# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1451 data_NaTm #------------------------------------------------------------------------------ _audit_creation_date 'Fri Sep 18 11:32:23 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.962(2) _cell_length_b 14.790(2) _cell_length_c 8.217(2) _cell_angle_alpha 83.55(1) _cell_angle_beta 78.08(2) _cell_angle_gamma 72.65(1) _cell_volume 1129.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 26.3 _cell_measurement_theta_max 31.9 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'tabular' _exptl_crystal_colour 'colourlesstabular' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 422.28 _chemical_formula_analytical ? _chemical_formula_sum 'C12 H16 B N6 Na O3 S3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 436.00 _exptl_absorpt_coefficient_mu 0.369 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.34 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5227 _reflns_number_total 4935 _reflns_number_observed 2299 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 4.37 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 26.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.09389 _diffrn_orient_matrix_UB_12 0.01241 _diffrn_orient_matrix_UB_13 0.07856 _diffrn_orient_matrix_UB_21 0.00367 _diffrn_orient_matrix_UB_22 0.06562 _diffrn_orient_matrix_UB_23 0.01279 _diffrn_orient_matrix_UB_31 -0.05110 _diffrn_orient_matrix_UB_32 0.02393 _diffrn_orient_matrix_UB_33 -0.09582 #------------------------------------------------------------------------------ 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 24 0.003 0.002 'International Tables' H 0 32 0.000 0.000 'International Tables' B 0 2 0.001 0.001 'International Tables' N 0 12 0.006 0.003 'International Tables' Na 0 2 0.036 0.025 'International Tables' S 0 6 0.125 0.123 'International Tables' O 0 6 0.011 0.006 'International Tables' #------------------------------------------------------------------------------ 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 S(1) 0.0362(3) 0.2344(2) 0.9195(3) 0.0560 Uij ? ? S(2) 0.4429(3) 0.3213(2) 1.0114(4) 0.0660 Uij ? ? S(3) 0.5111(3) 0.1172(2) 0.4766(3) 0.0586 Uij ? ? Na(2) 0.194(1) 0.0246(8) 1.103(1) 0.1018 Uij ? ? Na(3) 0.5000 0.0000 1.0000 0.14(2) Uij ? ? Na(4) 0.455(1) 0.0015(7) 1.004(1) 0.032(3) Uij ? ? O(1) 0.3907(7) -0.1134(5) 1.1615(9) 0.0729 Uij ? ? O(2) 0.316(1) 0.0281(6) 0.8299(10) 0.0978 Uij ? ? O(3) 0.3276(10) 0.1234(6) 1.161(1) 0.0972 Uij ? ? O(8) 1.0000 0.0000 1.0000 0.180(7) Uij ? ? O(9) 0.061(3) 0.043(2) 1.337(3) 0.137(8) Uij ? ? O(10) 0.146(4) 0.036(2) 1.440(4) 0.22(1) Uij ? ? N(1) 0.1763(7) 0.2899(4) 0.6195(8) 0.0374 Uij ? ? N(2) -0.0248(8) 0.2637(6) 0.606(1) 0.0579 Uij ? ? N(3) 0.2580(7) 0.3862(4) 0.7906(8) 0.0368 Uij ? ? N(4) 0.2376(8) 0.4857(5) 0.9779(9) 0.0440 Uij ? ? N(5) 0.4272(7) 0.3046(4) 0.5450(8) 0.0373 Uij ? ? N(6) 0.6103(7) 0.2683(5) 0.3435(8) 0.0459 Uij ? ? C(1) 0.156(1) 0.3071(7) 0.457(1) 0.0565 Uij ? ? C(2) 0.034(1) 0.2885(9) 0.448(1) 0.0709 Uij ? ? C(3) -0.160(1) 0.2353(9) 0.657(2) 0.0888 Uij ? ? C(4) 0.0638(9) 0.2630(6) 0.711(1) 0.0425 Uij ? ? C(5) 0.1505(9) 0.4693(6) 0.765(1) 0.0438 Uij ? ? C(6) 0.1374(10) 0.5296(6) 0.880(1) 0.0475 Uij ? ? C(7) 0.261(1) 0.5275(7) 1.118(1) 0.0662 Uij ? ? C(8) 0.3101(9) 0.3993(5) 0.925(1) 0.0400 Uij ? ? C(9) 0.4659(10) 0.3858(6) 0.487(1) 0.0495 Uij ? ? C(10) 0.579(1) 0.3622(7) 0.362(1) 0.0573 Uij ? ? C(11) 0.7239(10) 0.2125(8) 0.221(1) 0.0664 Uij ? ? C(12) 0.5161(9) 0.2316(6) 0.4559(10) 0.0416 Uij ? ? B(1) 0.305(1) 0.2963(7) 0.692(1) 0.036(2) Uij ? ? H(1) 0.338(7) 0.248(5) 0.774(8) 0.02(1) Uij ? ? H(2) 0.2198 0.3270 0.3660 0.0679 Uij ? ? H(3) -0.0049 0.2926 0.3505 0.0840 Uij ? ? H(4) -0.2039 0.2409 0.5616 0.1069 Uij ? ? H(5) -0.2231 0.2754 0.7387 0.1069 Uij ? ? H(6) -0.1392 0.1712 0.6995 0.1069 Uij ? ? H(7) 0.0943 0.4814 0.6801 0.0509 Uij ? ? H(8) 0.0727 0.5913 0.8914 0.0552 Uij ? ? H(9) 0.2867 0.5840 1.0806 0.0770 Uij ? ? H(10) 0.3327 0.4840 1.1681 0.0770 Uij ? ? H(11) 0.1731 0.5428 1.1978 0.0770 Uij ? ? H(12) 0.4213 0.4468 0.5275 0.0578 Uij ? ? H(13) 0.6273 0.4051 0.2985 0.0661 Uij ? ? H(14) 0.7841 0.1619 0.2781 0.0779 Uij ? ? H(15) 0.7778 0.2510 0.1576 0.0779 Uij ? ? H(16) 0.6821 0.1864 0.1500 0.0779 Uij ? ? 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 S(1) 0.046(1) 0.058(2) 0.055(2) -0.015(1) 0.011(1) -0.003(1) S(2) 0.072(2) 0.055(2) 0.075(2) -0.005(1) -0.038(2) -0.012(1) S(3) 0.078(2) 0.042(1) 0.050(2) -0.017(1) 0.009(1) -0.014(1) Na(2) 0.063(6) 0.125(9) 0.108(8) -0.014(6) -0.001(6) -0.028(7) O(1) 0.064(5) 0.079(5) 0.068(5) -0.009(4) -0.011(4) -0.002(4) O(2) 0.138(8) 0.081(6) 0.066(5) -0.027(5) -0.006(5) -0.003(4) O(3) 0.122(7) 0.080(6) 0.089(6) -0.030(5) 0.000(5) -0.031(5) N(1) 0.039(4) 0.036(4) 0.038(4) -0.014(3) -0.002(3) -0.005(3) N(2) 0.048(5) 0.059(5) 0.074(6) -0.022(4) -0.014(4) -0.010(4) N(3) 0.037(4) 0.035(4) 0.037(4) -0.012(3) 0.000(3) -0.004(3) N(4) 0.054(5) 0.036(4) 0.043(4) -0.015(3) -0.005(4) -0.008(3) N(5) 0.041(4) 0.032(3) 0.041(4) -0.016(3) 0.002(3) -0.008(3) N(6) 0.039(4) 0.064(5) 0.034(4) -0.019(4) 0.003(3) -0.007(4) C(1) 0.062(7) 0.070(7) 0.043(6) -0.027(5) -0.011(5) 0.001(5) C(2) 0.073(8) 0.095(9) 0.057(7) -0.034(7) -0.029(6) 0.000(6) C(3) 0.051(7) 0.100(9) 0.13(1) -0.037(7) -0.011(7) -0.036(8) C(4) 0.040(5) 0.034(4) 0.051(6) -0.010(4) -0.001(4) -0.007(4) C(5) 0.045(5) 0.036(5) 0.046(5) -0.006(4) -0.006(4) -0.004(4) C(6) 0.050(5) 0.034(4) 0.052(6) -0.009(4) 0.000(5) -0.004(4) C(7) 0.086(8) 0.054(6) 0.061(7) -0.016(6) -0.015(6) -0.023(5) C(8) 0.045(5) 0.026(4) 0.047(5) -0.008(4) -0.004(4) -0.007(4) C(9) 0.056(6) 0.041(5) 0.053(6) -0.023(4) 0.004(5) -0.013(4) C(10) 0.065(7) 0.063(6) 0.052(6) -0.039(5) 0.005(5) -0.005(5) C(11) 0.042(6) 0.096(8) 0.049(6) -0.012(6) 0.010(5) -0.009(6) C(12) 0.041(5) 0.053(5) 0.034(5) -0.017(4) -0.004(4) -0.006(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2299 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0712 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0914 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.449 _refine_ls_shift/esd_max 1.3850 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.49 _refine_diff_density_max 0.54 #------------------------------------------------------------------------------ _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 S(1) C(4) 1.706(9) ? ? yes S(2) C(8) 1.696(9) ? ? yes S(3) C(12) 1.696(9) ? ? yes Na(2) Na(3) 2.915(10) ? ? yes Na(2) Na(4) 2.49(2) ? ? yes Na(2) Na(4) 3.34(2) ? ? yes Na(2) O(1) 2.46(1) ? ? yes Na(2) O(2) 2.32(1) ? ? yes Na(2) O(3) 2.39(1) ? ? yes Na(2) O(8) 2.39(1) ? ? yes Na(2) O(9) 2.09(2) ? ? yes Na(3) Na(4) 0.44(1) ? ? yes Na(3) Na(4) 0.44(1) ? ? yes Na(3) O(1) 2.399(7) ? ? yes Na(3) O(1) 2.399(7) ? ? yes Na(3) O(2) 2.443(9) ? ? yes Na(3) O(2) 2.443(9) ? ? yes Na(3) O(3) 2.402(8) ? ? yes Na(3) O(3) 2.402(8) ? ? yes Na(4) Na(4) 0.87(3) ? ? yes Na(4) O(1) 2.19(1) ? ? yes Na(4) O(1) 2.66(1) ? ? yes Na(4) O(2) 2.12(2) ? ? yes Na(4) O(3) 2.24(1) ? ? yes Na(4) O(3) 2.63(1) ? ? yes O(9) O(10) 1.29(3) ? ? yes N(1) C(1) 1.38(1) ? ? yes N(1) C(4) 1.352(10) ? ? yes N(1) B(1) 1.55(1) ? ? yes N(2) C(2) 1.37(1) ? ? yes N(2) C(3) 1.49(1) ? ? yes N(2) C(4) 1.35(1) ? ? yes N(3) C(5) 1.396(10) ? ? yes N(3) C(8) 1.37(1) ? ? yes N(3) B(1) 1.54(1) ? ? yes N(4) C(6) 1.38(1) ? ? yes N(4) C(7) 1.45(1) ? ? yes N(4) C(8) 1.338(9) ? ? yes N(5) C(9) 1.37(1) ? ? yes N(5) C(12) 1.352(10) ? ? yes N(5) B(1) 1.55(1) ? ? yes N(6) C(10) 1.35(1) ? ? yes N(6) C(11) 1.46(1) ? ? yes N(6) C(12) 1.36(1) ? ? yes C(1) C(2) 1.35(1) ? ? yes C(1) H(2) 0.953 ? ? no C(2) H(3) 0.947 ? ? no C(3) H(4) 0.956 ? ? no C(3) H(5) 0.946 ? ? no C(3) H(6) 0.950 ? ? no C(5) C(6) 1.33(1) ? ? yes C(5) H(7) 0.954 ? ? no C(6) H(8) 0.949 ? ? no C(7) H(9) 0.947 ? ? no C(7) H(10) 0.941 ? ? no C(7) H(11) 0.961 ? ? no C(9) C(10) 1.34(1) ? ? yes C(9) H(12) 0.945 ? ? no C(10) H(13) 0.952 ? ? no C(11) H(14) 0.953 ? ? no C(11) H(15) 0.941 ? ? no C(11) H(16) 0.954 ? ? no B(1) H(1) 0.96(6) ? ? 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 Na(3) Na(2) Na(4) 2.3(2) ? ? ? yes Na(3) Na(2) Na(4) 1.7(2) ? ? ? yes Na(3) Na(2) O(1) 52.2(2) ? ? ? yes Na(3) Na(2) O(2) 54.2(3) ? ? ? yes Na(3) Na(2) O(3) 52.7(3) ? ? ? yes Na(3) Na(2) O(8) 139.3(4) ? ? ? yes Na(3) Na(2) O(9) 131.3(8) ? ? ? yes Na(4) Na(2) Na(4) 4.0(4) ? ? ? yes Na(4) Na(2) O(1) 52.5(4) ? ? ? yes Na(4) Na(2) O(2) 52.1(4) ? ? ? yes Na(4) Na(2) O(3) 54.5(4) ? ? ? yes Na(4) Na(2) O(8) 137.0(5) ? ? ? yes Na(4) Na(2) O(9) 133.5(9) ? ? ? yes Na(4) Na(2) O(1) 52.1(3) ? ? ? yes Na(4) Na(2) O(2) 55.7(4) ? ? ? yes Na(4) Na(2) O(3) 51.4(3) ? ? ? yes Na(4) Na(2) O(8) 141.0(4) ? ? ? yes Na(4) Na(2) O(9) 129.7(8) ? ? ? yes O(1) Na(2) O(2) 87.8(4) ? ? ? yes O(1) Na(2) O(3) 88.0(4) ? ? ? yes O(1) Na(2) O(8) 119.0(5) ? ? ? yes O(1) Na(2) O(9) 101.6(8) ? ? ? yes O(2) Na(2) O(3) 86.8(5) ? ? ? yes O(2) Na(2) O(8) 88.6(4) ? ? ? yes O(2) Na(2) O(9) 170.5(9) ? ? ? yes O(3) Na(2) O(8) 152.4(6) ? ? ? yes O(3) Na(2) O(9) 92.1(8) ? ? ? yes O(8) Na(2) O(9) 88.0(8) ? ? ? yes Na(2) Na(3) Na(2) 180.0 ? ? ? yes Na(2) Na(3) Na(4) 13(1) ? ? ? yes Na(2) Na(3) Na(4) 166(1) ? ? ? yes Na(2) Na(3) O(1) 54.0(3) ? ? ? yes Na(2) Na(3) O(1) 126.0(3) ? ? ? yes Na(2) Na(3) O(2) 50.4(3) ? ? ? yes Na(2) Na(3) O(2) 129.6(3) ? ? ? yes Na(2) Na(3) O(3) 52.4(3) ? ? ? yes Na(2) Na(3) O(3) 127.6(3) ? ? ? yes Na(2) Na(3) Na(4) 166(1) ? ? ? yes Na(2) Na(3) Na(4) 13(1) ? ? ? yes Na(2) Na(3) O(1) 126.0(3) ? ? ? yes Na(2) Na(3) O(1) 54.0(3) ? ? ? yes Na(2) Na(3) O(2) 129.6(3) ? ? ? yes Na(2) Na(3) O(2) 50.4(3) ? ? ? yes Na(2) Na(3) O(3) 127.6(3) ? ? ? yes Na(2) Na(3) O(3) 52.4(3) ? ? ? yes Na(4) Na(3) Na(4) 180.0 ? ? ? yes Na(4) Na(3) O(1) 56(1) ? ? ? yes Na(4) Na(3) O(1) 123(1) ? ? ? yes Na(4) Na(3) O(2) 38(1) ? ? ? yes Na(4) Na(3) O(2) 141(1) ? ? ? yes Na(4) Na(3) O(3) 63(1) ? ? ? yes Na(4) Na(3) O(3) 116(1) ? ? ? yes Na(4) Na(3) O(1) 123(1) ? ? ? yes Na(4) Na(3) O(1) 56(1) ? ? ? yes Na(4) Na(3) O(2) 141(1) ? ? ? yes Na(4) Na(3) O(2) 38(1) ? ? ? yes Na(4) Na(3) O(3) 116(1) ? ? ? yes Na(4) Na(3) O(3) 63(1) ? ? ? yes O(1) Na(3) O(1) 180.0 ? ? ? yes O(1) Na(3) O(2) 86.4(3) ? ? ? yes O(1) Na(3) O(2) 93.6(3) ? ? ? yes O(1) Na(3) O(3) 89.2(3) ? ? ? yes O(1) Na(3) O(3) 90.8(3) ? ? ? yes O(1) Na(3) O(2) 93.6(3) ? ? ? yes O(1) Na(3) O(2) 86.4(3) ? ? ? yes O(1) Na(3) O(3) 90.8(3) ? ? ? yes O(1) Na(3) O(3) 89.2(3) ? ? ? yes O(2) Na(3) O(2) 180.0 ? ? ? yes O(2) Na(3) O(3) 84.0(3) ? ? ? yes O(2) Na(3) O(3) 96.0(3) ? ? ? yes O(2) Na(3) O(3) 96.0(3) ? ? ? yes O(2) Na(3) O(3) 84.0(3) ? ? ? yes O(3) Na(3) O(3) 180.0 ? ? ? yes Na(2) Na(4) Na(2) 176.0(4) ? ? ? yes Na(2) Na(4) Na(3) 164(1) ? ? ? yes Na(2) Na(4) Na(4) 164(1) ? ? ? yes Na(2) Na(4) O(1) 62.9(5) ? ? ? yes Na(2) Na(4) O(1) 133.5(5) ? ? ? yes Na(2) Na(4) O(2) 59.8(5) ? ? ? yes Na(2) Na(4) O(3) 60.5(5) ? ? ? yes Na(2) Na(4) O(3) 137.7(6) ? ? ? yes Na(2) Na(4) Na(3) 11(1) ? ? ? yes Na(2) Na(4) Na(4) 11(1) ? ? ? yes Na(2) Na(4) O(1) 116.5(5) ? ? ? yes Na(2) Na(4) O(1) 46.6(3) ? ? ? yes Na(2) Na(4) O(2) 123.8(5) ? ? ? yes Na(2) Na(4) O(3) 116.3(5) ? ? ? yes Na(2) Na(4) O(3) 45.3(3) ? ? ? yes Na(3) Na(4) Na(4) 0.0 ? ? ? yes Na(3) Na(4) O(1) 114(1) ? ? ? yes Na(3) Na(4) O(1) 48(1) ? ? ? yes Na(3) Na(4) O(2) 133(1) ? ? ? yes Na(3) Na(4) O(3) 106(1) ? ? ? yes Na(3) Na(4) O(3) 54(1) ? ? ? yes Na(4) Na(4) O(1) 114(1) ? ? ? yes Na(4) Na(4) O(1) 48(1) ? ? ? yes Na(4) Na(4) O(2) 133(1) ? ? ? yes Na(4) Na(4) O(3) 106(1) ? ? ? yes Na(4) Na(4) O(3) 54(1) ? ? ? yes O(1) Na(4) O(1) 162.6(6) ? ? ? yes O(1) Na(4) O(2) 100.6(6) ? ? ? yes O(1) Na(4) O(3) 99.1(5) ? ? ? yes O(1) Na(4) O(3) 90.0(4) ? ? ? yes O(1) Na(4) O(2) 94.3(5) ? ? ? yes O(1) Na(4) O(3) 88.0(4) ? ? ? yes O(1) Na(4) O(3) 79.1(4) ? ? ? yes O(2) Na(4) O(3) 96.0(6) ? ? ? yes O(2) Na(4) O(3) 98.1(5) ? ? ? yes O(3) Na(4) O(3) 161.5(6) ? ? ? yes Na(2) O(1) Na(3) 73.8(3) ? ? ? yes Na(2) O(1) Na(4) 64.6(5) ? ? ? yes Na(2) O(1) Na(4) 81.3(4) ? ? ? yes Na(3) O(1) Na(4) 9.5(4) ? ? ? yes Na(3) O(1) Na(4) 7.8(3) ? ? ? yes Na(4) O(1) Na(4) 17.4(6) ? ? ? yes Na(2) O(2) Na(3) 75.4(4) ? ? ? yes Na(2) O(2) Na(4) 68.1(5) ? ? ? yes Na(3) O(2) Na(4) 7.4(3) ? ? ? yes Na(2) O(3) Na(3) 74.9(3) ? ? ? yes Na(2) O(3) Na(4) 65.0(5) ? ? ? yes Na(2) O(3) Na(4) 83.3(4) ? ? ? yes Na(3) O(3) Na(4) 10.0(4) ? ? ? yes Na(3) O(3) Na(4) 8.5(3) ? ? ? yes Na(4) O(3) Na(4) 18.5(6) ? ? ? yes Na(2) O(8) Na(2) 180.0000(1) ? ? ? yes Na(2) O(9) O(10) 105(2) ? ? ? yes C(1) N(1) C(4) 108.2(7) ? ? ? yes C(1) N(1) B(1) 127.8(7) ? ? ? yes C(4) N(1) B(1) 123.9(7) ? ? ? yes C(2) N(2) C(3) 126.5(9) ? ? ? yes C(2) N(2) C(4) 109.2(8) ? ? ? yes C(3) N(2) C(4) 124.2(9) ? ? ? yes C(5) N(3) C(8) 106.4(6) ? ? ? yes C(5) N(3) B(1) 127.0(7) ? ? ? yes C(8) N(3) B(1) 126.6(7) ? ? ? yes C(6) N(4) C(7) 124.8(7) ? ? ? yes C(6) N(4) C(8) 109.9(7) ? ? ? yes C(7) N(4) C(8) 125.2(8) ? ? ? yes C(9) N(5) C(12) 108.7(7) ? ? ? yes C(9) N(5) B(1) 126.3(7) ? ? ? yes C(12) N(5) B(1) 125.0(6) ? ? ? yes C(10) N(6) C(11) 126.7(8) ? ? ? yes C(10) N(6) C(12) 109.5(7) ? ? ? yes C(11) N(6) C(12) 123.8(8) ? ? ? yes N(1) C(1) C(2) 108.0(9) ? ? ? yes N(1) C(1) H(2) 125.8 ? ? ? no C(2) C(1) H(2) 126.1 ? ? ? no N(2) C(2) C(1) 107.2(9) ? ? ? yes N(2) C(2) H(3) 126.4 ? ? ? no C(1) C(2) H(3) 126.3 ? ? ? no N(2) C(3) H(4) 109.2 ? ? ? no N(2) C(3) H(5) 109.7 ? ? ? no N(2) C(3) H(6) 109.8 ? ? ? no H(4) C(3) H(5) 109.4 ? ? ? no H(4) C(3) H(6) 109.0 ? ? ? no H(5) C(3) H(6) 109.8 ? ? ? no S(1) C(4) N(1) 126.9(7) ? ? ? yes S(1) C(4) N(2) 125.8(7) ? ? ? yes N(1) C(4) N(2) 107.3(8) ? ? ? yes N(3) C(5) C(6) 109.4(8) ? ? ? yes N(3) C(5) H(7) 125.8 ? ? ? no C(6) C(5) H(7) 124.8 ? ? ? no N(4) C(6) C(5) 106.6(7) ? ? ? yes N(4) C(6) H(8) 126.4 ? ? ? no C(5) C(6) H(8) 127.0 ? ? ? no N(4) C(7) H(9) 109.6 ? ? ? no N(4) C(7) H(10) 109.9 ? ? ? no N(4) C(7) H(11) 108.7 ? ? ? no H(9) C(7) H(10) 110.5 ? ? ? no H(9) C(7) H(11) 108.8 ? ? ? no H(10) C(7) H(11) 109.3 ? ? ? no S(2) C(8) N(3) 127.0(6) ? ? ? yes S(2) C(8) N(4) 125.3(7) ? ? ? yes N(3) C(8) N(4) 107.7(7) ? ? ? yes N(5) C(9) C(10) 107.7(8) ? ? ? yes N(5) C(9) H(12) 126.0 ? ? ? no C(10) C(9) H(12) 126.3 ? ? ? no N(6) C(10) C(9) 107.7(8) ? ? ? yes N(6) C(10) H(13) 126.7 ? ? ? no C(9) C(10) H(13) 125.5 ? ? ? no N(6) C(11) H(14) 108.9 ? ? ? no N(6) C(11) H(15) 110.1 ? ? ? no N(6) C(11) H(16) 109.0 ? ? ? no H(14) C(11) H(15) 110.0 ? ? ? no H(14) C(11) H(16) 108.9 ? ? ? no H(15) C(11) H(16) 109.9 ? ? ? no S(3) C(12) N(5) 127.2(6) ? ? ? yes S(3) C(12) N(6) 126.5(6) ? ? ? yes N(5) C(12) N(6) 106.3(7) ? ? ? yes N(1) B(1) N(3) 108.7(7) ? ? ? yes N(1) B(1) N(5) 108.6(7) ? ? ? yes N(1) B(1) H(1) 117(3) ? ? ? no N(3) B(1) N(5) 108.7(6) ? ? ? yes N(3) B(1) H(1) 101(3) ? ? ? no N(5) B(1) H(1) 111(3) ? ? ? no #-------------------------------------------------------------------------- _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME 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_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_NaTp #------------------------------------------------------------------------------ _audit_creation_date 'Fri Sep 18 11:16:07 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.508(2) _cell_length_b 20.730(3) _cell_length_c 7.062(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1245.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _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' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourlessprism' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 254.03 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H12 B N6 Na O ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 528.00 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.813 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.04 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 1692 _reflns_number_total 1692 _reflns_number_observed 1212 _reflns_observed_criterion 1.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.11273 _diffrn_orient_matrix_UB_12 0.01346 _diffrn_orient_matrix_UB_13 -0.00715 _diffrn_orient_matrix_UB_21 -0.03204 _diffrn_orient_matrix_UB_22 -0.04614 _diffrn_orient_matrix_UB_23 -0.01472 _diffrn_orient_matrix_UB_31 -0.00906 _diffrn_orient_matrix_UB_32 -0.00411 _diffrn_orient_matrix_UB_33 0.14066 #------------------------------------------------------------------------------ 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 36 0.003 0.002 'International Tables' H 0 48 0.000 0.000 'International Tables' B 0 4 0.001 0.001 'International Tables' N 0 24 0.006 0.003 'International Tables' Na 0 4 0.036 0.025 'International Tables' O 0 4 0.011 0.006 'International Tables' #------------------------------------------------------------------------------ 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 Na(1) 0.7538(2) -0.00492(9) 0.0728(2) 0.0453(4) Uij ? ? O(1) 0.9120(3) 0.0399(1) -0.1738(5) 0.0494(8) Uij ? ? N(1) 0.8398(4) 0.1245(2) 0.3497(5) 0.0381(9) Uij ? ? N(2) 0.7294(4) 0.1020(2) 0.2260(5) 0.047(1) Uij ? ? N(3) 1.0529(4) 0.0431(1) 0.2768(5) 0.0339(8) Uij ? ? N(4) 0.9701(4) -0.0054(2) 0.3620(5) 0.0403(9) Uij ? ? N(5) 1.0851(4) 0.1565(2) 0.1624(6) 0.0402(9) Uij ? ? N(6) 1.0443(4) 0.1502(2) -0.0231(5) 0.045(1) Uij ? ? C(1) 0.7719(6) 0.1616(2) 0.4813(7) 0.051(1) Uij ? ? C(2) 0.6136(6) 0.1641(2) 0.4471(8) 0.058(1) Uij ? ? C(3) 0.5935(5) 0.1264(2) 0.2889(8) 0.055(1) Uij ? ? C(4) 1.0399(5) -0.0598(2) 0.3041(7) 0.044(1) Uij ? ? C(5) 1.1669(5) -0.0474(2) 0.1871(7) 0.050(1) Uij ? ? C(6) 1.1706(5) 0.0184(2) 0.1740(7) 0.046(1) Uij ? ? C(7) 1.1902(6) 0.2045(2) 0.1795(8) 0.058(1) Uij ? ? C(8) 1.2171(7) 0.2306(2) 0.0057(10) 0.073(2) Uij ? ? C(9) 1.1246(6) 0.1952(2) -0.1140(7) 0.055(1) Uij ? ? B(1) 1.0182(5) 0.1148(2) 0.3223(8) 0.036(1) Uij ? ? H(1) 1.0783 0.1279 0.4533 0.0805 Uij ? ? H(2) 0.8250 0.1828 0.5821 0.0614 Uij ? ? H(3) 0.5356 0.1867 0.5170 0.0693 Uij ? ? H(4) 0.4946 0.1187 0.2307 0.0663 Uij ? ? H(5) 1.0062 -0.1019 0.3390 0.0525 Uij ? ? H(6) 1.2357 -0.0777 0.1292 0.0594 Uij ? ? H(7) 1.2449 0.0426 0.1031 0.0547 Uij ? ? H(8) 1.2381 0.2180 0.2944 0.0701 Uij ? ? H(9) 1.2845 0.2656 -0.0254 0.0876 Uij ? ? H(10) 1.1188 0.2022 -0.2470 0.0658 Uij ? ? H(11) 0.9979 0.0152 -0.1943 0.0805 Uij ? ? H(12) 0.9605 0.0773 -0.1254 0.0805 Uij ? ? 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 Na(1) 0.0469(9) 0.0559(10) 0.0332(7) -0.0053(8) 0.0052(8) 0.0006(8) O(1) 0.046(2) 0.057(2) 0.045(2) -0.012(2) 0.000(2) -0.014(2) N(1) 0.037(2) 0.038(2) 0.039(2) 0.006(2) -0.001(2) -0.005(2) N(2) 0.036(2) 0.050(2) 0.056(2) 0.003(2) -0.003(2) -0.011(2) N(3) 0.029(2) 0.037(2) 0.036(2) 0.005(1) -0.001(2) -0.001(2) N(4) 0.038(2) 0.042(2) 0.042(2) -0.001(2) 0.004(2) 0.004(2) N(5) 0.035(2) 0.039(2) 0.046(2) -0.006(2) -0.006(2) -0.005(2) N(6) 0.046(2) 0.048(2) 0.042(2) -0.010(2) -0.005(2) 0.003(2) C(1) 0.058(3) 0.049(3) 0.046(3) 0.010(2) 0.004(2) -0.011(2) C(2) 0.050(3) 0.066(3) 0.058(3) 0.019(3) 0.013(3) 0.000(3) C(3) 0.038(2) 0.059(3) 0.068(4) 0.005(2) -0.003(3) -0.002(3) C(4) 0.049(2) 0.037(2) 0.045(3) 0.005(2) -0.005(2) -0.003(2) C(5) 0.045(2) 0.058(3) 0.046(2) 0.022(2) 0.000(2) -0.009(3) C(6) 0.034(2) 0.061(3) 0.042(2) 0.007(2) 0.005(2) -0.003(2) C(7) 0.054(3) 0.048(3) 0.073(3) -0.016(2) -0.013(3) -0.010(3) C(8) 0.070(4) 0.061(3) 0.088(4) -0.031(3) 0.000(4) 0.008(3) C(9) 0.060(3) 0.047(3) 0.057(3) -0.007(2) 0.004(3) 0.009(2) B(1) 0.033(2) 0.035(2) 0.041(2) 0.003(2) -0.002(2) -0.004(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 21.81855 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1212 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0455 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0432 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.618 _refine_ls_shift/esd_max 0.0080 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.21 _refine_diff_density_max 0.20 #------------------------------------------------------------------------------ _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 Na(1) O(1) 2.392(4) ? ? yes Na(1) O(1) 2.389(4) ? ? yes Na(1) N(2) 2.476(4) ? ? yes Na(1) N(4) 2.427(4) ? ? yes Na(1) N(4) 2.749(4) ? ? yes N(1) N(2) 1.365(5) ? ? yes N(1) C(1) 1.337(5) ? ? yes N(1) B(1) 1.543(5) ? ? yes N(2) C(3) 1.338(6) ? ? yes N(3) N(4) 1.366(4) ? ? yes N(3) C(6) 1.339(5) ? ? yes N(3) B(1) 1.549(5) ? ? yes N(4) C(4) 1.339(5) ? ? yes N(5) N(6) 1.362(5) ? ? yes N(5) C(7) 1.343(5) ? ? yes N(5) B(1) 1.532(6) ? ? yes N(6) C(9) 1.324(5) ? ? yes C(1) C(2) 1.369(7) ? ? yes C(2) C(3) 1.374(7) ? ? yes C(4) C(5) 1.384(6) ? ? yes C(5) C(6) 1.367(6) ? ? yes C(7) C(8) 1.361(8) ? ? yes C(8) C(9) 1.367(7) ? ? yes #------------------------------------------------------------------------------ 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 O(1) Na(1) O(1) 174.73(10) ? ? ? yes O(1) Na(1) N(2) 84.0(1) ? ? ? yes O(1) Na(1) N(4) 91.3(1) ? ? ? yes O(1) Na(1) N(4) 80.7(1) ? ? ? yes O(1) Na(1) N(2) 91.0(1) ? ? ? yes O(1) Na(1) N(4) 87.8(1) ? ? ? yes O(1) Na(1) N(4) 99.5(1) ? ? ? yes N(2) Na(1) N(4) 97.1(1) ? ? ? yes N(2) Na(1) N(4) 74.6(1) ? ? ? yes N(4) Na(1) N(4) 168.9(1) ? ? ? yes Na(1) O(1) Na(1) 95.46(10) ? ? ? yes N(2) N(1) C(1) 110.1(3) ? ? ? yes N(2) N(1) B(1) 123.5(4) ? ? ? yes C(1) N(1) B(1) 126.0(4) ? ? ? yes Na(1) N(2) N(1) 121.9(2) ? ? ? yes Na(1) N(2) C(3) 123.8(3) ? ? ? yes N(1) N(2) C(3) 104.6(4) ? ? ? yes N(4) N(3) C(6) 110.1(3) ? ? ? yes N(4) N(3) B(1) 121.0(3) ? ? ? yes C(6) N(3) B(1) 128.5(3) ? ? ? yes Na(1) N(4) Na(1) 85.97(10) ? ? ? yes Na(1) N(4) N(3) 127.6(2) ? ? ? yes Na(1) N(4) C(4) 127.5(3) ? ? ? yes Na(1) N(4) N(3) 90.9(2) ? ? ? yes Na(1) N(4) C(4) 94.2(3) ? ? ? yes N(3) N(4) C(4) 104.9(3) ? ? ? yes N(6) N(5) C(7) 109.1(4) ? ? ? yes N(6) N(5) B(1) 124.1(3) ? ? ? yes C(7) N(5) B(1) 126.8(4) ? ? ? yes N(5) N(6) C(9) 105.5(4) ? ? ? yes N(1) C(1) C(2) 108.9(4) ? ? ? yes C(1) C(2) C(3) 104.2(4) ? ? ? yes N(2) C(3) C(2) 112.2(4) ? ? ? yes N(4) C(4) C(5) 111.8(4) ? ? ? yes C(4) C(5) C(6) 104.1(4) ? ? ? yes N(3) C(6) C(5) 109.1(4) ? ? ? yes N(5) C(7) C(8) 109.0(5) ? ? ? yes C(7) C(8) C(9) 104.3(4) ? ? ? yes N(6) C(9) C(8) 112.1(5) ? ? ? yes N(1) B(1) N(3) 109.8(3) ? ? ? yes N(1) B(1) N(5) 112.6(4) ? ? ? yes N(3) B(1) N(5) 108.6(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME 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_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;