# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email NEIL.BURFORD@DAL.CA _publ_contact_author_name 'Prof Neil Burford' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_date 2003-06-13 _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; _publ_contact_author_address ; Department of Chemistry Dalhousie University Halifax Nova Scotia B3H 4J3 CANADA ; _publ_section_title ; Definitive Identification of Lead-Amino Acid Adducts and the Solid State Structure of a Valine Complex ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1997). SHELXL-97. Sheldrick, G.M. (1985). SHELXS-86. In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; loop_ _publ_author_name 'Neil Burford' 'T. Stanley Cameron' 'Melanie D. Eelman' 'Wesley G. LeBlanc' 'Katherine N. Robertson' #============================================================================== data_melanie24 _database_code_CSD 216995 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction ; teXsan for Windows version 1.06 (MSC, 1997-1999) ; _computing_structure_solution ; SHELXS-86 (Sheldrick, 1985) ; _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997) ; _computing_publication_material ? #------------------------------------------------------------------------------ _cell_length_a 13.609(6) _cell_length_b 26.75(1) _cell_length_c 5.416(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1971(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 19.6 _cell_measurement_theta_max 20.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 601.53 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H26 N4 O12 Pb1' _chemical_formula_moiety 'C10 H26 N4 O12 Pb1' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1168.00 _exptl_absorpt_coefficient_mu 8.624 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North,Phillips & Matthews, 1968 ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.548 _exptl_special_details ; The scan width was (0.99+0.45tan\q)\% with an \w scan speed of 16\% per minute (up to 7 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_decay_% -0.05 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 0 1 2 1 1 2 -1 _diffrn_reflns_number 3351 _reflns_number_total 3320 _reflns_number_gt 1504 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.00790 _diffrn_reflns_av_sigmaI/netI 0.1416 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 30.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04884 _diffrn_orient_matrix_UB_12 -0.02789 _diffrn_orient_matrix_UB_13 -0.00753 _diffrn_orient_matrix_UB_21 0.05381 _diffrn_orient_matrix_UB_22 0.02472 _diffrn_orient_matrix_UB_23 -0.03006 _diffrn_orient_matrix_UB_31 0.01091 _diffrn_orient_matrix_UB_32 0.00293 _diffrn_orient_matrix_UB_33 0.18202 #------------------------------------------------------------------------------ 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.60448(4) 0.781363(19) 0.7474(2) 0.03513(18) Uani 1 d U . . O1 O 0.4821(7) 0.8304(4) 0.972(2) 0.039(2) Uani 1 d U . . O2 O 0.4447(10) 0.8696(6) 0.627(3) 0.046(4) Uani 1 d U . . O3 O 0.7001(7) 0.8316(4) 1.014(2) 0.037(2) Uani 1 d U . . O4 O 0.8076(7) 0.8105(4) 0.732(4) 0.046(3) Uani 1 d U . . O5 O 0.1334(9) 0.8960(6) 0.672(3) 0.064(4) Uani 1 d U . . O6 O 0.0002(9) 0.8713(5) 0.500(2) 0.054(4) Uani 1 d U . . O7 O 0.1252(7) 0.8886(5) 0.274(3) 0.050(3) Uani 1 d U . . O8 O 0.5901(7) 0.7350(4) 0.205(2) 0.041(3) Uani 1 d U . . O9 O 0.7309(11) 0.7182(7) 0.029(3) 0.060(4) Uani 1 d U . . O10 O 0.7159(11) 0.7132(7) 0.423(3) 0.053(4) Uani 1 d U . . O11 O 0.4146(7) 0.7346(4) 0.684(2) 0.041(3) Uani 1 d . . . H11A H 0.4001 0.7348 0.5313 0.062 Uiso 1 d R . . H11B H 0.3691 0.7493 0.7631 0.062 Uiso 1 d R . . O12 O 0.6329(8) 0.8561(4) 0.476(2) 0.048(3) Uani 1 d U . . H12A H 0.6476 0.8482 0.3284 0.072 Uiso 1 d R . . H12B H 0.5768 0.8698 0.4892 0.072 Uiso 1 d R . . N1 N 0.3246(8) 0.8617(4) 1.212(3) 0.030(3) Uani 1 d U . . H1A H 0.3171 0.8282 1.1898 0.045 Uiso 1 calc R . . H1B H 0.2680 0.8748 1.2741 0.045 Uiso 1 calc R . . H1C H 0.3746 0.8674 1.3200 0.045 Uiso 1 calc R . . N2 N 0.9559(8) 0.8501(5) 0.997(3) 0.032(3) Uani 1 d U . . H2A H 1.0001 0.8713 1.0668 0.048 Uiso 1 calc R . . H2B H 0.9680 0.8477 0.8319 0.048 Uiso 1 calc R . . H2C H 0.9615 0.8193 1.0672 0.048 Uiso 1 calc R . . N3 N 0.0886(8) 0.8864(5) 0.481(3) 0.038(3) Uani 1 d U . . N4 N 0.6753(8) 0.7209(4) 0.228(4) 0.032(3) Uani 1 d U . . C1 C 0.4340(13) 0.8595(8) 0.851(4) 0.035(3) Uani 1 d DU . . C2 C 0.3471(9) 0.8855(5) 0.975(3) 0.031(3) Uani 1 d DU . . H2 H 0.2886 0.8807 0.8659 0.037 Uiso 1 calc R . . C3 C 0.3608(9) 0.9416(5) 1.011(3) 0.037(3) Uani 1 d DU . . H3 H 0.3126 0.9524 1.1398 0.045 Uiso 1 calc R . . C4 C 0.4636(10) 0.9533(6) 1.111(3) 0.042(4) Uani 1 d DU . . H4A H 0.4761 0.9329 1.2586 0.064 Uiso 1 calc R . . H4B H 0.4677 0.9888 1.1549 0.064 Uiso 1 calc R . . H4C H 0.5128 0.9455 0.9850 0.064 Uiso 1 calc R . . C5 C 0.3384(13) 0.9716(5) 0.778(4) 0.066(6) Uani 1 d DU . . H5A H 0.3489 1.0073 0.8100 0.099 Uiso 1 calc R . . H5B H 0.2698 0.9662 0.7291 0.099 Uiso 1 calc R . . H5C H 0.3819 0.9607 0.6440 0.099 Uiso 1 calc R . . C6 C 0.7831(10) 0.8331(5) 0.919(3) 0.031(3) Uani 1 d DU . . C7 C 0.8564(10) 0.8692(4) 1.036(3) 0.028(2) Uani 1 d DU . . H7 H 0.8441 0.8687 1.2177 0.033 Uiso 1 calc R . . C8 C 0.8433(9) 0.9233(4) 0.950(3) 0.038(3) Uani 1 d DU . . H8 H 0.8580 0.9235 0.7693 0.046 Uiso 1 calc R . . C9 C 0.7388(10) 0.9431(6) 0.977(5) 0.062(6) Uani 1 d DU . . H9A H 0.6930 0.9200 0.8960 0.094 Uiso 1 calc R . . H9B H 0.7340 0.9761 0.8988 0.094 Uiso 1 calc R . . H9C H 0.7221 0.9459 1.1521 0.094 Uiso 1 calc R . . C10 C 0.9162(11) 0.9595(6) 1.068(4) 0.060(6) Uani 1 d DU . . H10A H 0.9831 0.9467 1.0465 0.089 Uiso 1 calc R . . H10B H 0.9018 0.9627 1.2448 0.089 Uiso 1 calc R . . H10C H 0.9105 0.9923 0.9891 0.089 Uiso 1 calc R . . 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 Pb1 0.0385(2) 0.0336(3) 0.0333(3) -0.0094(6) 0.0036(8) -0.0028(3) O1 0.030(4) 0.040(6) 0.047(6) 0.004(5) 0.004(4) 0.007(4) O2 0.043(7) 0.072(11) 0.023(4) -0.017(6) -0.010(6) 0.016(7) O3 0.030(4) 0.044(7) 0.037(5) -0.009(5) 0.005(4) -0.001(4) O4 0.033(4) 0.047(6) 0.057(8) -0.028(8) 0.017(7) -0.012(4) O5 0.051(6) 0.085(10) 0.056(6) -0.012(8) -0.015(6) -0.014(7) O6 0.044(6) 0.088(10) 0.029(6) 0.000(7) -0.006(5) -0.016(6) O7 0.031(5) 0.073(8) 0.046(6) 0.003(9) 0.001(6) 0.003(5) O8 0.037(4) 0.051(6) 0.036(9) -0.004(5) 0.001(5) 0.007(4) O9 0.071(8) 0.053(10) 0.057(6) -0.023(9) 0.029(7) 0.021(9) O10 0.050(7) 0.059(11) 0.051(6) -0.019(8) -0.016(6) 0.025(8) O11 0.038(5) 0.038(6) 0.048(9) -0.014(5) -0.008(5) -0.001(4) O12 0.045(6) 0.056(7) 0.042(6) 0.007(5) 0.008(5) 0.009(5) N1 0.037(5) 0.026(5) 0.028(7) -0.012(5) -0.010(5) -0.004(4) N2 0.034(4) 0.037(7) 0.024(6) -0.010(7) -0.005(6) 0.000(5) N3 0.028(5) 0.049(9) 0.038(5) 0.008(7) -0.006(5) 0.013(5) N4 0.031(4) 0.029(5) 0.035(5) 0.018(6) 0.006(5) 0.002(4) C1 0.032(7) 0.035(8) 0.038(6) 0.001(6) -0.003(6) 0.001(5) C2 0.029(6) 0.033(5) 0.030(7) 0.000(5) -0.005(6) 0.003(4) C3 0.038(6) 0.037(5) 0.037(8) -0.005(6) 0.013(7) -0.004(6) C4 0.059(8) 0.033(8) 0.034(9) -0.007(7) -0.009(8) -0.009(7) C5 0.089(13) 0.030(7) 0.079(14) 0.006(9) -0.038(14) 0.006(8) C6 0.032(5) 0.040(7) 0.021(7) 0.000(6) 0.001(5) -0.004(5) C7 0.036(5) 0.032(5) 0.015(6) 0.003(5) -0.003(6) -0.002(4) C8 0.048(8) 0.034(6) 0.033(9) 0.011(7) -0.006(8) 0.000(5) C9 0.054(7) 0.043(10) 0.091(17) 0.010(12) -0.007(12) 0.008(6) C10 0.062(9) 0.031(7) 0.086(17) -0.002(10) -0.012(12) -0.006(7) #============================================================================== # REFINEMENT DATA _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 _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881 ; _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 3320 _refine_ls_number_parameters 244 _refine_ls_number_restraints 66 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1622 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O3 2.362(11) . ? Pb1 O1 2.442(10) . ? Pb1 O12 2.510(12) . ? O1 C1 1.21(2) . ? O2 C1 1.25(2) . ? O3 C6 1.241(16) . ? O4 C6 1.22(2) . ? O5 N3 1.226(18) . ? O6 N3 1.274(15) . ? O7 N3 1.23(2) . ? O8 N4 1.226(14) . ? O9 N4 1.32(2) . ? O10 N4 1.21(2) . ? O11 H11A 0.8500 . ? O11 H11B 0.8500 . ? O12 H12A 0.8500 . ? O12 H12B 0.8500 . ? N1 C2 1.46(2) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 C7 1.463(17) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? C1 C2 1.528(10) . ? C2 C3 1.526(9) . ? C2 H2 1.0000 . ? C3 C5 1.529(10) . ? C3 C4 1.533(9) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.525(9) . ? C7 C8 1.531(9) . ? C7 H7 1.0000 . ? C8 C9 1.523(9) . ? C8 C10 1.526(9) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 Pb1 O1 76.5(4) . . ? O3 Pb1 O12 79.6(4) . . ? O1 Pb1 O12 88.2(4) . . ? C1 O1 Pb1 116.5(11) . . ? C6 O3 Pb1 105.5(9) . . ? H11A O11 H11B 108.6 . . ? Pb1 O12 H12A 113.0 . . ? Pb1 O12 H12B 99.1 . . ? H12A O12 H12B 113.4 . . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C7 N2 H2A 109.5 . . ? C7 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C7 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? O5 N3 O7 123.9(13) . . ? O5 N3 O6 117.8(15) . . ? O7 N3 O6 118.2(15) . . ? O10 N4 O8 125.0(18) . . ? O10 N4 O9 116.3(11) . . ? O8 N4 O9 118.4(18) . . ? O1 C1 O2 126.9(17) . . ? O1 C1 C2 118.2(17) . . ? O2 C1 C2 115(2) . . ? N1 C2 C3 109.9(12) . . ? N1 C2 C1 110.6(14) . . ? C3 C2 C1 114.1(14) . . ? N1 C2 H2 107.3 . . ? C3 C2 H2 107.3 . . ? C1 C2 H2 107.3 . . ? C2 C3 C5 112.8(12) . . ? C2 C3 C4 110.9(11) . . ? C5 C3 C4 111.6(12) . . ? C2 C3 H3 107.1 . . ? C5 C3 H3 107.1 . . ? C4 C3 H3 107.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 125.0(13) . . ? O4 C6 C7 118.5(13) . . ? O3 C6 C7 116.3(13) . . ? N2 C7 C6 108.9(11) . . ? N2 C7 C8 113.3(11) . . ? C6 C7 C8 113.4(11) . . ? N2 C7 H7 106.9 . . ? C6 C7 H7 106.9 . . ? C8 C7 H7 106.9 . . ? C9 C8 C10 110.4(13) . . ? C9 C8 C7 114.1(12) . . ? C10 C8 C7 113.4(12) . . ? C9 C8 H8 106.1 . . ? C10 C8 H8 106.1 . . ? C7 C8 H8 106.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 Pb1 O1 C1 114.9(14) . . . . ? O12 Pb1 O1 C1 35.1(14) . . . . ? O1 Pb1 O3 C6 -158.3(11) . . . . ? O12 Pb1 O3 C6 -67.7(10) . . . . ? Pb1 O1 C1 O2 -5(3) . . . . ? Pb1 O1 C1 C2 171.5(11) . . . . ? O1 C1 C2 N1 -12(2) . . . . ? O2 C1 C2 N1 164.9(19) . . . . ? O1 C1 C2 C3 112(2) . . . . ? O2 C1 C2 C3 -71(2) . . . . ? N1 C2 C3 C5 -154.0(13) . . . . ? C1 C2 C3 C5 81.1(18) . . . . ? N1 C2 C3 C4 80.0(15) . . . . ? C1 C2 C3 C4 -45(2) . . . . ? Pb1 O3 C6 O4 -3(2) . . . . ? Pb1 O3 C6 C7 171.9(10) . . . . ? O4 C6 C7 N2 -32.9(19) . . . . ? O3 C6 C7 N2 151.7(14) . . . . ? O4 C6 C7 C8 94.2(18) . . . . ? O3 C6 C7 C8 -81.2(17) . . . . ? N2 C7 C8 C9 176.9(15) . . . . ? C6 C7 C8 C9 52.1(19) . . . . ? N2 C7 C8 C10 -55.5(18) . . . . ? C6 C7 C8 C10 179.7(13) . . . . ? #============================================================================== _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.516 _refine_diff_density_min -2.367 _refine_diff_density_rms 0.248 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================