# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_section_title ; Synthesis and Reactivity of Unexpected and Sensitive 3-Diazonio-5-nitrimino-1,2,4-triazole ; _publ_author_address ; Nordheider, Andreas Department Chemie Ludwig-Maximilians Univers Butenandtstrasse 5-13 (Hau D-81377 M\"unchen Bundesrepublik Deutschland Klap\"otke, Thomas M. Department Chemie Ludwig-Maximilians Universit\"at Butenandtstrasse 5-13 (Haus D) D-81377 M\"unchen Bundesrepublik Deutschland Stierstorfer, Joerg Department Chemie Ludwig-Maximilians Universit\"at Butenandtstrasse 5-13 (Haus D) D-81377 M\"unchen Bundesrepublik Deutschland ; _publ_contact_author_address ; Department Chemie Ludwig-Maximilians Universit\"at Butenandtstra\&se 5-13 (Haus D) D-81377 M\"unchen Bundesrepublik Deutschland ; _publ_contact_author_email tmk@cup.uni-muenchen.de _publ_contact_author_fax +49-89-2180-77491 _publ_contact_author_phone +49-89-2180-77492 #TrackingRef 'fx345_NaDATrCH2COO.cif' _publ_contact_author_name 'Nordheider, Andreas Thomas M. Klapotke Stierstorfer, Joerg' loop_ _publ_author_name J.Stierstorfer T.M.Klapotke A.Nordheider # Attachment 'fx345_NaDATrCH2COO.cif' data_fx345 _database_code_depnum_ccdc_archive 'CCDC 843029' _publ_section_abstract ? _publ_section_comment ? _audit_author_name 'Klap\"otke, Thomas M.' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date ; 'Tue Aug 17 13:23:17 2010' ; _audit_update_record 18.08.2010 _chemical_name_systematic 'Sodium 1-(Carboxylatomethyl-3,5-diaminotriazole dihydrate)' _chemical_compound_source ? _chemical_name_common 'Sodium 1-(Carboxylatomethyl-3,5-diaminotriazole dihydrate)' _chemical_formula_moiety 'C4 H10 N5 Na O4' _chemical_formula_sum 'C4 H10 N5 Na1 O4' _chemical_formula_weight 215.16 _diffrn_ambient_temperature 173 # in K _diffrn_source_type 'Spellman generator' _diffrn_source_power ? # in kW _diffrn_source_voltage 50 # kV _diffrn_source_current 40 # mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.5 _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method omega-scan _diffrn_radiation_type 'Mo K\a' _diffrn_detector_area_resol_mean 15.9809 _diffrn_reflns_number 2707 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.26 _diffrn_reflns_theta_max 23.99 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.963 _reflns_number_total 1325 _reflns_number_gt 881 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 -0.0694462731 _diffrn_orient_matrix_UB_12 0.0167630813 _diffrn_orient_matrix_UB_13 -0.0202150003 _diffrn_orient_matrix_UB_21 -0.0249491900 _diffrn_orient_matrix_UB_22 -0.0613290819 _diffrn_orient_matrix_UB_23 0.0383109452 _diffrn_orient_matrix_UB_31 -0.0064992407 _diffrn_orient_matrix_UB_32 0.0555214117 _diffrn_orient_matrix_UB_33 0.0484449806 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' 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' Na Na 0.0362 0.0249 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5655(9) _cell_length_b 8.3881(7) _cell_length_c 10.9272(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.718(8) _cell_angle_gamma 90.00 _cell_volume 876.36(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1031 _cell_measurement_theta_min 4.2482 _cell_measurement_theta_max 28.7246 _cell_special_details ? _exptl_crystal_description cone _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90811 _exptl_absorpt_correction_T_max 0.99000 _exptl_absorpt_process_details ;SCALE3 ABSPACK - An Oxford Diffraction program (1.0.4,gui:1.0.3) (C) 2005 Oxford Diffraction Ltd. ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_special_details ? _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_diff_density_max 0.177 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.042 _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid # Plot Program for Crystal Structure Illustrations, Oak Ridge National # Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. # Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), # Germany, 1995)' ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). # --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1325 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.801 _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 Na Na 0.08396(7) 0.45373(9) 0.35800(7) 0.0232(2) Uani 1 1 d . . . O1 O 0.17754(12) 0.23843(15) 0.24539(13) 0.0218(4) Uani 1 1 d . . . O2 O 0.14244(13) -0.02537(15) 0.23972(13) 0.0245(4) Uani 1 1 d . . . O3 O 0.17626(5) 0.64045(6) 0.22640(5) 0.0318(4) Uani 1 1 d . . . H31 H 0.1676 0.7476 0.2392 0.048 Uiso 1 1 d R . . H32 H 0.2092 0.6385 0.1502 0.048 Uiso 1 1 d R . . O4 O -0.01425(5) 0.69757(6) 0.46929(5) 0.0272(4) Uani 1 1 d R . . H41 H 0.0487 0.7520 0.4673 0.041 Uiso 1 1 d R . . H42 H -0.0609 0.7173 0.3974 0.041 Uiso 1 1 d R . . N1 N 0.35344(5) -0.07963(6) 0.41100(5) 0.0198(4) Uani 1 1 d R . . N2 N 0.27472(5) -0.18812(6) 0.47685(5) 0.0226(4) Uani 1 1 d R . . N3 N 0.46609(5) -0.30717(6) 0.39853(5) 0.0195(4) Uani 1 1 d R . . N4 N 0.56017(5) -0.08378(6) 0.29453(5) 0.0307(5) Uani 1 1 d R . . H4A H 0.5463 0.0038 0.2630 0.037 Uiso 1 1 d R . . H4B H 0.6387 -0.1321 0.2798 0.037 Uiso 1 1 d R . . N5 N 0.30235(5) -0.46595(6) 0.50827(5) 0.0239(4) Uani 1 1 d R . . H5A H 0.3649 -0.5373 0.5299 0.029 Uiso 1 1 d R . . H5B H 0.2426 -0.4637 0.5786 0.029 Uiso 1 1 d R . . C1 C 0.46358(5) -0.15339(6) 0.36389(5) 0.0202(5) Uani 1 1 d R . . C2 C 0.34799(5) -0.32063(6) 0.46461(5) 0.0205(5) Uani 1 1 d R . . C3 C 0.30321(5) 0.08159(6) 0.39059(5) 0.0226(5) Uani 1 1 d R . . H3A H 0.3843 0.1517 0.3759 0.027 Uiso 1 1 calc R . . H3B H 0.2585 0.1195 0.4658 0.027 Uiso 1 1 calc R . . C4 C 0.19836(19) 0.0975(2) 0.28264(19) 0.0186(5) 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 Na 0.0242(4) 0.0228(4) 0.0228(5) 0.0011(4) 0.0022(4) 0.0022(4) O1 0.0216(8) 0.0164(7) 0.0275(9) 0.0010(7) 0.0008(7) 0.0020(6) O2 0.0260(8) 0.0187(8) 0.0285(9) -0.0020(8) -0.0047(7) -0.0020(7) O3 0.0444(10) 0.0238(8) 0.0279(9) 0.0023(8) 0.0105(8) 0.0037(7) O4 0.0247(8) 0.0315(8) 0.0254(10) 0.0026(8) -0.0014(7) -0.0071(7) N1 0.0216(10) 0.0157(9) 0.0221(11) 0.0039(9) 0.0003(8) 0.0006(8) N2 0.0270(10) 0.0198(9) 0.0211(11) 0.0028(9) 0.0023(8) -0.0010(8) N3 0.0174(10) 0.0168(9) 0.0242(11) 0.0036(8) 0.0003(8) 0.0006(8) N4 0.0235(10) 0.0237(10) 0.0454(14) 0.0153(10) 0.0099(9) 0.0067(8) N5 0.0224(10) 0.0228(9) 0.0269(11) 0.0092(9) 0.0044(8) 0.0053(8) C1 0.0186(12) 0.0233(12) 0.0187(13) 0.0014(11) -0.0016(10) -0.0021(10) C2 0.0211(12) 0.0215(12) 0.0186(13) 0.0023(11) -0.0040(10) 0.0017(10) C3 0.0252(12) 0.0165(11) 0.0260(14) -0.0001(10) -0.0015(10) 0.0035(9) C4 0.0166(11) 0.0190(12) 0.0205(13) -0.0019(11) 0.0040(9) 0.0009(10) 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 Na O3 2.3188(9) . ? Na O1 2.3755(15) . ? Na O2 2.3921(14) 2 ? Na O4 2.5717 . ? Na H42 2.6510 . ? O1 C4 1.264(2) . ? O2 C4 1.247(2) . ? O3 H31 0.9137 . ? O3 H32 0.8986 . ? O4 H41 0.7564 . ? O4 H42 0.9070 . ? N1 C1 1.3380 . ? N1 N2 1.3948 . ? N1 C3 1.4501 . ? N2 C2 1.3229 . ? N3 C1 1.3443 . ? N3 C2 1.3636 . ? N4 C1 1.3457 . ? N4 H4A 0.8205 . ? N4 H4B 0.8725 . ? N5 C2 1.3844 . ? N5 H5A 0.8739 . ? N5 H5B 0.9716 . ? C3 C4 1.531(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? 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 O3 Na O1 92.06(5) . . ? O3 Na O2 91.72(4) . 2 ? O1 Na O2 100.06(5) . 2 ? O3 Na O4 84.68(3) . . ? O1 Na O4 176.64(5) . . ? O4 Na O4 86.2 3_566 . ? O2 Na O4 79.29(4) 2 . ? O4 Na N5 78.5 . 1_565 ? O3 Na H42 75.4 . . ? O1 Na H42 157.7 . . ? O4 Na H42 98.9 3_566 . ? O2 Na H42 62.7 2 . ? O4 Na H42 19.9 . . ? N5 Na H42 95.3 1_565 . ? Na Na H42 55.6 3_566 . ? C4 O1 Na 127.03(13) . . ? Na O3 H31 122.1 . . ? Na O3 H32 135.4 . . ? H31 O3 H32 101.3 . . ? Na O4 H41 99.4 . . ? Na O4 H42 129.8 3_566 . ? Na O4 H42 85.0 . . ? H41 O4 H42 103.7 . . ? C1 N1 N2 109.9 . . ? C1 N1 C3 129.3 . . ? N2 N1 C3 120.4 . . ? C2 N2 N1 101.5 . . ? C1 N3 C2 102.7 . . ? C1 N4 H4A 121.3 . . ? C1 N4 H4B 120.8 . . ? H4A N4 H4B 117.9 . . ? C2 N5 H5A 118.4 . . ? C2 N5 H5B 117.0 . . ? Na N5 H5B 91.3 1_545 . ? H5A N5 H5B 102.4 . . ? N1 C1 N3 110.1 . . ? N1 C1 N4 125.3 . . ? N3 C1 N4 124.6 . . ? N2 C2 N3 115.7 . . ? N2 C2 N5 122.1 . . ? N3 C2 N5 122.0 . . ? N1 C3 C4 113.97(7) . . ? N1 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N1 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? O2 C4 O1 126.19(18) . . ? O2 C4 C3 118.78(15) . . ? O1 C4 C3 115.03(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Na O1 C4 160.19(14) . . . . ? O4 Na O1 C4 -9.28(15) 3_566 . . . ? O2 Na O1 C4 -107.69(15) 2 . . . ? N5 Na O1 C4 75.23(14) 1_565 . . . ? Na Na O1 C4 -9.49(18) 3_566 . . . ? O3 Na O4 Na -169.40(3) . . . 3_566 ? O4 Na O4 Na 0.0 3_566 . . 3_566 ? O2 Na O4 Na 97.83(4) 2 . . 3_566 ? N5 Na O4 Na -83.80(3) 1_565 . . 3_566 ? C1 N1 N2 C2 1.0 . . . . ? C3 N1 N2 C2 174.3 . . . . ? N2 N1 C1 N3 -2.2 . . . . ? C3 N1 C1 N3 -174.7 . . . . ? N2 N1 C1 N4 179.4 . . . . ? C3 N1 C1 N4 6.9 . . . . ? C2 N3 C1 N1 2.3 . . . . ? C2 N3 C1 N4 -179.3 . . . . ? N1 N2 C2 N3 0.6 . . . . ? N1 N2 C2 N5 -174.8 . . . . ? C1 N3 C2 N2 -1.8 . . . . ? C1 N3 C2 N5 173.6 . . . . ? Na N5 C2 N2 70.9 1_545 . . . ? Na N5 C2 N3 -104.2 1_545 . . . ? C1 N1 C3 C4 89.35(8) . . . . ? N2 N1 C3 C4 -82.52(8) . . . . ? Na O2 C4 O1 -29.4(3) 2_545 . . . ? Na O2 C4 C3 150.80(10) 2_545 . . . ? Na O1 C4 O2 118.1(2) . . . . ? Na O1 C4 C3 -62.04(19) . . . . ? N1 C3 C4 O2 15.3(2) . . . . ? N1 C3 C4 O1 -164.54(12) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 O3 H31 O2 0.91 1.92 2.8260(14) 171.3 1_565 O3 H32 N2 0.90 2.06 2.939 167.0 4_565 O4 H41 N2 0.76 2.22 2.925 155.6 1_565 O4 H42 O1 0.91 1.90 2.8001(14) 172.0 2 O4 H42 O2 0.91 2.63 3.1699(14) 118.8 2 N4 H4A N3 0.82 2.37 3.141 156.1 2_655 N4 H4B O1 0.87 2.09 2.9622(13) 175.4 2_645 N5 H5A N3 0.87 2.20 3.071 172.4 3_646 N5 H5B O2 0.97 2.03 2.9956(16) 171.3 4_556 _geom_special_details ? _iucr_refine_instructions_details ; TITL v1 in P2(1)/c CELL 0.71073 9.5655 8.3881 10.9272 90.000 91.718 90.000 ZERR 1.00 0.0009 0.0007 0.0011 0.000 0.008 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N NA O UNIT 16 40 20 4 16 MERG 2 OMIT -2.00 48.00 OMIT 1 3 0 OMIT 3 0 0 OMIT -3 1 2 OMIT 0 0 4 OMIT 6 2 10 OMIT 2 3 2 OMIT -3 2 2 OMIT 2 3 0 OMIT 1 4 3 OMIT -4 1 1 OMIT 1 3 2 OMIT -1 2 1 OMIT 10 1 7 OMIT 2 2 2 OMIT -4 3 1 OMIT -3 3 1 OMIT 4 6 0 OMIT 11 4 1 OMIT -3 8 7 OMIT -1 2 3 OMIT 3 10 0 OMIT -3 4 1 OMIT 3 2 2 OMIT 4 3 0 OMIT 2 3 1 OMIT 2 7 2 OMIT -1 3 1 OMIT 1 0 4 OMIT -2 7 4 OMIT -2 0 4 OMIT 4 1 5 OMIT 3 7 0 OMIT -5 6 4 OMIT -5 1 11 OMIT 2 2 1 OMIT 8 6 2 OMIT -4 0 4 OMIT 5 7 1 OMIT -4 1 5 OMIT 0 2 0 OMIT -7 2 7 OMIT -1 6 6 OMIT -5 1 8 OMIT 1 2 3 OMIT -3 1 6 OMIT -5 4 3 OMIT 4 7 2 OMIT -8 1 4 OMIT -6 8 5 OMIT -4 3 2 EQIV $1 x, y+1, z EQIV $2 x, -y+1/2, z-1/2 EQIV $3 -x, y+1/2, -z+1/2 EQIV $4 -x+1, y+1/2, -z+1/2 EQIV $5 -x+1, y-1/2, -z+1/2 EQIV $6 -x+1, -y-1, -z+1 EQIV $7 x, -y-1/2, z+1/2 HTAB O3 O2_$1 HTAB O3 N2_$2 HTAB O4 N2_$1 HTAB O4 O1_$3 HTAB O4 O2_$3 HTAB N4 N3_$4 HTAB N4 O1_$5 HTAB N5 N3_$6 HTAB N5 O2_$7 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 5 TEMP -100.00 WGHT 0.017600 FVAR 0.17690 NA 4 0.083961 0.453728 0.358003 11.00000 0.02424 0.02282 = 0.02277 0.00106 0.00217 0.00216 O1 5 0.177543 0.238427 0.245393 11.00000 0.02163 0.01638 = 0.02745 0.00100 0.00081 0.00197 O2 5 0.142438 -0.025366 0.239717 11.00000 0.02602 0.01867 = 0.02845 -0.00200 -0.00467 -0.00200 O3 5 0.176262 0.640454 0.226396 11.00000 0.04443 0.02376 = 0.02787 0.00227 0.01049 0.00367 AFIX 3 H31 2 0.167562 0.747602 0.239156 11.00000 -1.50000 H32 2 0.209152 0.638474 0.150236 11.00000 -1.50000 O4 5 -0.014251 0.697574 0.469286 11.00000 0.02473 0.03150 = 0.02539 0.00264 -0.00139 -0.00711 H41 2 0.048709 0.751961 0.467275 11.00000 -1.50000 H42 2 -0.060871 0.717292 0.397375 11.00000 -1.50000 N1 3 0.353440 -0.079627 0.410998 11.00000 0.02160 0.01570 = 0.02213 0.00390 0.00027 0.00059 N2 3 0.274716 -0.188123 0.476849 11.00000 0.02699 0.01979 = 0.02112 0.00275 0.00233 -0.00102 N3 3 0.466093 -0.307173 0.398528 11.00000 0.01738 0.01679 = 0.02422 0.00358 0.00026 0.00060 N4 3 0.560173 -0.083782 0.294530 11.00000 0.02347 0.02368 = 0.04544 0.01528 0.00985 0.00666 H4A 2 0.546272 0.003778 0.262989 11.00000 -1.20000 H4B 2 0.638683 -0.132072 0.279799 11.00000 -1.20000 N5 3 0.302352 -0.465945 0.508267 11.00000 0.02240 0.02277 = 0.02689 0.00924 0.00437 0.00528 H5A 2 0.364942 -0.537255 0.529907 11.00000 -1.20000 H5B 2 0.242562 -0.463655 0.578578 11.00000 -1.20000 C1 1 0.463584 -0.153390 0.363893 11.00000 0.01864 0.02326 = 0.01866 0.00135 -0.00159 -0.00212 C2 1 0.347989 -0.320625 0.464613 11.00000 0.02115 0.02148 = 0.01860 0.00231 -0.00397 0.00173 C3 1 0.303215 0.081586 0.390592 11.00000 0.02521 0.01653 = 0.02596 -0.00007 -0.00154 0.00346 AFIX 23 H3A 2 0.384258 0.151721 0.375950 11.00000 -1.20000 H3B 2 0.258470 0.119513 0.465758 11.00000 -1.20000 AFIX 0 C4 1 0.198359 0.097540 0.282638 11.00000 0.01658 0.01900 = 0.02049 -0.00189 0.00400 0.00094 HKLF 4 REM v1 in P2(1)/c REM R1 = 0.0313 for 881 Fo > 4sig(Fo) and 0.0547 for all 1325 data REM 100 parameters refined using 0 restraints END WGHT 0.0176 0.0000 REM Highest difference peak 0.177, deepest hole -0.175, 1-sigma level 0.042 Q1 1 0.3278 -0.0061 0.3938 11.00000 0.05 0.18 Q2 1 0.4559 -0.3172 0.4809 11.00000 0.05 0.15 Q3 1 0.1345 -0.4474 0.6148 11.00000 0.05 0.14 Q4 1 0.5381 -0.3265 0.3905 11.00000 0.05 0.14 Q5 1 -0.1971 0.6525 0.3738 11.00000 0.05 0.14 Q6 1 0.4016 -0.2258 0.5083 11.00000 0.05 0.14 Q7 1 0.4429 -0.0789 0.4250 11.00000 0.05 0.14 Q8 1 0.0147 0.3623 0.3305 11.00000 0.05 0.13 Q9 1 0.1219 0.0510 0.3007 11.00000 0.05 0.13 Q10 1 0.3809 -0.1108 0.5820 11.00000 0.05 0.13 Q11 1 -0.0034 0.9676 0.5166 11.00000 0.05 0.13 Q12 1 0.3744 -0.1259 0.3373 11.00000 0.05 0.13 Q13 1 0.5310 -0.1267 0.3632 11.00000 0.05 0.13 Q14 1 0.3437 0.5893 0.1440 11.00000 0.05 0.12 Q15 1 0.2404 -0.2676 0.4286 11.00000 0.05 0.12 Q16 1 0.3413 0.1333 0.5026 11.00000 0.05 0.12 Q17 1 0.5420 -0.0222 0.2845 11.00000 0.05 0.12 Q18 1 0.3249 0.2188 0.4190 11.00000 0.05 0.12 Q19 1 0.0191 0.6208 0.5580 11.00000 0.05 0.12 Q20 1 0.1408 0.5213 0.4485 11.00000 0.05 0.12 ; # Attachment 'fx361_TrN2+NNO2.cif' data_fx361 _database_code_depnum_ccdc_archive 'CCDC 843030' _publ_section_abstract ? _publ_section_comment ? _audit_author_name 'Joerg Stierstorfer' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date ; 'Tue Aug 24 20:43:19 2010' ; _audit_update_record 25.08.2010 _chemical_name_systematic ? _chemical_compound_source ? _chemical_name_common ? _chemical_formula_moiety 'C4 H3 N7 O4, 2(H2 O) ' _chemical_formula_sum 'C4 H7 N7 O6' _chemical_formula_weight 249.17 _diffrn_ambient_temperature 173 # in K _diffrn_source_type 'Spellman generator' _diffrn_source_power ? # in kW _diffrn_source_voltage 50 # kV _diffrn_source_current 40 # mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.5 _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method omega-scan _diffrn_radiation_type 'Mo K\a' _diffrn_detector_area_resol_mean 15.9809 _diffrn_reflns_number 3351 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 25.99 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.985 _reflns_number_total 1923 _reflns_number_gt 1195 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 -0.0508932443 _diffrn_orient_matrix_UB_12 -0.0653281553 _diffrn_orient_matrix_UB_13 -0.0449051432 _diffrn_orient_matrix_UB_21 -0.1127906571 _diffrn_orient_matrix_UB_22 0.0093858458 _diffrn_orient_matrix_UB_23 0.0152097198 _diffrn_orient_matrix_UB_31 0.0054813796 _diffrn_orient_matrix_UB_32 0.0449154429 _diffrn_orient_matrix_UB_33 -0.0586201393 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' 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' O O 0.0106 0.0060 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9153(5) _cell_length_b 9.1960(8) _cell_length_c 9.4344(8) _cell_angle_alpha 93.949(7) _cell_angle_beta 90.503(7) _cell_angle_gamma 104.609(7) _cell_volume 495.25(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1295 _cell_measurement_theta_min 4.2142 _cell_measurement_theta_max 28.6832 _cell_special_details ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 256 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9408 _exptl_absorpt_correction_T_max 0.9847 _exptl_absorpt_process_details ;SCALE3 ABSPACK - An Oxford Diffraction program (1.0.4,gui:1.0.3) (C) 2005 Oxford Diffraction Ltd. ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_special_details ? _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_diff_density_max 0.211 _refine_diff_density_min -0.168 _refine_diff_density_rms 0.039 _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid # Plot Program for Crystal Structure Illustrations, Oak Ridge National # Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. # Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), # Germany, 1995)' ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). # --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1923 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0556 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 0.802 _refine_ls_restrained_S_all 0.802 _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 O5 O 0.5509(2) 0.49180(18) -0.25982(15) 0.0349(3) Uani 1 1 d . . . O6 O -0.2572(3) 0.71619(17) 0.58485(17) 0.0484(4) Uani 1 1 d . . . N6 N 0.8256(2) 1.31866(17) 0.23297(14) 0.0271(3) Uani 1 1 d . . . N7 N 0.8805(2) 1.44080(18) 0.23202(16) 0.0372(4) Uani 1 1 d . . . H3B H 0.993(3) 0.8468(16) 0.1202(15) 0.020(4) Uiso 1 1 d . . . H3A H 0.826(3) 0.7458(19) 0.2196(17) 0.034(5) Uiso 1 1 d . . . H6A H -0.304(3) 0.792(2) 0.596(2) 0.039(6) Uiso 1 1 d . . . H5A H 0.606(4) 0.555(3) -0.326(2) 0.069(8) Uiso 1 1 d . . . H5B H 0.561(4) 0.410(3) -0.285(3) 0.076(9) Uiso 1 1 d . . . H6B H -0.144(4) 0.734(3) 0.530(3) 0.081(9) Uiso 1 1 d . . . H4A H 0.682(3) 0.566(2) -0.109(2) 0.072(7) Uiso 1 1 d . . . N4 N 0.4430(2) 0.81699(15) 0.32002(14) 0.0266(3) Uani 1 1 d . . . O4 O 0.76674(19) 0.61673(13) -0.02973(13) 0.0312(3) Uani 1 1 d . . . N1 N 0.7643(2) 0.94361(14) 0.20013(13) 0.0228(3) Uani 1 1 d . . . C1 C 0.5746(3) 0.95055(18) 0.27957(17) 0.0230(4) Uani 1 1 d . . . N2 N 0.8846(2) 1.08266(15) 0.16906(14) 0.0256(3) Uani 1 1 d . . . N5 N 0.2524(2) 0.82054(16) 0.39232(14) 0.0285(3) Uani 1 1 d . . . O2 O 0.18013(19) 0.93426(14) 0.41672(13) 0.0355(3) Uani 1 1 d . . . N3 N 0.5665(2) 1.09468(15) 0.30407(14) 0.0251(3) Uani 1 1 d . . . O1 O 0.14389(19) 0.69535(13) 0.43421(13) 0.0388(3) Uani 1 1 d . . . O3 O 0.5145(2) 0.76206(13) -0.01873(12) 0.0355(3) Uani 1 1 d . . . C4 C 0.6862(3) 0.72860(18) 0.02256(17) 0.0253(4) Uani 1 1 d . . . C2 C 0.7568(3) 1.16178(18) 0.23513(17) 0.0232(4) Uani 1 1 d . . . C3 C 0.8373(3) 0.8123(2) 0.1472(2) 0.0249(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 O5 0.0440(8) 0.0239(8) 0.0358(8) -0.0030(7) 0.0089(6) 0.0078(6) O6 0.0514(10) 0.0354(9) 0.0648(11) 0.0131(8) 0.0254(8) 0.0198(8) N6 0.0250(8) 0.0251(9) 0.0305(9) -0.0002(7) 0.0013(7) 0.0056(7) N7 0.0337(9) 0.0304(10) 0.0471(11) 0.0004(8) 0.0010(8) 0.0077(7) N4 0.0288(8) 0.0232(8) 0.0268(8) 0.0014(7) 0.0107(7) 0.0049(6) O4 0.0359(7) 0.0243(7) 0.0337(8) -0.0068(6) 0.0033(6) 0.0104(6) N1 0.0249(7) 0.0191(8) 0.0247(8) 0.0006(7) 0.0032(6) 0.0065(6) C1 0.0260(9) 0.0243(10) 0.0181(9) -0.0002(8) -0.0019(7) 0.0057(7) N2 0.0259(8) 0.0211(8) 0.0287(8) 0.0009(7) 0.0025(6) 0.0040(6) N5 0.0302(8) 0.0278(9) 0.0251(8) -0.0015(7) 0.0017(7) 0.0037(7) O2 0.0367(7) 0.0311(8) 0.0419(8) 0.0009(6) 0.0102(6) 0.0148(6) N3 0.0306(8) 0.0211(8) 0.0234(8) -0.0013(6) 0.0016(6) 0.0069(6) O1 0.0403(7) 0.0251(7) 0.0454(8) 0.0018(6) 0.0163(6) -0.0028(6) O3 0.0389(7) 0.0367(8) 0.0336(7) -0.0056(6) -0.0071(6) 0.0171(6) C4 0.0304(10) 0.0215(10) 0.0235(10) 0.0042(8) 0.0082(8) 0.0046(8) C2 0.0266(9) 0.0170(9) 0.0252(10) -0.0004(8) -0.0019(8) 0.0049(7) C3 0.0241(10) 0.0217(10) 0.0296(11) 0.0008(8) 0.0035(8) 0.0075(8) 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 O5 H5A 0.89(2) . ? O5 H5B 0.79(3) . ? O6 H6A 0.814(19) . ? O6 H6B 0.84(3) . ? N6 N7 1.0884(17) . ? N6 C2 1.398(2) . ? N4 N5 1.3293(18) . ? N4 C1 1.359(2) . ? O4 C4 1.3077(19) . ? O4 H4A 0.92(2) . ? N1 N2 1.3504(17) . ? N1 C1 1.367(2) . ? N1 C3 1.441(2) . ? C1 N3 1.342(2) . ? N2 C2 1.309(2) . ? N5 O2 1.2342(17) . ? N5 O1 1.2600(16) . ? N3 C2 1.3372(19) . ? O3 C4 1.2024(17) . ? C4 C3 1.512(2) . ? C3 H3B 0.941(14) . ? C3 H3A 0.939(16) . ? 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 H5A O5 H5B 110(2) . . ? H6A O6 H6B 108(2) . . ? N7 N6 C2 179.48(17) . . ? N5 N4 C1 116.99(14) . . ? C4 O4 H4A 112.9(13) . . ? N2 N1 C1 110.89(13) . . ? N2 N1 C3 120.55(14) . . ? C1 N1 C3 128.53(14) . . ? N3 C1 N4 134.14(16) . . ? N3 C1 N1 109.75(14) . . ? N4 C1 N1 116.06(15) . . ? C2 N2 N1 99.01(13) . . ? O2 N5 O1 121.01(15) . . ? O2 N5 N4 124.49(14) . . ? O1 N5 N4 114.49(14) . . ? C2 N3 C1 99.36(13) . . ? O3 C4 O4 126.21(16) . . ? O3 C4 C3 123.08(15) . . ? O4 C4 C3 110.70(15) . . ? N2 C2 N3 120.97(14) . . ? N2 C2 N6 118.24(14) . . ? N3 C2 N6 120.79(14) . . ? N1 C3 C4 112.08(14) . . ? N1 C3 H3B 106.5(9) . . ? C4 C3 H3B 110.5(9) . . ? N1 C3 H3A 109.3(10) . . ? C4 C3 H3A 107.7(10) . . ? H3B C3 H3A 110.8(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 N4 C1 N3 5.4(3) . . . . ? N5 N4 C1 N1 -177.30(12) . . . . ? N2 N1 C1 N3 -0.63(17) . . . . ? C3 N1 C1 N3 -178.64(14) . . . . ? N2 N1 C1 N4 -178.54(12) . . . . ? C3 N1 C1 N4 3.5(2) . . . . ? C1 N1 N2 C2 0.88(16) . . . . ? C3 N1 N2 C2 179.07(13) . . . . ? C1 N4 N5 O2 4.9(2) . . . . ? C1 N4 N5 O1 -176.18(13) . . . . ? N4 C1 N3 C2 177.43(17) . . . . ? N1 C1 N3 C2 0.05(15) . . . . ? N1 N2 C2 N3 -0.95(18) . . . . ? N1 N2 C2 N6 178.43(12) . . . . ? C1 N3 C2 N2 0.60(19) . . . . ? C1 N3 C2 N6 -178.76(14) . . . . ? N2 N1 C3 C4 -103.00(17) . . . . ? C1 N1 C3 C4 74.8(2) . . . . ? O3 C4 C3 N1 -5.7(2) . . . . ? O4 C4 C3 N1 175.32(14) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 O6 H6A N3 0.814(19) 2.255(19) 2.977(2) 147.9(17) 2_576 O6 H6A O2 0.814(19) 2.450(19) 3.1318(19) 142.0(16) 2_576 O5 H5A O6 0.89(2) 1.78(2) 2.638(2) 164(2) 1_654 O5 H5B N4 0.79(3) 2.08(3) 2.867(2) 170(2) 2_665 O5 H5B O1 0.79(3) 2.58(2) 3.1870(19) 134(2) 2_665 O6 H6B O1 0.84(3) 2.03(3) 2.817(2) 155(2) . O6 H6B O2 0.84(3) 2.59(3) 3.335(2) 148(2) . O6 H6B N5 0.84(3) 2.66(3) 3.490(2) 170(2) . O4 H4A O5 0.92(2) 1.64(2) 2.5553(18) 173(2) . _geom_special_details ? _iucr_refine_instructions_details ; TITL fx361 in P-1 CELL 0.71073 5.9153 9.1960 9.4344 93.949 90.503 104.609 ZERR 2.00 0.0005 0.0008 0.0008 0.007 0.007 0.007 LATT 1 SFAC C H O N UNIT 8 14 12 14 MERG 2 OMIT -2.00 52.00 OMIT 1 0 1 OMIT 0 3 1 OMIT 1 -2 2 OMIT -1 1 2 OMIT -3 9 2 OMIT 0 2 1 OMIT -1 2 9 OMIT 5 4 5 OMIT -2 -7 4 OMIT -2 1 2 OMIT -2 7 3 OMIT 1 8 5 OMIT 0 0 2 OMIT -3 0 2 OMIT 5 -1 5 OMIT 2 -2 1 OMIT 6 -1 6 OMIT -2 4 0 OMIT -2 5 0 OMIT 1 -3 2 OMIT -3 9 0 EQIV $1 -x, -y+2, -z+1 EQIV $2 x+1, y, z-1 EQIV $3 -x+1, -y+1, -z HTAB O6 N3_$1 HTAB O6 O2_$1 HTAB O5 O6_$2 HTAB O5 N4_$3 HTAB O5 O1_$3 HTAB O6 O1 HTAB O6 O2 HTAB O6 N5 HTAB O4 O5 FMAP 2 PLAN 20 ACTA BOND $H SIZE 0.40 0.11 0.10 CONF L.S. 4 TEMP -100.00 WGHT 0.020300 FVAR 8.68859 O5 3 0.550936 0.491802 -0.259815 11.00000 0.04404 0.02387 = 0.03580 -0.00299 0.00886 0.00778 O6 3 -0.257162 0.716188 0.584853 11.00000 0.05145 0.03540 = 0.06479 0.01306 0.02545 0.01980 N6 4 0.825648 1.318662 0.232967 11.00000 0.02495 0.02511 = 0.03048 -0.00024 0.00131 0.00561 N7 4 0.880461 1.440805 0.232019 11.00000 0.03369 0.03043 = 0.04707 0.00035 0.00096 0.00774 H3B 2 0.993269 0.846751 0.120221 11.00000 0.01982 H3A 2 0.825873 0.745779 0.219582 11.00000 0.03351 H6A 2 -0.304089 0.792006 0.596247 11.00000 0.03930 H5A 2 0.605528 0.554623 -0.325834 11.00000 0.06916 H5B 2 0.560703 0.409992 -0.285363 11.00000 0.07589 H6B 2 -0.144086 0.734005 0.529836 11.00000 0.08124 H4A 2 0.682365 0.566021 -0.108909 11.00000 0.07249 MOLE 1 N4 4 0.442996 0.816986 0.320022 11.00000 0.02883 0.02319 = 0.02684 0.00141 0.01069 0.00487 O4 3 0.766735 0.616735 -0.029734 11.00000 0.03587 0.02432 = 0.03375 -0.00681 0.00326 0.01036 N1 4 0.764278 0.943608 0.200125 11.00000 0.02488 0.01905 = 0.02473 0.00057 0.00318 0.00647 C1 1 0.574552 0.950550 0.279569 11.00000 0.02598 0.02428 = 0.01810 -0.00020 -0.00193 0.00573 N2 4 0.884577 1.082662 0.169061 11.00000 0.02590 0.02115 = 0.02868 0.00088 0.00254 0.00402 N5 4 0.252353 0.820538 0.392325 11.00000 0.03023 0.02778 = 0.02515 -0.00154 0.00172 0.00368 O2 3 0.180130 0.934264 0.416718 11.00000 0.03667 0.03108 = 0.04194 0.00090 0.01020 0.01483 N3 4 0.566510 1.094680 0.304074 11.00000 0.03057 0.02108 = 0.02335 -0.00129 0.00158 0.00686 O1 3 0.143887 0.695349 0.434213 11.00000 0.04029 0.02506 = 0.04535 0.00181 0.01629 -0.00282 O3 3 0.514453 0.762060 -0.018730 11.00000 0.03893 0.03671 = 0.03359 -0.00558 -0.00705 0.01709 C4 1 0.686190 0.728599 0.022560 11.00000 0.03039 0.02153 = 0.02345 0.00420 0.00821 0.00460 C2 1 0.756760 1.161779 0.235132 11.00000 0.02658 0.01698 = 0.02525 -0.00042 -0.00191 0.00490 C3 1 0.837263 0.812323 0.147235 11.00000 0.02408 0.02172 = 0.02959 0.00081 0.00347 0.00749 HKLF 4 REM fx361 in P-1 REM R1 = 0.0322 for 1195 Fo > 4sig(Fo) and 0.0625 for all 1923 data REM 182 parameters refined using 0 restraints END WGHT 0.0203 0.0000 REM Highest difference peak 0.211, deepest hole -0.168, 1-sigma level 0.039 Q1 1 0.4786 0.7363 0.2867 11.00000 0.05 0.21 Q2 1 0.7772 0.8795 0.1654 11.00000 0.05 0.17 Q3 1 0.4969 0.8618 0.2930 11.00000 0.05 0.16 Q4 1 0.4771 1.1368 0.3650 11.00000 0.05 0.16 Q5 1 1.1074 0.9980 0.1703 11.00000 0.05 0.15 Q6 1 -0.0588 0.8112 0.6760 11.00000 0.05 0.15 Q7 1 0.4960 0.3870 -0.2994 11.00000 0.05 0.14 Q8 1 0.5456 1.2538 0.3382 11.00000 0.05 0.14 Q9 1 0.3422 0.8123 0.3175 11.00000 0.05 0.13 Q10 1 0.8870 0.7229 0.2998 11.00000 0.05 0.13 Q11 1 0.4332 0.7783 0.0876 11.00000 0.05 0.12 Q12 1 0.2675 0.6479 0.4524 11.00000 0.05 0.12 Q13 1 0.6670 0.8008 -0.0548 11.00000 0.05 0.12 Q14 1 0.0128 0.8576 0.3499 11.00000 0.05 0.12 Q15 1 0.3451 0.4119 -0.3199 11.00000 0.05 0.12 Q16 1 -0.0230 0.6143 0.3418 11.00000 0.05 0.11 Q17 1 0.1921 0.8789 0.2833 11.00000 0.05 0.11 Q18 1 0.7029 0.7464 0.1045 11.00000 0.05 0.11 Q19 1 -0.2605 0.7514 0.4875 11.00000 0.05 0.11 Q20 1 0.0895 0.9749 0.3043 11.00000 0.05 0.11 ; # Attachment 'fx441_NNO2_N3_CH2COOH_Trz.cif' data_fx441 _database_code_depnum_ccdc_archive 'CCDC 843031' _publ_section_abstract ? _publ_section_comment ? _audit_author_name 'Joerg Stierstorfer' _audit_block_code ? _audit_creation_method SHELXL-97 _audit_creation_date ; 'Wed Sep 29 23:52:48 2010' ; _audit_update_record 30.9.2010 _chemical_name_systematic 'to be inserted' _chemical_compound_source ? _chemical_name_common 'to be inserted' _chemical_formula_moiety 'C4 H4 N8 O4' _chemical_formula_sum 'C4 H4 N8 O4' _chemical_formula_weight 228.15 _diffrn_ambient_temperature 173 # in K _diffrn_source_type 'Spellman generator' _diffrn_source_power ? # in kW _diffrn_source_voltage 50 # kV _diffrn_source_current 40 # mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation 0.5 _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method omega-scan _diffrn_radiation_type 'Mo K\a' _diffrn_detector_area_resol_mean 15.9809 _diffrn_reflns_number 4250 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 25.98 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 1677 _reflns_number_gt 1124 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 -0.0320430045 _diffrn_orient_matrix_UB_12 -0.0126760475 _diffrn_orient_matrix_UB_13 -0.0552976719 _diffrn_orient_matrix_UB_21 -0.0614808033 _diffrn_orient_matrix_UB_22 0.0170774204 _diffrn_orient_matrix_UB_23 0.0174695740 _diffrn_orient_matrix_UB_31 0.0063436865 _diffrn_orient_matrix_UB_32 0.1009839870 _diffrn_orient_matrix_UB_33 -0.0099073426 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc ' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3123(7) _cell_length_b 6.8821(5) _cell_length_c 12.2305(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.873(7) _cell_angle_gamma 90.00 _cell_volume 857.61(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1516 _cell_measurement_theta_min 4.1715 _cell_measurement_theta_max 33.7518 _cell_special_details ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9561 _exptl_absorpt_correction_T_max 0.9800 _exptl_absorpt_process_details ;SCALE3 ABSPACK - An Oxford Diffraction program (1.0.4,gui:1.0.3) (C) 2005 Oxford Diffraction Ltd. ; _exptl_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? _diffrn_special_details ? _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_diff_density_max 0.170 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.039 _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET) (compiled Apr 1 2005,17:53:34) ; _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; 'ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid # Plot Program for Crystal Structure Illustrations, Oak Ridge National # Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. # Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), # Germany, 1995)' ; _computing_publication_material ;PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). # --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1677 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.001 _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 H3B H 0.0123(14) 0.360(2) 0.2396(13) 0.020(4) Uiso 1 1 d . . . H3A H 0.0359(15) 0.500(2) 0.1356(12) 0.026(4) Uiso 1 1 d . . . H31 H -0.082(2) 0.094(4) -0.0458(19) 0.087(8) Uiso 1 1 d . . . H3 H -0.431(2) 0.466(3) 0.1637(16) 0.058(7) Uiso 1 1 d . . . O4 O 0.07571(10) 0.09568(17) 0.11824(8) 0.0310(3) Uani 1 1 d . . . N1 N -0.15054(12) 0.46839(19) 0.14780(10) 0.0233(3) Uani 1 1 d . . . O3 O -0.08938(11) 0.22019(18) -0.00267(9) 0.0336(3) Uani 1 1 d . . . N4 N -0.22859(13) 0.2104(2) 0.24003(11) 0.0318(4) Uani 1 1 d . . . N2 N -0.18951(12) 0.6352(2) 0.08849(10) 0.0272(3) Uani 1 1 d . . . C4 C -0.00707(15) 0.2223(2) 0.08856(13) 0.0228(4) Uani 1 1 d . . . O1 O -0.44766(12) 0.1907(2) 0.24351(11) 0.0476(4) Uani 1 1 d . . . N3 N -0.35726(15) 0.4874(2) 0.14679(11) 0.0337(4) Uani 1 1 d . . . C3 C -0.01679(15) 0.3968(3) 0.16073(14) 0.0253(4) Uani 1 1 d . . . C1 C -0.25108(15) 0.3769(2) 0.18289(12) 0.0256(4) Uani 1 1 d . . . N7 N -0.36077(14) 0.8924(2) -0.02020(13) 0.0386(4) Uani 1 1 d . . . N6 N -0.40658(14) 0.7740(3) 0.04177(13) 0.0474(5) Uani 1 1 d . . . N5 N -0.33473(15) 0.1250(2) 0.27113(12) 0.0397(4) Uani 1 1 d . . . O2 O -0.31430(15) -0.0226(2) 0.32872(11) 0.0598(4) Uani 1 1 d . . . C2 C -0.31519(16) 0.6396(3) 0.09073(13) 0.0322(4) Uani 1 1 d . . . N8 N -0.33677(16) 1.0073(3) -0.07854(15) 0.0537(5) 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 O4 0.0341(7) 0.0304(7) 0.0282(6) 0.0004(5) 0.0038(5) 0.0110(6) N1 0.0221(7) 0.0235(7) 0.0246(7) -0.0006(6) 0.0048(6) 0.0028(6) O3 0.0324(7) 0.0385(8) 0.0279(6) -0.0073(6) -0.0019(5) 0.0086(6) N4 0.0307(8) 0.0337(9) 0.0323(8) 0.0065(7) 0.0089(6) -0.0031(7) N2 0.0283(8) 0.0270(8) 0.0271(7) 0.0031(6) 0.0066(6) 0.0074(6) C4 0.0201(8) 0.0252(9) 0.0241(9) 0.0036(7) 0.0070(7) -0.0006(8) O1 0.0314(7) 0.0630(10) 0.0504(8) 0.0035(7) 0.0126(6) -0.0105(7) N3 0.0235(8) 0.0467(10) 0.0334(8) 0.0085(7) 0.0122(7) 0.0086(8) C3 0.0201(9) 0.0263(10) 0.0292(10) 0.0011(8) 0.0032(7) 0.0015(8) C1 0.0230(8) 0.0325(10) 0.0220(8) -0.0031(8) 0.0060(7) 0.0020(8) N7 0.0257(8) 0.0443(10) 0.0459(10) 0.0099(9) 0.0057(7) 0.0153(8) N6 0.0340(9) 0.0597(11) 0.0526(10) 0.0279(9) 0.0198(8) 0.0210(8) N5 0.0416(10) 0.0477(11) 0.0306(8) 0.0014(8) 0.0077(7) -0.0106(9) O2 0.0718(10) 0.0533(10) 0.0536(9) 0.0257(8) 0.0075(7) -0.0166(8) C2 0.0289(9) 0.0407(11) 0.0289(9) 0.0076(8) 0.0099(7) 0.0114(9) N8 0.0333(9) 0.0555(12) 0.0721(12) 0.0248(11) 0.0078(9) 0.0096(8) 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 O4 C4 1.2346(18) . ? N1 C1 1.3390(19) . ? N1 N2 1.3842(17) . ? N1 C3 1.4502(19) . ? O3 C4 1.2937(18) . ? O3 H31 1.02(2) . ? N4 C1 1.343(2) . ? N4 N5 1.3478(19) . ? N2 C2 1.301(2) . ? C4 C3 1.503(2) . ? O1 N5 1.2463(18) . ? N3 C1 1.350(2) . ? N3 C2 1.359(2) . ? N3 H3 0.84(2) . ? C3 H3B 0.998(15) . ? C3 H3A 0.973(16) . ? N7 N8 1.118(2) . ? N7 N6 1.254(2) . ? N6 C2 1.388(2) . ? N5 O2 1.2356(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 N2 112.42(12) . . ? C1 N1 C3 125.15(14) . . ? N2 N1 C3 122.24(13) . . ? C4 O3 H31 111.1(12) . . ? C1 N4 N5 115.86(14) . . ? C2 N2 N1 102.58(13) . . ? O4 C4 O3 125.28(15) . . ? O4 C4 C3 119.80(14) . . ? O3 C4 C3 114.92(14) . . ? C1 N3 C2 107.04(14) . . ? C1 N3 H3 123.1(15) . . ? C2 N3 H3 129.6(15) . . ? N1 C3 C4 110.85(13) . . ? N1 C3 H3B 109.3(8) . . ? C4 C3 H3B 109.0(9) . . ? N1 C3 H3A 106.6(9) . . ? C4 C3 H3A 107.9(9) . . ? H3B C3 H3A 113.2(12) . . ? N1 C1 N4 119.18(14) . . ? N1 C1 N3 105.04(14) . . ? N4 C1 N3 135.78(15) . . ? N8 N7 N6 170.58(17) . . ? N7 N6 C2 113.55(14) . . ? O2 N5 O1 121.51(16) . . ? O2 N5 N4 116.42(16) . . ? O1 N5 N4 122.07(15) . . ? N2 C2 N3 112.91(15) . . ? N2 C2 N6 128.21(16) . . ? N3 C2 N6 118.85(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N1 N2 C2 0.54(17) . . . . ? C3 N1 N2 C2 175.75(14) . . . . ? C1 N1 C3 C4 69.53(19) . . . . ? N2 N1 C3 C4 -105.06(16) . . . . ? O4 C4 C3 N1 -149.38(14) . . . . ? O3 C4 C3 N1 30.98(19) . . . . ? N2 N1 C1 N4 178.81(13) . . . . ? C3 N1 C1 N4 3.8(2) . . . . ? N2 N1 C1 N3 -0.66(17) . . . . ? C3 N1 C1 N3 -175.71(14) . . . . ? N5 N4 C1 N1 -178.99(13) . . . . ? N5 N4 C1 N3 0.3(3) . . . . ? C2 N3 C1 N1 0.50(17) . . . . ? C2 N3 C1 N4 -178.84(18) . . . . ? C1 N4 N5 O2 -176.29(14) . . . . ? C1 N4 N5 O1 3.7(2) . . . . ? N1 N2 C2 N3 -0.20(18) . . . . ? N1 N2 C2 N6 -178.38(17) . . . . ? C1 N3 C2 N2 -0.19(19) . . . . ? C1 N3 C2 N6 178.18(15) . . . . ? N7 N6 C2 N2 7.4(3) . . . . ? N7 N6 C2 N3 -170.70(16) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 O3 H31 O4 1.02(2) 1.58(2) 2.6086(16) 177(2) 3 N3 H3 O1 0.84(2) 2.15(2) 2.603(2) 114.1(18) . N3 H3 O1 0.84(2) 2.38(2) 2.9389(19) 124.6(18) 2_455 N3 H3 O2 0.84(2) 2.64(2) 3.447(2) 162.8(18) 2_455 _geom_special_details ? _iucr_refine_instructions_details ; TITL v1 in P2(1)/c CELL 0.71073 10.3123 6.8821 12.2305 90.000 98.873 90.000 ZERR 4.00 0.0007 0.0005 0.0009 0.000 0.007 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 16 16 32 16 MERG 2 OMIT -2.00 52.00 EQIV $1 -x, -y, -z EQIV $2 -x-1, y+1/2, -z+1/2 HTAB O3 O4_$1 HTAB N3 O1 HTAB N3 O1_$2 HTAB N3 O2_$2 FMAP 2 SIZE 0.29 0.16 0.13 PLAN 20 ACTA BOND BOND $H CONF L.S. 4 TEMP -100.00 WGHT 0.034800 FVAR 0.68317 H3B 2 0.012253 0.359675 0.239587 11.00000 0.02049 H3A 2 0.035879 0.500133 0.135603 11.00000 0.02552 H31 2 -0.081528 0.094151 -0.045792 11.00000 0.08660 H3 2 -0.431409 0.465759 0.163690 11.00000 0.05797 MOLE 1 O4 4 0.075707 0.095679 0.118245 11.00000 0.03412 0.03043 = 0.02823 0.00044 0.00383 0.01105 N1 3 -0.150539 0.468387 0.147797 11.00000 0.02213 0.02351 = 0.02462 -0.00060 0.00484 0.00282 O3 4 -0.089376 0.220194 -0.002672 11.00000 0.03237 0.03851 = 0.02793 -0.00731 -0.00185 0.00855 N4 3 -0.228586 0.210433 0.240029 11.00000 0.03072 0.03368 = 0.03230 0.00645 0.00891 -0.00307 N2 3 -0.189506 0.635228 0.088490 11.00000 0.02832 0.02701 = 0.02710 0.00307 0.00655 0.00741 C4 1 -0.007070 0.222304 0.088564 11.00000 0.02008 0.02521 = 0.02414 0.00361 0.00696 -0.00057 O1 4 -0.447658 0.190678 0.243512 11.00000 0.03142 0.06303 = 0.05040 0.00348 0.01258 -0.01047 N3 3 -0.357264 0.487380 0.146791 11.00000 0.02354 0.04671 = 0.03338 0.00846 0.01223 0.00858 C3 1 -0.016788 0.396779 0.160731 11.00000 0.02005 0.02628 = 0.02925 0.00111 0.00320 0.00145 C1 1 -0.251083 0.376911 0.182889 11.00000 0.02299 0.03254 = 0.02195 -0.00314 0.00598 0.00204 N7 3 -0.360766 0.892410 -0.020200 11.00000 0.02574 0.04429 = 0.04592 0.00989 0.00574 0.01525 N6 3 -0.406582 0.773969 0.041770 11.00000 0.03400 0.05972 = 0.05265 0.02785 0.01975 0.02097 N5 3 -0.334727 0.125016 0.271125 11.00000 0.04157 0.04775 = 0.03057 0.00138 0.00766 -0.01064 O2 4 -0.314296 -0.022576 0.328724 11.00000 0.07177 0.05331 = 0.05359 0.02567 0.00747 -0.01658 C2 1 -0.315187 0.639618 0.090734 11.00000 0.02890 0.04071 = 0.02886 0.00758 0.00993 0.01144 N8 3 -0.336775 1.007350 -0.078541 11.00000 0.03332 0.05546 = 0.07211 0.02484 0.00780 0.00960 HKLF 4 REM v1 in P2(1)/c REM R1 = 0.0330 for 1124 Fo > 4sig(Fo) and 0.0557 for all 1677 data REM 161 parameters refined using 0 restraints END WGHT 0.0348 0.0000 REM Highest difference peak 0.170, deepest hole -0.216, 1-sigma level 0.039 Q1 1 -0.2298 0.7135 0.1421 11.00000 0.05 0.17 Q2 1 -0.3559 1.0340 0.0013 11.00000 0.05 0.17 Q3 1 -0.0808 0.4328 0.1575 11.00000 0.05 0.16 Q4 1 -0.1929 0.4328 0.1755 11.00000 0.05 0.15 Q5 1 -0.2527 0.2275 0.1711 11.00000 0.05 0.15 Q6 1 -0.2063 0.2156 0.0234 11.00000 0.05 0.15 Q7 1 0.1534 0.1846 0.0846 11.00000 0.05 0.14 Q8 1 -0.2111 0.3257 0.2384 11.00000 0.05 0.14 Q9 1 -0.4982 0.7699 0.0545 11.00000 0.05 0.13 Q10 1 -0.4409 0.2135 0.1610 11.00000 0.05 0.13 Q11 1 -0.2790 0.4837 0.2106 11.00000 0.05 0.13 Q12 1 -0.0380 0.2797 0.1402 11.00000 0.05 0.13 Q13 1 -0.1667 0.5388 0.1215 11.00000 0.05 0.12 Q14 1 -0.1007 0.3733 -0.0148 11.00000 0.05 0.12 Q15 1 -0.3939 -0.0909 0.3242 11.00000 0.05 0.12 Q16 1 -0.4428 0.0333 0.2023 11.00000 0.05 0.12 Q17 1 -0.4590 0.0916 0.1670 11.00000 0.05 0.11 Q18 1 -0.1460 0.6900 0.0633 11.00000 0.05 0.11 Q19 1 -0.2964 -0.1647 0.3199 11.00000 0.05 0.11 Q20 1 0.1538 0.1100 0.1973 11.00000 0.05 0.11 ;