data_bj335/MBE-518 #------------------------------------------------------------------------------ ### 98.7 % of data out to 0.84 Angstroms, only high angle data missing## _audit_creation_date '2004-08-04' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' ENTER CONTACT NAME HERE' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ' ENTER ANY FOOTNOTES TO TITLE ' _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1996-1998). d*TREK. Area Detector Software. Version 4.4. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Altomare, A., Burla, M.C., Cammalli, G., Cascarano, M., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G., Spagna, A. (1998). SIR97: a new tool for crystal structure determination and refinement. Submitted. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ loop_ _publ_manuscript_incl_extra_item '_geom_extra_table_head_3' '_geom_bond_atom_site_label_D' '_geom_bond_atom_site_label_H' '_geom_contact_atom_site_label_A' '_geom_bond_distance_DH' '_geom_contact_distance_HA' '_geom_contact_distance_DA' '_geom_angle_DHA' '_geom_contact_site_symmetry_A' # # #------------------------------------------------------------------------------ _computing_data_collection 'd*TREK (MSC, 1996-1998)' _computing_cell_refinement 'd*TREK (MSC, 1996-1998)' _computing_data_reduction 'd*TREK (MSC, 1996-1998)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1998) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 17.885(2) _cell_length_b 15.005(3) _cell_length_c 7.4444(8) _cell_angle_alpha 90.000(2) _cell_angle_beta 90.000(2) _cell_angle_gamma 90.000(2) _cell_volume 1998(1) _cell_formula_units_Z 8 _cell_measurement_temperature 198.2 _cell_measurement_reflns_used 9066 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 30.03 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n ' _symmetry_Int_Tables_number 56 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2-y, +z' '1/2+x, -y,1/2-z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2+y, -z' '1/2-x, +y,1/2+z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 191.23 _chemical_formula_analytical ? _chemical_formula_sum 'C10 H13 N3 O ' _chemical_formula_moiety 'C10 H13 N3 O ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 816.00 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.7416 _exptl_special_details ; Data were collected in 0.50\% oscillations with 43.0 s exposures. A sweep of data was done using \f oscillations from 0.0 to 190.0\% at \c = -90\% and a second sweep was performed using \w oscillations between -22.0 and 18.0\% at \c = -90.0\%. The crystal-to-detector distance was 38.30 mm. The detector swing angle was -10.5\%. The absorption correction is based on a three-dimensional analysis of symmetry-equivalent data and is performed along with batch scaling in a single step. The resulting transmission factors, therefore, include contributions from absorption, crystal decay, and detectable variations in beam intensity. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 198.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD' _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_detector_area_resol_mean 11.76 _diffrn_measurement_method 'area detector' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 18044 _reflns_number_total 2460 _reflns_number_gt 1587 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.05027 _diffrn_reflns_av_sigmaI/netI 0.110 _diffrn_reflns_theta_full 0.840 _diffrn_measured_fraction_theta_max 0.840 _diffrn_measured_fraction_theta_full 30.03 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 80 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 104 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 24 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom O(1) 0.26166(4) 0.14183(6) -0.1508(1) 0.0292(2) 1.000 . Uani d ? N(1) 0.07344(5) 0.14719(6) -0.0281(1) 0.0224(2) 1.000 . Uani d ? N(2) 0.14983(5) 0.14522(7) -0.0085(1) 0.0243(3) 1.000 . Uani d ? N(3) 0.15596(6) 0.15244(8) -0.3166(1) 0.0319(3) 1.000 . Uani d ? C(1) -0.04980(6) 0.13535(8) 0.0776(1) 0.0223(3) 1.000 . Uani d ? C(2) -0.08001(7) 0.18964(8) -0.0565(2) 0.0287(3) 1.000 . Uani d ? C(3) -0.15621(7) 0.19050(9) -0.0884(2) 0.0356(4) 1.000 . Uani d ? C(4) -0.20361(7) 0.13712(9) 0.0111(2) 0.0360(4) 1.000 . Uani d ? C(5) -0.17453(7) 0.08208(9) 0.1427(2) 0.0329(3) 1.000 . Uani d ? C(6) -0.09838(7) 0.08180(8) 0.1769(1) 0.0276(3) 1.000 . Uani d ? C(7) 0.03187(6) 0.13276(7) 0.1103(1) 0.0207(3) 1.000 . Uani d ? C(8) 0.06131(6) 0.11106(8) 0.2955(1) 0.0242(3) 1.000 . Uani d ? C(9) 0.08785(8) 0.01458(9) 0.3109(2) 0.0365(4) 1.000 . Uani d ? C(10) 0.19295(6) 0.14692(8) -0.1610(1) 0.0219(3) 1.000 . Uani d ? H(1) -0.0464 0.2279 -0.1278 0.033 1.000 . Uiso c ? H(2) -0.1774 0.2291 -0.1837 0.041 1.000 . Uiso c ? H(3) -0.2590 0.1382 -0.0100 0.041 1.000 . Uiso c ? H(4) -0.2079 0.0433 0.2123 0.037 1.000 . Uiso c ? H(5) -0.0783 0.0430 0.2723 0.032 1.000 . Uiso c ? H(6) 0.1030 0.1511 0.3229 0.027 1.000 . Uiso c ? H(7) 0.0210 0.1212 0.3837 0.027 1.000 . Uiso c ? H(8) 0.0462 -0.0264 0.2835 0.043 1.000 . Uiso c ? H(9) 0.1284 0.0036 0.2244 0.043 1.000 . Uiso c ? H(10) 0.1060 0.0023 0.4325 0.043 1.000 . Uiso c ? H(11) 0.1734(8) 0.1401(9) 0.094(2) 0.033(4) 1.000 . Uiso d ? H(12) 0.1061(8) 0.155(1) -0.311(2) 0.036(4) 1.000 . Uiso d ? H(13) 0.1805(9) 0.154(1) -0.415(2) 0.045(4) 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O(1) 0.0184(5) 0.0484(6) 0.0209(4) 0.0002(4) 0.0010(3) 0.0015(3) N(1) 0.0182(5) 0.0288(5) 0.0203(4) -0.0001(4) -0.0005(3) 0.0011(4) N(2) 0.0180(5) 0.0388(6) 0.0160(4) -0.0005(4) -0.0004(3) 0.0010(4) N(3) 0.0210(5) 0.0578(8) 0.0170(5) -0.0002(5) 0.0005(3) 0.0027(4) C(1) 0.0213(6) 0.0245(6) 0.0209(5) 0.0017(4) 0.0011(4) -0.0029(4) C(2) 0.0274(6) 0.0282(7) 0.0305(6) 0.0024(5) -0.0006(4) 0.0027(5) C(3) 0.0310(7) 0.0380(8) 0.0378(6) 0.0089(6) -0.0078(5) 0.0013(5) C(4) 0.0206(7) 0.0420(8) 0.0453(7) 0.0045(6) -0.0034(5) -0.0115(6) C(5) 0.0245(7) 0.0360(8) 0.0382(6) -0.0039(5) 0.0065(5) -0.0065(5) C(6) 0.0254(6) 0.0313(7) 0.0259(5) 0.0006(5) 0.0034(4) 0.0018(5) C(7) 0.0216(6) 0.0224(6) 0.0181(5) 0.0009(4) -0.0001(4) -0.0005(4) C(8) 0.0210(6) 0.0340(7) 0.0176(5) 0.0005(5) 0.0003(4) 0.0000(4) C(9) 0.0437(8) 0.0380(8) 0.0279(6) 0.0061(6) -0.0008(5) 0.0067(5) C(10) 0.0216(6) 0.0257(6) 0.0186(5) -0.0013(5) 0.0011(4) 0.0006(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)]' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2460 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_all 0.0912 _refine_ls_wR_factor_ref 0.0912 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_shift/su_max 0.0030 _refine_ls_shift/su_mean 0.0007 _refine_diff_density_min -0.29 _refine_diff_density_max 0.31 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(10) 1.234(1) . . yes N(1) N(2) 1.374(1) . . yes N(1) C(7) 1.289(1) . . yes N(2) C(10) 1.372(1) . . yes N(2) H(11) 0.88(1) . . no N(3) C(10) 1.337(1) . . yes N(3) H(12) 0.89(1) . . no N(3) H(13) 0.85(2) . . no C(1) C(2) 1.397(2) . . yes C(1) C(6) 1.395(2) . . yes C(1) C(7) 1.481(2) . . yes C(2) C(3) 1.383(2) . . yes C(2) H(1) 0.99 . . no C(3) C(4) 1.382(2) . . yes C(3) H(2) 0.99 . . no C(4) C(5) 1.383(2) . . yes C(4) H(3) 1.00 . . no C(5) C(6) 1.385(2) . . yes C(5) H(4) 0.98 . . no C(6) H(5) 0.99 . . no C(7) C(8) 1.511(1) . . yes C(8) C(9) 1.528(2) . . yes C(8) H(6) 0.98 . . no C(8) H(7) 0.99 . . no C(9) H(8) 0.99 . . no C(9) H(9) 0.98 . . no C(9) H(10) 0.98 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(2) N(1) C(7) 119.03(9) . . . yes N(1) N(2) C(10) 118.08(9) . . . yes N(1) N(2) H(11) 125.0(9) . . . no C(10) N(2) H(11) 116.8(9) . . . no C(10) N(3) H(12) 117.1(9) . . . no C(10) N(3) H(13) 119(1) . . . no H(12) N(3) H(13) 124(1) . . . no C(2) C(1) C(6) 118.3(1) . . . yes C(2) C(1) C(7) 120.9(1) . . . yes C(6) C(1) C(7) 120.8(1) . . . yes C(1) C(2) C(3) 120.6(1) . . . yes C(1) C(2) H(1) 119.3 . . . no C(3) C(2) H(1) 120.2 . . . no C(2) C(3) C(4) 120.5(1) . . . yes C(2) C(3) H(2) 120.3 . . . no C(4) C(3) H(2) 119.2 . . . no C(3) C(4) C(5) 119.7(1) . . . yes C(3) C(4) H(3) 120.9 . . . no C(5) C(4) H(3) 119.5 . . . no C(4) C(5) C(6) 120.1(1) . . . yes C(4) C(5) H(4) 120.0 . . . no C(6) C(5) H(4) 119.9 . . . no C(1) C(6) C(5) 120.9(1) . . . yes C(1) C(6) H(5) 119.6 . . . no C(5) C(6) H(5) 119.5 . . . no N(1) C(7) C(1) 115.64(9) . . . yes N(1) C(7) C(8) 124.4(1) . . . yes C(1) C(7) C(8) 119.96(9) . . . yes C(7) C(8) C(9) 112.38(9) . . . yes C(7) C(8) H(6) 108.9 . . . no C(7) C(8) H(7) 108.6 . . . no C(9) C(8) H(6) 109.2 . . . no C(9) C(8) H(7) 108.9 . . . no H(6) C(8) H(7) 108.9 . . . no C(8) C(9) H(8) 109.9 . . . no C(8) C(9) H(9) 109.9 . . . no C(8) C(9) H(10) 110.5 . . . no H(8) C(9) H(9) 108.5 . . . no H(8) C(9) H(10) 108.9 . . . no H(9) C(9) H(10) 109.2 . . . no O(1) C(10) N(2) 120.53(9) . . . yes O(1) C(10) N(3) 123.4(1) . . . yes N(2) C(10) N(3) 116.1(1) . . . yes #------------------------------------------------------------------------------ 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 O(1) N(3) 2.896(1) . 7 no O(1) N(2) 3.098(1) . 7_554 no O(1) C(8) 3.225(1) . 7_554 no O(1) O(1) 3.273(2) . 2 no O(1) C(10) 3.273(1) . 2 no O(1) C(9) 3.312(2) . 7_554 no N(2) N(3) 3.357(2) . 8 no N(2) C(5) 3.581(2) . 5 no N(3) C(8) 3.404(1) . 1_554 no C(4) C(5) 3.599(2) . 7_454 no C(5) C(10) 3.455(2) . 5 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O(1) C(10) N(2) N(1) . . . . -177.2(1) no N(1) N(2) C(10) N(3) . . . . 1.5(2) no N(1) C(7) C(1) C(2) . . . . -30.1(2) no N(1) C(7) C(1) C(6) . . . . 148.2(1) no N(1) C(7) C(8) C(9) . . . . -76.7(1) no N(2) N(1) C(7) C(1) . . . . -179.5(1) no N(2) N(1) C(7) C(8) . . . . -1.7(2) no C(1) C(2) C(3) C(4) . . . . -0.5(2) no C(1) C(6) C(5) C(4) . . . . -1.3(2) no C(1) C(7) C(8) C(9) . . . . 101.0(1) no C(2) C(1) C(6) C(5) . . . . 0.4(2) no C(2) C(1) C(7) C(8) . . . . 151.9(1) no C(2) C(3) C(4) C(5) . . . . -0.4(2) no C(3) C(2) C(1) C(6) . . . . 0.5(2) no C(3) C(2) C(1) C(7) . . . . 178.9(1) no C(3) C(4) C(5) C(6) . . . . 1.3(2) no C(5) C(6) C(1) C(7) . . . . -178.0(1) no C(6) C(1) C(7) C(8) . . . . -29.8(2) no C(7) N(1) N(2) C(10) . . . . 170.1(1) no #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_D _geom_bond_atom_site_label_H _geom_contact_atom_site_label_A _geom_bond_distance_DH _geom_contact_distance_HA _geom_contact_distance_DA _geom_angle_DHA _geom_contact_site_symmetry_A 'N(2)' 'H(11)' 'O(1)' '0.88(1)' '2.23(1)' '2.264(1)' '174(1)' '7' 'N(3)' 'H(12)' 'N(1)' '0.89(1)' '2.19(1)' '2.607(1)' '108(1)' '.' 'N(3)' 'H(13)' 'O(1)' '0.85' '2.05' '2.896(1)' '173.0' '7_554' 'N(3)' 'H(13)' 'N(2)' '0.85' '3.12' '2.299(1)' '133.7' '7_554'