data_s280 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 B F4 N5 O2 S' _chemical_formula_weight 303.06 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 24.375(1) _cell_length_b 30.163(2) _cell_length_c 13.653(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10038.0(11) _cell_formula_units_Z 32 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 11852 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 23.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4928 _exptl_absorpt_coefficient_mu 0.313 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi- and omega-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9666 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 21.00 _reflns_number_total 2699 _reflns_number_gt 2010 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement ? _computing_data_reduction 'DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Small crystal with low diffraction, only reflections until 2theta of 44 degrees were used. Two molecules in the asymmetric unit. One BF4-anion, on a general position, is disordered with a refined ratio (use of free varible) of 2:1 for the flurine atoms F1-F4 and F1A-F4A. The borone atoms of the the other anions lie on a twofold rotation axis, B2 and B3. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0901P)^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 constr _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 0.16(17) _refine_ls_number_reflns 2699 _refine_ls_number_parameters 383 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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 S1 S 0.17029(8) -0.11906(7) 0.24803(14) 0.0559(6) Uani 1 1 d . . . S2 S 0.15984(10) 0.12864(8) 0.9926(2) 0.0716(7) Uani 1 1 d . . . O1 O 0.2020(2) -0.10683(19) 0.3307(4) 0.0638(16) Uani 1 1 d . . . O2 O 0.1205(2) -0.09867(18) 0.2240(5) 0.076(2) Uani 1 1 d . . . O3 O 0.1849(3) 0.1457(2) 0.9086(5) 0.090(2) Uani 1 1 d . . . O4 O 0.1101(3) 0.1446(2) 1.0313(6) 0.102(3) Uani 1 1 d . . . N1 N 0.1563(2) -0.17367(18) 0.2684(4) 0.0422(15) Uani 1 1 d . . . N2 N 0.1289(2) -0.24057(19) 0.2478(6) 0.0498(16) Uani 1 1 d . . . N3 N 0.2056(3) -0.1207(2) 0.1462(5) 0.065(2) Uani 1 1 d . . . N4 N 0.2562(4) -0.1242(2) 0.1602(5) 0.064(2) Uani 1 1 d . . . N5 N 0.3019(4) -0.1272(3) 0.1638(8) 0.096(3) Uani 1 1 d . . . N6 N 0.1510(3) 0.0738(2) 0.9666(5) 0.0607(19) Uani 1 1 d . . . N7 N 0.1293(3) 0.0057(2) 0.9807(7) 0.0567(19) Uani 1 1 d . . . N8 N 0.1991(4) 0.1279(2) 1.0929(6) 0.077(2) Uani 1 1 d . . . N9 N 0.2477(4) 0.1256(2) 1.0752(6) 0.074(3) Uani 1 1 d . . . N10 N 0.2930(5) 0.1229(3) 1.0664(7) 0.103(3) Uani 1 1 d . . . C1 C 0.1256(3) -0.1998(3) 0.2091(5) 0.046(2) Uani 1 1 d . . . C2 C 0.1790(3) -0.1983(3) 0.3457(5) 0.054(2) Uani 1 1 d . . . H2 H 0.2017 -0.1881 0.3966 0.064 Uiso 1 1 calc . . . C3 C 0.1612(4) -0.2384(3) 0.3305(7) 0.065(2) Uani 1 1 d . . . H3 H 0.1694 -0.2627 0.3708 0.079 Uiso 1 1 calc . . . C4 C 0.0954(4) -0.1873(3) 0.1224(6) 0.063(2) Uani 1 1 d . . . H4A H 0.0965 -0.2120 0.0757 0.075 Uiso 1 1 calc . . . H4B H 0.1137 -0.1619 0.0917 0.075 Uiso 1 1 calc . . . C5 C 0.0352(4) -0.1751(4) 0.1423(8) 0.094(3) Uani 1 1 d . . . H5A H 0.0177 -0.1663 0.0816 0.142 Uiso 1 1 calc . . . H5B H 0.0337 -0.1508 0.1887 0.142 Uiso 1 1 calc . . . H5C H 0.0162 -0.2006 0.1694 0.142 Uiso 1 1 calc . . . C6 C 0.1035(4) -0.2802(3) 0.2060(7) 0.079(3) Uani 1 1 d . . . H6A H 0.0963 -0.2754 0.1369 0.119 Uiso 1 1 calc R . . H6B H 0.0692 -0.2862 0.2396 0.119 Uiso 1 1 calc R . . H6C H 0.1280 -0.3053 0.2137 0.119 Uiso 1 1 calc R . . C7 C 0.1256(3) 0.0441(3) 1.0238(5) 0.052(3) Uani 1 1 d . . . C8 C 0.1723(4) 0.0529(3) 0.8853(6) 0.061(2) Uani 1 1 d . . . H8 H 0.1926 0.0660 0.8344 0.073 Uiso 1 1 calc . . . C9 C 0.1583(3) 0.0102(3) 0.8930(7) 0.062(2) Uani 1 1 d . . . H9 H 0.1664 -0.0125 0.8480 0.074 Uiso 1 1 calc . . . C10 C 0.0959(4) 0.0511(3) 1.1211(6) 0.065(2) Uani 1 1 d . . . H10A H 0.0990 0.0243 1.1612 0.079 Uiso 1 1 calc . . . H10B H 0.1132 0.0756 1.1568 0.079 Uiso 1 1 calc . . . C11 C 0.0354(4) 0.0617(4) 1.1041(9) 0.107(4) Uani 1 1 d . . . H11A H 0.0171 0.0650 1.1667 0.161 Uiso 1 1 calc . . . H11B H 0.0185 0.0378 1.0674 0.161 Uiso 1 1 calc . . . H11C H 0.0323 0.0891 1.0674 0.161 Uiso 1 1 calc . . . C12 C 0.1112(4) -0.0375(3) 1.0128(8) 0.087(3) Uani 1 1 d . . . H12A H 0.0728 -0.0361 1.0316 0.130 Uiso 1 1 calc R . . H12B H 0.1330 -0.0469 1.0685 0.130 Uiso 1 1 calc R . . H12C H 0.1155 -0.0587 0.9598 0.130 Uiso 1 1 calc R . . B1 B 0.2485(5) -0.0010(4) 0.6593(10) 0.066(3) Uani 1 1 d . . . B2 B 0.2500 0.2500 0.5965(12) 0.066(5) Uani 1 2 d S . . B3 B 0.2500 0.2500 1.0752(14) 0.058(4) Uani 1 2 d S . . F5 F 0.2048(3) 0.2482(3) 0.5470(6) 0.156(4) Uani 1 1 d . . . F6 F 0.2495(3) 0.2154(2) 0.6573(8) 0.159(3) Uani 1 1 d . . . F7 F 0.2134(4) 0.2275(2) 1.0265(6) 0.177(4) Uani 1 1 d . . . F8 F 0.2264(4) 0.2798(3) 1.1302(9) 0.205(6) Uani 1 1 d . . . F1 F 0.2963(5) 0.0114(5) 0.7024(15) 0.115(6) Uani 0.657(18) 1 d P A 1 F2 F 0.2206(8) -0.0342(5) 0.7033(13) 0.142(6) Uani 0.657(18) 1 d P A 1 F3 F 0.2608(4) -0.0179(6) 0.5670(9) 0.118(6) Uani 0.657(18) 1 d P A 1 F4 F 0.2148(4) 0.0342(3) 0.6496(13) 0.100(5) Uani 0.657(18) 1 d P A 1 F1A F 0.2680(14) 0.0161(9) 0.7424(15) 0.105(9) Uani 0.343(18) 1 d P A 2 F2A F 0.1974(7) -0.0112(15) 0.6895(18) 0.128(17) Uani 0.343(18) 1 d P A 2 F3A F 0.2779(10) -0.0365(6) 0.637(2) 0.110(9) Uani 0.343(18) 1 d P A 2 F4A F 0.2460(11) 0.0276(7) 0.5767(15) 0.092(10) Uani 0.343(18) 1 d P A 2 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 S1 0.0695(13) 0.0389(12) 0.0593(14) -0.0042(10) 0.0072(15) 0.0007(12) S2 0.0829(16) 0.0483(14) 0.0835(18) 0.0018(13) -0.0146(18) -0.0015(12) O1 0.068(4) 0.057(4) 0.066(4) -0.016(3) 0.004(3) -0.007(3) O2 0.067(4) 0.053(4) 0.107(6) 0.007(4) 0.013(4) 0.020(3) O3 0.118(5) 0.060(4) 0.093(5) 0.026(4) 0.010(4) -0.010(4) O4 0.117(6) 0.055(5) 0.132(7) -0.010(4) 0.032(5) 0.014(4) N1 0.051(4) 0.034(4) 0.042(4) 0.000(3) -0.001(3) 0.002(3) N2 0.061(4) 0.036(4) 0.052(3) -0.020(5) 0.008(3) -0.006(3) N3 0.072(6) 0.060(5) 0.063(5) 0.007(4) 0.005(5) 0.002(4) N4 0.087(8) 0.044(5) 0.060(5) -0.003(4) 0.018(5) -0.014(5) N5 0.064(6) 0.102(8) 0.123(8) -0.005(6) 0.018(6) -0.004(5) N6 0.065(4) 0.047(4) 0.071(5) -0.003(4) -0.007(4) -0.006(4) N7 0.042(3) 0.043(5) 0.085(6) -0.004(5) -0.012(4) -0.005(3) N8 0.076(6) 0.073(6) 0.081(6) -0.010(4) -0.004(5) -0.018(4) N9 0.071(6) 0.064(6) 0.087(7) 0.002(4) -0.008(6) -0.003(5) N10 0.119(8) 0.101(8) 0.090(7) -0.012(5) -0.020(7) 0.015(7) C1 0.033(4) 0.052(6) 0.053(6) -0.003(4) 0.002(4) 0.004(4) C2 0.066(5) 0.043(6) 0.051(5) -0.002(4) -0.007(4) 0.001(5) C3 0.075(6) 0.045(6) 0.076(6) 0.017(5) 0.004(5) 0.004(5) C4 0.069(6) 0.066(6) 0.053(5) -0.007(4) -0.009(4) 0.000(4) C5 0.086(7) 0.097(8) 0.100(7) -0.008(6) -0.020(6) 0.030(6) C6 0.092(7) 0.056(6) 0.091(7) -0.014(5) 0.006(5) -0.016(5) C7 0.048(5) 0.050(7) 0.058(6) 0.020(5) -0.008(4) -0.004(4) C8 0.075(6) 0.052(6) 0.056(6) -0.010(5) 0.008(5) -0.001(5) C9 0.045(5) 0.077(8) 0.063(5) -0.015(5) -0.002(4) 0.013(4) C10 0.074(6) 0.074(6) 0.049(5) 0.006(4) -0.001(4) -0.012(5) C11 0.074(7) 0.135(11) 0.112(8) -0.011(7) 0.029(6) 0.022(7) C12 0.092(7) 0.052(6) 0.116(8) 0.009(6) -0.027(7) -0.016(5) B1 0.069(10) 0.059(9) 0.069(9) -0.004(7) 0.001(6) -0.005(7) B2 0.067(12) 0.084(13) 0.047(8) 0.000 0.000 0.052(9) B3 0.061(10) 0.035(9) 0.080(11) 0.000 0.000 0.010(8) F5 0.066(4) 0.282(11) 0.121(5) 0.081(7) -0.026(4) -0.014(5) F6 0.186(7) 0.071(5) 0.221(8) 0.009(6) -0.126(6) 0.006(4) F7 0.260(10) 0.115(6) 0.158(7) 0.012(5) -0.131(8) -0.072(6) F8 0.168(8) 0.141(7) 0.306(14) -0.106(8) 0.139(9) -0.062(5) F1 0.074(9) 0.118(10) 0.153(14) 0.051(10) -0.048(8) -0.006(7) F2 0.159(16) 0.096(10) 0.170(12) 0.023(8) 0.065(13) -0.030(9) F3 0.079(6) 0.208(18) 0.067(7) -0.028(9) 0.022(6) -0.008(7) F4 0.087(7) 0.076(7) 0.136(12) -0.034(7) -0.012(7) 0.018(6) F1A 0.15(2) 0.112(16) 0.054(12) -0.032(11) -0.036(14) -0.045(18) F2A 0.025(10) 0.27(5) 0.085(13) -0.01(2) 0.018(8) 0.026(15) F3A 0.151(18) 0.074(13) 0.106(19) -0.016(11) 0.051(15) 0.064(12) F4A 0.16(2) 0.058(13) 0.054(13) 0.010(10) -0.066(15) -0.001(12) _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 S1 O2 1.400(6) . ? S1 O1 1.417(6) . ? S1 N3 1.636(7) . ? S1 N1 1.705(6) . ? S2 O3 1.398(7) . ? S2 O4 1.408(7) . ? S2 N8 1.670(8) . ? S2 N6 1.704(7) . ? N1 C1 1.355(9) . ? N1 C2 1.404(9) . ? N2 C1 1.341(10) . ? N2 C3 1.378(11) . ? N2 C6 1.463(10) . ? N3 N4 1.252(11) . ? N4 N5 1.118(10) . ? N6 C7 1.342(10) . ? N6 C8 1.378(10) . ? N7 C7 1.302(10) . ? N7 C9 1.397(12) . ? N7 C12 1.444(11) . ? N8 N9 1.210(11) . ? N9 N10 1.114(11) . ? C1 C4 1.444(11) . ? C2 C3 1.301(11) . ? C4 C5 1.537(12) . ? C7 C10 1.528(12) . ? C8 C9 1.338(11) . ? C10 C11 1.525(13) . ? B1 F3A 1.322(19) . ? B1 F1A 1.33(2) . ? B1 F2A 1.35(3) . ? B1 F4 1.350(15) . ? B1 F2 1.351(18) . ? B1 F1 1.357(16) . ? B1 F3 1.392(17) . ? B1 F4A 1.42(2) . ? B2 F5 1.294(10) . ? B2 F5 1.294(10) 14 ? B2 F6 1.333(12) . ? B2 F6 1.333(12) 14 ? B3 F7 1.303(11) 14 ? B3 F7 1.303(11) . ? B3 F8 1.305(12) 14 ? B3 F8 1.305(12) . ? 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 O2 S1 O1 123.1(4) . . ? O2 S1 N3 105.7(4) . . ? O1 S1 N3 113.4(3) . . ? O2 S1 N1 106.8(3) . . ? O1 S1 N1 103.3(3) . . ? N3 S1 N1 102.3(3) . . ? O3 S2 O4 123.9(5) . . ? O3 S2 N8 115.3(4) . . ? O4 S2 N8 101.1(5) . . ? O3 S2 N6 103.9(4) . . ? O4 S2 N6 107.5(4) . . ? N8 S2 N6 103.3(4) . . ? C1 N1 C2 111.1(6) . . ? C1 N1 S1 125.1(5) . . ? C2 N1 S1 123.7(5) . . ? C1 N2 C3 108.3(6) . . ? C1 N2 C6 124.7(8) . . ? C3 N2 C6 127.0(8) . . ? N4 N3 S1 113.0(7) . . ? N5 N4 N3 173.8(10) . . ? C7 N6 C8 109.6(7) . . ? C7 N6 S2 125.8(6) . . ? C8 N6 S2 124.4(6) . . ? C7 N7 C9 109.6(7) . . ? C7 N7 C12 130.1(9) . . ? C9 N7 C12 120.1(8) . . ? N9 N8 S2 113.5(8) . . ? N10 N9 N8 174.6(11) . . ? N2 C1 N1 105.3(6) . . ? N2 C1 C4 126.4(8) . . ? N1 C1 C4 128.3(8) . . ? C3 C2 N1 103.9(7) . . ? C2 C3 N2 111.5(7) . . ? C1 C4 C5 113.8(8) . . ? N7 C7 N6 107.5(7) . . ? N7 C7 C10 123.3(8) . . ? N6 C7 C10 129.2(8) . . ? C9 C8 N6 106.4(8) . . ? C8 C9 N7 106.9(8) . . ? C11 C10 C7 110.9(8) . . ? F3A B1 F1A 108.3(19) . . ? F3A B1 F2A 113(2) . . ? F1A B1 F2A 99(2) . . ? F3A B1 F4 160.9(17) . . ? F1A B1 F4 89.7(17) . . ? F2A B1 F4 69.3(17) . . ? F3A B1 F2 77.0(13) . . ? F1A B1 F2 95.0(16) . . ? F2A B1 F2 39.7(14) . . ? F4 B1 F2 108.7(12) . . ? F3A B1 F1 81.8(15) . . ? F1A B1 F1 38.6(12) . . ? F2A B1 F1 136.3(17) . . ? F4 B1 F1 110.3(11) . . ? F2 B1 F1 116.3(15) . . ? F3A B1 F3 51.8(11) . . ? F1A B1 F3 146.6(19) . . ? F2A B1 F3 113.2(16) . . ? F4 B1 F3 109.3(13) . . ? F2 B1 F3 103.9(13) . . ? F1 B1 F3 108.0(13) . . ? F3A B1 F4A 109.5(16) . . ? F1A B1 F4A 117.1(17) . . ? F2A B1 F4A 109.9(18) . . ? F4 B1 F4A 54.4(12) . . ? F2 B1 F4A 141.4(15) . . ? F1 B1 F4A 102.4(13) . . ? F3 B1 F4A 60.8(12) . . ? F5 B2 F5 117.0(13) . 14 ? F5 B2 F6 106.6(5) . . ? F5 B2 F6 111.4(6) 14 . ? F5 B2 F6 111.4(6) . 14 ? F5 B2 F6 106.6(5) 14 14 ? F6 B2 F6 102.9(14) . 14 ? F7 B3 F7 118.7(16) 14 . ? F7 B3 F8 110.5(6) 14 14 ? F7 B3 F8 103.7(5) . 14 ? F7 B3 F8 103.7(5) 14 . ? F7 B3 F8 110.5(6) . . ? F8 B3 F8 109.7(19) 14 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.243 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.049