1.20000 H12J 2 0.308408 0.141482 0.749889 11.00000 -1.20000 AFIX 0 C125 1 0.498278 0.115226 0.722922 11.00000 0.09205 0.05224 = 0.04934 -0.00130 -0.02910 -0.00548 PART 1 AFIX 23 H12K 2 0.557105 0.162585 0.706153 10.65000 -1.20000 H12L 2 0.520702 0.047067 0.691627 10.65000 -1.20000 AFIX 23 PART 0 PART 2 H12M 2 0.551470 0.148884 0.685812 10.35000 -1.20000 H12N 2 0.504515 0.037701 0.705677 10.35000 -1.20000 AFIX 0 PART 0 PART 1 C126 1 0.504260 0.079084 0.800999 10.65000 0.05962 0.05024 = 0.04979 0.00108 -0.01757 -0.01917 AFIX 23 H12O 2 0.494236 0.147379 0.830388 10.65000 -1.20000 H12P 2 0.434860 0.044141 0.819865 10.65000 -1.20000 AFIX 0 C127 1 0.627689 -0.005584 0.805790 10.65000 0.06433 0.08728 = 0.07393 0.01739 -0.02646 -0.01471 AFIX 23 H12Q 2 0.697070 0.026922 0.783001 10.65000 -1.20000 H12R 2 0.634307 -0.076380 0.779662 10.65000 -1.20000 AFIX 0 C128 1 0.639979 -0.034545 0.883197 10.65000 0.08819 0.10107 = 0.08113 0.04063 -0.03793 -0.03225 AFIX 137 H12S 2 0.575458 -0.072436 0.904736 10.65000 -1.50000 H12T 2 0.629661 0.035826 0.909709 10.65000 -1.50000 H12U 2 0.722661 -0.085510 0.884554 10.65000 -1.50000 AFIX 0 PART 0 PART 2 C129 1 0.566531 0.096997 0.790333 10.35000 0.05101 0.06239 = 0.06143 0.01702 -0.02475 -0.02602 AFIX 23 H12V 2 0.658036 0.083240 0.775183 10.35000 -1.20000 H12W 2 0.535382 0.164547 0.822367 10.35000 -1.20000 AFIX 0 C130 1 0.533734 -0.006985 0.826844 10.35000 0.05477 0.04672 = 0.06715 0.00729 -0.01920 -0.00889 AFIX 23 H13A 2 0.574246 -0.074769 0.795762 10.35000 -1.20000 H13B 2 0.442280 0.003730 0.833539 10.35000 -1.20000 AFIX 0 C131 1 0.574724 -0.029401 0.899526 10.35000 0.07543 0.09381 = 0.07064 0.03070 -0.03523 -0.02822 AFIX 137 H13C 2 0.666087 -0.049235 0.892713 10.35000 -1.50000 H13D 2 0.544151 -0.092620 0.922687 10.35000 -1.50000 H13E 2 0.539994 0.039402 0.929388 10.35000 -1.50000 AFIX 6 PART 0 PART 1 O200 4 0.887560 0.332673 0.109781 10.50000 0.04863 0.08387 = 0.08613 -0.04485 -0.01033 0.00393 H20C 2 0.863550 0.347049 0.070174 10.50000 -1.50000 H20D 2 0.838823 0.378949 0.141273 10.50000 -1.50000 AFIX 6 PART 0 PART 2 O201 4 0.924817 0.374602 0.065009 10.50000 0.13340 0.12697 = 0.15357 -0.01758 -0.06996 -0.03246 H20E 2 0.968586 0.422616 0.060808 10.50000 -1.50000 H20F 2 0.866391 0.396738 0.041345 10.50000 -1.50000 AFIX 0 HKLF 4 REM njz_pe_longchain_a.res in P-1 REM R1 = 0.0568 for 6046 Fo > 4sig(Fo) and 0.1076 for all 10166 data REM 639 parameters refined using 2 restraints END WGHT 0.0717 0.3717 REM Instructions for potential hydrogen bonds HTAB N2 O1 EQIV $2 -x+2, -y, -z+1 HTAB C2 O200_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C10 O101_$3 HTAB N102 O101 EQIV $4 -x, -y+1, -z+1 HTAB C107 O1_$4 HTAB C110 O1_$4 EQIV $5 -x-1, -y+1, -z+1 HTAB C115 O102_$5 REM Highest difference peak 0.291, deepest hole -0.268, 1-sigma level 0.039 Q1 1 -0.7821 0.6601 0.0201 11.00000 0.05 0.29 Q2 1 -0.7062 0.6532 -0.0491 11.00000 0.05 0.28 Q3 1 -0.7361 0.7427 0.0374 11.00000 0.05 0.26 Q4 1 1.0000 0.5000 0.0000 10.50000 0.05 0.22 Q5 1 -0.5827 0.6387 -0.0607 11.00000 0.05 0.22 Q6 1 -0.1630 0.4232 0.4673 11.00000 0.05 0.20 Q7 1 -0.6176 0.6259 0.0749 11.00000 0.05 0.19 Q8 1 -0.4998 0.6442 -0.1328 11.00000 0.05 0.19 Q9 1 -0.5150 0.5525 0.3011 11.00000 0.05 0.17 Q10 1 0.2351 1.0194 0.4395 11.00000 0.05 0.17 Q11 1 -0.3185 0.4975 0.3428 11.00000 0.05 0.17 Q12 1 0.0015 0.3410 0.5362 11.00000 0.05 0.16 Q13 1 -0.7219 0.6425 0.0787 11.00000 0.05 0.16 Q14 1 0.5526 0.0545 0.6868 11.00000 0.05 0.16 Q15 1 -0.6811 0.7012 0.1014 11.00000 0.05 0.16 Q16 1 0.7085 0.0290 0.8720 11.00000 0.05 0.16 Q17 1 0.0606 1.1027 0.3676 11.00000 0.05 0.16 Q18 1 1.0288 0.3267 0.0029 11.00000 0.05 0.15 Q19 1 -0.1543 0.3823 0.5176 11.00000 0.05 0.15 Q20 1 0.4393 0.1413 0.7104 11.00000 0.05 0.15 ; _shelx_res_checksum 26438 _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 1.598 _oxdiff_exptl_absorpt_empirical_full_min 0.681 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 O1 O 0.85250(12) 0.36834(11) 0.74477(7) 0.0407(3) Uani 1 1 d . . . . . O2 O 0.72811(12) 0.74419(11) 0.65470(7) 0.0405(3) Uani 1 1 d . . . . . N1 N 0.96694(18) 0.12890(16) 0.83913(9) 0.0523(5) Uani 1 1 d . . . . . N2 N 1.02202(15) 0.32924(15) 0.82365(8) 0.0395(4) Uani 1 1 d . . . . . H2 H 0.961(2) 0.3066(19) 0.7998(12) 0.073(8) Uiso 1 1 d . . . . . C1 C 0.9383(2) 0.0305(2) 0.84564(12) 0.0619(7) Uani 1 1 d . . . . . H1 H 0.875211 0.020399 0.821729 0.074 Uiso 1 1 calc R . . . . C2 C 0.9947(3) -0.0611(2) 0.88570(14) 0.0712(8) Uani 1 1 d . . . . . H2A H 0.970393 -0.130592 0.888581 0.085 Uiso 1 1 calc R . . . . C3 C 1.0850(3) -0.0475(2) 0.92021(13) 0.0692(8) Uani 1 1 d . . . . . H3 H 1.124170 -0.108121 0.947722 0.083 Uiso 1 1 calc R . . . . C4 C 1.1210(2) 0.0562(2) 0.91539(11) 0.0560(6) Uani 1 1 d . . . . . C5 C 1.2135(2) 0.0786(2) 0.94916(12) 0.0663(7) Uani 1 1 d . . . . . H5 H 1.256591 0.021359 0.977277 0.080 Uiso 1 1 calc R . . . . C6 C 1.2413(2) 0.1811(2) 0.94174(12) 0.0651(7) Uani 1 1 d . . . . . H6 H 1.303507 0.194691 0.965011 0.078 Uiso 1 1 calc R . . . . C7 C 1.1797(2) 0.2681(2) 0.90021(11) 0.0535(6) Uani 1 1 d . . . . . H7 H 1.200360 0.339358 0.895715 0.064 Uiso 1 1 calc R . . . . C8 C 1.08981(19) 0.24917(18) 0.86639(10) 0.0445(5) Uani 1 1 d . . . . . C9 C 1.0582(2) 0.14306(19) 0.87363(10) 0.0479(5) Uani 1 1 d . . . . . C10 C 1.02787(18) 0.43542(17) 0.81147(10) 0.0400(5) Uani 1 1 d . . . . . H10 H 1.085386 0.463076 0.831732 0.048 Uiso 1 1 calc R . . . . C11 C 0.95301(17) 0.50874(16) 0.77002(9) 0.0360(4) Uani 1 1 d . . . . . C12 C 0.86451(17) 0.47015(16) 0.73720(9) 0.0349(4) Uani 1 1 d . . . . . C13 C 0.78966(17) 0.55162(16) 0.69676(9) 0.0354(4) Uani 1 1 d . . . . . H13 H 0.732267 0.528806 0.673643 0.043 Uiso 1 1 calc R . . . . C14 C 0.79902(17) 0.66138(16) 0.69073(9) 0.0358(4) Uani 1 1 d . . . . . C15 C 0.88502(18) 0.69913(17) 0.72352(10) 0.0417(5) Uani 1 1 d . . . . . H15 H 0.890434 0.775944 0.718863 0.050 Uiso 1 1 calc R . . . . C16 C 0.95886(18) 0.62417(17) 0.76138(10) 0.0410(5) Uani 1 1 d . . . . . H16 H 1.016544 0.649463 0.782909 0.049 Uiso 1 1 calc R . . . . C17 C 0.63715(17) 0.71175(16) 0.62207(10) 0.0373(5) Uani 1 1 d . . . . . H17A H 0.579262 0.681618 0.658346 0.045 Uiso 1 1 calc R . . . . H17B H 0.679430 0.651210 0.585922 0.045 Uiso 1 1 calc R . . . . C18 C 0.56537(18) 0.81543(16) 0.58763(10) 0.0379(5) Uani 1 1 d . . . . . H18A H 0.624197 0.846006 0.552253 0.046 Uiso 1 1 calc R . . . . H18B H 0.523190 0.875363 0.624178 0.046 Uiso 1 1 calc R . . . . C19 C 0.46844(18) 0.78625(16) 0.55119(10) 0.0374(5) Uani 1 1 d . . . . . H19A H 0.410300 0.755453 0.586910 0.045 Uiso 1 1 calc R . . . . H19B H 0.511303 0.725510 0.515258 0.045 Uiso 1 1 calc R . . . . C20 C 0.39297(18) 0.88765(15) 0.51494(10) 0.0362(4) Uani 1 1 d . . . . . H20A H 0.351454 0.949085 0.550621 0.043 Uiso 1 1 calc R . . . . H20B H 0.450809 0.917397 0.478418 0.043 Uiso 1 1 calc R . . . . C21 C 0.29460(18) 0.85824(16) 0.48010(10) 0.0371(5) Uani 1 1 d . . . . . H21A H 0.237354 0.827931 0.516684 0.045 Uiso 1 1 calc R . . . . H21B H 0.336438 0.796874 0.444417 0.045 Uiso 1 1 calc R . . . . C22 C 0.21782(18) 0.95810(16) 0.44393(10) 0.0373(5) Uani 1 1 d . . . . . H22A H 0.177741 1.020375 0.479235 0.045 Uiso 1 1 calc R . . . . H22B H 0.274646 0.987018 0.406318 0.045 Uiso 1 1 calc R . . . . C23 C 0.11728(18) 0.92843(16) 0.41103(10) 0.0375(5) Uani 1 1 d . . . . . H23A H 0.157093 0.865444 0.376183 0.045 Uiso 1 1 calc R . . . . H23B H 0.059552 0.900714 0.448727 0.045 Uiso 1 1 calc R . . . . C24 C 0.04231(19) 1.02837(16) 0.37407(10) 0.0405(5) Uani 1 1 d . . . . . H24A H 0.099930 1.053951 0.335264 0.049 Uiso 1 1 calc R . . . . H24B H 0.005858 1.092396 0.408527 0.049 Uiso 1 1 calc R . . . . C25 C -0.06243(19) 1.00246(16) 0.34320(10) 0.0386(5) Uani 1 1 d . . . . . H25A H -0.119033 0.974925 0.381651 0.046 Uiso 1 1 calc R . . . . H25B H -0.025968 0.940127 0.307567 0.046 Uiso 1 1 calc R . . . . C26 C -0.13883(19) 1.10495(16) 0.30817(10) 0.0388(5) Uani 1 1 d . . . . . H26A H -0.177485 1.166399 0.344187 0.047 Uiso 1 1 calc R . . . . H26B H -0.081834 1.133992 0.270736 0.047 Uiso 1 1 calc R . . . . C27 C -0.24094(18) 1.07813(16) 0.27535(10) 0.0382(5) Uani 1 1 d . . . . . H27A H -0.298362 1.049641 0.312825 0.046 Uiso 1 1 calc R . . . . H27B H -0.202425 1.016366 0.239524 0.046 Uiso 1 1 calc R . . . . C28 C -0.3162(2) 1.18055(18) 0.24007(11) 0.0472(5) Uani 1 1 d . . . . . H28A H -0.356372 1.241524 0.275412 0.071 Uiso 1 1 calc GR . . . . H28B H -0.380296 1.157842 0.220092 0.071 Uiso 1 1 calc GR . . . . H28C H -0.260461 1.208122 0.202023 0.071 Uiso 1 1 calc GR . . . . O101 O -0.29402(13) 0.49144(12) 0.18725(7) 0.0486(4) Uani 1 1 d . . . . . O102 O -0.31120(12) 0.45832(12) 0.43794(7) 0.0432(4) Uani 1 1 d . . . . . N101 N -0.35440(19) 0.59510(19) 0.01477(10) 0.0676(6) Uani 1 1 d . . . . . N102 N -0.49871(18) 0.59909(15) 0.14348(9) 0.0442(4) Uani 1 1 d . . . . . H102 H -0.414(2) 0.564(2) 0.1340(12) 0.071(8) Uiso 1 1 d . . . . . C101 C -0.2838(3) 0.5931(3) -0.04844(14) 0.0909(10) Uani 1 1 d . . . . . H101 H -0.195892 0.566936 -0.051581 0.109 Uiso 1 1 calc R . . . . C102 C -0.3288(3) 0.6268(2) -0.11142(13) 0.0782(8) Uani 1 1 d . . . . . H10A H -0.272621 0.622967 -0.155387 0.094 Uiso 1 1 calc R . . . . C103 C -0.4513(3) 0.6642(2) -0.10863(12) 0.0637(7) Uani 1 1 d . . . . . H103 H -0.483987 0.686975 -0.150667 0.076 Uiso 1 1 calc R . . . . C104 C -0.5326(2) 0.66975(19) -0.04220(11) 0.0567(6) Uani 1 1 d . . . . . C105 C -0.6621(3) 0.7099(3) -0.03414(14) 0.0905(10) Uani 1 1 d . . . . . H105 H -0.699651 0.733091 -0.074535 0.109 Uiso 1 1 calc R . . . . C106 C -0.7355(3) 0.7159(3) 0.03223(14) 0.1053(13) Uani 1 1 d . . . . . H106 H -0.823344 0.745489 0.037236 0.126 Uiso 1 1 calc R . . . . C107 C -0.6836(2) 0.6794(3) 0.09229(13) 0.0757(8) Uani 1 1 d . . . . . H107 H -0.735983 0.683041 0.137566 0.091 Uiso 1 1 calc R . . . . C108 C -0.5581(2) 0.63870(18) 0.08591(11) 0.0480(5) Uani 1 1 d . . . . . C109 C -0.4795(2) 0.63407(18) 0.01793(11) 0.0488(5) Uani 1 1 d . . . . . C110 C -0.55153(19) 0.60637(17) 0.21149(10) 0.0428(5) Uani 1 1 d . . . . . H110 H -0.638262 0.642348 0.223741 0.051 Uiso 1 1 calc R . . . . C111 C -0.48687(18) 0.56420(17) 0.26583(10) 0.0389(5) Uani 1 1 d . . . . . C112 C -0.35508(19) 0.50583(17) 0.25131(10) 0.0403(5) Uani 1 1 d . . . . . C113 C -0.29650(19) 0.46753(17) 0.31051(10) 0.0399(5) Uani 1 1 d . . . . . H113 H -0.210730 0.427278 0.302773 0.048 Uiso 1 1 calc R . . . . C114 C -0.36189(18) 0.48779(17) 0.37858(10) 0.0386(5) Uani 1 1 d . . . . . C115 C -0.49175(19) 0.54401(17) 0.39280(10) 0.0424(5) Uani 1 1 d . . . . . H115 H -0.536241 0.555413 0.440283 0.051 Uiso 1 1 calc R . . . . C116 C -0.55068(19) 0.58084(17) 0.33785(10) 0.0423(5) Uani 1 1 d . . . . . H116 H -0.637090 0.618937 0.347360 0.051 Uiso 1 1 calc R . . . . C117 C -0.17863(18) 0.40739(17) 0.42883(10) 0.0402(5) Uani 1 1 d . . . . . H11A H -0.132524 0.456084 0.398480 0.048 Uiso 1 1 calc R . . . . H11B H -0.157438 0.331400 0.405741 0.048 Uiso 1 1 calc R . . . . C118 C -0.14325(18) 0.39601(17) 0.50136(10) 0.0415(5) Uani 1 1 d . . . . . H11C H -0.192307 0.349358 0.531465 0.050 Uiso 1 1 calc R . . . . H11D H -0.165268 0.472650 0.523682 0.050 Uiso 1 1 calc R . . . . C119 C -0.00504(18) 0.34128(17) 0.49874(10) 0.0402(5) Uani 1 1 d . . . . . H11E H 0.044134 0.386721 0.467588 0.048 Uiso 1 1 calc R . . . . H11F H 0.016542 0.263759 0.477694 0.048 Uiso 1 1 calc R . . . . C120 C 0.03095(18) 0.33295(17) 0.57208(10) 0.0407(5) Uani 1 1 d . . . . . H12A H 0.010198 0.410834 0.592494 0.049 Uiso 1 1 calc R . . . . H12B H -0.020306 0.289329 0.603309 0.049 Uiso 1 1 calc R . . . . C121 C 0.16766(18) 0.27662(17) 0.57249(10) 0.0414(5) Uani 1 1 d . . . . . H12C H 0.219004 0.322543 0.543508 0.050 Uiso 1 1 calc R . . . . H12D H 0.189809 0.200195 0.549873 0.050 Uiso 1 1 calc R . . . . C122 C 0.20015(19) 0.26357(17) 0.64665(10) 0.0427(5) Uani 1 1 d . . . . . H12E H 0.181391 0.340292 0.668442 0.051 Uiso 1 1 calc R . . . . H12F H 0.146132 0.220590 0.676237 0.051 Uiso 1 1 calc R . . . . C123 C 0.33589(19) 0.20265(18) 0.64756(10) 0.0437(5) Uani 1 1 d . . . . . H12G H 0.389709 0.248430 0.620746 0.052 Uiso 1 1 calc R . . . . H12H H 0.356277 0.128096 0.622807 0.052 Uiso 1 1 calc R . . . . C124 C 0.3663(2) 0.18254(18) 0.72198(10) 0.0479(5) Uani 1 1 d . . . . . H12I H 0.351584 0.257337 0.745525 0.057 Uiso 1 1 calc R . . . . H12J H 0.308408 0.141482 0.749889 0.057 Uiso 1 1 calc R . . . . C125 C 0.4983(3) 0.1152(2) 0.72292(12) 0.0648(7) Uani 1 1 d . . . . . H12K H 0.557105 0.162585 0.706153 0.078 Uiso 0.65 1 calc R . P A 1 H12L H 0.520702 0.047067 0.691627 0.078 Uiso 0.65 1 calc R . P A 1 H12M H 0.551470 0.148884 0.685812 0.078 Uiso 0.35 1 calc R . P B 2 H12N H 0.504515 0.037701 0.705677 0.078 Uiso 0.35 1 calc R . P B 2 C126 C 0.5043(4) 0.0791(4) 0.8010(2) 0.0513(11) Uani 0.65 1 d . . P C 1 H12O H 0.494236 0.147379 0.830388 0.062 Uiso 0.65 1 calc R . P C 1 H12P H 0.434860 0.044141 0.819865 0.062 Uiso 0.65 1 calc R . P C 1 C127 C 0.6277(5) -0.0056(4) 0.8058(2) 0.0747(12) Uani 0.65 1 d D . P C 1 H12Q H 0.697070 0.026922 0.783001 0.090 Uiso 0.65 1 calc R . P C 1 H12R H 0.634307 -0.076380 0.779662 0.090 Uiso 0.65 1 calc R . P C 1 C128 C 0.6400(6) -0.0345(8) 0.8832(3) 0.087(2) Uani 0.65 1 d D . P C 1 H12S H 0.575458 -0.072436 0.904736 0.130 Uiso 0.65 1 calc GR . P C 1 H12T H 0.629661 0.035826 0.909709 0.130 Uiso 0.65 1 calc GR . P C 1 H12U H 0.722661 -0.085510 0.884554 0.130 Uiso 0.65 1 calc GR . P C 1 C129 C 0.5665(9) 0.0970(8) 0.7903(5) 0.055(2) Uani 0.35 1 d . . P C 2 H12V H 0.658036 0.083240 0.775183 0.066 Uiso 0.35 1 calc R . P C 2 H12W H 0.535382 0.164547 0.822367 0.066 Uiso 0.35 1 calc R . P C 2 C130 C 0.5337(8) -0.0070(6) 0.8268(4) 0.0561(17) Uani 0.35 1 d D . P C 2 H13A H 0.574246 -0.074769 0.795762 0.067 Uiso 0.35 1 calc R . P C 2 H13B H 0.442280 0.003730 0.833539 0.067 Uiso 0.35 1 calc R . P C 2 C131 C 0.5747(10) -0.0294(13) 0.8995(5) 0.077(3) Uani 0.35 1 d D . P C 2 H13C H 0.666087 -0.049235 0.892713 0.115 Uiso 0.35 1 calc GR . P C 2 H13D H 0.544151 -0.092620 0.922687 0.115 Uiso 0.35 1 calc GR . P C 2 H13E H 0.539994 0.039402 0.929388 0.115 Uiso 0.35 1 calc GR . P C 2 O200 O 0.8876(4) 0.3327(4) 0.1098(3) 0.0759(14) Uani 0.5 1 d . . P D 1 H20C H 0.863550 0.347049 0.070174 0.114 Uiso 0.5 1 d G . P D 1 H20D H 0.838823 0.378949 0.141273 0.114 Uiso 0.5 1 d G . P D 1 O201 O 0.9248(7) 0.3746(6) 0.0650(4) 0.132(2) Uani 0.5 1 d . . P E 2 H20E H 0.968586 0.422616 0.060808 0.198 Uiso 0.5 1 d G . P E 2 H20F H 0.866391 0.396738 0.041345 0.198 Uiso 0.5 1 d G . P E 2 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 O1 0.0419(8) 0.0442(8) 0.0368(7) 0.0073(6) -0.0086(6) -0.0126(6) O2 0.0407(8) 0.0408(8) 0.0419(8) 0.0095(6) -0.0129(6) -0.0117(6) N1 0.0598(12) 0.0532(12) 0.0398(10) 0.0014(9) 0.0010(9) -0.0146(9) N2 0.0373(10) 0.0489(11) 0.0297(9) 0.0054(8) -0.0067(7) -0.0068(8) C1 0.0731(17) 0.0594(16) 0.0488(14) 0.0028(12) 0.0061(12) -0.0217(13) C2 0.093(2) 0.0552(16) 0.0527(15) 0.0031(13) 0.0168(15) -0.0187(15) C3 0.088(2) 0.0551(16) 0.0403(13) 0.0111(12) 0.0120(13) 0.0050(14) C4 0.0659(16) 0.0560(15) 0.0293(11) 0.0065(10) 0.0057(11) 0.0025(12) C5 0.0725(18) 0.0713(18) 0.0374(13) 0.0088(12) -0.0119(12) 0.0127(14) C6 0.0620(16) 0.0771(19) 0.0475(14) -0.0004(13) -0.0206(12) 0.0048(14) C7 0.0544(14) 0.0598(15) 0.0426(12) 0.0008(11) -0.0149(11) -0.0039(11) C8 0.0459(13) 0.0516(13) 0.0294(10) 0.0021(9) -0.0041(9) -0.0033(10) C9 0.0544(14) 0.0524(14) 0.0272(10) 0.0030(9) 0.0006(10) -0.0030(11) C10 0.0359(11) 0.0488(13) 0.0346(11) 0.0004(9) -0.0041(9) -0.0115(9) C11 0.0327(11) 0.0449(12) 0.0290(10) 0.0043(9) -0.0029(8) -0.0102(9) C12 0.0329(11) 0.0426(12) 0.0260(9) 0.0012(8) 0.0011(8) -0.0089(9) C13 0.0341(11) 0.0436(12) 0.0285(10) 0.0032(8) -0.0043(8) -0.0114(9) C14 0.0326(11) 0.0433(12) 0.0291(10) 0.0056(9) -0.0017(8) -0.0094(9) C15 0.0432(12) 0.0420(12) 0.0421(11) 0.0057(9) -0.0084(10) -0.0152(9) C16 0.0366(12) 0.0504(13) 0.0392(11) 0.0024(10) -0.0070(9) -0.0171(9) C17 0.0383(11) 0.0409(11) 0.0337(10) 0.0042(9) -0.0081(9) -0.0116(9) C18 0.0415(12) 0.0375(11) 0.0342(10) 0.0031(9) -0.0069(9) -0.0096(9) C19 0.0442(12) 0.0357(11) 0.0328(10) 0.0054(8) -0.0077(9) -0.0113(9) C20 0.0431(12) 0.0326(10) 0.0326(10) 0.0043(8) -0.0068(9) -0.0099(9) C21 0.0471(12) 0.0349(11) 0.0315(10) 0.0046(8) -0.0101(9) -0.0130(9) C22 0.0465(12) 0.0348(11) 0.0334(10) 0.0043(8) -0.0105(9) -0.0134(9) C23 0.0500(12) 0.0350(11) 0.0310(10) 0.0058(8) -0.0116(9) -0.0149(9) C24 0.0525(13) 0.0381(11) 0.0358(11) 0.0068(9) -0.0154(10) -0.0158(9) C25 0.0520(13) 0.0361(11) 0.0306(10) 0.0059(8) -0.0109(9) -0.0151(9) C26 0.0501(12) 0.0378(11) 0.0321(10) 0.0055(8) -0.0121(9) -0.0154(9) C27 0.0471(12) 0.0383(11) 0.0319(10) 0.0052(8) -0.0092(9) -0.0148(9) C28 0.0546(14) 0.0504(13) 0.0384(11) 0.0077(10) -0.0120(10) -0.0151(10) O101 0.0464(9) 0.0614(10) 0.0345(8) -0.0042(7) 0.0023(6) -0.0140(7) O102 0.0413(8) 0.0590(9) 0.0331(7) -0.0059(7) -0.0030(6) -0.0213(7) N101 0.0535(13) 0.0972(16) 0.0436(11) -0.0151(11) 0.0070(9) -0.0136(11) N102 0.0437(11) 0.0499(11) 0.0383(10) 0.0010(8) -0.0026(8) -0.0143(9) C101 0.0622(18) 0.146(3) 0.0489(16) -0.0191(17) 0.0119(14) -0.0118(18) C102 0.076(2) 0.094(2) 0.0439(15) -0.0039(14) 0.0153(13) -0.0042(16) C103 0.0745(18) 0.0559(15) 0.0416(13) 0.0094(11) 0.0045(12) 0.0048(13) C104 0.0620(16) 0.0506(14) 0.0412(12) 0.0125(10) 0.0029(11) 0.0037(11) C105 0.069(2) 0.130(3) 0.0449(15) 0.0355(16) -0.0033(13) 0.0124(18) C106 0.0567(18) 0.178(3) 0.0477(16) 0.0450(19) 0.0013(13) 0.0151(19) C107 0.0534(16) 0.116(2) 0.0421(14) 0.0271(14) 0.0012(12) -0.0057(15) C108 0.0500(14) 0.0500(13) 0.0387(12) 0.0091(10) 0.0000(10) -0.0108(10) C109 0.0554(15) 0.0417(12) 0.0419(12) 0.0027(10) 0.0028(10) -0.0080(10) C110 0.0417(12) 0.0455(12) 0.0422(12) -0.0051(10) 0.0018(10) -0.0192(9) C111 0.0404(12) 0.0436(12) 0.0366(11) -0.0053(9) -0.0026(9) -0.0197(9) C112 0.0443(12) 0.0426(12) 0.0364(11) -0.0069(9) 0.0016(9) -0.0209(9) C113 0.0395(12) 0.0452(12) 0.0373(11) -0.0051(9) -0.0009(9) -0.0187(9) C114 0.0420(12) 0.0423(11) 0.0379(11) -0.0044(9) -0.0052(9) -0.0230(9) C115 0.0436(13) 0.0534(13) 0.0341(11) -0.0096(9) 0.0005(9) -0.0234(10) C116 0.0385(12) 0.0492(13) 0.0419(12) -0.0094(10) 0.0012(9) -0.0209(9) C117 0.0418(12) 0.0447(12) 0.0366(11) -0.0045(9) -0.0003(9) -0.0199(9) C118 0.0489(13) 0.0434(12) 0.0370(11) -0.0038(9) -0.0022(9) -0.0236(10) C119 0.0476(13) 0.0409(11) 0.0348(11) -0.0026(9) 0.0000(9) -0.0213(9) C120 0.0472(13) 0.0450(12) 0.0342(11) -0.0051(9) -0.0009(9) -0.0231(10) C121 0.0482(13) 0.0443(12) 0.0333(11) -0.0021(9) 0.0007(9) -0.0203(10) C122 0.0516(13) 0.0465(12) 0.0347(11) -0.0024(9) -0.0002(9) -0.0258(10) C123 0.0537(14) 0.0453(12) 0.0363(11) 0.0002(9) -0.0020(10) -0.0245(10) C124 0.0705(16) 0.0455(12) 0.0341(11) 0.0011(9) -0.0056(10) -0.0293(11) C125 0.092(2) 0.0522(14) 0.0493(14) -0.0013(11) -0.0291(14) -0.0055(13) C126 0.060(3) 0.050(3) 0.050(2) 0.001(2) -0.018(2) -0.019(2) C127 0.064(3) 0.087(4) 0.074(3) 0.017(2) -0.026(3) -0.015(3) C128 0.088(5) 0.101(4) 0.081(4) 0.041(3) -0.038(4) -0.032(5) C129 0.051(6) 0.062(5) 0.061(5) 0.017(4) -0.025(5) -0.026(5) C130 0.055(5) 0.047(4) 0.067(5) 0.007(4) -0.019(4) -0.009(4) C131 0.075(8) 0.094(8) 0.071(7) 0.031(6) -0.035(6) -0.028(8) O200 0.049(2) 0.084(3) 0.086(3) -0.045(3) -0.010(2) 0.004(2) O201 0.133(6) 0.127(5) 0.154(7) -0.018(5) -0.070(5) -0.032(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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 O2 C17 116.72(14) . . ? C1 N1 C9 117.7(2) . . ? C8 N2 H2 119.0(13) . . ? C10 N2 H2 113.6(13) . . ? C10 N2 C8 127.39(18) . . ? N1 C1 H1 117.8 . . ? N1 C1 C2 124.3(3) . . ? C2 C1 H1 117.8 . . ? C1 C2 H2A 120.8 . . ? C3 C2 C1 118.3(3) . . ? C3 C2 H2A 120.8 . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 120.4(2) . . ? C4 C3 H3 119.8 . . ? C3 C4 C9 116.7(2) . . ? C5 C4 C3 124.7(2) . . ? C5 C4 C9 118.6(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 C4 120.5(2) . . ? C6 C5 H5 119.8 . . ? C5 C6 H6 119.3 . . ? C5 C6 C7 121.4(2) . . ? C7 C6 H6 119.3 . . ? C6 C7 H7 120.2 . . ? C8 C7 C6 119.6(2) . . ? C8 C7 H7 120.2 . . ? N2 C8 C9 115.04(19) . . ? C7 C8 N2 124.8(2) . . ? C7 C8 C9 120.1(2) . . ? N1 C9 C4 122.5(2) . . ? N1 C9 C8 117.78(19) . . ? C4 C9 C8 119.7(2) . . ? N2 C10 H10 118.7 . . ? N2 C10 C11 122.58(18) . . ? C11 C10 H10 118.7 . . ? C10 C11 C12 120.83(18) . . ? C10 C11 C16 120.24(18) . . ? C16 C11 C12 118.89(17) . . ? O1 C12 C11 121.73(17) . . ? O1 C12 C13 121.13(17) . . ? C13 C12 C11 117.13(17) . . ? C12 C13 H13 119.4 . . ? C14 C13 C12 121.27(18) . . ? C14 C13 H13 119.4 . . ? O2 C14 C15 114.24(17) . . ? C13 C14 O2 124.33(17) . . ? C13 C14 C15 121.42(18) . . ? C14 C15 H15 120.4 . . ? C16 C15 C14 119.11(19) . . ? C16 C15 H15 120.4 . . ? C11 C16 H16 118.9 . . ? C15 C16 C11 122.17(18) . . ? C15 C16 H16 118.9 . . ? O2 C17 H17A 110.0 . . ? O2 C17 H17B 110.0 . . ? O2 C17 C18 108.69(15) . . ? H17A C17 H17B 108.3 . . ? C18 C17 H17A 110.0 . . ? C18 C17 H17B 110.0 . . ? C17 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C17 C18 C19 111.26(16) . . ? H18A C18 H18B 108.0 . . ? C19 C18 H18A 109.4 . . ? C19 C18 H18B 109.4 . . ? C18 C19 H19A 108.8 . . ? C18 C19 H19B 108.8 . . ? C18 C19 C20 113.81(16) . . ? H19A C19 H19B 107.7 . . ? C20 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? C19 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? C21 C20 C19 113.40(16) . . ? C21 C20 H20A 108.9 . . ? C21 C20 H20B 108.9 . . ? C20 C21 H21A 108.7 . . ? C20 C21 H21B 108.7 . . ? C20 C21 C22 114.34(16) . . ? H21A C21 H21B 107.6 . . ? C22 C21 H21A 108.7 . . ? C22 C21 H21B 108.7 . . ? C21 C22 H22A 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C23 C22 C21 113.86(16) . . ? C23 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C22 C23 H23A 108.9 . . ? C22 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C24 C23 C22 113.45(16) . . ? C24 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? C23 C24 H24A 108.6 . . ? C23 C24 H24B 108.6 . . ? C23 C24 C25 114.62(16) . . ? H24A C24 H24B 107.6 . . ? C25 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? C24 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C24 C25 C26 113.72(16) . . ? H25A C25 H25B 107.7 . . ? C26 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C25 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C27 C26 C25 113.71(16) . . ? C27 C26 H26A 108.8 . . ? C27 C26 H26B 108.8 . . ? C26 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? C26 C27 C28 113.44(16) . . ? H27A C27 H27B 107.7 . . ? C28 C27 H27A 108.9 . . ? C28 C27 H27B 108.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C114 O102 C117 117.96(14) . . ? C101 N101 C109 116.4(2) . . ? C108 N102 H102 118.0(15) . . ? C110 N102 H102 115.4(15) . . ? C110 N102 C108 126.6(2) . . ? N101 C101 H101 117.6 . . ? N101 C101 C102 124.8(3) . . ? C102 C101 H101 117.6 . . ? C101 C102 H10A 120.5 . . ? C103 C102 C101 118.9(2) . . ? C103 C102 H10A 120.5 . . ? C102 C103 H103 120.4 . . ? C102 C103 C104 119.2(2) . . ? C104 C103 H103 120.4 . . ? C105 C104 C103 123.0(2) . . ? C105 C104 C109 118.9(2) . . ? C109 C104 C103 118.0(2) . . ? C104 C105 H105 120.0 . . ? C106 C105 C104 120.1(2) . . ? C106 C105 H105 120.0 . . ? C105 C106 H106 119.3 . . ? C105 C106 C107 121.4(3) . . ? C107 C106 H106 119.3 . . ? C106 C107 H107 120.1 . . ? C108 C107 C106 119.8(2) . . ? C108 C107 H107 120.1 . . ? N102 C108 C109 116.6(2) . . ? C107 C108 N102 123.4(2) . . ? C107 C108 C109 120.0(2) . . ? N101 C109 C104 122.6(2) . . ? N101 C109 C108 117.6(2) . . ? C104 C109 C108 119.8(2) . . ? N102 C110 H110 118.3 . . ? N102 C110 C111 123.5(2) . . ? C111 C110 H110 118.3 . . ? C110 C111 C112 121.53(18) . . ? C110 C111 C116 119.41(19) . . ? C116 C111 C112 119.05(18) . . ? O101 C112 C111 120.78(18) . . ? O101 C112 C113 121.80(19) . . ? C113 C112 C111 117.41(17) . . ? C112 C113 H113 119.5 . . ? C114 C113 C112 121.00(19) . . ? C114 C113 H113 119.5 . . ? O102 C114 C113 124.47(18) . . ? O102 C114 C115 114.00(17) . . ? C113 C114 C115 121.53(19) . . ? C114 C115 H115 120.5 . . ? C116 C115 C114 119.06(18) . . ? C116 C115 H115 120.5 . . ? C111 C116 H116 119.0 . . ? C115 C116 C111 121.9(2) . . ? C115 C116 H116 119.0 . . ? O102 C117 H11A 110.1 . . ? O102 C117 H11B 110.1 . . ? O102 C117 C118 107.80(15) . . ? H11A C117 H11B 108.5 . . ? C118 C117 H11A 110.1 . . ? C118 C117 H11B 110.1 . . ? C117 C118 H11C 109.0 . . ? C117 C118 H11D 109.0 . . ? C117 C118 C119 112.73(16) . . ? H11C C118 H11D 107.8 . . ? C119 C118 H11C 109.0 . . ? C119 C118 H11D 109.0 . . ? C118 C119 H11E 109.1 . . ? C118 C119 H11F 109.1 . . ? C118 C119 C120 112.52(16) . . ? H11E C119 H11F 107.8 . . ? C120 C119 H11E 109.1 . . ? C120 C119 H11F 109.1 . . ? C119 C120 H12A 108.6 . . ? C119 C120 H12B 108.6 . . ? H12A C120 H12B 107.6 . . ? C121 C120 C119 114.55(16) . . ? C121 C120 H12A 108.6 . . ? C121 C120 H12B 108.6 . . ? C120 C121 H12C 108.8 . . ? C120 C121 H12D 108.8 . . ? C120 C121 C122 113.66(16) . . ? H12C C121 H12D 107.7 . . ? C122 C121 H12C 108.8 . . ? C122 C121 H12D 108.8 . . ? C121 C122 H12E 108.8 . . ? C121 C122 H12F 108.8 . . ? H12E C122 H12F 107.7 . . ? C123 C122 C121 113.83(16) . . ? C123 C122 H12E 108.8 . . ? C123 C122 H12F 108.8 . . ? C122 C123 H12G 108.8 . . ? C122 C123 H12H 108.8 . . ? C122 C123 C124 113.80(17) . . ? H12G C123 H12H 107.7 . . ? C124 C123 H12G 108.8 . . ? C124 C123 H12H 108.8 . . ? C123 C124 H12I 108.8 . . ? C123 C124 H12J 108.8 . . ? H12I C124 H12J 107.7 . . ? C125 C124 C123 113.69(18) . . ? C125 C124 H12I 108.8 . . ? C125 C124 H12J 108.8 . . ? C124 C125 H12K 110.4 . . ? C124 C125 H12L 110.4 . . ? C124 C125 H12M 105.8 . . ? C124 C125 H12N 105.8 . . ? C124 C125 C126 106.7(2) . . ? C124 C125 C129 126.2(4) . . ? H12K C125 H12L 108.6 . . ? H12M C125 H12N 106.2 . . ? C126 C125 H12K 110.4 . . ? C126 C125 H12L 110.4 . . ? C129 C125 H12M 105.8 . . ? C129 C125 H12N 105.8 . . ? C125 C126 H12O 109.5 . . ? C125 C126 H12P 109.5 . . ? H12O C126 H12P 108.1 . . ? C127 C126 C125 110.8(4) . . ? C127 C126 H12O 109.5 . . ? C127 C126 H12P 109.5 . . ? C126 C127 H12Q 109.3 . . ? C126 C127 H12R 109.3 . . ? C126 C127 C128 111.6(5) . . ? H12Q C127 H12R 108.0 . . ? C128 C127 H12Q 109.3 . . ? C128 C127 H12R 109.3 . . ? C127 C128 H12S 109.5 . . ? C127 C128 H12T 109.5 . . ? C127 C128 H12U 109.5 . . ? H12S C128 H12T 109.5 . . ? H12S C128 H12U 109.5 . . ? H12T C128 H12U 109.5 . . ? C125 C129 H12V 110.8 . . ? C125 C129 H12W 110.8 . . ? H12V C129 H12W 108.9 . . ? C130 C129 C125 104.5(6) . . ? C130 C129 H12V 110.8 . . ? C130 C129 H12W 110.8 . . ? C129 C130 H13A 109.0 . . ? C129 C130 H13B 109.0 . . ? C129 C130 C131 113.0(7) . . ? H13A C130 H13B 107.8 . . ? C131 C130 H13A 109.0 . . ? C131 C130 H13B 109.0 . . ? C130 C131 H13C 109.5 . . ? C130 C131 H13D 109.5 . . ? C130 C131 H13E 109.5 . . ? H13C C131 H13D 109.5 . . ? H13C C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? H20C O200 H20D 109.5 . . ? H20E O201 H20F 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 O1 C12 1.278(2) . ? O2 C14 1.364(2) . ? O2 C17 1.439(2) . ? N1 C1 1.313(3) . ? N1 C9 1.372(3) . ? N2 H2 1.00(2) . ? N2 C8 1.410(2) . ? N2 C10 1.318(2) . ? C1 H1 0.9500 . ? C1 C2 1.407(3) . ? C2 H2A 0.9500 . ? C2 C3 1.360(4) . ? C3 H3 0.9500 . ? C3 C4 1.415(4) . ? C4 C5 1.413(3) . ? C4 C9 1.418(3) . ? C5 H5 0.9500 . ? C5 C6 1.358(4) . ? C6 H6 0.9500 . ? C6 C7 1.411(3) . ? C7 H7 0.9500 . ? C7 C8 1.371(3) . ? C8 C9 1.419(3) . ? C10 H10 0.9500 . ? C10 C11 1.394(3) . ? C11 C12 1.454(3) . ? C11 C16 1.422(3) . ? C12 C13 1.429(3) . ? C13 H13 0.9500 . ? C13 C14 1.363(3) . ? C14 C15 1.424(3) . ? C15 H15 0.9500 . ? C15 C16 1.353(3) . ? C16 H16 0.9500 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.510(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.522(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.527(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.519(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.521(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.521(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.521(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C25 1.522(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.528(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.520(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.525(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O101 C112 1.285(2) . ? O102 C114 1.362(2) . ? O102 C117 1.442(2) . ? N101 C101 1.318(3) . ? N101 C109 1.357(3) . ? N102 H102 0.93(2) . ? N102 C108 1.403(3) . ? N102 C110 1.324(2) . ? C101 H101 0.9500 . ? C101 C102 1.402(4) . ? C102 H10A 0.9500 . ? C102 C103 1.329(3) . ? C103 H103 0.9500 . ? C103 C104 1.416(3) . ? C104 C105 1.395(3) . ? C104 C109 1.400(3) . ? C105 H105 0.9500 . ? C105 C106 1.376(3) . ? C106 H106 0.9500 . ? C106 C107 1.394(3) . ? C107 H107 0.9500 . ? C107 C108 1.356(3) . ? C108 C109 1.427(3) . ? C110 H110 0.9500 . ? C110 C111 1.389(3) . ? C111 C112 1.450(3) . ? C111 C116 1.428(3) . ? C112 C113 1.422(3) . ? C113 H113 0.9500 . ? C113 C114 1.370(3) . ? C114 C115 1.425(3) . ? C115 H115 0.9500 . ? C115 C116 1.350(3) . ? C116 H116 0.9500 . ? C117 H11A 0.9900 . ? C117 H11B 0.9900 . ? C117 C118 1.509(3) . ? C118 H11C 0.9900 . ? C118 H11D 0.9900 . ? C118 C119 1.519(3) . ? C119 H11E 0.9900 . ? C119 H11F 0.9900 . ? C119 C120 1.527(3) . ? C120 H12A 0.9900 . ? C120 H12B 0.9900 . ? C120 C121 1.517(3) . ? C121 H12C 0.9900 . ? C121 H12D 0.9900 . ? C121 C122 1.526(3) . ? C122 H12E 0.9900 . ? C122 H12F 0.9900 . ? C122 C123 1.520(3) . ? C123 H12G 0.9900 . ? C123 H12H 0.9900 . ? C123 C124 1.525(3) . ? C124 H12I 0.9900 . ? C124 H12J 0.9900 . ? C124 C125 1.504(3) . ? C125 H12K 0.9900 . ? C125 H12L 0.9900 . ? C125 H12M 0.9900 . ? C125 H12N 0.9900 . ? C125 C126 1.553(5) . ? C125 C129 1.604(8) . ? C126 H12O 0.9900 . ? C126 H12P 0.9900 . ? C126 C127 1.516(6) . ? C127 H12Q 0.9900 . ? C127 H12R 0.9900 . ? C127 C128 1.535(6) . ? C128 H12S 0.9800 . ? C128 H12T 0.9800 . ? C128 H12U 0.9800 . ? C129 H12V 0.9900 . ? C129 H12W 0.9900 . ? C129 C130 1.517(11) . ? C130 H13A 0.9900 . ? C130 H13B 0.9900 . ? C130 C131 1.541(8) . ? C131 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? O200 H20C 0.8501 . ? O200 H20D 0.8503 . ? O201 H20E 0.8497 . ? O201 H20F 0.8501 . ? 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 N2 H2 O1 1.00(2) 1.76(2) 2.593(2) 138.4(19) . yes N102 H102 O101 0.93(2) 1.86(2) 2.610(2) 136(2) . yes O200 H20D O101 0.85 1.85 2.672(4) 162.4 1_655 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 O1 C12 C13 C14 177.58(17) . . . . ? O2 C14 C15 C16 179.18(17) . . . . ? O2 C17 C18 C19 179.25(15) . . . . ? N1 C1 C2 C3 0.1(4) . . . . ? N2 C8 C9 N1 0.0(3) . . . . ? N2 C8 C9 C4 179.87(17) . . . . ? N2 C10 C11 C12 -0.7(3) . . . . ? N2 C10 C11 C16 176.96(18) . . . . ? C1 N1 C9 C4 -0.1(3) . . . . ? C1 N1 C9 C8 179.70(19) . . . . ? C1 C2 C3 C4 -0.2(4) . . . . ? C2 C3 C4 C5 180.0(2) . . . . ? C2 C3 C4 C9 0.2(3) . . . . ? C3 C4 C5 C6 -179.6(2) . . . . ? C3 C4 C9 N1 0.0(3) . . . . ? C3 C4 C9 C8 -179.87(19) . . . . ? C4 C5 C6 C7 -0.3(4) . . . . ? C5 C4 C9 N1 -179.82(19) . . . . ? C5 C4 C9 C8 0.4(3) . . . . ? C5 C6 C7 C8 -0.1(4) . . . . ? C6 C7 C8 N2 179.93(19) . . . . ? C6 C7 C8 C9 0.5(3) . . . . ? C7 C8 C9 N1 179.48(19) . . . . ? C7 C8 C9 C4 -0.7(3) . . . . ? C8 N2 C10 C11 -177.71(18) . . . . ? C9 N1 C1 C2 0.1(3) . . . . ? C9 C4 C5 C6 0.1(3) . . . . ? C10 N2 C8 C7 -3.5(3) . . . . ? C10 N2 C8 C9 175.95(18) . . . . ? C10 C11 C12 O1 -0.3(3) . . . . ? C10 C11 C12 C13 178.75(16) . . . . ? C10 C11 C16 C15 -177.83(18) . . . . ? C11 C12 C13 C14 -1.5(3) . . . . ? C12 C11 C16 C15 -0.1(3) . . . . ? C12 C13 C14 O2 -178.09(16) . . . . ? C12 C13 C14 C15 1.0(3) . . . . ? C13 C14 C15 C16 0.0(3) . . . . ? C14 O2 C17 C18 177.78(15) . . . . ? C14 C15 C16 C11 -0.4(3) . . . . ? C16 C11 C12 O1 -177.98(17) . . . . ? C16 C11 C12 C13 1.1(3) . . . . ? C17 O2 C14 C13 0.7(3) . . . . ? C17 O2 C14 C15 -178.38(16) . . . . ? C17 C18 C19 C20 -179.71(16) . . . . ? C18 C19 C20 C21 -178.76(16) . . . . ? C19 C20 C21 C22 179.73(16) . . . . ? C20 C21 C22 C23 -178.38(16) . . . . ? C21 C22 C23 C24 -179.15(16) . . . . ? C22 C23 C24 C25 -177.67(16) . . . . ? C23 C24 C25 C26 178.36(16) . . . . ? C24 C25 C26 C27 178.23(16) . . . . ? C25 C26 C27 C28 -179.62(16) . . . . ? O101 C112 C113 C114 177.26(18) . . . . ? O102 C114 C115 C116 177.58(16) . . . . ? O102 C117 C118 C119 179.10(15) . . . . ? N101 C101 C102 C103 0.2(5) . . . . ? N102 C108 C109 N101 -1.8(3) . . . . ? N102 C108 C109 C104 178.55(19) . . . . ? N102 C110 C111 C112 -1.5(3) . . . . ? N102 C110 C111 C116 177.06(18) . . . . ? C101 N101 C109 C104 0.5(4) . . . . ? C101 N101 C109 C108 -179.1(2) . . . . ? C101 C102 C103 C104 0.5(4) . . . . ? C102 C103 C104 C105 178.8(3) . . . . ? C102 C103 C104 C109 -0.6(4) . . . . ? C103 C104 C105 C106 -178.2(3) . . . . ? C103 C104 C109 N101 0.2(3) . . . . ? C103 C104 C109 C108 179.8(2) . . . . ? C104 C105 C106 C107 -1.9(6) . . . . ? C105 C104 C109 N101 -179.3(2) . . . . ? C105 C104 C109 C108 0.3(4) . . . . ? C105 C106 C107 C108 1.1(5) . . . . ? C106 C107 C108 N102 -179.2(3) . . . . ? C106 C107 C108 C109 0.5(4) . . . . ? C107 C108 C109 N101 178.5(2) . . . . ? C107 C108 C109 C104 -1.1(3) . . . . ? C108 N102 C110 C111 179.40(19) . . . . ? C109 N101 C101 C102 -0.7(4) . . . . ? C109 C104 C105 C106 1.2(5) . . . . ? C110 N102 C108 C107 -7.8(4) . . . . ? C110 N102 C108 C109 172.54(19) . . . . ? C110 C111 C112 O101 0.0(3) . . . . ? C110 C111 C112 C113 178.88(17) . . . . ? C110 C111 C116 C115 -178.44(18) . . . . ? C111 C112 C113 C114 -1.6(3) . . . . ? C112 C111 C116 C115 0.1(3) . . . . ? C112 C113 C114 O102 -176.99(17) . . . . ? C112 C113 C114 C115 2.4(3) . . . . ? C113 C114 C115 C116 -1.8(3) . . . . ? C114 O102 C117 C118 173.24(15) . . . . ? C114 C115 C116 C111 0.6(3) . . . . ? C116 C111 C112 O101 -178.53(17) . . . . ? C116 C111 C112 C113 0.3(3) . . . . ? C117 O102 C114 C113 3.2(3) . . . . ? C117 O102 C114 C115 -176.22(15) . . . . ? C117 C118 C119 C120 178.42(15) . . . . ? C118 C119 C120 C121 178.80(16) . . . . ? C119 C120 C121 C122 -176.97(16) . . . . ? C120 C121 C122 C123 177.55(16) . . . . ? C121 C122 C123 C124 -176.12(16) . . . . ? C122 C123 C124 C125 176.03(18) . . . . ? C123 C124 C125 C126 -167.3(2) . . . . ? C123 C124 C125 C129 169.3(4) . . . . ? C124 C125 C126 C127 170.6(3) . . . . ? C124 C125 C129 C130 87.2(7) . . . . ? C125 C126 C127 C128 175.1(4) . . . . ? C125 C129 C130 C131 -171.7(7) . . . . ?