data_shelxa _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '1,3-bis(4-nitrophenyl)urea with TMA2SO4.' _chemical_melting_point ? _chemical_formula_moiety '2(C13 H10 N4 O5), O4 S, 2(C4 H12 N), H2 O' _chemical_formula_sum 'C34 H46 N10 O15 S' _chemical_formula_weight 866.87 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.5775(5) _cell_length_b 27.1142(19) _cell_length_c 21.9859(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.063(7) _cell_angle_gamma 90.00 _cell_volume 3915.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20301 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 28.7 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.167 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9754 _exptl_absorpt_correction_T_max 0.9967 _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, HF 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_decay_% ? _diffrn_reflns_number 32551 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.1181 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6889 _reflns_number_gt 4731 _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 ? _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. ; _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^)+(0.0521P)^2^+1.7340P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6889 _refine_ls_number_parameters 586 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1126 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.021 _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 C1 C 0.1659(4) -0.00771(10) 0.33820(12) 0.0258(6) Uani 1 1 d . . . C2 C 0.1417(4) 0.00449(10) 0.27697(12) 0.0277(7) Uani 1 1 d . . . H2 H 0.1450 -0.0203 0.2466 0.033 Uiso 1 1 calc R . . C3 C 0.1131(4) 0.05296(10) 0.26107(12) 0.0265(6) Uani 1 1 d . . . H3 H 0.0980 0.0617 0.2192 0.032 Uiso 1 1 calc R . . C4 C 0.1057(4) 0.08980(10) 0.30559(11) 0.0247(6) Uani 1 1 d . . . C5 C 0.1299(4) 0.07657(10) 0.36725(11) 0.0260(6) Uani 1 1 d . . . H5 H 0.1248 0.1011 0.3980 0.031 Uiso 1 1 calc R . . C6 C 0.1610(4) 0.02794(10) 0.38300(12) 0.0262(6) Uani 1 1 d . . . H6 H 0.1792 0.0189 0.4247 0.031 Uiso 1 1 calc R . . C7 C 0.0631(4) 0.18034(10) 0.31815(11) 0.0252(6) Uani 1 1 d . . . C8 C 0.0177(4) 0.26990(10) 0.29794(12) 0.0243(6) Uani 1 1 d . . . C9 C -0.0006(4) 0.30483(10) 0.25079(12) 0.0264(6) Uani 1 1 d . . . H9 H -0.0040 0.2941 0.2096 0.032 Uiso 1 1 calc R . . C10 C -0.0136(4) 0.35428(10) 0.26329(12) 0.0266(6) Uani 1 1 d . . . H10 H -0.0288 0.3777 0.2312 0.032 Uiso 1 1 calc R . . C11 C -0.0043(4) 0.36950(10) 0.32380(12) 0.0255(6) Uani 1 1 d . . . C12 C 0.0149(4) 0.33572(10) 0.37110(12) 0.0258(6) Uani 1 1 d . . . H12 H 0.0207 0.3469 0.4121 0.031 Uiso 1 1 calc R . . C13 C 0.0254(4) 0.28633(10) 0.35874(11) 0.0257(6) Uani 1 1 d . . . H13 H 0.0380 0.2632 0.3912 0.031 Uiso 1 1 calc R . . C14 C 0.0066(4) 0.11275(10) 0.88706(11) 0.0238(6) Uani 1 1 d . . . C15 C -0.0020(4) 0.12821(10) 0.82654(12) 0.0246(6) Uani 1 1 d . . . H15 H -0.0135 0.1049 0.7943 0.030 Uiso 1 1 calc R . . C16 C 0.0064(4) 0.17757(10) 0.81429(11) 0.0247(6) Uani 1 1 d . . . H16 H -0.0013 0.1885 0.7732 0.030 Uiso 1 1 calc R . . C17 C 0.0262(4) 0.21230(10) 0.86129(11) 0.0248(6) Uani 1 1 d . . . C18 C 0.0334(4) 0.19617(10) 0.92223(11) 0.0247(6) Uani 1 1 d . . . H18 H 0.0450 0.2194 0.9546 0.030 Uiso 1 1 calc R . . C19 C 0.0234(4) 0.14655(10) 0.93465(12) 0.0255(6) Uani 1 1 d . . . H19 H 0.0280 0.1354 0.9757 0.031 Uiso 1 1 calc R . . C20 C 0.0676(4) 0.30226(10) 0.88008(12) 0.0257(6) Uani 1 1 d . . . C21 C 0.1109(4) 0.39258(10) 0.86600(11) 0.0248(6) Uani 1 1 d . . . C22 C 0.1207(4) 0.42892(10) 0.82097(12) 0.0249(6) Uani 1 1 d . . . H22 H 0.1048 0.4197 0.7793 0.030 Uiso 1 1 calc R . . C23 C 0.1527(4) 0.47743(10) 0.83561(11) 0.0259(6) Uani 1 1 d . . . H23 H 0.1595 0.5018 0.8047 0.031 Uiso 1 1 calc R . . C24 C 0.1749(4) 0.49012(10) 0.89680(12) 0.0266(6) Uani 1 1 d . . . C25 C 0.1638(4) 0.45533(10) 0.94228(12) 0.0276(7) Uani 1 1 d . . . H25 H 0.1785 0.4650 0.9838 0.033 Uiso 1 1 calc R . . C26 C 0.1313(4) 0.40664(10) 0.92742(11) 0.0256(6) Uani 1 1 d . . . H26 H 0.1228 0.3826 0.9586 0.031 Uiso 1 1 calc R . . C50 C -0.0140(5) 0.16384(11) 0.52231(13) 0.0423(8) Uani 1 1 d . . . H50A H 0.0285 0.1645 0.4803 0.063 Uiso 1 1 calc R . . H50B H -0.1573 0.1736 0.5230 0.063 Uiso 1 1 calc R . . H50C H 0.0030 0.1304 0.5388 0.063 Uiso 1 1 calc R . . C51 C 0.3339(5) 0.18391(12) 0.55940(15) 0.0423(8) Uani 1 1 d . . . H51A H 0.3772 0.1843 0.5174 0.064 Uiso 1 1 calc R . . H51B H 0.3507 0.1506 0.5762 0.064 Uiso 1 1 calc R . . H51C H 0.4172 0.2071 0.5842 0.064 Uiso 1 1 calc R . . C52 C 0.0913(6) 0.24946(10) 0.53504(14) 0.0428(8) Uani 1 1 d . . . H52A H 0.1326 0.2499 0.4929 0.064 Uiso 1 1 calc R . . H52B H 0.1778 0.2721 0.5597 0.064 Uiso 1 1 calc R . . H52C H -0.0511 0.2599 0.5361 0.064 Uiso 1 1 calc R . . C53 C 0.0519(5) 0.19770(12) 0.62368(12) 0.0391(8) Uani 1 1 d . . . H53A H 0.0672 0.1641 0.6398 0.059 Uiso 1 1 calc R . . H53B H -0.0907 0.2080 0.6250 0.059 Uiso 1 1 calc R . . H53C H 0.1383 0.2203 0.6484 0.059 Uiso 1 1 calc R . . C54 C 0.3137(4) 0.05064(11) 0.07996(13) 0.0323(7) Uani 1 1 d . . . H54A H 0.2153 0.0708 0.1008 0.049 Uiso 1 1 calc R . . H54B H 0.3276 0.0185 0.1001 0.049 Uiso 1 1 calc R . . H54C H 0.2659 0.0459 0.0374 0.049 Uiso 1 1 calc R . . C55 C 0.5862(5) 0.08313(11) 0.14737(12) 0.0337(7) Uani 1 1 d . . . H55A H 0.4859 0.1028 0.1682 0.051 Uiso 1 1 calc R . . H55B H 0.7174 0.1004 0.1494 0.051 Uiso 1 1 calc R . . H55C H 0.6020 0.0509 0.1673 0.051 Uiso 1 1 calc R . . C56 C 0.4927(5) 0.12484(10) 0.05136(13) 0.0352(7) Uani 1 1 d . . . H56A H 0.3920 0.1447 0.0717 0.053 Uiso 1 1 calc R . . H56B H 0.4472 0.1199 0.0086 0.053 Uiso 1 1 calc R . . H56C H 0.6240 0.1420 0.0534 0.053 Uiso 1 1 calc R . . C57 C 0.6687(5) 0.04624(11) 0.05114(13) 0.0335(7) Uani 1 1 d . . . H57A H 0.6229 0.0414 0.0084 0.050 Uiso 1 1 calc R . . H57B H 0.6845 0.0141 0.0712 0.050 Uiso 1 1 calc R . . H57C H 0.7996 0.0636 0.0533 0.050 Uiso 1 1 calc R . . N1 N 0.2010(4) -0.05896(8) 0.35536(10) 0.0298(6) Uani 1 1 d . . . N2 N 0.0762(4) 0.13778(8) 0.28442(9) 0.0270(5) Uani 1 1 d . . . H2A H 0.0645 0.1413 0.2446 0.032 Uiso 1 1 calc R . . N3 N 0.0281(3) 0.22071(8) 0.28109(9) 0.0247(5) Uani 1 1 d . . . H3A H 0.0101 0.2145 0.2419 0.030 Uiso 1 1 calc R . . N4 N -0.0171(4) 0.42156(9) 0.33835(11) 0.0314(6) Uani 1 1 d . . . N5 N 0.0002(4) 0.06057(8) 0.90041(10) 0.0277(5) Uani 1 1 d . . . N6 N 0.0381(3) 0.26153(8) 0.84356(9) 0.0257(5) Uani 1 1 d . . . H6A H 0.0252 0.2672 0.8041 0.031 Uiso 1 1 calc R . . N7 N 0.0780(3) 0.34452(8) 0.84565(9) 0.0243(5) Uani 1 1 d . . . H7A H 0.0619 0.3406 0.8059 0.029 Uiso 1 1 calc R . . N8 N 0.2184(4) 0.54120(8) 0.91287(10) 0.0298(6) Uani 1 1 d . . . N10 N 0.1134(4) 0.19881(8) 0.55998(10) 0.0287(6) Uani 1 1 d . . . N11 N 0.5153(3) 0.07604(8) 0.08234(9) 0.0242(5) Uani 1 1 d . . . O1 O 0.2475(4) -0.06849(7) 0.40920(8) 0.0402(5) Uani 1 1 d . . . O2 O 0.1826(3) -0.09104(7) 0.31576(8) 0.0361(5) Uani 1 1 d . . . O3 O 0.0805(3) 0.18221(7) 0.37375(8) 0.0294(5) Uani 1 1 d . . . O4 O -0.0093(3) 0.43393(7) 0.39293(9) 0.0379(5) Uani 1 1 d . . . O5 O -0.0348(3) 0.45169(7) 0.29659(9) 0.0403(5) Uani 1 1 d . . . O6 O 0.0063(3) 0.04699(7) 0.95407(8) 0.0312(5) Uani 1 1 d . . . O7 O -0.0096(3) 0.03107(7) 0.85748(8) 0.0386(5) Uani 1 1 d . . . O8 O 0.0834(3) 0.30106(7) 0.93554(8) 0.0315(5) Uani 1 1 d . . . O9 O 0.2421(4) 0.55246(7) 0.96707(9) 0.0402(5) Uani 1 1 d . . . O10 O 0.2312(3) 0.57157(7) 0.87134(9) 0.0384(5) Uani 1 1 d . . . O100 O 0.5358(4) 0.19559(8) 0.22395(9) 0.0325(5) Uani 1 1 d D . . S1 S 0.04443(11) 0.18307(3) 0.12489(3) 0.02514(18) Uani 1 1 d D . . O20A O -0.130(3) 0.2071(7) 0.1585(9) 0.027(6) Uani 0.350(5) 1 d PDU A 1 O21A O 0.0789(11) 0.1348(2) 0.1589(2) 0.0304(18) Uani 0.350(5) 1 d PDU A 1 O22A O -0.0177(10) 0.1763(3) 0.0646(2) 0.0344(19) Uani 0.350(5) 1 d PDU A 1 O23A O 0.2206(8) 0.2147(2) 0.1373(3) 0.034(2) Uani 0.350(5) 1 d PDU A 1 O20B O -0.1117(15) 0.2063(4) 0.1599(5) 0.029(3) Uani 0.650(5) 1 d PDU A 2 O21B O 0.1971(5) 0.15880(13) 0.16680(12) 0.0287(10) Uani 0.650(5) 1 d PDU A 2 O22B O -0.0434(5) 0.14577(15) 0.08254(15) 0.0313(10) Uani 0.650(5) 1 d PDU A 2 O23B O 0.1506(5) 0.22059(11) 0.08873(15) 0.0366(11) Uani 0.650(5) 1 d PDU A 2 H2W H 0.634(4) 0.1952(11) 0.1995(12) 0.036(9) Uiso 1 1 d D . . H1W H 0.438(5) 0.1912(14) 0.1982(15) 0.081(14) Uiso 1 1 d 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 0.0212(16) 0.0286(16) 0.0277(14) -0.0010(12) 0.0015(12) -0.0018(12) C2 0.0232(16) 0.0354(17) 0.0245(14) -0.0078(12) -0.0001(12) -0.0012(13) C3 0.0223(16) 0.0377(18) 0.0195(13) -0.0028(12) -0.0001(12) -0.0006(13) C4 0.0148(15) 0.0323(16) 0.0270(14) -0.0017(12) 0.0010(12) -0.0009(12) C5 0.0203(16) 0.0347(17) 0.0231(14) -0.0034(12) 0.0008(12) -0.0016(12) C6 0.0195(16) 0.0365(17) 0.0227(13) -0.0004(12) 0.0007(12) -0.0037(12) C7 0.0169(15) 0.0355(17) 0.0232(14) -0.0001(12) 0.0016(11) -0.0034(12) C8 0.0148(15) 0.0315(16) 0.0265(14) -0.0035(12) -0.0011(11) 0.0018(12) C9 0.0201(15) 0.0350(18) 0.0239(14) -0.0045(12) 0.0000(12) -0.0027(12) C10 0.0181(16) 0.0366(18) 0.0251(14) 0.0003(12) 0.0000(12) -0.0024(12) C11 0.0177(15) 0.0301(16) 0.0286(14) -0.0022(12) 0.0015(12) -0.0021(12) C12 0.0179(15) 0.0360(17) 0.0235(13) -0.0078(12) 0.0017(12) -0.0029(12) C13 0.0184(15) 0.0360(17) 0.0227(13) -0.0014(12) 0.0007(11) 0.0009(12) C14 0.0169(15) 0.0282(16) 0.0261(14) 0.0014(12) -0.0009(12) 0.0000(12) C15 0.0163(15) 0.0337(17) 0.0237(14) -0.0002(12) -0.0009(11) 0.0002(12) C16 0.0185(15) 0.0347(17) 0.0207(13) 0.0014(12) 0.0003(11) 0.0009(12) C17 0.0158(15) 0.0326(17) 0.0258(14) 0.0029(12) 0.0001(11) 0.0011(12) C18 0.0181(15) 0.0339(17) 0.0221(13) -0.0013(11) 0.0007(11) 0.0010(12) C19 0.0184(15) 0.0338(17) 0.0241(14) 0.0034(12) 0.0003(12) 0.0011(12) C20 0.0187(16) 0.0334(17) 0.0250(14) -0.0005(12) -0.0002(12) 0.0024(12) C21 0.0166(15) 0.0322(16) 0.0253(14) 0.0004(12) -0.0012(12) 0.0022(12) C22 0.0186(15) 0.0335(17) 0.0227(13) 0.0000(12) 0.0012(11) 0.0006(12) C23 0.0190(16) 0.0343(17) 0.0245(14) 0.0046(12) 0.0021(12) 0.0027(12) C24 0.0199(16) 0.0310(17) 0.0292(15) 0.0023(12) 0.0033(12) 0.0029(12) C25 0.0221(16) 0.0373(18) 0.0234(14) -0.0005(12) 0.0006(12) -0.0009(13) C26 0.0202(16) 0.0330(17) 0.0234(13) 0.0046(12) -0.0014(12) 0.0000(12) C50 0.054(2) 0.0403(19) 0.0308(16) -0.0038(14) -0.0105(15) -0.0104(16) C51 0.035(2) 0.0404(19) 0.0527(19) -0.0030(15) 0.0123(16) 0.0043(15) C52 0.056(2) 0.0308(18) 0.0407(18) 0.0029(14) -0.0102(17) -0.0006(16) C53 0.041(2) 0.052(2) 0.0249(14) -0.0053(14) 0.0037(14) -0.0077(16) C54 0.0244(17) 0.0334(17) 0.0387(16) -0.0017(13) -0.0031(14) -0.0040(13) C55 0.0374(19) 0.0407(18) 0.0226(14) -0.0016(12) -0.0022(13) -0.0062(14) C56 0.038(2) 0.0292(17) 0.0386(16) 0.0084(13) 0.0057(15) 0.0051(14) C57 0.0283(18) 0.0354(17) 0.0374(16) -0.0031(13) 0.0070(14) 0.0074(13) N1 0.0263(15) 0.0342(14) 0.0295(13) -0.0012(11) 0.0062(11) -0.0019(11) N2 0.0300(14) 0.0325(14) 0.0182(11) -0.0032(10) -0.0023(10) 0.0045(11) N3 0.0241(14) 0.0316(14) 0.0180(11) -0.0027(10) -0.0015(10) 0.0026(10) N4 0.0253(15) 0.0347(15) 0.0345(14) -0.0050(12) 0.0032(11) -0.0043(11) N5 0.0236(14) 0.0321(14) 0.0272(13) 0.0004(11) -0.0003(10) -0.0023(10) N6 0.0263(14) 0.0303(14) 0.0203(11) 0.0022(10) 0.0004(10) 0.0013(10) N7 0.0245(14) 0.0284(13) 0.0199(11) 0.0009(10) -0.0004(10) 0.0012(10) N8 0.0243(14) 0.0336(14) 0.0316(13) 0.0025(11) 0.0006(11) -0.0008(11) N10 0.0315(15) 0.0307(13) 0.0239(11) -0.0011(10) -0.0002(10) 0.0013(11) N11 0.0248(14) 0.0260(13) 0.0221(11) -0.0013(9) 0.0029(10) 0.0035(10) O1 0.0541(16) 0.0389(12) 0.0272(11) 0.0038(9) -0.0017(10) -0.0004(11) O2 0.0412(14) 0.0344(12) 0.0327(11) -0.0084(9) 0.0043(10) -0.0008(10) O3 0.0325(12) 0.0348(11) 0.0208(9) -0.0019(8) -0.0014(8) -0.0013(9) O4 0.0435(14) 0.0380(12) 0.0320(11) -0.0106(9) -0.0006(10) -0.0049(10) O5 0.0489(15) 0.0349(12) 0.0374(12) 0.0036(10) 0.0037(11) -0.0023(10) O6 0.0313(13) 0.0375(12) 0.0249(10) 0.0066(8) 0.0023(9) 0.0003(9) O7 0.0530(15) 0.0336(12) 0.0288(11) -0.0035(9) -0.0023(10) -0.0073(10) O8 0.0353(13) 0.0354(11) 0.0234(10) 0.0013(8) -0.0012(9) -0.0026(9) O9 0.0509(15) 0.0416(13) 0.0277(11) -0.0052(9) -0.0021(10) -0.0067(11) O10 0.0531(15) 0.0298(11) 0.0325(11) 0.0058(9) 0.0046(10) -0.0046(10) O100 0.0304(13) 0.0447(13) 0.0225(10) -0.0028(9) 0.0013(10) -0.0035(10) S1 0.0222(4) 0.0285(4) 0.0243(3) -0.0007(3) -0.0022(3) 0.0006(3) O20A 0.027(9) 0.022(10) 0.033(11) 0.002(7) 0.003(7) -0.002(6) O21A 0.041(5) 0.021(3) 0.030(3) 0.000(2) 0.008(3) 0.006(3) O22A 0.045(4) 0.044(5) 0.014(3) -0.002(3) -0.006(3) 0.008(3) O23A 0.013(3) 0.037(4) 0.052(4) 0.002(3) -0.002(3) -0.015(2) O20B 0.020(4) 0.047(7) 0.019(5) -0.007(4) -0.001(3) 0.010(4) O21B 0.023(2) 0.040(2) 0.0231(15) 0.0001(14) -0.0027(14) 0.0068(17) O22B 0.0288(19) 0.039(2) 0.0256(18) -0.0095(16) -0.0035(14) -0.0038(17) O23B 0.027(2) 0.0395(19) 0.044(2) 0.0119(15) 0.0037(17) -0.0032(15) _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 C1 C6 1.382(4) . ? C1 C2 1.387(4) . ? C1 N1 1.455(4) . ? C2 C3 1.370(4) . ? C2 H2 0.9500 . ? C3 C4 1.401(4) . ? C3 H3 0.9500 . ? C4 N2 1.392(3) . ? C4 C5 1.403(4) . ? C5 C6 1.376(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O3 1.223(3) . ? C7 N3 1.377(3) . ? C7 N2 1.377(3) . ? C8 N3 1.387(3) . ? C8 C9 1.405(4) . ? C8 C13 1.407(3) . ? C9 C10 1.372(4) . ? C9 H9 0.9500 . ? C10 C11 1.391(4) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 N4 1.451(4) . ? C12 C13 1.369(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.391(4) . ? C14 C15 1.393(3) . ? C14 N5 1.446(3) . ? C15 C16 1.367(4) . ? C15 H15 0.9500 . ? C16 C17 1.399(4) . ? C16 H16 0.9500 . ? C17 N6 1.394(3) . ? C17 C18 1.408(4) . ? C18 C19 1.375(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 O8 1.219(3) . ? C20 N6 1.373(3) . ? C20 N7 1.377(3) . ? C21 N7 1.391(3) . ? C21 C22 1.401(4) . ? C21 C26 1.403(3) . ? C22 C23 1.368(4) . ? C22 H22 0.9500 . ? C23 C24 1.389(4) . ? C23 H23 0.9500 . ? C24 C25 1.379(4) . ? C24 N8 1.454(4) . ? C25 C26 1.374(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C50 N10 1.488(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 N10 1.506(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 N10 1.483(4) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 N10 1.479(3) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 N11 1.493(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N11 1.492(3) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 N11 1.492(3) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N11 1.488(3) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? N1 O2 1.232(3) . ? N1 O1 1.234(3) . ? N2 H2A 0.8800 . ? N3 H3A 0.8800 . ? N4 O5 1.230(3) . ? N4 O4 1.245(3) . ? N5 O6 1.234(3) . ? N5 O7 1.236(3) . ? N6 H6A 0.8800 . ? N7 H7A 0.8800 . ? N8 O9 1.232(3) . ? N8 O10 1.236(3) . ? O100 H2W 0.864(18) . ? O100 H1W 0.844(19) . ? S1 O22A 1.380(5) . ? S1 O23A 1.455(5) . ? S1 O20B 1.458(6) . ? S1 O22B 1.472(3) . ? S1 O21B 1.480(3) . ? S1 O23B 1.488(3) . ? S1 O21A 1.518(5) . ? S1 O20A 1.543(10) . ? 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 C6 C1 C2 121.3(3) . . ? C6 C1 N1 119.5(2) . . ? C2 C1 N1 119.2(2) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 121.0(2) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? N2 C4 C3 116.2(2) . . ? N2 C4 C5 124.6(2) . . ? C3 C4 C5 119.1(2) . . ? C6 C5 C4 119.7(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? O3 C7 N3 124.2(2) . . ? O3 C7 N2 124.6(2) . . ? N3 C7 N2 111.1(2) . . ? N3 C8 C9 117.1(2) . . ? N3 C8 C13 123.9(2) . . ? C9 C8 C13 119.0(2) . . ? C10 C9 C8 121.0(2) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 118.8(3) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 121.3(2) . . ? C12 C11 N4 118.8(2) . . ? C10 C11 N4 120.0(2) . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 119.9(3) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C19 C14 C15 121.2(2) . . ? C19 C14 N5 119.6(2) . . ? C15 C14 N5 119.2(2) . . ? C16 C15 C14 118.9(2) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C17 121.1(2) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? N6 C17 C16 116.3(2) . . ? N6 C17 C18 124.3(2) . . ? C16 C17 C18 119.4(2) . . ? C19 C18 C17 119.6(2) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C14 119.9(2) . . ? C18 C19 H19 120.1 . . ? C14 C19 H19 120.1 . . ? O8 C20 N6 124.4(2) . . ? O8 C20 N7 124.6(2) . . ? N6 C20 N7 110.9(2) . . ? N7 C21 C22 116.4(2) . . ? N7 C21 C26 124.7(2) . . ? C22 C21 C26 118.9(2) . . ? C23 C22 C21 121.5(2) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 118.2(2) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C25 C24 C23 121.7(3) . . ? C25 C24 N8 119.5(2) . . ? C23 C24 N8 118.7(2) . . ? C26 C25 C24 119.9(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 119.7(2) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? N10 C50 H50A 109.5 . . ? N10 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N10 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N10 C51 H51A 109.5 . . ? N10 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N10 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N10 C52 H52A 109.5 . . ? N10 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N10 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N10 C53 H53A 109.5 . . ? N10 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N10 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N11 C54 H54A 109.5 . . ? N11 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N11 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N11 C55 H55A 109.5 . . ? N11 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N11 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N11 C56 H56A 109.5 . . ? N11 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N11 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N11 C57 H57A 109.5 . . ? N11 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N11 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O2 N1 O1 122.7(2) . . ? O2 N1 C1 118.9(2) . . ? O1 N1 C1 118.4(2) . . ? C7 N2 C4 127.9(2) . . ? C7 N2 H2A 116.0 . . ? C4 N2 H2A 116.0 . . ? C7 N3 C8 128.0(2) . . ? C7 N3 H3A 116.0 . . ? C8 N3 H3A 116.0 . . ? O5 N4 O4 122.6(2) . . ? O5 N4 C11 119.1(2) . . ? O4 N4 C11 118.4(2) . . ? O6 N5 O7 122.3(2) . . ? O6 N5 C14 119.1(2) . . ? O7 N5 C14 118.6(2) . . ? C20 N6 C17 128.0(2) . . ? C20 N6 H6A 116.0 . . ? C17 N6 H6A 116.0 . . ? C20 N7 C21 127.9(2) . . ? C20 N7 H7A 116.1 . . ? C21 N7 H7A 116.1 . . ? O9 N8 O10 122.7(2) . . ? O9 N8 C24 118.9(2) . . ? O10 N8 C24 118.4(2) . . ? C53 N10 C52 110.0(2) . . ? C53 N10 C50 109.9(2) . . ? C52 N10 C50 110.1(2) . . ? C53 N10 C51 108.4(2) . . ? C52 N10 C51 108.7(2) . . ? C50 N10 C51 109.8(2) . . ? C57 N11 C56 108.9(2) . . ? C57 N11 C55 109.1(2) . . ? C56 N11 C55 110.0(2) . . ? C57 N11 C54 110.9(2) . . ? C56 N11 C54 109.0(2) . . ? C55 N11 C54 108.9(2) . . ? H2W O100 H1W 99(3) . . ? O22A S1 O23A 116.8(4) . . ? O22A S1 O20B 112.6(6) . . ? O23A S1 O20B 102.9(6) . . ? O22A S1 O22B 38.2(3) . . ? O23A S1 O22B 143.6(3) . . ? O20B S1 O22B 111.5(5) . . ? O22A S1 O21B 134.1(3) . . ? O23A S1 O21B 68.8(3) . . ? O20B S1 O21B 109.7(5) . . ? O22B S1 O21B 108.58(19) . . ? O22A S1 O23B 72.6(4) . . ? O23A S1 O23B 46.0(2) . . ? O20B S1 O23B 110.5(5) . . ? O22B S1 O23B 108.1(2) . . ? O21B S1 O23B 108.33(19) . . ? O22A S1 O21A 112.8(4) . . ? O23A S1 O21A 108.6(4) . . ? O20B S1 O21A 101.7(5) . . ? O22B S1 O21A 76.3(3) . . ? O21B S1 O21A 39.8(2) . . ? O23B S1 O21A 142.2(3) . . ? O22A S1 O20A 109.1(9) . . ? O23A S1 O20A 105.5(8) . . ? O20B S1 O20A 3.5(13) . . ? O22B S1 O20A 108.5(8) . . ? O21B S1 O20A 112.8(8) . . ? O23B S1 O20A 110.4(7) . . ? O21A S1 O20A 102.9(8) . . ? 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 H2A O21A 0.88 1.90 2.762(6) 165.9 . N2 H2A O21B 0.88 2.02 2.804(4) 148.3 . N2 H2A S1 0.88 2.86 3.711(2) 162.9 . N3 H3A O20B 0.88 1.95 2.800(12) 163.1 . N3 H3A O20A 0.88 2.02 2.86(2) 160.1 . N3 H3A O21B 0.88 2.60 3.266(3) 133.6 . N3 H3A S1 0.88 2.73 3.590(2) 165.6 . N6 H6A O100 0.88 2.04 2.875(3) 159.0 4_566 N7 H7A O100 0.88 2.05 2.888(3) 158.2 4_566 O100 H2W O20A 0.864(18) 1.86(2) 2.708(14) 166(3) 1_655 O100 H2W O20B 0.864(18) 1.95(2) 2.792(9) 165(3) 1_655 O100 H1W O21B 0.844(19) 1.91(2) 2.691(4) 154(4) . O100 H1W O23A 0.844(19) 2.01(3) 2.789(6) 153(4) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.245 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.054 _iucr_refine_instructions_details ; TITL shelxa in P2(1)/n CELL 0.71073 6.5775 27.1142 21.9859 90.000 93.063 90.000 ZERR 4.00 0.0005 0.0019 0.0015 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S UNIT 136 184 40 60 4 MERG 2 OMIT 2 8 2 OMIT 0 14 6 OMIT 3 6 4 OMIT -3 13 5 OMIT 3 10 3 OMIT 3 2 4 OMIT 1 1 7 OMIT 2 4 4 SHEL 7 0.84 LIST 4 DFIX 0.84 0.02 H1W O100 DFIX 0.84 0.02 H2W O100 SADI S1 O20A S1 O20B SADI S1 O21A S1 O21B SADI S1 O22A S1 O22B SADI S1 O23A S1 O23B DANG 2.45 0.02 O20A O21A DANG 2.45 0.02 O20B O21B DANG 2.45 0.02 O20A O22A DANG 2.45 0.02 O20B O22B DANG 2.45 0.02 O20A O23A DANG 2.45 0.02 O20B O23B DANG 2.45 0.02 O21A O22A DANG 2.45 0.02 O21B O22B DANG 2.45 0.02 O21A O23A DANG 2.45 0.02 O21B O23B DANG 2.45 0.02 O23A O22A DANG 2.45 0.02 O23B O22B SIMU O20A O20B O21A O21B O22A O22B O23A O23B FMAP 2 PLAN 20 SIZE 0.02 0.02 0.15 ACTA 55.00 BOND BOND $H HTAB HTAB N2 O21A HTAB N2 O21B HTAB N2 S1 HTAB N3 O20B HTAB N3 O20A HTAB N3 O21B HTAB N3 S1 HTAB N6 O100_$1 HTAB N7 O100_$1 HTAB O100 O20A_$2 HTAB O100 O20B_$2 HTAB O100 O21B HTAB O100 O23A HTAB O100 S1 EQIV $1 x-1/2, -y+1/2, z+1/2 EQIV $2 x+1, y, z L.S. 10 SIZE 0.15 0.02 0.02 TEMP -173.00 WGHT 0.052100 1.734000 FVAR 0.06597 0.35005 C1 1 0.165878 -0.007706 0.338202 11.00000 0.02124 0.02865 = 0.02766 -0.00097 0.00149 -0.00183 C2 1 0.141723 0.004491 0.276969 11.00000 0.02321 0.03535 = 0.02448 -0.00778 -0.00014 -0.00122 AFIX 43 H2 2 0.144983 -0.020347 0.246560 11.00000 -1.20000 AFIX 0 C3 1 0.113084 0.052957 0.261069 11.00000 0.02227 0.03773 = 0.01948 -0.00285 -0.00013 -0.00062 AFIX 43 H3 2 0.097977 0.061714 0.219233 11.00000 -1.20000 AFIX 0 C4 1 0.105747 0.089796 0.305594 11.00000 0.01484 0.03227 = 0.02699 -0.00168 0.00103 -0.00091 C5 1 0.129885 0.076574 0.367255 11.00000 0.02028 0.03465 = 0.02305 -0.00341 0.00078 -0.00158 AFIX 43 H5 2 0.124755 0.101095 0.397998 11.00000 -1.20000 AFIX 0 C6 1 0.161018 0.027941 0.383002 11.00000 0.01945 0.03646 = 0.02266 -0.00042 0.00066 -0.00368 AFIX 43 H6 2 0.179171 0.018875 0.424676 11.00000 -1.20000 AFIX 0 C7 1 0.063115 0.180343 0.318153 11.00000 0.01688 0.03552 = 0.02322 -0.00013 0.00160 -0.00336 C8 1 0.017738 0.269900 0.297937 11.00000 0.01484 0.03151 = 0.02646 -0.00352 -0.00108 0.00184 C9 1 -0.000581 0.304832 0.250787 11.00000 0.02014 0.03500 = 0.02389 -0.00448 0.00001 -0.00266 AFIX 43 H9 2 -0.003992 0.294064 0.209627 11.00000 -1.20000 AFIX 0 C10 1 -0.013625 0.354278 0.263290 11.00000 0.01805 0.03658 = 0.02509 0.00034 -0.00004 -0.00244 AFIX 43 H10 2 -0.028772 0.377685 0.231215 11.00000 -1.20000 AFIX 0 C11 1 -0.004259 0.369501 0.323803 11.00000 0.01770 0.03013 = 0.02855 -0.00223 0.00146 -0.00211 C12 1 0.014878 0.335722 0.371098 11.00000 0.01788 0.03598 = 0.02351 -0.00780 0.00168 -0.00292 AFIX 43 H12 2 0.020668 0.346860 0.412122 11.00000 -1.20000 AFIX 0 C13 1 0.025441 0.286330 0.358740 11.00000 0.01835 0.03595 = 0.02271 -0.00142 0.00071 0.00090 AFIX 43 H13 2 0.037952 0.263180 0.391158 11.00000 -1.20000 AFIX 0 C14 1 0.006590 0.112749 0.887060 11.00000 0.01692 0.02815 = 0.02605 0.00144 -0.00089 0.00002 C15 1 -0.002012 0.128215 0.826540 11.00000 0.01630 0.03368 = 0.02366 -0.00020 -0.00093 0.00022 AFIX 43 H15 2 -0.013529 0.104852 0.794339 11.00000 -1.20000 AFIX 0 C16 1 0.006402 0.177567 0.814293 11.00000 0.01854 0.03467 = 0.02072 0.00138 0.00032 0.00094 AFIX 43 H16 2 -0.001312 0.188470 0.773171 11.00000 -1.20000 AFIX 0 C17 1 0.026181 0.212301 0.861291 11.00000 0.01584 0.03258 = 0.02579 0.00292 0.00015 0.00113 C18 1 0.033380 0.196167 0.922228 11.00000 0.01807 0.03393 = 0.02213 -0.00133 0.00071 0.00101 AFIX 43 H18 2 0.045038 0.219408 0.954560 11.00000 -1.20000 AFIX 0 C19 1 0.023426 0.146545 0.934648 11.00000 0.01839 0.03378 = 0.02410 0.00340 0.00025 0.00109 AFIX 43 H19 2 0.028041 0.135372 0.975652 11.00000 -1.20000 AFIX 0 C20 1 0.067567 0.302261 0.880077 11.00000 0.01868 0.03343 = 0.02497 -0.00047 -0.00023 0.00242 C21 1 0.110943 0.392576 0.865996 11.00000 0.01663 0.03217 = 0.02528 0.00036 -0.00116 0.00216 C22 1 0.120711 0.428920 0.820973 11.00000 0.01856 0.03354 = 0.02274 0.00004 0.00117 0.00061 AFIX 43 H22 2 0.104751 0.419666 0.779316 11.00000 -1.20000 AFIX 0 C23 1 0.152706 0.477435 0.835614 11.00000 0.01898 0.03430 = 0.02448 0.00462 0.00214 0.00266 AFIX 43 H23 2 0.159548 0.501804 0.804744 11.00000 -1.20000 AFIX 0 C24 1 0.174917 0.490117 0.896797 11.00000 0.01988 0.03104 = 0.02923 0.00233 0.00326 0.00294 C25 1 0.163767 0.455331 0.942282 11.00000 0.02210 0.03732 = 0.02342 -0.00050 0.00055 -0.00088 AFIX 43 H25 2 0.178482 0.465024 0.983807 11.00000 -1.20000 AFIX 0 C26 1 0.131344 0.406641 0.927424 11.00000 0.02023 0.03297 = 0.02338 0.00464 -0.00140 -0.00002 AFIX 43 H26 2 0.122776 0.382601 0.958616 11.00000 -1.20000 AFIX 0 C50 1 -0.013956 0.163842 0.522308 11.00000 0.05445 0.04033 = 0.03082 -0.00375 -0.01051 -0.01037 AFIX 33 H50A 2 0.028508 0.164490 0.480264 11.00000 -1.50000 H50B 2 -0.157308 0.173565 0.523026 11.00000 -1.50000 H50C 2 0.003012 0.130433 0.538816 11.00000 -1.50000 AFIX 0 C51 1 0.333869 0.183911 0.559402 11.00000 0.03503 0.04038 = 0.05270 -0.00302 0.01230 0.00434 AFIX 33 H51A 2 0.377202 0.184350 0.517445 11.00000 -1.50000 H51B 2 0.350661 0.150592 0.576200 11.00000 -1.50000 H51C 2 0.417200 0.207093 0.584182 11.00000 -1.50000 AFIX 0 C52 1 0.091326 0.249460 0.535044 11.00000 0.05568 0.03079 = 0.04070 0.00293 -0.01018 -0.00057 AFIX 33 H52A 2 0.132616 0.249857 0.492873 11.00000 -1.50000 H52B 2 0.177836 0.272099 0.559652 11.00000 -1.50000 H52C 2 -0.051085 0.259894 0.536125 11.00000 -1.50000 AFIX 0 C53 1 0.051854 0.197699 0.623684 11.00000 0.04065 0.05191 = 0.02494 -0.00529 0.00370 -0.00772 AFIX 33 H53A 2 0.067163 0.164129 0.639801 11.00000 -1.50000 H53B 2 -0.090680 0.207978 0.625014 11.00000 -1.50000 H53C 2 0.138269 0.220252 0.648449 11.00000 -1.50000 AFIX 0 C54 1 0.313692 0.050638 0.079958 11.00000 0.02440 0.03335 = 0.03873 -0.00168 -0.00311 -0.00398 AFIX 33 H54A 2 0.215287 0.070845 0.100781 11.00000 -1.50000 H54B 2 0.327564 0.018500 0.100150 11.00000 -1.50000 H54C 2 0.265863 0.045892 0.037379 11.00000 -1.50000 AFIX 0 C55 1 0.586243 0.083132 0.147372 11.00000 0.03739 0.04074 = 0.02260 -0.00159 -0.00223 -0.00621 AFIX 33 H55A 2 0.485918 0.102769 0.168175 11.00000 -1.50000 H55B 2 0.717404 0.100361 0.149357 11.00000 -1.50000 H55C 2 0.601966 0.050919 0.167285 11.00000 -1.50000 AFIX 0 C56 1 0.492688 0.124841 0.051359 11.00000 0.03821 0.02920 = 0.03862 0.00842 0.00572 0.00510 AFIX 33 H56A 2 0.391969 0.144724 0.071663 11.00000 -1.50000 H56B 2 0.447196 0.119857 0.008627 11.00000 -1.50000 H56C 2 0.624020 0.141994 0.053436 11.00000 -1.50000 AFIX 0 C57 1 0.668672 0.046242 0.051138 11.00000 0.02825 0.03538 = 0.03737 -0.00307 0.00703 0.00735 AFIX 33 H57A 2 0.622925 0.041434 0.008396 11.00000 -1.50000 H57B 2 0.684452 0.014097 0.071217 11.00000 -1.50000 H57C 2 0.799614 0.063570 0.053254 11.00000 -1.50000 AFIX 0 N1 3 0.200981 -0.058964 0.355357 11.00000 0.02632 0.03416 = 0.02947 -0.00119 0.00623 -0.00190 N2 3 0.076225 0.137776 0.284420 11.00000 0.03004 0.03250 = 0.01820 -0.00325 -0.00230 0.00454 AFIX 43 H2A 2 0.064503 0.141347 0.244604 11.00000 -1.20000 AFIX 0 N3 3 0.028099 0.220705 0.281086 11.00000 0.02408 0.03164 = 0.01802 -0.00269 -0.00155 0.00264 AFIX 43 H3A 2 0.010068 0.214538 0.241872 11.00000 -1.20000 AFIX 0 N4 3 -0.017095 0.421555 0.338349 11.00000 0.02535 0.03467 = 0.03445 -0.00502 0.00321 -0.00431 N5 3 0.000236 0.060571 0.900414 11.00000 0.02363 0.03211 = 0.02721 0.00039 -0.00027 -0.00231 N6 3 0.038120 0.261531 0.843562 11.00000 0.02627 0.03027 = 0.02033 0.00222 0.00036 0.00132 AFIX 43 H6A 2 0.025201 0.267197 0.804134 11.00000 -1.20000 AFIX 0 N7 3 0.078020 0.344517 0.845650 11.00000 0.02454 0.02842 = 0.01990 0.00090 -0.00035 0.00119 AFIX 43 H7A 2 0.061913 0.340646 0.805945 11.00000 -1.20000 AFIX 0 N8 3 0.218419 0.541204 0.912868 11.00000 0.02427 0.03355 = 0.03158 0.00252 0.00057 -0.00077 N10 3 0.113436 0.198813 0.559984 11.00000 0.03146 0.03069 = 0.02388 -0.00105 -0.00023 0.00131 N11 3 0.515338 0.076043 0.082340 11.00000 0.02480 0.02601 = 0.02209 -0.00125 0.00290 0.00346 O1 4 0.247508 -0.068487 0.409196 11.00000 0.05411 0.03894 = 0.02718 0.00378 -0.00165 -0.00044 O2 4 0.182641 -0.091044 0.315757 11.00000 0.04125 0.03444 = 0.03275 -0.00843 0.00427 -0.00083 O3 4 0.080498 0.182215 0.373749 11.00000 0.03248 0.03477 = 0.02079 -0.00187 -0.00138 -0.00129 O4 4 -0.009341 0.433927 0.392935 11.00000 0.04355 0.03797 = 0.03202 -0.01057 -0.00059 -0.00490 O5 4 -0.034843 0.451693 0.296587 11.00000 0.04886 0.03488 = 0.03737 0.00361 0.00367 -0.00228 O6 4 0.006274 0.046987 0.954068 11.00000 0.03130 0.03746 = 0.02486 0.00661 0.00233 0.00028 O7 4 -0.009638 0.031074 0.857485 11.00000 0.05300 0.03361 = 0.02883 -0.00345 -0.00232 -0.00733 O8 4 0.083358 0.301055 0.935545 11.00000 0.03532 0.03538 = 0.02342 0.00129 -0.00117 -0.00259 O9 4 0.242141 0.552456 0.967071 11.00000 0.05094 0.04162 = 0.02771 -0.00517 -0.00207 -0.00667 O10 4 0.231170 0.571572 0.871338 11.00000 0.05313 0.02978 = 0.03251 0.00584 0.00464 -0.00455 O100 4 0.535844 0.195591 0.223953 11.00000 0.03042 0.04471 = 0.02249 -0.00277 0.00134 -0.00352 S1 5 0.044430 0.183066 0.124895 11.00000 0.02222 0.02851 = 0.02432 -0.00073 -0.00221 0.00056 PART 1 O20A 4 -0.130130 0.207110 0.158506 21.00000 0.02720 0.02156 = 0.03309 0.00235 0.00327 -0.00217 O21A 4 0.078947 0.134833 0.158911 21.00000 0.04116 0.02059 = 0.03010 0.00011 0.00763 0.00641 O22A 4 -0.017698 0.176268 0.064550 21.00000 0.04476 0.04388 = 0.01388 -0.00223 -0.00588 0.00829 O23A 4 0.220571 0.214680 0.137295 21.00000 0.01304 0.03662 = 0.05219 0.00181 -0.00195 -0.01461 PART 2 O20B 4 -0.111658 0.206272 0.159868 -21.00000 0.01962 0.04738 = 0.01927 -0.00716 -0.00063 0.01045 O21B 4 0.197052 0.158804 0.166802 -21.00000 0.02300 0.03954 = 0.02306 0.00015 -0.00269 0.00681 O22B 4 -0.043356 0.145767 0.082543 -21.00000 0.02879 0.03888 = 0.02562 -0.00947 -0.00349 -0.00379 O23B 4 0.150564 0.220593 0.088735 -21.00000 0.02681 0.03954 = 0.04359 0.01195 0.00366 -0.00317 PART 0 H2W 2 0.634365 0.195163 0.199463 11.00000 0.03632 H1W 2 0.437527 0.191201 0.198239 11.00000 0.08102 HKLF 4 REM shelxa in P2(1)/n REM R1 = 0.0501 for 4731 Fo > 4sig(Fo) and 0.0830 for all 6889 data REM 586 parameters refined using 54 restraints END WGHT 0.0514 1.7812 REM Highest difference peak 0.245, deepest hole -0.397, 1-sigma level 0.054 Q1 1 0.0253 -0.0055 0.3009 11.00000 0.05 0.24 Q2 1 -0.0686 0.1177 0.8610 11.00000 0.05 0.23 Q3 1 -0.1548 -0.0056 0.8604 11.00000 0.05 0.23 Q4 1 0.3795 0.1835 0.1239 11.00000 0.05 0.22 Q5 1 0.5861 0.2034 0.5677 11.00000 0.05 0.22 Q6 1 -0.0777 0.1823 0.1652 11.00000 0.05 0.21 Q7 1 0.1924 0.3945 0.8994 11.00000 0.05 0.20 Q8 1 -0.1965 0.1918 0.5777 11.00000 0.05 0.20 Q9 1 0.0223 0.0809 0.3197 11.00000 0.05 0.20 Q10 1 -0.0331 0.2096 0.1427 11.00000 0.05 0.20 Q11 1 0.1570 0.0806 0.3419 11.00000 0.05 0.19 Q12 1 -0.1477 0.0570 0.8595 11.00000 0.05 0.18 Q13 1 -0.1427 0.0255 0.8990 11.00000 0.05 0.18 Q14 1 0.3121 0.1940 0.5179 11.00000 0.05 0.18 Q15 1 0.1089 0.2124 0.9007 11.00000 0.05 0.18 Q16 1 0.2136 0.0655 0.3745 11.00000 0.05 0.18 Q17 1 0.1664 0.5142 0.7986 11.00000 0.05 0.18 Q18 1 0.1137 0.1116 0.3020 11.00000 0.05 0.18 Q19 1 0.1753 0.1854 0.0794 11.00000 0.05 0.18 Q20 1 0.1601 0.3389 0.4155 11.00000 0.05 0.18 ;