# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jack Passmore' _publ_contact_author_address ; Department of Chemistry, University of New Brunswick, Fredericton CANADA ; _publ_contact_author_email PASSMORE@UNB.CA _publ_section_title ; Characterisation of the Thermally Accessible Spin Triplet State in Dimers of the 7pi ClCNSSS+. in the Solid State ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2004). CrystalStructure 3.6.0. Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'Jack Passmore' 'T. Stanley Cameron' 'Andreas Decken' 'Radoslaw M. Kowalczyk' 'E. McInnes' ; J.Rawson ; 'Konstantin V. Shuvaev' 'Laurence Thompson' #============================================================================== # 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 #============================================================================== # Attachment 'Cl_353K.cif' #============================================================================== data_afc5r.xtl_Cu_radiation_353K _database_code_depnum_ccdc_archive 'CCDC 273159' _audit_creation_date 2005-05-20 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C As Cl F6 N S3 ' _chemical_formula_moiety 'C As Cl F6 N S3 ' _chemical_formula_weight 346.56 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.964(6) _cell_length_b 9.900(3) _cell_length_c 6.147(5) _cell_angle_alpha 95.32(4) _cell_angle_beta 109.05(5) _cell_angle_gamma 88.83(4) _cell_volume 456.1(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.7 _cell_measurement_theta_max 20.0 _cell_measurement_temperature 353.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 2.523 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 330.00 _exptl_absorpt_coefficient_mu 4.751 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.477 _exptl_absorpt_correction_T_max 1.000 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 2858 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_max 30.03 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.69 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+0.5288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2680 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; As As 0.050 2.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.23110(7) 0.76410(5) 0.03432(10) 0.04227(18) Uani 1 d . . . Cl1 Cl 0.7903(3) 0.90641(18) 0.3524(3) 0.0695(5) Uani 1 d . . . S1 S 0.6556(2) 0.80931(14) 0.6920(3) 0.0524(4) Uani 1 d . . . S2 S 0.6372(2) 0.61811(14) 0.7712(3) 0.0536(4) Uani 1 d . . . S3 S 0.7496(2) 0.52407(14) 0.5392(3) 0.0533(4) Uani 1 d . . . F1 F 0.1690(15) 0.6336(10) -0.1688(15) 0.149(4) Uani 0.82 d P . . F2 F 0.3049(13) 0.8898(6) 0.2430(14) 0.123(3) Uani 0.82 d P . . F3 F 0.0700(10) 0.7174(10) 0.128(2) 0.128(3) Uani 0.82 d P . . F4 F 0.3975(12) 0.8049(11) -0.060(2) 0.123(3) Uani 0.82 d P . . F5 F 0.0901(7) 0.8730(6) -0.1243(12) 0.134(2) Uani 1 d . . . F6 F 0.3776(6) 0.6560(4) 0.2021(11) 0.116(2) Uani 1 d . . . F7 F 0.386(3) 0.883(3) 0.087(7) 0.090(9) Uani 0.18 d P . . F8 F 0.089(4) 0.646(3) -0.046(8) 0.104(11) Uani 0.18 d P . . F9 F 0.254(7) 0.757(4) -0.225(6) 0.134(14) Uani 0.18 d P . . F10 F 0.223(6) 0.787(5) 0.295(4) 0.140(14) Uani 0.18 d P . . N1 N 0.7888(7) 0.6509(5) 0.4147(9) 0.0535(12) Uani 1 d . . . C1 C 0.7500(7) 0.7713(6) 0.4763(9) 0.0467(12) Uani 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0434(3) 0.0382(3) 0.0448(3) 0.0063(2) 0.0133(2) 0.0028(2) Cl1 0.0844(12) 0.0636(9) 0.0642(10) 0.0171(7) 0.0250(9) -0.0184(8) S1 0.0702(10) 0.0394(7) 0.0518(8) 0.0006(6) 0.0265(7) -0.0019(6) S2 0.0727(10) 0.0462(7) 0.0465(8) 0.0067(6) 0.0251(7) -0.0005(7) S3 0.0550(9) 0.0438(7) 0.0643(9) 0.0031(6) 0.0245(7) 0.0051(6) F1 0.183(10) 0.122(7) 0.102(6) -0.069(6) 0.012(6) -0.013(7) F2 0.174(8) 0.054(3) 0.111(6) -0.033(4) 0.015(5) -0.001(4) F3 0.097(5) 0.147(7) 0.189(9) 0.083(7) 0.095(6) 0.023(5) F4 0.099(6) 0.158(8) 0.151(8) 0.046(7) 0.083(6) 0.008(6) F5 0.082(3) 0.115(4) 0.185(6) 0.083(4) -0.001(4) 0.019(3) F6 0.080(3) 0.062(3) 0.162(5) 0.045(3) -0.028(3) 0.000(2) F7 0.054(14) 0.073(17) 0.13(3) 0.047(16) -0.004(16) -0.033(12) F8 0.045(15) 0.079(19) 0.15(3) 0.02(2) -0.024(17) -0.029(13) F9 0.23(5) 0.12(3) 0.08(2) 0.02(2) 0.08(3) 0.00(3) F10 0.17(4) 0.22(4) 0.041(13) -0.02(2) 0.059(18) -0.02(3) N1 0.056(3) 0.054(3) 0.056(3) -0.001(2) 0.027(2) -0.008(2) C1 0.044(3) 0.054(3) 0.043(3) 0.002(2) 0.015(2) -0.008(2) _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 As1 F8 1.57(2) . ? As1 F10 1.62(2) . ? As1 F7 1.65(2) . ? As1 F9 1.66(3) . ? As1 F3 1.659(6) . ? As1 F2 1.668(5) . ? As1 F1 1.672(6) . ? As1 F5 1.675(5) . ? As1 F4 1.680(7) . ? As1 F6 1.714(4) . ? Cl1 C1 1.685(6) . ? S1 C1 1.735(6) . ? S1 S2 2.018(2) . ? S2 S3 2.063(2) . ? S3 N1 1.616(5) . ? F1 F8 1.13(5) . ? F1 F9 1.53(4) . ? F2 F7 1.32(4) . ? F2 F10 1.34(4) . ? F3 F8 1.28(5) . ? F3 F10 1.45(4) . ? F4 F7 1.16(4) . ? F4 F9 1.32(5) . ? N1 C1 1.279(7) . ? 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 F8 As1 F10 95(2) . . ? F8 As1 F7 172(3) . . ? F10 As1 F7 92(2) . . ? F8 As1 F9 92(2) . . ? F10 As1 F9 173(2) . . ? F7 As1 F9 81(2) . . ? F8 As1 F3 46.6(18) . . ? F10 As1 F3 52.5(15) . . ? F7 As1 F3 140.8(17) . . ? F9 As1 F3 133.5(19) . . ? F8 As1 F2 141(2) . . ? F10 As1 F2 48.0(17) . . ? F7 As1 F2 46.7(15) . . ? F9 As1 F2 125.2(16) . . ? F3 As1 F2 94.4(6) . . ? F8 As1 F1 40.6(18) . . ? F10 As1 F1 131.9(18) . . ? F7 As1 F1 131.9(17) . . ? F9 As1 F1 54.8(15) . . ? F3 As1 F1 87.2(6) . . ? F2 As1 F1 176.6(5) . . ? F8 As1 F5 92.2(11) . . ? F10 As1 F5 107.9(17) . . ? F7 As1 F5 86.8(9) . . ? F9 As1 F5 70.8(15) . . ? F3 As1 F5 88.7(3) . . ? F2 As1 F5 88.9(4) . . ? F1 As1 F5 94.2(4) . . ? F8 As1 F4 132(2) . . ? F10 As1 F4 127.8(17) . . ? F7 As1 F4 40.7(15) . . ? F9 As1 F4 46.4(18) . . ? F3 As1 F4 177.6(4) . . ? F2 As1 F4 86.9(5) . . ? F1 As1 F4 91.4(6) . . ? F5 As1 F4 93.3(4) . . ? F8 As1 F6 88.9(10) . . ? F10 As1 F6 71.1(17) . . ? F7 As1 F6 92.2(9) . . ? F9 As1 F6 110.0(16) . . ? F3 As1 F6 91.5(3) . . ? F2 As1 F6 89.7(3) . . ? F1 As1 F6 87.2(4) . . ? F5 As1 F6 178.5(3) . . ? F4 As1 F6 86.5(4) . . ? C1 S1 S2 97.7(2) . . ? S1 S2 S3 96.69(9) . . ? N1 S3 S2 101.90(19) . . ? F8 F1 F9 120(2) . . ? F8 F1 As1 64.9(14) . . ? F9 F1 As1 62.1(12) . . ? F7 F2 F10 125.7(19) . . ? F7 F2 As1 66.0(12) . . ? F10 F2 As1 64.1(12) . . ? F8 F3 F10 119.0(18) . . ? F8 F3 As1 63.1(12) . . ? F10 F3 As1 62.3(11) . . ? F7 F4 F9 120(2) . . ? F7 F4 As1 68.4(12) . . ? F9 F4 As1 65.8(15) . . ? F4 F7 F2 137.0(19) . . ? F4 F7 As1 70.9(13) . . ? F2 F7 As1 67.3(11) . . ? F1 F8 F3 145(2) . . ? F1 F8 As1 74.5(17) . . ? F3 F8 As1 70.3(15) . . ? F4 F9 F1 115(2) . . ? F4 F9 As1 67.7(15) . . ? F1 F9 As1 63.2(12) . . ? F2 F10 F3 122(2) . . ? F2 F10 As1 67.9(13) . . ? F3 F10 As1 65.2(11) . . ? C1 N1 S3 120.0(4) . . ? N1 C1 Cl1 121.5(5) . . ? N1 C1 S1 123.6(5) . . ? Cl1 C1 S1 114.9(3) . . ? 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 C1 S1 S2 S3 1.1(2) . . . . ? S1 S2 S3 N1 -1.1(2) . . . . ? F10 As1 F1 F8 30(3) . . . . ? F7 As1 F1 F8 -178(2) . . . . ? F9 As1 F1 F8 -151(3) . . . . ? F3 As1 F1 F8 0.0(18) . . . . ? F2 As1 F1 F8 118(9) . . . . ? F5 As1 F1 F8 -88.5(18) . . . . ? F4 As1 F1 F8 178.1(18) . . . . ? F6 As1 F1 F8 91.6(18) . . . . ? F8 As1 F1 F9 151(3) . . . . ? F10 As1 F1 F9 -178(3) . . . . ? F7 As1 F1 F9 -27(2) . . . . ? F3 As1 F1 F9 151(2) . . . . ? F2 As1 F1 F9 -91(10) . . . . ? F5 As1 F1 F9 63(2) . . . . ? F4 As1 F1 F9 -31(2) . . . . ? F6 As1 F1 F9 -117(2) . . . . ? F8 As1 F2 F7 -179(2) . . . . ? F10 As1 F2 F7 158(3) . . . . ? F9 As1 F2 F7 -21(2) . . . . ? F3 As1 F2 F7 -175.2(13) . . . . ? F1 As1 F2 F7 67(10) . . . . ? F5 As1 F2 F7 -86.7(13) . . . . ? F4 As1 F2 F7 6.8(14) . . . . ? F6 As1 F2 F7 93.3(13) . . . . ? F8 As1 F2 F10 23(3) . . . . ? F7 As1 F2 F10 -158(3) . . . . ? F9 As1 F2 F10 -179(3) . . . . ? F3 As1 F2 F10 27(2) . . . . ? F1 As1 F2 F10 -90(10) . . . . ? F5 As1 F2 F10 116(2) . . . . ? F4 As1 F2 F10 -151(2) . . . . ? F6 As1 F2 F10 -64(2) . . . . ? F10 As1 F3 F8 -152(3) . . . . ? F7 As1 F3 F8 178(2) . . . . ? F9 As1 F3 F8 33(2) . . . . ? F2 As1 F3 F8 -176.9(15) . . . . ? F1 As1 F3 F8 0.0(16) . . . . ? F5 As1 F3 F8 94.3(15) . . . . ? F4 As1 F3 F8 -54(14) . . . . ? F6 As1 F3 F8 -87.1(15) . . . . ? F8 As1 F3 F10 152(3) . . . . ? F7 As1 F3 F10 -31(3) . . . . ? F9 As1 F3 F10 -176(3) . . . . ? F2 As1 F3 F10 -25(2) . . . . ? F1 As1 F3 F10 152(2) . . . . ? F5 As1 F3 F10 -114(2) . . . . ? F4 As1 F3 F10 98(14) . . . . ? F6 As1 F3 F10 65(2) . . . . ? F8 As1 F4 F7 177(2) . . . . ? F10 As1 F4 F7 -35(3) . . . . ? F9 As1 F4 F7 140(3) . . . . ? F3 As1 F4 F7 -130(14) . . . . ? F2 As1 F4 F7 -7.5(15) . . . . ? F1 As1 F4 F7 175.5(15) . . . . ? F5 As1 F4 F7 81.1(15) . . . . ? F6 As1 F4 F7 -97.4(15) . . . . ? F8 As1 F4 F9 37(2) . . . . ? F10 As1 F4 F9 -175(3) . . . . ? F7 As1 F4 F9 -140(3) . . . . ? F3 As1 F4 F9 89(14) . . . . ? F2 As1 F4 F9 -148(2) . . . . ? F1 As1 F4 F9 35(2) . . . . ? F5 As1 F4 F9 -59(2) . . . . ? F6 As1 F4 F9 122(2) . . . . ? F9 F4 F7 F2 56(4) . . . . ? As1 F4 F7 F2 14(3) . . . . ? F9 F4 F7 As1 42(2) . . . . ? F10 F2 F7 F4 10(5) . . . . ? As1 F2 F7 F4 -14(3) . . . . ? F10 F2 F7 As1 25(3) . . . . ? F8 As1 F7 F4 -16(11) . . . . ? F10 As1 F7 F4 153(2) . . . . ? F9 As1 F7 F4 -28(2) . . . . ? F3 As1 F7 F4 177.1(6) . . . . ? F2 As1 F7 F4 170(2) . . . . ? F1 As1 F7 F4 -6(2) . . . . ? F5 As1 F7 F4 -98.9(12) . . . . ? F6 As1 F7 F4 82.1(12) . . . . ? F8 As1 F7 F2 174(10) . . . . ? F10 As1 F7 F2 -16(2) . . . . ? F9 As1 F7 F2 162.5(19) . . . . ? F3 As1 F7 F2 8(2) . . . . ? F1 As1 F7 F2 -175.7(6) . . . . ? F5 As1 F7 F2 91.5(10) . . . . ? F4 As1 F7 F2 -170(2) . . . . ? F6 As1 F7 F2 -87.5(10) . . . . ? F9 F1 F8 F3 -29(6) . . . . ? As1 F1 F8 F3 0(4) . . . . ? F9 F1 F8 As1 -29(3) . . . . ? F10 F3 F8 F1 -29(6) . . . . ? As1 F3 F8 F1 0(4) . . . . ? F10 F3 F8 As1 -29(3) . . . . ? F10 As1 F8 F1 -158(2) . . . . ? F7 As1 F8 F1 12(11) . . . . ? F9 As1 F8 F1 23(2) . . . . ? F3 As1 F8 F1 180(2) . . . . ? F2 As1 F8 F1 -175.2(7) . . . . ? F5 As1 F8 F1 93.9(15) . . . . ? F4 As1 F8 F1 -3(2) . . . . ? F6 As1 F8 F1 -87.0(15) . . . . ? F10 As1 F8 F3 22(2) . . . . ? F7 As1 F8 F3 -168(10) . . . . ? F9 As1 F8 F3 -156.9(19) . . . . ? F2 As1 F8 F3 5(2) . . . . ? F1 As1 F8 F3 -180(2) . . . . ? F5 As1 F8 F3 -86.1(11) . . . . ? F4 As1 F8 F3 177.4(6) . . . . ? F6 As1 F8 F3 93.1(11) . . . . ? F7 F4 F9 F1 -87(3) . . . . ? As1 F4 F9 F1 -43.5(19) . . . . ? F7 F4 F9 As1 -43(2) . . . . ? F8 F1 F9 F4 76(4) . . . . ? As1 F1 F9 F4 46(2) . . . . ? F8 F1 F9 As1 30(3) . . . . ? F8 As1 F9 F4 -153.6(18) . . . . ? F10 As1 F9 F4 34(19) . . . . ? F7 As1 F9 F4 24.8(17) . . . . ? F3 As1 F9 F4 -176.7(6) . . . . ? F2 As1 F9 F4 40(2) . . . . ? F1 As1 F9 F4 -135(3) . . . . ? F5 As1 F9 F4 114.6(17) . . . . ? F6 As1 F9 F4 -64.2(17) . . . . ? F8 As1 F9 F1 -18.2(18) . . . . ? F10 As1 F9 F1 170(17) . . . . ? F7 As1 F9 F1 160.3(19) . . . . ? F3 As1 F9 F1 -41(2) . . . . ? F2 As1 F9 F1 175.8(6) . . . . ? F5 As1 F9 F1 -110.0(17) . . . . ? F4 As1 F9 F1 135(3) . . . . ? F6 As1 F9 F1 71.3(17) . . . . ? F7 F2 F10 F3 -63(5) . . . . ? As1 F2 F10 F3 -38(2) . . . . ? F7 F2 F10 As1 -25(3) . . . . ? F8 F3 F10 F2 68(4) . . . . ? As1 F3 F10 F2 39(2) . . . . ? F8 F3 F10 As1 29(3) . . . . ? F8 As1 F10 F2 -165.4(18) . . . . ? F7 As1 F10 F2 16.0(19) . . . . ? F9 As1 F10 F2 7(19) . . . . ? F3 As1 F10 F2 -145(3) . . . . ? F1 As1 F10 F2 175.4(6) . . . . ? F5 As1 F10 F2 -71.4(17) . . . . ? F4 As1 F10 F2 38(3) . . . . ? F6 As1 F10 F2 107.5(17) . . . . ? F8 As1 F10 F3 -20.2(19) . . . . ? F7 As1 F10 F3 161.2(17) . . . . ? F9 As1 F10 F3 152(17) . . . . ? F2 As1 F10 F3 145(3) . . . . ? F1 As1 F10 F3 -39(3) . . . . ? F5 As1 F10 F3 73.8(17) . . . . ? F4 As1 F10 F3 -177.0(5) . . . . ? F6 As1 F10 F3 -107.4(17) . . . . ? S2 S3 N1 C1 0.7(5) . . . . ? S3 N1 C1 Cl1 179.5(3) . . . . ? S3 N1 C1 S1 0.2(8) . . . . ? S2 S1 C1 N1 -1.0(5) . . . . ? S2 S1 C1 Cl1 179.7(3) . . . . ? #_diffrn_measured_fraction_theta_max 1.000 #_diffrn_reflns_theta_full 30.03 #_diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.688 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.123 # Attachment 'Cl_168K.cif' #============================================================================== data_afc5r.xtl_Cu_radiation_168K _database_code_depnum_ccdc_archive 'CCDC 273160' _audit_creation_date 2005-05-20 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C As Cl F6 N S3 ' _chemical_formula_moiety 'C As Cl F6 N S3 ' _chemical_formula_weight 346.56 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.8360(5) _cell_length_b 9.851(2) _cell_length_c 6.12(1) _cell_angle_alpha 95.7(7) _cell_angle_beta 109.7(5) _cell_angle_gamma 89.33(8) _cell_volume 442.5(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 19.6 _cell_measurement_temperature 168.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 2.523 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 330.00 _exptl_absorpt_coefficient_mu 4.751 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 1.000 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 5445 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_theta_max 30.08 _diffrn_measured_fraction_theta_max 1.0000 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 1.0000 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.01 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+0.4660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2595 _refine_ls_number_parameters 155 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; As As 0.050 2.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; F F 0.017 0.010 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.22677(6) 0.76752(4) 0.03137(7) 0.02403(15) Uani 1 d DU . . Cl1 Cl 0.79268(19) 0.90155(13) 0.3450(2) 0.0379(3) Uani 1 d . . . S1 S 0.64937(17) 0.81056(11) 0.6861(2) 0.0301(3) Uani 1 d . . . S2 S 0.62575(17) 0.61916(12) 0.77074(19) 0.0298(3) Uani 1 d . . . S3 S 0.74792(16) 0.52057(12) 0.5500(2) 0.0297(3) Uani 1 d . . . F1 F 0.1666(7) 0.6432(5) -0.1948(8) 0.0790(17) Uani 0.92 d P . . F2 F 0.2941(8) 0.8863(4) 0.2627(8) 0.0712(15) Uani 0.92 d P . . F3 F 0.0593(6) 0.7082(5) 0.1157(9) 0.0637(13) Uani 0.92 d P . . F4 F 0.3993(6) 0.8205(6) -0.0533(9) 0.0659(13) Uani 0.92 d P . . F5 F 0.0829(5) 0.8801(4) -0.1296(7) 0.0534(10) Uani 1 d D . . F6 F 0.3757(4) 0.6533(3) 0.1951(7) 0.0478(9) Uani 1 d D . . F7 F 0.390(4) 0.890(3) 0.100(8) 0.048(10) Uani 0.08 d PDU . . F8 F 0.059(4) 0.649(3) -0.049(8) 0.051(8) Uani 0.08 d PDU . . F9 F 0.274(5) 0.719(4) -0.214(4) 0.044(8) Uani 0.08 d PDU . . F10 F 0.168(6) 0.820(5) 0.265(5) 0.069(13) Uani 0.08 d PDU . . N1 N 0.7898(6) 0.6452(4) 0.4207(7) 0.0309(8) Uani 1 d . . . C1 C 0.7502(6) 0.7679(5) 0.4755(8) 0.0287(9) Uani 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0258(2) 0.0254(2) 0.0203(2) 0.00316(15) 0.00685(16) 0.00303(15) Cl1 0.0507(7) 0.0350(6) 0.0288(6) 0.0077(4) 0.0129(5) -0.0090(5) S1 0.0403(6) 0.0259(5) 0.0244(5) 0.0003(4) 0.0121(5) -0.0008(4) S2 0.0400(6) 0.0286(5) 0.0221(5) 0.0033(4) 0.0120(4) -0.0008(4) S3 0.0315(6) 0.0265(5) 0.0327(6) 0.0032(4) 0.0128(5) 0.0025(4) F1 0.082(4) 0.074(3) 0.050(3) -0.035(2) -0.006(3) 0.008(3) F2 0.098(4) 0.043(2) 0.046(2) -0.0203(19) -0.002(2) 0.013(2) F3 0.050(2) 0.071(3) 0.091(4) 0.041(3) 0.043(2) 0.009(2) F4 0.044(2) 0.091(4) 0.083(3) 0.041(3) 0.039(2) 0.005(2) F5 0.0425(19) 0.051(2) 0.061(2) 0.0302(18) 0.0037(16) 0.0089(15) F6 0.0370(17) 0.0348(16) 0.060(2) 0.0171(15) -0.0020(15) 0.0032(13) F7 0.043(17) 0.019(15) 0.08(3) 0.022(17) 0.01(2) -0.001(9) F8 0.037(14) 0.048(15) 0.060(17) 0.009(15) 0.005(15) -0.013(9) F9 0.054(16) 0.048(16) 0.026(14) -0.005(13) 0.011(13) 0.008(14) F10 0.08(3) 0.09(3) 0.05(2) -0.03(2) 0.05(2) 0.00(2) N1 0.031(2) 0.036(2) 0.0260(18) 0.0012(16) 0.0100(16) -0.0034(16) C1 0.028(2) 0.036(2) 0.0193(18) 0.0036(16) 0.0034(16) -0.0073(17) _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 As1 F10 1.676(18) . ? As1 F8 1.677(18) . ? As1 F2 1.684(12) . ? As1 F9 1.689(18) . ? As1 F7 1.690(18) . ? As1 F3 1.693(6) . ? As1 F1 1.696(12) . ? As1 F5 1.706(10) . ? As1 F4 1.707(5) . ? As1 F6 1.742(10) . ? Cl1 C1 1.697(9) . ? S1 C1 1.742(8) . ? S1 S2 2.031(6) . ? S2 S3 2.068(9) . ? S3 N1 1.618(8) . ? F1 F9 1.17(4) . ? F1 F8 1.41(4) . ? F2 F10 1.20(5) . ? F2 F7 1.44(4) . ? F3 F8 1.11(5) . ? F3 F10 1.44(5) . ? F4 F7 1.13(4) . ? F4 F9 1.45(4) . ? N1 C1 1.285(8) . ? 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 F10 As1 F8 89(2) . . ? F10 As1 F2 41.8(17) . . ? F8 As1 F2 130.8(17) . . ? F10 As1 F9 176.4(19) . . ? F8 As1 F9 89.6(19) . . ? F2 As1 F9 139.4(15) . . ? F10 As1 F7 92(2) . . ? F8 As1 F7 177.1(19) . . ? F2 As1 F7 50.7(17) . . ? F9 As1 F7 89(2) . . ? F10 As1 F3 50.5(18) . . ? F8 As1 F3 38.6(16) . . ? F2 As1 F3 92.2(4) . . ? F9 As1 F3 128.2(15) . . ? F7 As1 F3 142.8(16) . . ? F10 As1 F1 138.5(18) . . ? F8 As1 F1 49.6(17) . . ? F2 As1 F1 177.4(2) . . ? F9 As1 F1 40.6(14) . . ? F7 As1 F1 129.1(17) . . ? F3 As1 F1 88.1(4) . . ? F10 As1 F5 90.9(16) . . ? F8 As1 F5 90.3(14) . . ? F2 As1 F5 90.6(4) . . ? F9 As1 F5 85.7(13) . . ? F7 As1 F5 87.2(12) . . ? F3 As1 F5 90.8(3) . . ? F1 As1 F5 92.0(4) . . ? F10 As1 F4 130.8(18) . . ? F8 As1 F4 140.0(17) . . ? F2 As1 F4 89.1(4) . . ? F9 As1 F4 50.7(15) . . ? F7 As1 F4 38.7(16) . . ? F3 As1 F4 177.6(2) . . ? F1 As1 F4 90.5(4) . . ? F5 As1 F4 91.3(4) . . ? F10 As1 F6 89.4(16) . . ? F8 As1 F6 90.2(14) . . ? F2 As1 F6 89.3(4) . . ? F9 As1 F6 94.0(13) . . ? F7 As1 F6 92.3(12) . . ? F3 As1 F6 89.8(3) . . ? F1 As1 F6 88.1(4) . . ? F5 As1 F6 179.36(17) . . ? F4 As1 F6 88.1(3) . . ? C1 S1 S2 97.7(4) . . ? S1 S2 S3 96.6(3) . . ? N1 S3 S2 102.0(3) . . ? F9 F1 F8 132.8(15) . . ? F9 F1 As1 69.4(11) . . ? F8 F1 As1 64.5(11) . . ? F10 F2 F7 133.6(15) . . ? F10 F2 As1 68.8(12) . . ? F7 F2 As1 64.9(11) . . ? F8 F3 F10 134.1(16) . . ? F8 F3 As1 69.9(12) . . ? F10 F3 As1 64.2(11) . . ? F7 F4 F9 132.3(16) . . ? F7 F4 As1 69.9(12) . . ? F9 F4 As1 64.0(10) . . ? F4 F7 F2 135.1(15) . . ? F4 F7 As1 71.4(13) . . ? F2 F7 As1 64.4(11) . . ? F3 F8 F1 137.3(15) . . ? F3 F8 As1 71.5(13) . . ? F1 F8 As1 65.9(11) . . ? F1 F9 F4 133.5(16) . . ? F1 F9 As1 70.1(12) . . ? F4 F9 As1 65.3(10) . . ? F2 F10 F3 134.8(14) . . ? F2 F10 As1 69.5(13) . . ? F3 F10 As1 65.4(11) . . ? C1 N1 S3 120.4(4) . . ? N1 C1 Cl1 121.9(4) . . ? N1 C1 S1 123.3(6) . . ? Cl1 C1 S1 114.9(4) . . ? 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 C1 S1 S2 S3 1.87(16) . . . . ? S1 S2 S3 N1 -2.18(17) . . . . ? F10 As1 F1 F9 175(3) . . . . ? F8 As1 F1 F9 170(3) . . . . ? F2 As1 F1 F9 -91(7) . . . . ? F7 As1 F1 F9 -7(2) . . . . ? F3 As1 F1 F9 171.7(19) . . . . ? F5 As1 F1 F9 81.0(19) . . . . ? F4 As1 F1 F9 -10.3(19) . . . . ? F6 As1 F1 F9 -98(2) . . . . ? F10 As1 F1 F8 5(3) . . . . ? F2 As1 F1 F8 100(7) . . . . ? F9 As1 F1 F8 -170(3) . . . . ? F7 As1 F1 F8 -177(2) . . . . ? F3 As1 F1 F8 2.0(18) . . . . ? F5 As1 F1 F8 -88.7(18) . . . . ? F4 As1 F1 F8 -179.9(18) . . . . ? F6 As1 F1 F8 92.0(18) . . . . ? F8 As1 F2 F10 0(3) . . . . ? F9 As1 F2 F10 175(3) . . . . ? F7 As1 F2 F10 177(3) . . . . ? F3 As1 F2 F10 0(2) . . . . ? F1 As1 F2 F10 -98(7) . . . . ? F5 As1 F2 F10 91(2) . . . . ? F4 As1 F2 F10 -178(2) . . . . ? F6 As1 F2 F10 -90(2) . . . . ? F10 As1 F2 F7 -177(3) . . . . ? F8 As1 F2 F7 -177(2) . . . . ? F9 As1 F2 F7 -2(2) . . . . ? F3 As1 F2 F7 -176.7(15) . . . . ? F1 As1 F2 F7 86(7) . . . . ? F5 As1 F2 F7 -85.9(15) . . . . ? F4 As1 F2 F7 5.3(15) . . . . ? F6 As1 F2 F7 93.5(15) . . . . ? F10 As1 F3 F8 -180(3) . . . . ? F2 As1 F3 F8 -180(2) . . . . ? F9 As1 F3 F8 4(3) . . . . ? F7 As1 F3 F8 176(3) . . . . ? F1 As1 F3 F8 -2(2) . . . . ? F5 As1 F3 F8 90(2) . . . . ? F4 As1 F3 F8 -58(6) . . . . ? F6 As1 F3 F8 -91(2) . . . . ? F8 As1 F3 F10 180(3) . . . . ? F2 As1 F3 F10 0(2) . . . . ? F9 As1 F3 F10 -176(2) . . . . ? F7 As1 F3 F10 -4(3) . . . . ? F1 As1 F3 F10 177(2) . . . . ? F5 As1 F3 F10 -91(2) . . . . ? F4 As1 F3 F10 122(6) . . . . ? F6 As1 F3 F10 89(2) . . . . ? F10 As1 F4 F7 -8(3) . . . . ? F8 As1 F4 F7 176(3) . . . . ? F2 As1 F4 F7 -6.6(19) . . . . ? F9 As1 F4 F7 167(2) . . . . ? F3 As1 F4 F7 -129(6) . . . . ? F1 As1 F4 F7 176.0(19) . . . . ? F5 As1 F4 F7 83.9(19) . . . . ? F6 As1 F4 F7 -96.0(19) . . . . ? F10 As1 F4 F9 -176(3) . . . . ? F8 As1 F4 F9 9(3) . . . . ? F2 As1 F4 F9 -174.0(16) . . . . ? F7 As1 F4 F9 -167(2) . . . . ? F3 As1 F4 F9 64(6) . . . . ? F1 As1 F4 F9 8.6(16) . . . . ? F5 As1 F4 F9 -83.4(17) . . . . ? F6 As1 F4 F9 96.7(17) . . . . ? F9 F4 F7 F2 26(6) . . . . ? As1 F4 F7 F2 11(3) . . . . ? F9 F4 F7 As1 15(3) . . . . ? F10 F2 F7 F4 -16(6) . . . . ? As1 F2 F7 F4 -12(3) . . . . ? F10 F2 F7 As1 -4(4) . . . . ? F10 As1 F7 F4 174(2) . . . . ? F8 As1 F7 F4 -66(40) . . . . ? F2 As1 F7 F4 171(2) . . . . ? F9 As1 F7 F4 -9.8(19) . . . . ? F3 As1 F7 F4 176.9(3) . . . . ? F1 As1 F7 F4 -5(2) . . . . ? F5 As1 F7 F4 -95.5(15) . . . . ? F6 As1 F7 F4 84.2(15) . . . . ? F10 As1 F7 F2 2.3(19) . . . . ? F8 As1 F7 F2 123(40) . . . . ? F9 As1 F7 F2 178.8(16) . . . . ? F3 As1 F7 F2 5(2) . . . . ? F1 As1 F7 F2 -176.6(3) . . . . ? F5 As1 F7 F2 93.1(10) . . . . ? F4 As1 F7 F2 -171(2) . . . . ? F6 As1 F7 F2 -87.3(10) . . . . ? F10 F3 F8 F1 4(7) . . . . ? As1 F3 F8 F1 4(4) . . . . ? F10 F3 F8 As1 0(4) . . . . ? F9 F1 F8 F3 -18(7) . . . . ? As1 F1 F8 F3 -5(4) . . . . ? F9 F1 F8 As1 -13(3) . . . . ? F10 As1 F8 F3 0(2) . . . . ? F2 As1 F8 F3 0(3) . . . . ? F9 As1 F8 F3 -177(2) . . . . ? F7 As1 F8 F3 -121(40) . . . . ? F1 As1 F8 F3 177(3) . . . . ? F5 As1 F8 F3 -90.9(17) . . . . ? F4 As1 F8 F3 176.8(4) . . . . ? F6 As1 F8 F3 89.5(17) . . . . ? F10 As1 F8 F1 -177(2) . . . . ? F2 As1 F8 F1 -176.6(3) . . . . ? F9 As1 F8 F1 6.7(17) . . . . ? F7 As1 F8 F1 63(41) . . . . ? F3 As1 F8 F1 -177(3) . . . . ? F5 As1 F8 F1 92.4(12) . . . . ? F4 As1 F8 F1 0(3) . . . . ? F6 As1 F8 F1 -87.3(12) . . . . ? F8 F1 F9 F4 30(6) . . . . ? As1 F1 F9 F4 17(3) . . . . ? F8 F1 F9 As1 13(3) . . . . ? F7 F4 F9 F1 -34(5) . . . . ? As1 F4 F9 F1 -17(3) . . . . ? F7 F4 F9 As1 -16(3) . . . . ? F10 As1 F9 F1 -77(32) . . . . ? F8 As1 F9 F1 -8(2) . . . . ? F2 As1 F9 F1 175.9(3) . . . . ? F7 As1 F9 F1 174.5(19) . . . . ? F3 As1 F9 F1 -11(2) . . . . ? F5 As1 F9 F1 -98.2(15) . . . . ? F4 As1 F9 F1 167(2) . . . . ? F6 As1 F9 F1 82.3(15) . . . . ? F10 As1 F9 F4 116(32) . . . . ? F8 As1 F9 F4 -174.5(17) . . . . ? F2 As1 F9 F4 9(2) . . . . ? F7 As1 F9 F4 7.9(15) . . . . ? F3 As1 F9 F4 -177.2(3) . . . . ? F1 As1 F9 F4 -167(2) . . . . ? F5 As1 F9 F4 95.2(11) . . . . ? F6 As1 F9 F4 -84.3(11) . . . . ? F7 F2 F10 F3 4(7) . . . . ? As1 F2 F10 F3 0(4) . . . . ? F7 F2 F10 As1 4(3) . . . . ? F8 F3 F10 F2 0(7) . . . . ? As1 F3 F10 F2 0(4) . . . . ? F8 F3 F10 As1 0(4) . . . . ? F8 As1 F10 F2 180(2) . . . . ? F9 As1 F10 F2 -111(32) . . . . ? F7 As1 F10 F2 -3(2) . . . . ? F3 As1 F10 F2 180(3) . . . . ? F1 As1 F10 F2 176.1(4) . . . . ? F5 As1 F10 F2 -89.9(18) . . . . ? F4 As1 F10 F2 3(3) . . . . ? F6 As1 F10 F2 89.6(18) . . . . ? F8 As1 F10 F3 0.0(18) . . . . ? F2 As1 F10 F3 -180(3) . . . . ? F9 As1 F10 F3 69(32) . . . . ? F7 As1 F10 F3 177.5(17) . . . . ? F1 As1 F10 F3 -4(3) . . . . ? F5 As1 F10 F3 90.3(13) . . . . ? F4 As1 F10 F3 -177.3(3) . . . . ? F6 As1 F10 F3 -90.3(13) . . . . ? S2 S3 N1 C1 1.9(4) . . . . ? S3 N1 C1 Cl1 179.7(2) . . . . ? S3 N1 C1 S1 -0.5(6) . . . . ? S2 S1 C1 N1 -1.2(4) . . . . ? S2 S1 C1 Cl1 178.5(2) . . . . ? #_diffrn_measured_fraction_theta_max 0.999 #_diffrn_reflns_theta_full 30.07 #_diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.755 _refine_diff_density_min -1.092 _refine_diff_density_rms 0.181 # Attachment 'BrCNSSSAsF6.cif' data_jp1 _database_code_depnum_ccdc_archive 'CCDC 273161' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C As Br F6 N S3' _chemical_formula_weight 391.03 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' N N 0.0061 0.0033 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.1479(4) _cell_length_b 7.9522(5) _cell_length_c 9.9240(6) _cell_angle_alpha 88.791(1) _cell_angle_beta 84.421(1) _cell_angle_gamma 70.508(1) _cell_volume 455.17(5) _cell_formula_units_Z 2 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Parralelepiped _exptl_crystal_colour Red/Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 366 _exptl_absorpt_coefficient_mu 8.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(1) _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3186 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1989 _reflns_number_gt 1845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0353P)^2^+0.3375P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1989 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0647 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 C1 C 0.4635(5) 0.7647(4) 0.2323(3) 0.0227(5) Uani 1 1 d . . . N2 N 0.4044(4) 0.7229(3) 0.3528(2) 0.0252(5) Uani 1 1 d . . . S3 S 0.53568(13) 0.75756(9) 0.47830(7) 0.02607(16) Uani 1 1 d . . . S4 S 0.76471(12) 0.87309(10) 0.38288(7) 0.02608(16) Uani 1 1 d . . . S5 S 0.67852(12) 0.85943(10) 0.19285(7) 0.02586(16) Uani 1 1 d . . . Br Br 0.32433(5) 0.72488(4) 0.08442(3) 0.03100(10) Uani 1 1 d . . . As As 0.02648(5) 0.28342(3) 0.24113(3) 0.02016(10) Uani 1 1 d . . . F1 F -0.1441(5) 0.4296(3) 0.1359(3) 0.0593(7) Uani 1 1 d . . . F2 F 0.1995(4) 0.1316(3) 0.3476(2) 0.0471(6) Uani 1 1 d . . . F3 F -0.1770(5) 0.3555(4) 0.3758(3) 0.0718(8) Uani 1 1 d . . . F4 F -0.0887(5) 0.1245(3) 0.2043(3) 0.0664(7) Uani 1 1 d . . . F5 F 0.2317(4) 0.2037(4) 0.1108(2) 0.0667(8) Uani 1 1 d . . . F6 F 0.1420(5) 0.4376(4) 0.2832(3) 0.0725(9) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0219(13) 0.0209(12) 0.0240(14) -0.0037(10) -0.0033(11) -0.0049(10) N2 0.0295(12) 0.0259(12) 0.0212(12) -0.0029(9) -0.0026(10) -0.0102(9) S3 0.0346(4) 0.0263(3) 0.0193(3) 0.0022(3) -0.0042(3) -0.0125(3) S4 0.0235(3) 0.0357(4) 0.0215(4) -0.0014(3) -0.0036(3) -0.0126(3) S5 0.0253(3) 0.0355(4) 0.0189(3) -0.0016(3) -0.0006(3) -0.0133(3) Br 0.02955(17) 0.03947(18) 0.02588(17) -0.00698(12) -0.00656(12) -0.01249(13) As 0.02295(15) 0.02013(15) 0.01773(15) 0.00158(10) -0.00352(11) -0.00725(11) F1 0.0750(16) 0.0377(11) 0.0541(14) 0.0066(10) -0.0363(13) 0.0038(11) F2 0.0661(14) 0.0354(10) 0.0273(10) 0.0032(8) -0.0201(10) 0.0038(9) F3 0.0611(16) 0.0796(18) 0.0507(15) -0.0089(13) 0.0254(12) 0.0005(13) F4 0.0877(19) 0.0568(15) 0.0787(18) 0.0062(13) -0.0280(15) -0.0507(14) F5 0.0582(15) 0.0913(19) 0.0285(12) 0.0049(12) 0.0161(11) -0.0015(13) F6 0.108(2) 0.0619(16) 0.080(2) 0.0172(14) -0.0416(17) -0.0629(16) _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 C1 N2 1.285(4) . ? C1 S5 1.738(3) . ? C1 Br 1.852(3) . ? N2 S3 1.624(2) . ? S3 S4 2.0714(10) . ? S4 S5 2.0224(10) . ? As F6 1.686(2) . ? As F5 1.688(2) . ? As F1 1.700(2) . ? As F4 1.702(2) . ? As F3 1.705(2) . ? As F2 1.7357(18) . ? 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 N2 C1 S5 123.9(2) . . ? N2 C1 Br 121.7(2) . . ? S5 C1 Br 114.34(16) . . ? C1 N2 S3 119.6(2) . . ? N2 S3 S4 102.03(9) . . ? S5 S4 S3 96.62(4) . . ? C1 S5 S4 97.80(10) . . ? F6 As F5 92.68(16) . . ? F6 As F1 90.82(13) . . ? F5 As F1 90.27(13) . . ? F6 As F4 177.94(12) . . ? F5 As F4 88.35(15) . . ? F1 As F4 90.97(13) . . ? F6 As F3 88.45(16) . . ? F5 As F3 177.62(13) . . ? F1 As F3 91.81(14) . . ? F4 As F3 90.46(16) . . ? F6 As F2 90.03(12) . . ? F5 As F2 89.56(11) . . ? F1 As F2 179.14(11) . . ? F4 As F2 88.19(12) . . ? F3 As F2 88.35(13) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.744 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.098 #============================================================================== # 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 #============================================================================== # Attachment 'ICNSSS.cif' data_jp _database_code_depnum_ccdc_archive 'CCDC 273162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C As F6 I N S3' _chemical_formula_weight 438.02 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' N N 0.0061 0.0033 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2389(10) _cell_length_b 8.0343(12) _cell_length_c 10.1430(16) _cell_angle_alpha 87.847(2) _cell_angle_beta 84.629(2) _cell_angle_gamma 70.804(2) _cell_volume 478.03(13) _cell_formula_units_Z 2 _cell_measurement_temperature 198(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Irregular _exptl_crystal_colour Green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.043 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 7.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(1) _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2385 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1550 _reflns_number_gt 1471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0739P)^2^+7.8110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1550 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 C1 C 0.9512(16) 0.7822(12) 0.2351(11) 0.032(2) Uani 1 1 d . . . I I 0.80246(12) 0.74707(10) 0.06837(7) 0.0432(3) Uani 1 1 d . . . N2 N 0.8783(12) 0.7287(9) 0.3535(7) 0.0232(16) Uani 1 1 d . . . S3 S 1.0220(4) 0.7627(3) 0.4788(3) 0.0336(6) Uani 1 1 d . . . S4 S 1.2508(4) 0.8736(4) 0.3856(3) 0.0352(6) Uani 1 1 d . . . S5 S 1.1641(5) 0.8718(4) 0.2012(3) 0.0394(6) Uani 1 1 d . . . As As 0.48391(15) 0.70301(12) 0.74520(10) 0.0259(3) Uani 1 1 d . . . F1 F 0.6066(17) 0.8573(13) 0.7717(10) 0.081(3) Uani 1 1 d . . . F2 F 0.356(2) 0.5555(14) 0.7145(12) 0.096(4) Uani 1 1 d . . . F3 F 0.6591(16) 0.6332(13) 0.6079(9) 0.081(3) Uani 1 1 d . . . F4 F 0.2997(16) 0.8573(10) 0.6510(8) 0.072(3) Uani 1 1 d . . . F5 F 0.3078(16) 0.7808(13) 0.8821(9) 0.078(3) Uani 1 1 d . . . F6 F 0.6615(19) 0.5542(11) 0.8414(10) 0.090(3) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(5) 0.023(5) 0.043(6) -0.012(4) -0.004(4) 0.000(4) I 0.0388(5) 0.0469(5) 0.0401(5) -0.0150(3) -0.0080(3) -0.0061(3) N2 0.024(4) 0.020(4) 0.016(4) -0.007(3) 0.000(3) 0.007(3) S3 0.0360(13) 0.0286(12) 0.0363(14) 0.0005(10) 0.0000(11) -0.0116(10) S4 0.0259(12) 0.0398(14) 0.0394(15) -0.0022(11) -0.0020(10) -0.0101(11) S5 0.0325(14) 0.0447(15) 0.0413(15) -0.0040(12) 0.0017(11) -0.0138(12) As 0.0236(5) 0.0218(5) 0.0304(6) -0.0019(4) -0.0024(4) -0.0048(4) F1 0.096(7) 0.084(6) 0.096(7) -0.010(5) -0.009(5) -0.072(6) F2 0.131(9) 0.081(6) 0.116(9) -0.004(6) -0.025(7) -0.084(7) F3 0.078(6) 0.083(6) 0.063(6) -0.021(5) 0.036(5) -0.009(5) F4 0.091(6) 0.053(5) 0.052(5) -0.003(4) -0.031(4) 0.013(4) F5 0.072(6) 0.090(6) 0.056(5) -0.005(5) 0.031(4) -0.015(5) F6 0.108(8) 0.053(5) 0.085(7) -0.001(5) -0.051(6) 0.020(5) _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 C1 N2 1.350(14) . ? C1 S5 1.710(11) . ? C1 I 2.075(10) . ? N2 S3 1.701(8) . ? S3 S4 2.061(4) . ? S4 S5 1.997(4) . ? As F3 1.679(8) . ? As F2 1.684(8) . ? As F5 1.689(8) . ? As F6 1.689(8) . ? As F1 1.698(7) . ? As F4 1.717(7) . ? 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 N2 C1 S5 128.0(8) . . ? N2 C1 I 118.4(7) . . ? S5 C1 I 113.6(6) . . ? C1 N2 S3 112.3(7) . . ? N2 S3 S4 103.8(3) . . ? S5 S4 S3 97.72(16) . . ? C1 S5 S4 98.1(4) . . ? F3 As F2 88.2(6) . . ? F3 As F5 177.9(5) . . ? F2 As F5 93.5(6) . . ? F3 As F6 92.3(5) . . ? F2 As F6 90.5(6) . . ? F5 As F6 88.9(5) . . ? F3 As F1 91.4(5) . . ? F2 As F1 177.7(5) . . ? F5 As F1 86.8(5) . . ? F6 As F1 91.8(5) . . ? F3 As F4 89.1(5) . . ? F2 As F4 90.0(5) . . ? F5 As F4 89.6(5) . . ? F6 As F4 178.5(5) . . ? F1 As F4 87.8(5) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 3.983 _refine_diff_density_min -1.760 _refine_diff_density_rms 0.257