# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_3b _database_code_depnum_ccdc_archive 'CCDC 859837' #TrackingRef '3b.cif' #============================================================================= # start Validation Reply Form _vrf_PLAT220_3b ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.7 Ratio RESPONSE: One methylbenzene terminal moiety (belonging to the large fused substituent group attached to the porphyrin core) is severely affected by thermal disorder which is translated into large Ueq values for a number of carbon atoms, namely C57, C60 and C62, hence giving rise to this alert. ; _vrf_PLAT241_3b ; PROBLEM: Check High Ueq as Compared to Neighbors for C62 RESPONSE: Please see our response to _vrf_PLAT220_3b. ; _vrf_PLAT242_3b ; PROBLEM: Check High Ueq as Compared to Neighbors for C57 RESPONSE: Please see our response to _vrf_PLAT220_3b. ; # end Validation Reply Form #============================================================================= # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '22 December 2011' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H45 N5' _chemical_formula_sum 'C63 H45 N5' _chemical_formula_weight 872.04 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' #============================================================================== # CRYSTAL DATA #============================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4707(7) _cell_length_b 13.9517(11) _cell_length_c 17.6764(11) _cell_angle_alpha 82.155(3) _cell_angle_beta 83.403(3) _cell_angle_gamma 78.502(4) _cell_volume 2258.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2299 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 23.32 _exptl_crystal_description Needle _exptl_crystal_colour Violet _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9918 _exptl_absorpt_correction_T_max 0.9977 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; #============================================================================== # EXPERIMENTAL DATA #============================================================================== _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Kappa CCD APEX II' _diffrn_measurement_method '\w / \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 31489 _diffrn_reflns_av_R_equivalents 0.1052 _diffrn_reflns_av_sigmaI/netI 0.1393 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8173 _reflns_number_gt 4221 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'SAINT+ (Bruker, 2005)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' #============================================================================== # REFINEMENT DATA #============================================================================== _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.2702P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8173 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1661 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1656 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.6860(3) 0.7411(2) 0.92069(14) 0.0231(7) Uani 1 1 d . . . H1 H 0.7047 0.6765 0.9300 0.028 Uiso 1 1 calc R . . N2 N 0.8129(3) 0.5995(2) 1.04154(14) 0.0231(7) Uani 1 1 d . . . N3 N 0.6156(3) 0.5813(2) 0.85295(14) 0.0214(7) Uani 1 1 d . . . N4 N 0.7110(3) 0.4421(2) 0.98553(14) 0.0242(7) Uani 1 1 d . . . H4 H 0.7207 0.5027 0.9676 0.029 Uiso 1 1 calc R . . N5 N 0.5574(3) 0.7052(2) 0.48548(15) 0.0297(8) Uani 1 1 d . . . C1 C 0.6184(4) 0.7937(2) 0.85919(18) 0.0216(8) Uani 1 1 d . . . C2 C 0.6037(4) 0.8952(3) 0.86839(18) 0.0250(9) Uani 1 1 d . . . H2 H 0.5580 0.9490 0.8353 0.030 Uiso 1 1 calc R . . C3 C 0.6654(4) 0.9021(3) 0.93203(19) 0.0273(9) Uani 1 1 d . . . H3 H 0.6716 0.9614 0.9512 0.033 Uiso 1 1 calc R . . C4 C 0.7197(4) 0.8049(2) 0.96541(17) 0.0200(8) Uani 1 1 d . . . C5 C 0.8048(4) 0.7786(3) 1.02751(18) 0.0227(8) Uani 1 1 d . . . C6 C 0.8549(4) 0.6815(3) 1.05948(17) 0.0234(9) Uani 1 1 d . . . C7 C 0.9473(4) 0.6541(3) 1.12173(19) 0.0275(9) Uani 1 1 d . . . H7 H 0.9922 0.6970 1.1443 0.033 Uiso 1 1 calc R . . C8 C 0.9575(4) 0.5560(3) 1.14160(19) 0.0275(9) Uani 1 1 d . . . H8 H 1.0128 0.5166 1.1800 0.033 Uiso 1 1 calc R . . C9 C 0.8681(4) 0.5222(3) 1.09319(18) 0.0229(8) Uani 1 1 d . . . C10 C 0.8354(4) 0.4275(2) 1.10283(18) 0.0212(8) Uani 1 1 d . . . C11 C 0.7551(4) 0.3931(3) 1.05382(17) 0.0219(8) Uani 1 1 d . . . C12 C 0.7113(4) 0.2995(3) 1.06327(18) 0.0222(8) Uani 1 1 d . . . H12 H 0.7247 0.2508 1.1063 0.027 Uiso 1 1 calc R . . C13 C 0.6473(4) 0.2928(3) 0.99999(18) 0.0233(8) Uani 1 1 d . . . H13 H 0.6078 0.2385 0.9907 0.028 Uiso 1 1 calc R . . C14 C 0.6498(4) 0.3820(2) 0.94974(18) 0.0211(8) Uani 1 1 d . . . C15 C 0.6055(4) 0.4035(3) 0.87570(18) 0.0219(8) Uani 1 1 d . . . C16 C 0.6000(4) 0.4948(3) 0.83012(18) 0.0210(8) Uani 1 1 d . . . C17 C 0.5763(4) 0.5106(3) 0.74973(18) 0.0236(8) Uani 1 1 d . . . H17 H 0.5639 0.4620 0.7196 0.028 Uiso 1 1 calc R . . C18 C 0.5749(4) 0.6073(3) 0.72493(18) 0.0228(8) Uani 1 1 d . . . C19 C 0.5943(4) 0.6531(3) 0.79179(17) 0.0207(8) Uani 1 1 d . . . C20 C 0.5817(3) 0.7539(3) 0.79683(18) 0.0213(8) Uani 1 1 d . . . C21 C 0.8466(4) 0.8596(3) 1.06160(18) 0.0255(9) Uani 1 1 d . . . C22 C 0.9898(4) 0.8696(3) 1.0584(2) 0.0323(10) Uani 1 1 d . . . H22 H 1.0629 0.8252 1.0327 0.039 Uiso 1 1 calc R . . C23 C 1.0275(5) 0.9440(3) 1.0925(2) 0.0444(12) Uani 1 1 d . . . H23 H 1.1263 0.9497 1.0903 0.053 Uiso 1 1 calc R . . C24 C 0.9240(5) 1.0088(3) 1.1289(2) 0.0493(12) Uani 1 1 d . . . H24 H 0.9505 1.0592 1.1522 0.059 Uiso 1 1 calc R . . C25 C 0.7819(5) 1.0012(3) 1.1317(2) 0.0451(11) Uani 1 1 d . . . H25 H 0.7098 1.0467 1.1568 0.054 Uiso 1 1 calc R . . C26 C 0.7422(4) 0.9275(3) 1.0982(2) 0.0350(10) Uani 1 1 d . . . H26 H 0.6430 0.9233 1.1002 0.042 Uiso 1 1 calc R . . C27 C 0.8885(4) 0.3590(3) 1.17013(18) 0.0237(8) Uani 1 1 d . . . C28 C 0.9785(4) 0.2701(3) 1.1601(2) 0.0275(9) Uani 1 1 d . . . H28 H 1.0062 0.2523 1.1098 0.033 Uiso 1 1 calc R . . C29 C 1.0291(4) 0.2061(3) 1.2227(2) 0.0325(10) Uani 1 1 d . . . H29 H 1.0906 0.1449 1.2150 0.039 Uiso 1 1 calc R . . C30 C 0.9906(4) 0.2311(3) 1.2953(2) 0.0334(10) Uani 1 1 d . . . H30 H 1.0264 0.1874 1.3378 0.040 Uiso 1 1 calc R . . C31 C 0.9013(4) 0.3184(3) 1.3072(2) 0.0343(10) Uani 1 1 d . . . H31 H 0.8745 0.3352 1.3579 0.041 Uiso 1 1 calc R . . C32 C 0.8493(4) 0.3832(3) 1.24456(18) 0.0291(9) Uani 1 1 d . . . H32 H 0.7869 0.4439 1.2528 0.035 Uiso 1 1 calc R . . C33 C 0.5653(4) 0.3226(3) 0.84014(18) 0.0231(8) Uani 1 1 d . . . C34 C 0.6623(4) 0.2340(3) 0.83339(19) 0.0309(9) Uani 1 1 d . . . H34 H 0.7535 0.2237 0.8537 0.037 Uiso 1 1 calc R . . C35 C 0.6273(4) 0.1611(3) 0.7975(2) 0.0324(10) Uani 1 1 d . . . H35 H 0.6946 0.1012 0.7936 0.039 Uiso 1 1 calc R . . C36 C 0.4965(5) 0.1740(3) 0.7674(2) 0.0366(10) Uani 1 1 d . . . H36 H 0.4736 0.1238 0.7422 0.044 Uiso 1 1 calc R . . C37 C 0.3991(4) 0.2605(3) 0.77436(19) 0.0335(10) Uani 1 1 d . . . H37 H 0.3080 0.2698 0.7541 0.040 Uiso 1 1 calc R . . C38 C 0.4323(4) 0.3338(3) 0.81033(18) 0.0277(9) Uani 1 1 d . . . H38 H 0.3635 0.3929 0.8148 0.033 Uiso 1 1 calc R . . C39 C 0.5212(4) 0.8270(2) 0.73234(18) 0.0217(8) Uani 1 1 d . . . C40 C 0.3851(4) 0.8254(3) 0.71030(19) 0.0275(9) Uani 1 1 d . . . H40 H 0.3290 0.7803 0.7376 0.033 Uiso 1 1 calc R . . C41 C 0.3314(4) 0.8892(3) 0.6489(2) 0.0361(10) Uani 1 1 d . . . H41 H 0.2392 0.8867 0.6339 0.043 Uiso 1 1 calc R . . C42 C 0.4098(4) 0.9561(3) 0.6093(2) 0.0403(11) Uani 1 1 d . . . H42 H 0.3720 0.9996 0.5672 0.048 Uiso 1 1 calc R . . C43 C 0.5446(4) 0.9599(3) 0.6314(2) 0.0369(10) Uani 1 1 d . . . H43 H 0.5991 1.0063 0.6046 0.044 Uiso 1 1 calc R . . C44 C 0.5988(4) 0.8959(3) 0.69226(19) 0.0276(9) Uani 1 1 d . . . H44 H 0.6909 0.8989 0.7072 0.033 Uiso 1 1 calc R . . C45 C 0.5680(4) 0.6462(3) 0.64290(18) 0.0240(9) Uani 1 1 d . . . C46 C 0.4643(4) 0.6227(3) 0.60273(19) 0.0259(9) Uani 1 1 d . . . H46 H 0.3951 0.5860 0.6287 0.031 Uiso 1 1 calc R . . C47 C 0.4616(4) 0.6529(3) 0.52426(19) 0.0258(9) Uani 1 1 d . . . C49 C 0.6597(4) 0.7271(3) 0.52373(19) 0.0271(9) Uani 1 1 d . . . C50 C 0.6674(4) 0.6984(3) 0.60258(19) 0.0261(9) Uani 1 1 d . . . H50 H 0.7408 0.7148 0.6281 0.031 Uiso 1 1 calc R . . C51 C 0.3529(4) 0.6290(3) 0.47915(19) 0.0274(9) Uani 1 1 d . . . C52 C 0.2818(4) 0.5500(3) 0.5048(2) 0.0306(9) Uani 1 1 d . . . H52 H 0.3026 0.5109 0.5519 0.037 Uiso 1 1 calc R . . C53 C 0.1809(4) 0.5286(3) 0.4615(2) 0.0357(10) Uani 1 1 d . . . H53 H 0.1341 0.4745 0.4792 0.043 Uiso 1 1 calc R . . C54 C 0.1475(4) 0.5851(3) 0.3929(2) 0.0353(10) Uani 1 1 d . . . C55 C 0.2178(4) 0.6623(3) 0.3682(2) 0.0397(11) Uani 1 1 d . . . H55 H 0.1961 0.7016 0.3213 0.048 Uiso 1 1 calc R . . C56 C 0.3193(4) 0.6842(3) 0.41007(19) 0.0332(10) Uani 1 1 d . . . H56 H 0.3668 0.7377 0.3912 0.040 Uiso 1 1 calc R . . C57 C 0.7647(4) 0.7815(3) 0.4777(2) 0.0323(10) Uani 1 1 d . . . C58 C 0.7727(5) 0.7936(3) 0.3987(2) 0.0457(12) Uani 1 1 d . . . H58 H 0.7097 0.7657 0.3737 0.055 Uiso 1 1 calc R . . C59 C 0.8698(5) 0.8453(3) 0.3547(2) 0.0527(13) Uani 1 1 d . . . H59 H 0.8704 0.8530 0.3004 0.063 Uiso 1 1 calc R . . C60 C 0.9649(4) 0.8853(3) 0.3875(2) 0.0443(11) Uani 1 1 d . . . C61 C 0.9569(6) 0.8747(4) 0.4661(3) 0.0738(18) Uani 1 1 d . . . H61 H 1.0197 0.9029 0.4910 0.089 Uiso 1 1 calc R . . C62 C 0.8585(5) 0.8235(4) 0.5097(2) 0.0740(18) Uani 1 1 d . . . H62 H 0.8562 0.8174 0.5640 0.089 Uiso 1 1 calc R . . C63 C 0.0398(5) 0.5590(3) 0.3450(2) 0.0532(13) Uani 1 1 d . . . H63A H 0.0333 0.6040 0.2974 0.080 Uiso 1 1 calc R . . H63B H -0.0555 0.5649 0.3741 0.080 Uiso 1 1 calc R . . H63C H 0.0724 0.4912 0.3329 0.080 Uiso 1 1 calc R . . C64 C 1.0725(5) 0.9423(3) 0.3421(3) 0.0650(15) Uani 1 1 d . . . H64A H 1.1673 0.8990 0.3368 0.098 Uiso 1 1 calc R . . H64B H 1.0799 0.9979 0.3689 0.098 Uiso 1 1 calc R . . H64C H 1.0401 0.9670 0.2912 0.098 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 N1 0.0289(18) 0.0172(17) 0.0244(15) 0.0001(14) -0.0052(13) -0.0070(14) N2 0.0262(18) 0.0223(18) 0.0210(15) -0.0027(14) -0.0017(13) -0.0056(14) N3 0.0247(17) 0.0196(18) 0.0204(15) 0.0000(13) -0.0030(12) -0.0064(13) N4 0.0318(18) 0.0186(17) 0.0229(15) 0.0021(14) -0.0045(13) -0.0082(14) N5 0.0345(19) 0.034(2) 0.0227(16) -0.0028(14) -0.0024(14) -0.0116(16) C1 0.025(2) 0.020(2) 0.0213(18) 0.0004(16) -0.0052(16) -0.0080(17) C2 0.029(2) 0.022(2) 0.0236(19) 0.0036(16) -0.0050(16) -0.0069(17) C3 0.034(2) 0.023(2) 0.029(2) -0.0045(17) -0.0100(17) -0.0107(18) C4 0.027(2) 0.017(2) 0.0168(17) -0.0030(16) 0.0005(15) -0.0078(17) C5 0.023(2) 0.026(2) 0.0210(18) -0.0036(16) -0.0032(16) -0.0080(17) C6 0.027(2) 0.029(2) 0.0167(17) -0.0056(17) -0.0021(15) -0.0081(18) C7 0.029(2) 0.027(2) 0.030(2) -0.0013(18) -0.0104(17) -0.0117(18) C8 0.027(2) 0.034(3) 0.0236(19) -0.0043(17) -0.0101(16) -0.0071(18) C9 0.022(2) 0.026(2) 0.0202(18) -0.0016(16) -0.0009(15) -0.0045(17) C10 0.023(2) 0.019(2) 0.0192(18) -0.0037(16) -0.0005(15) 0.0014(16) C11 0.020(2) 0.026(2) 0.0180(18) -0.0040(16) 0.0010(15) -0.0009(17) C12 0.026(2) 0.021(2) 0.0187(18) 0.0009(16) 0.0006(15) -0.0054(17) C13 0.028(2) 0.018(2) 0.0243(19) -0.0026(16) -0.0012(16) -0.0053(17) C14 0.022(2) 0.021(2) 0.0218(18) -0.0045(16) -0.0021(15) -0.0051(16) C15 0.023(2) 0.020(2) 0.0226(18) -0.0027(16) -0.0035(15) -0.0041(16) C16 0.020(2) 0.019(2) 0.0235(18) -0.0037(16) -0.0034(15) -0.0030(16) C17 0.027(2) 0.024(2) 0.0226(18) -0.0069(17) -0.0041(16) -0.0071(17) C18 0.025(2) 0.026(2) 0.0192(18) -0.0004(16) -0.0025(15) -0.0098(17) C19 0.021(2) 0.024(2) 0.0189(18) -0.0027(16) -0.0023(15) -0.0078(16) C20 0.020(2) 0.021(2) 0.0225(18) -0.0012(16) -0.0021(15) -0.0036(16) C21 0.027(2) 0.030(2) 0.0218(19) 0.0019(17) -0.0077(16) -0.0096(19) C22 0.033(2) 0.027(2) 0.039(2) 0.0029(19) -0.0113(18) -0.0112(19) C23 0.047(3) 0.035(3) 0.057(3) 0.008(2) -0.030(2) -0.017(2) C24 0.068(4) 0.033(3) 0.056(3) -0.010(2) -0.032(3) -0.012(3) C25 0.059(3) 0.035(3) 0.047(3) -0.018(2) -0.012(2) -0.009(2) C26 0.039(3) 0.035(3) 0.035(2) -0.011(2) -0.0034(19) -0.011(2) C27 0.028(2) 0.024(2) 0.0203(18) -0.0033(16) -0.0037(16) -0.0049(18) C28 0.027(2) 0.030(2) 0.026(2) -0.0061(18) -0.0032(17) -0.0059(19) C29 0.026(2) 0.029(2) 0.043(2) -0.0050(19) -0.0174(18) -0.0004(18) C30 0.038(3) 0.032(3) 0.031(2) 0.0035(19) -0.0180(19) -0.006(2) C31 0.042(3) 0.043(3) 0.0202(19) -0.0020(19) -0.0087(18) -0.012(2) C32 0.032(2) 0.029(2) 0.027(2) -0.0029(18) -0.0056(17) -0.0054(18) C33 0.031(2) 0.022(2) 0.0176(17) -0.0011(16) -0.0021(16) -0.0079(18) C34 0.037(2) 0.027(2) 0.028(2) 0.0015(18) -0.0058(18) -0.008(2) C35 0.046(3) 0.019(2) 0.031(2) -0.0062(18) 0.0022(19) -0.0040(19) C36 0.058(3) 0.032(3) 0.027(2) -0.0062(19) -0.003(2) -0.022(2) C37 0.042(3) 0.040(3) 0.023(2) -0.0014(19) -0.0075(18) -0.018(2) C38 0.035(2) 0.027(2) 0.0202(18) -0.0017(17) -0.0027(17) -0.0051(18) C39 0.028(2) 0.020(2) 0.0188(17) -0.0020(16) -0.0048(16) -0.0061(17) C40 0.031(2) 0.027(2) 0.0254(19) -0.0041(17) -0.0050(17) -0.0049(18) C41 0.037(2) 0.038(3) 0.034(2) -0.003(2) -0.0150(19) -0.003(2) C42 0.050(3) 0.035(3) 0.034(2) 0.010(2) -0.017(2) -0.005(2) C43 0.049(3) 0.034(3) 0.029(2) 0.0056(19) -0.0059(19) -0.014(2) C44 0.030(2) 0.025(2) 0.029(2) 0.0011(17) -0.0071(17) -0.0077(18) C45 0.028(2) 0.022(2) 0.0197(18) 0.0001(16) -0.0023(16) -0.0012(17) C46 0.026(2) 0.028(2) 0.0267(19) -0.0040(17) -0.0006(16) -0.0110(17) C47 0.027(2) 0.024(2) 0.027(2) 0.0005(17) -0.0057(17) -0.0058(18) C49 0.031(2) 0.027(2) 0.0248(19) -0.0006(17) -0.0047(17) -0.0082(18) C50 0.031(2) 0.026(2) 0.0237(19) -0.0037(17) -0.0053(17) -0.0071(18) C51 0.031(2) 0.029(2) 0.0239(19) -0.0083(17) -0.0052(17) -0.0051(18) C52 0.032(2) 0.035(3) 0.026(2) -0.0075(18) -0.0092(17) -0.0031(19) C53 0.038(2) 0.036(3) 0.036(2) -0.011(2) -0.0036(19) -0.007(2) C54 0.033(2) 0.042(3) 0.034(2) -0.013(2) -0.0084(18) -0.005(2) C55 0.041(3) 0.051(3) 0.029(2) -0.004(2) -0.0146(19) -0.007(2) C56 0.036(2) 0.037(3) 0.027(2) -0.0023(18) -0.0056(18) -0.006(2) C57 0.033(2) 0.033(2) 0.032(2) 0.0030(19) -0.0056(18) -0.012(2) C58 0.054(3) 0.058(3) 0.029(2) 0.000(2) -0.006(2) -0.022(2) C59 0.063(3) 0.063(3) 0.035(2) 0.007(2) 0.002(2) -0.029(3) C60 0.037(3) 0.035(3) 0.054(3) 0.002(2) 0.009(2) -0.004(2) C61 0.080(4) 0.110(5) 0.047(3) 0.011(3) -0.011(3) -0.068(4) C62 0.078(4) 0.131(5) 0.031(2) 0.013(3) -0.016(2) -0.073(4) C63 0.055(3) 0.069(3) 0.044(3) -0.018(2) -0.020(2) -0.014(3) C64 0.058(3) 0.053(3) 0.074(3) 0.010(3) 0.028(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #============================================================================== # GEOMETRY #============================================================================== 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 N1 C4 1.372(4) . ? N1 C1 1.373(4) . ? N1 H1 0.8800 . ? N2 C6 1.371(4) . ? N2 C9 1.373(4) . ? N3 C16 1.363(4) . ? N3 C19 1.373(4) . ? N4 C14 1.365(4) . ? N4 C11 1.369(4) . ? N4 H4 0.8800 . ? N5 C47 1.345(4) . ? N5 C49 1.347(4) . ? C1 C20 1.406(4) . ? C1 C2 1.424(5) . ? C2 C3 1.349(4) . ? C2 H2 0.9500 . ? C3 C4 1.423(5) . ? C3 H3 0.9500 . ? C4 C5 1.402(4) . ? C5 C6 1.405(5) . ? C5 C21 1.489(5) . ? C6 C7 1.447(4) . ? C7 C8 1.353(5) . ? C7 H7 0.9500 . ? C8 C9 1.451(4) . ? C8 H8 0.9500 . ? C9 C10 1.401(5) . ? C10 C11 1.403(4) . ? C10 C27 1.489(4) . ? C11 C12 1.430(5) . ? C12 C13 1.354(4) . ? C12 H12 0.9500 . ? C13 C14 1.429(4) . ? C13 H13 0.9500 . ? C14 C15 1.396(4) . ? C15 C16 1.407(4) . ? C15 C33 1.495(5) . ? C16 C17 1.444(4) . ? C17 C18 1.359(5) . ? C17 H17 0.9500 . ? C18 C19 1.463(4) . ? C18 C45 1.481(4) . ? C19 C20 1.403(5) . ? C20 C39 1.506(4) . ? C21 C22 1.385(5) . ? C21 C26 1.393(5) . ? C22 C23 1.392(5) . ? C22 H22 0.9500 . ? C23 C24 1.361(6) . ? C23 H23 0.9500 . ? C24 C25 1.365(6) . ? C24 H24 0.9500 . ? C25 C26 1.385(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.378(5) . ? C27 C32 1.393(5) . ? C28 C29 1.390(5) . ? C28 H28 0.9500 . ? C29 C30 1.365(5) . ? C29 H29 0.9500 . ? C30 C31 1.364(5) . ? C30 H30 0.9500 . ? C31 C32 1.400(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.393(5) . ? C33 C34 1.396(5) . ? C34 C35 1.380(5) . ? C34 H34 0.9500 . ? C35 C36 1.373(5) . ? C35 H35 0.9500 . ? C36 C37 1.376(5) . ? C36 H36 0.9500 . ? C37 C38 1.379(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.393(4) . ? C39 C44 1.395(5) . ? C40 C41 1.382(5) . ? C40 H40 0.9500 . ? C41 C42 1.376(5) . ? C41 H41 0.9500 . ? C42 C43 1.389(5) . ? C42 H42 0.9500 . ? C43 C44 1.379(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.379(5) . ? C45 C46 1.389(4) . ? C46 C47 1.395(4) . ? C46 H46 0.9500 . ? C47 C51 1.485(5) . ? C49 C50 1.403(4) . ? C49 C57 1.474(5) . ? C50 H50 0.9500 . ? C51 C56 1.386(4) . ? C51 C52 1.401(5) . ? C52 C53 1.389(5) . ? C52 H52 0.9500 . ? C53 C54 1.386(5) . ? C53 H53 0.9500 . ? C54 C55 1.372(5) . ? C54 C63 1.522(5) . ? C55 C56 1.381(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.365(5) . ? C57 C58 1.380(5) . ? C58 C59 1.385(5) . ? C58 H58 0.9500 . ? C59 C60 1.367(6) . ? C59 H59 0.9500 . ? C60 C61 1.372(6) . ? C60 C64 1.508(5) . ? C61 C62 1.387(6) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? 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 C4 N1 C1 109.5(3) . . ? C4 N1 H1 125.2 . . ? C1 N1 H1 125.3 . . ? C6 N2 C9 106.8(3) . . ? C16 N3 C19 107.8(3) . . ? C14 N4 C11 109.2(3) . . ? C14 N4 H4 125.4 . . ? C11 N4 H4 125.4 . . ? C47 N5 C49 118.6(3) . . ? N1 C1 C20 125.8(3) . . ? N1 C1 C2 106.7(3) . . ? C20 C1 C2 127.3(3) . . ? C3 C2 C1 108.6(3) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? C2 C3 C4 107.9(3) . . ? C2 C3 H3 126.0 . . ? C4 C3 H3 126.0 . . ? N1 C4 C5 125.8(3) . . ? N1 C4 C3 107.2(3) . . ? C5 C4 C3 126.7(3) . . ? C4 C5 C6 125.0(3) . . ? C4 C5 C21 117.5(3) . . ? C6 C5 C21 117.6(3) . . ? N2 C6 C5 125.1(3) . . ? N2 C6 C7 109.7(3) . . ? C5 C6 C7 124.9(3) . . ? C8 C7 C6 107.0(3) . . ? C8 C7 H7 126.5 . . ? C6 C7 H7 126.5 . . ? C7 C8 C9 107.1(3) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C10 126.1(3) . . ? N2 C9 C8 109.3(3) . . ? C10 C9 C8 124.4(3) . . ? C9 C10 C11 124.5(3) . . ? C9 C10 C27 117.6(3) . . ? C11 C10 C27 117.9(3) . . ? N4 C11 C10 125.5(3) . . ? N4 C11 C12 107.5(3) . . ? C10 C11 C12 126.9(3) . . ? C13 C12 C11 107.8(3) . . ? C13 C12 H12 126.1 . . ? C11 C12 H12 126.1 . . ? C12 C13 C14 107.8(3) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? N4 C14 C15 125.2(3) . . ? N4 C14 C13 107.7(3) . . ? C15 C14 C13 127.1(3) . . ? C14 C15 C16 125.3(3) . . ? C14 C15 C33 118.0(3) . . ? C16 C15 C33 116.7(3) . . ? N3 C16 C15 126.9(3) . . ? N3 C16 C17 109.2(3) . . ? C15 C16 C17 123.9(3) . . ? C18 C17 C16 107.8(3) . . ? C18 C17 H17 126.1 . . ? C16 C17 H17 126.1 . . ? C17 C18 C19 106.3(3) . . ? C17 C18 C45 121.6(3) . . ? C19 C18 C45 131.9(3) . . ? N3 C19 C20 123.9(3) . . ? N3 C19 C18 108.8(3) . . ? C20 C19 C18 127.1(3) . . ? C19 C20 C1 124.9(3) . . ? C19 C20 C39 118.9(3) . . ? C1 C20 C39 116.2(3) . . ? C22 C21 C26 118.0(3) . . ? C22 C21 C5 121.3(3) . . ? C26 C21 C5 120.8(3) . . ? C21 C22 C23 120.6(4) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.9(4) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 120.6(4) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 118.4(3) . . ? C28 C27 C10 120.6(3) . . ? C32 C27 C10 121.0(3) . . ? C27 C28 C29 120.8(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 120.1(4) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.5(3) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C27 C32 C31 120.3(4) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C38 C33 C34 117.6(3) . . ? C38 C33 C15 121.4(3) . . ? C34 C33 C15 120.9(3) . . ? C35 C34 C33 120.7(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 120.9(4) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 119.1(4) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C36 C37 C38 120.7(4) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C33 121.0(4) . . ? C37 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? C40 C39 C44 118.3(3) . . ? C40 C39 C20 119.9(3) . . ? C44 C39 C20 121.8(3) . . ? C41 C40 C39 120.3(3) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C42 C41 C40 120.8(4) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 119.6(3) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 119.6(4) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C39 121.3(3) . . ? C43 C44 H44 119.3 . . ? C39 C44 H44 119.3 . . ? C50 C45 C46 117.9(3) . . ? C50 C45 C18 122.9(3) . . ? C46 C45 C18 118.9(3) . . ? C45 C46 C47 120.1(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? N5 C47 C46 121.8(3) . . ? N5 C47 C51 116.5(3) . . ? C46 C47 C51 121.7(3) . . ? N5 C49 C50 121.9(3) . . ? N5 C49 C57 116.2(3) . . ? C50 C49 C57 121.9(3) . . ? C45 C50 C49 119.7(3) . . ? C45 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C56 C51 C52 118.0(3) . . ? C56 C51 C47 120.8(3) . . ? C52 C51 C47 121.2(3) . . ? C53 C52 C51 120.3(3) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C54 C53 C52 121.0(4) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C55 C54 C53 118.2(3) . . ? C55 C54 C63 121.4(4) . . ? C53 C54 C63 120.3(4) . . ? C54 C55 C56 121.6(4) . . ? C54 C55 H55 119.2 . . ? C56 C55 H55 119.2 . . ? C55 C56 C51 120.8(4) . . ? C55 C56 H56 119.6 . . ? C51 C56 H56 119.6 . . ? C62 C57 C58 115.8(4) . . ? C62 C57 C49 122.9(3) . . ? C58 C57 C49 121.2(3) . . ? C57 C58 C59 121.9(4) . . ? C57 C58 H58 119.0 . . ? C59 C58 H58 119.0 . . ? C60 C59 C58 121.6(4) . . ? C60 C59 H59 119.2 . . ? C58 C59 H59 119.2 . . ? C59 C60 C61 117.1(4) . . ? C59 C60 C64 123.6(4) . . ? C61 C60 C64 119.3(4) . . ? C60 C61 C62 120.9(4) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C57 C62 C61 122.7(4) . . ? C57 C62 H62 118.7 . . ? C61 C62 H62 118.7 . . ? C54 C63 H63A 109.5 . . ? C54 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C54 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C60 C64 H64A 109.5 . . ? C60 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C60 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? 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 C4 N1 C1 C20 172.9(3) . . . . ? C4 N1 C1 C2 -2.8(4) . . . . ? N1 C1 C2 C3 2.1(4) . . . . ? C20 C1 C2 C3 -173.5(3) . . . . ? C1 C2 C3 C4 -0.6(4) . . . . ? C1 N1 C4 C5 -171.5(3) . . . . ? C1 N1 C4 C3 2.4(4) . . . . ? C2 C3 C4 N1 -1.1(4) . . . . ? C2 C3 C4 C5 172.8(3) . . . . ? N1 C4 C5 C6 -8.0(6) . . . . ? C3 C4 C5 C6 179.2(3) . . . . ? N1 C4 C5 C21 171.3(3) . . . . ? C3 C4 C5 C21 -1.5(5) . . . . ? C9 N2 C6 C5 -170.7(3) . . . . ? C9 N2 C6 C7 3.6(4) . . . . ? C4 C5 C6 N2 -9.0(6) . . . . ? C21 C5 C6 N2 171.7(3) . . . . ? C4 C5 C6 C7 177.6(3) . . . . ? C21 C5 C6 C7 -1.8(5) . . . . ? N2 C6 C7 C8 -1.2(4) . . . . ? C5 C6 C7 C8 173.1(3) . . . . ? C6 C7 C8 C9 -1.6(4) . . . . ? C6 N2 C9 C10 170.6(3) . . . . ? C6 N2 C9 C8 -4.5(4) . . . . ? C7 C8 C9 N2 3.9(4) . . . . ? C7 C8 C9 C10 -171.4(3) . . . . ? N2 C9 C10 C11 8.9(6) . . . . ? C8 C9 C10 C11 -176.6(3) . . . . ? N2 C9 C10 C27 -170.5(3) . . . . ? C8 C9 C10 C27 3.9(5) . . . . ? C14 N4 C11 C10 173.3(3) . . . . ? C14 N4 C11 C12 -3.6(4) . . . . ? C9 C10 C11 N4 7.7(6) . . . . ? C27 C10 C11 N4 -172.9(3) . . . . ? C9 C10 C11 C12 -176.0(3) . . . . ? C27 C10 C11 C12 3.4(5) . . . . ? N4 C11 C12 C13 2.2(4) . . . . ? C10 C11 C12 C13 -174.6(3) . . . . ? C11 C12 C13 C14 0.0(4) . . . . ? C11 N4 C14 C15 -173.4(3) . . . . ? C11 N4 C14 C13 3.6(4) . . . . ? C12 C13 C14 N4 -2.2(4) . . . . ? C12 C13 C14 C15 174.7(3) . . . . ? N4 C14 C15 C16 -8.4(6) . . . . ? C13 C14 C15 C16 175.2(3) . . . . ? N4 C14 C15 C33 169.2(3) . . . . ? C13 C14 C15 C33 -7.2(5) . . . . ? C19 N3 C16 C15 -176.5(3) . . . . ? C19 N3 C16 C17 3.5(4) . . . . ? C14 C15 C16 N3 -10.4(6) . . . . ? C33 C15 C16 N3 171.9(3) . . . . ? C14 C15 C16 C17 169.6(3) . . . . ? C33 C15 C16 C17 -8.1(5) . . . . ? N3 C16 C17 C18 -1.2(4) . . . . ? C15 C16 C17 C18 178.8(3) . . . . ? C16 C17 C18 C19 -1.5(4) . . . . ? C16 C17 C18 C45 173.6(3) . . . . ? C16 N3 C19 C20 170.6(3) . . . . ? C16 N3 C19 C18 -4.5(4) . . . . ? C17 C18 C19 N3 3.7(4) . . . . ? C45 C18 C19 N3 -170.7(3) . . . . ? C17 C18 C19 C20 -171.2(3) . . . . ? C45 C18 C19 C20 14.4(6) . . . . ? N3 C19 C20 C1 14.0(5) . . . . ? C18 C19 C20 C1 -171.8(3) . . . . ? N3 C19 C20 C39 -164.4(3) . . . . ? C18 C19 C20 C39 9.7(5) . . . . ? N1 C1 C20 C19 7.3(5) . . . . ? C2 C1 C20 C19 -177.9(3) . . . . ? N1 C1 C20 C39 -174.2(3) . . . . ? C2 C1 C20 C39 0.5(5) . . . . ? C4 C5 C21 C22 -115.2(4) . . . . ? C6 C5 C21 C22 64.1(4) . . . . ? C4 C5 C21 C26 65.1(4) . . . . ? C6 C5 C21 C26 -115.5(4) . . . . ? C26 C21 C22 C23 1.5(5) . . . . ? C5 C21 C22 C23 -178.1(3) . . . . ? C21 C22 C23 C24 -0.7(5) . . . . ? C22 C23 C24 C25 -0.3(6) . . . . ? C23 C24 C25 C26 0.4(6) . . . . ? C24 C25 C26 C21 0.5(6) . . . . ? C22 C21 C26 C25 -1.4(5) . . . . ? C5 C21 C26 C25 178.2(3) . . . . ? C9 C10 C27 C28 -121.5(4) . . . . ? C11 C10 C27 C28 59.1(4) . . . . ? C9 C10 C27 C32 58.3(5) . . . . ? C11 C10 C27 C32 -121.2(4) . . . . ? C32 C27 C28 C29 -0.1(5) . . . . ? C10 C27 C28 C29 179.6(3) . . . . ? C27 C28 C29 C30 -0.4(5) . . . . ? C28 C29 C30 C31 0.6(6) . . . . ? C29 C30 C31 C32 -0.4(6) . . . . ? C28 C27 C32 C31 0.4(5) . . . . ? C10 C27 C32 C31 -179.4(3) . . . . ? C30 C31 C32 C27 -0.1(5) . . . . ? C14 C15 C33 C38 126.3(3) . . . . ? C16 C15 C33 C38 -55.9(4) . . . . ? C14 C15 C33 C34 -55.9(5) . . . . ? C16 C15 C33 C34 122.0(4) . . . . ? C38 C33 C34 C35 0.8(5) . . . . ? C15 C33 C34 C35 -177.2(3) . . . . ? C33 C34 C35 C36 0.2(5) . . . . ? C34 C35 C36 C37 -0.8(5) . . . . ? C35 C36 C37 C38 0.6(5) . . . . ? C36 C37 C38 C33 0.4(5) . . . . ? C34 C33 C38 C37 -1.0(5) . . . . ? C15 C33 C38 C37 176.9(3) . . . . ? C19 C20 C39 C40 56.2(5) . . . . ? C1 C20 C39 C40 -122.3(4) . . . . ? C19 C20 C39 C44 -122.4(4) . . . . ? C1 C20 C39 C44 59.0(5) . . . . ? C44 C39 C40 C41 1.7(5) . . . . ? C20 C39 C40 C41 -177.1(3) . . . . ? C39 C40 C41 C42 -1.0(6) . . . . ? C40 C41 C42 C43 -0.1(6) . . . . ? C41 C42 C43 C44 0.6(6) . . . . ? C42 C43 C44 C39 0.1(6) . . . . ? C40 C39 C44 C43 -1.2(5) . . . . ? C20 C39 C44 C43 177.4(3) . . . . ? C17 C18 C45 C50 -125.6(4) . . . . ? C19 C18 C45 C50 48.1(6) . . . . ? C17 C18 C45 C46 49.1(5) . . . . ? C19 C18 C45 C46 -137.3(4) . . . . ? C50 C45 C46 C47 -0.8(5) . . . . ? C18 C45 C46 C47 -175.7(3) . . . . ? C49 N5 C47 C46 1.2(5) . . . . ? C49 N5 C47 C51 -178.8(3) . . . . ? C45 C46 C47 N5 -0.2(5) . . . . ? C45 C46 C47 C51 179.8(3) . . . . ? C47 N5 C49 C50 -1.0(5) . . . . ? C47 N5 C49 C57 177.9(3) . . . . ? C46 C45 C50 C49 1.0(5) . . . . ? C18 C45 C50 C49 175.7(3) . . . . ? N5 C49 C50 C45 -0.1(5) . . . . ? C57 C49 C50 C45 -178.9(4) . . . . ? N5 C47 C51 C56 -21.6(5) . . . . ? C46 C47 C51 C56 158.4(4) . . . . ? N5 C47 C51 C52 158.1(4) . . . . ? C46 C47 C51 C52 -21.9(6) . . . . ? C56 C51 C52 C53 0.0(6) . . . . ? C47 C51 C52 C53 -179.7(3) . . . . ? C51 C52 C53 C54 -0.6(6) . . . . ? C52 C53 C54 C55 0.7(6) . . . . ? C52 C53 C54 C63 178.3(4) . . . . ? C53 C54 C55 C56 -0.1(6) . . . . ? C63 C54 C55 C56 -177.7(4) . . . . ? C54 C55 C56 C51 -0.5(6) . . . . ? C52 C51 C56 C55 0.6(6) . . . . ? C47 C51 C56 C55 -179.7(4) . . . . ? N5 C49 C57 C62 168.5(4) . . . . ? C50 C49 C57 C62 -12.6(6) . . . . ? N5 C49 C57 C58 -11.0(6) . . . . ? C50 C49 C57 C58 168.0(4) . . . . ? C62 C57 C58 C59 -0.1(7) . . . . ? C49 C57 C58 C59 179.4(4) . . . . ? C57 C58 C59 C60 1.3(7) . . . . ? C58 C59 C60 C61 -1.9(7) . . . . ? C58 C59 C60 C64 -179.9(4) . . . . ? C59 C60 C61 C62 1.4(8) . . . . ? C64 C60 C61 C62 179.5(5) . . . . ? C58 C57 C62 C61 -0.4(8) . . . . ? C49 C57 C62 C61 -179.9(5) . . . . ? C60 C61 C62 C57 -0.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.255 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.056 data_3e _database_code_depnum_ccdc_archive 'CCDC 859838' #TrackingRef '3e.cif' #============================================================================= # start Validation Reply Form _vrf_PLAT220_3e ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.3 Ratio RESPONSE: One phenyl substituent group attached to the central porphyrin core is severely affected by thermal disorder (large vibrations perpendicular to the plane of the aromatic ring), hence leading to large Ueq values and to this particular alert. The ring affected by this thermal disorder is that composed of C33-C34-C35-C36-C37-C38. ; _vrf_PLAT241_3e ; PROBLEM: Check High Ueq as Compared to Neighbors RESPONSE: Please see our response to _vrf_PLAT220_3e. ; _vrf_PLAT242_3e ; PROBLEM: Check High Ueq as Compared to Neighbors RESPONSE: Please see our response to _vrf_PLAT220_3e. ; _vrf_PLAT213_3e ; PROBLEM: Atom C34 has ADP max/min Ratio ..... 3.1 prola RESPONSE: Please see our response to _vrf_PLAT220_3e. ; _vrf_PLAT250_3e ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.1 RESPONSE: Please see our response to _vrf_PLAT220_3e. ; _vrf_PLAT366_3e ; PROBLEM: Short? C(sp?)-C(sp?) Bond RESPONSE: This alert is associated with two bonds: C46-C47 and C48-C49. As described in the technical section of the manuscript the two peripheral pyridine rings of the large tertpyridine moiety attached to the central porphyrin core are disordered over two distinct crystallographic locations. The pivot atoms are C47 and C48 (common to both locations of the terminal pyridyl groups). Because structural resolution did not allow a sensible refinement of two locations for the C47 and C48 atoms, the final model is affected by a systematic error translated into unusual C-C distances within the central pyridyl group. ; _vrf_RFACR01_3e ; PROBLEM: The value of the weighted R factor is > 0.25 RESPONSE: The compound crystallizes as small red block crystals which systematically exhibited very poor diffraction at high angles. The largest crystal from several batches was selected for full data collection (crystal size: 0.07 X 0.07 x 0.04 mm) at the low temperature of 150 K. Even for long exposure times the Rint value for a resolution better than ca. 1.8 A was always above 0.10, with the crystal diffracting very poorly above that resolution (e.g., the mean I/s between 1.03 and 0.99 A was only of about 1.2). A better data set which may allow a sensible refinement of the structure may only be collected using either a synchrotron source or a rotating anode instrument. ; _vrf_PLAT020_3e ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.137 RESPONSE: Please see our response to _vrf_RFACR01_3e. ; _vrf_RINTA01_3e ; PROBLEM: The value of Rint is greater than 0.12 RESPONSE: Please see our response to _vrf_RFACR01_3e. ; _vrf_DIFMX01_3e ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 RESPONSE: The largest peak and deepest hole are located at 0.92 A and 0.43 A from H60' and N61, respectively, which belong to the same disordered phenyl substituent group. ; _vrf_PLAT094_3e ; PROBLEM: Ratio of Maximum / Minimum Residual Density .... 2.10 RESPONSE: Please see our response to _vrf_DIFMX01_3e. ; # end Validation Reply Form #============================================================================= # ======================================================================= _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '22 December 2011' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H39 N7' _chemical_formula_sum 'C59 H39 N7' _chemical_formula_weight 845.97 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' #============================================================================== # CRYSTAL DATA #============================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6667(14) _cell_length_b 13.6339(17) _cell_length_c 18.488(3) _cell_angle_alpha 76.355(8) _cell_angle_beta 78.393(8) _cell_angle_gamma 71.138(7) _cell_volume 2449.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1440 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 20.30 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9939 _exptl_absorpt_correction_T_max 0.9973 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1997) ; #============================================================================== # EXPERIMENTAL DATA #============================================================================== _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Kappa CCD APEX II' _diffrn_measurement_method '\w / \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 30441 _diffrn_reflns_av_R_equivalents 0.1369 _diffrn_reflns_av_sigmaI/netI 0.2630 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.34 _reflns_number_total 8820 _reflns_number_gt 2983 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 (Bruker, 2006)' _computing_data_reduction 'SAINT+ (Bruker, 2005)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' #============================================================================== # REFINEMENT DATA #============================================================================== _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1162P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8820 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2447 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2542 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 1.0363(4) 0.7405(3) 0.6632(2) 0.0306(11) Uani 1 1 d . . . N2 N 1.1286(4) 0.5526(3) 0.5947(2) 0.0362(11) Uani 1 1 d . . . H2 H 1.1356 0.6171 0.5807 0.043 Uiso 1 1 calc R . . N3 N 1.2840(4) 0.6594(3) 0.4724(2) 0.0313(11) Uani 1 1 d . . . N4 N 1.1895(4) 0.8499(3) 0.5390(2) 0.0296(11) Uani 1 1 d . . . H4 H 1.1685 0.7905 0.5479 0.036 Uiso 1 1 calc R . . N5 N 0.5676(5) 0.6889(4) 0.9470(3) 0.0578(15) Uani 1 1 d . A . C1 C 1.0028(5) 0.8346(4) 0.6858(3) 0.0318(13) Uani 1 1 d . . . C2 C 0.9028(5) 0.8386(4) 0.7517(3) 0.0383(14) Uani 1 1 d . . . H2A H 0.8654 0.8957 0.7781 0.046 Uiso 1 1 calc R . . C3 C 0.8728(5) 0.7464(4) 0.7686(3) 0.0362(14) Uani 1 1 d . . . C4 C 0.9609(5) 0.6825(4) 0.7138(3) 0.0338(14) Uani 1 1 d . . . C5 C 0.9719(5) 0.5773(4) 0.7132(3) 0.0360(14) Uani 1 1 d . . . C6 C 1.0543(5) 0.5176(4) 0.6589(3) 0.0381(14) Uani 1 1 d . . . C7 C 1.0708(6) 0.4105(4) 0.6612(3) 0.0508(17) Uani 1 1 d . . . H7 H 1.0322 0.3654 0.7002 0.061 Uiso 1 1 calc R . . C8 C 1.1519(6) 0.3821(4) 0.5976(3) 0.0539(18) Uani 1 1 d . . . H8 H 1.1781 0.3147 0.5839 0.065 Uiso 1 1 calc R . . C9 C 1.1901(5) 0.4731(4) 0.5555(3) 0.0402(15) Uani 1 1 d . . . C10 C 1.2738(5) 0.4779(4) 0.4859(3) 0.0377(14) Uani 1 1 d . . . C11 C 1.3163(5) 0.5669(4) 0.4475(3) 0.0292(13) Uani 1 1 d . . . C12 C 1.4018(5) 0.5712(4) 0.3766(3) 0.0340(14) Uani 1 1 d . . . H12 H 1.4351 0.5175 0.3470 0.041 Uiso 1 1 calc R . . C13 C 1.4259(5) 0.6664(4) 0.3598(3) 0.0343(14) Uani 1 1 d . . . H13 H 1.4812 0.6918 0.3173 0.041 Uiso 1 1 calc R . . C14 C 1.3500(5) 0.7215(4) 0.4202(3) 0.0304(13) Uani 1 1 d . . . C15 C 1.3483(5) 0.8244(4) 0.4232(3) 0.0317(13) Uani 1 1 d . . . C16 C 1.2752(5) 0.8812(4) 0.4787(3) 0.0286(13) Uani 1 1 d . . . C17 C 1.2802(5) 0.9805(4) 0.4853(3) 0.0395(15) Uani 1 1 d . . . H17 H 1.3318 1.0212 0.4511 0.047 Uiso 1 1 calc R . . C18 C 1.1994(5) 1.0090(4) 0.5485(3) 0.0406(15) Uani 1 1 d . . . H18 H 1.1842 1.0725 0.5661 0.049 Uiso 1 1 calc R . . C19 C 1.1417(5) 0.9248(4) 0.5834(3) 0.0300(13) Uani 1 1 d . . . C20 C 1.0553(4) 0.9209(4) 0.6504(3) 0.0299(13) Uani 1 1 d . . . C21 C 0.8933(5) 0.5188(4) 0.7737(3) 0.0338(13) Uani 1 1 d . . . C22 C 0.9185(5) 0.4900(4) 0.8464(3) 0.0397(15) Uani 1 1 d . . . H22 H 0.9905 0.5060 0.8594 0.048 Uiso 1 1 calc R . . C23 C 0.8412(6) 0.4378(4) 0.9019(4) 0.0515(17) Uani 1 1 d . . . H23 H 0.8601 0.4189 0.9522 0.062 Uiso 1 1 calc R . . C24 C 0.7362(6) 0.4132(4) 0.8834(4) 0.0463(16) Uani 1 1 d . . . H24 H 0.6819 0.3788 0.9212 0.056 Uiso 1 1 calc R . . C25 C 0.7115(6) 0.4390(4) 0.8104(4) 0.0474(16) Uani 1 1 d . . . H25 H 0.6408 0.4213 0.7973 0.057 Uiso 1 1 calc R . . C26 C 0.7889(5) 0.4905(4) 0.7556(3) 0.0372(14) Uani 1 1 d . . . H26 H 0.7716 0.5071 0.7050 0.045 Uiso 1 1 calc R . . C27 C 1.3217(5) 0.3815(4) 0.4519(3) 0.0312(13) Uani 1 1 d . . . C28 C 1.2294(5) 0.3377(4) 0.4360(3) 0.0377(14) Uani 1 1 d . . . H28 H 1.1363 0.3703 0.4470 0.045 Uiso 1 1 calc R . . C29 C 1.2729(6) 0.2481(4) 0.4047(3) 0.0394(15) Uani 1 1 d . . . H29 H 1.2094 0.2190 0.3951 0.047 Uiso 1 1 calc R . . C30 C 1.4071(5) 0.2006(4) 0.3872(3) 0.0405(15) Uani 1 1 d . . . H30 H 1.4366 0.1390 0.3655 0.049 Uiso 1 1 calc R . . C31 C 1.4986(6) 0.2433(4) 0.4014(3) 0.0420(15) Uani 1 1 d . . . H31 H 1.5915 0.2115 0.3885 0.050 Uiso 1 1 calc R . . C32 C 1.4570(5) 0.3312(4) 0.4340(3) 0.0317(13) Uani 1 1 d . . . H32 H 1.5218 0.3582 0.4445 0.038 Uiso 1 1 calc R . . C33 C 1.4336(5) 0.8776(4) 0.3627(3) 0.0280(13) Uani 1 1 d . . . C34 C 1.3885(6) 0.9407(6) 0.3012(4) 0.093(3) Uani 1 1 d . . . H34 H 1.2985 0.9511 0.2950 0.111 Uiso 1 1 calc R . . C35 C 1.4655(6) 0.9929(6) 0.2450(4) 0.092(3) Uani 1 1 d . . . H35 H 1.4286 1.0377 0.2020 0.110 Uiso 1 1 calc R . . C36 C 1.5913(6) 0.9784(5) 0.2530(3) 0.0482(16) Uani 1 1 d . . . H36 H 1.6460 1.0123 0.2150 0.058 Uiso 1 1 calc R . . C37 C 1.6407(7) 0.9172(6) 0.3135(4) 0.082(2) Uani 1 1 d . . . H37 H 1.7304 0.9086 0.3192 0.098 Uiso 1 1 calc R . . C38 C 1.5634(6) 0.8654(6) 0.3688(4) 0.073(2) Uani 1 1 d . . . H38 H 1.6013 0.8207 0.4116 0.087 Uiso 1 1 calc R . . C39 C 1.0200(5) 1.0112(4) 0.6909(3) 0.0276(13) Uani 1 1 d . . . C40 C 1.0535(5) 0.9958(4) 0.7617(3) 0.0394(15) Uani 1 1 d . . . H40 H 1.1005 0.9271 0.7846 0.047 Uiso 1 1 calc R . . C41 C 1.0197(6) 1.0793(5) 0.8007(3) 0.0473(16) Uani 1 1 d . . . H41 H 1.0441 1.0675 0.8494 0.057 Uiso 1 1 calc R . . C42 C 0.9508(6) 1.1788(5) 0.7677(4) 0.0476(16) Uani 1 1 d . . . H42 H 0.9276 1.2358 0.7938 0.057 Uiso 1 1 calc R . . C43 C 0.9154(5) 1.1963(5) 0.6975(4) 0.0475(16) Uani 1 1 d . . . H43 H 0.8673 1.2651 0.6753 0.057 Uiso 1 1 calc R . . C44 C 0.9504(5) 1.1124(4) 0.6583(3) 0.0366(14) Uani 1 1 d . . . H44 H 0.9265 1.1246 0.6095 0.044 Uiso 1 1 calc R . . C45 C 0.7671(5) 0.7247(4) 0.8310(3) 0.0349(14) Uani 1 1 d . . . C46 C 0.7766(5) 0.7238(4) 0.9038(3) 0.0437(16) Uani 1 1 d . A . H46 H 0.8532 0.7355 0.9150 0.052 Uiso 1 1 calc R . . C47 C 0.6772(5) 0.7063(4) 0.9614(3) 0.0433(15) Uani 1 1 d . . . C48 C 0.5550(6) 0.6935(5) 0.8752(3) 0.0520(17) Uani 1 1 d . . . C49 C 0.6516(5) 0.7104(4) 0.8166(3) 0.0447(16) Uani 1 1 d . A . H49 H 0.6398 0.7124 0.7666 0.054 Uiso 1 1 calc R . . C50 C 0.6980(7) 0.6854(5) 1.0470(3) 0.0463(8) Uiso 0.50 1 d PG A -1 C51 C 0.7603(7) 0.7491(5) 1.0660(4) 0.0463(8) Uiso 0.50 1 d PG A -1 H51 H 0.7964 0.7966 1.0278 0.056 Uiso 0.50 1 calc PR A -1 C52 C 0.7697(7) 0.7434(5) 1.1408(4) 0.0463(8) Uiso 0.50 1 d PG A -1 H52 H 0.8122 0.7870 1.1538 0.056 Uiso 0.50 1 calc PR A -1 C53 C 0.7168(7) 0.6739(6) 1.1967(3) 0.0463(8) Uiso 0.50 1 d PG A -1 H53 H 0.7232 0.6700 1.2479 0.056 Uiso 0.50 1 calc PR A -1 C54 C 0.6545(6) 0.6102(5) 1.1777(3) 0.0463(8) Uiso 0.50 1 d PG A -1 H54 H 0.6184 0.5627 1.2159 0.056 Uiso 0.50 1 calc PR A -1 N55 N 0.6451(6) 0.6159(5) 1.1028(4) 0.0463(8) Uiso 0.50 1 d PG A -1 C50' C 0.6716(7) 0.7210(6) 1.0355(3) 0.0463(8) Uiso 0.50 1 d PG A -2 C51' C 0.7896(6) 0.7132(6) 1.0605(4) 0.0463(8) Uiso 0.50 1 d PG A -2 H51' H 0.8706 0.7049 1.0266 0.056 Uiso 0.50 1 calc PR A -2 C52' C 0.7891(6) 0.7178(6) 1.1348(4) 0.0463(8) Uiso 0.50 1 d PG A -2 H52' H 0.8698 0.7125 1.1519 0.056 Uiso 0.50 1 calc PR A -2 C53' C 0.6706(7) 0.7300(6) 1.1843(3) 0.0463(8) Uiso 0.50 1 d PG A -2 H53' H 0.6703 0.7331 1.2351 0.056 Uiso 0.50 1 calc PR A -2 C54' C 0.5527(6) 0.7377(6) 1.1594(3) 0.0463(8) Uiso 0.50 1 d PG A -2 H54' H 0.4717 0.7461 1.1932 0.056 Uiso 0.50 1 calc PR A -2 N55' N 0.5531(6) 0.7332(5) 1.0850(4) 0.0463(8) Uiso 0.50 1 d PG A -2 C56 C 0.4512(6) 0.6507(6) 0.8655(4) 0.0515(9) Uiso 0.50 1 d PG A -3 C57 C 0.3997(8) 0.6968(5) 0.7981(4) 0.0515(9) Uiso 0.50 1 d PG A -3 H57 H 0.4352 0.7477 0.7632 0.062 Uiso 0.50 1 calc PR A -3 C58 C 0.2960(8) 0.6683(6) 0.7818(3) 0.0515(9) Uiso 0.50 1 d PG A -3 H58 H 0.2607 0.6997 0.7357 0.062 Uiso 0.50 1 calc PR A -3 C59 C 0.2439(6) 0.5938(6) 0.8328(4) 0.0515(9) Uiso 0.50 1 d PG A -3 H59 H 0.1730 0.5743 0.8216 0.062 Uiso 0.50 1 calc PR A -3 C60 C 0.2955(7) 0.5478(5) 0.9002(4) 0.0515(9) Uiso 0.50 1 d PG A -3 H60 H 0.2599 0.4969 0.9351 0.062 Uiso 0.50 1 calc PR A -3 N61 N 0.3992(7) 0.5763(5) 0.9165(3) 0.0515(9) Uiso 0.50 1 d PG A -3 C56' C 0.4122(6) 0.7017(6) 0.8588(4) 0.0515(9) Uiso 0.50 1 d PG A -4 N61' N 0.3000(7) 0.7278(5) 0.9117(3) 0.0515(9) Uiso 0.50 1 d PG A -4 C60' C 0.1785(6) 0.7198(5) 0.9012(4) 0.0515(9) Uiso 0.50 1 d PG A -4 H60' H 0.1018 0.7377 0.9374 0.062 Uiso 0.50 1 calc PR A -4 C59' C 0.1691(6) 0.6856(6) 0.8379(4) 0.0515(9) Uiso 0.50 1 d PG A -4 H59' H 0.0861 0.6801 0.8308 0.062 Uiso 0.50 1 calc PR A -4 C58' C 0.2813(8) 0.6595(6) 0.7850(3) 0.0515(9) Uiso 0.50 1 d PG A -4 H58' H 0.2749 0.6361 0.7418 0.062 Uiso 0.50 1 calc PR A -4 C57' C 0.4028(7) 0.6675(6) 0.7955(4) 0.0515(9) Uiso 0.50 1 d PG A -4 H57' H 0.4795 0.6496 0.7594 0.062 Uiso 0.50 1 calc PR A -4 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 N1 0.024(2) 0.024(2) 0.044(3) -0.006(2) 0.006(2) -0.0136(19) N2 0.030(3) 0.030(3) 0.047(3) -0.009(2) 0.011(2) -0.015(2) N3 0.031(3) 0.033(3) 0.033(3) -0.001(2) -0.001(2) -0.020(2) N4 0.030(3) 0.024(2) 0.039(3) -0.015(2) 0.004(2) -0.012(2) N5 0.055(3) 0.106(4) 0.037(3) -0.041(3) 0.028(3) -0.057(3) C1 0.022(3) 0.028(3) 0.041(4) -0.005(3) 0.008(3) -0.010(2) C2 0.035(3) 0.029(3) 0.050(4) -0.010(3) 0.007(3) -0.015(3) C3 0.024(3) 0.035(3) 0.047(4) -0.008(3) 0.009(3) -0.013(2) C4 0.023(3) 0.034(3) 0.046(4) -0.013(3) 0.003(3) -0.011(2) C5 0.032(3) 0.037(4) 0.039(4) -0.008(3) 0.006(3) -0.017(3) C6 0.030(3) 0.034(3) 0.047(4) -0.012(3) 0.019(3) -0.017(3) C7 0.065(4) 0.039(4) 0.048(4) -0.015(3) 0.025(3) -0.029(3) C8 0.080(5) 0.027(3) 0.055(4) -0.010(3) 0.014(4) -0.027(3) C9 0.041(3) 0.030(3) 0.051(4) -0.015(3) 0.011(3) -0.018(3) C10 0.029(3) 0.039(4) 0.049(4) -0.008(3) 0.002(3) -0.019(3) C11 0.029(3) 0.029(3) 0.030(3) -0.009(3) -0.003(3) -0.007(2) C12 0.032(3) 0.039(3) 0.034(3) -0.015(3) 0.005(3) -0.013(3) C13 0.034(3) 0.046(4) 0.030(3) -0.007(3) 0.005(3) -0.028(3) C14 0.027(3) 0.038(3) 0.031(3) -0.003(3) -0.006(3) -0.016(3) C15 0.030(3) 0.027(3) 0.036(4) 0.004(3) -0.006(3) -0.011(2) C16 0.027(3) 0.032(3) 0.024(3) 0.001(3) 0.006(3) -0.014(2) C17 0.034(3) 0.029(3) 0.055(4) -0.005(3) 0.011(3) -0.021(3) C18 0.036(3) 0.034(3) 0.052(4) -0.011(3) 0.012(3) -0.018(3) C19 0.028(3) 0.024(3) 0.041(4) -0.007(3) 0.000(3) -0.014(2) C20 0.016(3) 0.032(3) 0.045(4) -0.015(3) 0.001(3) -0.010(2) C21 0.034(3) 0.037(3) 0.035(4) -0.010(3) 0.004(3) -0.020(3) C22 0.037(3) 0.037(3) 0.048(4) -0.018(3) 0.006(3) -0.015(3) C23 0.049(4) 0.053(4) 0.047(4) -0.006(3) 0.009(3) -0.020(3) C24 0.053(4) 0.037(4) 0.048(4) -0.012(3) 0.017(3) -0.023(3) C25 0.051(4) 0.047(4) 0.056(4) -0.020(3) 0.013(3) -0.035(3) C26 0.048(4) 0.033(3) 0.034(3) -0.006(3) 0.010(3) -0.026(3) C27 0.029(3) 0.034(3) 0.032(3) -0.007(3) -0.001(3) -0.012(3) C28 0.031(3) 0.028(3) 0.050(4) -0.006(3) 0.005(3) -0.010(3) C29 0.041(4) 0.033(3) 0.049(4) -0.009(3) -0.003(3) -0.019(3) C30 0.040(4) 0.033(3) 0.046(4) -0.005(3) -0.006(3) -0.008(3) C31 0.036(3) 0.040(4) 0.042(4) -0.013(3) 0.007(3) -0.002(3) C32 0.031(3) 0.037(3) 0.031(3) -0.004(3) -0.007(3) -0.014(3) C33 0.029(3) 0.028(3) 0.028(3) -0.008(3) -0.003(3) -0.007(2) C34 0.030(4) 0.125(7) 0.094(6) 0.053(5) -0.012(4) -0.033(4) C35 0.029(4) 0.113(6) 0.091(6) 0.060(5) -0.015(4) -0.014(4) C36 0.051(4) 0.062(4) 0.034(4) -0.001(3) 0.009(3) -0.035(3) C37 0.042(4) 0.148(7) 0.059(5) 0.021(5) -0.014(4) -0.057(5) C38 0.034(4) 0.131(7) 0.051(5) 0.024(4) -0.018(3) -0.041(4) C39 0.020(3) 0.026(3) 0.040(4) -0.010(3) 0.001(3) -0.009(2) C40 0.043(4) 0.028(3) 0.050(4) -0.009(3) 0.005(3) -0.021(3) C41 0.055(4) 0.060(4) 0.038(4) -0.019(3) 0.008(3) -0.034(3) C42 0.044(4) 0.039(4) 0.066(5) -0.027(3) 0.010(4) -0.018(3) C43 0.022(3) 0.045(4) 0.075(5) -0.013(4) -0.001(3) -0.011(3) C44 0.023(3) 0.037(4) 0.056(4) -0.019(3) -0.001(3) -0.013(3) C45 0.034(3) 0.032(3) 0.042(4) -0.016(3) 0.011(3) -0.017(3) C46 0.031(3) 0.051(4) 0.059(4) -0.030(3) 0.008(3) -0.019(3) C47 0.032(3) 0.066(4) 0.045(4) -0.031(3) 0.012(3) -0.028(3) C48 0.046(4) 0.084(5) 0.041(4) -0.032(3) 0.024(3) -0.042(3) C49 0.047(4) 0.049(4) 0.049(4) -0.018(3) 0.010(3) -0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #============================================================================== # GEOMETRY #============================================================================== 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 N1 C1 1.357(6) . ? N1 C4 1.381(6) . ? N2 C9 1.360(6) . ? N2 C6 1.365(6) . ? N2 H2 0.8800 . ? N3 C11 1.362(6) . ? N3 C14 1.368(6) . ? N4 C19 1.365(6) . ? N4 C16 1.370(6) . ? N4 H4 0.8800 . ? N5 C48 1.345(7) . ? N5 C47 1.352(6) . ? C1 C20 1.430(6) . ? C1 C2 1.448(7) . ? C2 C3 1.348(6) . ? C2 H2A 0.9500 . ? C3 C4 1.474(7) . ? C3 C45 1.490(7) . ? C4 C5 1.402(7) . ? C5 C6 1.418(7) . ? C5 C21 1.491(7) . ? C6 C7 1.405(7) . ? C7 C8 1.367(7) . ? C7 H7 0.9500 . ? C8 C9 1.432(7) . ? C8 H8 0.9500 . ? C9 C10 1.413(7) . ? C10 C11 1.415(7) . ? C10 C27 1.486(7) . ? C11 C12 1.439(6) . ? C12 C13 1.357(6) . ? C12 H12 0.9500 . ? C13 C14 1.450(7) . ? C13 H13 0.9500 . ? C14 C15 1.410(6) . ? C15 C16 1.388(7) . ? C15 C33 1.496(7) . ? C16 C17 1.407(6) . ? C17 C18 1.359(7) . ? C17 H17 0.9500 . ? C18 C19 1.436(6) . ? C18 H18 0.9500 . ? C19 C20 1.388(6) . ? C20 C39 1.497(6) . ? C21 C22 1.365(7) . ? C21 C26 1.411(7) . ? C22 C23 1.390(7) . ? C22 H22 0.9500 . ? C23 C24 1.391(8) . ? C23 H23 0.9500 . ? C24 C25 1.370(8) . ? C24 H24 0.9500 . ? C25 C26 1.379(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.392(6) . ? C27 C28 1.411(7) . ? C28 C29 1.379(7) . ? C28 H28 0.9500 . ? C29 C30 1.374(7) . ? C29 H29 0.9500 . ? C30 C31 1.380(7) . ? C30 H30 0.9500 . ? C31 C32 1.373(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.326(8) . ? C33 C38 1.365(7) . ? C34 C35 1.395(8) . ? C34 H34 0.9500 . ? C35 C36 1.325(8) . ? C35 H35 0.9500 . ? C36 C37 1.318(8) . ? C36 H36 0.9500 . ? C37 C38 1.387(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.376(7) . ? C39 C44 1.394(7) . ? C40 C41 1.401(7) . ? C40 H40 0.9500 . ? C41 C42 1.378(8) . ? C41 H41 0.9500 . ? C42 C43 1.370(8) . ? C42 H42 0.9500 . ? C43 C44 1.407(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.367(7) . ? C45 C49 1.393(7) . ? C46 C47 1.380(7) . ? C46 H46 0.9500 . ? C47 C50' 1.418(7) . ? C47 C50 1.588(8) . ? C48 C49 1.370(7) . ? C48 C56 1.464(7) . ? C48 C56' 1.577(8) . ? C49 H49 0.9500 . ? C50 C51 1.3900 . ? C50 N55 1.3900 . ? C51 C52 1.3900 . ? C51 H51 0.9500 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 N55 1.3900 . ? C54 H54 0.9500 . ? C50' C51' 1.3900 . ? C50' N55' 1.3900 . ? C51' C52' 1.3900 . ? C51' H51' 0.9500 . ? C52' C53' 1.3900 . ? C52' H52' 0.9500 . ? C53' C54' 1.3900 . ? C53' H53' 0.9500 . ? C54' N55' 1.3900 . ? C54' H54' 0.9500 . ? C56 C57 1.3900 . ? C56 N61 1.3900 . ? C57 C58 1.3900 . ? C57 H57 0.9500 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 N61 1.3900 . ? C60 H60 0.9500 . ? C56' N61' 1.3900 . ? C56' C57' 1.3900 . ? N61' C60' 1.3900 . ? C60' C59' 1.3900 . ? C60' H60' 0.9500 . ? C59' C58' 1.3900 . ? C59' H59' 0.9500 . ? C58' C57' 1.3900 . ? C58' H58' 0.9500 . ? C57' H57' 0.9500 . ? 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 C1 N1 C4 105.8(4) . . ? C9 N2 C6 110.0(4) . . ? C9 N2 H2 125.0 . . ? C6 N2 H2 125.0 . . ? C11 N3 C14 105.9(4) . . ? C19 N4 C16 109.9(4) . . ? C19 N4 H4 125.1 . . ? C16 N4 H4 125.1 . . ? C48 N5 C47 118.7(5) . . ? N1 C1 C20 126.2(4) . . ? N1 C1 C2 111.1(4) . . ? C20 C1 C2 122.7(4) . . ? C3 C2 C1 107.2(4) . . ? C3 C2 H2A 126.4 . . ? C1 C2 H2A 126.4 . . ? C2 C3 C4 106.0(4) . . ? C2 C3 C45 122.3(5) . . ? C4 C3 C45 131.7(5) . . ? N1 C4 C5 124.0(4) . . ? N1 C4 C3 109.8(4) . . ? C5 C4 C3 126.2(5) . . ? C4 C5 C6 125.7(5) . . ? C4 C5 C21 119.9(5) . . ? C6 C5 C21 114.4(5) . . ? N2 C6 C7 107.5(4) . . ? N2 C6 C5 127.2(5) . . ? C7 C6 C5 125.3(5) . . ? C8 C7 C6 108.3(5) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? C7 C8 C9 107.2(5) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C10 127.4(5) . . ? N2 C9 C8 107.0(5) . . ? C10 C9 C8 125.7(5) . . ? C9 C10 C11 124.6(5) . . ? C9 C10 C27 117.0(4) . . ? C11 C10 C27 118.4(5) . . ? N3 C11 C10 125.1(5) . . ? N3 C11 C12 110.6(4) . . ? C10 C11 C12 124.3(5) . . ? C13 C12 C11 107.1(4) . . ? C13 C12 H12 126.5 . . ? C11 C12 H12 126.5 . . ? C12 C13 C14 105.9(4) . . ? C12 C13 H13 127.0 . . ? C14 C13 H13 127.0 . . ? N3 C14 C15 126.2(5) . . ? N3 C14 C13 110.5(4) . . ? C15 C14 C13 123.3(5) . . ? C16 C15 C14 125.5(4) . . ? C16 C15 C33 116.1(4) . . ? C14 C15 C33 118.4(4) . . ? N4 C16 C15 126.9(5) . . ? N4 C16 C17 107.0(4) . . ? C15 C16 C17 126.0(4) . . ? C18 C17 C16 109.2(4) . . ? C18 C17 H17 125.4 . . ? C16 C17 H17 125.4 . . ? C17 C18 C19 106.9(5) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? N4 C19 C20 127.2(4) . . ? N4 C19 C18 107.1(4) . . ? C20 C19 C18 125.7(5) . . ? C19 C20 C1 124.9(4) . . ? C19 C20 C39 117.8(4) . . ? C1 C20 C39 117.3(4) . . ? C22 C21 C26 117.8(5) . . ? C22 C21 C5 123.0(5) . . ? C26 C21 C5 119.2(5) . . ? C21 C22 C23 121.6(5) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C24 119.8(6) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 119.6(5) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.3(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 121.0(5) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C32 C27 C28 117.2(5) . . ? C32 C27 C10 122.4(4) . . ? C28 C27 C10 120.3(4) . . ? C29 C28 C27 120.8(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C30 C29 C28 120.6(5) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 119.3(5) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 120.8(5) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C27 121.3(5) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C34 C33 C38 115.8(5) . . ? C34 C33 C15 122.9(5) . . ? C38 C33 C15 121.3(5) . . ? C33 C34 C35 123.8(6) . . ? C33 C34 H34 118.1 . . ? C35 C34 H34 118.1 . . ? C36 C35 C34 118.5(6) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C37 C36 C35 120.2(6) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.8(6) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C33 C38 C37 120.9(6) . . ? C33 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C44 118.6(5) . . ? C40 C39 C20 120.7(5) . . ? C44 C39 C20 120.6(5) . . ? C39 C40 C41 121.3(5) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 119.3(6) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C43 C42 C41 120.6(5) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 119.9(6) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C39 C44 C43 120.2(6) . . ? C39 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C46 C45 C49 117.6(5) . . ? C46 C45 C3 121.3(5) . . ? C49 C45 C3 121.0(5) . . ? C45 C46 C47 121.3(5) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? N5 C47 C46 120.4(5) . . ? N5 C47 C50' 115.4(5) . . ? C46 C47 C50' 123.5(5) . . ? N5 C47 C50 117.1(5) . . ? C46 C47 C50 121.6(5) . . ? N5 C48 C49 122.5(5) . . ? N5 C48 C56 115.1(5) . . ? C49 C48 C56 120.3(6) . . ? N5 C48 C56' 116.8(5) . . ? C49 C48 C56' 119.6(6) . . ? C48 C49 C45 119.3(5) . . ? C48 C49 H49 120.4 . . ? C45 C49 H49 120.4 . . ? C51 C50 N55 120.0 . . ? C51 C50 C47 116.5(5) . . ? N55 C50 C47 123.2(5) . . ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? N55 C54 C53 120.0 . . ? N55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 N55 C50 120.0 . . ? C51' C50' N55' 120.0 . . ? C51' C50' C47 118.7(5) . . ? N55' C50' C47 121.0(5) . . ? C50' C51' C52' 120.0 . . ? C50' C51' H51' 120.0 . . ? C52' C51' H51' 120.0 . . ? C53' C52' C51' 120.0 . . ? C53' C52' H52' 120.0 . . ? C51' C52' H52' 120.0 . . ? C52' C53' C54' 120.0 . . ? C52' C53' H53' 120.0 . . ? C54' C53' H53' 120.0 . . ? C53' C54' N55' 120.0 . . ? C53' C54' H54' 120.0 . . ? N55' C54' H54' 120.0 . . ? C54' N55' C50' 120.0 . . ? C57 C56 N61 120.0 . . ? C57 C56 C48 112.8(6) . . ? N61 C56 C48 127.1(6) . . ? C56 C57 C58 120.0 . . ? C56 C57 H57 120.0 . . ? C58 C57 H57 120.0 . . ? C59 C58 C57 120.0 . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C60 120.0 . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? N61 C60 C59 120.0 . . ? N61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 N61 C56 120.0 . . ? N61' C56' C57' 120.0 . . ? N61' C56' C48 120.8(5) . . ? C57' C56' C48 118.6(5) . . ? C60' N61' C56' 120.0 . . ? N61' C60' C59' 120.0 . . ? N61' C60' H60' 120.0 . . ? C59' C60' H60' 120.0 . . ? C60' C59' C58' 120.0 . . ? C60' C59' H59' 120.0 . . ? C58' C59' H59' 120.0 . . ? C59' C58' C57' 120.0 . . ? C59' C58' H58' 120.0 . . ? C57' C58' H58' 120.0 . . ? C58' C57' C56' 120.0 . . ? C58' C57' H57' 120.0 . . ? C56' C57' H57' 120.0 . . ? 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 C4 N1 C1 C20 -179.9(5) . . . . ? C4 N1 C1 C2 -0.6(6) . . . . ? N1 C1 C2 C3 -1.3(6) . . . . ? C20 C1 C2 C3 178.0(5) . . . . ? C1 C2 C3 C4 2.5(6) . . . . ? C1 C2 C3 C45 -176.3(5) . . . . ? C1 N1 C4 C5 -175.8(5) . . . . ? C1 N1 C4 C3 2.2(6) . . . . ? C2 C3 C4 N1 -3.1(6) . . . . ? C45 C3 C4 N1 175.7(5) . . . . ? C2 C3 C4 C5 174.9(5) . . . . ? C45 C3 C4 C5 -6.4(9) . . . . ? N1 C4 C5 C6 -4.1(9) . . . . ? C3 C4 C5 C6 178.2(5) . . . . ? N1 C4 C5 C21 175.4(5) . . . . ? C3 C4 C5 C21 -2.3(8) . . . . ? C9 N2 C6 C7 0.9(6) . . . . ? C9 N2 C6 C5 -177.6(6) . . . . ? C4 C5 C6 N2 -5.9(9) . . . . ? C21 C5 C6 N2 174.5(5) . . . . ? C4 C5 C6 C7 176.0(5) . . . . ? C21 C5 C6 C7 -3.6(8) . . . . ? N2 C6 C7 C8 -1.6(7) . . . . ? C5 C6 C7 C8 176.9(6) . . . . ? C6 C7 C8 C9 1.6(7) . . . . ? C6 N2 C9 C10 179.0(5) . . . . ? C6 N2 C9 C8 0.1(6) . . . . ? C7 C8 C9 N2 -1.1(7) . . . . ? C7 C8 C9 C10 -180.0(6) . . . . ? N2 C9 C10 C11 5.2(9) . . . . ? C8 C9 C10 C11 -176.1(6) . . . . ? N2 C9 C10 C27 -176.0(5) . . . . ? C8 C9 C10 C27 2.7(8) . . . . ? C14 N3 C11 C10 177.6(5) . . . . ? C14 N3 C11 C12 -1.7(5) . . . . ? C9 C10 C11 N3 0.7(8) . . . . ? C27 C10 C11 N3 -178.1(5) . . . . ? C9 C10 C11 C12 179.9(5) . . . . ? C27 C10 C11 C12 1.1(7) . . . . ? N3 C11 C12 C13 2.4(6) . . . . ? C10 C11 C12 C13 -176.8(5) . . . . ? C11 C12 C13 C14 -2.0(6) . . . . ? C11 N3 C14 C15 -178.8(5) . . . . ? C11 N3 C14 C13 0.4(5) . . . . ? C12 C13 C14 N3 1.1(6) . . . . ? C12 C13 C14 C15 -179.7(5) . . . . ? N3 C14 C15 C16 -2.4(8) . . . . ? C13 C14 C15 C16 178.5(5) . . . . ? N3 C14 C15 C33 176.5(5) . . . . ? C13 C14 C15 C33 -2.6(7) . . . . ? C19 N4 C16 C15 176.8(5) . . . . ? C19 N4 C16 C17 -0.5(5) . . . . ? C14 C15 C16 N4 -1.8(8) . . . . ? C33 C15 C16 N4 179.3(5) . . . . ? C14 C15 C16 C17 175.0(5) . . . . ? C33 C15 C16 C17 -3.9(8) . . . . ? N4 C16 C17 C18 0.1(6) . . . . ? C15 C16 C17 C18 -177.2(5) . . . . ? C16 C17 C18 C19 0.3(6) . . . . ? C16 N4 C19 C20 -178.3(5) . . . . ? C16 N4 C19 C18 0.7(6) . . . . ? C17 C18 C19 N4 -0.6(6) . . . . ? C17 C18 C19 C20 178.4(5) . . . . ? N4 C19 C20 C1 1.3(8) . . . . ? C18 C19 C20 C1 -177.5(5) . . . . ? N4 C19 C20 C39 177.8(5) . . . . ? C18 C19 C20 C39 -0.9(8) . . . . ? N1 C1 C20 C19 5.4(8) . . . . ? C2 C1 C20 C19 -173.7(5) . . . . ? N1 C1 C20 C39 -171.1(5) . . . . ? C2 C1 C20 C39 9.7(7) . . . . ? C4 C5 C21 C22 -68.9(7) . . . . ? C6 C5 C21 C22 110.7(6) . . . . ? C4 C5 C21 C26 111.8(6) . . . . ? C6 C5 C21 C26 -68.6(7) . . . . ? C26 C21 C22 C23 -2.3(8) . . . . ? C5 C21 C22 C23 178.3(5) . . . . ? C21 C22 C23 C24 0.5(8) . . . . ? C22 C23 C24 C25 1.2(8) . . . . ? C23 C24 C25 C26 -1.1(8) . . . . ? C24 C25 C26 C21 -0.8(8) . . . . ? C22 C21 C26 C25 2.5(8) . . . . ? C5 C21 C26 C25 -178.1(5) . . . . ? C9 C10 C27 C32 -122.5(6) . . . . ? C11 C10 C27 C32 56.4(7) . . . . ? C9 C10 C27 C28 58.1(7) . . . . ? C11 C10 C27 C28 -123.0(5) . . . . ? C32 C27 C28 C29 0.7(8) . . . . ? C10 C27 C28 C29 -179.8(5) . . . . ? C27 C28 C29 C30 -1.1(8) . . . . ? C28 C29 C30 C31 0.1(8) . . . . ? C29 C30 C31 C32 1.2(8) . . . . ? C30 C31 C32 C27 -1.6(8) . . . . ? C28 C27 C32 C31 0.7(8) . . . . ? C10 C27 C32 C31 -178.8(5) . . . . ? C16 C15 C33 C34 -87.6(7) . . . . ? C14 C15 C33 C34 93.4(7) . . . . ? C16 C15 C33 C38 90.9(7) . . . . ? C14 C15 C33 C38 -88.1(7) . . . . ? C38 C33 C34 C35 0.0(12) . . . . ? C15 C33 C34 C35 178.6(7) . . . . ? C33 C34 C35 C36 0.3(13) . . . . ? C34 C35 C36 C37 -1.0(12) . . . . ? C35 C36 C37 C38 1.4(12) . . . . ? C34 C33 C38 C37 0.3(10) . . . . ? C15 C33 C38 C37 -178.3(6) . . . . ? C36 C37 C38 C33 -1.0(12) . . . . ? C19 C20 C39 C40 -117.6(6) . . . . ? C1 C20 C39 C40 59.2(6) . . . . ? C19 C20 C39 C44 63.6(6) . . . . ? C1 C20 C39 C44 -119.6(5) . . . . ? C44 C39 C40 C41 -0.4(7) . . . . ? C20 C39 C40 C41 -179.2(4) . . . . ? C39 C40 C41 C42 0.5(8) . . . . ? C40 C41 C42 C43 0.0(8) . . . . ? C41 C42 C43 C44 -0.4(8) . . . . ? C40 C39 C44 C43 -0.1(7) . . . . ? C20 C39 C44 C43 178.7(4) . . . . ? C42 C43 C44 C39 0.5(7) . . . . ? C2 C3 C45 C46 -61.9(8) . . . . ? C4 C3 C45 C46 119.6(6) . . . . ? C2 C3 C45 C49 114.6(6) . . . . ? C4 C3 C45 C49 -63.9(8) . . . . ? C49 C45 C46 C47 1.8(8) . . . . ? C3 C45 C46 C47 178.4(5) . . . . ? C48 N5 C47 C46 -2.7(9) . . . . ? C48 N5 C47 C50' 168.0(6) . . . . ? C48 N5 C47 C50 -172.1(5) . . . . ? C45 C46 C47 N5 0.4(9) . . . . ? C45 C46 C47 C50' -169.6(6) . . . . ? C45 C46 C47 C50 169.2(5) . . . . ? C47 N5 C48 C49 2.9(9) . . . . ? C47 N5 C48 C56 166.6(6) . . . . ? C47 N5 C48 C56' -164.9(6) . . . . ? N5 C48 C49 C45 -0.7(9) . . . . ? C56 C48 C49 C45 -163.6(6) . . . . ? C56' C48 C49 C45 166.8(5) . . . . ? C46 C45 C49 C48 -1.7(8) . . . . ? C3 C45 C49 C48 -178.3(5) . . . . ? N5 C47 C50 C51 -147.7(5) . . . . ? C46 C47 C50 C51 43.0(7) . . . . ? C50' C47 C50 C51 -58.6(14) . . . . ? N5 C47 C50 N55 25.3(7) . . . . ? C46 C47 C50 N55 -143.9(5) . . . . ? C50' C47 C50 N55 114.4(16) . . . . ? N55 C50 C51 C52 0.0 . . . . ? C47 C50 C51 C52 173.3(6) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 N55 0.0 . . . . ? C53 C54 N55 C50 0.0 . . . . ? C51 C50 N55 C54 0.0 . . . . ? C47 C50 N55 C54 -172.8(6) . . . . ? N5 C47 C50' C51' 164.3(5) . . . . ? C46 C47 C50' C51' -25.2(8) . . . . ? C50 C47 C50' C51' 64.6(14) . . . . ? N5 C47 C50' N55' -9.8(8) . . . . ? C46 C47 C50' N55' 160.6(5) . . . . ? C50 C47 C50' N55' -109.6(16) . . . . ? N55' C50' C51' C52' 0.0 . . . . ? C47 C50' C51' C52' -174.2(6) . . . . ? C50' C51' C52' C53' 0.0 . . . . ? C51' C52' C53' C54' 0.0 . . . . ? C52' C53' C54' N55' 0.0 . . . . ? C53' C54' N55' C50' 0.0 . . . . ? C51' C50' N55' C54' 0.0 . . . . ? C47 C50' N55' C54' 174.1(6) . . . . ? N5 C48 C56 C57 152.6(5) . . . . ? C49 C48 C56 C57 -43.3(8) . . . . ? C56' C48 C56 C57 52.7(9) . . . . ? N5 C48 C56 N61 -24.2(9) . . . . ? C49 C48 C56 N61 139.8(6) . . . . ? C56' C48 C56 N61 -124.2(12) . . . . ? N61 C56 C57 C58 0.0 . . . . ? C48 C56 C57 C58 -177.1(6) . . . . ? C56 C57 C58 C59 0.0 . . . . ? C57 C58 C59 C60 0.0 . . . . ? C58 C59 C60 N61 0.0 . . . . ? C59 C60 N61 C56 0.0 . . . . ? C57 C56 N61 C60 0.0 . . . . ? C48 C56 N61 C60 176.7(7) . . . . ? N5 C48 C56' N61' 14.7(8) . . . . ? C49 C48 C56' N61' -153.6(5) . . . . ? C56 C48 C56' N61' 107.4(11) . . . . ? N5 C48 C56' C57' -156.1(5) . . . . ? C49 C48 C56' C57' 35.7(7) . . . . ? C56 C48 C56' C57' -63.4(10) . . . . ? C57' C56' N61' C60' 0.0 . . . . ? C48 C56' N61' C60' -170.6(6) . . . . ? C56' N61' C60' C59' 0.0 . . . . ? N61' C60' C59' C58' 0.0 . . . . ? C60' C59' C58' C57' 0.0 . . . . ? C59' C58' C57' C56' 0.0 . . . . ? N61' C56' C57' C58' 0.0 . . . . ? C48 C56' C57' C58' 170.8(6) . . . . ? # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.010 0.000 0.000 268 84 ' ' 2 0.000 0.500 0.000 13 2 ' ' 3 0.021 0.236 0.500 7 0 ' ' 4 0.979 0.764 0.500 7 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.793 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.068 #============================================================================== # END #==============================================================================