#------------------------------------------------------------------------------ #$Date: 2018-01-16 04:30:34 +0200 (Tue, 16 Jan 2018) $ #$Revision: 205236 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229960.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_7229960 loop_ _publ_author_name 'Aghabali, Amineh' 'Jun, Sharon' 'Olmstead, Marilyn M.' 'Balch, Alan L.' _publ_section_title ; The Directional Character of the Piperazine Double Addition Product, e{N(CH2CH2)2N}2C60, as a Building Block for Forming Crystalline Fullerene Polymers ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE02117H _journal_year 2018 _chemical_formula_moiety '2(C34 H8 N2), 2(I2), 2(C3 H3), 0.5(C S2), 0.5(C S2)' _chemical_formula_sum 'C72 H19 I4 N4 S2' _chemical_formula_weight 1511.63 _chemical_name_systematic 'e{N(CH2CH2)2N}2C60?3I2?CS2?C6H6 ' _chemical_properties_physical Efflorescent _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-09-15 deposited with the CCDC. 2018-01-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.744(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.4566(7) _cell_length_b 10.6707(5) _cell_length_c 16.0942(7) _cell_measurement_reflns_used 9966 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 43.948 _cell_measurement_theta_min 2.585 _cell_volume 2390.99(19) _computing_cell_refinement 'SAINT (Bruker, 2014)' _computing_data_collection 'Apex 2 (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'XT (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.42 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker D8 with Photon 100 CMOS detector' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7749 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_unetI/netI 0.0319 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 61791 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 27.706 _diffrn_reflns_theta_max 43.971 _diffrn_reflns_theta_min 2.584 _diffrn_source 'Advanced Light Source, beamline 11.3.1' _exptl_absorpt_coefficient_mu 3.428 _exptl_absorpt_correction_T_max 0.4458 _exptl_absorpt_correction_T_min 0.3944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2014)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.100 _exptl_crystal_description block _exptl_crystal_F_000 1446 _exptl_crystal_recrystallization_method 'diffusion of a CS2 solution of the fullerene with a solution of I2 in benzene' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.060 _refine_diff_density_max 3.182 _refine_diff_density_min -2.267 _refine_diff_density_rms 0.171 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 405 _refine_ls_number_reflns 14780 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0369 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+6.1659P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.0927 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12163 _reflns_number_total 14780 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02117h1.cif _cod_data_source_block aa96 _cod_database_code 7229960 _shelx_shelxl_version_number 2014/7 _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_min 0.279 _shelx_estimated_absorpt_t_max 0.821 _shelx_res_file ; aa96.res created by SHELXL-2014/7 TITL aa96x_a.res in P2(1)/m CELL 0.7749 15.4566 10.6707 16.0942 90 115.744 90 ZERR 2 0.0007 0.0005 0.0007 0 0.002 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H I N S DISP C 0.004 0.002 13.6 DISP H 0.0000 0.0000 0.7 DISP I -0.3071 2.1212 9635.7 DISP N 0.0076 0.004 23.9 DISP S 0.1430 0.1480 674.2 UNIT 144 38 8 8 4 DFIX 1.55 0.02 C37 S1 C37 S2 C38 S3 C38 S4 DFIX 3.10 0.08 S1 S2 S3 S4 L.S. 10 SIZE 0.06 0.08 0.5 TEMP -173 BOND $H acta MORE -1 CONF eqiv $1 x, 2.5-y, z rtab bond I1 N1 rtab bond I2 N3 rtab angl N1 I1 I1_$1 rtab angl N3 I2 I3 MERG 2 WGHT 0.035100 6.165900 FVAR 0.28412 I1 3 0.684982 1.121784 0.908419 11.00000 0.01243 0.01573 = 0.01336 -0.00206 0.00325 -0.00011 I2 3 0.416717 0.750000 0.540632 10.50000 0.00819 0.01357 = 0.01274 0.00000 0.00291 0.00000 I3 3 0.309031 0.750000 0.640923 10.50000 0.02008 0.02997 = 0.02562 0.00000 0.01572 0.00000 N1 4 0.698640 0.868709 0.900603 11.00000 0.01355 0.01317 = 0.00989 -0.00233 0.00486 0.00076 N2 4 0.615706 0.750000 0.354155 10.50000 0.00882 0.02715 = 0.00633 0.00000 0.00082 0.00000 N3 4 0.521377 0.750000 0.451503 10.50000 0.00641 0.01606 = 0.00755 0.00000 0.00128 0.00000 C1 1 0.752170 0.825672 0.846981 11.00000 0.01016 0.01327 = 0.00793 -0.00113 0.00355 0.00056 C2 1 0.852809 0.884733 0.885553 11.00000 0.01030 0.01414 = 0.00961 -0.00331 0.00340 -0.00155 C3 1 0.936709 0.819528 0.931493 11.00000 0.01147 0.01719 = 0.00754 -0.00169 0.00216 -0.00151 C4 1 1.024485 0.860188 0.927591 11.00000 0.00976 0.02066 = 0.00963 -0.00262 0.00167 -0.00212 C5 1 1.077748 0.750000 0.925014 10.50000 0.00915 0.02162 = 0.00858 0.00000 0.00051 0.00000 C6 1 1.129844 0.750000 0.872421 10.50000 0.00717 0.02317 = 0.01163 0.00000 0.00057 0.00000 C7 1 1.129523 0.860107 0.819497 11.00000 0.00818 0.02367 = 0.01339 -0.00079 0.00260 -0.00369 C8 1 1.128557 0.818126 0.733410 11.00000 0.00826 0.02469 = 0.01360 -0.00135 0.00454 -0.00291 C9 1 1.074644 0.883272 0.652123 11.00000 0.00933 0.02287 = 0.01399 0.00070 0.00534 -0.00319 C10 1 1.018311 0.814980 0.567842 11.00000 0.00918 0.02433 = 0.01245 0.00088 0.00558 -0.00125 C11 1 0.929199 0.883515 0.518108 11.00000 0.00985 0.02366 = 0.01171 0.00298 0.00571 -0.00177 C12 1 0.843056 0.817907 0.470905 11.00000 0.01056 0.02172 = 0.00873 0.00194 0.00456 0.00004 C13 1 0.755425 0.860274 0.472189 11.00000 0.00919 0.01899 = 0.00854 0.00320 0.00321 0.00009 C14 1 0.685431 0.750000 0.452746 10.50000 0.00824 0.01788 = 0.00802 0.00000 0.00286 0.00000 C15 1 0.627435 0.750000 0.515812 10.50000 0.00637 0.01385 = 0.00714 0.00000 0.00169 0.00000 C16 1 0.652014 0.859807 0.583447 11.00000 0.00821 0.01140 = 0.00891 0.00047 0.00301 0.00078 C17 1 0.656612 0.818624 0.669965 11.00000 0.00805 0.00991 = 0.00858 0.00033 0.00308 -0.00005 C18 1 0.707782 0.884216 0.750479 11.00000 0.00948 0.01086 = 0.00873 -0.00098 0.00343 0.00048 C19 1 0.762653 0.990346 0.747551 11.00000 0.01120 0.01017 = 0.01175 -0.00097 0.00400 0.00050 C20 1 0.852331 0.991810 0.830898 11.00000 0.01244 0.01109 = 0.01126 -0.00280 0.00399 -0.00229 C21 1 0.936101 1.033844 0.827273 11.00000 0.01307 0.01240 = 0.01410 -0.00419 0.00425 -0.00467 C22 1 1.024523 0.966412 0.877112 11.00000 0.01120 0.01699 = 0.01148 -0.00374 0.00263 -0.00444 C23 1 1.078051 0.965860 0.821781 11.00000 0.00977 0.02004 = 0.01345 -0.00217 0.00229 -0.00482 C24 1 1.021873 1.034034 0.737057 11.00000 0.01163 0.01684 = 0.01737 -0.00078 0.00513 -0.00572 C25 1 1.020358 0.993611 0.653877 11.00000 0.01116 0.01940 = 0.01604 0.00144 0.00532 -0.00555 C26 1 0.930424 0.993121 0.570574 11.00000 0.01118 0.01938 = 0.01416 0.00336 0.00552 -0.00312 C27 1 0.845795 1.031999 0.574120 11.00000 0.01270 0.01385 = 0.01437 0.00388 0.00513 -0.00163 C28 1 0.757325 0.963446 0.523522 11.00000 0.00999 0.01534 = 0.01087 0.00373 0.00384 -0.00007 C29 1 0.704234 0.962765 0.580990 11.00000 0.00972 0.01127 = 0.01130 0.00325 0.00369 0.00115 C30 1 0.760311 1.030674 0.663959 11.00000 0.01223 0.00957 = 0.01355 0.00057 0.00509 0.00006 C31 1 0.847930 1.073742 0.660438 11.00000 0.01385 0.00992 = 0.01515 0.00123 0.00501 -0.00173 C32 1 0.933956 1.075674 0.740415 11.00000 0.01322 0.01252 = 0.01667 -0.00177 0.00497 -0.00427 C33 1 0.747747 0.822678 0.996394 11.00000 0.01907 0.02219 = 0.00968 -0.00231 0.00670 -0.00054 AFIX 23 H33A 2 0.714279 0.854080 1.032555 11.00000 -1.20000 H33B 2 0.814643 0.854086 1.025447 11.00000 -1.20000 AFIX 0 C34 1 0.599210 0.822568 0.857532 11.00000 0.01282 0.01909 = 0.01549 -0.00085 0.00752 0.00052 AFIX 23 H34A 2 0.566225 0.853932 0.793401 11.00000 -1.20000 H34B 2 0.564091 0.853925 0.892164 11.00000 -1.20000 AFIX 0 C35 1 0.496561 0.636803 0.392076 11.00000 0.00944 0.02142 = 0.01114 -0.00489 0.00254 -0.00302 AFIX 23 H35A 2 0.426853 0.636136 0.350859 11.00000 -1.20000 H35B 2 0.512214 0.560492 0.430864 11.00000 -1.20000 AFIX 0 C36 1 0.554462 0.637623 0.333538 11.00000 0.01072 0.02963 = 0.01014 -0.00691 0.00283 -0.00234 AFIX 23 H36A 2 0.595005 0.561551 0.347300 11.00000 -1.20000 H36B 2 0.509483 0.636453 0.267139 11.00000 -1.20000 AFIX 0 PART 1 C37 1 0.612473 0.377679 0.110224 10.25000 0.01915 S1 5 0.618520 0.250000 0.096585 10.25000 0.01616 0.07172 = 0.02040 0.00000 0.01384 0.00000 S2 5 0.607091 0.516414 0.128233 10.25000 0.07547 0.03197 = 0.09654 -0.01486 0.07551 -0.01960 PART 2 C38 1 0.690556 0.676705 0.186392 10.25000 0.02619 S3 5 0.791470 0.750000 0.239879 10.25000 0.02195 0.07985 = 0.01464 0.00000 0.00700 0.00000 S4 5 0.585068 0.624436 0.124343 10.25000 0.04235 0.10700 = 0.03861 -0.02247 0.03074 -0.02903 PART -3 AFIX 6 C39 1 0.580673 0.755084 0.123302 10.25000 0.06090 H39 2 0.514872 0.765742 0.081915 10.25000 -1.20000 C40 1 0.618576 0.635291 0.147828 10.25000 0.04156 H40 2 0.578678 0.564078 0.123204 10.25000 -1.20000 C41 1 0.714851 0.619695 0.208386 10.25000 0.03339 H41 2 0.740756 0.537822 0.225145 10.25000 -1.20000 C42 1 0.773228 0.723893 0.244412 10.25000 0.02814 H42 2 0.839028 0.713233 0.285798 10.25000 -1.20000 C43 1 0.735327 0.843686 0.219887 10.25000 0.03484 H43 2 0.775226 0.914900 0.244511 10.25000 -1.20000 C44 1 0.639053 0.859282 0.159334 10.25000 0.09369 H44 2 0.613151 0.941158 0.142568 10.25000 -1.20000 AFIX 0 HKLF 4 REM aa96x_a.res in P2(1)/m REM R1 = 0.0369 for 12163 Fo > 4sig(Fo) and 0.0502 for all 14780 data REM 405 parameters refined using 6 restraints END WGHT 0.0351 6.1661 REM Highest difference peak 3.182, deepest hole -2.267, 1-sigma level 0.171 Q1 1 0.6548 1.1170 0.9280 11.00000 0.05 3.18 Q2 1 0.4092 0.7500 0.5715 10.50000 0.05 2.38 Q3 1 0.6820 1.0642 0.9163 11.00000 0.05 2.22 Q4 1 0.6829 1.1868 0.9026 11.00000 0.05 1.89 Q5 1 0.4092 0.8282 0.0091 11.00000 0.05 1.27 Q6 1 0.3118 0.7500 0.6787 10.50000 0.05 1.26 Q7 1 0.6434 0.9519 0.1664 11.00000 0.05 1.18 Q8 1 0.5925 0.7500 0.8574 10.50000 0.05 1.10 Q9 1 1.0999 0.7500 0.8933 10.50000 0.05 1.01 Q10 1 0.7480 0.7500 0.9955 10.50000 0.05 1.01 Q11 1 0.8425 0.9574 0.8567 11.00000 0.05 0.99 Q12 1 0.6495 0.7500 0.6807 10.50000 0.05 0.93 Q13 1 0.6971 0.9267 0.8940 11.00000 0.05 0.89 Q14 1 0.7517 0.9133 0.4893 11.00000 0.05 0.87 Q15 1 1.0219 0.7500 0.5770 10.50000 0.05 0.87 Q16 1 0.6982 0.7500 0.2312 10.50000 0.05 0.84 Q17 1 0.9227 0.7500 0.9284 10.50000 0.05 0.83 Q18 1 0.6904 1.2500 0.8867 10.50000 0.05 0.81 Q19 1 0.6490 0.8320 0.6196 11.00000 0.05 0.73 Q20 1 1.0626 0.7017 0.9299 11.00000 0.05 0.73 ; _shelx_res_checksum 32559 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -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 I1 I 0.68498(2) 1.12178(2) 0.90842(2) 0.01468(3) Uani 1 1 d . . . . . I2 I 0.41672(2) 0.7500 0.54063(2) 0.01208(3) Uani 1 2 d S T P . . I3 I 0.30903(2) 0.7500 0.64092(2) 0.02315(5) Uani 1 2 d S T P . . N1 N 0.69864(12) 0.86871(16) 0.90060(11) 0.0123(3) Uani 1 1 d . . . . . N2 N 0.61571(17) 0.7500 0.35415(16) 0.0150(4) Uani 1 2 d S T P . . N3 N 0.52138(15) 0.7500 0.45150(15) 0.0106(3) Uani 1 2 d S T P . . C1 C 0.75217(13) 0.82567(18) 0.84698(12) 0.0106(3) Uani 1 1 d . . . . . C2 C 0.85281(13) 0.88473(18) 0.88555(12) 0.0117(3) Uani 1 1 d . . . . . C3 C 0.93671(13) 0.81953(19) 0.93149(12) 0.0128(3) Uani 1 1 d . . . . . C4 C 1.02448(13) 0.8602(2) 0.92759(13) 0.0143(3) Uani 1 1 d . . . . . C5 C 1.07775(19) 0.7500 0.92501(18) 0.0143(4) Uani 1 2 d S T P . . C6 C 1.12984(19) 0.7500 0.87242(19) 0.0152(5) Uani 1 2 d S T P . . C7 C 1.12952(13) 0.8601(2) 0.81950(14) 0.0158(3) Uani 1 1 d . . . . . C8 C 1.12856(13) 0.8181(2) 0.73341(14) 0.0156(3) Uani 1 1 d . . . . . C9 C 1.07464(14) 0.8833(2) 0.65212(14) 0.0153(3) Uani 1 1 d . . . . . C10 C 1.01831(13) 0.8150(2) 0.56784(14) 0.0150(3) Uani 1 1 d . . . . . C11 C 0.92920(13) 0.8835(2) 0.51811(13) 0.0147(3) Uani 1 1 d . . . . . C12 C 0.84306(13) 0.8179(2) 0.47090(13) 0.0135(3) Uani 1 1 d . . . . . C13 C 0.75543(13) 0.86027(19) 0.47219(12) 0.0125(3) Uani 1 1 d . . . . . C14 C 0.68543(18) 0.7500 0.45275(17) 0.0116(4) Uani 1 2 d S T P . . C15 C 0.62744(17) 0.7500 0.51581(17) 0.0096(4) Uani 1 2 d S T P . . C16 C 0.65201(12) 0.85981(17) 0.58345(12) 0.0098(3) Uani 1 1 d . . . . . C17 C 0.65661(12) 0.81862(17) 0.66996(12) 0.0090(2) Uani 1 1 d . . . . . C18 C 0.70778(12) 0.88422(17) 0.75048(12) 0.0099(3) Uani 1 1 d . . . . . C19 C 0.76265(13) 0.99035(17) 0.74755(13) 0.0114(3) Uani 1 1 d . . . . . C20 C 0.85233(13) 0.99181(18) 0.83090(13) 0.0120(3) Uani 1 1 d . . . . . C21 C 0.93610(14) 1.03384(19) 0.82727(14) 0.0138(3) Uani 1 1 d . . . . . C22 C 1.02452(14) 0.9664(2) 0.87711(13) 0.0140(3) Uani 1 1 d . . . . . C23 C 1.07805(14) 0.9659(2) 0.82178(14) 0.0154(3) Uani 1 1 d . . . . . C24 C 1.02187(14) 1.0340(2) 0.73706(15) 0.0157(3) Uani 1 1 d . . . . . C25 C 1.02036(14) 0.9936(2) 0.65388(14) 0.0157(3) Uani 1 1 d . . . . . C26 C 0.93042(14) 0.9931(2) 0.57057(14) 0.0149(3) Uani 1 1 d . . . . . C27 C 0.84580(14) 1.03200(19) 0.57412(14) 0.0139(3) Uani 1 1 d . . . . . C28 C 0.75732(13) 0.96345(19) 0.52352(13) 0.0123(3) Uani 1 1 d . . . . . C29 C 0.70423(13) 0.96276(18) 0.58099(13) 0.0111(3) Uani 1 1 d . . . . . C30 C 0.76031(13) 1.03067(17) 0.66396(13) 0.0120(3) Uani 1 1 d . . . . . C31 C 0.84793(14) 1.07374(18) 0.66044(14) 0.0134(3) Uani 1 1 d . . . . . C32 C 0.93396(14) 1.07567(19) 0.74042(14) 0.0147(3) Uani 1 1 d . . . . . C33 C 0.74775(16) 0.8227(2) 0.99639(14) 0.0168(3) Uani 1 1 d . . . . . H33A H 0.7143 0.8541 1.0326 0.020 Uiso 1 1 calc R U . . . H33B H 0.8146 0.8541 1.0254 0.020 Uiso 1 1 calc R U . . . C34 C 0.59921(14) 0.8226(2) 0.85753(14) 0.0153(3) Uani 1 1 d . . . . . H34A H 0.5662 0.8539 0.7934 0.018 Uiso 1 1 calc R U . . . H34B H 0.5641 0.8539 0.8922 0.018 Uiso 1 1 calc R U . . . C35 C 0.49656(13) 0.6368(2) 0.39208(13) 0.0147(3) Uani 1 1 d . . . . . H35A H 0.4269 0.6361 0.3509 0.018 Uiso 1 1 calc R U . . . H35B H 0.5122 0.5605 0.4309 0.018 Uiso 1 1 calc R U . . . C36 C 0.55446(14) 0.6376(2) 0.33354(14) 0.0174(4) Uani 1 1 d . . . . . H36A H 0.5950 0.5616 0.3473 0.021 Uiso 1 1 calc R U . . . H36B H 0.5095 0.6365 0.2671 0.021 Uiso 1 1 calc R U . . . C37 C 0.6125(7) 0.3777(7) 0.1102(6) 0.0192(14) Uiso 0.25 1 d D . P A 1 S1 S 0.61852(13) 0.2500 0.09659(13) 0.0340(5) Uani 0.5 2 d DS T P A 1 S2 S 0.6071(4) 0.5164(4) 0.1282(4) 0.0544(12) Uani 0.25 1 d D . P A 1 C38 C 0.6906(7) 0.6767(11) 0.1864(7) 0.0262(18) Uiso 0.25 1 d D . P B 2 S3 S 0.7915(2) 0.7500 0.23988(15) 0.0392(6) Uani 0.5 2 d DS T P B 2 S4 S 0.5851(3) 0.6244(6) 0.1243(3) 0.0580(14) Uani 0.25 1 d D . P B 2 C39 C 0.5807(6) 0.7551(16) 0.1233(7) 0.061(3) Uiso 0.25 1 d G . P C -3 H39 H 0.5149 0.7657 0.0819 0.073 Uiso 0.25 1 d G U P C -3 C40 C 0.6186(7) 0.6353(13) 0.1478(8) 0.042(4) Uiso 0.25 1 d G . P C -3 H40 H 0.5787 0.5641 0.1232 0.050 Uiso 0.25 1 d G U P C -3 C41 C 0.7149(8) 0.6197(8) 0.2084(8) 0.033(2) Uiso 0.25 1 d G . P C -3 H41 H 0.7408 0.5378 0.2251 0.040 Uiso 0.25 1 d G U P C -3 C42 C 0.7732(5) 0.7239(8) 0.2444(6) 0.028(3) Uiso 0.25 1 d G . P C -3 H42 H 0.8390 0.7132 0.2858 0.034 Uiso 0.25 1 d G U P C -3 C43 C 0.7353(8) 0.8437(7) 0.2199(9) 0.035(2) Uiso 0.25 1 d G . P C -3 H43 H 0.7752 0.9149 0.2445 0.042 Uiso 0.25 1 d G U P C -3 C44 C 0.6391(9) 0.8593(12) 0.1593(9) 0.094(10) Uiso 0.25 1 d G . P C -3 H44 H 0.6132 0.9412 0.1426 0.112 Uiso 0.25 1 d G U P C -3 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 I1 0.01243(5) 0.01573(5) 0.01336(5) -0.00206(4) 0.00325(4) -0.00011(4) I2 0.00819(6) 0.01357(7) 0.01274(7) 0.000 0.00291(5) 0.000 I3 0.02008(9) 0.02997(11) 0.02562(10) 0.000 0.01572(8) 0.000 N1 0.0136(6) 0.0132(6) 0.0099(6) -0.0023(5) 0.0049(5) 0.0008(5) N2 0.0088(8) 0.0272(12) 0.0063(8) 0.000 0.0008(6) 0.000 N3 0.0064(7) 0.0161(9) 0.0075(8) 0.000 0.0013(6) 0.000 C1 0.0102(6) 0.0133(7) 0.0079(6) -0.0011(5) 0.0035(5) 0.0006(5) C2 0.0103(6) 0.0141(7) 0.0096(6) -0.0033(5) 0.0034(5) -0.0016(5) C3 0.0115(7) 0.0172(8) 0.0075(6) -0.0017(6) 0.0022(5) -0.0015(6) C4 0.0098(6) 0.0207(9) 0.0096(7) -0.0026(6) 0.0017(5) -0.0021(6) C5 0.0092(9) 0.0216(12) 0.0086(9) 0.000 0.0005(7) 0.000 C6 0.0072(9) 0.0232(13) 0.0116(10) 0.000 0.0006(7) 0.000 C7 0.0082(6) 0.0237(9) 0.0134(7) -0.0008(7) 0.0026(5) -0.0037(6) C8 0.0083(6) 0.0247(9) 0.0136(7) -0.0014(7) 0.0045(5) -0.0029(6) C9 0.0093(6) 0.0229(9) 0.0140(7) 0.0007(7) 0.0053(6) -0.0032(6) C10 0.0092(6) 0.0243(9) 0.0125(7) 0.0009(6) 0.0056(5) -0.0012(6) C11 0.0099(6) 0.0237(9) 0.0117(7) 0.0030(6) 0.0057(5) -0.0018(6) C12 0.0106(6) 0.0217(8) 0.0087(6) 0.0019(6) 0.0046(5) 0.0000(6) C13 0.0092(6) 0.0190(8) 0.0085(6) 0.0032(6) 0.0032(5) 0.0001(6) C14 0.0082(9) 0.0179(11) 0.0080(9) 0.000 0.0029(7) 0.000 C15 0.0064(8) 0.0138(10) 0.0071(8) 0.000 0.0017(6) 0.000 C16 0.0082(6) 0.0114(7) 0.0089(6) 0.0005(5) 0.0030(5) 0.0008(5) C17 0.0080(6) 0.0099(6) 0.0086(6) 0.0003(5) 0.0031(5) 0.0000(5) C18 0.0095(6) 0.0109(6) 0.0087(6) -0.0010(5) 0.0034(5) 0.0005(5) C19 0.0112(6) 0.0102(7) 0.0118(7) -0.0010(5) 0.0040(5) 0.0005(5) C20 0.0124(7) 0.0111(7) 0.0113(7) -0.0028(5) 0.0040(5) -0.0023(5) C21 0.0131(7) 0.0124(7) 0.0141(7) -0.0042(6) 0.0043(6) -0.0047(6) C22 0.0112(7) 0.0170(8) 0.0115(7) -0.0037(6) 0.0026(5) -0.0044(6) C23 0.0098(6) 0.0200(9) 0.0135(7) -0.0022(6) 0.0023(5) -0.0048(6) C24 0.0116(7) 0.0168(8) 0.0174(8) -0.0008(6) 0.0051(6) -0.0057(6) C25 0.0112(7) 0.0194(8) 0.0160(8) 0.0014(7) 0.0053(6) -0.0055(6) C26 0.0112(7) 0.0194(8) 0.0142(7) 0.0034(6) 0.0055(6) -0.0031(6) C27 0.0127(7) 0.0139(7) 0.0144(7) 0.0039(6) 0.0051(6) -0.0016(6) C28 0.0100(6) 0.0153(7) 0.0109(7) 0.0037(6) 0.0038(5) -0.0001(6) C29 0.0097(6) 0.0113(7) 0.0113(7) 0.0032(5) 0.0037(5) 0.0012(5) C30 0.0122(7) 0.0096(6) 0.0135(7) 0.0006(5) 0.0051(5) 0.0001(5) C31 0.0139(7) 0.0099(7) 0.0151(7) 0.0012(6) 0.0050(6) -0.0017(6) C32 0.0132(7) 0.0125(7) 0.0167(8) -0.0018(6) 0.0050(6) -0.0043(6) C33 0.0191(8) 0.0222(9) 0.0097(7) -0.0023(6) 0.0067(6) -0.0005(7) C34 0.0128(7) 0.0191(8) 0.0155(8) -0.0008(6) 0.0075(6) 0.0005(6) C35 0.0094(6) 0.0214(9) 0.0111(7) -0.0049(6) 0.0025(5) -0.0030(6) C36 0.0107(7) 0.0296(11) 0.0101(7) -0.0069(7) 0.0028(5) -0.0023(7) S1 0.0162(7) 0.0717(16) 0.0204(7) 0.000 0.0138(6) 0.000 S2 0.075(3) 0.0320(16) 0.097(3) -0.0149(19) 0.076(3) -0.0196(17) S3 0.0219(9) 0.080(2) 0.0146(8) 0.000 0.0070(7) 0.000 S4 0.042(2) 0.107(4) 0.0386(19) -0.022(2) 0.0307(18) -0.029(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 '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' I I -0.3071 2.1212 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0076 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1430 0.1480 '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 C34 N1 C33 109.83(16) . . C34 N1 C1 110.51(15) . . C33 N1 C1 109.66(15) . . C36 N2 C36 108.9(2) . 4_575 C36 N2 C14 109.79(14) . . C36 N2 C14 109.79(14) 4_575 . C35 N3 C35 109.0(2) . 4_575 C35 N3 C15 109.95(13) . . C35 N3 C15 109.95(13) 4_575 . N1 C1 C18 109.97(14) . . N1 C1 C2 110.83(14) . . C18 C1 C2 99.86(15) . . N1 C1 C1 107.78(10) . 4_575 C18 C1 C1 114.06(10) . 4_575 C2 C1 C1 114.20(10) . 4_575 C3 C2 C20 119.00(17) . . C3 C2 C1 124.33(18) . . C20 C2 C1 110.05(15) . . C2 C3 C4 120.53(18) . . C2 C3 C3 120.50(12) . 4_575 C4 C3 C3 107.39(12) . 4_575 C22 C4 C5 119.98(19) . . C22 C4 C3 120.33(18) . . C5 C4 C3 108.22(19) . . C6 C5 C4 120.12(15) . . C6 C5 C4 120.12(15) . 4_575 C4 C5 C4 108.8(2) . 4_575 C5 C6 C7 119.96(15) . . C5 C6 C7 119.96(15) . 4_575 C7 C6 C7 108.3(3) . 4_575 C23 C7 C6 119.9(2) . . C23 C7 C8 120.50(19) . . C6 C7 C8 107.9(2) . . C9 C8 C7 119.8(2) . . C9 C8 C8 119.92(13) . 4_575 C7 C8 C8 107.99(13) . 4_575 C8 C9 C10 119.9(2) . . C8 C9 C25 120.05(19) . . C10 C9 C25 107.95(17) . . C10 C10 C9 120.17(12) 4_575 . C10 C10 C11 120.19(12) 4_575 . C9 C10 C11 107.61(19) . . C12 C11 C26 119.48(18) . . C12 C11 C10 119.8(2) . . C26 C11 C10 108.55(17) . . C11 C12 C13 121.00(19) . . C11 C12 C12 119.99(12) . 4_575 C13 C12 C12 108.34(12) . 4_575 C28 C13 C12 119.24(17) . . C28 C13 C14 124.58(17) . . C12 C13 C14 109.94(18) . . N2 C14 C13 109.79(15) . . N2 C14 C13 109.80(15) . 4_575 C13 C14 C13 100.0(2) . 4_575 N2 C14 C15 109.2(2) . . C13 C14 C15 113.88(14) . . C13 C14 C15 113.88(14) 4_575 . N3 C15 C16 110.32(14) . . N3 C15 C16 110.32(14) . 4_575 C16 C15 C16 99.90(19) . 4_575 N3 C15 C14 107.56(19) . . C16 C15 C14 114.31(13) . . C16 C15 C14 114.31(13) 4_575 . C29 C16 C17 119.45(16) . . C29 C16 C15 123.99(17) . . C17 C16 C15 110.41(15) . . C18 C17 C16 121.57(16) . . C18 C17 C17 120.48(10) . 4_575 C16 C17 C17 107.87(10) . 4_575 C17 C18 C19 118.53(16) . . C17 C18 C1 124.52(16) . . C19 C18 C1 110.24(15) . . C30 C19 C18 120.56(17) . . C30 C19 C20 120.09(17) . . C18 C19 C20 108.70(16) . . C21 C20 C2 121.47(18) . . C21 C20 C19 119.74(18) . . C2 C20 C19 107.79(16) . . C20 C21 C22 119.29(18) . . C20 C21 C32 120.32(17) . . C22 C21 C32 107.97(17) . . C4 C22 C21 119.32(18) . . C4 C22 C23 119.83(19) . . C21 C22 C23 108.38(18) . . C7 C23 C24 119.79(19) . . C7 C23 C22 120.2(2) . . C24 C23 C22 107.77(18) . . C25 C24 C32 120.23(18) . . C25 C24 C23 119.9(2) . . C32 C24 C23 107.78(18) . . C24 C25 C26 119.77(19) . . C24 C25 C9 119.95(19) . . C26 C25 C9 107.95(19) . . C27 C26 C11 119.46(18) . . C27 C26 C25 119.92(19) . . C11 C26 C25 107.95(18) . . C26 C27 C31 119.99(18) . . C26 C27 C28 119.92(19) . . C31 C27 C28 108.52(17) . . C13 C28 C27 120.84(18) . . C13 C28 C29 120.07(17) . . C27 C28 C29 107.18(16) . . C16 C29 C30 120.17(17) . . C16 C29 C28 120.95(17) . . C30 C29 C28 107.75(16) . . C19 C30 C29 119.56(17) . . C19 C30 C31 119.97(17) . . C29 C30 C31 108.66(16) . . C32 C31 C27 120.47(19) . . C32 C31 C30 120.01(18) . . C27 C31 C30 107.89(16) . . C31 C32 C24 119.62(19) . . C31 C32 C21 119.87(18) . . C24 C32 C21 108.11(18) . . N1 C33 C33 109.44(11) . 4_575 N1 C33 H33A 109.8 . . C33 C33 H33A 109.8 4_575 . N1 C33 H33B 109.8 . . C33 C33 H33B 109.8 4_575 . H33A C33 H33B 108.2 . . N1 C34 C34 109.57(11) . 4_575 N1 C34 H34A 109.8 . . C34 C34 H34A 109.8 4_575 . N1 C34 H34B 109.8 . . C34 C34 H34B 109.8 4_575 . H34A C34 H34B 108.2 . . N3 C35 C36 109.27(17) . . N3 C35 H35A 109.8 . . C36 C35 H35A 109.8 . . N3 C35 H35B 109.8 . . C36 C35 H35B 109.8 . . H35A C35 H35B 108.3 . . N2 C36 C35 110.51(18) . . N2 C36 H36A 109.5 . . C35 C36 H36A 109.5 . . N2 C36 H36B 109.5 . . C35 C36 H36B 109.5 . . H36A C36 H36B 108.1 . . S1 C37 S2 178.3(8) . . C37 S1 C37 157.3(8) 4_565 . C38 C38 S4 110.4(5) 4_575 . C38 C38 S3 61.1(4) 4_575 . S4 C38 S3 170.9(9) . . C38 S3 C38 57.8(8) 4_575 . C40 C39 C44 120.0 . . C40 C39 H39 120.0 . . C44 C39 H39 120.0 . . C41 C40 C39 120.0 . . C41 C40 H40 120.0 . . C39 C40 H40 120.0 . . C40 C41 C42 120.0 . . C40 C41 H41 120.0 . . C42 C41 H41 120.0 . . C43 C42 C41 120.0 . . C43 C42 H42 120.0 . . C41 C42 H42 120.0 . . C44 C43 C42 120.0 . . C44 C43 H43 120.0 . . C42 C43 H43 120.0 . . C43 C44 C39 120.0 . . C43 C44 H44 120.0 . . C39 C44 H44 120.0 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 I1 I1 2.7363(3) 4_585 I2 I3 2.7766(3) . N1 C34 1.469(3) . N1 C33 1.476(3) . N1 C1 1.504(2) . N2 C36 1.474(3) . N2 C36 1.474(3) 4_575 N2 C14 1.481(3) . N3 C35 1.484(2) . N3 C35 1.484(2) 4_575 N3 C15 1.511(3) . C1 C18 1.532(3) . C1 C2 1.537(3) . C1 C1 1.615(4) 4_575 C2 C3 1.371(3) . C2 C20 1.440(3) . C3 C4 1.452(3) . C3 C3 1.484(4) 4_575 C4 C22 1.395(3) . C4 C5 1.446(3) . C5 C6 1.399(4) . C5 C4 1.446(3) 4_575 C6 C7 1.450(3) . C6 C7 1.450(3) 4_575 C7 C23 1.390(3) . C7 C8 1.450(3) . C8 C9 1.394(3) . C8 C8 1.454(5) 4_575 C9 C10 1.450(3) . C9 C25 1.453(3) . C10 C10 1.387(5) 4_575 C10 C11 1.454(3) . C11 C12 1.400(3) . C11 C26 1.438(3) . C12 C13 1.437(3) . C12 C12 1.449(4) 4_575 C13 C28 1.369(3) . C13 C14 1.536(3) . C14 C13 1.536(3) 4_575 C14 C15 1.620(4) . C15 C16 1.531(2) . C15 C16 1.531(2) 4_575 C16 C29 1.374(3) . C16 C17 1.432(2) . C17 C18 1.380(2) . C17 C17 1.465(4) 4_575 C18 C19 1.428(3) . C19 C30 1.398(3) . C19 C20 1.451(3) . C20 C21 1.395(3) . C21 C22 1.441(3) . C21 C32 1.454(3) . C22 C23 1.455(3) . C23 C24 1.454(3) . C24 C25 1.397(3) . C24 C32 1.453(3) . C25 C26 1.453(3) . C26 C27 1.397(3) . C27 C31 1.446(3) . C27 C28 1.449(3) . C28 C29 1.479(3) . C29 C30 1.433(3) . C30 C31 1.454(3) . C31 C32 1.392(3) . C33 C33 1.551(5) 4_575 C33 H33A 0.9900 . C33 H33B 0.9900 . C34 C34 1.549(4) 4_575 C34 H34A 0.9900 . C34 H34B 0.9900 . C35 C36 1.556(3) . C35 H35A 0.9900 . C35 H35B 0.9900 . C36 H36A 0.9900 . C36 H36B 0.9900 . C37 S1 1.390(8) . C37 S2 1.518(9) . S1 C37 1.390(8) 4_565 C38 C38 1.56(2) 4_575 C38 S4 1.598(10) . C38 S3 1.618(9) . S3 C38 1.618(9) 4_575 C39 C40 1.3900 . C39 C44 1.3900 . C39 H39 0.9500 . C40 C41 1.3900 . C40 H40 0.9500 . C41 C42 1.3900 . C41 H41 0.9500 . C42 C43 1.3900 . C42 H42 0.9500 . C43 C44 1.3900 . C43 H43 0.9500 . C44 H44 0.9500 . 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_4 C34 N1 C1 C18 64.6(2) . . C33 N1 C1 C18 -174.16(16) . . C34 N1 C1 C2 174.08(16) . . C33 N1 C1 C2 -64.7(2) . . C34 N1 C1 C1 -60.28(15) . 4_575 C33 N1 C1 C1 60.94(15) . 4_575 N1 C1 C2 C3 110.7(2) . . C18 C1 C2 C3 -133.42(19) . . C1 C1 C2 C3 -11.3(2) 4_575 . N1 C1 C2 C20 -98.40(18) . . C18 C1 C2 C20 17.51(19) . . C1 C1 C2 C20 139.65(12) 4_575 . C20 C2 C3 C4 2.0(3) . . C1 C2 C3 C4 150.55(18) . . C20 C2 C3 C3 -136.59(13) . 4_575 C1 C2 C3 C3 12.0(2) . 4_575 C2 C3 C4 C22 0.1(3) . . C3 C3 C4 C22 143.46(16) 4_575 . C2 C3 C4 C5 -143.2(2) . . C3 C3 C4 C5 0.12(17) 4_575 . C22 C4 C5 C6 0.4(3) . . C3 C4 C5 C6 143.9(2) . . C22 C4 C5 C4 -143.69(16) . 4_575 C3 C4 C5 C4 -0.2(3) . 4_575 C4 C5 C6 C7 -0.7(3) . . C4 C5 C6 C7 139.3(2) 4_575 . C4 C5 C6 C7 -139.3(2) . 4_575 C4 C5 C6 C7 0.7(3) 4_575 4_575 C5 C6 C7 C23 0.5(3) . . C7 C6 C7 C23 143.41(17) 4_575 . C5 C6 C7 C8 -142.6(2) . . C7 C6 C7 C8 0.3(3) 4_575 . C23 C7 C8 C9 -0.8(3) . . C6 C7 C8 C9 142.0(2) . . C23 C7 C8 C8 -143.04(16) . 4_575 C6 C7 C8 C8 -0.16(17) . 4_575 C7 C8 C9 C10 -137.4(2) . . C8 C8 C9 C10 0.3(2) 4_575 . C7 C8 C9 C25 0.6(3) . . C8 C8 C9 C25 138.33(15) 4_575 . C8 C9 C10 C10 -0.3(2) . 4_575 C25 C9 C10 C10 -142.83(12) . 4_575 C8 C9 C10 C11 142.32(19) . . C25 C9 C10 C11 -0.2(2) . . C10 C10 C11 C12 0.7(2) 4_575 . C9 C10 C11 C12 -141.96(19) . . C10 C10 C11 C26 142.89(12) 4_575 . C9 C10 C11 C26 0.3(2) . . C26 C11 C12 C13 1.6(3) . . C10 C11 C12 C13 139.77(19) . . C26 C11 C12 C12 -138.82(15) . 4_575 C10 C11 C12 C12 -0.7(2) . 4_575 C11 C12 C13 C28 -2.7(3) . . C12 C12 C13 C28 141.75(15) 4_575 . C11 C12 C13 C14 -156.23(19) . . C12 C12 C13 C14 -11.78(16) 4_575 . C36 N2 C14 C13 174.65(17) . . C36 N2 C14 C13 -65.6(2) 4_575 . C36 N2 C14 C13 65.6(2) . 4_575 C36 N2 C14 C13 -174.65(17) 4_575 4_575 C36 N2 C14 C15 -59.87(15) . . C36 N2 C14 C15 59.87(15) 4_575 . C28 C13 C14 N2 110.3(2) . . C12 C13 C14 N2 -97.86(19) . . C28 C13 C14 C13 -134.26(16) . 4_575 C12 C13 C14 C13 17.6(2) . 4_575 C28 C13 C14 C15 -12.4(3) . . C12 C13 C14 C15 139.41(16) . . C35 N3 C15 C16 -174.73(16) . . C35 N3 C15 C16 65.3(2) 4_575 . C35 N3 C15 C16 -65.3(2) . 4_575 C35 N3 C15 C16 174.73(16) 4_575 4_575 C35 N3 C15 C14 59.99(14) . . C35 N3 C15 C14 -59.99(14) 4_575 . N2 C14 C15 N3 0.000(1) . . C13 C14 C15 N3 123.08(14) . . C13 C14 C15 N3 -123.08(14) 4_575 . N2 C14 C15 C16 -122.86(14) . . C13 C14 C15 C16 0.2(2) . . C13 C14 C15 C16 114.05(16) 4_575 . N2 C14 C15 C16 122.87(14) . 4_575 C13 C14 C15 C16 -114.05(16) . 4_575 C13 C14 C15 C16 -0.2(2) 4_575 4_575 N3 C15 C16 C29 -109.7(2) . . C16 C15 C16 C29 134.16(15) 4_575 . C14 C15 C16 C29 11.7(3) . . N3 C15 C16 C17 98.22(17) . . C16 C15 C16 C17 -17.9(2) 4_575 . C14 C15 C16 C17 -140.43(16) . . C29 C16 C17 C18 3.9(3) . . C15 C16 C17 C18 157.45(17) . . C29 C16 C17 C17 -141.52(14) . 4_575 C15 C16 C17 C17 12.00(16) . 4_575 C16 C17 C18 C19 -4.5(3) . . C17 C17 C18 C19 136.68(13) 4_575 . C16 C17 C18 C1 -152.96(17) . . C17 C17 C18 C1 -11.7(2) 4_575 . N1 C1 C18 C17 -110.13(19) . . C2 C1 C18 C17 133.31(18) . . C1 C1 C18 C17 11.1(2) 4_575 . N1 C1 C18 C19 99.23(17) . . C2 C1 C18 C19 -17.34(18) . . C1 C1 C18 C19 -139.57(11) 4_575 . C17 C18 C19 C30 3.4(3) . . C1 C18 C19 C30 156.02(17) . . C17 C18 C19 C20 -141.15(17) . . C1 C18 C19 C20 11.5(2) . . C3 C2 C20 C21 -3.1(3) . . C1 C2 C20 C21 -155.75(17) . . C3 C2 C20 C19 140.75(18) . . C1 C2 C20 C19 -11.9(2) . . C30 C19 C20 C21 0.1(3) . . C18 C19 C20 C21 144.87(18) . . C30 C19 C20 C2 -144.42(18) . . C18 C19 C20 C2 0.3(2) . . C2 C20 C21 C22 1.9(3) . . C19 C20 C21 C22 -137.76(19) . . C2 C20 C21 C32 139.4(2) . . C19 C20 C21 C32 -0.2(3) . . C5 C4 C22 C21 137.8(2) . . C3 C4 C22 C21 -1.3(3) . . C5 C4 C22 C23 0.1(3) . . C3 C4 C22 C23 -138.94(19) . . C20 C21 C22 C4 0.3(3) . . C32 C21 C22 C4 -141.92(19) . . C20 C21 C22 C23 142.28(19) . . C32 C21 C22 C23 0.1(2) . . C6 C7 C23 C24 -137.8(2) . . C8 C7 C23 C24 0.8(3) . . C6 C7 C23 C22 0.0(3) . . C8 C7 C23 C22 138.5(2) . . C4 C22 C23 C7 -0.4(3) . . C21 C22 C23 C7 -142.10(19) . . C4 C22 C23 C24 141.88(19) . . C21 C22 C23 C24 0.1(2) . . C7 C23 C24 C25 -0.5(3) . . C22 C23 C24 C25 -142.88(19) . . C7 C23 C24 C32 142.17(19) . . C22 C23 C24 C32 -0.3(2) . . C32 C24 C25 C26 -0.1(3) . . C23 C24 C25 C26 137.9(2) . . C32 C24 C25 C9 -137.8(2) . . C23 C24 C25 C9 0.2(3) . . C8 C9 C25 C24 -0.3(3) . . C10 C9 C25 C24 142.16(19) . . C8 C9 C25 C26 -142.41(19) . . C10 C9 C25 C26 0.1(2) . . C12 C11 C26 C27 0.4(3) . . C10 C11 C26 C27 -141.98(19) . . C12 C11 C26 C25 142.14(19) . . C10 C11 C26 C25 -0.2(2) . . C24 C25 C26 C27 -0.5(3) . . C9 C25 C26 C27 141.6(2) . . C24 C25 C26 C11 -142.1(2) . . C9 C25 C26 C11 0.1(2) . . C11 C26 C27 C31 137.7(2) . . C25 C26 C27 C31 0.6(3) . . C11 C26 C27 C28 -1.3(3) . . C25 C26 C27 C28 -138.5(2) . . C12 C13 C28 C27 1.8(3) . . C14 C13 C28 C27 151.18(19) . . C12 C13 C28 C29 -136.22(18) . . C14 C13 C28 C29 13.2(3) . . C26 C27 C28 C13 0.2(3) . . C31 C27 C28 C13 -143.03(18) . . C26 C27 C28 C29 142.89(18) . . C31 C27 C28 C29 -0.3(2) . . C17 C16 C29 C30 -2.0(3) . . C15 C16 C29 C30 -151.77(18) . . C17 C16 C29 C28 137.41(18) . . C15 C16 C29 C28 -12.3(3) . . C13 C28 C29 C16 -0.4(3) . . C27 C28 C29 C16 -143.44(18) . . C13 C28 C29 C30 143.42(18) . . C27 C28 C29 C30 0.4(2) . . C18 C19 C30 C29 -1.6(3) . . C20 C19 C30 C29 138.96(19) . . C18 C19 C30 C31 -140.36(19) . . C20 C19 C30 C31 0.2(3) . . C16 C29 C30 C19 1.0(3) . . C28 C29 C30 C19 -143.20(18) . . C16 C29 C30 C31 143.87(18) . . C28 C29 C30 C31 -0.3(2) . . C26 C27 C31 C32 0.1(3) . . C28 C27 C31 C32 143.26(19) . . C26 C27 C31 C30 -143.04(19) . . C28 C27 C31 C30 0.2(2) . . C19 C30 C31 C32 -0.5(3) . . C29 C30 C31 C32 -143.21(19) . . C19 C30 C31 C27 142.82(18) . . C29 C30 C31 C27 0.1(2) . . C27 C31 C32 C24 -0.7(3) . . C30 C31 C32 C24 138.0(2) . . C27 C31 C32 C21 -138.3(2) . . C30 C31 C32 C21 0.4(3) . . C25 C24 C32 C31 0.7(3) . . C23 C24 C32 C31 -141.76(19) . . C25 C24 C32 C21 142.8(2) . . C23 C24 C32 C21 0.3(2) . . C20 C21 C32 C31 0.0(3) . . C22 C21 C32 C31 141.73(19) . . C20 C21 C32 C24 -141.98(19) . . C22 C21 C32 C24 -0.2(2) . . C34 N1 C33 C33 59.67(15) . 4_575 C1 N1 C33 C33 -61.96(14) . 4_575 C33 N1 C34 C34 -59.75(15) . 4_575 C1 N1 C34 C34 61.37(14) . 4_575 C35 N3 C35 C36 60.0(2) 4_575 . C15 N3 C35 C36 -60.6(2) . . C36 N2 C36 C35 -59.1(3) 4_575 . C14 N2 C36 C35 61.2(2) . . N3 C35 C36 N2 -0.3(2) . . C44 C39 C40 C41 0.0 . . C39 C40 C41 C42 0.0 . . C40 C41 C42 C43 0.0 . . C41 C42 C43 C44 0.0 . . C42 C43 C44 C39 0.0 . . C40 C39 C44 C43 0.0 . .