Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global ##################################################################### # AUTHOR AND PUBLICATION DATA # ##################################################################### _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' _audit_creation_date '25/01/01' _audit_creation_method 'ModiCIF v1.02' _audit_update_record ? _publ_contact_author 'Prof Lucedio Greci' _publ_contact_author_address ; Prof Lucedio Greci Dipartimento di Scienze dei Materiali e della Terra University of Ancona Via Brecce Bianche Ancona I-60131 ITALY ; _publ_section_title ; Reaction of indolinonic aminoxyls with nitric oxide ; loop_ _publ_author_name _publ_author_address 'Elisabetta Damiani' ; Dip. di Scienze dei Materiali e della Terra Universit\'a di Ancona Via Brecce Bianche I-60132 Ancona Italy ; 'Lucedio Greci' ; Dip. di Scienze dei Materiali e della Terra Universit\'a di Ancona Via Brecce Bianche I-60132 Ancona Italy ; 'Corrado Rizzoli' ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisica Viale delle Scienze 78 Universit\'a di Parma I-43100 Parma Italy ; _publ_section_references ; Belletti, D., Cantoni, A. & Pasquinelli, G. (1993) Gestione on-line di diffrattometro a cristallo singolo Siemens AED con personal computer. Centro di Studio per la Strutturistica Diffrattometrica del C.N.R.,Parma. Internal report 1/93. Sheldrick, G.M. (1986). SHELX86, Programs for the solution of crystal structures. Univ. of Gottingen, Germany Sheldrick, G.M. (1993). SHELXL93, Program for the crystal structure refinement. Univ. of Gottingen, Germany Nardelli, M. (1983). PARST. A system of computer routines for calculating molecular parameters from the results of crystal structure analysis. Univ. of Parma, Italy ; _publ_section_explt_prep ; ; _publ_section_explt_refinement ; ; data_Compound5a _database_code_CSD 157039 ##################################################################### # CHEMICAL INFORMATION # ##################################################################### _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15H12N2O2' _chemical_formula_weight 252.27 _chemical_melting_point ? _chemical_compound_source ? ##################################################################### # UNIT CELL INFORMATION # ##################################################################### _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/N' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '1/2-x,1/2+y,1/2-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 10.076(2) _cell_length_b 13.318(3) _cell_length_c 10.721(2) _cell_angle_alpha 90.00(0) _cell_angle_beta 117.39(0) _cell_angle_gamma 90.00(0) _cell_volume 1277.4(5) _cell_formula_units_Z 4.00 _cell_measurement_temperature 293 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 18.0 _cell_measurement_theta_max 35.0 ##################################################################### # CRYSTAL INFORMATION # ##################################################################### _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.3118 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 528.0 _exptl_special_details ; ? ; ##################################################################### # ABSORPTION CORRECTION # ##################################################################### _exptl_absorpt_coefficient_mu 0.6852 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.989 _exptl_absorpt_correction_T_max 1.000 ##################################################################### # DATA COLLECTION # ##################################################################### _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.03 _diffrn_reflns_number 2665 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0120 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.68 _reflns_number_total 2418 _reflns_number_observed 1639 _reflns_threshold_expression '>2 sigma(I)' ##################################################################### # COMPUTING PROGRAMS # ##################################################################### _computing_data_collection 'Belletti, Cantoni & Pasquinelli,1993' _computing_cell_refinement 'Belletti et al., 1993' _computing_data_reduction 'DIFAU (Belletti et al.)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'PARST (Nardelli, 1983)' ##################################################################### # REFINEMENT INFORMATION # ##################################################################### _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2036 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs 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 w=1/[\s^2^(Fo^2^)+(0.1607)^2^+ 0.13P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1639 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_obs 0.0712 _refine_ls_wR_factor_all 0.2889 _refine_ls_wR_factor_obs 0.2157 _refine_ls_goodness_of_fit_all 1.287 _refine_ls_goodness_of_fit_obs 1.163 _refine_ls_restrained_S_all 1.287 _refine_ls_restrained_S_obs 1.163 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.47 _refine_diff_density_min -0.25 _refine_diff_density_rms 0.00 ##################################################################### # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # ##################################################################### 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_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio _atom_site_occupancy # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # # atom x/a y/b z/c Ueq tmf calc att R #SOF O1 -0.2248(2) 0.0159(2) 0.0604(2) 0.0855(10) aniso . . 2.10 1.0000 O2 0.0941(4) 0.3246(2) 0.3092(3) 0.1268(18) aniso . . 2.76 1.0000 N1 -0.1060(3) 0.2446(2) 0.2430(2) 0.0757(10) aniso . . 1.72 1.0000 N2 -0.0266(4) 0.3245(2) 0.3046(3) 0.0959(15) aniso . . 2.41 1.0000 C1 -0.2087(3) 0.0959(2) 0.1231(3) 0.0649(11) aniso . . 1.39 1.0000 C2 -0.3142(3) 0.1459(2) 0.1610(3) 0.0700(12) aniso . . 1.30 1.0000 C3 -0.4587(3) 0.1187(3) 0.1336(4) 0.0897(16) aniso . . 1.81 1.0000 C4 -0.5367(4) 0.1839(4) 0.1748(4) 0.1086(20) aniso . . 2.06 1.0000 C5 -0.4736(5) 0.2716(4) 0.2416(4) 0.1108(22) aniso . . 2.45 1.0000 C6 -0.3276(5) 0.3003(3) 0.2746(4) 0.0960(19) aniso . . 1.78 1.0000 C7 -0.2511(3) 0.2342(2) 0.2296(3) 0.0733(11) aniso . . 1.48 1.0000 C8 -0.0657(3) 0.1608(2) 0.1752(3) 0.0672(11) aniso . . 1.43 1.0000 C9 0.0655(2) 0.0998(1) 0.2825(2) 0.0699(11) aniso . . 1.61 1.0000 C10 0.1579(2) 0.0474(2) 0.2409(2) 0.0932(16) aniso . . 1.96 1.0000 C11 0.2728(2) -0.0120(2) 0.3372(3) 0.1169(24) aniso . . 2.77 1.0000 C12 0.2954(2) -0.0190(2) 0.4749(3) 0.1056(20) aniso . . 2.43 1.0000 C13 0.2030(2) 0.0334(2) 0.5164(2) 0.0967(17) aniso . . 1.87 1.0000 C14 0.0881(2) 0.0928(2) 0.4202(2) 0.0794(14) aniso . . 1.36 1.0000 C15 -0.0484(4) 0.1991(3) 0.0492(4) 0.0918(16) aniso . . 1.63 1.0000 H3 -0.50520(0) 0.03510(0) 0.10130(0) 0.1000(0) iso . . 1.00 1.0000 H4 -0.64630(0) 0.15830(0) 0.15930(0) 0.1000(0) iso . . 1.00 1.0000 H5 -0.52050(0) 0.31740(0) 0.29670(0) 0.1000(0) iso . . 1.00 1.0000 H6 -0.27830(0) 0.35860(0) 0.33420(0) 0.1000(0) iso . . 1.00 1.0000 H10 0.13790(0) 0.05600(0) 0.13200(0) 0.1000(0) iso . . 1.00 1.0000 H11 0.35590(0) -0.06350(0) 0.32940(0) 0.1000(0) iso . . 1.00 1.0000 H12 0.37210(0) -0.06340(0) 0.55100(0) 0.1000(0) iso . . 1.00 1.0000 H13 0.22610(0) 0.02620(0) 0.61630(0) 0.1000(0) iso . . 1.00 1.0000 H14 0.02370(0) 0.12920(0) 0.44700(0) 0.1000(0) iso . . 1.00 1.0000 H151 -0.05840(0) 0.14640(0) -0.00880(0) 0.1000(0) iso . . 1.00 1.0000 H152 -0.12990(0) 0.24250(0) -0.01460(0) 0.1000(0) iso . . 1.00 1.0000 H153 0.05460(0) 0.23510(0) 0.07890(0) 0.1000(0) iso . . 1.00 1.0000 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 # #label U11 U22 U33 U23 U13 U12 # O1 0.0858(14) 0.0671(12) 0.0848(14) -0.0095(10) 0.0231(11) -0.0154(9) O2 0.1234(25) 0.0996(20) 0.1268(23) -0.0084(16) 0.0313(19) -0.0414(17) N1 0.0785(16) 0.0587(12) 0.0778(14) -0.0037(10) 0.0256(11) -0.0055(10) N2 0.0971(21) 0.0729(17) 0.0962(19) -0.0086(13) 0.0261(16) -0.0247(14) C1 0.0583(14) 0.0651(14) 0.0629(14) 0.0006(11) 0.0205(10) -0.0038(11) C2 0.0644(15) 0.0764(16) 0.0638(14) 0.0032(12) 0.0248(11) -0.0004(13) C3 0.0658(17) 0.1154(26) 0.0867(21) 0.0018(18) 0.0341(15) -0.0043(17) C4 0.0791(22) 0.1532(39) 0.0970(24) -0.0020(26) 0.0436(19) 0.0063(24) C5 0.0982(27) 0.1487(37) 0.0946(24) 0.0167(26) 0.0522(22) 0.0417(27) C6 0.1163(29) 0.0910(22) 0.0812(20) 0.0030(17) 0.0459(19) 0.0231(21) C7 0.0734(17) 0.0748(17) 0.0650(15) 0.0075(12) 0.0260(12) 0.0106(12) C8 0.0615(15) 0.0657(14) 0.0689(14) -0.0048(12) 0.0255(12) -0.0099(11) C9 0.0572(14) 0.0689(15) 0.0765(16) -0.0048(12) 0.0247(12) -0.0090(11) C10 0.0657(18) 0.1074(24) 0.1047(23) -0.0175(20) 0.0377(17) -0.0067(17) C11 0.0695(21) 0.1067(29) 0.1621(41) -0.0146(27) 0.0425(25) 0.0078(19) C12 0.0704(20) 0.0907(24) 0.1243(32) 0.0057(21) 0.0180(21) 0.0068(16) C13 0.0870(22) 0.0929(24) 0.0856(22) 0.0111(17) 0.0185(17) 0.0066(18) C14 0.0689(16) 0.0809(19) 0.0807(18) 0.0051(15) 0.0278(14) 0.0031(14) C15 0.0941(22) 0.1026(23) 0.0786(19) 0.0005(17) 0.0397(16) -0.0187(19) ##################################################################### # MOLECULAR GEOMETRY # ##################################################################### loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 1.230(4) yes O2 N2 1.194(6) yes N1 N2 1.312(4) yes N1 C7 1.409(5) yes N1 C8 1.487(4) yes C1 C2 1.462(5) yes C1 C8 1.548(4) yes C2 C3 1.394(5) yes C2 C7 1.378(4) yes C3 C4 1.373(7) yes C4 C5 1.365(7) yes C5 C6 1.399(7) yes C6 C7 1.394(6) yes C8 C9 1.527(3) yes C8 C15 1.527(6) yes C9 C10 1.391(3) yes C9 C14 1.390(3) yes C10 C11 1.390(3) yes C11 C12 1.390(5) yes C12 C13 1.390(4) yes C13 C14 1.390(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C7 N1 C8 112.4(3) yes N2 N1 C8 127.9(3) yes N2 N1 C7 119.7(3) yes O2 N2 N1 113.3(4) yes O1 C1 C8 123.2(3) yes O1 C1 C2 128.1(3) yes C2 C1 C8 108.7(2) yes C1 C2 C7 108.7(3) yes C1 C2 C3 130.2(3) yes C3 C2 C7 121.0(3) yes C2 C3 C4 117.7(4) yes C3 C4 C5 120.8(4) yes C4 C5 C6 123.3(5) yes C5 C6 C7 115.1(4) yes C2 C7 C6 122.1(3) yes N1 C7 C6 128.0(3) yes N1 C7 C2 109.9(3) yes N1 C8 C1 100.2(2) yes C1 C8 C15 109.5(3) yes C1 C8 C9 108.3(2) yes N1 C8 C15 110.5(2) yes N1 C8 C9 111.6(2) yes C9 C8 C15 115.6(3) yes C8 C9 C14 119.9(2) yes C8 C9 C10 120.0(2) yes C10 C9 C14 120.0(2) yes C9 C10 C11 119.9(2) yes C10 C11 C12 120.1(2) yes C11 C12 C13 120.0(3) yes C12 C13 C14 120.0(2) yes C9 C14 C13 120.0(2) yes #=END ##################################################################### data_Compound5b _database_code_CSD 157040 ##################################################################### # CHEMICAL INFORMATION # ##################################################################### _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15H12N2O3' _chemical_formula_weight 268.27 _chemical_melting_point ? _chemical_compound_source ? ##################################################################### # UNIT CELL INFORMATION # ##################################################################### _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P21/N' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '1/2-x,1/2+y,1/2-z' '1/2+x,1/2-y,1/2+z' _cell_length_a 9.871(2) _cell_length_b 13.901(3) _cell_length_c 10.714(2) _cell_angle_alpha 90.00(0) _cell_angle_beta 115.30(0) _cell_angle_gamma 90.00(0) _cell_volume 1329.1(5) _cell_formula_units_Z 4.00 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 29.5 ##################################################################### # CRYSTAL INFORMATION # ##################################################################### _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.3406 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 560.0 _exptl_special_details ; ? ; ##################################################################### # ABSORPTION CORRECTION # ##################################################################### _exptl_absorpt_coefficient_mu 0.7467 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.947 _exptl_absorpt_correction_T_max 1.000 ##################################################################### # DATA COLLECTION # ##################################################################### _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focussealedtube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens AED' _diffrn_measurement_method 'theta/2theta' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 2765 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.67 _reflns_number_total 2514 _reflns_number_observed 970 _reflns_threshold_expression '>2 sigma(I)' ##################################################################### # COMPUTING PROGRAMS # ##################################################################### _computing_data_collection 'Belletti, Cantoni & Pasquinelli,1993' _computing_cell_refinement 'Belletti et al., 1993' _computing_data_reduction 'DIFAU (Belletti et al.)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXS-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material 'PARST (Nardelli, 1983)' ##################################################################### # REFINEMENT INFORMATION # ##################################################################### _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2036 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R factor obs 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 w=1/[\s^2^(Fo^2^)+(0.1957)^2^+ 0.00P] 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 not_refined _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1170 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_obs 0.0873 _refine_ls_wR_factor_all 0.3004 _refine_ls_wR_factor_obs 0.2311 _refine_ls_goodness_of_fit_all 0.980 _refine_ls_goodness_of_fit_obs 1.106 _refine_ls_restrained_S_all 0.980 _refine_ls_restrained_S_obs 1.106 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.31 _refine_diff_density_min -0.23 _refine_diff_density_rms 0.00 ##################################################################### # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # ##################################################################### 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_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_aniso_ratio _atom_site_occupancy # # R=Rmax./Rmin.=ratio of the maximum and minimum # principal axes of atomic displacement ellipsoids # # Table of coordinates # -------------------- # # atom x/a y/b z/c Ueq tmf calc att R #SOF O1 0.2761(4) 0.5156(3) -0.4330(3) 0.1139(18) aniso . . 1.91 1.0000 O2 0.6219(7) 0.8005(4) -0.2100(5) 0.1627(29) aniso . . 2.64 1.0000 O3 0.4567(7) 0.8810(5) -0.1823(5) 0.1781(30) aniso . . 3.12 1.0000 N1 0.4027(5) 0.7367(3) -0.2630(4) 0.1110(22) aniso . . 1.84 1.0000 N2 0.4981(8) 0.8106(4) -0.2145(6) 0.1242(29) aniso . . 1.92 1.0000 C1 0.2943(5) 0.5945(4) -0.3751(4) 0.0907(21) aniso . . 1.68 1.0000 C2 0.1896(5) 0.6489(4) -0.3395(4) 0.0918(21) aniso . . 1.71 1.0000 C3 0.0431(6) 0.6281(5) -0.3632(5) 0.1094(25) aniso . . 1.46 1.0000 C4 -0.0356(8) 0.6933(6) -0.3247(7) 0.1349(36) aniso . . 1.74 1.0000 C5 0.0313(10) 0.7777(7) -0.2617(7) 0.1366(41) aniso . . 2.12 1.0000 C6 0.1774(9) 0.8000(5) -0.2330(5) 0.1219(29) aniso . . 2.12 1.0000 C7 0.2557(6) 0.7339(4) -0.2747(4) 0.0995(23) aniso . . 1.88 1.0000 C8 0.4415(5) 0.6533(4) -0.3261(4) 0.0983(22) aniso . . 1.58 1.0000 C9 0.5692(5) 0.5951(4) -0.2211(4) 0.0906(20) aniso . . 1.48 1.0000 C10 0.6649(7) 0.5444(5) -0.2575(7) 0.1235(33) aniso . . 1.53 1.0000 C11 0.7776(8) 0.4897(5) -0.1618(11) 0.1488(48) aniso . . 2.06 1.0000 C12 0.7946(8) 0.4835(5) -0.0271(10) 0.1422(41) aniso . . 2.03 1.0000 C13 0.6972(7) 0.5310(5) 0.0081(6) 0.1264(30) aniso . . 1.95 1.0000 C14 0.5863(6) 0.5889(4) -0.0860(5) 0.1067(24) aniso . . 1.47 1.0000 C15 0.4633(8) 0.6833(5) -0.4560(6) 0.1419(33) aniso . . 2.97 1.0000 H3 -0.0011(6) 0.5704(5) -0.4050(5) 0.1313(0) iso . . 1.00 1.0000 H4 -0.1342(8) 0.6804(6) -0.3411(7) 0.1620(0) iso . . 1.00 1.0000 H5 -0.0245(10) 0.8215(7) -0.2374(7) 0.1640(0) iso . . 1.00 1.0000 H6 0.2218(9) 0.8567(5) -0.1878(5) 0.1464(0) iso . . 1.00 1.0000 H10 0.6539(7) 0.5469(5) -0.3481(7) 0.1482(0) iso . . 1.00 1.0000 H11 0.8430(8) 0.4564(5) -0.1880(11) 0.1786(0) iso . . 1.00 1.0000 H12 0.8717(8) 0.4472(5) 0.0379(10) 0.1708(0) iso . . 1.00 1.0000 H13 0.7046(7) 0.5248(5) 0.0972(6) 0.1518(0) iso . . 1.00 1.0000 H14 0.5232(6) 0.6236(4) -0.0586(5) 0.1281(0) iso . . 1.00 1.0000 H151 0.3780(8) 0.7198(5) -0.5171(6) 0.1703(0) iso . . 1.00 1.0000 H152 0.4734(8) 0.6267(5) -0.5028(6) 0.1703(0) iso . . 1.00 1.0000 H153 0.5520(8) 0.7220(5) -0.4285(6) 0.1703(0) iso . . 1.00 1.0000 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 # #label U11 U22 U33 U23 U13 U12 # O1 0.1358(30) 0.0967(24) 0.0939(21) -0.0140(18) 0.0345(20) -0.0131(19) O2 0.1375(37) 0.1534(44) 0.1518(40) 0.0205(29) 0.0184(32) -0.0464(34) O3 0.2239(56) 0.1343(40) 0.1275(36) -0.0261(32) 0.0287(34) -0.0472(41) N1 0.1170(34) 0.0923(27) 0.1014(28) 0.0014(23) 0.0253(24) -0.0162(26) N2 0.1364(45) 0.0982(36) 0.1084(32) 0.0017(27) 0.0240(32) -0.0138(35) C1 0.0827(27) 0.1124(35) 0.0697(22) 0.0066(24) 0.0254(19) -0.0004(25) C2 0.0960(32) 0.1034(32) 0.0658(22) 0.0082(21) 0.0249(20) 0.0008(26) C3 0.1009(35) 0.1315(42) 0.0925(31) 0.0058(28) 0.0383(26) -0.0039(33) C4 0.1291(49) 0.1715(62) 0.1150(43) 0.0115(43) 0.0625(39) 0.0142(48) C5 0.1574(63) 0.1597(60) 0.1006(39) 0.0083(40) 0.0626(41) 0.0356(52) C6 0.1532(52) 0.1177(42) 0.0826(30) 0.0008(26) 0.0387(34) 0.0213(40) C7 0.1151(38) 0.1054(35) 0.0680(25) 0.0076(23) 0.0296(24) 0.0043(30) C8 0.1019(31) 0.1092(34) 0.0766(25) -0.0013(24) 0.0314(22) -0.0108(27) C9 0.0812(25) 0.1043(31) 0.0800(27) -0.0070(24) 0.0283(21) -0.0101(24) C10 0.1092(41) 0.1448(48) 0.1153(44) -0.0209(38) 0.0469(36) -0.0126(40) C11 0.1128(46) 0.1582(62) 0.1748(82) -0.0314(54) 0.0610(51) 0.0109(42) C12 0.1187(49) 0.1272(49) 0.1440(65) 0.0037(41) 0.0210(43) 0.0179(37) C13 0.1146(41) 0.1426(46) 0.0927(36) 0.0072(33) 0.0162(31) 0.0105(39) C14 0.1107(34) 0.1174(39) 0.0829(30) -0.0022(27) 0.0325(26) 0.0008(29) C15 0.1386(46) 0.1957(68) 0.0886(33) 0.0188(34) 0.0459(31) -0.0411(42) ##################################################################### # MOLECULAR GEOMETRY # ##################################################################### loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O1 C1 1.235(7) yes O2 N2 1.210(11) yes O3 N2 1.168(10) yes N1 N2 1.339(7) yes N1 C7 1.403(8) yes N1 C8 1.473(7) yes C1 C2 1.457(8) yes C1 C8 1.550(7) yes C2 C3 1.388(8) yes C2 C7 1.384(7) yes C3 C4 1.367(11) yes C4 C5 1.374(12) yes C5 C6 1.375(13) yes C6 C7 1.392(10) yes C8 C9 1.516(6) yes C8 C15 1.553(9) yes C9 C10 1.362(10) yes C9 C14 1.386(7) yes C10 C11 1.376(9) yes C11 C12 1.383(16) yes C12 C13 1.346(12) yes C13 C14 1.385(8) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C7 N1 C8 113.5(4) yes N2 N1 C8 120.3(5) yes N2 N1 C7 125.8(5) yes O3 N2 N1 118.7(7) yes O2 N2 N1 117.2(6) yes O2 N2 O3 124.1(8) yes O1 C1 C8 123.5(5) yes O1 C1 C2 128.7(5) yes C2 C1 C8 107.8(4) yes C1 C2 C7 109.8(5) yes C1 C2 C3 130.1(5) yes C3 C2 C7 120.0(5) yes C2 C3 C4 119.3(6) yes C3 C4 C5 119.9(8) yes C4 C5 C6 122.7(8) yes C5 C6 C7 116.9(7) yes C2 C7 C6 121.1(6) yes N1 C7 C6 130.4(5) yes N1 C7 C2 108.4(5) yes N1 C8 C1 100.4(4) yes C1 C8 C15 107.9(4) yes C1 C8 C9 109.4(4) yes N1 C8 C15 111.3(5) yes N1 C8 C9 112.1(4) yes C9 C8 C15 114.8(5) yes C8 C9 C14 120.0(5) yes C8 C9 C10 121.5(4) yes C10 C9 C14 118.5(5) yes C9 C10 C11 120.8(7) yes C10 C11 C12 120.8(8) yes C11 C12 C13 118.6(8) yes C12 C13 C14 121.2(7) yes C9 C14 C13 120.1(5) yes #=END ### END FILE ###