# Electronic Supplementary Material (ESI) for Chemical Science # 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_2011sot0753 _database_code_depnum_ccdc_archive 'CCDC 892348' #TrackingRef '2011sot0753.cif' #BISMNO2 HCO3 _audit_creation_method SHELXL-97 _chemical_compound_source 'Stephen Moore' _database_code_CSD 11ST0753 _database_code_depnum_ccdc_archive ? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C20 H16 N6 O6), 2(C8 H20 N), C O3' _chemical_formula_sum 'C57 H72 N14 O15' _chemical_formula_weight 1193.29 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.1445(18) _cell_length_b 14.338(2) _cell_length_c 16.719(3) _cell_angle_alpha 86.271(8) _cell_angle_beta 81.687(8) _cell_angle_gamma 61.358(5) _cell_volume 2944.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9250 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9882 _exptl_absorpt_correction_T_max 0.9921 _exptl_absorpt_process_details ; Jacobson, R. (1998). REQAB. Private communication to the Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_source_power 2.475 _diffrn_source_voltage 45.0 _diffrn_source_current 55.0 _diffrn_source 'Rotating Anode' _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_collimation 'Confocal mirrors, VHF Varimax ' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_device 'four-circle \k diffractometer' _diffrn_measurement_device_type 'Rigaku AFC12 (Right)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'MiTeGen MicroMesh' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33949 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13317 _reflns_number_gt 10816 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Images generated using CrystalMaker: a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd, Oxford, England (www.crystalmaker.com) ; _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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. The counter-ions balancing the 2 negative charges of the carbonate ion comprise 1 whole and 2 half TEA molecules. The 2 half molecules lie on inversion centres and were refined using thermal parameter and geometrical restraints. ; _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^)+(0.0632P)^2^+1.2345P] 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 13317 _refine_ls_number_parameters 770 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.007 _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 N14 N 0.5000 0.0000 0.0000 0.0408(7) Uani 1 2 d SDU . . C50A C 0.5788(4) -0.1031(4) 0.0007(3) 0.0428(4) Uani 0.50 1 d PD A 1 H50A H 0.6144 -0.1242 -0.0555 0.051 Uiso 0.50 1 calc PR A 1 H50B H 0.5435 -0.1476 0.0182 0.051 Uiso 0.50 1 calc PR A 1 C51A C 0.6690(5) -0.1295(5) 0.0556(4) 0.0428(4) Uani 0.50 1 d PD A 1 H51A H 0.7212 -0.2055 0.0513 0.064 Uiso 0.50 1 calc PR A 1 H51B H 0.6357 -0.1116 0.1118 0.064 Uiso 0.50 1 calc PR A 1 H51C H 0.7067 -0.0880 0.0380 0.064 Uiso 0.50 1 calc PR A 1 C52A C 0.4655(4) -0.0852(4) 0.0343(3) 0.0428(4) Uani 0.50 1 d PD A 1 H52A H 0.4137 -0.0862 0.0009 0.051 Uiso 0.50 1 calc PR A 1 H52B H 0.5304 -0.1563 0.0306 0.051 Uiso 0.50 1 calc PR A 1 C53A C 0.4126(5) -0.0621(4) 0.1225(3) 0.0428(4) Uani 0.50 1 d PD A 1 H53A H 0.3923 -0.1169 0.1418 0.064 Uiso 0.50 1 calc PR A 1 H53B H 0.3475 0.0077 0.1263 0.064 Uiso 0.50 1 calc PR A 1 H53C H 0.4642 -0.0623 0.1560 0.064 Uiso 0.50 1 calc PR A 1 C50B C 0.5928(4) -0.0160(4) 0.0487(3) 0.0428(4) Uani 0.50 1 d PD A 2 H50C H 0.6161 0.0373 0.0289 0.051 Uiso 0.50 1 calc PR A 2 H50D H 0.5603 0.0023 0.1057 0.051 Uiso 0.50 1 calc PR A 2 C51B C 0.6911(4) -0.1187(4) 0.0487(4) 0.0428(4) Uani 0.50 1 d PD A 2 H51D H 0.7534 -0.1122 0.0204 0.064 Uiso 0.50 1 calc PR A 2 H51E H 0.6822 -0.1717 0.0211 0.064 Uiso 0.50 1 calc PR A 2 H51F H 0.7036 -0.1410 0.1046 0.064 Uiso 0.50 1 calc PR A 2 C52B C 0.4390(4) 0.0530(4) 0.0848(3) 0.0428(4) Uani 0.50 1 d PD A 2 H52C H 0.4916 0.0556 0.1166 0.051 Uiso 0.50 1 calc PR A 2 H52D H 0.3829 0.1270 0.0765 0.051 Uiso 0.50 1 calc PR A 2 C53B C 0.3851(5) -0.0072(4) 0.1329(3) 0.0428(4) Uani 0.50 1 d PD A 2 H53D H 0.3070 0.0408 0.1457 0.064 Uiso 0.50 1 calc PR A 2 H53E H 0.4173 -0.0337 0.1831 0.064 Uiso 0.50 1 calc PR A 2 H53F H 0.3964 -0.0672 0.1006 0.064 Uiso 0.50 1 calc PR A 2 N15 N 0.0000 0.0000 0.0000 0.0403(7) Uani 1 2 d SDU . . C54A C 0.1049(4) -0.0032(4) 0.0166(3) 0.0396(4) Uani 0.50 1 d PD B 3 H54A H 0.1617 -0.0472 -0.0271 0.048 Uiso 0.50 1 calc PR B 3 H54B H 0.0941 0.0701 0.0079 0.048 Uiso 0.50 1 calc PR B 3 C55A C 0.1517(5) -0.0381(5) 0.0891(4) 0.0396(4) Uani 0.50 1 d PD B 3 H55A H 0.2190 -0.0330 0.0845 0.059 Uiso 0.50 1 calc PR B 3 H55B H 0.1681 -0.1121 0.0991 0.059 Uiso 0.50 1 calc PR B 3 H55C H 0.1007 0.0066 0.1341 0.059 Uiso 0.50 1 calc PR B 3 C56A C -0.0773(4) 0.0282(4) 0.0820(3) 0.0396(4) Uani 0.50 1 d PD B 3 H56A H -0.1426 0.0221 0.0757 0.048 Uiso 0.50 1 calc PR B 3 H56B H -0.0395 -0.0225 0.1241 0.048 Uiso 0.50 1 calc PR B 3 C57A C -0.1112(4) 0.1415(4) 0.1081(3) 0.0396(4) Uani 0.50 1 d PD B 3 H57A H -0.1595 0.1582 0.1594 0.059 Uiso 0.50 1 calc PR B 3 H57B H -0.1494 0.1917 0.0666 0.059 Uiso 0.50 1 calc PR B 3 H57C H -0.0465 0.1472 0.1149 0.059 Uiso 0.50 1 calc PR B 3 C54B C 0.0375(4) -0.0494(4) 0.0681(3) 0.0396(4) Uani 0.50 1 d PD B 4 H54C H 0.0495 -0.1230 0.0642 0.048 Uiso 0.50 1 calc PR B 4 H54D H -0.0219 -0.0145 0.1128 0.048 Uiso 0.50 1 calc PR B 4 C55B C 0.1397(5) -0.0573(5) 0.0945(4) 0.0396(4) Uani 0.50 1 d PD B 4 H55D H 0.1533 -0.0957 0.1458 0.059 Uiso 0.50 1 calc PR B 4 H55E H 0.1298 0.0142 0.1016 0.059 Uiso 0.50 1 calc PR B 4 H55F H 0.2016 -0.0956 0.0532 0.059 Uiso 0.50 1 calc PR B 4 C56B C -0.0334(4) 0.1284(4) -0.0001(3) 0.0396(4) Uani 0.50 1 d PD B 4 H56C H 0.0332 0.1356 -0.0028 0.048 Uiso 0.50 1 calc PR B 4 H56D H -0.0691 0.1629 -0.0485 0.048 Uiso 0.50 1 calc PR B 4 C57B C -0.1094(4) 0.1836(4) 0.0753(3) 0.0396(4) Uani 0.50 1 d PD B 4 H57D H -0.1279 0.2589 0.0740 0.059 Uiso 0.50 1 calc PR B 4 H57E H -0.0736 0.1503 0.1232 0.059 Uiso 0.50 1 calc PR B 4 H57F H -0.1758 0.1775 0.0776 0.059 Uiso 0.50 1 calc PR B 4 O1 O 0.07225(19) 0.23801(17) 0.07120(15) 0.0652(6) Uani 1 1 d . C 4 O2 O 0.17987(17) 0.23199(14) 0.15344(13) 0.0548(5) Uani 1 1 d . C 4 O3 O -0.02525(12) 0.78041(12) 0.18380(10) 0.0351(4) Uani 1 1 d . C 4 O4 O 0.40694(12) 0.80053(12) 0.27496(11) 0.0366(4) Uani 1 1 d . C 4 O5 O 0.77127(13) 0.26186(13) 0.28199(12) 0.0481(5) Uani 1 1 d . C 4 O6 O 0.91771(13) 0.27817(14) 0.26737(14) 0.0559(5) Uani 1 1 d . C 4 N1 N 0.10263(19) 0.28120(17) 0.11520(14) 0.0457(5) Uani 1 1 d . C 4 N2 N 0.07623(14) 0.60296(13) 0.21215(11) 0.0278(4) Uani 1 1 d . C 4 H902 H 0.1314 0.5584 0.2373 0.033 Uiso 1 1 calc R C 4 N3 N 0.09717(13) 0.72670(13) 0.27547(11) 0.0280(4) Uani 1 1 d . C 4 H903 H 0.1391 0.6719 0.3035 0.034 Uiso 1 1 calc R C 4 N4 N 0.28457(13) 0.73606(12) 0.28993(10) 0.0245(4) Uani 1 1 d . C 4 H904 H 0.2803 0.6767 0.2929 0.029 Uiso 1 1 calc R C 4 N5 N 0.46540(13) 0.62040(13) 0.27620(10) 0.0249(4) Uani 1 1 d . C 4 H905 H 0.4434 0.5726 0.2755 0.030 Uiso 1 1 calc R C 4 N6 N 0.81839(15) 0.31625(15) 0.27473(12) 0.0370(5) Uani 1 1 d . C 4 C1 C 0.08513(18) 0.44691(17) 0.16212(13) 0.0311(5) Uani 1 1 d . C 4 H1 H 0.1494 0.4059 0.1865 0.037 Uiso 1 1 calc R C 4 C2 C 0.04324(19) 0.39792(19) 0.12086(15) 0.0357(5) Uani 1 1 d . C 4 C3 C -0.0498(2) 0.4527(2) 0.08412(16) 0.0419(6) Uani 1 1 d . C 4 H3 H -0.0773 0.4169 0.0566 0.050 Uiso 1 1 calc R C 4 C4 C -0.1013(2) 0.5629(2) 0.08939(16) 0.0419(6) Uani 1 1 d . C 4 H4 H -0.1653 0.6032 0.0645 0.050 Uiso 1 1 calc R C 4 C5 C -0.06211(18) 0.61593(19) 0.12997(14) 0.0351(5) Uani 1 1 d . C 4 H5 H -0.0987 0.6914 0.1323 0.042 Uiso 1 1 calc R C 4 C6 C 0.03174(17) 0.55769(17) 0.16751(13) 0.0292(5) Uani 1 1 d . C 4 C7 C 0.04309(16) 0.70992(16) 0.22112(13) 0.0276(4) Uani 1 1 d . C 4 C8 C 0.09037(17) 0.82617(16) 0.28974(13) 0.0278(4) Uani 1 1 d . C 4 C9 C -0.00929(18) 0.91894(18) 0.29658(15) 0.0374(5) Uani 1 1 d . C 4 H9 H -0.0738 0.9151 0.2932 0.045 Uiso 1 1 calc R C 4 C10 C -0.0156(2) 1.01661(18) 0.30829(17) 0.0434(6) Uani 1 1 d . C 4 H10 H -0.0837 1.0794 0.3116 0.052 Uiso 1 1 calc R C 4 C11 C 0.07761(19) 1.02232(17) 0.31509(16) 0.0392(6) Uani 1 1 d . C 4 H11 H 0.0732 1.0893 0.3232 0.047 Uiso 1 1 calc R C 4 C12 C 0.17791(18) 0.93102(16) 0.31014(14) 0.0324(5) Uani 1 1 d . C 4 H12 H 0.2413 0.9357 0.3159 0.039 Uiso 1 1 calc R C 4 C13 C 0.18560(16) 0.83183(15) 0.29660(12) 0.0258(4) Uani 1 1 d . C 4 C14 C 0.38643(16) 0.72641(16) 0.27923(12) 0.0253(4) Uani 1 1 d . C 4 C15 C 0.57716(16) 0.58301(16) 0.27409(12) 0.0236(4) Uani 1 1 d . C 4 C16 C 0.62657(17) 0.64821(17) 0.27014(14) 0.0320(5) Uani 1 1 d . C 4 H16 H 0.5837 0.7232 0.2677 0.038 Uiso 1 1 calc R C 4 C17 C 0.73797(18) 0.60295(19) 0.26985(15) 0.0370(5) Uani 1 1 d . C 4 H17 H 0.7704 0.6479 0.2682 0.044 Uiso 1 1 calc R C 4 C18 C 0.80283(18) 0.49434(19) 0.27186(14) 0.0354(5) Uani 1 1 d . C 4 H18 H 0.8792 0.4636 0.2716 0.042 Uiso 1 1 calc R C 4 C19 C 0.75233(17) 0.43206(17) 0.27421(13) 0.0289(5) Uani 1 1 d . C 4 C20 C 0.64127(16) 0.47323(16) 0.27591(12) 0.0247(4) Uani 1 1 d . C 4 H20 H 0.6096 0.4276 0.2783 0.030 Uiso 1 1 calc R C 4 O7 O -0.22726(15) 0.62866(18) 0.46877(14) 0.0637(6) Uani 1 1 d . D 4 O8 O -0.10958(15) 0.64380(15) 0.37755(13) 0.0517(5) Uani 1 1 d . D 4 O9 O 0.28934(13) 0.11116(13) 0.36823(10) 0.0376(4) Uani 1 1 d . D 4 O10 O 0.65379(11) 0.16336(11) 0.08129(9) 0.0269(3) Uani 1 1 d . D 4 O11 O 0.59125(18) 0.66956(14) 0.07938(11) 0.0537(5) Uani 1 1 d . D 4 O12 O 0.68125(15) 0.65970(13) -0.03843(10) 0.0426(4) Uani 1 1 d . D 4 N7 N -0.13836(17) 0.59121(19) 0.42623(15) 0.0471(6) Uani 1 1 d . D 4 N8 N 0.20935(14) 0.29106(15) 0.34337(11) 0.0290(4) Uani 1 1 d . D 4 H908 H 0.2212 0.3399 0.3161 0.035 Uiso 1 1 calc R D 4 N9 N 0.37980(14) 0.18400(14) 0.28257(10) 0.0284(4) Uani 1 1 d . D 4 H909 H 0.3682 0.2403 0.2525 0.034 Uiso 1 1 calc R D 4 N10 N 0.54536(13) 0.21956(13) 0.20319(10) 0.0243(4) Uani 1 1 d . D 4 H910 H 0.4978 0.2755 0.2325 0.029 Uiso 1 1 calc R D 4 N11 N 0.56273(14) 0.34034(13) 0.11638(10) 0.0261(4) Uani 1 1 d . D 4 H911 H 0.5119 0.3864 0.1517 0.031 Uiso 1 1 calc R D 4 N12 N 0.63819(16) 0.62394(14) 0.01454(11) 0.0314(4) Uani 1 1 d . D 4 C21 C 0.03610(18) 0.43501(19) 0.38613(14) 0.0329(5) Uani 1 1 d . D 4 H21 H 0.0554 0.4795 0.3507 0.039 Uiso 1 1 calc R D 4 C22 C -0.06414(19) 0.4768(2) 0.43349(15) 0.0380(5) Uani 1 1 d . D 4 C23 C -0.0960(2) 0.4155(2) 0.48682(16) 0.0456(6) Uani 1 1 d . D 4 H23 H -0.1646 0.4459 0.5195 0.055 Uiso 1 1 calc R D 4 C24 C -0.0236(2) 0.3086(2) 0.49016(15) 0.0454(6) Uani 1 1 d . D 4 H24 H -0.0433 0.2646 0.5258 0.055 Uiso 1 1 calc R D 4 C25 C 0.07703(19) 0.2633(2) 0.44304(14) 0.0378(5) Uani 1 1 d . D 4 H25 H 0.1247 0.1892 0.4461 0.045 Uiso 1 1 calc R D 4 C26 C 0.10823(17) 0.32691(19) 0.39107(13) 0.0305(5) Uani 1 1 d . D 4 C27 C 0.29185(17) 0.18849(18) 0.33440(12) 0.0281(4) Uani 1 1 d . D 4 C28 C 0.48598(17) 0.09793(16) 0.27338(12) 0.0252(4) Uani 1 1 d . D 4 C29 C 0.51239(19) -0.00489(17) 0.30126(13) 0.0313(5) Uani 1 1 d . D 4 H29 H 0.4564 -0.0199 0.3260 0.038 Uiso 1 1 calc R D 4 C30 C 0.61932(19) -0.08478(17) 0.29306(14) 0.0346(5) Uani 1 1 d . D 4 H30 H 0.6359 -0.1538 0.3129 0.041 Uiso 1 1 calc R D 4 C31 C 0.70251(18) -0.06553(17) 0.25630(14) 0.0330(5) Uani 1 1 d . D 4 H31 H 0.7758 -0.1205 0.2514 0.040 Uiso 1 1 calc R D 4 C32 C 0.67714(17) 0.03544(16) 0.22669(13) 0.0283(4) Uani 1 1 d . D 4 H32 H 0.7337 0.0491 0.2009 0.034 Uiso 1 1 calc R D 4 C33 C 0.57013(16) 0.11712(15) 0.23414(12) 0.0235(4) Uani 1 1 d . D 4 C34 C 0.59236(15) 0.23503(15) 0.12954(12) 0.0221(4) Uani 1 1 d . D 4 C35 C 0.60646(16) 0.38114(15) 0.05143(12) 0.0231(4) Uani 1 1 d . D 4 C36 C 0.64965(17) 0.33168(16) -0.02433(12) 0.0280(4) Uani 1 1 d . D 4 H36 H 0.6512 0.2663 -0.0337 0.034 Uiso 1 1 calc R D 4 C37 C 0.69033(18) 0.37761(17) -0.08595(13) 0.0308(5) Uani 1 1 d . D 4 H37 H 0.7201 0.3426 -0.1369 0.037 Uiso 1 1 calc R D 4 C38 C 0.68831(17) 0.47394(16) -0.07453(12) 0.0276(4) Uani 1 1 d . D 4 H38 H 0.7160 0.5057 -0.1165 0.033 Uiso 1 1 calc R D 4 C39 C 0.64398(16) 0.52120(15) 0.00085(12) 0.0234(4) Uani 1 1 d . D 4 C40 C 0.60334(16) 0.47769(15) 0.06386(12) 0.0236(4) Uani 1 1 d . D 4 H40 H 0.5739 0.5130 0.1146 0.028 Uiso 1 1 calc R D 4 O13 O 0.29023(13) 0.41407(13) 0.25668(9) 0.0344(4) Uani 1 1 d . E 4 O14 O 0.27071(12) 0.55152(11) 0.32518(9) 0.0328(4) Uani 1 1 d . E 4 O15 O 0.43384(11) 0.43768(11) 0.26377(9) 0.0279(3) Uani 1 1 d . E 4 C49 C 0.33161(16) 0.46714(15) 0.28176(12) 0.0228(4) Uani 1 1 d . E 4 N13 N 0.59207(15) 0.21163(14) 0.47660(11) 0.0304(4) Uani 1 1 d . F 4 C41 C 0.52805(19) 0.30281(18) 0.42171(14) 0.0333(5) Uani 1 1 d . F 4 H41A H 0.5799 0.3177 0.3840 0.040 Uiso 1 1 calc R F 4 H41B H 0.4900 0.2796 0.3889 0.040 Uiso 1 1 calc R F 4 C42 C 0.4451(2) 0.40501(19) 0.46515(16) 0.0404(6) Uani 1 1 d . F 4 H42A H 0.3910 0.3923 0.5008 0.061 Uiso 1 1 calc R F 4 H42B H 0.4089 0.4594 0.4254 0.061 Uiso 1 1 calc R F 4 H42C H 0.4817 0.4294 0.4974 0.061 Uiso 1 1 calc R F 4 C43 C 0.51644(19) 0.18190(19) 0.53306(13) 0.0339(5) Uani 1 1 d . F 4 H43A H 0.5606 0.1229 0.5679 0.041 Uiso 1 1 calc R F 4 H43B H 0.4668 0.2435 0.5686 0.041 Uiso 1 1 calc R F 4 C44 C 0.4489(2) 0.14878(19) 0.49179(15) 0.0387(5) Uani 1 1 d . F 4 H44A H 0.4035 0.2070 0.4579 0.058 Uiso 1 1 calc R F 4 H44B H 0.4024 0.1319 0.5327 0.058 Uiso 1 1 calc R F 4 H44C H 0.4970 0.0859 0.4580 0.058 Uiso 1 1 calc R F 4 C45 C 0.6722(2) 0.11904(19) 0.42228(14) 0.0376(5) Uani 1 1 d . F 4 H45A H 0.7177 0.1424 0.3848 0.045 Uiso 1 1 calc R F 4 H45B H 0.6311 0.1003 0.3892 0.045 Uiso 1 1 calc R F 4 C46 C 0.7465(2) 0.0201(2) 0.46533(17) 0.0494(7) Uani 1 1 d . F 4 H46A H 0.7940 0.0353 0.4933 0.074 Uiso 1 1 calc R F 4 H46B H 0.7908 -0.0371 0.4258 0.074 Uiso 1 1 calc R F 4 H46C H 0.7027 -0.0019 0.5048 0.074 Uiso 1 1 calc R F 4 C47 C 0.6495(2) 0.2444(2) 0.53003(14) 0.0369(5) Uani 1 1 d . F 4 H47A H 0.5938 0.3039 0.5651 0.044 Uiso 1 1 calc R F 4 H47B H 0.6887 0.1841 0.5657 0.044 Uiso 1 1 calc R F 4 C48 C 0.7294(2) 0.2782(3) 0.48630(18) 0.0531(7) Uani 1 1 d . F 4 H48A H 0.7882 0.2185 0.4542 0.080 Uiso 1 1 calc R F 4 H48B H 0.7598 0.3002 0.5258 0.080 Uiso 1 1 calc R F 4 H48C H 0.6921 0.3378 0.4505 0.080 Uiso 1 1 calc R F 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 N14 0.0455(10) 0.0437(10) 0.0392(10) -0.0009(8) -0.0070(8) -0.0254(8) C50A 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) C51A 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) C52A 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) C53A 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) C50B 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) C51B 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) C52B 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) C53B 0.0543(12) 0.0356(9) 0.0406(9) 0.0029(8) -0.0053(9) -0.0238(9) N15 0.0375(10) 0.0444(10) 0.0429(11) -0.0120(8) -0.0025(8) -0.0219(8) C54A 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) C55A 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) C56A 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) C57A 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) C54B 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) C55B 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) C56B 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) C57B 0.0355(9) 0.0391(11) 0.0465(10) -0.0116(8) 0.0023(8) -0.0202(8) O1 0.0734(14) 0.0519(12) 0.0800(15) -0.0157(11) -0.0111(12) -0.0353(12) O2 0.0555(12) 0.0329(9) 0.0705(14) 0.0016(9) -0.0124(11) -0.0157(9) O3 0.0298(8) 0.0263(8) 0.0420(9) 0.0080(7) -0.0098(7) -0.0071(6) O4 0.0318(8) 0.0218(7) 0.0546(10) 0.0013(7) -0.0013(7) -0.0126(6) O5 0.0296(9) 0.0267(8) 0.0765(13) 0.0147(8) -0.0023(9) -0.0071(7) O6 0.0218(8) 0.0389(10) 0.0903(16) 0.0071(10) -0.0083(9) -0.0016(7) N1 0.0496(13) 0.0377(11) 0.0531(14) -0.0078(10) 0.0028(11) -0.0249(11) N2 0.0221(8) 0.0241(8) 0.0345(10) 0.0069(7) -0.0068(7) -0.0087(7) N3 0.0211(8) 0.0233(8) 0.0348(10) 0.0056(7) -0.0043(7) -0.0073(7) N4 0.0225(8) 0.0153(7) 0.0320(9) -0.0019(7) -0.0041(7) -0.0056(7) N5 0.0198(8) 0.0203(8) 0.0333(9) -0.0004(7) -0.0033(7) -0.0086(7) N6 0.0245(9) 0.0306(10) 0.0447(12) 0.0098(9) -0.0038(8) -0.0055(8) C1 0.0261(11) 0.0307(11) 0.0340(12) 0.0022(9) 0.0000(9) -0.0129(9) C2 0.0358(12) 0.0332(12) 0.0377(13) -0.0002(10) 0.0016(10) -0.0177(10) C3 0.0428(14) 0.0506(15) 0.0402(13) -0.0026(11) -0.0043(11) -0.0284(12) C4 0.0340(13) 0.0496(15) 0.0434(14) 0.0037(12) -0.0103(11) -0.0198(12) C5 0.0282(11) 0.0344(12) 0.0404(13) 0.0058(10) -0.0066(10) -0.0131(10) C6 0.0246(10) 0.0310(11) 0.0313(11) 0.0039(9) -0.0005(9) -0.0141(9) C7 0.0204(10) 0.0252(10) 0.0319(11) 0.0055(8) 0.0007(8) -0.0084(8) C8 0.0253(10) 0.0206(9) 0.0305(11) 0.0008(8) -0.0003(8) -0.0064(8) C9 0.0240(11) 0.0273(11) 0.0487(14) -0.0018(10) -0.0002(10) -0.0035(9) C10 0.0321(12) 0.0245(11) 0.0561(16) -0.0048(11) -0.0025(11) 0.0003(9) C11 0.0389(13) 0.0186(10) 0.0494(14) -0.0040(10) -0.0092(11) -0.0038(9) C12 0.0325(12) 0.0228(10) 0.0361(12) -0.0017(9) -0.0070(10) -0.0077(9) C13 0.0251(10) 0.0189(9) 0.0248(10) -0.0009(7) -0.0017(8) -0.0039(8) C14 0.0262(10) 0.0217(9) 0.0264(10) -0.0001(8) -0.0026(8) -0.0101(8) C15 0.0205(9) 0.0272(10) 0.0206(9) -0.0015(8) -0.0014(8) -0.0095(8) C16 0.0273(11) 0.0271(10) 0.0397(12) -0.0072(9) -0.0002(9) -0.0118(9) C17 0.0293(11) 0.0388(12) 0.0469(14) -0.0125(11) 0.0015(10) -0.0196(10) C18 0.0235(11) 0.0444(13) 0.0359(12) -0.0058(10) -0.0031(9) -0.0139(10) C19 0.0251(10) 0.0271(10) 0.0264(10) 0.0029(8) -0.0033(8) -0.0063(9) C20 0.0230(10) 0.0262(10) 0.0224(10) 0.0035(8) -0.0026(8) -0.0102(8) O7 0.0310(10) 0.0747(15) 0.0739(14) -0.0349(12) 0.0160(10) -0.0180(10) O8 0.0372(10) 0.0469(11) 0.0694(13) -0.0150(10) 0.0009(9) -0.0190(9) O9 0.0371(9) 0.0395(9) 0.0392(9) 0.0081(7) 0.0026(7) -0.0236(8) O10 0.0292(7) 0.0224(7) 0.0286(8) -0.0053(6) 0.0042(6) -0.0133(6) O11 0.0954(16) 0.0375(10) 0.0337(9) -0.0076(8) 0.0101(10) -0.0400(11) O12 0.0567(11) 0.0353(9) 0.0410(9) 0.0060(7) 0.0048(8) -0.0297(8) N7 0.0292(11) 0.0574(14) 0.0545(14) -0.0253(12) 0.0022(10) -0.0195(10) N8 0.0259(9) 0.0348(10) 0.0277(9) 0.0018(7) 0.0026(7) -0.0173(8) N9 0.0232(9) 0.0312(9) 0.0280(9) 0.0085(7) -0.0001(7) -0.0125(7) N10 0.0231(8) 0.0193(8) 0.0257(9) -0.0007(6) 0.0041(7) -0.0081(7) N11 0.0275(9) 0.0194(8) 0.0246(9) -0.0018(7) 0.0069(7) -0.0084(7) N12 0.0397(10) 0.0252(9) 0.0299(10) 0.0046(7) -0.0051(8) -0.0161(8) C21 0.0284(11) 0.0458(13) 0.0301(11) -0.0081(10) -0.0002(9) -0.0221(10) C22 0.0281(11) 0.0530(15) 0.0355(12) -0.0150(11) 0.0017(10) -0.0212(11) C23 0.0278(12) 0.0734(19) 0.0403(14) -0.0124(13) 0.0065(11) -0.0293(13) C24 0.0337(13) 0.0719(19) 0.0373(13) 0.0038(13) 0.0029(11) -0.0328(13) C25 0.0310(12) 0.0547(15) 0.0326(12) 0.0028(11) 0.0001(10) -0.0258(11) C26 0.0250(10) 0.0463(13) 0.0260(11) -0.0029(9) -0.0010(9) -0.0218(10) C27 0.0275(11) 0.0372(11) 0.0243(10) 0.0039(9) -0.0030(8) -0.0198(9) C28 0.0273(10) 0.0261(10) 0.0224(10) 0.0023(8) -0.0038(8) -0.0128(8) C29 0.0374(12) 0.0307(11) 0.0295(11) 0.0032(9) -0.0008(9) -0.0204(10) C30 0.0430(13) 0.0222(10) 0.0355(12) 0.0020(9) -0.0035(10) -0.0138(10) C31 0.0322(11) 0.0229(10) 0.0382(12) -0.0013(9) -0.0042(10) -0.0084(9) C32 0.0254(10) 0.0257(10) 0.0327(11) -0.0007(8) -0.0029(9) -0.0114(9) C33 0.0247(10) 0.0220(9) 0.0235(10) 0.0013(7) -0.0022(8) -0.0113(8) C34 0.0199(9) 0.0221(9) 0.0250(10) -0.0007(8) -0.0007(8) -0.0109(8) C35 0.0217(9) 0.0216(9) 0.0221(9) 0.0014(7) 0.0002(8) -0.0081(8) C36 0.0318(11) 0.0248(10) 0.0260(10) -0.0051(8) 0.0035(9) -0.0137(9) C37 0.0340(12) 0.0327(11) 0.0224(10) -0.0035(8) 0.0057(9) -0.0154(10) C38 0.0274(10) 0.0284(10) 0.0241(10) 0.0028(8) 0.0014(8) -0.0126(9) C39 0.0245(10) 0.0207(9) 0.0253(10) 0.0025(8) -0.0041(8) -0.0110(8) C40 0.0255(10) 0.0213(9) 0.0203(9) 0.0007(7) -0.0025(8) -0.0085(8) O13 0.0429(9) 0.0427(9) 0.0292(8) 0.0016(7) -0.0016(7) -0.0307(8) O14 0.0267(8) 0.0176(7) 0.0406(9) 0.0018(6) 0.0055(7) -0.0026(6) O15 0.0215(7) 0.0263(7) 0.0320(8) -0.0065(6) 0.0007(6) -0.0085(6) C49 0.0250(10) 0.0175(8) 0.0234(10) 0.0073(7) -0.0036(8) -0.0087(8) N13 0.0344(10) 0.0323(9) 0.0259(9) 0.0044(7) -0.0038(8) -0.0174(8) C41 0.0389(12) 0.0338(11) 0.0302(11) 0.0091(9) -0.0093(10) -0.0195(10) C42 0.0407(13) 0.0373(13) 0.0425(14) 0.0033(11) -0.0111(11) -0.0169(11) C43 0.0412(13) 0.0348(12) 0.0281(11) 0.0009(9) 0.0026(10) -0.0220(10) C44 0.0463(14) 0.0371(13) 0.0362(13) -0.0059(10) 0.0022(11) -0.0239(11) C45 0.0378(13) 0.0352(12) 0.0315(12) 0.0045(10) 0.0004(10) -0.0126(10) C46 0.0510(16) 0.0382(14) 0.0426(14) 0.0087(11) -0.0025(12) -0.0103(12) C47 0.0402(13) 0.0435(13) 0.0334(12) 0.0072(10) -0.0115(10) -0.0241(11) C48 0.0537(17) 0.073(2) 0.0492(16) 0.0113(14) -0.0132(13) -0.0435(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N14 C50A 1.360(5) 2_655 ? N14 C50A 1.360(5) . ? N14 C50B 1.560(5) 2_655 ? N14 C50B 1.560(5) . ? N14 C52A 1.567(4) 2_655 ? N14 C52A 1.567(4) . ? N14 C52B 1.578(5) 2_655 ? N14 C52B 1.578(5) . ? C50A C51A 1.563(6) . ? C52A C53A 1.534(6) . ? C50B C51B 1.463(6) . ? C50B C52B 1.926(7) . ? C52B C53B 1.528(6) . ? N15 C54B 1.338(5) 2 ? N15 C54B 1.338(5) . ? N15 C54A 1.528(4) . ? N15 C54A 1.528(4) 2 ? N15 C56A 1.566(4) 2 ? N15 C56A 1.566(4) . ? N15 C56B 1.667(5) . ? N15 C56B 1.667(5) 2 ? C54A C55A 1.413(6) . ? C56A C57A 1.531(5) . ? C54B C55B 1.522(6) . ? C56B C57B 1.514(6) . ? O1 N1 1.231(3) . ? O2 N1 1.227(3) . ? O3 C7 1.225(2) . ? O4 C14 1.224(2) . ? O5 N6 1.237(3) . ? O6 N6 1.229(2) . ? N1 C2 1.471(3) . ? N2 C7 1.384(3) . ? N2 C6 1.402(3) . ? N3 C7 1.369(3) . ? N3 C8 1.416(3) . ? N4 C14 1.365(3) . ? N4 C13 1.411(2) . ? N5 C14 1.388(2) . ? N5 C15 1.401(2) . ? N6 C19 1.464(3) . ? C1 C2 1.379(3) . ? C1 C6 1.396(3) . ? C2 C3 1.381(4) . ? C3 C4 1.389(4) . ? C4 C5 1.388(3) . ? C5 C6 1.401(3) . ? C8 C9 1.395(3) . ? C8 C13 1.409(3) . ? C9 C10 1.385(3) . ? C10 C11 1.380(4) . ? C11 C12 1.390(3) . ? C12 C13 1.404(3) . ? C15 C20 1.391(3) . ? C15 C16 1.404(3) . ? C16 C17 1.386(3) . ? C17 C18 1.379(3) . ? C18 C19 1.381(3) . ? C19 C20 1.385(3) . ? O7 N7 1.233(3) . ? O8 N7 1.231(3) . ? O9 C27 1.225(3) . ? O10 C34 1.229(2) . ? O11 N12 1.230(2) . ? O12 N12 1.226(2) . ? N7 C22 1.472(3) . ? N8 C27 1.371(3) . ? N8 C26 1.402(3) . ? N9 C27 1.386(3) . ? N9 C28 1.408(3) . ? N10 C34 1.370(2) . ? N10 C33 1.417(2) . ? N11 C34 1.371(2) . ? N11 C35 1.405(2) . ? N12 C39 1.467(3) . ? C21 C22 1.385(3) . ? C21 C26 1.393(3) . ? C22 C23 1.390(4) . ? C23 C24 1.379(4) . ? C24 C25 1.388(3) . ? C25 C26 1.397(3) . ? C28 C29 1.401(3) . ? C28 C33 1.410(3) . ? C29 C30 1.385(3) . ? C30 C31 1.385(3) . ? C31 C32 1.389(3) . ? C32 C33 1.394(3) . ? C35 C40 1.392(3) . ? C35 C36 1.399(3) . ? C36 C37 1.389(3) . ? C37 C38 1.393(3) . ? C38 C39 1.384(3) . ? C39 C40 1.383(3) . ? O13 C49 1.279(2) . ? O14 C49 1.291(2) . ? O15 C49 1.290(2) . ? N13 C45 1.513(3) . ? N13 C43 1.520(3) . ? N13 C47 1.520(3) . ? N13 C41 1.523(3) . ? C41 C42 1.515(3) . ? C43 C44 1.511(3) . ? C45 C46 1.513(3) . ? C47 C48 1.512(3) . ? 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 C50A N14 C50A 180.0(7) 2_655 . ? C50A N14 C50B 67.4(3) 2_655 2_655 ? C50A N14 C50B 112.6(3) . 2_655 ? C50A N14 C50B 112.6(3) 2_655 . ? C50A N14 C50B 67.4(3) . . ? C50B N14 C50B 180.0(4) 2_655 . ? C50A N14 C52A 62.1(3) 2_655 2_655 ? C50A N14 C52A 117.9(3) . 2_655 ? C50B N14 C52A 104.9(3) 2_655 2_655 ? C50B N14 C52A 75.1(3) . 2_655 ? C50A N14 C52A 117.9(3) 2_655 . ? C50A N14 C52A 62.1(3) . . ? C50B N14 C52A 75.1(3) 2_655 . ? C50B N14 C52A 104.9(3) . . ? C52A N14 C52A 180.0(4) 2_655 . ? C50A N14 C52B 116.6(3) 2_655 2_655 ? C50A N14 C52B 63.4(3) . 2_655 ? C50B N14 C52B 75.7(3) 2_655 2_655 ? C50B N14 C52B 104.3(3) . 2_655 ? C52A N14 C52B 81.3(2) 2_655 2_655 ? C52A N14 C52B 98.7(2) . 2_655 ? C50A N14 C52B 63.4(3) 2_655 . ? C50A N14 C52B 116.6(3) . . ? C50B N14 C52B 104.3(3) 2_655 . ? C50B N14 C52B 75.7(3) . . ? C52A N14 C52B 98.7(2) 2_655 . ? C52A N14 C52B 81.3(2) . . ? C52B N14 C52B 180.00(18) 2_655 . ? N14 C50A C51A 116.5(4) . . ? C53A C52A N14 111.9(3) . . ? C51B C50B N14 120.8(4) . . ? C51B C50B C52B 142.1(4) . . ? N14 C50B C52B 52.6(2) . . ? C53B C52B N14 112.5(4) . . ? C53B C52B C50B 121.2(4) . . ? N14 C52B C50B 51.7(2) . . ? C54B N15 C54B 180.0(8) 2 . ? C54B N15 C54A 115.2(3) 2 . ? C54B N15 C54A 64.8(3) . . ? C54B N15 C54A 64.8(3) 2 2 ? C54B N15 C54A 115.2(3) . 2 ? C54A N15 C54A 180.0(5) . 2 ? C54B N15 C56A 59.6(3) 2 2 ? C54B N15 C56A 120.4(3) . 2 ? C54A N15 C56A 73.1(3) . 2 ? C54A N15 C56A 106.9(3) 2 2 ? C54B N15 C56A 120.4(3) 2 . ? C54B N15 C56A 59.6(3) . . ? C54A N15 C56A 106.9(3) . . ? C54A N15 C56A 73.1(3) 2 . ? C56A N15 C56A 180.0(4) 2 . ? C54B N15 C56B 67.0(3) 2 . ? C54B N15 C56B 113.0(3) . . ? C54A N15 C56B 77.6(3) . . ? C54A N15 C56B 102.4(3) 2 . ? C56A N15 C56B 96.0(2) 2 . ? C56A N15 C56B 84.0(2) . . ? C54B N15 C56B 113.0(3) 2 2 ? C54B N15 C56B 67.0(3) . 2 ? C54A N15 C56B 102.4(3) . 2 ? C54A N15 C56B 77.6(3) 2 2 ? C56A N15 C56B 84.0(2) 2 2 ? C56A N15 C56B 96.0(2) . 2 ? C56B N15 C56B 180.0(5) . 2 ? C55A C54A N15 125.3(4) . . ? C57A C56A N15 110.2(3) . . ? N15 C54B C55B 121.8(4) . . ? C57B C56B N15 110.9(4) . . ? O2 N1 O1 123.3(2) . . ? O2 N1 C2 119.0(2) . . ? O1 N1 C2 117.7(2) . . ? C7 N2 C6 127.22(18) . . ? C7 N3 C8 124.56(17) . . ? C14 N4 C13 126.41(17) . . ? C14 N5 C15 125.60(17) . . ? O6 N6 O5 123.45(19) . . ? O6 N6 C19 118.3(2) . . ? O5 N6 C19 118.23(17) . . ? C2 C1 C6 119.1(2) . . ? C1 C2 C3 123.4(2) . . ? C1 C2 N1 117.6(2) . . ? C3 C2 N1 119.0(2) . . ? C2 C3 C4 116.8(2) . . ? C5 C4 C3 122.0(2) . . ? C4 C5 C6 119.7(2) . . ? C1 C6 C5 119.1(2) . . ? C1 C6 N2 116.55(19) . . ? C5 C6 N2 124.4(2) . . ? O3 C7 N3 124.5(2) . . ? O3 C7 N2 123.7(2) . . ? N3 C7 N2 111.78(17) . . ? C9 C8 C13 119.4(2) . . ? C9 C8 N3 120.9(2) . . ? C13 C8 N3 119.66(17) . . ? C10 C9 C8 120.9(2) . . ? C11 C10 C9 119.8(2) . . ? C10 C11 C12 120.7(2) . . ? C11 C12 C13 120.1(2) . . ? C12 C13 C8 119.12(18) . . ? C12 C13 N4 123.29(19) . . ? C8 C13 N4 117.58(18) . . ? O4 C14 N4 125.24(19) . . ? O4 C14 N5 123.59(19) . . ? N4 C14 N5 111.14(17) . . ? C20 C15 N5 116.05(18) . . ? C20 C15 C16 119.37(18) . . ? N5 C15 C16 124.59(18) . . ? C17 C16 C15 119.9(2) . . ? C18 C17 C16 121.6(2) . . ? C17 C18 C19 117.3(2) . . ? C18 C19 C20 123.5(2) . . ? C18 C19 N6 119.11(19) . . ? C20 C19 N6 117.43(19) . . ? C19 C20 C15 118.40(19) . . ? O8 N7 O7 123.6(3) . . ? O8 N7 C22 118.8(2) . . ? O7 N7 C22 117.6(2) . . ? C27 N8 C26 127.30(18) . . ? C27 N9 C28 126.21(17) . . ? C34 N10 C33 122.69(17) . . ? C34 N11 C35 125.69(17) . . ? O12 N12 O11 123.07(18) . . ? O12 N12 C39 118.79(18) . . ? O11 N12 C39 118.13(17) . . ? C22 C21 C26 119.2(2) . . ? C21 C22 C23 122.7(2) . . ? C21 C22 N7 117.6(2) . . ? C23 C22 N7 119.7(2) . . ? C24 C23 C22 117.1(2) . . ? C23 C24 C25 122.0(2) . . ? C24 C25 C26 119.9(2) . . ? C21 C26 C25 119.1(2) . . ? C21 C26 N8 115.9(2) . . ? C25 C26 N8 125.0(2) . . ? O9 C27 N8 124.94(19) . . ? O9 C27 N9 124.3(2) . . ? N8 C27 N9 110.77(18) . . ? C29 C28 N9 123.76(19) . . ? C29 C28 C33 118.50(19) . . ? N9 C28 C33 117.74(17) . . ? C30 C29 C28 120.6(2) . . ? C29 C30 C31 121.0(2) . . ? C30 C31 C32 118.9(2) . . ? C31 C32 C33 121.1(2) . . ? C32 C33 C28 119.75(18) . . ? C32 C33 N10 120.52(18) . . ? C28 C33 N10 119.72(17) . . ? O10 C34 N10 124.20(18) . . ? O10 C34 N11 124.15(18) . . ? N10 C34 N11 111.65(17) . . ? C40 C35 C36 119.15(18) . . ? C40 C35 N11 117.08(17) . . ? C36 C35 N11 123.75(18) . . ? C37 C36 C35 120.40(19) . . ? C36 C37 C38 121.26(19) . . ? C39 C38 C37 116.79(18) . . ? C40 C39 C38 123.67(18) . . ? C40 C39 N12 117.99(18) . . ? C38 C39 N12 118.33(17) . . ? C39 C40 C35 118.72(18) . . ? O13 C49 O15 120.73(18) . . ? O13 C49 O14 119.93(18) . . ? O15 C49 O14 119.33(18) . . ? C45 N13 C43 110.81(17) . . ? C45 N13 C47 111.44(18) . . ? C43 N13 C47 106.51(16) . . ? C45 N13 C41 106.94(17) . . ? C43 N13 C41 110.65(17) . . ? C47 N13 C41 110.54(17) . . ? C42 C41 N13 114.99(19) . . ? C44 C43 N13 115.20(18) . . ? N13 C45 C46 115.4(2) . . ? C48 C47 N13 115.9(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H902 O13 0.88 2.26 3.095(2) 158.7 . N2 H902 O14 0.88 2.59 3.326(2) 142.2 . N3 H903 O14 0.88 1.90 2.726(2) 155.7 . N4 H904 O14 0.88 1.90 2.765(2) 166.9 . N5 H905 O15 0.88 2.03 2.885(2) 165.1 . N5 H905 O14 0.88 2.61 3.329(2) 139.0 . N8 H908 O13 0.88 1.91 2.765(2) 163.1 . N9 H909 O13 0.88 2.19 2.939(2) 142.8 . N10 H910 O15 0.88 2.12 2.918(2) 150.2 . N10 H910 O13 0.88 2.63 3.368(2) 142.5 . N11 H911 O15 0.88 2.02 2.838(2) 154.5 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.630 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.049 _iucr_refine_instructions_details ; TITL 2011sot0753 in P-1 CELL 0.71073 14.1445 14.3376 16.7194 86.271 81.687 61.358 ZERR 2 0.0018 0.0023 0.0030 0.008 0.008 0.005 LATT 1 SFAC C H N O UNIT 114 144 28 30 MERG 2 SHEL 7 0.77 OMIT 2 1 1 ISOR 0.0Q N14 N15 EADP C50A C50B C52A C52B C53A C53B C51A C51B EADP C54A C54B C56A C56B C57A C57B C55A C55B DFIX 1.50 0.01 N15 C56A N15 C56A N15 C54A N15 C54B DFIX 1.50 0.01 N14 C52A N14 C52B N14 C50A N14 C50B DFIX 1.54 0.01 C56A C57A C56B C57B C54A C55A C54B C55B DFIX 1.54 0.01 C50A C51A C50B C51B C52A C53A C52B C53B DFIX 2.56 0.01 N14 C51A N14 C51B N14 C53A N14 C53B DFIX 2.56 0.01 N15 C55A N15 C55B N15 C57A N15 C57B EQIV $1 -x+1, -y, -z EQIV $2 -x, -y, -z FREE C56A C54A_$2 FREE C56B C54B_$2 FREE C54B C56B_$2 FREE C54A C56A_$2 FREE C50A C52A TEMP -173 SIZE 0.12 0.1 0.08 HTAB HTAB N2 O13 HTAB N2 O14 HTAB N3 O14 HTAB N4 O14 HTAB N5 O15 HTAB N5 O14 HTAB N8 O13 HTAB N9 O13 HTAB N10 O15 HTAB N10 O13 HTAB N11 O15 FMAP 2 PLAN 20 ACTA 55.00 BOND L.S. 10 WGHT 0.063200 1.234500 FVAR 0.33614 N14 3 0.500000 0.000000 0.000000 10.50000 0.04545 0.04371 = 0.03915 -0.00090 -0.00699 -0.02537 PART 1 C50A 1 0.578828 -0.103072 0.000666 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 23 H50A 2 0.614416 -0.124218 -0.055463 10.50000 -1.20000 H50B 2 0.543547 -0.147551 0.018192 10.50000 -1.20000 AFIX 0 C51A 1 0.669018 -0.129522 0.055574 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 33 H51A 2 0.721207 -0.205488 0.051309 10.50000 -1.50000 H51B 2 0.635689 -0.111633 0.111846 10.50000 -1.50000 H51C 2 0.706701 -0.088027 0.037991 10.50000 -1.50000 AFIX 0 C52A 1 0.465543 -0.085159 0.034280 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 23 H52A 2 0.413689 -0.086217 0.000885 10.50000 -1.20000 H52B 2 0.530398 -0.156276 0.030593 10.50000 -1.20000 AFIX 0 C53A 1 0.412634 -0.062085 0.122532 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 33 H53A 2 0.392340 -0.116909 0.141765 10.50000 -1.50000 H53B 2 0.347546 0.007663 0.126257 10.50000 -1.50000 H53C 2 0.464218 -0.062269 0.155951 10.50000 -1.50000 AFIX 0 PART 2 C50B 1 0.592806 -0.016008 0.048670 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 23 H50C 2 0.616094 0.037348 0.028909 10.50000 -1.20000 H50D 2 0.560284 0.002343 0.105711 10.50000 -1.20000 AFIX 0 C51B 1 0.691105 -0.118717 0.048703 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 33 H51D 2 0.753372 -0.112211 0.020437 10.50000 -1.50000 H51E 2 0.682196 -0.171737 0.021135 10.50000 -1.50000 H51F 2 0.703614 -0.141025 0.104559 10.50000 -1.50000 AFIX 0 C52B 1 0.439024 0.053041 0.084831 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 23 H52C 2 0.491627 0.055648 0.116574 10.50000 -1.20000 H52D 2 0.382917 0.127023 0.076499 10.50000 -1.20000 AFIX 0 C53B 1 0.385089 -0.007152 0.132870 10.50000 0.05429 0.03565 = 0.04064 0.00288 -0.00529 -0.02378 AFIX 33 H53D 2 0.307036 0.040758 0.145703 10.50000 -1.50000 H53E 2 0.417273 -0.033660 0.183109 10.50000 -1.50000 H53F 2 0.396373 -0.067151 0.100601 10.50000 -1.50000 AFIX 0 PART 0 N15 3 0.000000 0.000000 0.000000 10.50000 0.03745 0.04436 = 0.04294 -0.01204 -0.00246 -0.02190 PART 3 C54A 1 0.104913 -0.003187 0.016587 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 23 H54A 2 0.161650 -0.047225 -0.027061 10.50000 -1.20000 H54B 2 0.094069 0.070079 0.007939 10.50000 -1.20000 AFIX 0 C55A 1 0.151750 -0.038110 0.089143 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 33 H55A 2 0.218980 -0.032997 0.084488 10.50000 -1.50000 H55B 2 0.168087 -0.112126 0.099114 10.50000 -1.50000 H55C 2 0.100667 0.006572 0.134147 10.50000 -1.50000 AFIX 0 C56A 1 -0.077270 0.028238 0.081972 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 23 H56A 2 -0.142607 0.022095 0.075695 10.50000 -1.20000 H56B 2 -0.039517 -0.022486 0.124104 10.50000 -1.20000 AFIX 0 C57A 1 -0.111250 0.141523 0.108084 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 33 H57A 2 -0.159525 0.158242 0.159405 10.50000 -1.50000 H57B 2 -0.149448 0.191677 0.066629 10.50000 -1.50000 H57C 2 -0.046530 0.147179 0.114935 10.50000 -1.50000 AFIX 0 PART 4 C54B 1 0.037524 -0.049437 0.068099 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 23 H54C 2 0.049492 -0.123002 0.064166 10.50000 -1.20000 H54D 2 -0.021925 -0.014485 0.112814 10.50000 -1.20000 AFIX 0 C55B 1 0.139655 -0.057332 0.094508 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 33 H55D 2 0.153285 -0.095732 0.145801 10.50000 -1.50000 H55E 2 0.129804 0.014245 0.101559 10.50000 -1.50000 H55F 2 0.201645 -0.095594 0.053170 10.50000 -1.50000 AFIX 0 C56B 1 -0.033425 0.128432 -0.000084 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 23 H56C 2 0.033180 0.135611 -0.002830 10.50000 -1.20000 H56D 2 -0.069142 0.162869 -0.048453 10.50000 -1.20000 AFIX 0 C57B 1 -0.109387 0.183629 0.075310 10.50000 0.03555 0.03913 = 0.04649 -0.01156 0.00228 -0.02022 AFIX 33 H57D 2 -0.127897 0.258863 0.073955 10.50000 -1.50000 H57E 2 -0.073617 0.150259 0.123170 10.50000 -1.50000 H57F 2 -0.175812 0.177489 0.077602 10.50000 -1.50000 AFIX 0 MOLE 1 O1 4 0.072245 0.238010 0.071196 11.00000 0.07337 0.05194 = 0.07997 -0.01566 -0.01111 -0.03527 O2 4 0.179874 0.231989 0.153444 11.00000 0.05555 0.03292 = 0.07046 0.00156 -0.01238 -0.01565 O3 4 -0.025245 0.780410 0.183800 11.00000 0.02985 0.02631 = 0.04198 0.00803 -0.00982 -0.00713 O4 4 0.406938 0.800530 0.274955 11.00000 0.03179 0.02176 = 0.05459 0.00131 -0.00127 -0.01260 O5 4 0.771268 0.261864 0.281994 11.00000 0.02962 0.02668 = 0.07652 0.01466 -0.00226 -0.00710 O6 4 0.917715 0.278166 0.267369 11.00000 0.02183 0.03888 = 0.09029 0.00708 -0.00826 -0.00162 N1 3 0.102629 0.281204 0.115197 11.00000 0.04960 0.03771 = 0.05315 -0.00779 0.00279 -0.02495 N2 3 0.076226 0.602964 0.212149 11.00000 0.02212 0.02406 = 0.03446 0.00689 -0.00684 -0.00868 AFIX 43 H902 2 0.131351 0.558418 0.237254 11.00000 -1.20000 AFIX 0 N3 3 0.097166 0.726704 0.275466 11.00000 0.02114 0.02328 = 0.03482 0.00560 -0.00427 -0.00733 AFIX 43 H903 2 0.139067 0.671872 0.303482 11.00000 -1.20000 AFIX 0 N4 3 0.284574 0.736063 0.289926 11.00000 0.02246 0.01530 = 0.03197 -0.00191 -0.00414 -0.00561 AFIX 43 H904 2 0.280251 0.676688 0.292950 11.00000 -1.20000 AFIX 0 N5 3 0.465404 0.620401 0.276201 11.00000 0.01983 0.02033 = 0.03329 -0.00037 -0.00331 -0.00857 AFIX 43 H905 2 0.443359 0.572578 0.275547 11.00000 -1.20000 AFIX 0 N6 3 0.818387 0.316246 0.274733 11.00000 0.02446 0.03063 = 0.04469 0.00982 -0.00383 -0.00545 C1 1 0.085127 0.446913 0.162122 11.00000 0.02611 0.03072 = 0.03402 0.00215 0.00001 -0.01290 AFIX 43 H1 2 0.149395 0.405897 0.186542 11.00000 -1.20000 AFIX 0 C2 1 0.043239 0.397919 0.120855 11.00000 0.03583 0.03319 = 0.03775 -0.00024 0.00163 -0.01772 C3 1 -0.049828 0.452749 0.084117 11.00000 0.04278 0.05055 = 0.04025 -0.00260 -0.00435 -0.02837 AFIX 43 H3 2 -0.077317 0.416861 0.056568 11.00000 -1.20000 AFIX 0 C4 1 -0.101314 0.562924 0.089389 11.00000 0.03401 0.04956 = 0.04338 0.00369 -0.01035 -0.01984 AFIX 43 H4 2 -0.165278 0.603177 0.064461 11.00000 -1.20000 AFIX 0 C5 1 -0.062108 0.615935 0.129974 11.00000 0.02822 0.03443 = 0.04040 0.00579 -0.00656 -0.01311 AFIX 43 H5 2 -0.098734 0.691384 0.132299 11.00000 -1.20000 AFIX 0 C6 1 0.031743 0.557686 0.167512 11.00000 0.02464 0.03104 = 0.03129 0.00390 -0.00048 -0.01405 C7 1 0.043088 0.709918 0.221120 11.00000 0.02041 0.02519 = 0.03188 0.00548 0.00070 -0.00836 C8 1 0.090372 0.826174 0.289742 11.00000 0.02533 0.02062 = 0.03048 0.00082 -0.00027 -0.00639 C9 1 -0.009292 0.918940 0.296577 11.00000 0.02398 0.02728 = 0.04868 -0.00176 -0.00019 -0.00349 AFIX 43 H9 2 -0.073797 0.915094 0.293152 11.00000 -1.20000 AFIX 0 C10 1 -0.015552 1.016605 0.308291 11.00000 0.03212 0.02445 = 0.05608 -0.00478 -0.00250 0.00026 AFIX 43 H10 2 -0.083729 1.079418 0.311633 11.00000 -1.20000 AFIX 0 C11 1 0.077607 1.022316 0.315087 11.00000 0.03887 0.01858 = 0.04945 -0.00400 -0.00918 -0.00378 AFIX 43 H11 2 0.073161 1.089337 0.323233 11.00000 -1.20000 AFIX 0 C12 1 0.177910 0.931020 0.310138 11.00000 0.03251 0.02285 = 0.03613 -0.00171 -0.00697 -0.00771 AFIX 43 H12 2 0.241319 0.935744 0.315923 11.00000 -1.20000 AFIX 0 C13 1 0.185602 0.831830 0.296599 11.00000 0.02508 0.01892 = 0.02478 -0.00086 -0.00175 -0.00393 C14 1 0.386428 0.726414 0.279235 11.00000 0.02615 0.02166 = 0.02636 -0.00012 -0.00256 -0.01014 C15 1 0.577164 0.583014 0.274091 11.00000 0.02055 0.02715 = 0.02061 -0.00145 -0.00143 -0.00953 C16 1 0.626571 0.648209 0.270138 11.00000 0.02730 0.02712 = 0.03968 -0.00720 -0.00016 -0.01175 AFIX 43 H16 2 0.583721 0.723230 0.267663 11.00000 -1.20000 AFIX 0 C17 1 0.737974 0.602955 0.269851 11.00000 0.02928 0.03883 = 0.04689 -0.01249 0.00149 -0.01960 AFIX 43 H17 2 0.770385 0.647859 0.268234 11.00000 -1.20000 AFIX 0 C18 1 0.802832 0.494337 0.271858 11.00000 0.02349 0.04444 = 0.03594 -0.00578 -0.00307 -0.01390 AFIX 43 H18 2 0.879153 0.463571 0.271635 11.00000 -1.20000 AFIX 0 C19 1 0.752328 0.432064 0.274206 11.00000 0.02515 0.02711 = 0.02639 0.00292 -0.00335 -0.00632 C20 1 0.641274 0.473230 0.275914 11.00000 0.02303 0.02615 = 0.02236 0.00346 -0.00257 -0.01020 AFIX 43 H20 2 0.609631 0.427586 0.278274 11.00000 -1.20000 AFIX 0 MOLE 2 O7 4 -0.227263 0.628662 0.468768 11.00000 0.03103 0.07472 = 0.07389 -0.03489 0.01597 -0.01802 O8 4 -0.109580 0.643801 0.377547 11.00000 0.03716 0.04691 = 0.06937 -0.01497 0.00091 -0.01904 O9 4 0.289336 0.111156 0.368228 11.00000 0.03714 0.03952 = 0.03924 0.00814 0.00260 -0.02361 O10 4 0.653788 0.163365 0.081290 11.00000 0.02919 0.02240 = 0.02863 -0.00533 0.00421 -0.01327 O11 4 0.591252 0.669564 0.079384 11.00000 0.09539 0.03751 = 0.03375 -0.00759 0.01008 -0.04005 O12 4 0.681246 0.659701 -0.038429 11.00000 0.05667 0.03531 = 0.04100 0.00604 0.00482 -0.02967 N7 3 -0.138358 0.591210 0.426234 11.00000 0.02916 0.05742 = 0.05448 -0.02534 0.00216 -0.01950 N8 3 0.209346 0.291061 0.343372 11.00000 0.02587 0.03484 = 0.02767 0.00182 0.00257 -0.01730 AFIX 43 H908 2 0.221211 0.339867 0.316123 11.00000 -1.20000 AFIX 0 N9 3 0.379799 0.183999 0.282568 11.00000 0.02317 0.03123 = 0.02801 0.00848 -0.00006 -0.01251 AFIX 43 H909 2 0.368177 0.240294 0.252547 11.00000 -1.20000 AFIX 0 N10 3 0.545362 0.219562 0.203186 11.00000 0.02305 0.01931 = 0.02568 -0.00067 0.00413 -0.00813 AFIX 43 H910 2 0.497841 0.275531 0.232476 11.00000 -1.20000 AFIX 0 N11 3 0.562727 0.340337 0.116381 11.00000 0.02752 0.01945 = 0.02459 -0.00185 0.00694 -0.00835 AFIX 43 H911 2 0.511883 0.386378 0.151697 11.00000 -1.20000 AFIX 0 N12 3 0.638190 0.623941 0.014543 11.00000 0.03966 0.02518 = 0.02988 0.00462 -0.00506 -0.01613 C21 1 0.036102 0.435012 0.386129 11.00000 0.02839 0.04577 = 0.03010 -0.00815 -0.00024 -0.02211 AFIX 43 H21 2 0.055429 0.479465 0.350723 11.00000 -1.20000 AFIX 0 C22 1 -0.064141 0.476849 0.433490 11.00000 0.02805 0.05301 = 0.03553 -0.01495 0.00166 -0.02119 C23 1 -0.095973 0.415527 0.486815 11.00000 0.02784 0.07341 = 0.04030 -0.01236 0.00650 -0.02928 AFIX 43 H23 2 -0.164561 0.445945 0.519527 11.00000 -1.20000 AFIX 0 C24 1 -0.023624 0.308576 0.490163 11.00000 0.03371 0.07189 = 0.03730 0.00380 0.00291 -0.03279 AFIX 43 H24 2 -0.043307 0.264558 0.525805 11.00000 -1.20000 AFIX 0 C25 1 0.077035 0.263349 0.443042 11.00000 0.03099 0.05473 = 0.03259 0.00279 0.00012 -0.02579 AFIX 43 H25 2 0.124693 0.189231 0.446116 11.00000 -1.20000 AFIX 0 C26 1 0.108234 0.326912 0.391069 11.00000 0.02495 0.04629 = 0.02599 -0.00285 -0.00099 -0.02176 C27 1 0.291852 0.188488 0.334395 11.00000 0.02750 0.03720 = 0.02431 0.00389 -0.00304 -0.01975 C28 1 0.485975 0.097932 0.273378 11.00000 0.02728 0.02608 = 0.02239 0.00229 -0.00379 -0.01281 C29 1 0.512387 -0.004889 0.301262 11.00000 0.03739 0.03071 = 0.02955 0.00319 -0.00084 -0.02042 AFIX 43 H29 2 0.456410 -0.019948 0.326034 11.00000 -1.20000 AFIX 0 C30 1 0.619320 -0.084777 0.293055 11.00000 0.04299 0.02223 = 0.03551 0.00199 -0.00351 -0.01383 AFIX 43 H30 2 0.635860 -0.153808 0.312933 11.00000 -1.20000 AFIX 0 C31 1 0.702513 -0.065531 0.256299 11.00000 0.03216 0.02293 = 0.03821 -0.00129 -0.00423 -0.00841 AFIX 43 H31 2 0.775764 -0.120514 0.251414 11.00000 -1.20000 AFIX 0 C32 1 0.677140 0.035438 0.226692 11.00000 0.02541 0.02575 = 0.03270 -0.00072 -0.00287 -0.01139 AFIX 43 H32 2 0.733686 0.049055 0.200930 11.00000 -1.20000 AFIX 0 C33 1 0.570135 0.117118 0.234135 11.00000 0.02472 0.02201 = 0.02349 0.00132 -0.00224 -0.01127 C34 1 0.592363 0.235031 0.129539 11.00000 0.01985 0.02211 = 0.02496 -0.00065 -0.00066 -0.01094 C35 1 0.606462 0.381137 0.051427 11.00000 0.02174 0.02157 = 0.02214 0.00141 0.00016 -0.00814 C36 1 0.649646 0.331680 -0.024328 11.00000 0.03179 0.02482 = 0.02595 -0.00510 0.00348 -0.01370 AFIX 43 H36 2 0.651154 0.266300 -0.033673 11.00000 -1.20000 AFIX 0 C37 1 0.690327 0.377608 -0.085954 11.00000 0.03405 0.03273 = 0.02236 -0.00350 0.00568 -0.01542 AFIX 43 H37 2 0.720094 0.342639 -0.136858 11.00000 -1.20000 AFIX 0 C38 1 0.688305 0.473941 -0.074534 11.00000 0.02740 0.02835 = 0.02412 0.00281 0.00144 -0.01256 AFIX 43 H38 2 0.716017 0.505692 -0.116467 11.00000 -1.20000 AFIX 0 C39 1 0.643977 0.521196 0.000852 11.00000 0.02447 0.02069 = 0.02526 0.00250 -0.00409 -0.01101 C40 1 0.603344 0.477686 0.063859 11.00000 0.02550 0.02131 = 0.02034 0.00067 -0.00251 -0.00847 AFIX 43 H40 2 0.573870 0.513008 0.114647 11.00000 -1.20000 AFIX 0 MOLE 3 O13 4 0.290231 0.414068 0.256680 11.00000 0.04287 0.04273 = 0.02923 0.00156 -0.00159 -0.03071 O14 4 0.270709 0.551520 0.325180 11.00000 0.02666 0.01762 = 0.04062 0.00177 0.00548 -0.00259 O15 4 0.433837 0.437684 0.263771 11.00000 0.02146 0.02627 = 0.03195 -0.00654 0.00071 -0.00848 C49 1 0.331605 0.467136 0.281759 11.00000 0.02495 0.01750 = 0.02336 0.00730 -0.00358 -0.00873 MOLE 4 N13 3 0.592069 0.211626 0.476597 11.00000 0.03443 0.03229 = 0.02589 0.00443 -0.00377 -0.01744 C41 1 0.528055 0.302811 0.421707 11.00000 0.03889 0.03383 = 0.03018 0.00907 -0.00932 -0.01954 AFIX 23 H41A 2 0.579930 0.317700 0.384013 11.00000 -1.20000 H41B 2 0.490038 0.279639 0.388926 11.00000 -1.20000 AFIX 0 C42 1 0.445123 0.405005 0.465148 11.00000 0.04075 0.03733 = 0.04248 0.00333 -0.01110 -0.01690 AFIX 137 H42A 2 0.391048 0.392304 0.500758 11.00000 -1.50000 H42B 2 0.408943 0.459406 0.425390 11.00000 -1.50000 H42C 2 0.481728 0.429418 0.497401 11.00000 -1.50000 AFIX 0 C43 1 0.516440 0.181903 0.533063 11.00000 0.04121 0.03476 = 0.02805 0.00085 0.00265 -0.02203 AFIX 23 H43A 2 0.560560 0.122879 0.567926 11.00000 -1.20000 H43B 2 0.466797 0.243509 0.568643 11.00000 -1.20000 AFIX 0 C44 1 0.448892 0.148782 0.491785 11.00000 0.04629 0.03708 = 0.03621 -0.00589 0.00218 -0.02394 AFIX 137 H44A 2 0.403548 0.207023 0.457867 11.00000 -1.50000 H44B 2 0.402358 0.131900 0.532681 11.00000 -1.50000 H44C 2 0.496959 0.085940 0.458035 11.00000 -1.50000 AFIX 0 C45 1 0.672238 0.119044 0.422280 11.00000 0.03782 0.03523 = 0.03150 0.00447 0.00042 -0.01256 AFIX 23 H45A 2 0.717685 0.142398 0.384829 11.00000 -1.20000 H45B 2 0.631092 0.100250 0.389196 11.00000 -1.20000 AFIX 0 C46 1 0.746499 0.020132 0.465326 11.00000 0.05101 0.03823 = 0.04264 0.00869 -0.00249 -0.01028 AFIX 137 H46A 2 0.794002 0.035277 0.493252 11.00000 -1.50000 H46B 2 0.790849 -0.037067 0.425791 11.00000 -1.50000 H46C 2 0.702733 -0.001867 0.504809 11.00000 -1.50000 AFIX 0 C47 1 0.649527 0.244423 0.530030 11.00000 0.04020 0.04354 = 0.03339 0.00721 -0.01148 -0.02412 AFIX 23 H47A 2 0.593758 0.303942 0.565090 11.00000 -1.20000 H47B 2 0.688697 0.184053 0.565681 11.00000 -1.20000 AFIX 0 C48 1 0.729416 0.278209 0.486299 11.00000 0.05366 0.07348 = 0.04919 0.01131 -0.01321 -0.04346 AFIX 137 H48A 2 0.788171 0.218478 0.454213 11.00000 -1.50000 H48B 2 0.759795 0.300204 0.525844 11.00000 -1.50000 H48C 2 0.692065 0.337845 0.450493 11.00000 -1.50000 HKLF 4 REM 2011sot0753 in P-1 REM R1 = 0.0618 for 10816 Fo > 4sig(Fo) and 0.0780 for all 13317 data REM 770 parameters refined using 36 restraints END WGHT 0.0610 1.3920 REM Highest difference peak 0.630, deepest hole -0.513, 1-sigma level 0.049 Q1 1 0.0198 -0.0332 0.0187 11.00000 0.05 0.63 Q2 1 0.4599 0.0318 0.0062 11.00000 0.05 0.52 Q3 1 0.3407 0.3585 0.2668 11.00000 0.05 0.42 Q4 1 0.9219 0.2352 0.2123 11.00000 0.05 0.37 Q5 1 0.1227 -0.0244 0.0349 11.00000 0.05 0.35 Q6 1 0.3536 -0.0294 0.1164 11.00000 0.05 0.34 Q7 1 0.0164 -0.0833 0.0541 11.00000 0.05 0.34 Q8 1 -0.0542 0.1434 0.0177 11.00000 0.05 0.33 Q9 1 0.7816 0.2246 0.2316 11.00000 0.05 0.31 Q10 1 -0.1058 0.2036 0.0222 11.00000 0.05 0.30 Q11 1 0.4567 -0.1133 0.1223 11.00000 0.05 0.30 Q12 1 0.0820 -0.0483 0.0705 11.00000 0.05 0.28 Q13 1 0.8209 0.2704 0.2327 11.00000 0.05 0.27 Q14 1 0.7792 0.3773 0.2628 11.00000 0.05 0.26 Q15 1 0.3028 0.0079 0.1007 11.00000 0.05 0.26 Q16 1 0.3786 0.0271 0.1584 11.00000 0.05 0.25 Q17 1 0.6661 -0.1787 0.0884 11.00000 0.05 0.25 Q18 1 0.3867 0.4976 0.4791 11.00000 0.05 0.25 Q19 1 0.7420 -0.1648 -0.0002 11.00000 0.05 0.25 Q20 1 0.7773 -0.0785 0.4282 11.00000 0.05 0.24 ;