data_sfax68 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 As3 N O12' _chemical_formula_weight 555.07 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' 'As' 'As' 0.0499 2.0058 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.105 _cell_length_b 7.342 _cell_length_c 15.292 _cell_angle_alpha 90.00 _cell_angle_beta 115.00 _cell_angle_gamma 90.00 _cell_volume 2045.8 _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 9.846 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.2604 _exptl_absorpt_correction_T_max 0.5745 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5066 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.08 _reflns_number_total 4383 _reflns_number_gt 3366 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'calc w=1/[\s^2^(Fo^2^)+(0.1687P)^2^+1.7854P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 4383 _refine_ls_number_parameters 197 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.2200 _refine_ls_wR_factor_gt 0.1960 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 O8 O 0.3340(7) -0.2459(17) 0.3250(10) 0.065(4) Uani 1 1 d . . . C1 C -0.0094(7) 0.1379(19) 0.2730(11) 0.056(3) Uani 1 1 d . . . H1A H -0.0056 0.1317 0.2119 0.067 Uiso 1 1 calc R . . H1B H -0.0110 0.0159 0.2963 0.067 Uiso 1 1 calc R . . C2 C 0.1092(7) 0.296(2) 0.3038(11) 0.069(4) Uani 1 1 d D . . H2A H 0.1360 0.1852 0.3058 0.083 Uiso 1 1 calc R . . H2B H 0.1446 0.3869 0.3422 0.083 Uiso 1 1 calc R . . C3 C 0.0229(7) 0.4288(16) 0.3659(10) 0.055(3) Uani 1 1 d D . . H3A H -0.0137 0.4028 0.3899 0.067 Uiso 1 1 calc R . . H3B H -0.0006 0.4942 0.3054 0.067 Uiso 1 1 calc R . . C5 C 0.0856(6) 0.5467(13) 0.4405(8) 0.042(2) Uani 1 1 d D . . H5A H 0.0657 0.6597 0.4502 0.063 Uiso 1 1 calc R . . H5B H 0.1218 0.5707 0.4166 0.063 Uiso 1 1 calc R . . H5C H 0.1079 0.4823 0.5006 0.063 Uiso 1 1 calc R . . C8 C 0.0702(8) 0.366(2) 0.1938(9) 0.069(4) Uani 1 1 d D . . H8A H 0.1066 0.3846 0.1695 0.058 Uiso 1 1 calc R . . H8B H 0.0454 0.4794 0.1914 0.088 Uiso 1 1 calc R . . H8C H 0.0353 0.2772 0.1550 0.088 Uiso 1 1 calc R . . As1 As 0.36285(4) 0.2190(2) 0.42953(4) 0.0324(4) Uani 1 1 d . . . As2 As 0.25063(4) -0.2164(2) 0.26201(5) 0.0339(4) Uani 1 1 d . . . As3 As 0.30657(14) 0.25920(11) 0.09615(16) 0.0360(3) Uani 1 1 d . . . N N 0.0546(8) 0.258(2) 0.3507(12) 0.0357(18) Uani 1 1 d D . . O1 O 0.3873(6) 0.0054(18) 0.4669(8) 0.057(3) Uani 1 1 d . . . H11 H 0.3758 -0.0620 0.4200 0.086 Uiso 1 1 calc R . . O2 O 0.4040(6) 0.2751(19) 0.3591(12) 0.071(4) Uani 1 1 d . . . O3 O 0.3849(6) 0.352(2) 0.5224(9) 0.065(4) Uani 1 1 d . . . H13 H 0.3731 0.4567 0.5041 0.098 Uiso 1 1 calc R . . O4 O 0.2665(4) 0.2446(14) 0.3545(7) 0.035(2) Uani 1 1 d . . . H14 H 0.2545 0.1761 0.3079 0.053 Uiso 1 1 calc R . . O5 O 0.1999(5) -0.2871(14) 0.3233(6) 0.039(2) Uani 1 1 d . . . H22 H 0.2081 -0.3951 0.3374 0.059 Uiso 1 1 calc R . . O6 O 0.2320(7) -0.3652(17) 0.1660(8) 0.062(4) Uani 1 1 d . . . H23 H 0.2418 -0.4696 0.1864 0.093 Uiso 1 1 calc R . . O7 O 0.2276(5) -0.0063(12) 0.2207(7) 0.038(2) Uani 1 1 d . . . O12 O 0.2870(6) 0.3837(16) -0.0054(8) 0.050(3) Uani 1 1 d . . . H31 H 0.3217 0.4504 0.0025 0.074 Uiso 1 1 calc R . . O9 O 0.3177(6) 0.3816(16) 0.1906(6) 0.043(3) Uani 1 1 d . . . O10 O 0.2300(5) 0.1249(12) 0.0655(7) 0.053(3) Uani 1 1 d . . . H33 H 0.2355 0.0569 0.1106 0.079 Uiso 1 1 calc R . . O11 O 0.3817(4) 0.1219(11) 0.1308(4) 0.077(5) Uani 1 1 d . . . H34 H 0.3703 0.0175 0.1378 0.116 Uiso 1 1 calc R . . C4 C 0.1015(4) 0.1585(11) 0.4379(4) 0.058(3) Uani 1 1 d R . . H4A H 0.1387 0.2404 0.4811 0.070 Uiso 1 1 calc R . . H4B H 0.1262 0.0610 0.4206 0.070 Uiso 1 1 calc R . . C6 C 0.0601(4) 0.0803(11) 0.4890(4) 0.055 Uani 1 1 d R . . H6A H 0.0931 0.0154 0.5451 0.069 Uiso 1 1 calc R . . H6B H 0.0234 -0.0019 0.4468 0.069 Uiso 1 1 calc R . . H6C H 0.0368 0.1765 0.5084 0.069 Uiso 1 1 calc R . . C7 C -0.0767(4) 0.2575(11) 0.2663(4) 0.060 Uani 1 1 d R . . H7A H -0.1216 0.2023 0.2218 0.090 Uiso 1 1 calc R . . H7B H -0.0726 0.3776 0.2443 0.090 Uiso 1 1 calc R . . H7C H -0.0770 0.2653 0.3288 0.090 Uiso 1 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 O8 0.085(9) 0.061(8) 0.067(8) -0.034(6) 0.049(8) -0.015(6) C1 0.054(6) 0.054(7) 0.067(8) -0.015(6) 0.033(6) -0.016(6) C2 0.068(8) 0.070(9) 0.100(12) -0.016(8) 0.066(9) -0.016(7) C3 0.064(7) 0.056(7) 0.064(8) 0.012(6) 0.044(6) 0.009(6) C5 0.069(7) 0.023(4) 0.040(5) -0.016(4) 0.030(5) -0.020(4) C8 0.112(11) 0.060(8) 0.070(9) 0.019(7) 0.073(9) 0.022(8) As1 0.0384(7) 0.0352(9) 0.0237(8) -0.0003(9) 0.0133(6) 0.0003(9) As2 0.0469(8) 0.0320(8) 0.0252(8) -0.0027(9) 0.0175(7) 0.0007(9) As3 0.0597(5) 0.0312(4) 0.0209(4) -0.0015(10) 0.0208(4) -0.0010(12) N 0.032(3) 0.041(4) 0.039(4) -0.002(3) 0.020(3) -0.004(3) O1 0.079(8) 0.057(8) 0.035(6) 0.009(6) 0.022(6) 0.000(7) O2 0.039(5) 0.083(9) 0.099(11) -0.022(7) 0.037(6) -0.021(5) O3 0.077(7) 0.078(9) 0.038(6) 0.006(6) 0.022(6) 0.051(7) O4 0.007(3) 0.064(6) 0.022(4) -0.004(4) -0.006(3) 0.011(3) O5 0.043(5) 0.052(5) 0.016(4) 0.019(4) 0.004(3) -0.012(4) O6 0.092(8) 0.040(6) 0.027(5) -0.027(5) -0.001(5) 0.002(6) O7 0.067(6) 0.019(5) 0.034(5) -0.003(4) 0.026(5) -0.005(5) O12 0.071(7) 0.037(7) 0.046(6) 0.015(5) 0.031(5) 0.000(5) O9 0.072(6) 0.045(7) 0.015(4) 0.006(4) 0.022(4) 0.009(5) O10 0.080(8) 0.036(6) 0.042(6) 0.008(5) 0.026(6) -0.028(5) O11 0.097(10) 0.096(13) 0.032(6) 0.013(7) 0.021(7) 0.040(9) C4 0.054(6) 0.058(8) 0.050(7) 0.007(6) 0.009(6) -0.003(6) C6 0.056 0.054 0.044 0.006 0.011 -0.001 C7 0.060 0.057 0.048 0.015 0.009 -0.006 _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 O8 As2 1.556(14) . ? C1 C7 1.580(15) . ? C1 N 1.60(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N 1.571(14) . ? C2 C8 1.611(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N 1.470(14) . ? C3 C5 1.556(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? As1 O3 1.622(13) . ? As1 O2 1.663(14) . ? As1 O1 1.671(12) . ? As1 O4 1.796(7) . ? As2 O7 1.657(9) 1 ? As2 O7 1.657(9) . ? As2 O5 1.731(9) . ? As2 O6 1.739(10) . ? As3 O9 1.634(10) . ? As3 O12 1.698(11) . ? As3 O11 1.704(7) . ? As3 O10 1.718(8) . ? N C4 1.462(17) . ? O1 H11 0.8200 . ? O3 H13 0.8200 . ? O4 H14 0.8200 . ? O5 H22 0.8200 . ? O6 H23 0.8200 . ? O7 O7 0.000(18) 1 ? O12 H31 0.8200 . ? O10 H33 0.8200 . ? O11 H34 0.8200 . ? C4 C6 1.4777 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? 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 C7 C1 N 98.1(9) . . ? C7 C1 H1A 112.1 . . ? N C1 H1A 112.1 . . ? C7 C1 H1B 112.1 . . ? N C1 H1B 112.1 . . ? H1A C1 H1B 109.8 . . ? N C2 C8 114.1(12) . . ? N C2 H2A 108.7 . . ? C8 C2 H2A 108.7 . . ? N C2 H2B 108.7 . . ? C8 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N C3 C5 108.7(10) . . ? N C3 H3A 110.0 . . ? C5 C3 H3A 110.0 . . ? N C3 H3B 110.0 . . ? C5 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? 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 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 As1 O2 113.0(6) . . ? O3 As1 O1 109.4(6) . . ? O2 As1 O1 107.4(7) . . ? O3 As1 O4 108.6(5) . . ? O2 As1 O4 104.9(6) . . ? O1 As1 O4 113.5(6) . . ? O8 As2 O7 114.8(6) . 1 ? O8 As2 O7 114.8(6) . . ? O7 As2 O7 0.0(12) 1 . ? O8 As2 O5 110.5(6) . . ? O7 As2 O5 110.6(5) 1 . ? O7 As2 O5 110.6(5) . . ? O8 As2 O6 103.1(6) . . ? O7 As2 O6 109.7(5) 1 . ? O7 As2 O6 109.7(5) . . ? O5 As2 O6 107.6(6) . . ? O9 As3 O12 113.8(3) . . ? O9 As3 O11 106.2(5) . . ? O12 As3 O11 115.8(5) . . ? O9 As3 O10 109.2(5) . . ? O12 As3 O10 103.0(5) . . ? O11 As3 O10 108.6(4) . . ? C4 N C3 115.9(12) . . ? C4 N C2 101.6(10) . . ? C3 N C2 110.7(12) . . ? C4 N C1 114.2(12) . . ? C3 N C1 108.8(12) . . ? C2 N C1 104.9(11) . . ? As1 O1 H11 109.5 . . ? As1 O3 H13 109.5 . . ? As1 O4 H14 109.5 . . ? As2 O5 H22 109.5 . . ? As2 O6 H23 109.5 . . ? O7 O7 As2 0(10) 1 . ? As3 O12 H31 109.5 . . ? As3 O10 H33 109.5 . . ? As3 O11 H34 109.5 . . ? N C4 C6 112.7(6) . . ? N C4 H4A 109.1 . . ? C6 C4 H4A 109.1 . . ? N C4 H4B 109.1 . . ? C6 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.735 _refine_diff_density_min -2.448 _refine_diff_density_rms 0.224