#------------------------------------------------------------------------------ #$Date: 2024-11-04 03:32:52 +0200 (Mon, 04 Nov 2024) $ #$Revision: 295740 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/02/7160203.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_7160203 loop_ _publ_author_name 'Wani, Aabid' 'Bhujbal, Shivkanya Madhavrao' 'Sherpa, Deekey' 'Kathuria, Deepika' 'Chourasiya, Sumit S.' 'Sahoo, Subash Chandra' 'Bharatam, Prasad V.' _publ_section_title ; 1,1-Diaminoazine based Pd(II) NNN Pincer Complex: Generation, Characterization, and Application in Catalyzing the Acceptorless Dehydrogenative Coupling ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB01576B _journal_year 2024 _chemical_compound_source synthesized _chemical_formula_moiety '2(C29 H22 N2)' _chemical_formula_sum 'C58 H44 N4' _chemical_formula_weight 796.97 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2022-03-31 _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _audit_update_record ; 2022-05-05 deposited with the CCDC. 2024-11-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.5849(5) _cell_length_b 17.0570(7) _cell_length_c 26.1460(17) _cell_measurement_reflns_used 11610 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 23.1600 _cell_measurement_theta_min 3.5310 _cell_volume 4274.6(4) _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_unetI/netI 0.1062 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 22670 _diffrn_reflns_point_group_measured_fraction_full 0.929 _diffrn_reflns_point_group_measured_fraction_max 0.917 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.197 _diffrn_source 'sealed tube x-ray' _diffrn_source_type 'supernova Mo' _exptl_absorpt_coefficient_mu 0.072 _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.238 _exptl_crystal_description block _exptl_crystal_F_000 1680 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.173 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.037 _refine_ls_abs_structure_details ; Flack x determined using 1064 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.6(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 561 _refine_ls_number_reflns 8007 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.916 _refine_ls_R_factor_all 0.1614 _refine_ls_R_factor_gt 0.0631 _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^)+(0.0796P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1341 _refine_ls_wR_factor_ref 0.1779 _reflns_Friedel_coverage 0.655 _reflns_Friedel_fraction_full 0.844 _reflns_Friedel_fraction_max 0.822 _reflns_number_gt 3569 _reflns_number_total 8007 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01576b2.cif _cod_data_source_block PVB-MD-55 _cod_database_code 7160203 _shelx_shelxl_version_number 2017/1 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C19(H19A,H19B), C48(H48A,H48B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C21(H21), C10(H10), C28(H28), C52(H52), C50(H50), C9(H9), C51(H51), C16(H16), C6(H6), C38(H38), C22(H22), C33(H33), C4(H4), C25(H25), C23(H23), C14(H14), C8(H8), C31(H31), C32(H32), C15(H15), C57(H57), C45(H45), C43(H43), C5(H5), C27(H27), C56(H56), C26(H26), C37(H37), C36(H36), C35(H35), C44(H44), C54(H54), C55(H55) 2.c Idealised Me refined as rotating group: C47(H47A,H47B,H47C), C18(H18A,H18B,H18C) ; _shelx_res_file ; TITL scs-niper-55_a.res in P2(1)2(1)2(1) ov_scs-niper-55.res created by SHELXL-2017/1 at 17:42:16 on 31-Mar-2022 REM Old TITL SCS-NIPER-55 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.160, Rweak 0.031, Alpha 0.001, Orientation as input REM Flack x = -0.628 ( 4.000 ) from Parsons' quotients REM Formula found by SHELXT: C55 N4 CELL 0.71073 9.58492 17.057043 26.145998 90 90 90 ZERR 4 0.000543 0.000746 0.00166 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N UNIT 232 176 16 L.S. 18 PLAN 2 CONF BOND $H LIST 6 MORE -1 fmap 2 acta REM REM REM WGHT 0.079600 FVAR 0.20599 N2 3 -0.292912 -0.550554 -0.613652 11.00000 0.05731 0.05458 = 0.05341 -0.00096 0.00430 -0.00307 N3 3 -0.815495 -0.450035 -0.054121 11.00000 0.05277 0.06424 = 0.06639 0.00237 -0.00172 -0.00588 N4 3 -0.709753 -0.458154 -0.131018 11.00000 0.05749 0.06595 = 0.05974 0.00238 0.00455 -0.00601 N1 3 -0.188018 -0.569592 -0.689178 11.00000 0.05801 0.05438 = 0.06395 0.00033 0.00487 -0.00388 C20 1 -0.251698 -0.524608 -0.520653 11.00000 0.05376 0.05102 = 0.05311 0.00412 -0.00144 0.00061 C2 1 -0.224334 -0.387712 -0.693926 11.00000 0.04685 0.05360 = 0.05699 -0.00421 0.00439 0.00049 C40 1 -0.784682 -0.495817 -0.093530 11.00000 0.05305 0.06200 = 0.05761 0.00352 0.00126 -0.00337 C49 1 -0.748128 -0.469986 -0.224649 11.00000 0.04791 0.05748 = 0.05636 0.00713 -0.00070 -0.00495 C12 1 -0.250092 -0.638638 -0.673513 11.00000 0.05331 0.05217 = 0.06175 0.00442 -0.00273 -0.00317 C29 1 -0.293710 -0.488415 -0.473944 11.00000 0.05870 0.05027 = 0.05892 0.00271 -0.00070 -0.00374 C24 1 -0.213251 -0.498627 -0.429548 11.00000 0.06686 0.06088 = 0.05991 0.00099 -0.00745 -0.00457 C17 1 -0.316867 -0.627969 -0.626728 11.00000 0.05818 0.05408 = 0.06132 0.00878 -0.00961 -0.00051 C41 1 -0.754728 -0.377885 -0.066308 11.00000 0.05007 0.05482 = 0.06609 0.00286 -0.01059 -0.00002 C3 1 -0.308832 -0.414985 -0.734508 11.00000 0.06641 0.06369 = 0.06436 -0.00065 -0.00020 -0.00055 AFIX 43 H3 2 -0.335255 -0.467433 -0.735285 11.00000 -1.20000 AFIX 0 C39 1 -0.786226 -0.631761 -0.057345 11.00000 0.05084 0.05893 = 0.06406 -0.00465 0.00233 0.00341 C11 1 -0.216686 -0.519110 -0.652635 11.00000 0.05592 0.05231 = 0.05182 0.00706 -0.00043 -0.00331 C7 1 -0.183358 -0.306593 -0.694908 11.00000 0.06055 0.05029 = 0.07913 0.00017 0.01255 -0.00011 C1 1 -0.176822 -0.435231 -0.653123 11.00000 0.04617 0.05993 = 0.05526 -0.00141 -0.00128 -0.00131 C21 1 -0.132872 -0.568451 -0.521910 11.00000 0.06263 0.06522 = 0.06545 0.00376 0.00233 0.00877 AFIX 43 H21 2 -0.104445 -0.591307 -0.552476 11.00000 -1.20000 AFIX 0 C13 1 -0.253124 -0.711709 -0.697865 11.00000 0.06970 0.06332 = 0.07102 -0.00264 -0.00649 0.00219 C30 1 -0.825656 -0.578879 -0.096998 11.00000 0.04428 0.06286 = 0.06280 0.00084 0.00165 -0.00613 C46 1 -0.687954 -0.382958 -0.113528 11.00000 0.05458 0.05942 = 0.06709 0.00254 -0.01299 -0.00653 C19 1 -0.342131 -0.512595 -0.567311 11.00000 0.05398 0.06774 = 0.05384 0.00608 0.00459 0.00535 AFIX 23 H19A 2 -0.435064 -0.531907 -0.559764 11.00000 -1.20000 H19B 2 -0.349667 -0.456757 -0.573773 11.00000 -1.20000 AFIX 0 C10 1 -0.096960 -0.403025 -0.615705 11.00000 0.07356 0.06382 = 0.06065 0.00275 -0.00500 0.00045 AFIX 43 H10 2 -0.067324 -0.434506 -0.588772 11.00000 -1.20000 AFIX 0 C28 1 -0.414409 -0.440024 -0.470869 11.00000 0.05854 0.06891 = 0.07174 -0.01256 0.00004 0.00757 AFIX 43 H28 2 -0.470895 -0.433063 -0.499431 11.00000 -1.20000 AFIX 0 C48 1 -0.659034 -0.489942 -0.179129 11.00000 0.05429 0.06904 = 0.06536 0.00352 0.00563 0.00355 AFIX 23 H48A 2 -0.653364 -0.546537 -0.176153 11.00000 -1.20000 H48B 2 -0.565386 -0.470421 -0.185093 11.00000 -1.20000 AFIX 0 C58 1 -0.704969 -0.497836 -0.272964 11.00000 0.06816 0.05684 = 0.06623 0.00356 -0.00803 -0.01329 C52 1 -0.904312 -0.435946 -0.312378 11.00000 0.09096 0.08616 = 0.07866 0.01998 -0.01950 -0.02437 AFIX 43 H52 2 -0.956423 -0.423766 -0.341311 11.00000 -1.20000 AFIX 0 C50 1 -0.869270 -0.428374 -0.221510 11.00000 0.06015 0.06372 = 0.07624 0.00875 0.00220 -0.00421 AFIX 43 H50 2 -0.901298 -0.411435 -0.189805 11.00000 -1.20000 AFIX 0 C9 1 -0.057800 -0.323893 -0.616385 11.00000 0.06877 0.06705 = 0.08772 -0.01510 -0.00441 -0.00882 AFIX 43 H9 2 -0.001805 -0.303715 -0.590491 11.00000 -1.20000 AFIX 0 C34 1 -0.825615 -0.711064 -0.061347 11.00000 0.07187 0.05733 = 0.08324 0.01777 0.01042 0.00559 C51 1 -0.946619 -0.410779 -0.266164 11.00000 0.06507 0.08090 = 0.09275 0.01996 -0.02106 0.00550 AFIX 43 H51 2 -1.027979 -0.381351 -0.263509 11.00000 -1.20000 AFIX 0 C16 1 -0.392287 -0.687191 -0.602268 11.00000 0.07502 0.07569 = 0.06706 0.01384 0.00535 -0.01281 AFIX 43 H16 2 -0.437799 -0.679463 -0.571261 11.00000 -1.20000 AFIX 0 C6 1 -0.232743 -0.258757 -0.735008 11.00000 0.07112 0.06302 = 0.09376 0.01361 -0.00254 0.00078 AFIX 43 H6 2 -0.207760 -0.206086 -0.735800 11.00000 -1.20000 AFIX 0 C38 1 -0.709978 -0.608775 -0.014476 11.00000 0.07988 0.06980 = 0.07120 0.00052 0.00247 0.01115 AFIX 43 H38 2 -0.684445 -0.556460 -0.010901 11.00000 -1.20000 AFIX 0 C22 1 -0.053074 -0.579407 -0.477510 11.00000 0.06388 0.07810 = 0.08178 0.01133 -0.00394 0.01483 AFIX 43 H22 2 0.027398 -0.609788 -0.478951 11.00000 -1.20000 AFIX 0 C33 1 -0.901803 -0.736166 -0.105240 11.00000 0.07876 0.06017 = 0.10575 -0.00205 0.00620 -0.01258 AFIX 43 H33 2 -0.927767 -0.788484 -0.108347 11.00000 -1.20000 AFIX 0 C4 1 -0.352529 -0.366003 -0.772605 11.00000 0.08795 0.07700 = 0.06929 -0.00010 -0.01168 0.00563 AFIX 43 H4 2 -0.407658 -0.385393 -0.799001 11.00000 -1.20000 AFIX 0 C25 1 -0.251781 -0.461880 -0.383603 11.00000 0.07481 0.10745 = 0.06405 -0.01185 -0.00765 -0.00304 AFIX 43 H25 2 -0.199284 -0.469937 -0.354155 11.00000 -1.20000 AFIX 0 C23 1 -0.091496 -0.546425 -0.432657 11.00000 0.07446 0.06698 = 0.07617 0.00583 -0.01747 0.00370 AFIX 43 H23 2 -0.037961 -0.554999 -0.403524 11.00000 -1.20000 AFIX 0 C14 1 -0.325177 -0.769628 -0.673522 11.00000 0.07873 0.06305 = 0.10232 0.00413 -0.01827 -0.00578 AFIX 43 H14 2 -0.328104 -0.819102 -0.688432 11.00000 -1.20000 AFIX 0 C42 1 -0.757336 -0.308172 -0.038488 11.00000 0.06931 0.06272 = 0.08876 -0.00006 -0.02790 -0.00053 C53 1 -0.781133 -0.480781 -0.317184 11.00000 0.07629 0.06990 = 0.07301 0.00283 -0.01408 -0.01520 C8 1 -0.101690 -0.277016 -0.654798 11.00000 0.07294 0.05264 = 0.09336 -0.00344 -0.00632 -0.01658 AFIX 43 H8 2 -0.077339 -0.224238 -0.654643 11.00000 -1.20000 AFIX 0 C31 1 -0.899294 -0.605547 -0.138111 11.00000 0.07517 0.05844 = 0.08129 0.00001 0.00550 -0.00593 AFIX 43 H31 2 -0.925111 -0.570615 -0.163729 11.00000 -1.20000 AFIX 0 C32 1 -0.936646 -0.684583 -0.142390 11.00000 0.08085 0.07098 = 0.08249 -0.00808 -0.00277 -0.01132 AFIX 43 H32 2 -0.985732 -0.701747 -0.170956 11.00000 -1.20000 AFIX 0 C15 1 -0.393950 -0.758201 -0.627780 11.00000 0.08712 0.06096 = 0.10140 0.01292 -0.00958 -0.01897 AFIX 43 H15 2 -0.443268 -0.799799 -0.613572 11.00000 -1.20000 AFIX 0 C57 1 -0.579865 -0.543483 -0.278447 11.00000 0.07384 0.08758 = 0.07921 -0.01823 0.01121 0.00284 AFIX 43 H57 2 -0.526519 -0.555827 -0.249848 11.00000 -1.20000 AFIX 0 C45 1 -0.614510 -0.319997 -0.134469 11.00000 0.09417 0.07557 = 0.07140 0.01570 -0.00066 -0.02271 AFIX 43 H45 2 -0.568330 -0.323206 -0.165681 11.00000 -1.20000 AFIX 0 C43 1 -0.685981 -0.247106 -0.059587 11.00000 0.08929 0.07052 = 0.11253 -0.00574 -0.03366 -0.00623 AFIX 43 H43 2 -0.684425 -0.199371 -0.042410 11.00000 -1.20000 AFIX 0 C5 1 -0.315101 -0.287613 -0.772094 11.00000 0.09423 0.07599 = 0.08685 0.02240 -0.00977 0.00459 AFIX 43 H5 2 -0.347380 -0.254494 -0.797752 11.00000 -1.20000 AFIX 0 C27 1 -0.446925 -0.403892 -0.425867 11.00000 0.07346 0.09162 = 0.10237 -0.02305 0.00132 0.01643 AFIX 43 H27 2 -0.524813 -0.371471 -0.424265 11.00000 -1.20000 AFIX 0 C47 1 -0.832872 -0.303707 0.012155 11.00000 0.08868 0.10431 = 0.08480 -0.02749 -0.00579 0.01456 AFIX 137 H47A 2 -0.799439 -0.344414 0.034351 11.00000 -1.50000 H47B 2 -0.931201 -0.310310 0.006659 11.00000 -1.50000 H47C 2 -0.815965 -0.253559 0.027629 11.00000 -1.50000 AFIX 0 C56 1 -0.539928 -0.568428 -0.325258 11.00000 0.09930 0.10590 = 0.09881 -0.02877 -0.00097 -0.00201 AFIX 43 H56 2 -0.457923 -0.597189 -0.328323 11.00000 -1.20000 AFIX 0 C26 1 -0.365405 -0.414698 -0.382174 11.00000 0.09168 0.11116 = 0.08597 -0.03953 -0.00207 0.00752 AFIX 43 H26 2 -0.389249 -0.389359 -0.351916 11.00000 -1.20000 AFIX 0 C18 1 -0.178217 -0.723332 -0.748197 11.00000 0.10049 0.08430 = 0.09565 -0.02120 0.00115 0.00884 AFIX 137 H18A 2 -0.093432 -0.693370 -0.748248 11.00000 -1.50000 H18B 2 -0.237034 -0.706126 -0.775715 11.00000 -1.50000 H18C 2 -0.156631 -0.777878 -0.752582 11.00000 -1.50000 AFIX 0 C37 1 -0.671538 -0.661864 0.022764 11.00000 0.10139 0.09682 = 0.08927 0.00833 -0.00968 0.03046 AFIX 43 H37 2 -0.618352 -0.645773 0.050600 11.00000 -1.20000 AFIX 0 C36 1 -0.713255 -0.739946 0.018249 11.00000 0.09687 0.09090 = 0.11310 0.03351 0.00520 0.02633 AFIX 43 H36 2 -0.688145 -0.775810 0.043409 11.00000 -1.20000 AFIX 0 C35 1 -0.790613 -0.764385 -0.022720 11.00000 0.08674 0.07621 = 0.12355 0.02110 0.00994 0.00323 AFIX 43 H35 2 -0.819865 -0.816263 -0.024907 11.00000 -1.20000 AFIX 0 C44 1 -0.615746 -0.253530 -0.105645 11.00000 0.11364 0.07003 = 0.10571 0.01445 -0.01541 -0.02660 AFIX 43 H44 2 -0.566785 -0.210132 -0.117538 11.00000 -1.20000 AFIX 0 C54 1 -0.735999 -0.508635 -0.365818 11.00000 0.11661 0.10784 = 0.06705 -0.00055 -0.01296 -0.03922 AFIX 43 H54 2 -0.786592 -0.497173 -0.395233 11.00000 -1.20000 AFIX 0 C55 1 -0.616387 -0.552717 -0.368418 11.00000 0.11929 0.11733 = 0.09273 -0.03461 0.00397 -0.01614 AFIX 43 H55 2 -0.586813 -0.572175 -0.399827 11.00000 -1.20000 AFIX 0 HKLF 4 REM scs-niper-55_a.res in P2(1)2(1)2(1) REM R1 = 0.0631 for 3569 Fo > 4sig(Fo) and 0.1614 for all 8007 data REM 561 parameters refined using 0 restraints END WGHT 0.0796 0.0000 REM Highest difference peak 0.173, deepest hole -0.225, 1-sigma level 0.037 Q1 1 -0.1769 -0.6621 -0.7756 11.00000 0.05 0.17 Q2 1 -0.7642 -0.5344 -0.2322 11.00000 0.05 0.17 ; _shelx_res_checksum 18626 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N2 N -0.2929(4) -0.5506(2) -0.61365(16) 0.0551(11) Uani 1 1 d . . . . . N3 N -0.8155(5) -0.4500(2) -0.05412(17) 0.0611(12) Uani 1 1 d . . . . . N4 N -0.7098(5) -0.4582(2) -0.13102(17) 0.0611(12) Uani 1 1 d . . . . . N1 N -0.1880(4) -0.5696(2) -0.68918(16) 0.0588(12) Uani 1 1 d . . . . . C20 C -0.2517(6) -0.5246(3) -0.5207(2) 0.0526(14) Uani 1 1 d . . . . . C2 C -0.2243(5) -0.3877(3) -0.6939(2) 0.0525(14) Uani 1 1 d . . . . . C40 C -0.7847(6) -0.4958(3) -0.0935(2) 0.0576(14) Uani 1 1 d . . . . . C49 C -0.7481(6) -0.4700(3) -0.2246(2) 0.0539(14) Uani 1 1 d . . . . . C12 C -0.2501(5) -0.6386(3) -0.6735(2) 0.0557(14) Uani 1 1 d . . . . . C29 C -0.2937(6) -0.4884(3) -0.4739(2) 0.0560(14) Uani 1 1 d . . . . . C24 C -0.2133(7) -0.4986(3) -0.4295(2) 0.0625(15) Uani 1 1 d . . . . . C17 C -0.3169(6) -0.6280(3) -0.6267(2) 0.0579(14) Uani 1 1 d . . . . . C41 C -0.7547(6) -0.3779(3) -0.0663(2) 0.0570(14) Uani 1 1 d . . . . . C3 C -0.3088(6) -0.4150(3) -0.7345(2) 0.0648(15) Uani 1 1 d . . . . . H3 H -0.335255 -0.467433 -0.735285 0.078 Uiso 1 1 calc R U . . . C39 C -0.7862(5) -0.6318(3) -0.0573(2) 0.0579(14) Uani 1 1 d . . . . . C11 C -0.2167(6) -0.5191(3) -0.6526(2) 0.0533(14) Uani 1 1 d . . . . . C7 C -0.1834(6) -0.3066(3) -0.6949(2) 0.0633(16) Uani 1 1 d . . . . . C1 C -0.1768(6) -0.4352(3) -0.6531(2) 0.0538(14) Uani 1 1 d . . . . . C21 C -0.1329(6) -0.5685(3) -0.5219(2) 0.0644(15) Uani 1 1 d . . . . . H21 H -0.104445 -0.591307 -0.552476 0.077 Uiso 1 1 calc R U . . . C13 C -0.2531(6) -0.7117(3) -0.6979(2) 0.0680(16) Uani 1 1 d . . . . . C30 C -0.8257(5) -0.5789(3) -0.0970(2) 0.0566(14) Uani 1 1 d . . . . . C46 C -0.6880(6) -0.3830(3) -0.1135(2) 0.0604(14) Uani 1 1 d . . . . . C19 C -0.3421(5) -0.5126(3) -0.56731(19) 0.0585(14) Uani 1 1 d . . . . . H19A H -0.435064 -0.531907 -0.559764 0.070 Uiso 1 1 calc R U . . . H19B H -0.349667 -0.456757 -0.573773 0.070 Uiso 1 1 calc R U . . . C10 C -0.0970(6) -0.4030(3) -0.6157(2) 0.0660(16) Uani 1 1 d . . . . . H10 H -0.067324 -0.434506 -0.588772 0.079 Uiso 1 1 calc R U . . . C28 C -0.4144(6) -0.4400(3) -0.4709(2) 0.0664(16) Uani 1 1 d . . . . . H28 H -0.470895 -0.433063 -0.499431 0.080 Uiso 1 1 calc R U . . . C48 C -0.6590(5) -0.4899(3) -0.1791(2) 0.0629(15) Uani 1 1 d . . . . . H48A H -0.653364 -0.546537 -0.176153 0.075 Uiso 1 1 calc R U . . . H48B H -0.565386 -0.470421 -0.185093 0.075 Uiso 1 1 calc R U . . . C58 C -0.7050(7) -0.4978(3) -0.2730(2) 0.0637(15) Uani 1 1 d . . . . . C52 C -0.9043(8) -0.4359(4) -0.3124(3) 0.085(2) Uani 1 1 d . . . . . H52 H -0.956423 -0.423766 -0.341311 0.102 Uiso 1 1 calc R U . . . C50 C -0.8693(6) -0.4284(3) -0.2215(2) 0.0667(16) Uani 1 1 d . . . . . H50 H -0.901298 -0.411435 -0.189805 0.080 Uiso 1 1 calc R U . . . C9 C -0.0578(6) -0.3239(3) -0.6164(2) 0.0745(18) Uani 1 1 d . . . . . H9 H -0.001805 -0.303715 -0.590491 0.089 Uiso 1 1 calc R U . . . C34 C -0.8256(7) -0.7111(3) -0.0613(3) 0.0708(17) Uani 1 1 d . . . . . C51 C -0.9466(7) -0.4108(3) -0.2662(3) 0.0796(19) Uani 1 1 d . . . . . H51 H -1.027979 -0.381351 -0.263509 0.095 Uiso 1 1 calc R U . . . C16 C -0.3923(6) -0.6872(3) -0.6023(2) 0.0726(16) Uani 1 1 d . . . . . H16 H -0.437799 -0.679463 -0.571261 0.087 Uiso 1 1 calc R U . . . C6 C -0.2327(7) -0.2588(3) -0.7350(3) 0.0760(18) Uani 1 1 d . . . . . H6 H -0.207760 -0.206086 -0.735800 0.091 Uiso 1 1 calc R U . . . C38 C -0.7100(6) -0.6088(3) -0.0145(2) 0.0736(17) Uani 1 1 d . . . . . H38 H -0.684445 -0.556460 -0.010901 0.088 Uiso 1 1 calc R U . . . C22 C -0.0531(6) -0.5794(3) -0.4775(3) 0.0746(17) Uani 1 1 d . . . . . H22 H 0.027398 -0.609788 -0.478951 0.090 Uiso 1 1 calc R U . . . C33 C -0.9018(7) -0.7362(3) -0.1052(3) 0.0816(19) Uani 1 1 d . . . . . H33 H -0.927767 -0.788484 -0.108347 0.098 Uiso 1 1 calc R U . . . C4 C -0.3525(6) -0.3660(3) -0.7726(2) 0.0781(18) Uani 1 1 d . . . . . H4 H -0.407658 -0.385393 -0.799001 0.094 Uiso 1 1 calc R U . . . C25 C -0.2518(7) -0.4619(4) -0.3836(2) 0.0821(18) Uani 1 1 d . . . . . H25 H -0.199284 -0.469937 -0.354155 0.099 Uiso 1 1 calc R U . . . C23 C -0.0915(7) -0.5464(3) -0.4327(3) 0.0725(17) Uani 1 1 d . . . . . H23 H -0.037961 -0.554999 -0.403524 0.087 Uiso 1 1 calc R U . . . C14 C -0.3252(7) -0.7696(3) -0.6735(3) 0.0814(19) Uani 1 1 d . . . . . H14 H -0.328104 -0.819102 -0.688432 0.098 Uiso 1 1 calc R U . . . C42 C -0.7573(6) -0.3082(3) -0.0385(3) 0.0736(18) Uani 1 1 d . . . . . C53 C -0.7811(8) -0.4808(3) -0.3172(3) 0.0731(17) Uani 1 1 d . . . . . C8 C -0.1017(7) -0.2770(3) -0.6548(3) 0.0730(18) Uani 1 1 d . . . . . H8 H -0.077339 -0.224238 -0.654643 0.088 Uiso 1 1 calc R U . . . C31 C -0.8993(6) -0.6055(3) -0.1381(2) 0.0716(16) Uani 1 1 d . . . . . H31 H -0.925111 -0.570615 -0.163729 0.086 Uiso 1 1 calc R U . . . C32 C -0.9366(6) -0.6846(3) -0.1424(3) 0.0781(18) Uani 1 1 d . . . . . H32 H -0.985732 -0.701747 -0.170956 0.094 Uiso 1 1 calc R U . . . C15 C -0.3940(7) -0.7582(3) -0.6278(3) 0.083(2) Uani 1 1 d . . . . . H15 H -0.443268 -0.799799 -0.613572 0.100 Uiso 1 1 calc R U . . . C57 C -0.5799(7) -0.5435(3) -0.2784(3) 0.0802(18) Uani 1 1 d . . . . . H57 H -0.526519 -0.555827 -0.249848 0.096 Uiso 1 1 calc R U . . . C45 C -0.6145(6) -0.3200(4) -0.1345(2) 0.0804(18) Uani 1 1 d . . . . . H45 H -0.568330 -0.323206 -0.165681 0.096 Uiso 1 1 calc R U . . . C43 C -0.6860(8) -0.2471(4) -0.0596(3) 0.091(2) Uani 1 1 d . . . . . H43 H -0.684425 -0.199371 -0.042410 0.109 Uiso 1 1 calc R U . . . C5 C -0.3151(8) -0.2876(3) -0.7721(3) 0.0857(19) Uani 1 1 d . . . . . H5 H -0.347380 -0.254494 -0.797752 0.103 Uiso 1 1 calc R U . . . C27 C -0.4469(7) -0.4039(3) -0.4259(3) 0.089(2) Uani 1 1 d . . . . . H27 H -0.524813 -0.371471 -0.424265 0.107 Uiso 1 1 calc R U . . . C47 C -0.8329(7) -0.3037(3) 0.0122(2) 0.093(2) Uani 1 1 d . . . . . H47A H -0.799439 -0.344414 0.034351 0.139 Uiso 1 1 calc R U . . . H47B H -0.931201 -0.310310 0.006659 0.139 Uiso 1 1 calc R U . . . H47C H -0.815965 -0.253559 0.027629 0.139 Uiso 1 1 calc R U . . . C56 C -0.5399(8) -0.5684(4) -0.3253(3) 0.101(2) Uani 1 1 d . . . . . H56 H -0.457923 -0.597189 -0.328323 0.122 Uiso 1 1 calc R U . . . C26 C -0.3654(8) -0.4147(4) -0.3822(3) 0.096(2) Uani 1 1 d . . . . . H26 H -0.389249 -0.389359 -0.351916 0.116 Uiso 1 1 calc R U . . . C18 C -0.1782(8) -0.7233(3) -0.7482(2) 0.093(2) Uani 1 1 d . . . . . H18A H -0.093432 -0.693370 -0.748248 0.140 Uiso 1 1 calc R U . . . H18B H -0.237034 -0.706126 -0.775715 0.140 Uiso 1 1 calc R U . . . H18C H -0.156631 -0.777878 -0.752582 0.140 Uiso 1 1 calc R U . . . C37 C -0.6715(7) -0.6619(4) 0.0228(3) 0.096(2) Uani 1 1 d . . . . . H37 H -0.618352 -0.645773 0.050600 0.115 Uiso 1 1 calc R U . . . C36 C -0.7133(8) -0.7399(4) 0.0182(3) 0.100(2) Uani 1 1 d . . . . . H36 H -0.688145 -0.775810 0.043409 0.120 Uiso 1 1 calc R U . . . C35 C -0.7906(8) -0.7644(4) -0.0227(3) 0.096(2) Uani 1 1 d . . . . . H35 H -0.819865 -0.816263 -0.024907 0.115 Uiso 1 1 calc R U . . . C44 C -0.6157(8) -0.2535(4) -0.1056(3) 0.096(2) Uani 1 1 d . . . . . H44 H -0.566785 -0.210132 -0.117538 0.116 Uiso 1 1 calc R U . . . C54 C -0.7360(10) -0.5086(4) -0.3658(3) 0.097(2) Uani 1 1 d . . . . . H54 H -0.786592 -0.497173 -0.395233 0.117 Uiso 1 1 calc R U . . . C55 C -0.6164(10) -0.5527(5) -0.3684(3) 0.110(3) Uani 1 1 d . . . . . H55 H -0.586813 -0.572175 -0.399827 0.132 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N2 0.057(3) 0.055(2) 0.053(3) -0.001(2) 0.004(3) -0.003(2) N3 0.053(3) 0.064(3) 0.066(3) 0.002(2) -0.002(3) -0.006(2) N4 0.057(3) 0.066(3) 0.060(3) 0.002(2) 0.005(3) -0.006(2) N1 0.058(3) 0.054(2) 0.064(3) 0.000(2) 0.005(3) -0.004(2) C20 0.054(4) 0.051(3) 0.053(4) 0.004(3) -0.001(3) 0.001(3) C2 0.047(3) 0.054(3) 0.057(4) -0.004(3) 0.004(3) 0.000(2) C40 0.053(4) 0.062(3) 0.058(4) 0.004(3) 0.001(3) -0.003(3) C49 0.048(4) 0.057(3) 0.056(4) 0.007(3) -0.001(3) -0.005(3) C12 0.053(4) 0.052(3) 0.062(4) 0.004(3) -0.003(3) -0.003(3) C29 0.059(4) 0.050(3) 0.059(4) 0.003(3) -0.001(3) -0.004(3) C24 0.067(4) 0.061(3) 0.060(4) 0.001(3) -0.007(4) -0.005(3) C17 0.058(4) 0.054(3) 0.061(4) 0.009(3) -0.010(3) -0.001(3) C41 0.050(4) 0.055(3) 0.066(4) 0.003(3) -0.011(3) 0.000(3) C3 0.066(4) 0.064(3) 0.064(4) -0.001(3) 0.000(3) -0.001(3) C39 0.051(4) 0.059(3) 0.064(4) -0.005(3) 0.002(3) 0.003(3) C11 0.056(4) 0.052(3) 0.052(4) 0.007(3) 0.000(3) -0.003(3) C7 0.061(4) 0.050(3) 0.079(4) 0.000(3) 0.013(4) 0.000(3) C1 0.046(3) 0.060(3) 0.055(4) -0.001(3) -0.001(3) -0.001(3) C21 0.063(4) 0.065(3) 0.065(4) 0.004(3) 0.002(3) 0.009(3) C13 0.070(4) 0.063(4) 0.071(4) -0.003(3) -0.006(3) 0.002(3) C30 0.044(3) 0.063(3) 0.063(4) 0.001(3) 0.002(3) -0.006(3) C46 0.055(4) 0.059(3) 0.067(4) 0.003(3) -0.013(3) -0.007(3) C19 0.054(3) 0.068(3) 0.054(4) 0.006(3) 0.005(3) 0.005(3) C10 0.074(4) 0.064(3) 0.061(4) 0.003(3) -0.005(4) 0.000(3) C28 0.059(4) 0.069(3) 0.072(4) -0.013(3) 0.000(3) 0.008(3) C48 0.054(4) 0.069(3) 0.065(4) 0.004(3) 0.006(3) 0.004(3) C58 0.068(4) 0.057(3) 0.066(4) 0.004(3) -0.008(4) -0.013(3) C52 0.091(6) 0.086(4) 0.079(5) 0.020(4) -0.020(5) -0.024(4) C50 0.060(4) 0.064(3) 0.076(5) 0.009(3) 0.002(3) -0.004(3) C9 0.069(4) 0.067(4) 0.088(5) -0.015(4) -0.004(4) -0.009(3) C34 0.072(5) 0.057(3) 0.083(5) 0.018(4) 0.010(4) 0.006(3) C51 0.065(4) 0.081(4) 0.093(5) 0.020(4) -0.021(4) 0.005(3) C16 0.075(4) 0.076(4) 0.067(4) 0.014(4) 0.005(4) -0.013(3) C6 0.071(5) 0.063(3) 0.094(5) 0.014(4) -0.003(4) 0.001(3) C38 0.080(5) 0.070(3) 0.071(4) 0.001(3) 0.002(4) 0.011(3) C22 0.064(4) 0.078(4) 0.082(5) 0.011(4) -0.004(4) 0.015(3) C33 0.079(5) 0.060(4) 0.106(5) -0.002(4) 0.006(4) -0.013(3) C4 0.088(5) 0.077(4) 0.069(4) 0.000(4) -0.012(4) 0.006(3) C25 0.075(5) 0.107(5) 0.064(5) -0.012(4) -0.008(4) -0.003(4) C23 0.074(5) 0.067(3) 0.076(5) 0.006(3) -0.017(4) 0.004(3) C14 0.079(5) 0.063(4) 0.102(6) 0.004(4) -0.018(5) -0.006(3) C42 0.069(4) 0.063(4) 0.089(5) 0.000(4) -0.028(4) -0.001(3) C53 0.076(5) 0.070(4) 0.073(5) 0.003(3) -0.014(4) -0.015(3) C8 0.073(4) 0.053(3) 0.093(5) -0.003(4) -0.006(4) -0.017(3) C31 0.075(4) 0.058(3) 0.081(4) 0.000(3) 0.006(4) -0.006(3) C32 0.081(5) 0.071(4) 0.082(5) -0.008(4) -0.003(4) -0.011(4) C15 0.087(5) 0.061(4) 0.101(6) 0.013(4) -0.010(4) -0.019(3) C57 0.074(5) 0.088(4) 0.079(5) -0.018(4) 0.011(4) 0.003(4) C45 0.094(5) 0.076(4) 0.071(4) 0.016(4) -0.001(4) -0.023(4) C43 0.089(5) 0.071(4) 0.113(6) -0.006(5) -0.034(5) -0.006(4) C5 0.094(5) 0.076(4) 0.087(5) 0.022(4) -0.010(5) 0.005(4) C27 0.073(5) 0.092(4) 0.102(6) -0.023(4) 0.001(4) 0.016(4) C47 0.089(5) 0.104(5) 0.085(5) -0.027(4) -0.006(4) 0.015(4) C56 0.099(6) 0.106(5) 0.099(6) -0.029(5) -0.001(6) -0.002(4) C26 0.092(6) 0.111(5) 0.086(6) -0.040(4) -0.002(5) 0.008(4) C18 0.100(5) 0.084(4) 0.096(5) -0.021(4) 0.001(5) 0.009(4) C37 0.101(5) 0.097(5) 0.089(5) 0.008(4) -0.010(5) 0.030(4) C36 0.097(6) 0.091(5) 0.113(7) 0.034(5) 0.005(5) 0.026(4) C35 0.087(5) 0.076(4) 0.124(6) 0.021(5) 0.010(5) 0.003(4) C44 0.114(6) 0.070(5) 0.106(6) 0.014(5) -0.015(5) -0.027(4) C54 0.117(7) 0.108(5) 0.067(5) -0.001(4) -0.013(5) -0.039(5) C55 0.119(7) 0.117(6) 0.093(7) -0.035(5) 0.004(6) -0.016(6) 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' 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 C17 N2 C19 125.3(4) . . ? C11 N2 C17 106.2(4) . . ? C11 N2 C19 128.5(4) . . ? C40 N3 C41 104.4(4) . . ? C40 N4 C46 106.1(4) . . ? C40 N4 C48 128.1(4) . . ? C46 N4 C48 125.7(5) . . ? C11 N1 C12 104.6(4) . . ? C29 C20 C19 118.1(5) . . ? C21 C20 C29 119.6(5) . . ? C21 C20 C19 122.3(5) . . ? C3 C2 C7 117.4(5) . . ? C3 C2 C1 124.2(5) . . ? C1 C2 C7 118.5(5) . . ? N3 C40 N4 113.3(4) . . ? N3 C40 C30 123.7(5) . . ? N4 C40 C30 123.0(5) . . ? C58 C49 C48 117.8(5) . . ? C50 C49 C48 123.6(5) . . ? C50 C49 C58 118.6(5) . . ? N1 C12 C17 110.3(4) . . ? N1 C12 C13 129.3(5) . . ? C17 C12 C13 120.4(5) . . ? C24 C29 C20 119.9(5) . . ? C24 C29 C28 118.1(5) . . ? C28 C29 C20 121.9(5) . . ? C29 C24 C25 120.5(5) . . ? C29 C24 C23 118.2(5) . . ? C25 C24 C23 121.3(6) . . ? N2 C17 C12 105.4(4) . . ? N2 C17 C16 131.5(6) . . ? C12 C17 C16 123.1(5) . . ? C46 C41 N3 109.8(5) . . ? C46 C41 C42 121.6(5) . . ? C42 C41 N3 128.6(6) . . ? C2 C3 H3 119.3 . . ? C4 C3 C2 121.5(5) . . ? C4 C3 H3 119.3 . . ? C34 C39 C30 118.9(5) . . ? C38 C39 C30 123.1(5) . . ? C38 C39 C34 118.1(5) . . ? N2 C11 C1 121.6(5) . . ? N1 C11 N2 113.4(4) . . ? N1 C11 C1 124.9(5) . . ? C6 C7 C2 118.6(6) . . ? C8 C7 C2 119.0(5) . . ? C8 C7 C6 122.3(5) . . ? C2 C1 C11 118.5(5) . . ? C10 C1 C2 119.5(4) . . ? C10 C1 C11 122.0(5) . . ? C20 C21 H21 119.7 . . ? C20 C21 C22 120.6(6) . . ? C22 C21 H21 119.7 . . ? C12 C13 C18 120.2(5) . . ? C14 C13 C12 116.3(6) . . ? C14 C13 C18 123.5(6) . . ? C39 C30 C40 119.6(5) . . ? C31 C30 C40 120.5(5) . . ? C31 C30 C39 120.0(5) . . ? N4 C46 C41 106.4(5) . . ? N4 C46 C45 131.5(6) . . ? C41 C46 C45 122.1(5) . . ? N2 C19 C20 115.3(4) . . ? N2 C19 H19A 108.5 . . ? N2 C19 H19B 108.5 . . ? C20 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C1 C10 H10 118.9 . . ? C1 C10 C9 122.1(5) . . ? C9 C10 H10 118.9 . . ? C29 C28 H28 120.1 . . ? C27 C28 C29 119.8(6) . . ? C27 C28 H28 120.1 . . ? N4 C48 C49 114.2(4) . . ? N4 C48 H48A 108.7 . . ? N4 C48 H48B 108.7 . . ? C49 C48 H48A 108.7 . . ? C49 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? C49 C58 C57 121.1(6) . . ? C53 C58 C49 121.1(6) . . ? C53 C58 C57 117.8(6) . . ? C51 C52 H52 119.8 . . ? C51 C52 C53 120.3(6) . . ? C53 C52 H52 119.8 . . ? C49 C50 H50 119.8 . . ? C49 C50 C51 120.5(6) . . ? C51 C50 H50 119.8 . . ? C10 C9 H9 120.1 . . ? C8 C9 C10 119.7(5) . . ? C8 C9 H9 120.1 . . ? C39 C34 C33 119.0(5) . . ? C35 C34 C39 120.4(6) . . ? C35 C34 C33 120.5(6) . . ? C52 C51 C50 121.0(6) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C17 C16 H16 122.6 . . ? C15 C16 C17 114.7(6) . . ? C15 C16 H16 122.6 . . ? C7 C6 H6 119.3 . . ? C5 C6 C7 121.4(5) . . ? C5 C6 H6 119.3 . . ? C39 C38 H38 119.2 . . ? C37 C38 C39 121.5(6) . . ? C37 C38 H38 119.2 . . ? C21 C22 H22 119.5 . . ? C23 C22 C21 120.9(6) . . ? C23 C22 H22 119.5 . . ? C34 C33 H33 119.7 . . ? C32 C33 C34 120.6(5) . . ? C32 C33 H33 119.7 . . ? C3 C4 H4 119.9 . . ? C3 C4 C5 120.3(6) . . ? C5 C4 H4 119.9 . . ? C24 C25 H25 120.0 . . ? C26 C25 C24 120.0(6) . . ? C26 C25 H25 120.0 . . ? C24 C23 H23 119.7 . . ? C22 C23 C24 120.7(6) . . ? C22 C23 H23 119.7 . . ? C13 C14 H14 118.5 . . ? C13 C14 C15 123.0(6) . . ? C15 C14 H14 118.5 . . ? C41 C42 C47 120.6(6) . . ? C43 C42 C41 115.6(6) . . ? C43 C42 C47 123.8(6) . . ? C58 C53 C52 118.4(7) . . ? C58 C53 C54 120.7(7) . . ? C52 C53 C54 120.9(7) . . ? C7 C8 H8 119.4 . . ? C9 C8 C7 121.1(5) . . ? C9 C8 H8 119.4 . . ? C30 C31 H31 119.4 . . ? C30 C31 C32 121.1(6) . . ? C32 C31 H31 119.4 . . ? C33 C32 C31 120.4(6) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C16 C15 H15 118.8 . . ? C14 C15 C16 122.4(6) . . ? C14 C15 H15 118.8 . . ? C58 C57 H57 120.1 . . ? C56 C57 C58 119.8(7) . . ? C56 C57 H57 120.1 . . ? C46 C45 H45 122.6 . . ? C44 C45 C46 114.8(6) . . ? C44 C45 H45 122.6 . . ? C42 C43 H43 118.8 . . ? C42 C43 C44 122.4(6) . . ? C44 C43 H43 118.8 . . ? C6 C5 C4 120.9(6) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C28 C27 H27 119.4 . . ? C28 C27 C26 121.2(6) . . ? C26 C27 H27 119.4 . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C57 C56 H56 118.9 . . ? C57 C56 C55 122.2(7) . . ? C55 C56 H56 118.9 . . ? C25 C26 C27 120.4(6) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C38 C37 H37 120.3 . . ? C38 C37 C36 119.3(7) . . ? C36 C37 H37 120.3 . . ? C37 C36 H36 119.6 . . ? C35 C36 C37 120.8(6) . . ? C35 C36 H36 119.6 . . ? C34 C35 H35 120.1 . . ? C36 C35 C34 119.8(6) . . ? C36 C35 H35 120.1 . . ? C45 C44 C43 123.5(6) . . ? C45 C44 H44 118.3 . . ? C43 C44 H44 118.3 . . ? C53 C54 H54 120.6 . . ? C55 C54 C53 118.7(7) . . ? C55 C54 H54 120.6 . . ? C56 C55 C54 120.8(8) . . ? C56 C55 H55 119.6 . . ? C54 C55 H55 119.6 . . ? 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 N2 C17 1.383(6) . ? N2 C11 1.364(6) . ? N2 C19 1.453(6) . ? N3 C40 1.326(6) . ? N3 C41 1.398(6) . ? N4 C40 1.374(6) . ? N4 C46 1.378(6) . ? N4 C48 1.454(6) . ? N1 C12 1.382(6) . ? N1 C11 1.315(6) . ? C20 C29 1.426(7) . ? C20 C21 1.363(7) . ? C20 C19 1.510(6) . ? C2 C3 1.414(7) . ? C2 C7 1.439(6) . ? C2 C1 1.415(6) . ? C40 C30 1.473(7) . ? C49 C48 1.504(6) . ? C49 C58 1.412(7) . ? C49 C50 1.363(7) . ? C12 C17 1.392(7) . ? C12 C13 1.400(7) . ? C29 C24 1.404(7) . ? C29 C28 1.423(7) . ? C24 C25 1.404(7) . ? C24 C23 1.426(8) . ? C17 C16 1.397(7) . ? C41 C46 1.393(7) . ? C41 C42 1.394(7) . ? C3 H3 0.9300 . ? C3 C4 1.366(7) . ? C39 C30 1.425(7) . ? C39 C34 1.408(7) . ? C39 C38 1.394(7) . ? C11 C1 1.481(6) . ? C7 C6 1.410(7) . ? C7 C8 1.403(7) . ? C1 C10 1.358(6) . ? C21 H21 0.9300 . ? C21 C22 1.403(7) . ? C13 C14 1.363(8) . ? C13 C18 1.512(8) . ? C30 C31 1.364(7) . ? C46 C45 1.396(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C10 H10 0.9300 . ? C10 C9 1.401(7) . ? C28 H28 0.9300 . ? C28 C27 1.364(7) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C58 C53 1.398(7) . ? C58 C57 1.437(8) . ? C52 H52 0.9300 . ? C52 C51 1.345(8) . ? C52 C53 1.412(9) . ? C50 H50 0.9300 . ? C50 C51 1.415(8) . ? C9 H9 0.9300 . ? C9 C8 1.351(7) . ? C34 C33 1.426(8) . ? C34 C35 1.400(8) . ? C51 H51 0.9300 . ? C16 H16 0.9300 . ? C16 C15 1.383(8) . ? C6 H6 0.9300 . ? C6 C5 1.344(8) . ? C38 H38 0.9300 . ? C38 C37 1.380(7) . ? C22 H22 0.9300 . ? C22 C23 1.352(7) . ? C33 H33 0.9300 . ? C33 C32 1.352(8) . ? C4 H4 0.9300 . ? C4 C5 1.384(7) . ? C25 H25 0.9300 . ? C25 C26 1.355(8) . ? C23 H23 0.9300 . ? C14 H14 0.9300 . ? C14 C15 1.379(8) . ? C42 C43 1.363(8) . ? C42 C47 1.511(8) . ? C53 C54 1.425(9) . ? C8 H8 0.9300 . ? C31 H31 0.9300 . ? C31 C32 1.399(7) . ? C32 H32 0.9300 . ? C15 H15 0.9300 . ? C57 H57 0.9300 . ? C57 C56 1.351(8) . ? C45 H45 0.9300 . ? C45 C44 1.361(8) . ? C43 H43 0.9300 . ? C43 C44 1.384(9) . ? C5 H5 0.9300 . ? C27 H27 0.9300 . ? C27 C26 1.396(8) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C56 H56 0.9300 . ? C56 C55 1.372(10) . ? C26 H26 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C37 H37 0.9300 . ? C37 C36 1.396(9) . ? C36 H36 0.9300 . ? C36 C35 1.368(8) . ? C35 H35 0.9300 . ? C44 H44 0.9300 . ? C54 H54 0.9300 . ? C54 C55 1.373(10) . ? C55 H55 0.9300 . ? 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 N2 C17 C16 C15 179.2(5) . . . . ? N2 C11 C1 C2 -119.3(6) . . . . ? N2 C11 C1 C10 60.5(7) . . . . ? N3 C40 C30 C39 -55.8(7) . . . . ? N3 C40 C30 C31 125.1(6) . . . . ? N3 C41 C46 N4 1.1(6) . . . . ? N3 C41 C46 C45 -178.0(5) . . . . ? N3 C41 C42 C43 178.8(5) . . . . ? N3 C41 C42 C47 0.1(9) . . . . ? N4 C40 C30 C39 123.9(6) . . . . ? N4 C40 C30 C31 -55.2(7) . . . . ? N4 C46 C45 C44 -179.9(6) . . . . ? N1 C12 C17 N2 -0.7(6) . . . . ? N1 C12 C17 C16 178.0(5) . . . . ? N1 C12 C13 C14 -178.9(5) . . . . ? N1 C12 C13 C18 1.5(9) . . . . ? N1 C11 C1 C2 58.3(7) . . . . ? N1 C11 C1 C10 -121.9(6) . . . . ? C20 C29 C24 C25 178.6(5) . . . . ? C20 C29 C24 C23 -0.8(7) . . . . ? C20 C29 C28 C27 -177.1(5) . . . . ? C20 C21 C22 C23 -0.4(8) . . . . ? C2 C3 C4 C5 -0.3(9) . . . . ? C2 C7 C6 C5 -0.7(9) . . . . ? C2 C7 C8 C9 2.0(9) . . . . ? C2 C1 C10 C9 -0.9(8) . . . . ? C40 N3 C41 C46 -0.1(6) . . . . ? C40 N3 C41 C42 178.7(5) . . . . ? C40 N4 C46 C41 -1.6(5) . . . . ? C40 N4 C46 C45 177.3(6) . . . . ? C40 N4 C48 C49 99.6(6) . . . . ? C40 C30 C31 C32 178.8(5) . . . . ? C49 C58 C53 C52 -1.1(8) . . . . ? C49 C58 C53 C54 179.5(5) . . . . ? C49 C58 C57 C56 -179.0(5) . . . . ? C49 C50 C51 C52 1.4(8) . . . . ? C12 N1 C11 N2 0.4(6) . . . . ? C12 N1 C11 C1 -177.4(5) . . . . ? C12 C17 C16 C15 1.0(8) . . . . ? C12 C13 C14 C15 0.9(9) . . . . ? C29 C20 C21 C22 1.2(7) . . . . ? C29 C20 C19 N2 179.6(4) . . . . ? C29 C24 C25 C26 -1.6(8) . . . . ? C29 C24 C23 C22 1.5(8) . . . . ? C29 C28 C27 C26 -1.3(9) . . . . ? C24 C29 C28 C27 1.4(7) . . . . ? C24 C25 C26 C27 1.7(10) . . . . ? C17 N2 C11 N1 -0.9(6) . . . . ? C17 N2 C11 C1 177.0(5) . . . . ? C17 N2 C19 C20 83.7(6) . . . . ? C17 C12 C13 C14 0.7(8) . . . . ? C17 C12 C13 C18 -178.9(5) . . . . ? C17 C16 C15 C14 0.6(9) . . . . ? C41 N3 C40 N4 -1.0(6) . . . . ? C41 N3 C40 C30 178.8(5) . . . . ? C41 C46 C45 C44 -1.1(8) . . . . ? C41 C42 C43 C44 0.2(9) . . . . ? C3 C2 C7 C6 1.9(7) . . . . ? C3 C2 C7 C8 178.8(5) . . . . ? C3 C2 C1 C11 0.4(8) . . . . ? C3 C2 C1 C10 -179.4(5) . . . . ? C3 C4 C5 C6 1.6(10) . . . . ? C39 C30 C31 C32 -0.4(8) . . . . ? C39 C34 C33 C32 -0.4(9) . . . . ? C39 C34 C35 C36 -2.4(9) . . . . ? C39 C38 C37 C36 -1.9(10) . . . . ? C11 N2 C17 C12 0.9(5) . . . . ? C11 N2 C17 C16 -177.6(6) . . . . ? C11 N2 C19 C20 -96.8(6) . . . . ? C11 N1 C12 C17 0.2(6) . . . . ? C11 N1 C12 C13 179.8(5) . . . . ? C11 C1 C10 C9 179.3(5) . . . . ? C7 C2 C3 C4 -1.4(8) . . . . ? C7 C2 C1 C11 -178.8(5) . . . . ? C7 C2 C1 C10 1.4(7) . . . . ? C7 C6 C5 C4 -1.1(10) . . . . ? C1 C2 C3 C4 179.4(5) . . . . ? C1 C2 C7 C6 -178.8(5) . . . . ? C1 C2 C7 C8 -1.9(7) . . . . ? C1 C10 C9 C8 1.0(9) . . . . ? C21 C20 C29 C24 -0.5(7) . . . . ? C21 C20 C29 C28 178.0(5) . . . . ? C21 C20 C19 N2 -0.5(7) . . . . ? C21 C22 C23 C24 -0.9(8) . . . . ? C13 C12 C17 N2 179.7(5) . . . . ? C13 C12 C17 C16 -1.7(8) . . . . ? C13 C14 C15 C16 -1.6(10) . . . . ? C30 C39 C34 C33 0.9(8) . . . . ? C30 C39 C34 C35 -179.0(5) . . . . ? C30 C39 C38 C37 -178.9(5) . . . . ? C30 C31 C32 C33 0.9(9) . . . . ? C46 N4 C40 N3 1.6(6) . . . . ? C46 N4 C40 C30 -178.1(5) . . . . ? C46 N4 C48 C49 -82.1(6) . . . . ? C46 C41 C42 C43 -2.5(8) . . . . ? C46 C41 C42 C47 178.8(5) . . . . ? C46 C45 C44 C43 -1.3(10) . . . . ? C19 N2 C17 C12 -179.5(4) . . . . ? C19 N2 C17 C16 2.0(9) . . . . ? C19 N2 C11 N1 179.6(5) . . . . ? C19 N2 C11 C1 -2.6(8) . . . . ? C19 C20 C29 C24 179.5(4) . . . . ? C19 C20 C29 C28 -2.0(7) . . . . ? C19 C20 C21 C22 -178.8(5) . . . . ? C10 C9 C8 C7 -1.6(9) . . . . ? C28 C29 C24 C25 0.0(7) . . . . ? C28 C29 C24 C23 -179.4(5) . . . . ? C28 C27 C26 C25 -0.2(10) . . . . ? C48 N4 C40 N3 -179.8(5) . . . . ? C48 N4 C40 C30 0.4(8) . . . . ? C48 N4 C46 C41 179.8(5) . . . . ? C48 N4 C46 C45 -1.2(9) . . . . ? C48 C49 C58 C53 -179.1(5) . . . . ? C48 C49 C58 C57 -0.2(7) . . . . ? C48 C49 C50 C51 179.0(5) . . . . ? C58 C49 C48 N4 179.2(4) . . . . ? C58 C49 C50 C51 -2.7(7) . . . . ? C58 C53 C54 C55 0.1(9) . . . . ? C58 C57 C56 C55 -1.0(10) . . . . ? C52 C53 C54 C55 -179.3(6) . . . . ? C50 C49 C48 N4 -2.5(7) . . . . ? C50 C49 C58 C53 2.5(7) . . . . ? C50 C49 C58 C57 -178.6(5) . . . . ? C34 C39 C30 C40 -179.7(5) . . . . ? C34 C39 C30 C31 -0.5(8) . . . . ? C34 C39 C38 C37 1.1(8) . . . . ? C34 C33 C32 C31 -0.5(9) . . . . ? C51 C52 C53 C58 -0.2(8) . . . . ? C51 C52 C53 C54 179.2(6) . . . . ? C6 C7 C8 C9 178.8(5) . . . . ? C38 C39 C30 C40 0.3(8) . . . . ? C38 C39 C30 C31 179.4(5) . . . . ? C38 C39 C34 C33 -179.0(5) . . . . ? C38 C39 C34 C35 1.1(8) . . . . ? C38 C37 C36 C35 0.5(10) . . . . ? C33 C34 C35 C36 177.7(6) . . . . ? C25 C24 C23 C22 -177.8(5) . . . . ? C23 C24 C25 C26 177.8(6) . . . . ? C42 C41 C46 N4 -177.8(5) . . . . ? C42 C41 C46 C45 3.1(8) . . . . ? C42 C43 C44 C45 1.8(11) . . . . ? C53 C58 C57 C56 -0.1(8) . . . . ? C53 C52 C51 C50 0.1(9) . . . . ? C53 C54 C55 C56 -1.3(10) . . . . ? C8 C7 C6 C5 -177.5(6) . . . . ? C57 C58 C53 C52 -180.0(5) . . . . ? C57 C58 C53 C54 0.6(8) . . . . ? C57 C56 C55 C54 1.8(11) . . . . ? C47 C42 C43 C44 178.8(6) . . . . ? C18 C13 C14 C15 -179.5(6) . . . . ? C37 C36 C35 C34 1.6(10) . . . . ? C35 C34 C33 C32 179.5(6) . . . . ?