data_exp_3894-sr _audit_creation_date 2014-07-27 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C84 H41 N3 O' _chemical_formula_sum 'C84 H41 N3 O' _chemical_formula_weight 1108.20 _chemical_melting_point ? _chemical_oxdiff_formula C77H22N3O1 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.1629(8) _cell_length_b 20.3663(4) _cell_length_c 19.4299(3) _cell_angle_alpha 90 _cell_angle_beta 104.204(2) _cell_angle_gamma 90 _cell_volume 13105.5(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 29154 _cell_measurement_temperature 180.00(10) _cell_measurement_theta_max 28.8950 _cell_measurement_theta_min 3.2770 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour '' _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description '' _exptl_crystal_F_000 4592 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0361 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 96995 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.022 _diffrn_reflns_theta_min 3.063 _diffrn_ambient_temperature 180.00(10) _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.9980 _diffrn_measured_fraction_theta_max 0.9131 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -7.00 60.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 10.8579 -111.0000 -33.0643 67 #__ type_ start__ end____ width___ exp.time_ 2 omega -45.00 40.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 10.8579 -57.0000 -180.0000 85 #__ type_ start__ end____ width___ exp.time_ 3 omega -14.00 67.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 10.8579 77.0000 30.0000 81 #__ type_ start__ end____ width___ exp.time_ 4 omega -5.00 87.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 10.8579 38.0000 150.0000 92 #__ type_ start__ end____ width___ exp.time_ 5 omega -59.00 37.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 10.8579 -38.0000 90.0000 96 #__ type_ start__ end____ width___ exp.time_ 6 omega -20.00 92.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - 10.8579 19.0000 -90.0000 112 #__ type_ start__ end____ width___ exp.time_ 7 omega -20.00 30.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - -11.7173 -99.0000 -120.0000 50 #__ type_ start__ end____ width___ exp.time_ 8 omega -70.00 -24.00 1.0000 35.0000 omega____ theta____ kappa____ phi______ frames - -11.7173 126.0000 -20.1878 46 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0047861000 _diffrn_orient_matrix_UB_12 -0.0322739000 _diffrn_orient_matrix_UB_13 0.0089794000 _diffrn_orient_matrix_UB_21 -0.0207029000 _diffrn_orient_matrix_UB_22 0.0059260000 _diffrn_orient_matrix_UB_23 -0.0159516000 _diffrn_orient_matrix_UB_31 0.0027159000 _diffrn_orient_matrix_UB_32 -0.0116771000 _diffrn_orient_matrix_UB_33 -0.0328947000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9286 _reflns_number_total 12844 _reflns_odcompleteness_completeness 99.80 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 0.449 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.084 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 796 _refine_ls_number_reflns 12844 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0817 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1490P)^2^+12.5457P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2338 _refine_ls_wR_factor_ref 0.2481 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Riding coordinates: C3(H3), C9(H9), C15(H15) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B) 2.c Aromatic/amide H refined with riding coordinates: C20(H20), C21(H21), C22(H22), C23(H23), C24(H24) 2.d Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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 C1 C 0.40336(11) 0.80367(17) 0.01360(18) 0.0476(8) Uani 1 1 d . . . . . H1A H 0.3889 0.7786 -0.0286 0.057 Uiso 1 1 calc R U . . . H1B H 0.4290 0.7806 0.0348 0.057 Uiso 1 1 calc R U . . . C2 C 0.41226(12) 0.87218(18) -0.0084(2) 0.0552(9) Uani 1 1 d . . . . . H2A H 0.4290 0.8955 0.0333 0.066 Uiso 1 1 calc R U . . . H2B H 0.4281 0.8691 -0.0447 0.066 Uiso 1 1 calc R U . . . C3 C 0.37466(13) 0.91135(19) -0.03799(19) 0.0584(10) Uani 1 1 d . . . . . H3 H 0.3596 0.8902 -0.0832 0.070 Uiso 1 1 d R U . . . C4 C 0.34818(11) 0.91043(16) 0.01367(17) 0.0465(8) Uani 1 1 d . . . . . H4A H 0.3221 0.9318 -0.0084 0.056 Uiso 1 1 calc R U . . . H4B H 0.3613 0.9359 0.0565 0.056 Uiso 1 1 calc R U . . . C5 C 0.34048(10) 0.84087(15) 0.03515(17) 0.0415(7) Uani 1 1 d . . . . . H5A H 0.3239 0.8421 0.0703 0.050 Uiso 1 1 calc R U . . . H5B H 0.3252 0.8165 -0.0070 0.050 Uiso 1 1 calc R U . . . C6 C 0.38467(16) 0.9810(2) -0.0542(3) 0.0791(13) Uani 1 1 d . . . . . H6A H 0.4032 1.0001 -0.0124 0.119 Uiso 1 1 calc R U . . . H6B H 0.3598 1.0070 -0.0667 0.119 Uiso 1 1 calc R U . . . H6C H 0.3975 0.9810 -0.0941 0.119 Uiso 1 1 calc R U . . . C7 C 0.46509(9) 0.77670(18) 0.31942(19) 0.0501(8) Uani 1 1 d . . . . . H7A H 0.4785 0.7609 0.2828 0.060 Uiso 1 1 calc R U . . . H7B H 0.4697 0.7440 0.3583 0.060 Uiso 1 1 calc R U . . . C8 C 0.48270(11) 0.8433(2) 0.3484(2) 0.0639(11) Uani 1 1 d . . . . . H8A H 0.5123 0.8392 0.3673 0.077 Uiso 1 1 calc R U . . . H8B H 0.4776 0.8759 0.3095 0.077 Uiso 1 1 calc R U . . . C9 C 0.46356(11) 0.8669(2) 0.4074(2) 0.0605(10) Uani 1 1 d . . . . . H9 H 0.4694 0.8340 0.4467 0.073 Uiso 1 1 d R U . . . C10 C 0.41872(10) 0.86985(16) 0.37682(18) 0.0453(8) Uani 1 1 d . . . . . H10A H 0.4126 0.9049 0.3405 0.054 Uiso 1 1 calc R U . . . H10B H 0.4054 0.8816 0.4150 0.054 Uiso 1 1 calc R U . . . C11 C 0.40149(10) 0.80592(16) 0.34360(16) 0.0416(7) Uani 1 1 d . . . . . H11A H 0.4050 0.7717 0.3808 0.050 Uiso 1 1 calc R U . . . H11B H 0.3722 0.8113 0.3226 0.050 Uiso 1 1 calc R U . . . C12 C 0.47986(14) 0.9335(3) 0.4369(3) 0.0908(17) Uani 1 1 d . . . . . H12A H 0.4781 0.9645 0.3976 0.136 Uiso 1 1 calc R U . . . H12B H 0.5081 0.9289 0.4632 0.136 Uiso 1 1 calc R U . . . H12C H 0.4639 0.9500 0.4687 0.136 Uiso 1 1 calc R U . . . C13 C 0.34274(9) 0.69428(14) 0.44369(13) 0.0338(6) Uani 1 1 d . . . . . H13A H 0.3705 0.6772 0.4495 0.041 Uiso 1 1 calc R U . . . H13B H 0.3256 0.6579 0.4531 0.041 Uiso 1 1 calc R U . . . C14 C 0.34309(10) 0.74889(15) 0.49605(14) 0.0399(7) Uani 1 1 d . . . . . H14A H 0.3616 0.7840 0.4882 0.048 Uiso 1 1 calc R U . . . H14B H 0.3535 0.7319 0.5448 0.048 Uiso 1 1 calc R U . . . C15 C 0.30132(10) 0.77748(15) 0.48901(14) 0.0403(7) Uani 1 1 d . . . . . H15 H 0.2840 0.7423 0.5021 0.048 Uiso 1 1 d R U . . . C16 C 0.28333(11) 0.79546(16) 0.41140(15) 0.0434(7) Uani 1 1 d . . . . . H16A H 0.2547 0.8082 0.4054 0.052 Uiso 1 1 calc R U . . . H16B H 0.2979 0.8340 0.3991 0.052 Uiso 1 1 calc R U . . . C17 C 0.28558(10) 0.74041(15) 0.36106(15) 0.0384(7) Uani 1 1 d . . . . . H17A H 0.2685 0.7034 0.3695 0.046 Uiso 1 1 calc R U . . . H17B H 0.2750 0.7556 0.3116 0.046 Uiso 1 1 calc R U . . . C18 C 0.30114(14) 0.8355(2) 0.5377(2) 0.0629(10) Uani 1 1 d . . . . . H18A H 0.3119 0.8219 0.5871 0.094 Uiso 1 1 calc R U . . . H18B H 0.2734 0.8514 0.5315 0.094 Uiso 1 1 calc R U . . . H18C H 0.3179 0.8707 0.5259 0.094 Uiso 1 1 calc R U . . . C19 C 0.21752(8) 0.69099(13) 0.20039(14) 0.0297(6) Uani 1 1 d . . . . . C20 C 0.19220(10) 0.66243(17) 0.23773(18) 0.0462(8) Uani 1 1 d . . . . . H20 H 0.1995 0.6218 0.2615 0.055 Uiso 1 1 calc R U . . . C21 C 0.15613(11) 0.69302(19) 0.2406(2) 0.0549(9) Uani 1 1 d . . . . . H21 H 0.1399 0.6745 0.2688 0.066 Uiso 1 1 calc R U . . . C22 C 0.14384(10) 0.74948(18) 0.20309(19) 0.0505(8) Uani 1 1 d . . . . . H22 H 0.1186 0.7688 0.2034 0.061 Uiso 1 1 calc R U . . . C23 C 0.16851(10) 0.77806(16) 0.16499(16) 0.0414(7) Uani 1 1 d . . . . . H23 H 0.1610 0.8186 0.1413 0.050 Uiso 1 1 calc R U . . . C24 C 0.20440(9) 0.74740(14) 0.16135(15) 0.0360(6) Uani 1 1 d . . . . . H24 H 0.2201 0.7653 0.1318 0.043 Uiso 1 1 calc R U . . . C84 C 0.41038(8) 0.70326(14) 0.12633(14) 0.0318(6) Uani 1 1 d . . . . . C25 C 0.30142(8) 0.72626(12) 0.12673(13) 0.0255(5) Uani 1 1 d . . . . . C26 C 0.34528(8) 0.74217(12) 0.14515(13) 0.0258(5) Uani 1 1 d . . . . . C27 C 0.35876(8) 0.73122(12) 0.21557(13) 0.0248(5) Uani 1 1 d . . . . . C28 C 0.32541(8) 0.70556(12) 0.24455(12) 0.0248(5) Uani 1 1 d . . . . . C29 C 0.29108(8) 0.70207(12) 0.19233(12) 0.0241(5) Uani 1 1 d . . . . . C30 C 0.25586(8) 0.65651(13) 0.19257(13) 0.0281(6) Uani 1 1 d . . . . . C31 C 0.24793(8) 0.61440(13) 0.12349(13) 0.0281(6) Uani 1 1 d . . . . . C32 C 0.25798(8) 0.63280(13) 0.06275(13) 0.0293(6) Uani 1 1 d . . . . . C33 C 0.28361(8) 0.69206(13) 0.05891(12) 0.0263(5) Uani 1 1 d . . . . . C34 C 0.31168(8) 0.67257(13) 0.01464(12) 0.0282(6) Uani 1 1 d . . . . . C35 C 0.35170(9) 0.69127(13) 0.03208(13) 0.0304(6) Uani 1 1 d . . . . . C36 C 0.37115(8) 0.74065(13) 0.09126(13) 0.0285(6) Uani 1 1 d . . . . . C37 C 0.42444(8) 0.69550(14) 0.19921(13) 0.0294(6) Uani 1 1 d . . . . . C38 C 0.40304(8) 0.72280(13) 0.25355(13) 0.0280(6) Uani 1 1 d . . . . . C39 C 0.40534(8) 0.66252(13) 0.30346(13) 0.0290(6) Uani 1 1 d . . . . . C40 C 0.37461(8) 0.64032(13) 0.33082(12) 0.0281(6) Uani 1 1 d . . . . . C41 C 0.33245(8) 0.67151(13) 0.31544(12) 0.0267(5) Uani 1 1 d . . . . . C42 C 0.30571(8) 0.60893(12) 0.30359(12) 0.0266(5) Uani 1 1 d . . . . . C43 C 0.27170(8) 0.60227(12) 0.24828(13) 0.0271(5) Uani 1 1 d . . . . . C44 C 0.26163(9) 0.53880(13) 0.21638(14) 0.0319(6) Uani 1 1 d . . . . . C45 C 0.24651(8) 0.54703(14) 0.14079(14) 0.0317(6) Uani 1 1 d . . . . . C46 C 0.25394(9) 0.49826(14) 0.09400(15) 0.0353(6) Uani 1 1 d . . . . . C47 C 0.26453(9) 0.51782(15) 0.03059(14) 0.0363(7) Uani 1 1 d . . . . . C48 C 0.26722(8) 0.58409(14) 0.01587(13) 0.0316(6) Uani 1 1 d . . . . . C49 C 0.30012(9) 0.60832(14) -0.01302(13) 0.0327(6) Uani 1 1 d . . . . . C50 C 0.32881(9) 0.56450(15) -0.02605(13) 0.0362(7) Uani 1 1 d . . . . . C51 C 0.37076(9) 0.58304(15) -0.00784(13) 0.0355(6) Uani 1 1 d . . . . . C52 C 0.38148(9) 0.64501(14) 0.02200(13) 0.0327(6) Uani 1 1 d . . . . . C53 C 0.41713(8) 0.65184(15) 0.07969(14) 0.0337(6) Uani 1 1 d . . . . . C54 C 0.44013(9) 0.59652(15) 0.10566(15) 0.0370(7) Uani 1 1 d . . . . . C55 C 0.45539(8) 0.58884(15) 0.18151(14) 0.0357(6) Uani 1 1 d . . . . . C56 C 0.44637(8) 0.63613(15) 0.22640(14) 0.0337(6) Uani 1 1 d . . . . . C57 C 0.43506(8) 0.61712(14) 0.29018(13) 0.0320(6) Uani 1 1 d . . . . . C58 C 0.43353(9) 0.55118(15) 0.30734(14) 0.0367(7) Uani 1 1 d . . . . . C59 C 0.40164(9) 0.52735(14) 0.33597(13) 0.0353(7) Uani 1 1 d . . . . . C60 C 0.37224(9) 0.57162(13) 0.34525(13) 0.0304(6) Uani 1 1 d . . . . . C61 C 0.32998(9) 0.55240(13) 0.32814(13) 0.0300(6) Uani 1 1 d . . . . . C62 C 0.31881(10) 0.48976(13) 0.30062(14) 0.0346(6) Uani 1 1 d . . . . . C63 C 0.28401(9) 0.48326(13) 0.24294(15) 0.0347(6) Uani 1 1 d . . . . . C64 C 0.29220(10) 0.43368(13) 0.19484(15) 0.0379(7) Uani 1 1 d . . . . . C65 C 0.27729(10) 0.44111(14) 0.12285(16) 0.0401(7) Uani 1 1 d . . . . . C66 C 0.30300(11) 0.42466(14) 0.07442(16) 0.0422(7) Uani 1 1 d . . . . . C67 C 0.29485(10) 0.47202(14) 0.01737(14) 0.0380(7) Uani 1 1 d . . . . . C68 C 0.32645(10) 0.49506(14) -0.00979(14) 0.0371(7) Uani 1 1 d . . . . . C69 C 0.36714(10) 0.47198(15) 0.01838(14) 0.0390(7) Uani 1 1 d . . . . . C70 C 0.39463(10) 0.52538(16) 0.01984(14) 0.0400(7) Uani 1 1 d . . . . . C71 C 0.42875(9) 0.53273(16) 0.07561(14) 0.0404(7) Uani 1 1 d . . . . . C72 C 0.43675(9) 0.48462(16) 0.13258(15) 0.0408(7) Uani 1 1 d . . . . . C73 C 0.45341(9) 0.52050(16) 0.19817(15) 0.0400(7) Uani 1 1 d . . . . . C74 C 0.44269(10) 0.50107(16) 0.26016(15) 0.0413(7) Uani 1 1 d . . . . . C75 C 0.41527(10) 0.44695(15) 0.25915(15) 0.0411(7) Uani 1 1 d . . . . . C76 C 0.38975(10) 0.46255(14) 0.30628(15) 0.0399(7) Uani 1 1 d . . . . . C77 C 0.34965(10) 0.44484(14) 0.28891(15) 0.0386(7) Uani 1 1 d . . . . . C78 C 0.33259(11) 0.40960(13) 0.22335(16) 0.0403(7) Uani 1 1 d . . . . . C79 C 0.35720(11) 0.39416(14) 0.17822(16) 0.0409(7) Uani 1 1 d . . . . . C80 C 0.39949(10) 0.41293(15) 0.19621(16) 0.0425(7) Uani 1 1 d . . . . . C81 C 0.41045(11) 0.43238(15) 0.13193(17) 0.0461(8) Uani 1 1 d . . . . . C82 C 0.37495(10) 0.42512(15) 0.07326(16) 0.0427(7) Uani 1 1 d . . . . . C83 C 0.34176(11) 0.40205(14) 0.10195(16) 0.0416(7) Uani 1 1 d . . . . . N1 N 0.37840(7) 0.80684(12) 0.06569(12) 0.0346(5) Uani 1 1 d . . . . . N2 N 0.42131(7) 0.78459(12) 0.28817(11) 0.0324(5) Uani 1 1 d . . . . . N3 N 0.32718(7) 0.71800(11) 0.37068(11) 0.0286(5) Uani 1 1 d . . . . . O1 O 0.27214(5) 0.75753(9) 0.06935(9) 0.0282(4) Uani 1 1 d . . . . . 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 C1 0.0471(19) 0.057(2) 0.0430(17) 0.0040(15) 0.0197(15) -0.0089(16) C2 0.060(2) 0.058(2) 0.055(2) -0.0019(17) 0.0269(18) -0.0157(18) C3 0.071(3) 0.057(2) 0.0420(18) 0.0172(16) 0.0050(17) -0.0126(19) C4 0.0465(19) 0.0423(17) 0.0445(17) 0.0070(14) -0.0008(14) -0.0063(14) C5 0.0415(17) 0.0402(16) 0.0406(16) 0.0110(13) 0.0061(13) 0.0002(13) C6 0.097(3) 0.069(3) 0.079(3) 0.028(2) 0.036(3) -0.015(2) C7 0.0311(16) 0.066(2) 0.0508(18) -0.0217(17) 0.0060(14) -0.0026(15) C8 0.0314(18) 0.088(3) 0.069(2) -0.033(2) 0.0053(17) -0.0087(18) C9 0.0398(19) 0.072(2) 0.059(2) -0.0288(19) -0.0082(16) 0.0024(17) C10 0.0427(18) 0.0454(17) 0.0465(17) -0.0159(14) 0.0085(14) -0.0013(14) C11 0.0410(17) 0.0454(17) 0.0380(15) -0.0129(13) 0.0092(13) -0.0007(14) C12 0.050(2) 0.097(3) 0.116(4) -0.055(3) 0.000(3) -0.003(2) C13 0.0414(16) 0.0381(15) 0.0206(12) 0.0044(11) 0.0049(11) 0.0061(12) C14 0.0513(19) 0.0433(16) 0.0233(13) -0.0014(12) 0.0055(13) 0.0013(14) C15 0.0518(19) 0.0439(16) 0.0275(14) -0.0053(12) 0.0139(13) 0.0079(14) C16 0.057(2) 0.0440(16) 0.0318(15) 0.0034(13) 0.0149(14) 0.0184(15) C17 0.0439(17) 0.0410(16) 0.0297(14) 0.0025(12) 0.0082(13) 0.0104(13) C18 0.077(3) 0.067(2) 0.0467(19) -0.0148(18) 0.0184(19) 0.012(2) C19 0.0337(15) 0.0280(13) 0.0289(13) -0.0003(10) 0.0105(11) 0.0008(11) C20 0.0385(17) 0.0477(18) 0.0555(19) 0.0138(15) 0.0175(15) 0.0027(14) C21 0.0423(19) 0.065(2) 0.064(2) 0.0097(18) 0.0247(17) -0.0061(17) C22 0.0334(17) 0.063(2) 0.055(2) 0.0054(17) 0.0112(15) 0.0135(16) C23 0.0414(17) 0.0407(16) 0.0398(16) -0.0033(13) 0.0058(13) 0.0071(13) C24 0.0390(16) 0.0396(15) 0.0301(13) 0.0057(12) 0.0097(12) 0.0010(13) C84 0.0298(14) 0.0388(15) 0.0278(13) 0.0001(11) 0.0092(11) -0.0034(12) C25 0.0267(13) 0.0291(12) 0.0193(11) 0.0042(10) 0.0028(10) 0.0000(10) C26 0.0271(13) 0.0267(12) 0.0226(12) 0.0019(10) 0.0043(10) 0.0007(10) C27 0.0267(13) 0.0245(12) 0.0221(11) 0.0002(9) 0.0038(10) 0.0022(10) C28 0.0280(13) 0.0269(12) 0.0184(11) -0.0002(9) 0.0034(10) 0.0034(10) C29 0.0304(13) 0.0239(12) 0.0187(11) 0.0010(9) 0.0071(10) 0.0012(10) C30 0.0319(14) 0.0313(13) 0.0208(11) 0.0016(10) 0.0056(10) -0.0028(11) C31 0.0212(13) 0.0351(14) 0.0260(12) 0.0005(11) 0.0019(10) -0.0012(10) C32 0.0257(13) 0.0338(14) 0.0241(12) -0.0006(11) -0.0024(10) -0.0018(11) C33 0.0264(13) 0.0328(13) 0.0174(11) 0.0054(10) 0.0012(10) 0.0017(10) C34 0.0324(14) 0.0379(14) 0.0142(11) 0.0047(10) 0.0055(10) 0.0008(11) C35 0.0364(15) 0.0378(14) 0.0175(11) 0.0041(10) 0.0076(11) -0.0014(12) C36 0.0285(13) 0.0336(13) 0.0231(12) 0.0008(10) 0.0059(10) -0.0012(11) C37 0.0232(13) 0.0380(14) 0.0250(12) -0.0046(11) 0.0020(10) -0.0026(11) C38 0.0261(13) 0.0340(14) 0.0220(12) -0.0021(10) 0.0024(10) -0.0027(11) C39 0.0325(14) 0.0317(13) 0.0189(11) -0.0020(10) -0.0009(10) 0.0050(11) C40 0.0359(15) 0.0320(13) 0.0143(11) -0.0009(10) 0.0024(10) 0.0054(11) C41 0.0314(14) 0.0311(13) 0.0172(11) 0.0028(10) 0.0053(10) 0.0049(11) C42 0.0367(14) 0.0284(12) 0.0161(11) 0.0032(9) 0.0090(10) 0.0041(11) C43 0.0321(14) 0.0272(12) 0.0251(12) 0.0008(10) 0.0127(11) 0.0011(11) C44 0.0377(15) 0.0341(14) 0.0263(13) 0.0016(11) 0.0126(12) -0.0074(12) C45 0.0291(14) 0.0353(14) 0.0290(13) 0.0004(11) 0.0036(11) -0.0058(11) C46 0.0408(16) 0.0337(14) 0.0298(14) -0.0051(11) 0.0058(12) -0.0096(12) C47 0.0380(16) 0.0430(16) 0.0234(13) -0.0064(11) -0.0009(12) -0.0088(13) C48 0.0317(14) 0.0405(15) 0.0173(11) -0.0017(10) -0.0044(10) -0.0033(12) C49 0.0367(15) 0.0419(15) 0.0156(11) -0.0001(10) -0.0010(11) 0.0001(12) C50 0.0445(17) 0.0479(16) 0.0153(11) -0.0060(11) 0.0054(11) 0.0011(13) C51 0.0392(16) 0.0477(16) 0.0192(12) -0.0050(11) 0.0067(11) 0.0026(13) C52 0.0365(15) 0.0438(15) 0.0215(12) 0.0021(11) 0.0144(11) 0.0023(12) C53 0.0278(14) 0.0489(16) 0.0264(13) -0.0013(12) 0.0105(11) 0.0004(12) C54 0.0358(16) 0.0482(17) 0.0291(14) -0.0044(12) 0.0118(12) 0.0070(13) C55 0.0282(14) 0.0505(17) 0.0265(13) -0.0011(12) 0.0028(11) 0.0118(13) C56 0.0208(13) 0.0501(17) 0.0272(13) -0.0036(12) 0.0003(10) 0.0030(12) C57 0.0270(14) 0.0448(15) 0.0198(11) -0.0033(11) -0.0026(10) 0.0087(12) C58 0.0366(16) 0.0421(16) 0.0271(13) -0.0014(12) -0.0008(12) 0.0176(13) C59 0.0469(17) 0.0356(14) 0.0192(12) 0.0031(11) -0.0001(12) 0.0153(13) C60 0.0389(15) 0.0324(13) 0.0169(11) 0.0021(10) 0.0014(11) 0.0092(12) C61 0.0442(16) 0.0284(13) 0.0186(11) 0.0041(10) 0.0098(11) 0.0057(12) C62 0.0528(18) 0.0261(13) 0.0251(13) 0.0068(10) 0.0098(12) 0.0020(12) C63 0.0442(17) 0.0255(13) 0.0358(14) 0.0042(11) 0.0125(13) -0.0025(12) C64 0.0528(19) 0.0259(13) 0.0349(14) 0.0025(11) 0.0104(13) -0.0023(13) C65 0.0529(19) 0.0261(13) 0.0400(15) -0.0044(12) 0.0090(14) -0.0079(13) C66 0.061(2) 0.0295(14) 0.0345(15) -0.0107(12) 0.0096(14) -0.0014(14) C67 0.0491(18) 0.0369(15) 0.0249(13) -0.0108(11) 0.0032(12) -0.0046(13) C68 0.0488(18) 0.0395(15) 0.0206(12) -0.0107(11) 0.0040(12) 0.0025(13) C69 0.0525(19) 0.0418(16) 0.0230(13) -0.0121(12) 0.0098(13) 0.0064(14) C70 0.0458(18) 0.0503(17) 0.0246(13) -0.0083(12) 0.0098(12) 0.0082(14) C71 0.0392(16) 0.0571(19) 0.0263(13) -0.0102(13) 0.0107(12) 0.0132(14) C72 0.0393(17) 0.0527(18) 0.0311(14) -0.0055(13) 0.0100(13) 0.0213(14) C73 0.0318(15) 0.0538(18) 0.0312(14) -0.0048(13) 0.0018(12) 0.0193(13) C74 0.0417(17) 0.0476(17) 0.0293(14) -0.0021(12) -0.0015(12) 0.0246(14) C75 0.0542(19) 0.0373(15) 0.0292(14) 0.0059(12) 0.0052(13) 0.0196(14) C76 0.0515(19) 0.0349(15) 0.0308(14) 0.0064(12) 0.0053(13) 0.0201(14) C77 0.057(2) 0.0297(14) 0.0285(13) 0.0047(11) 0.0096(13) 0.0065(13) C78 0.062(2) 0.0238(13) 0.0346(14) 0.0021(11) 0.0118(14) 0.0054(13) C79 0.059(2) 0.0283(14) 0.0356(15) -0.0037(12) 0.0112(14) 0.0102(13) C80 0.0514(19) 0.0343(15) 0.0380(15) -0.0012(12) 0.0038(14) 0.0188(14) C81 0.060(2) 0.0372(16) 0.0396(16) -0.0084(13) 0.0102(15) 0.0224(15) C82 0.055(2) 0.0360(15) 0.0360(15) -0.0143(12) 0.0093(14) 0.0119(14) C83 0.061(2) 0.0302(14) 0.0346(15) -0.0073(12) 0.0130(14) 0.0078(14) N1 0.0317(13) 0.0425(13) 0.0300(11) 0.0014(10) 0.0084(10) -0.0027(10) N2 0.0278(12) 0.0398(13) 0.0272(11) -0.0086(10) 0.0021(9) -0.0013(10) N3 0.0373(13) 0.0307(11) 0.0179(10) -0.0004(8) 0.0069(9) 0.0055(10) O1 0.0278(10) 0.0344(10) 0.0189(8) 0.0037(7) -0.0011(7) 0.0000(8) _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. ; 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 C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.512(5) . ? C1 N1 1.476(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.501(6) . ? C3 H3 1.0001 . ? C3 C4 1.507(5) . ? C3 C6 1.510(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.518(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 N1 1.461(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.534(5) . ? C7 N2 1.478(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.530(5) . ? C9 H9 0.9999 . ? C9 C10 1.502(5) . ? C9 C12 1.523(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.507(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 N2 1.471(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.505(4) . ? C13 N3 1.469(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.516(5) . ? C15 H15 1.0002 . ? C15 C16 1.527(4) . ? C15 C18 1.514(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.502(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 N3 1.461(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.386(4) . ? C19 C24 1.389(4) . ? C19 C30 1.526(4) . ? C20 H20 0.9500 . ? C20 C21 1.394(5) . ? C21 H21 0.9500 . ? C21 C22 1.371(5) . ? C22 H22 0.9500 . ? C22 C23 1.380(5) . ? C23 H23 0.9500 . ? C23 C24 1.393(4) . ? C24 H24 0.9500 . ? C84 C36 1.547(4) . ? C84 C37 1.388(4) . ? C84 C53 1.440(4) . ? C25 C26 1.488(4) . ? C25 C29 1.488(3) . ? C25 C33 1.483(3) . ? C25 O1 1.450(3) . ? C26 C27 1.351(3) . ? C26 C36 1.527(4) . ? C27 C28 1.484(4) . ? C27 C38 1.521(4) . ? C28 C29 1.351(4) . ? C28 C41 1.508(3) . ? C29 C30 1.520(4) . ? C30 C31 1.559(4) . ? C30 C43 1.548(3) . ? C31 C32 1.360(4) . ? C31 C45 1.416(4) . ? C32 C33 1.504(4) . ? C32 C48 1.433(4) . ? C33 C34 1.491(4) . ? C33 O1 1.418(3) . ? C34 C35 1.379(4) . ? C34 C49 1.433(4) . ? C35 C36 1.549(4) . ? C35 C52 1.435(4) . ? C36 N1 1.478(4) . ? C37 C38 1.529(4) . ? C37 C56 1.452(4) . ? C38 C39 1.554(4) . ? C38 N2 1.490(3) . ? C39 C40 1.365(4) . ? C39 C57 1.443(4) . ? C40 C41 1.535(4) . ? C40 C60 1.433(4) . ? C41 C42 1.552(4) . ? C41 N3 1.475(3) . ? C42 C43 1.382(4) . ? C42 C61 1.431(4) . ? C43 C44 1.438(4) . ? C44 C45 1.442(4) . ? C44 C63 1.392(4) . ? C45 C46 1.411(4) . ? C46 C47 1.424(4) . ? C46 C65 1.444(4) . ? C47 C48 1.387(4) . ? C47 C67 1.463(4) . ? C48 C49 1.460(4) . ? C49 C50 1.394(4) . ? C50 C51 1.440(4) . ? C50 C68 1.456(4) . ? C51 C52 1.400(4) . ? C51 C70 1.455(4) . ? C52 C53 1.445(4) . ? C53 C54 1.395(4) . ? C54 C55 1.446(4) . ? C54 C71 1.438(4) . ? C55 C56 1.384(4) . ? C55 C73 1.434(5) . ? C56 C57 1.439(4) . ? C57 C58 1.388(4) . ? C58 C59 1.424(4) . ? C58 C74 1.456(4) . ? C59 C60 1.394(4) . ? C59 C76 1.458(4) . ? C60 C61 1.453(4) . ? C61 C62 1.400(4) . ? C62 C63 1.426(4) . ? C62 C77 1.455(4) . ? C63 C64 1.449(4) . ? C64 C65 1.375(4) . ? C64 C78 1.441(5) . ? C65 C66 1.475(5) . ? C66 C67 1.444(4) . ? C66 C83 1.380(5) . ? C67 C68 1.394(4) . ? C68 C69 1.442(4) . ? C69 C70 1.432(5) . ? C69 C82 1.407(4) . ? C70 C71 1.391(4) . ? C71 C72 1.453(4) . ? C72 C73 1.458(4) . ? C72 C81 1.391(5) . ? C73 C74 1.399(5) . ? C74 C75 1.444(5) . ? C75 C76 1.446(4) . ? C75 C80 1.394(4) . ? C76 C77 1.376(5) . ? C77 C78 1.454(4) . ? C78 C79 1.392(4) . ? C79 C80 1.452(5) . ? C79 C83 1.455(4) . ? C80 C81 1.444(5) . ? C81 C82 1.454(5) . ? C82 C83 1.459(5) . ? 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 H1A C1 H1B 108.2 . . ? C2 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? N1 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? N1 C1 C2 110.1(3) . . ? C1 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C3 C2 C1 112.7(3) . . ? C3 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C2 C3 H3 108.4 . . ? C2 C3 C4 109.6(3) . . ? C2 C3 C6 111.3(4) . . ? C4 C3 H3 108.4 . . ? C4 C3 C6 110.7(3) . . ? C6 C3 H3 108.4 . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C3 C4 C5 111.6(3) . . ? H4A C4 H4B 108.0 . . ? C5 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C4 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N1 C5 C4 111.0(3) . . ? N1 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? H7A C7 H7B 108.3 . . ? C8 C7 H7A 109.9 . . ? C8 C7 H7B 109.9 . . ? N2 C7 H7A 109.9 . . ? N2 C7 H7B 109.9 . . ? N2 C7 C8 108.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C9 C8 C7 110.6(3) . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C8 C9 H9 108.7 . . ? C10 C9 C8 107.3(3) . . ? C10 C9 H9 108.7 . . ? C10 C9 C12 110.9(3) . . ? C12 C9 C8 112.2(4) . . ? C12 C9 H9 108.9 . . ? C9 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? C9 C10 C11 112.9(3) . . ? H10A C10 H10B 107.8 . . ? C11 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? C10 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N2 C11 C10 111.5(3) . . ? N2 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H13A C13 H13B 108.1 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? N3 C13 C14 110.5(2) . . ? C13 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C13 C14 C15 111.8(3) . . ? H14A C14 H14B 107.9 . . ? C15 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C14 C15 H15 107.7 . . ? C14 C15 C16 108.8(2) . . ? C16 C15 H15 107.7 . . ? C18 C15 C14 113.0(3) . . ? C18 C15 H15 107.8 . . ? C18 C15 C16 111.5(3) . . ? C15 C16 H16A 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C17 C16 C15 113.1(2) . . ? C17 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N3 C17 C16 110.7(3) . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 118.3(3) . . ? C20 C19 C30 121.3(2) . . ? C24 C19 C30 119.8(2) . . ? C19 C20 H20 119.9 . . ? C19 C20 C21 120.3(3) . . ? C21 C20 H20 119.9 . . ? C20 C21 H21 119.6 . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C21 C22 H22 120.3 . . ? C21 C22 C23 119.4(3) . . ? C23 C22 H22 120.3 . . ? C22 C23 H23 120.0 . . ? C22 C23 C24 119.9(3) . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 120.9(3) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C37 C84 C36 123.4(2) . . ? C37 C84 C53 119.4(3) . . ? C53 C84 C36 109.6(2) . . ? C29 C25 C26 107.6(2) . . ? C33 C25 C26 119.0(2) . . ? C33 C25 C29 118.3(2) . . ? O1 C25 C26 123.6(2) . . ? O1 C25 C29 122.7(2) . . ? O1 C25 C33 57.84(15) . . ? C25 C26 C36 123.3(2) . . ? C27 C26 C25 106.3(2) . . ? C27 C26 C36 125.5(2) . . ? C26 C27 C28 109.9(2) . . ? C26 C27 C38 124.1(2) . . ? C28 C27 C38 122.7(2) . . ? C27 C28 C41 122.9(2) . . ? C29 C28 C27 109.8(2) . . ? C29 C28 C41 125.2(2) . . ? C25 C29 C30 124.0(2) . . ? C28 C29 C25 106.3(2) . . ? C28 C29 C30 124.9(2) . . ? C19 C30 C31 111.5(2) . . ? C19 C30 C43 114.8(2) . . ? C29 C30 C19 114.7(2) . . ? C29 C30 C31 107.7(2) . . ? C29 C30 C43 107.2(2) . . ? C43 C30 C31 99.6(2) . . ? C32 C31 C30 124.6(2) . . ? C32 C31 C45 120.2(2) . . ? C45 C31 C30 109.7(2) . . ? C31 C32 C33 122.6(2) . . ? C31 C32 C48 120.2(2) . . ? C48 C32 C33 107.6(2) . . ? C25 C33 C32 116.7(2) . . ? C25 C33 C34 117.1(2) . . ? C34 C33 C32 106.3(2) . . ? O1 C33 C25 59.93(15) . . ? O1 C33 C32 124.2(2) . . ? O1 C33 C34 124.9(2) . . ? C35 C34 C33 121.6(2) . . ? C35 C34 C49 120.6(3) . . ? C49 C34 C33 107.6(2) . . ? C34 C35 C36 125.5(2) . . ? C34 C35 C52 118.6(3) . . ? C52 C35 C36 109.8(2) . . ? C84 C36 C35 100.1(2) . . ? C26 C36 C84 107.0(2) . . ? C26 C36 C35 107.9(2) . . ? N1 C36 C84 113.5(2) . . ? N1 C36 C26 112.6(2) . . ? N1 C36 C35 114.8(2) . . ? C84 C37 C38 124.0(2) . . ? C84 C37 C56 119.0(2) . . ? C56 C37 C38 110.1(2) . . ? C27 C38 C37 107.05(19) . . ? C27 C38 C39 106.5(2) . . ? C37 C38 C39 100.6(2) . . ? N2 C38 C27 112.4(2) . . ? N2 C38 C37 113.6(2) . . ? N2 C38 C39 115.7(2) . . ? C40 C39 C38 125.3(2) . . ? C40 C39 C57 120.0(2) . . ? C57 C39 C38 108.9(2) . . ? C39 C40 C41 124.2(2) . . ? C39 C40 C60 119.0(2) . . ? C60 C40 C41 110.3(2) . . ? C28 C41 C40 107.5(2) . . ? C28 C41 C42 106.6(2) . . ? C40 C41 C42 100.3(2) . . ? N3 C41 C28 110.4(2) . . ? N3 C41 C40 113.6(2) . . ? N3 C41 C42 117.6(2) . . ? C43 C42 C41 123.2(2) . . ? C43 C42 C61 119.2(2) . . ? C61 C42 C41 109.8(2) . . ? C42 C43 C30 123.8(2) . . ? C42 C43 C44 119.3(2) . . ? C44 C43 C30 109.5(2) . . ? C43 C44 C45 108.8(2) . . ? C63 C44 C43 121.3(3) . . ? C63 C44 C45 119.9(2) . . ? C31 C45 C44 109.2(2) . . ? C46 C45 C31 120.5(2) . . ? C46 C45 C44 119.9(3) . . ? C45 C46 C47 119.0(3) . . ? C45 C46 C65 119.1(3) . . ? C47 C46 C65 109.1(3) . . ? C46 C47 C67 108.3(3) . . ? C48 C47 C46 119.6(3) . . ? C48 C47 C67 119.9(3) . . ? C32 C48 C49 108.7(2) . . ? C47 C48 C32 120.4(2) . . ? C47 C48 C49 120.3(3) . . ? C34 C49 C48 109.4(2) . . ? C50 C49 C34 120.8(3) . . ? C50 C49 C48 119.7(3) . . ? C49 C50 C51 119.3(3) . . ? C49 C50 C68 120.2(3) . . ? C51 C50 C68 107.8(3) . . ? C50 C51 C70 108.2(3) . . ? C52 C51 C50 118.8(3) . . ? C52 C51 C70 120.6(3) . . ? C35 C52 C53 108.8(2) . . ? C51 C52 C35 121.8(3) . . ? C51 C52 C53 119.5(3) . . ? C84 C53 C52 108.9(2) . . ? C54 C53 C84 121.5(2) . . ? C54 C53 C52 119.7(3) . . ? C53 C54 C55 119.1(2) . . ? C53 C54 C71 120.7(3) . . ? C71 C54 C55 108.1(3) . . ? C56 C55 C54 119.1(3) . . ? C56 C55 C73 120.2(3) . . ? C73 C55 C54 108.0(3) . . ? C55 C56 C37 121.7(2) . . ? C55 C56 C57 120.3(3) . . ? C57 C56 C37 108.3(2) . . ? C56 C57 C39 109.3(2) . . ? C58 C57 C39 120.5(3) . . ? C58 C57 C56 120.1(2) . . ? C57 C58 C59 120.1(3) . . ? C57 C58 C74 120.0(3) . . ? C59 C58 C74 108.1(3) . . ? C58 C59 C76 108.6(2) . . ? C60 C59 C58 118.3(3) . . ? C60 C59 C76 119.8(3) . . ? C40 C60 C61 108.6(2) . . ? C59 C60 C40 121.9(3) . . ? C59 C60 C61 120.2(3) . . ? C42 C61 C60 108.7(2) . . ? C62 C61 C42 121.6(3) . . ? C62 C61 C60 119.7(3) . . ? C61 C62 C63 118.8(2) . . ? C61 C62 C77 119.5(3) . . ? C63 C62 C77 108.4(2) . . ? C44 C63 C62 119.5(2) . . ? C44 C63 C64 120.2(3) . . ? C62 C63 C64 108.4(3) . . ? C65 C64 C63 119.9(3) . . ? C65 C64 C78 120.6(3) . . ? C78 C64 C63 107.9(3) . . ? C46 C65 C66 107.1(3) . . ? C64 C65 C46 121.0(3) . . ? C64 C65 C66 119.6(3) . . ? C67 C66 C65 107.8(3) . . ? C83 C66 C65 119.6(3) . . ? C83 C66 C67 120.4(3) . . ? C66 C67 C47 107.6(3) . . ? C68 C67 C47 119.9(3) . . ? C68 C67 C66 119.6(3) . . ? C67 C68 C50 119.9(3) . . ? C67 C68 C69 120.7(3) . . ? C69 C68 C50 107.4(3) . . ? C70 C69 C68 109.0(3) . . ? C82 C69 C68 119.6(3) . . ? C82 C69 C70 119.9(3) . . ? C69 C70 C51 107.5(3) . . ? C71 C70 C51 119.2(3) . . ? C71 C70 C69 121.1(3) . . ? C54 C71 C72 108.6(2) . . ? C70 C71 C54 120.3(3) . . ? C70 C71 C72 119.1(3) . . ? C71 C72 C73 106.7(3) . . ? C81 C72 C71 120.6(3) . . ? C81 C72 C73 120.3(3) . . ? C55 C73 C72 108.6(3) . . ? C74 C73 C55 120.4(3) . . ? C74 C73 C72 118.8(3) . . ? C73 C74 C58 119.1(3) . . ? C73 C74 C75 120.7(3) . . ? C75 C74 C58 107.7(3) . . ? C74 C75 C76 108.3(3) . . ? C80 C75 C74 120.1(3) . . ? C80 C75 C76 120.1(3) . . ? C75 C76 C59 107.3(3) . . ? C77 C76 C59 119.9(3) . . ? C77 C76 C75 120.4(3) . . ? C76 C77 C62 120.8(3) . . ? C76 C77 C78 120.4(3) . . ? C78 C77 C62 107.3(3) . . ? C64 C78 C77 108.0(3) . . ? C79 C78 C64 120.3(3) . . ? C79 C78 C77 119.3(3) . . ? C78 C79 C80 120.5(3) . . ? C78 C79 C83 119.5(3) . . ? C80 C79 C83 107.9(3) . . ? C75 C80 C79 119.3(3) . . ? C75 C80 C81 119.7(3) . . ? C81 C80 C79 108.5(3) . . ? C72 C81 C80 120.4(3) . . ? C72 C81 C82 119.9(3) . . ? C80 C81 C82 107.9(3) . . ? C69 C82 C81 119.5(3) . . ? C69 C82 C83 119.2(3) . . ? C81 C82 C83 108.1(3) . . ? C66 C83 C79 120.4(3) . . ? C66 C83 C82 120.4(3) . . ? C79 C83 C82 107.7(3) . . ? C1 N1 C36 111.3(2) . . ? C5 N1 C1 110.3(2) . . ? C5 N1 C36 111.4(2) . . ? C7 N2 C38 111.3(2) . . ? C11 N2 C7 109.4(2) . . ? C11 N2 C38 111.3(2) . . ? C13 N3 C41 114.3(2) . . ? C17 N3 C13 109.7(2) . . ? C17 N3 C41 113.3(2) . . ? C33 O1 C25 62.24(16) . . ? _platon_squeeze_details ; ; # SQUEEZE RESULTS (APPEND TO CIF) # 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 0.000 0.003 -0.003 2329 534 ' ' 2 0.500 0.071 0.047 2330 534 ' ' 3 0.351 0.567 0.160 23 4 ' ' 4 0.851 0.067 0.160 23 4 ' ' 5 0.304 0.281 0.146 7 1 ' ' 6 0.804 0.781 0.146 7 1 ' ' 7 0.149 0.067 0.340 23 3 ' ' 8 0.649 0.567 0.340 23 3 ' ' 9 0.196 0.781 0.354 7 1 ' ' 10 0.696 0.281 0.354 7 1 ' ' 11 0.351 0.433 0.660 23 4 ' ' 12 0.851 0.933 0.660 23 4 ' ' 13 0.304 0.719 0.646 7 1 ' ' 14 0.804 0.219 0.646 7 1 ' ' 15 0.149 0.933 0.839 23 3 ' ' 16 0.649 0.433 0.839 23 3 ' ' 17 0.196 0.219 0.854 7 1 ' ' 18 0.696 0.719 0.854 7 1 ' ' _shelx_estimated_absorpt_T_max 0.997 _shelx_estimated_absorpt_T_min 0.993 _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. ; _shelxl_version_number 2013-3