#------------------------------------------------------------------------------ #$Date: 2020-07-06 05:03:39 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253818 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/64/7126499.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_7126499 loop_ _publ_author_name 'Yelgaonkar, Shweta P.' 'Kiani, Daniyal' 'Baltrusaitis, Jonas' 'MacGillivray, Leonard R.' _publ_section_title ; Superstructural diversity in salt-cocrystals: higher-order hydrogen-bonded assemblies formed using U-shaped dications and with assistance of \p--\p stacking. ; _journal_issue 49 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 6708 _journal_page_last 6710 _journal_paper_doi 10.1039/d0cc02671a _journal_volume 56 _journal_year 2020 _chemical_formula_moiety '2(C20 H11 O8), C24 H20 N2' _chemical_formula_sum 'C64 H42 N2 O16' _chemical_formula_weight 1094.99 _chemical_name_systematic Isocoumarin-3-aqcid.DEPN _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 mixed _audit_creation_date 2019-03-22 _audit_creation_method ; Olex2 1.2 (compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337) ; _audit_update_record ; 2019-03-27 deposited with the CCDC. 2020-05-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.155(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4167(5) _cell_length_b 28.6453(15) _cell_length_c 20.8697(12) _cell_measurement_reflns_used 9623 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 148.7 _cell_measurement_theta_min 9.135 _cell_volume 4952.8(5) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_temperature 100.02 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 VENTURE ?-geometry diffractometer' _diffrn_measurement_method 'Area detector phi/chi scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_unetI/netI 0.0543 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 60014 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.241 _diffrn_reflns_theta_min 2.647 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0978 before and 0.0821 after correction. The Ratio of minimum to maximum transmission is 0.8619. The \l/2 correction factor is Not present.' _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.468 _exptl_crystal_description parallelepiped _exptl_crystal_F_000 2272 _exptl_crystal_recrystallization_method 'slow evaporation from nitromethane/methanol (v:v 4:1)' _exptl_crystal_size_max 0.129 _exptl_crystal_size_mid 0.071 _exptl_crystal_size_min 0.039 _exptl_transmission_factor_max 0.7427 _exptl_transmission_factor_min 0.6401 _refine_diff_density_max 0.370 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.075 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 752 _refine_ls_number_reflns 9044 _refine_ls_number_restraints 633 _refine_ls_restrained_S_all 1.003 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0589 _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^)+(0.1049P)^2^+1.6353P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1595 _refine_ls_wR_factor_ref 0.1752 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6833 _reflns_number_total 9044 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02671a2.cif _cod_data_source_block isodepn_0m _cod_depositor_comments 'Adding full bibliography for 7126497--7126499.cif.' _cod_database_code 7126499 _shelx_shelxl_version_number 2016/4 _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 0.966 _shelx_estimated_absorpt_t_min 0.894 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All N(H) groups, All O(H) groups 2. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C2(H2A), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24) ; _shelx_res_file ; TITL isodepn_0m in P2(1)/c isodepn_0m.res created by SHELXL-2016/4 at 12:34:58 on 22-Mar-2019 REM ##### CELL 1.54178 8.4167 28.6453 20.8697 90 100.1546 90 ZERR 4 0.0005 0.0015 0.0012 0 0.0047 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 256 168 8 64 RIGU L.S. 10 PLAN -20 SIZE 0.039 0.071 0.129 TEMP -173.13 LIST 6 BOND $H fmap 2 acta SHEL 99 0.83 OMIT 1 1 14 OMIT 0 1 10 OMIT -1 1 10 OMIT 0 1 18 OMIT 5 1 8 OMIT 5 1 14 REM REM REM WGHT 0.104900 1.635300 FVAR 0.11344 H2 2 0.750351 0.504871 0.519705 11.00000 0.12477 RESI COUM 1 O1 4 0.255177 0.304723 0.615405 11.00000 0.02520 0.04110 = 0.02347 0.00045 0.00465 -0.00125 O2 4 0.458601 0.300863 0.728654 11.00000 0.02774 0.03966 = 0.02529 -0.00204 0.00286 0.00008 O3 4 0.270528 0.331390 0.779881 11.00000 0.03172 0.04745 = 0.02415 -0.00408 0.00609 -0.00513 O4 4 0.223612 0.299495 0.508719 11.00000 0.03054 0.05639 = 0.02508 0.00068 0.00705 -0.00148 C1 1 0.191155 0.307874 0.671716 11.00000 0.02932 0.03030 = 0.02373 0.00113 0.00644 -0.00035 C2 1 0.158581 0.299543 0.555617 11.00000 0.02992 0.03494 = 0.02354 0.00014 0.00521 -0.00054 C3 1 -0.016322 0.295182 0.554475 11.00000 0.02709 0.02879 = 0.02769 0.00323 0.00303 0.00016 C4 1 -0.118643 0.286994 0.495330 11.00000 0.03441 0.03404 = 0.02613 0.00416 0.00351 -0.00035 AFIX 43 H4 2 -0.075548 0.283162 0.456540 11.00000 -1.20000 AFIX 0 C5 1 -0.283820 0.284499 0.493671 11.00000 0.03224 0.04242 = 0.02938 0.00423 -0.00238 -0.00208 AFIX 43 H5 2 -0.354230 0.278742 0.453616 11.00000 -1.20000 AFIX 0 C6 1 -0.347159 0.290425 0.550736 11.00000 0.02639 0.03626 = 0.03973 0.00599 0.00069 -0.00031 AFIX 43 H6 2 -0.460726 0.289635 0.548858 11.00000 -1.20000 AFIX 0 C7 1 -0.247389 0.297360 0.609353 11.00000 0.02817 0.03527 = 0.03037 0.00393 0.00627 0.00121 AFIX 43 H7 2 -0.291598 0.300875 0.647933 11.00000 -1.20000 AFIX 0 C8 1 -0.079347 0.299251 0.612165 11.00000 0.02852 0.02844 = 0.02701 0.00280 0.00393 0.00036 C9 1 0.032269 0.305495 0.672264 11.00000 0.02722 0.03215 = 0.02416 0.00045 0.00719 -0.00047 AFIX 43 H9 2 -0.006523 0.307925 0.712212 11.00000 -1.20000 AFIX 0 C10 1 0.316011 0.313912 0.732400 11.00000 0.02830 0.03100 = 0.02281 0.00152 0.00641 -0.00405 RESI COUM 2 O1 4 0.569170 0.431794 0.360359 11.00000 0.04259 0.03724 = 0.01823 -0.00037 0.00529 -0.00331 O2 4 0.677827 0.480608 0.464373 11.00000 0.05158 0.03986 = 0.02234 -0.00179 0.00482 -0.00699 O3 4 0.601835 0.426321 0.530431 11.00000 0.07078 0.04394 = 0.02074 -0.00086 0.00710 -0.01003 O4 4 0.552428 0.428004 0.254247 11.00000 0.05163 0.04141 = 0.02088 -0.00021 0.00765 -0.00630 C1 1 0.538992 0.413642 0.418327 11.00000 0.03843 0.03620 = 0.01929 0.00101 0.00541 0.00372 C2 1 0.515440 0.410181 0.301672 11.00000 0.03925 0.03391 = 0.02028 0.00017 0.00497 0.00438 C3 1 0.418822 0.367719 0.303018 11.00000 0.03495 0.03243 = 0.02196 -0.00083 0.00369 0.00544 C4 1 0.360842 0.344426 0.244908 11.00000 0.04608 0.03422 = 0.02009 0.00081 0.00434 0.00426 AFIX 43 H4 2 0.381668 0.356422 0.204763 11.00000 -1.20000 AFIX 0 C5 1 0.273425 0.304027 0.246086 11.00000 0.04940 0.03518 = 0.02661 -0.00514 0.00327 0.00167 AFIX 43 H5 2 0.233383 0.288220 0.206514 11.00000 -1.20000 AFIX 0 C6 1 0.242923 0.286014 0.304701 11.00000 0.04511 0.03414 = 0.03303 -0.00070 0.00784 -0.00129 AFIX 43 H6 2 0.182904 0.257935 0.304806 11.00000 -1.20000 AFIX 0 C7 1 0.299333 0.308687 0.362754 11.00000 0.04643 0.03350 = 0.02720 0.00101 0.00971 0.00107 AFIX 43 H7 2 0.277379 0.296400 0.402566 11.00000 -1.20000 AFIX 0 C8 1 0.389056 0.349884 0.362553 11.00000 0.03403 0.03259 = 0.02358 0.00048 0.00580 0.00435 C9 1 0.453625 0.374928 0.421305 11.00000 0.04311 0.03488 = 0.01919 0.00124 0.00803 0.00358 AFIX 43 H9 2 0.435116 0.363738 0.462205 11.00000 -1.20000 AFIX 0 C10 1 0.611724 0.442156 0.475959 11.00000 0.04495 0.03661 = 0.02141 0.00080 0.00507 0.00014 RESI COUM 3 O1 4 0.910458 0.565912 0.671062 11.00000 0.03982 0.03481 = 0.02108 -0.00194 0.00748 -0.00472 O2 4 0.797831 0.522382 0.563793 11.00000 0.04713 0.03750 = 0.02326 -0.00273 0.00599 -0.00716 O3 4 0.932958 0.567782 0.504316 11.00000 0.05491 0.04719 = 0.02314 -0.00290 0.01003 -0.01168 O4 4 0.918721 0.566611 0.777448 11.00000 0.05670 0.04304 = 0.02340 -0.00268 0.01341 -0.01367 C1 1 0.960186 0.582891 0.616113 11.00000 0.03494 0.03314 = 0.02294 0.00150 0.00650 0.00273 C2 1 0.962219 0.585465 0.731808 11.00000 0.03628 0.03444 = 0.02221 -0.00141 0.00764 -0.00139 C3 1 1.064208 0.626876 0.734824 11.00000 0.02978 0.03108 = 0.02263 0.00066 0.00473 0.00289 C4 1 1.110131 0.649203 0.794637 11.00000 0.03337 0.03433 = 0.02417 -0.00017 0.00480 0.00133 AFIX 43 H4 2 1.076161 0.637279 0.832500 11.00000 -1.20000 AFIX 0 C5 1 1.204961 0.688615 0.798472 11.00000 0.03583 0.03625 = 0.02817 -0.00403 0.00057 -0.00031 AFIX 43 H5 2 1.235723 0.704145 0.838982 11.00000 -1.20000 AFIX 0 C6 1 1.255831 0.705731 0.742927 11.00000 0.03378 0.03631 = 0.03496 0.00146 0.00226 -0.00460 AFIX 43 H6 2 1.322676 0.732652 0.746070 11.00000 -1.20000 AFIX 0 C7 1 1.210336 0.684064 0.683307 11.00000 0.03642 0.03919 = 0.02862 0.00496 0.00538 -0.00307 AFIX 43 H7 2 1.245605 0.696175 0.645818 11.00000 -1.20000 AFIX 0 C8 1 1.112149 0.644217 0.678182 11.00000 0.02872 0.03584 = 0.02393 0.00111 0.00355 0.00220 C9 1 1.057448 0.619986 0.617605 11.00000 0.03556 0.03607 = 0.02274 0.00170 0.00774 0.00180 AFIX 43 H9 2 1.090549 0.630393 0.578784 11.00000 -1.20000 AFIX 0 C10 1 0.892699 0.556062 0.555930 11.00000 0.03575 0.03556 = 0.02165 -0.00052 0.00448 0.00143 RESI COUM 4 O1 4 0.840726 0.323579 0.947049 11.00000 0.02418 0.04205 = 0.02083 -0.00247 0.00480 0.00032 O2 4 0.637035 0.307474 0.836745 11.00000 0.02567 0.04725 = 0.02371 -0.00014 0.00396 -0.00364 H2 2 0.558571 0.303977 0.784085 11.00000 -1.50000 O3 4 0.816812 0.333905 0.778011 11.00000 0.03078 0.05435 = 0.02257 0.00391 0.00561 -0.00031 O4 4 0.876608 0.326692 1.054193 11.00000 0.02947 0.05170 = 0.02261 -0.00311 0.00574 0.00123 C1 1 0.902325 0.322972 0.890238 11.00000 0.02905 0.03041 = 0.02203 0.00016 0.00562 -0.00124 C2 1 0.940158 0.323782 1.006705 11.00000 0.02993 0.03245 = 0.02390 -0.00098 0.00443 -0.00053 C3 1 1.114683 0.320011 1.007397 11.00000 0.02779 0.03032 = 0.02569 -0.00212 0.00317 -0.00074 C4 1 1.219807 0.317041 1.066847 11.00000 0.03269 0.03913 = 0.02542 -0.00197 0.00393 0.00251 AFIX 43 H4 2 1.178516 0.317507 1.106373 11.00000 -1.20000 AFIX 0 C5 1 1.383669 0.313428 1.068281 11.00000 0.02987 0.03798 = 0.03613 -0.00293 -0.00368 0.00216 AFIX 43 H5 2 1.455059 0.311042 1.108828 11.00000 -1.20000 AFIX 0 C6 1 1.445382 0.313262 1.010149 11.00000 0.02463 0.03495 = 0.04076 -0.00107 0.00219 0.00099 AFIX 43 H6 2 1.558612 0.311379 1.011496 11.00000 -1.20000 AFIX 0 C7 1 1.342431 0.315821 0.950937 11.00000 0.02760 0.03194 = 0.03402 -0.00062 0.00697 -0.00058 AFIX 43 H7 2 1.384687 0.315375 0.911629 11.00000 -1.20000 AFIX 0 C8 1 1.175290 0.319082 0.948905 11.00000 0.02599 0.02898 = 0.02878 0.00009 0.00468 -0.00082 C9 1 1.060873 0.321723 0.889052 11.00000 0.02970 0.03117 = 0.02458 0.00063 0.00718 -0.00048 AFIX 43 H9 2 1.097827 0.322583 0.848603 11.00000 -1.20000 AFIX 0 C10 1 0.777891 0.322324 0.829400 11.00000 0.02504 0.03483 = 0.02621 -0.00228 0.00707 0.00014 RESI DEPN 5 N1 3 0.899287 0.545797 0.378221 11.00000 0.04214 0.03778 = 0.02262 0.00247 0.00830 0.00474 H1 2 0.892409 0.545380 0.422447 11.00000 -1.50000 N2 3 0.400323 0.555466 0.345697 11.00000 0.03646 0.04247 = 0.02021 -0.00011 0.00629 0.00126 H2 2 0.404880 0.556649 0.391637 11.00000 -1.50000 C1 1 0.798733 0.553552 0.060543 11.00000 0.03029 0.03101 = 0.02452 -0.00049 0.00554 -0.00129 C2 1 0.936797 0.552353 0.033643 11.00000 0.02674 0.04093 = 0.02722 -0.00014 0.00286 0.00057 AFIX 43 H2A 2 1.038133 0.548193 0.061371 11.00000 -1.20000 AFIX 0 C3 1 0.931870 0.557134 -0.033979 11.00000 0.03265 0.03875 = 0.02710 -0.00130 0.01031 -0.00173 AFIX 43 H3 2 1.029072 0.556457 -0.051198 11.00000 -1.20000 AFIX 0 C4 1 0.787557 0.562719 -0.074502 11.00000 0.03762 0.03427 = 0.02129 -0.00071 0.00899 -0.00276 AFIX 43 H4 2 0.784436 0.565023 -0.120117 11.00000 -1.20000 AFIX 0 C5 1 0.642165 0.565128 -0.049401 11.00000 0.03322 0.02963 = 0.02064 -0.00066 0.00659 -0.00146 C6 1 0.492833 0.570748 -0.092161 11.00000 0.03491 0.04084 = 0.02020 0.00090 0.00515 -0.00347 AFIX 43 H6 2 0.490224 0.571619 -0.137839 11.00000 -1.20000 AFIX 0 C7 1 0.352663 0.574921 -0.068244 11.00000 0.03126 0.04562 = 0.02700 0.00463 0.00198 -0.00337 AFIX 43 H7 2 0.252703 0.577823 -0.097297 11.00000 -1.20000 AFIX 0 C8 1 0.356093 0.574931 -0.000618 11.00000 0.02900 0.04343 = 0.02484 0.00132 0.00522 -0.00319 AFIX 43 H8 2 0.258151 0.579083 0.015395 11.00000 -1.20000 AFIX 0 C9 1 0.497452 0.569089 0.042843 11.00000 0.03162 0.03098 = 0.02407 0.00062 0.00734 -0.00295 C10 1 0.646536 0.562287 0.019270 11.00000 0.02982 0.02975 = 0.01923 -0.00051 0.00510 -0.00251 C11 1 0.808709 0.543007 0.130231 11.00000 0.02826 0.03599 = 0.02376 0.00312 0.00579 0.00047 AFIX 43 H11 2 0.733362 0.521208 0.141670 11.00000 -1.20000 AFIX 0 C12 1 0.914532 0.561489 0.178504 11.00000 0.02899 0.03825 = 0.02403 0.00223 0.00770 -0.00045 AFIX 43 H12 2 0.996650 0.581091 0.167447 11.00000 -1.20000 AFIX 0 C13 1 0.912047 0.553406 0.247905 11.00000 0.02789 0.03540 = 0.02457 0.00075 0.00395 0.00446 C14 1 1.004156 0.582350 0.293948 11.00000 0.03477 0.03782 = 0.02822 -0.00143 0.00698 -0.00078 AFIX 43 H14 2 1.073309 0.605130 0.280404 11.00000 -1.20000 AFIX 0 C15 1 0.995219 0.578037 0.358385 11.00000 0.03785 0.03874 = 0.02638 -0.00270 0.00424 -0.00076 AFIX 43 H15 2 1.057515 0.598056 0.389377 11.00000 -1.20000 AFIX 0 C16 1 0.811490 0.516409 0.336185 11.00000 0.03534 0.03536 = 0.02798 0.00459 0.00689 0.00225 AFIX 43 H16 2 0.745832 0.493501 0.351618 11.00000 -1.20000 AFIX 0 C17 1 0.816142 0.519304 0.271046 11.00000 0.02975 0.03527 = 0.02690 0.00146 0.00522 0.00110 AFIX 43 H17 2 0.754457 0.498232 0.241443 11.00000 -1.20000 AFIX 0 C18 1 0.493188 0.574278 0.112788 11.00000 0.02427 0.03565 = 0.02453 -0.00219 0.00553 -0.00069 AFIX 43 H18 2 0.564352 0.596147 0.137161 11.00000 -1.20000 AFIX 0 C19 1 0.394146 0.549757 0.143833 11.00000 0.02777 0.03351 = 0.02026 -0.00191 0.00388 -0.00123 AFIX 43 H19 2 0.319516 0.529022 0.118921 11.00000 -1.20000 AFIX 0 C20 1 0.394229 0.553055 0.213921 11.00000 0.02619 0.03164 = 0.02463 0.00032 0.00736 0.00129 C21 1 0.466269 0.590176 0.251702 11.00000 0.03193 0.03601 = 0.02430 -0.00080 0.00831 -0.00209 AFIX 43 H21 2 0.515026 0.614958 0.231922 11.00000 -1.20000 AFIX 0 C22 1 0.466427 0.590750 0.317312 11.00000 0.03593 0.03559 = 0.02563 -0.00369 0.00538 -0.00225 AFIX 43 H22 2 0.513623 0.616284 0.342867 11.00000 -1.20000 AFIX 0 C23 1 0.328322 0.519447 0.311389 11.00000 0.03735 0.03549 = 0.02722 0.00285 0.01086 -0.00257 AFIX 43 H23 2 0.281548 0.495089 0.332753 11.00000 -1.20000 AFIX 0 C24 1 0.322193 0.517775 0.245001 11.00000 0.03094 0.03434 = 0.02639 -0.00082 0.00749 -0.00231 AFIX 43 H24 2 0.268959 0.492619 0.220399 11.00000 -1.20000 AFIX 0 HKLF 4 REM isodepn_0m in P2(1)/c REM R1 = 0.0589 for 6833 Fo > 4sig(Fo) and 0.0790 for all 9044 data REM 752 parameters refined using 633 restraints END WGHT 0.1050 1.6390 REM Highest difference peak 0.370, deepest hole -0.258, 1-sigma level 0.075 Q1 1 0.2998 0.3483 0.7373 11.00000 0.05 0.37 Q2 1 0.4623 0.2591 0.7324 11.00000 0.05 0.34 Q3 1 0.5821 0.4694 0.3567 11.00000 0.05 0.33 Q4 1 0.5587 0.3909 0.5234 11.00000 0.05 0.33 Q5 1 0.8251 0.3707 0.7763 11.00000 0.05 0.31 Q6 1 0.2522 0.3428 0.6223 11.00000 0.05 0.31 Q7 1 0.4429 0.3409 0.7262 11.00000 0.05 0.31 Q8 1 0.7599 0.2474 0.7607 11.00000 0.05 0.31 Q9 1 0.4863 0.3387 0.7374 11.00000 0.05 0.30 Q10 1 0.9113 0.5230 0.6740 11.00000 0.05 0.30 Q11 1 0.4518 0.4074 0.4176 11.00000 0.05 0.30 Q12 1 1.0534 0.5877 0.6196 11.00000 0.05 0.29 Q13 1 0.3611 0.3098 0.2438 11.00000 0.05 0.28 Q14 1 1.1205 0.6819 0.6800 11.00000 0.05 0.28 Q15 1 0.9606 0.6056 0.5031 11.00000 0.05 0.28 Q16 1 0.5027 0.3725 0.3009 11.00000 0.05 0.28 Q17 1 0.9099 0.5267 0.7802 11.00000 0.05 0.27 Q18 1 0.3906 0.5850 0.1368 11.00000 0.05 0.27 Q19 1 0.7662 0.2838 0.7615 11.00000 0.05 0.27 Q20 1 0.4663 0.5555 0.3266 11.00000 0.05 0.27 ; _shelx_res_checksum 76543 _shelx_hkl_file ; 1 0 0 53.4646 3.98295 3 2 0 0 33.5980 3.87960 10 2 0 0 36.1874 3.71827 3 3 0 0 32.4106 4.35728 3 3 0 0 39.2923 4.59588 10 4 0 0 14.2750 3.02251 10 -5 0 0 4.86503 0.67341 8 5 0 0 4.20072 2.19931 10 -6 0 0 20.5907 1.68322 9 6 0 0 20.7767 1.96681 4 -6 0 0 21.8198 1.78921 8 -6 0 0 17.4748 1.82936 11 6 0 0 18.3678 4.22746 10 -6 0 0 17.8650 1.69831 13 -7 0 0 111.071 7.44679 13 -7 0 0 110.269 7.54685 11 7 0 0 109.153 7.65987 4 -7 0 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35.0167 2.71406 11 -6 -10 0 33.6335 2.46681 9 -6 10 0 33.0869 2.36628 5 6 10 0 27.1600 2.71249 4 -7 -10 0 5.40320 0.81063 9 -7 -10 0 5.44333 0.90060 7 -7 -10 0 4.20840 0.84334 12 -7 -10 0 4.72188 0.78518 8 -7 -10 0 6.03977 1.16341 11 7 -10 0 5.08723 1.10981 4 7 -10 0 3.91695 0.94291 6 -7 -10 0 5.76315 0.88486 13 7 10 0 6.03900 1.12311 4 -7 10 0 4.59994 0.67939 5 -8 -10 0 -0.0789 0.46398 7 -8 -10 0 0.53788 0.50665 13 8 -10 0 -0.0033 0.65391 4 -8 -10 0 -0.8635 0.46037 9 -8 -10 0 -0.1879 0.64749 11 -8 -10 0 -0.1076 0.53479 12 8 -10 0 0.02659 0.66977 6 8 10 0 -0.7107 0.69180 4 -8 10 0 -0.6311 0.69827 11 -8 10 0 0.00692 0.32878 5 9 -10 0 4.65430 0.78147 4 -9 -10 0 4.50912 0.76569 11 -9 -10 0 3.57994 0.58091 9 -9 -10 0 2.50036 0.57334 12 9 10 0 2.96459 0.68200 4 0 -11 0 1.31934 1.42156 2 0 11 0 0.48922 1.14692 2 0 11 0 0.07399 1.24769 10 1 11 0 -0.4118 0.90825 2 -1 11 0 -0.6409 0.97354 2 -1 11 0 0.74153 1.33331 10 1 11 0 2.34763 1.73289 10 2 -11 0 36.1803 4.17034 10 2 -11 0 39.4399 4.05444 3 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0.56937 5 0 -12 24 -0.1731 0.24006 5 0 -12 -24 -0.2655 0.22921 9 0 -12 -24 -0.2433 0.24756 8 0 12 -24 -0.3731 0.25904 13 3 -13 -24 0.89492 0.28079 8 -3 -13 24 0.61415 0.24374 5 -2 -13 24 4.02904 0.46416 5 2 -13 -24 3.70821 0.45566 8 1 -13 -24 3.15921 0.47339 9 -1 -13 24 2.94279 0.37809 5 1 -13 -24 3.58623 0.43849 8 -2 -14 24 0.31053 0.23358 5 2 -14 -24 0.52004 0.25938 8 -4 0 25 0.25953 0.28015 5 4 0 -25 -0.2225 0.30562 9 -3 0 25 0.02154 0.19196 5 3 0 -25 0.10821 0.30344 9 2 0 -25 0.24794 0.32828 9 -2 0 25 0.25969 0.24767 5 -1 0 25 -0.0577 0.35298 5 1 0 -25 0.03197 0.32292 9 0 0 25 -0.1625 0.31240 5 0 0 -25 -0.0499 0.41202 9 -1 0 -25 0.53099 0.28201 9 4 -1 -25 4.97065 0.62854 9 -4 -1 25 4.02129 0.47313 5 -4 1 25 2.83832 0.52845 5 4 1 -25 2.06225 0.43863 9 -3 -1 25 -0.0826 0.15585 5 3 1 -25 -0.2180 0.25925 9 -3 1 25 -0.0119 0.17982 5 2 -1 -25 4.34370 0.54394 9 2 1 -25 4.12263 0.51647 9 -2 1 25 3.53067 0.50328 5 1 -1 -25 1.43178 0.38521 9 -1 1 25 0.72570 0.27189 5 1 1 -25 1.39823 0.37714 9 0 -1 -25 4.27686 0.55026 9 0 -1 25 3.38140 0.45802 5 0 1 -25 2.20542 0.49136 9 0 1 -25 2.29626 0.48884 13 0 1 25 2.98880 0.55250 5 -1 -1 -25 -0.0786 0.26774 9 -1 1 -25 0.28643 0.32892 13 -1 1 -25 0.12746 0.32257 9 4 -2 -25 1.54419 0.43420 9 -4 -2 25 1.51155 0.44642 5 4 2 -25 1.20845 0.45743 9 -4 2 25 1.14841 0.32251 5 -3 -2 25 0.10025 0.17105 5 3 -2 -25 0.38400 0.29822 9 3 2 -25 -0.2985 0.24158 9 2 -2 -25 0.56241 0.36464 9 -2 -2 25 0.26785 0.16765 5 -2 2 25 0.58556 0.32289 5 2 2 -25 0.14213 0.29553 9 1 -2 -25 0.43461 0.35090 9 -1 -2 25 0.22303 0.34720 5 1 2 -25 -0.0656 0.41060 13 1 2 -25 0.77896 0.33323 9 0 -2 25 0.28075 0.29920 5 0 -2 -25 0.26119 0.29761 9 0 2 -25 0.09977 0.26874 9 0 2 -25 -0.4432 0.28912 13 0 2 25 -0.4778 0.58697 5 -1 -2 -25 3.44570 0.42105 9 -1 2 -25 2.79329 0.47690 13 -4 -3 25 6.91226 0.68500 5 -4 3 25 5.45521 0.60024 5 3 -3 -25 1.14887 0.34352 9 -3 -3 25 0.41124 0.22794 5 -3 3 25 0.63838 0.26680 5 3 3 -25 0.40314 0.24902 9 2 -3 -25 1.56497 0.42101 9 -2 -3 25 1.01131 0.21392 5 2 3 -25 1.25924 0.30891 9 -2 3 25 0.66251 0.25935 5 -1 -3 25 0.39674 0.31954 5 1 -3 -25 0.04680 0.32300 9 -1 3 25 -0.0480 0.34858 5 1 3 -25 0.26315 0.32256 9 1 3 -25 -0.0722 0.31179 13 0 -3 25 -0.0883 0.27485 5 0 -3 -25 0.30567 0.29387 9 0 3 -25 0.02832 0.28274 13 0 3 -25 -0.2597 0.22738 9 -1 -3 -25 0.51005 0.28151 9 -1 3 -25 0.08469 0.30991 13 4 -4 -25 1.07636 0.30840 9 -4 -4 25 0.71590 0.28203 5 -4 4 25 1.00081 0.29254 5 4 4 -25 0.31292 0.21697 9 3 -4 -25 0.05025 0.29695 9 -3 -4 25 0.16075 0.21262 5 3 4 -25 0.31109 0.34936 9 -3 4 25 0.25340 0.20819 5 2 -4 -25 0.34355 0.33020 9 -2 -4 25 -0.0035 0.18597 5 -2 4 25 0.52814 0.23732 5 2 4 -25 0.29512 0.26757 9 -1 -4 25 1.54903 0.37627 5 1 -4 -25 1.97374 0.41654 9 1 -4 -25 2.00749 0.41172 8 1 4 -25 1.53202 0.35925 13 -1 4 25 1.75940 0.52273 5 0 -4 25 0.45349 0.29004 5 0 -4 -25 0.73732 0.35066 9 0 4 -25 -0.0632 0.20614 9 0 4 -25 0.21232 0.28035 13 -4 -5 25 0.03992 0.20417 5 4 -5 -25 0.15815 0.23875 9 4 5 -25 0.04022 0.17524 9 -4 5 25 0.03545 0.23616 5 -3 -5 25 1.60822 0.28526 5 3 -5 -25 2.30835 0.39270 9 -3 5 25 1.10944 0.24795 5 3 5 -25 0.77407 0.29075 9 -2 -5 25 0.00497 0.19760 5 2 -5 -25 0.19741 0.42254 8 2 -5 -25 0.32853 0.32104 9 2 5 -25 0.05059 0.31161 9 -2 5 25 -0.1195 0.21180 5 1 -5 -25 0.39206 0.35610 8 1 -5 -25 0.17230 0.34343 9 -1 -5 25 0.42391 0.30816 5 1 5 -25 0.46260 0.33626 13 1 5 -25 0.36725 0.25003 9 0 -5 25 1.91736 0.38154 5 0 -5 -25 2.07520 0.46942 9 0 5 -25 2.32385 0.36026 13 -4 -6 25 1.32399 0.27793 5 4 -6 -25 2.13623 0.32521 9 -4 6 25 1.15572 0.27151 5 4 6 -25 1.08860 0.22054 9 3 -6 -25 -0.3727 0.33324 9 -3 -6 25 0.20189 0.22981 5 -3 6 25 0.07677 0.20528 5 3 6 -25 0.09227 0.19411 9 -2 -6 25 4.61055 0.51176 5 2 -6 -25 4.29761 0.46613 8 2 -6 -25 5.94201 0.62309 9 2 6 -25 3.29615 0.41369 9 2 6 -25 3.59654 0.60817 13 -2 6 25 2.89076 0.40692 5 -1 -6 25 0.64258 0.31359 5 1 -6 -25 0.32183 0.30155 9 1 -6 -25 0.61733 0.31423 8 1 6 -25 0.59300 0.28470 9 1 6 -25 0.44215 0.32387 13 0 -6 -25 -0.2275 0.32225 9 0 -6 25 0.22254 0.27483 5 0 -6 -25 0.29439 0.25734 8 0 6 -25 0.02524 0.27330 13 -4 7 25 3.03797 0.42580 5 3 -7 -25 0.19769 0.27371 8 -3 -7 25 0.02582 0.30585 5 3 -7 -25 0.08429 0.25148 9 -3 7 25 0.85273 0.26968 5 3 7 -25 -0.0895 0.17890 9 2 -7 -25 -0.2185 0.26594 8 2 -7 -25 0.32614 0.38630 9 -2 -7 25 0.10922 0.26322 5 2 7 -25 0.18722 0.23198 9 2 7 -25 0.05759 0.41449 13 1 -7 -25 3.63260 0.46072 8 1 -7 -25 5.13687 0.61945 9 -1 -7 25 4.27506 0.64688 5 1 7 -25 4.22258 0.51259 13 0 -7 25 0.33808 0.26513 5 0 -7 -25 0.20191 0.28457 8 0 -7 -25 0.17056 0.28347 9 0 7 -25 0.13415 0.25879 13 3 -8 -25 0.91830 0.30081 8 3 -8 -25 0.79389 0.29370 9 -3 -8 25 0.62305 0.26064 5 3 8 -25 0.51817 0.37338 9 2 -8 -25 4.90029 0.55540 9 2 -8 -25 5.18517 0.55873 8 -2 -8 25 4.80109 0.60911 5 2 8 -25 4.36300 0.55973 13 -1 -8 25 2.08045 0.44562 5 1 -8 -25 2.44022 0.38774 8 1 -8 -25 2.38549 0.42016 9 1 8 -25 2.31450 0.40092 13 0 -8 25 -0.2926 0.23199 5 0 -8 -25 -0.0425 0.27313 8 0 -8 -25 0.58750 0.25956 9 0 8 -25 0.11819 0.25199 13 3 -9 -25 0.50612 0.25717 8 -3 -9 25 0.58402 0.23918 5 3 -9 -25 0.78262 0.27454 9 2 -9 -25 0.73879 0.26702 9 2 -9 -25 0.40941 0.27271 8 -2 -9 25 0.79749 0.30310 5 2 9 -25 0.32137 0.30203 13 1 -9 -25 -0.0295 0.24253 9 -1 -9 25 0.38200 0.23428 5 1 -9 -25 0.53997 0.28244 8 1 9 -25 0.25157 0.26078 13 2 -10 -25 5.24005 0.56843 8 -2 -10 25 5.29626 0.54233 5 2 -10 -25 6.39340 0.57709 9 2 10 -25 5.78028 0.66042 13 -1 -10 25 -0.0003 0.21440 5 1 10 -25 -0.2699 0.23411 13 -2 0 26 0.24703 0.26423 5 2 0 -26 -0.1044 0.26018 9 1 0 -26 1.32198 0.29764 9 -1 0 26 0.55626 0.48156 5 -2 -1 26 0.39806 0.27278 5 2 -1 -26 -0.1532 0.24539 9 -2 1 26 0.46445 0.41387 5 2 1 -26 0.12991 0.24952 9 1 -1 -26 2.98693 0.38555 9 -1 -1 26 3.15096 0.41990 5 1 1 -26 2.59149 0.36210 9 2 -2 -26 -0.1116 0.25154 9 -2 -2 26 0.21099 0.24244 5 2 2 -26 0.09093 0.24612 9 -2 2 26 -0.2085 0.25492 5 -2 -3 26 6.63618 0.63573 5 2 -3 -26 6.71836 0.65899 9 2 3 -26 7.24805 0.62995 9 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7427 _exptl_absorpt_correction_T_min 0.6401 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54177 8.421 28.681 20.887 90.022 100.085 89.982 ) ; _shelx_hkl_checksum 46288 _olex2_submission_special_instructions 'No special instructions were received' 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_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group H2 H 0.750(8) 0.505(2) 0.520(4) 0.12(2) Uiso 1 1 d . . . . . O1_1 O 0.2552(2) 0.30472(7) 0.61541(9) 0.0299(4) Uani 1 1 d . U . . . O2_1 O 0.4586(2) 0.30086(7) 0.72865(9) 0.0311(4) Uani 1 1 d . U . . . O3_1 O 0.2705(2) 0.33139(7) 0.77988(9) 0.0343(4) Uani 1 1 d . U . . . O4_1 O 0.2236(2) 0.29950(8) 0.50872(9) 0.0371(4) Uani 1 1 d . U . . . C1_1 C 0.1912(3) 0.30787(9) 0.67172(12) 0.0276(5) Uani 1 1 d . U . . . C2_1 C 0.1586(3) 0.29954(9) 0.55562(13) 0.0294(5) Uani 1 1 d . U . . . C3_1 C -0.0163(3) 0.29518(9) 0.55447(13) 0.0281(5) Uani 1 1 d . U . . . C4_1 C -0.1186(3) 0.28699(9) 0.49533(13) 0.0317(5) Uani 1 1 d . U . . . H4_1 H -0.075548 0.283162 0.456540 0.038 Uiso 1 1 calc R . . . . C5_1 C -0.2838(3) 0.28450(10) 0.49367(14) 0.0356(6) Uani 1 1 d . U . . . H5_1 H -0.354230 0.278742 0.453616 0.043 Uiso 1 1 calc R . . . . C6_1 C -0.3472(3) 0.29043(10) 0.55074(15) 0.0348(6) Uani 1 1 d . U . . . H6_1 H -0.460726 0.289635 0.548858 0.042 Uiso 1 1 calc R . . . . C7_1 C -0.2474(3) 0.29736(9) 0.60935(13) 0.0311(5) Uani 1 1 d . U . . . H7_1 H -0.291598 0.300875 0.647933 0.037 Uiso 1 1 calc R . . . . C8_1 C -0.0793(3) 0.29925(9) 0.61216(13) 0.0281(5) Uani 1 1 d . U . . . C9_1 C 0.0323(3) 0.30550(9) 0.67226(12) 0.0275(5) Uani 1 1 d . U . . . H9_1 H -0.006523 0.307925 0.712212 0.033 Uiso 1 1 calc R . . . . C10_1 C 0.3160(3) 0.31391(9) 0.73240(12) 0.0271(5) Uani 1 1 d . U . . . O1_2 O 0.5692(2) 0.43179(7) 0.36036(9) 0.0327(4) Uani 1 1 d . U . . . O2_2 O 0.6778(3) 0.48061(7) 0.46437(9) 0.0381(4) Uani 1 1 d . U . . . O3_2 O 0.6018(3) 0.42632(8) 0.53043(9) 0.0453(5) Uani 1 1 d . U . . . O4_2 O 0.5524(3) 0.42800(7) 0.25425(9) 0.0378(4) Uani 1 1 d . U . . . C1_2 C 0.5390(3) 0.41364(10) 0.41833(12) 0.0313(5) Uani 1 1 d . U . . . C2_2 C 0.5154(3) 0.41018(9) 0.30167(12) 0.0312(5) Uani 1 1 d . U . . . C3_2 C 0.4188(3) 0.36772(9) 0.30302(12) 0.0299(5) Uani 1 1 d . U . . . C4_2 C 0.3608(4) 0.34443(10) 0.24491(13) 0.0336(6) Uani 1 1 d . U . . . H4_2 H 0.381668 0.356422 0.204763 0.040 Uiso 1 1 calc R . . . . C5_2 C 0.2734(4) 0.30403(10) 0.24609(14) 0.0375(6) Uani 1 1 d . U . . . H5_2 H 0.233383 0.288220 0.206514 0.045 Uiso 1 1 calc R . . . . C6_2 C 0.2429(4) 0.28601(10) 0.30470(14) 0.0373(6) Uani 1 1 d . U . . . H6_2 H 0.182904 0.257935 0.304806 0.045 Uiso 1 1 calc R . . . . C7_2 C 0.2993(4) 0.30869(10) 0.36275(14) 0.0353(6) Uani 1 1 d . U . . . H7_2 H 0.277379 0.296400 0.402566 0.042 Uiso 1 1 calc R . . . . C8_2 C 0.3891(3) 0.34988(9) 0.36255(13) 0.0300(5) Uani 1 1 d . U . . . C9_2 C 0.4536(3) 0.37493(9) 0.42131(12) 0.0321(6) Uani 1 1 d . U . . . H9_2 H 0.435116 0.363738 0.462205 0.039 Uiso 1 1 calc R . . . . C10_2 C 0.6117(4) 0.44216(10) 0.47596(13) 0.0344(6) Uani 1 1 d . U . . . O1_3 O 0.9105(2) 0.56591(6) 0.67106(9) 0.0316(4) Uani 1 1 d . U . . . O2_3 O 0.7978(2) 0.52238(7) 0.56379(9) 0.0360(4) Uani 1 1 d . U . . . O3_3 O 0.9330(3) 0.56778(7) 0.50432(9) 0.0414(5) Uani 1 1 d . U . . . O4_3 O 0.9187(3) 0.56661(7) 0.77745(9) 0.0403(5) Uani 1 1 d . U . . . C1_3 C 0.9602(3) 0.58289(9) 0.61611(12) 0.0302(5) Uani 1 1 d . U . . . C2_3 C 0.9622(3) 0.58547(9) 0.73181(12) 0.0307(5) Uani 1 1 d . U . . . C3_3 C 1.0642(3) 0.62688(9) 0.73482(12) 0.0278(5) Uani 1 1 d . U . . . C4_3 C 1.1101(3) 0.64920(9) 0.79464(13) 0.0307(5) Uani 1 1 d . U . . . H4_3 H 1.076161 0.637279 0.832500 0.037 Uiso 1 1 calc R . . . . C5_3 C 1.2050(3) 0.68862(10) 0.79847(13) 0.0340(6) Uani 1 1 d . U . . . H5_3 H 1.235723 0.704145 0.838982 0.041 Uiso 1 1 calc R . . . . C6_3 C 1.2558(3) 0.70573(10) 0.74293(14) 0.0355(6) Uani 1 1 d . U . . . H6_3 H 1.322676 0.732652 0.746070 0.043 Uiso 1 1 calc R . . . . C7_3 C 1.2103(3) 0.68406(10) 0.68331(14) 0.0348(6) Uani 1 1 d . U . . . H7_3 H 1.245605 0.696175 0.645818 0.042 Uiso 1 1 calc R . . . . C8_3 C 1.1121(3) 0.64422(9) 0.67818(12) 0.0296(5) Uani 1 1 d . U . . . C9_3 C 1.0574(3) 0.61999(10) 0.61761(12) 0.0311(5) Uani 1 1 d . U . . . H9_3 H 1.090549 0.630393 0.578784 0.037 Uiso 1 1 calc R . . . . C10_3 C 0.8927(3) 0.55606(9) 0.55593(12) 0.0311(5) Uani 1 1 d . U . . . O1_4 O 0.8407(2) 0.32358(7) 0.94705(8) 0.0289(4) Uani 1 1 d . U . . . O2_4 O 0.6370(2) 0.30747(7) 0.83675(9) 0.0323(4) Uani 1 1 d . U . . . H2_4 H 0.559(5) 0.3040(13) 0.784(2) 0.048 Uiso 1 1 d R . . . . O3_4 O 0.8168(2) 0.33391(7) 0.77801(9) 0.0358(4) Uani 1 1 d . U . . . O4_4 O 0.8766(2) 0.32669(7) 1.05419(9) 0.0345(4) Uani 1 1 d . U . . . C1_4 C 0.9023(3) 0.32297(9) 0.89024(12) 0.0270(5) Uani 1 1 d . U . . . C2_4 C 0.9402(3) 0.32378(9) 1.00670(12) 0.0288(5) Uani 1 1 d . U . . . C3_4 C 1.1147(3) 0.32001(9) 1.00740(12) 0.0281(5) Uani 1 1 d . U . . . C4_4 C 1.2198(3) 0.31704(10) 1.06685(13) 0.0326(6) Uani 1 1 d . U . . . H4_4 H 1.178516 0.317507 1.106373 0.039 Uiso 1 1 calc R . . . . C5_4 C 1.3837(3) 0.31343(10) 1.06828(15) 0.0358(6) Uani 1 1 d . U . . . H5_4 H 1.455059 0.311042 1.108828 0.043 Uiso 1 1 calc R . . . . C6_4 C 1.4454(3) 0.31326(10) 1.01015(14) 0.0339(6) Uani 1 1 d . U . . . H6_4 H 1.558612 0.311379 1.011496 0.041 Uiso 1 1 calc R . . . . C7_4 C 1.3424(3) 0.31582(9) 0.95094(14) 0.0310(5) Uani 1 1 d . U . . . H7_4 H 1.384687 0.315375 0.911629 0.037 Uiso 1 1 calc R . . . . C8_4 C 1.1753(3) 0.31908(9) 0.94890(13) 0.0279(5) Uani 1 1 d . U . . . C9_4 C 1.0609(3) 0.32172(9) 0.88905(12) 0.0282(5) Uani 1 1 d . U . . . H9_4 H 1.097827 0.322583 0.848603 0.034 Uiso 1 1 calc R . . . . C10_4 C 0.7779(3) 0.32232(9) 0.82940(12) 0.0284(5) Uani 1 1 d . U . . . N1_5 N 0.8993(3) 0.54580(8) 0.37822(11) 0.0339(5) Uani 1 1 d . U . . . H1_5 H 0.892(5) 0.5454(14) 0.422(2) 0.051 Uiso 1 1 d R . . . . N2_5 N 0.4003(3) 0.55547(8) 0.34570(11) 0.0329(5) Uani 1 1 d . U . . . H2_5 H 0.405(5) 0.5566(13) 0.392(2) 0.049 Uiso 1 1 d R . . . . C1_5 C 0.7987(3) 0.55355(9) 0.06054(12) 0.0285(5) Uani 1 1 d . U . . . C2_5 C 0.9368(3) 0.55235(10) 0.03364(13) 0.0319(5) Uani 1 1 d . U . . . H2A_5 H 1.038133 0.548193 0.061371 0.038 Uiso 1 1 calc R . . . . C3_5 C 0.9319(3) 0.55713(10) -0.03398(13) 0.0322(6) Uani 1 1 d . U . . . H3_5 H 1.029072 0.556457 -0.051198 0.039 Uiso 1 1 calc R . . . . C4_5 C 0.7876(3) 0.56272(9) -0.07450(12) 0.0306(5) Uani 1 1 d . U . . . H4_5 H 0.784436 0.565023 -0.120117 0.037 Uiso 1 1 calc R . . . . C5_5 C 0.6422(3) 0.56513(9) -0.04940(12) 0.0276(5) Uani 1 1 d . U . . . C6_5 C 0.4928(3) 0.57075(10) -0.09216(12) 0.0319(5) Uani 1 1 d . U . . . H6_5 H 0.490224 0.571619 -0.137839 0.038 Uiso 1 1 calc R . . . . C7_5 C 0.3527(3) 0.57492(10) -0.06824(13) 0.0350(6) Uani 1 1 d . U . . . H7_5 H 0.252703 0.577823 -0.097297 0.042 Uiso 1 1 calc R . . . . C8_5 C 0.3561(3) 0.57493(10) -0.00062(13) 0.0324(6) Uani 1 1 d . U . . . H8_5 H 0.258151 0.579083 0.015395 0.039 Uiso 1 1 calc R . . . . C9_5 C 0.4975(3) 0.56909(9) 0.04284(12) 0.0286(5) Uani 1 1 d . U . . . C10_5 C 0.6465(3) 0.56229(9) 0.01927(12) 0.0262(5) Uani 1 1 d . U . . . C11_5 C 0.8087(3) 0.54301(9) 0.13023(12) 0.0292(5) Uani 1 1 d . U . . . H11_5 H 0.733362 0.521208 0.141670 0.035 Uiso 1 1 calc R . . . . C12_5 C 0.9145(3) 0.56149(9) 0.17850(12) 0.0301(5) Uani 1 1 d . U . . . H12_5 H 0.996650 0.581091 0.167447 0.036 Uiso 1 1 calc R . . . . C13_5 C 0.9120(3) 0.55341(9) 0.24791(12) 0.0294(5) Uani 1 1 d . U . . . C14_5 C 1.0042(3) 0.58235(10) 0.29395(13) 0.0334(6) Uani 1 1 d . U . . . H14_5 H 1.073309 0.605130 0.280404 0.040 Uiso 1 1 calc R . . . . C15_5 C 0.9952(3) 0.57804(10) 0.35839(13) 0.0345(6) Uani 1 1 d . U . . . H15_5 H 1.057515 0.598056 0.389377 0.041 Uiso 1 1 calc R . . . . C16_5 C 0.8115(3) 0.51641(10) 0.33618(13) 0.0327(6) Uani 1 1 d . U . . . H16_5 H 0.745832 0.493501 0.351618 0.039 Uiso 1 1 calc R . . . . C17_5 C 0.8161(3) 0.51930(9) 0.27105(13) 0.0306(5) Uani 1 1 d . U . . . H17_5 H 0.754457 0.498232 0.241443 0.037 Uiso 1 1 calc R . . . . C18_5 C 0.4932(3) 0.57428(9) 0.11279(12) 0.0280(5) Uani 1 1 d . U . . . H18_5 H 0.564352 0.596147 0.137161 0.034 Uiso 1 1 calc R . . . . C19_5 C 0.3941(3) 0.54976(9) 0.14383(12) 0.0272(5) Uani 1 1 d . U . . . H19_5 H 0.319516 0.529022 0.118921 0.033 Uiso 1 1 calc R . . . . C20_5 C 0.3942(3) 0.55306(9) 0.21392(12) 0.0271(5) Uani 1 1 d . U . . . C21_5 C 0.4663(3) 0.59018(10) 0.25170(13) 0.0303(5) Uani 1 1 d . U . . . H21_5 H 0.515026 0.614958 0.231922 0.036 Uiso 1 1 calc R . . . . C22_5 C 0.4664(3) 0.59075(10) 0.31731(13) 0.0324(6) Uani 1 1 d . U . . . H22_5 H 0.513623 0.616284 0.342867 0.039 Uiso 1 1 calc R . . . . C23_5 C 0.3283(3) 0.51945(10) 0.31139(13) 0.0327(6) Uani 1 1 d . U . . . H23_5 H 0.281548 0.495089 0.332753 0.039 Uiso 1 1 calc R . . . . C24_5 C 0.3222(3) 0.51777(9) 0.24500(13) 0.0303(5) Uani 1 1 d . U . . . H24_5 H 0.268959 0.492619 0.220399 0.036 Uiso 1 1 calc R . . . . 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_1 0.0252(9) 0.0411(10) 0.0235(8) 0.0004(7) 0.0047(7) -0.0012(7) O2_1 0.0277(9) 0.0397(10) 0.0253(9) -0.0020(7) 0.0029(7) 0.0001(7) O3_1 0.0317(9) 0.0475(11) 0.0242(9) -0.0041(8) 0.0061(7) -0.0051(8) O4_1 0.0305(10) 0.0564(12) 0.0251(9) 0.0007(8) 0.0071(7) -0.0015(8) C1_1 0.0293(12) 0.0303(12) 0.0237(12) 0.0011(9) 0.0064(10) -0.0003(9) C2_1 0.0299(13) 0.0349(13) 0.0235(12) 0.0001(10) 0.0052(10) -0.0005(10) C3_1 0.0271(12) 0.0288(12) 0.0277(12) 0.0032(10) 0.0030(10) 0.0002(9) C4_1 0.0344(13) 0.0340(13) 0.0261(13) 0.0042(10) 0.0035(10) -0.0003(10) C5_1 0.0322(13) 0.0424(15) 0.0294(13) 0.0042(11) -0.0024(10) -0.0021(11) C6_1 0.0264(13) 0.0363(14) 0.0397(15) 0.0060(11) 0.0007(11) -0.0003(10) C7_1 0.0282(13) 0.0353(14) 0.0304(13) 0.0039(10) 0.0063(10) 0.0012(10) C8_1 0.0285(12) 0.0284(12) 0.0270(12) 0.0028(10) 0.0039(10) 0.0004(9) C9_1 0.0272(12) 0.0321(13) 0.0242(12) 0.0004(10) 0.0072(9) -0.0005(9) C10_1 0.0283(12) 0.0310(12) 0.0228(12) 0.0015(9) 0.0064(9) -0.0040(9) O1_2 0.0426(10) 0.0372(10) 0.0182(8) -0.0004(7) 0.0053(7) -0.0033(8) O2_2 0.0516(12) 0.0399(11) 0.0223(9) -0.0018(8) 0.0048(8) -0.0070(9) O3_2 0.0708(15) 0.0439(11) 0.0207(9) -0.0009(8) 0.0071(9) -0.0100(10) O4_2 0.0516(12) 0.0414(11) 0.0209(9) -0.0002(8) 0.0076(8) -0.0063(9) C1_2 0.0384(14) 0.0362(13) 0.0193(11) 0.0010(10) 0.0054(10) 0.0037(10) C2_2 0.0392(14) 0.0339(13) 0.0203(12) 0.0002(10) 0.0050(10) 0.0044(10) C3_2 0.0350(13) 0.0324(13) 0.0220(12) -0.0008(10) 0.0037(10) 0.0054(10) C4_2 0.0461(15) 0.0342(14) 0.0201(12) 0.0008(10) 0.0043(10) 0.0043(11) C5_2 0.0494(16) 0.0352(14) 0.0266(13) -0.0051(11) 0.0033(11) 0.0017(11) C6_2 0.0451(16) 0.0341(14) 0.0330(14) -0.0007(11) 0.0078(12) -0.0013(11) C7_2 0.0464(16) 0.0335(13) 0.0272(13) 0.0010(10) 0.0097(11) 0.0011(11) C8_2 0.0340(13) 0.0326(13) 0.0236(12) 0.0005(10) 0.0058(10) 0.0043(10) C9_2 0.0431(15) 0.0349(13) 0.0192(11) 0.0012(10) 0.0080(10) 0.0036(11) C10_2 0.0449(15) 0.0366(14) 0.0214(12) 0.0008(10) 0.0051(11) 0.0001(11) O1_3 0.0398(10) 0.0348(10) 0.0211(9) -0.0019(7) 0.0075(7) -0.0047(7) O2_3 0.0471(11) 0.0375(10) 0.0233(9) -0.0027(8) 0.0060(8) -0.0072(8) O3_3 0.0549(12) 0.0472(12) 0.0231(9) -0.0029(8) 0.0100(8) -0.0117(9) O4_3 0.0567(13) 0.0430(11) 0.0234(9) -0.0027(8) 0.0134(8) -0.0137(9) C1_3 0.0349(13) 0.0331(13) 0.0229(12) 0.0015(10) 0.0065(10) 0.0027(10) C2_3 0.0363(14) 0.0344(13) 0.0222(12) -0.0014(10) 0.0076(10) -0.0014(10) C3_3 0.0298(12) 0.0311(13) 0.0226(11) 0.0007(9) 0.0047(9) 0.0029(10) C4_3 0.0334(13) 0.0343(13) 0.0242(12) -0.0002(10) 0.0048(10) 0.0013(10) C5_3 0.0358(14) 0.0362(14) 0.0282(13) -0.0040(10) 0.0006(10) -0.0003(11) C6_3 0.0338(14) 0.0363(14) 0.0350(14) 0.0015(11) 0.0023(11) -0.0046(11) C7_3 0.0364(14) 0.0392(14) 0.0286(13) 0.0050(11) 0.0054(11) -0.0031(11) C8_3 0.0287(12) 0.0358(13) 0.0239(12) 0.0011(10) 0.0035(9) 0.0022(10) C9_3 0.0356(13) 0.0361(13) 0.0227(12) 0.0017(10) 0.0077(10) 0.0018(10) C10_3 0.0358(13) 0.0356(13) 0.0217(12) -0.0005(10) 0.0045(10) 0.0014(10) O1_4 0.0242(8) 0.0420(10) 0.0208(8) -0.0025(7) 0.0048(7) 0.0003(7) O2_4 0.0257(9) 0.0472(11) 0.0237(9) -0.0001(8) 0.0040(7) -0.0036(7) O3_4 0.0308(9) 0.0543(12) 0.0226(9) 0.0039(8) 0.0056(7) -0.0003(8) O4_4 0.0295(9) 0.0517(11) 0.0226(9) -0.0031(8) 0.0057(7) 0.0012(8) C1_4 0.0291(12) 0.0304(12) 0.0220(11) 0.0002(9) 0.0056(9) -0.0012(9) C2_4 0.0299(12) 0.0325(13) 0.0239(12) -0.0010(10) 0.0044(10) -0.0005(10) C3_4 0.0278(12) 0.0303(13) 0.0257(12) -0.0021(10) 0.0032(10) -0.0007(9) C4_4 0.0327(13) 0.0391(14) 0.0254(12) -0.0020(10) 0.0039(10) 0.0025(10) C5_4 0.0299(13) 0.0380(14) 0.0361(14) -0.0029(11) -0.0037(11) 0.0022(11) C6_4 0.0246(12) 0.0350(14) 0.0408(15) -0.0011(11) 0.0022(10) 0.0010(10) C7_4 0.0276(12) 0.0319(13) 0.0340(13) -0.0006(10) 0.0070(10) -0.0006(10) C8_4 0.0260(12) 0.0290(12) 0.0288(13) 0.0001(10) 0.0047(10) -0.0008(9) C9_4 0.0297(12) 0.0312(13) 0.0246(12) 0.0006(10) 0.0072(10) -0.0005(9) C10_4 0.0250(12) 0.0348(13) 0.0262(12) -0.0023(10) 0.0071(9) 0.0001(9) N1_5 0.0421(13) 0.0378(12) 0.0226(11) 0.0025(9) 0.0083(9) 0.0047(9) N2_5 0.0365(12) 0.0425(13) 0.0202(11) -0.0001(9) 0.0063(9) 0.0013(9) C1_5 0.0303(13) 0.0310(13) 0.0245(12) -0.0005(10) 0.0055(10) -0.0013(9) C2_5 0.0267(12) 0.0409(14) 0.0272(13) -0.0001(11) 0.0029(10) 0.0006(10) C3_5 0.0326(13) 0.0388(14) 0.0271(13) -0.0013(10) 0.0103(10) -0.0017(10) C4_5 0.0376(14) 0.0343(13) 0.0213(11) -0.0007(10) 0.0090(10) -0.0028(10) C5_5 0.0332(13) 0.0296(12) 0.0206(11) -0.0007(9) 0.0066(9) -0.0015(10) C6_5 0.0349(13) 0.0408(14) 0.0202(12) 0.0009(10) 0.0051(10) -0.0035(11) C7_5 0.0313(13) 0.0456(16) 0.0270(13) 0.0046(11) 0.0020(10) -0.0034(11) C8_5 0.0290(13) 0.0434(15) 0.0248(12) 0.0013(11) 0.0052(10) -0.0032(11) C9_5 0.0316(13) 0.0310(13) 0.0241(12) 0.0006(10) 0.0073(10) -0.0029(10) C10_5 0.0298(12) 0.0298(12) 0.0192(11) -0.0005(9) 0.0051(9) -0.0025(9) C11_5 0.0283(12) 0.0360(13) 0.0238(12) 0.0031(10) 0.0058(9) 0.0005(10) C12_5 0.0290(12) 0.0382(14) 0.0240(12) 0.0022(10) 0.0077(10) -0.0005(10) C13_5 0.0279(12) 0.0354(13) 0.0246(12) 0.0007(10) 0.0040(10) 0.0045(10) C14_5 0.0348(14) 0.0378(14) 0.0282(13) -0.0014(11) 0.0070(10) -0.0008(11) C15_5 0.0378(14) 0.0387(14) 0.0264(13) -0.0027(11) 0.0042(10) -0.0008(11) C16_5 0.0353(14) 0.0354(13) 0.0280(13) 0.0046(10) 0.0069(10) 0.0022(10) C17_5 0.0298(12) 0.0353(13) 0.0269(12) 0.0015(10) 0.0052(10) 0.0011(10) C18_5 0.0243(12) 0.0357(13) 0.0245(12) -0.0022(10) 0.0055(9) -0.0007(9) C19_5 0.0278(12) 0.0335(13) 0.0203(11) -0.0019(9) 0.0039(9) -0.0012(9) C20_5 0.0262(12) 0.0316(12) 0.0246(12) 0.0003(9) 0.0074(9) 0.0013(9) C21_5 0.0319(13) 0.0360(13) 0.0243(12) -0.0008(10) 0.0083(10) -0.0021(10) C22_5 0.0359(14) 0.0356(14) 0.0256(12) -0.0037(10) 0.0054(10) -0.0022(10) C23_5 0.0374(14) 0.0355(14) 0.0272(12) 0.0029(10) 0.0109(10) -0.0026(11) C24_5 0.0309(12) 0.0343(13) 0.0264(12) -0.0008(10) 0.0075(10) -0.0023(10) 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_ _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 C2_1 O1_1 C1_1 121.6(2) . . ? C10_1 O2_1 H2_4 113.1(17) . . ? O1_1 C1_1 C10_1 113.9(2) . . ? C9_1 C1_1 O1_1 122.9(2) . . ? C9_1 C1_1 C10_1 123.2(2) . . ? O1_1 C2_1 C3_1 117.0(2) . . ? O4_1 C2_1 O1_1 117.3(2) . . ? O4_1 C2_1 C3_1 125.7(2) . . ? C4_1 C3_1 C2_1 119.2(2) . . ? C4_1 C3_1 C8_1 120.4(2) . . ? C8_1 C3_1 C2_1 120.4(2) . . ? C3_1 C4_1 H4_1 120.3 . . ? C5_1 C4_1 C3_1 119.4(3) . . ? C5_1 C4_1 H4_1 120.3 . . ? C4_1 C5_1 H5_1 119.9 . . ? C4_1 C5_1 C6_1 120.2(3) . . ? C6_1 C5_1 H5_1 119.9 . . ? C5_1 C6_1 H6_1 119.6 . . ? C7_1 C6_1 C5_1 120.8(3) . . ? C7_1 C6_1 H6_1 119.6 . . ? C6_1 C7_1 H7_1 120.1 . . ? C6_1 C7_1 C8_1 119.8(3) . . ? C8_1 C7_1 H7_1 120.1 . . ? C3_1 C8_1 C7_1 119.4(2) . . ? C3_1 C8_1 C9_1 118.1(2) . . ? C7_1 C8_1 C9_1 122.6(2) . . ? C1_1 C9_1 C8_1 119.8(2) . . ? C1_1 C9_1 H9_1 120.1 . . ? C8_1 C9_1 H9_1 120.1 . . ? O2_1 C10_1 C1_1 116.1(2) . . ? O3_1 C10_1 O2_1 126.9(2) . . ? O3_1 C10_1 C1_1 117.0(2) . . ? C2_2 O1_2 C1_2 121.9(2) . . ? C10_2 O2_2 H2 115(3) . . ? O1_2 C1_2 C10_2 112.8(2) . . ? C9_2 C1_2 O1_2 122.7(2) . . ? C9_2 C1_2 C10_2 124.6(2) . . ? O1_2 C2_2 C3_2 116.9(2) . . ? O4_2 C2_2 O1_2 116.7(2) . . ? O4_2 C2_2 C3_2 126.4(2) . . ? C4_2 C3_2 C2_2 119.4(2) . . ? C4_2 C3_2 C8_2 120.3(3) . . ? C8_2 C3_2 C2_2 120.3(2) . . ? C3_2 C4_2 H4_2 120.2 . . ? C5_2 C4_2 C3_2 119.6(3) . . ? C5_2 C4_2 H4_2 120.2 . . ? C4_2 C5_2 H5_2 119.7 . . ? C4_2 C5_2 C6_2 120.7(3) . . ? C6_2 C5_2 H5_2 119.7 . . ? C5_2 C6_2 H6_2 119.7 . . ? C7_2 C6_2 C5_2 120.5(3) . . ? C7_2 C6_2 H6_2 119.7 . . ? C6_2 C7_2 H7_2 120.2 . . ? C6_2 C7_2 C8_2 119.7(3) . . ? C8_2 C7_2 H7_2 120.2 . . ? C3_2 C8_2 C9_2 118.1(2) . . ? C7_2 C8_2 C3_2 119.2(2) . . ? C7_2 C8_2 C9_2 122.6(2) . . ? C1_2 C9_2 C8_2 120.1(2) . . ? C1_2 C9_2 H9_2 120.0 . . ? C8_2 C9_2 H9_2 120.0 . . ? O2_2 C10_2 C1_2 116.7(2) . . ? O3_2 C10_2 O2_2 126.2(3) . . ? O3_2 C10_2 C1_2 117.0(3) . . ? C1_3 O1_3 C2_3 121.8(2) . . ? C10_3 O2_3 H2 113(4) . . ? O1_3 C1_3 C10_3 113.0(2) . . ? C9_3 C1_3 O1_3 122.4(2) . . ? C9_3 C1_3 C10_3 124.6(2) . . ? O1_3 C2_3 C3_3 117.1(2) . . ? O4_3 C2_3 O1_3 116.8(2) . . ? O4_3 C2_3 C3_3 126.0(2) . . ? C4_3 C3_3 C2_3 118.6(2) . . ? C4_3 C3_3 C8_3 121.0(2) . . ? C8_3 C3_3 C2_3 120.3(2) . . ? C3_3 C4_3 H4_3 120.2 . . ? C5_3 C4_3 C3_3 119.6(2) . . ? C5_3 C4_3 H4_3 120.2 . . ? C4_3 C5_3 H5_3 120.0 . . ? C4_3 C5_3 C6_3 120.0(3) . . ? C6_3 C5_3 H5_3 120.0 . . ? C5_3 C6_3 H6_3 119.5 . . ? C7_3 C6_3 C5_3 120.9(3) . . ? C7_3 C6_3 H6_3 119.5 . . ? C6_3 C7_3 H7_3 120.0 . . ? C6_3 C7_3 C8_3 120.0(3) . . ? C8_3 C7_3 H7_3 120.0 . . ? C3_3 C8_3 C9_3 118.2(2) . . ? C7_3 C8_3 C3_3 118.4(2) . . ? C7_3 C8_3 C9_3 123.4(2) . . ? C1_3 C9_3 C8_3 120.1(2) . . ? C1_3 C9_3 H9_3 120.0 . . ? C8_3 C9_3 H9_3 120.0 . . ? O2_3 C10_3 C1_3 115.6(2) . . ? O3_3 C10_3 O2_3 126.2(2) . . ? O3_3 C10_3 C1_3 118.2(2) . . ? C2_4 O1_4 C1_4 121.32(19) . . ? C10_4 O2_4 H2_4 106.9(19) . . ? O1_4 C1_4 C10_4 114.7(2) . . ? C9_4 C1_4 O1_4 123.0(2) . . ? C9_4 C1_4 C10_4 122.3(2) . . ? O1_4 C2_4 C3_4 117.2(2) . . ? O4_4 C2_4 O1_4 117.2(2) . . ? O4_4 C2_4 C3_4 125.6(2) . . ? C4_4 C3_4 C2_4 119.3(2) . . ? C4_4 C3_4 C8_4 120.1(2) . . ? C8_4 C3_4 C2_4 120.6(2) . . ? C3_4 C4_4 H4_4 120.0 . . ? C5_4 C4_4 C3_4 120.0(3) . . ? C5_4 C4_4 H4_4 120.0 . . ? C4_4 C5_4 H5_4 119.9 . . ? C4_4 C5_4 C6_4 120.2(3) . . ? C6_4 C5_4 H5_4 119.9 . . ? C5_4 C6_4 H6_4 119.8 . . ? C7_4 C6_4 C5_4 120.3(2) . . ? C7_4 C6_4 H6_4 119.8 . . ? C6_4 C7_4 H7_4 120.1 . . ? C6_4 C7_4 C8_4 119.9(3) . . ? C8_4 C7_4 H7_4 120.1 . . ? C3_4 C8_4 C9_4 117.6(2) . . ? C7_4 C8_4 C3_4 119.4(2) . . ? C7_4 C8_4 C9_4 123.0(2) . . ? C1_4 C9_4 C8_4 120.1(2) . . ? C1_4 C9_4 H9_4 119.9 . . ? C8_4 C9_4 H9_4 119.9 . . ? O2_4 C10_4 C1_4 115.0(2) . . ? O3_4 C10_4 O2_4 125.9(2) . . ? O3_4 C10_4 C1_4 119.1(2) . . ? C15_5 N1_5 H1_5 117(2) . . ? C15_5 N1_5 C16_5 121.6(2) . . ? C16_5 N1_5 H1_5 121(2) . . ? C22_5 N2_5 H2_5 118(2) . . ? C23_5 N2_5 H2_5 120(2) . . ? C23_5 N2_5 C22_5 121.9(2) . . ? C2_5 C1_5 C10_5 119.2(2) . . ? C2_5 C1_5 C11_5 119.5(2) . . ? C10_5 C1_5 C11_5 121.2(2) . . ? C1_5 C2_5 H2A_5 119.1 . . ? C1_5 C2_5 C3_5 121.8(2) . . ? C3_5 C2_5 H2A_5 119.1 . . ? C2_5 C3_5 H3_5 120.1 . . ? C4_5 C3_5 C2_5 119.9(2) . . ? C4_5 C3_5 H3_5 120.1 . . ? C3_5 C4_5 H4_5 119.6 . . ? C3_5 C4_5 C5_5 120.7(2) . . ? C5_5 C4_5 H4_5 119.6 . . ? C4_5 C5_5 C6_5 120.1(2) . . ? C4_5 C5_5 C10_5 119.8(2) . . ? C6_5 C5_5 C10_5 120.1(2) . . ? C5_5 C6_5 H6_5 119.7 . . ? C7_5 C6_5 C5_5 120.5(2) . . ? C7_5 C6_5 H6_5 119.7 . . ? C6_5 C7_5 H7_5 120.0 . . ? C6_5 C7_5 C8_5 120.1(3) . . ? C8_5 C7_5 H7_5 120.0 . . ? C7_5 C8_5 H8_5 119.2 . . ? C9_5 C8_5 C7_5 121.7(3) . . ? C9_5 C8_5 H8_5 119.2 . . ? C8_5 C9_5 C10_5 119.8(2) . . ? C8_5 C9_5 C18_5 118.2(2) . . ? C10_5 C9_5 C18_5 121.8(2) . . ? C1_5 C10_5 C9_5 124.0(2) . . ? C5_5 C10_5 C1_5 118.3(2) . . ? C5_5 C10_5 C9_5 117.7(2) . . ? C1_5 C11_5 H11_5 117.3 . . ? C12_5 C11_5 C1_5 125.4(2) . . ? C12_5 C11_5 H11_5 117.3 . . ? C11_5 C12_5 H12_5 118.0 . . ? C11_5 C12_5 C13_5 124.0(2) . . ? C13_5 C12_5 H12_5 118.0 . . ? C14_5 C13_5 C12_5 118.8(2) . . ? C14_5 C13_5 C17_5 117.3(2) . . ? C17_5 C13_5 C12_5 123.8(2) . . ? C13_5 C14_5 H14_5 119.9 . . ? C15_5 C14_5 C13_5 120.2(3) . . ? C15_5 C14_5 H14_5 119.9 . . ? N1_5 C15_5 C14_5 120.5(3) . . ? N1_5 C15_5 H15_5 119.7 . . ? C14_5 C15_5 H15_5 119.7 . . ? N1_5 C16_5 H16_5 119.9 . . ? N1_5 C16_5 C17_5 120.2(3) . . ? C17_5 C16_5 H16_5 119.9 . . ? C13_5 C17_5 H17_5 119.9 . . ? C16_5 C17_5 C13_5 120.1(3) . . ? C16_5 C17_5 H17_5 119.9 . . ? C9_5 C18_5 H18_5 118.3 . . ? C19_5 C18_5 C9_5 123.5(2) . . ? C19_5 C18_5 H18_5 118.3 . . ? C18_5 C19_5 H19_5 118.1 . . ? C18_5 C19_5 C20_5 123.9(2) . . ? C20_5 C19_5 H19_5 118.1 . . ? C21_5 C20_5 C19_5 122.4(2) . . ? C24_5 C20_5 C19_5 119.6(2) . . ? C24_5 C20_5 C21_5 118.0(2) . . ? C20_5 C21_5 H21_5 120.1 . . ? C22_5 C21_5 C20_5 119.8(2) . . ? C22_5 C21_5 H21_5 120.1 . . ? N2_5 C22_5 C21_5 120.4(2) . . ? N2_5 C22_5 H22_5 119.8 . . ? C21_5 C22_5 H22_5 119.8 . . ? N2_5 C23_5 H23_5 120.1 . . ? N2_5 C23_5 C24_5 119.9(2) . . ? C24_5 C23_5 H23_5 120.1 . . ? C20_5 C24_5 H24_5 120.0 . . ? C23_5 C24_5 C20_5 120.0(2) . . ? C23_5 C24_5 H24_5 120.0 . . ? 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_1 C1_1 1.379(3) . ? O1_1 C2_1 1.372(3) . ? O2_1 C10_1 1.272(3) . ? O2_1 H2_4 1.31(4) . ? O3_1 C10_1 1.230(3) . ? O4_1 C2_1 1.203(3) . ? C1_1 C9_1 1.341(4) . ? C1_1 C10_1 1.506(4) . ? C2_1 C3_1 1.473(4) . ? C3_1 C4_1 1.395(4) . ? C3_1 C8_1 1.403(4) . ? C4_1 H4_1 0.9500 . ? C4_1 C5_1 1.386(4) . ? C5_1 H5_1 0.9500 . ? C5_1 C6_1 1.398(4) . ? C6_1 H6_1 0.9500 . ? C6_1 C7_1 1.371(4) . ? C7_1 H7_1 0.9500 . ? C7_1 C8_1 1.406(4) . ? C8_1 C9_1 1.440(4) . ? C9_1 H9_1 0.9500 . ? O1_2 C1_2 1.381(3) . ? O1_2 C2_2 1.376(3) . ? O2_2 H2 1.39(7) . ? O2_2 C10_2 1.276(4) . ? O3_2 C10_2 1.240(4) . ? O4_2 C2_2 1.202(3) . ? C1_2 C9_2 1.329(4) . ? C1_2 C10_2 1.493(4) . ? C2_2 C3_2 1.466(4) . ? C3_2 C4_2 1.395(4) . ? C3_2 C8_2 1.406(4) . ? C4_2 H4_2 0.9500 . ? C4_2 C5_2 1.374(4) . ? C5_2 H5_2 0.9500 . ? C5_2 C6_2 1.393(4) . ? C6_2 H6_2 0.9500 . ? C6_2 C7_2 1.383(4) . ? C7_2 H7_2 0.9500 . ? C7_2 C8_2 1.401(4) . ? C8_2 C9_2 1.442(4) . ? C9_2 H9_2 0.9500 . ? O1_3 C1_3 1.377(3) . ? O1_3 C2_3 1.384(3) . ? O2_3 H2 1.06(7) . ? O2_3 C10_3 1.281(4) . ? O3_3 C10_3 1.231(3) . ? O4_3 C2_3 1.207(3) . ? C1_3 C9_3 1.338(4) . ? C1_3 C10_3 1.496(4) . ? C2_3 C3_3 1.459(4) . ? C3_3 C4_3 1.395(4) . ? C3_3 C8_3 1.405(4) . ? C4_3 H4_3 0.9500 . ? C4_3 C5_3 1.377(4) . ? C5_3 H5_3 0.9500 . ? C5_3 C6_3 1.394(4) . ? C6_3 H6_3 0.9500 . ? C6_3 C7_3 1.383(4) . ? C7_3 H7_3 0.9500 . ? C7_3 C8_3 1.402(4) . ? C8_3 C9_3 1.445(4) . ? C9_3 H9_3 0.9500 . ? O1_4 C1_4 1.375(3) . ? O1_4 C2_4 1.372(3) . ? O2_4 H2_4 1.18(4) . ? O2_4 C10_4 1.294(3) . ? O3_4 C10_4 1.221(3) . ? O4_4 C2_4 1.209(3) . ? C1_4 C9_4 1.340(4) . ? C1_4 C10_4 1.497(4) . ? C2_4 C3_4 1.470(4) . ? C3_4 C4_4 1.394(4) . ? C3_4 C8_4 1.404(4) . ? C4_4 H4_4 0.9500 . ? C4_4 C5_4 1.378(4) . ? C5_4 H5_4 0.9500 . ? C5_4 C6_4 1.401(4) . ? C6_4 H6_4 0.9500 . ? C6_4 C7_4 1.380(4) . ? C7_4 H7_4 0.9500 . ? C7_4 C8_4 1.403(4) . ? C8_4 C9_4 1.438(4) . ? C9_4 H9_4 0.9500 . ? N1_5 H1_5 0.94(4) . ? N1_5 C15_5 1.339(4) . ? N1_5 C16_5 1.340(4) . ? N2_5 H2_5 0.95(4) . ? N2_5 C22_5 1.341(4) . ? N2_5 C23_5 1.338(4) . ? C1_5 C2_5 1.377(4) . ? C1_5 C10_5 1.434(4) . ? C1_5 C11_5 1.473(4) . ? C2_5 H2A_5 0.9500 . ? C2_5 C3_5 1.411(4) . ? C3_5 H3_5 0.9500 . ? C3_5 C4_5 1.362(4) . ? C4_5 H4_5 0.9500 . ? C4_5 C5_5 1.415(4) . ? C5_5 C6_5 1.417(4) . ? C5_5 C10_5 1.429(3) . ? C6_5 H6_5 0.9500 . ? C6_5 C7_5 1.365(4) . ? C7_5 H7_5 0.9500 . ? C7_5 C8_5 1.407(4) . ? C8_5 H8_5 0.9500 . ? C8_5 C9_5 1.373(4) . ? C9_5 C10_5 1.439(4) . ? C9_5 C18_5 1.474(4) . ? C11_5 H11_5 0.9500 . ? C11_5 C12_5 1.331(4) . ? C12_5 H12_5 0.9500 . ? C12_5 C13_5 1.471(4) . ? C13_5 C14_5 1.396(4) . ? C13_5 C17_5 1.406(4) . ? C14_5 H14_5 0.9500 . ? C14_5 C15_5 1.366(4) . ? C15_5 H15_5 0.9500 . ? C16_5 H16_5 0.9500 . ? C16_5 C17_5 1.369(4) . ? C17_5 H17_5 0.9500 . ? C18_5 H18_5 0.9500 . ? C18_5 C19_5 1.341(4) . ? C19_5 H19_5 0.9500 . ? C19_5 C20_5 1.466(3) . ? C20_5 C21_5 1.397(4) . ? C20_5 C24_5 1.396(4) . ? C21_5 H21_5 0.9500 . ? C21_5 C22_5 1.369(4) . ? C22_5 H22_5 0.9500 . ? C23_5 H23_5 0.9500 . ? C23_5 C24_5 1.378(4) . ? C24_5 H24_5 0.9500 . ?