Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global6 _journal_coden_Cambridge 222 _publ_contact_author_name 'Simon Parsons' _publ_contact_author_address ;School of Chemistry University of Edinburgh Scotland ; _publ_contact_author_email S.Parsons@ed.ac.uk loop_ _publ_author_name _publ_author_address 'Parsons, Simon' ;School of Chemistry University of Edinburgh Scotland ; 'Rankin, D.' ;School of Chemistry University of Edinburgh Scotland ; 'Wood, P.' ;School of Chemistry University of Edinburgh Scotland ; data_ed2275 _database_code_depnum_ccdc_archive 'CCDC 247843' # original edinburgh code so3fnf _audit_creation_date 97-02-12 _audit_creation_method CRYSTALS _computing_data_collection 'Stoe DIF4 (Stoe and Cie, 1990a)' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4 (Stoe and Cie, 1990b)' _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_melting_point 197 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe Stadi-4 diffractometer' _refine_ls_matrix_type full _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary Direct _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _chemical_name_systematic ; ? ; _cell_length_a 6.753(2) _cell_angle_alpha 90 _cell_length_b 18.304(6) _cell_angle_beta 90 _cell_length_c 7.371(2) _cell_angle_gamma 90 _cell_volume 911.1 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z -x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C2 H0 N1 S2 F7 O4 ' _chemical_formula_moiety ' C2 H0 N1 S2 F7 O4 ' _chemical_compound_source ; ? ; _chemical_formula_weight 299.13 _cell_measurement_reflns_used 45 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _cell_measurement_temperature 150(2) _cell_formula_units_Z 4.00 _exptl_crystal_description ' cylinder ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.76 _exptl_crystal_density_diffrn 2.18 _exptl_crystal_density_meas ? _exptl_crystal_F_000 585.37 _exptl_absorpt_coefficient_mu 0.67 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 3 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150(2) _diffrn_reflns_number 5076 _reflns_number_total 2458 _diffrn_reflns_av_R_equivalents 0.08 _reflns_number_observed 1751 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _reflns_limit_h_min 0 _reflns_limit_h_max 9 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min -10 _reflns_limit_l_max 10 _reflns_observed_criterion >2.00\s(I) _refine_special_details ; Used CRYSTALS F-refinement. Crystal not single. Indexed with DIRAX. Some overlap presumably keeping the R-factor quite high. ; _refine_diff_density_min -0.86 _refine_diff_density_max 0.71 _refine_ls_number_reflns 1751 _refine_ls_number_parameters 147 _refine_ls_R_factor_obs 0.0745 _refine_ls_wR_factor_obs 0.0794 _refine_ls_goodness_of_fit_obs 1.1075 _refine_ls_shift/esd_max 0.005595 _refine_ls_abs_structure_details ' from Flack enantiopole 0.0(2)' _refine_ls_structure_factor_coef F _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method omega-theta loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type N1 0.8536(7) 0.8573(3) -0.0685(7) 0.0292 1.0000 Uani S11 0.8470(2) 0.90467(8) -0.2683(3) 0.0363 1.0000 Uani S12 0.6616(2) 0.82718(7) 0.0557(2) 0.0295 1.0000 Uani C21 1.024(1) 0.8492(4) -0.3968(9) 0.0395 1.0000 Uani C22 0.542(1) 0.9114(4) 0.135(1) 0.0434 1.0000 Uani F1 1.0066(6) 0.8820(3) 0.0402(7) 0.0487 1.0000 Uani F11 0.9557(8) 0.7835(2) -0.4200(6) 0.0514 1.0000 Uani F12 0.4013(8) 0.8939(4) 0.250(1) 0.0722 1.0000 Uani F21 1.1940(7) 0.8462(3) -0.3111(7) 0.0592 1.0000 Uani F22 0.6715(8) 0.9514(3) 0.225(1) 0.0675 1.0000 Uani F31 1.0473(8) 0.8812(3) -0.5546(6) 0.0547 1.0000 Uani F32 0.465(1) 0.9468(3) 0.0010(8) 0.0707 1.0000 Uani O11 0.6585(7) 0.8936(4) -0.3429(8) 0.0488 1.0000 Uani O12 0.5312(8) 0.7939(3) -0.0708(7) 0.0427 1.0000 Uani O21 0.933(1) 0.9733(3) -0.238(1) 0.0631 1.0000 Uani O22 0.7434(9) 0.7923(3) 0.2078(6) 0.0483 1.0000 Uani 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 N1 0.021(2) 0.043(3) 0.028(2) 0.002(2) 0.000(2) 0.001(2) S11 0.0396(8) 0.0325(6) 0.0456(8) 0.0137(6) 0.0102(9) 0.0063(6) S12 0.0319(6) 0.0307(6) 0.0266(5) -0.0006(5) 0.0016(7) -0.0027(5) C21 0.039(3) 0.052(4) 0.034(3) 0.011(3) 0.007(3) 0.004(3) C22 0.038(3) 0.054(4) 0.048(4) -0.017(3) 0.005(3) 0.009(3) F1 0.032(2) 0.084(3) 0.046(2) -0.012(2) -0.002(2) -0.008(2) F11 0.080(3) 0.045(2) 0.038(2) -0.001(2) 0.000(2) 0.002(2) F12 0.052(3) 0.126(5) 0.073(3) -0.013(4) 0.025(3) 0.010(3) F21 0.035(2) 0.111(4) 0.058(3) 0.001(3) -0.001(2) 0.018(3) F22 0.066(3) 0.070(3) 0.111(5) -0.054(3) 0.013(4) -0.001(3) F31 0.067(3) 0.080(3) 0.042(2) 0.022(2) 0.018(2) -0.000(3) F32 0.128(6) 0.084(4) 0.065(3) 0.005(3) 0.006(4) 0.072(4) O11 0.034(2) 0.093(4) 0.051(3) 0.031(3) 0.006(3) 0.019(3) O12 0.053(3) 0.045(2) 0.045(3) -0.006(2) -0.001(2) -0.024(2) O21 0.115(6) 0.032(2) 0.087(5) 0.004(3) 0.036(5) -0.015(3) O22 0.068(3) 0.055(3) 0.032(2) 0.009(2) 0.002(2) 0.009(2) _refine_ls_extinction_coef 6.8(192) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 . S11 . 1.710(5) yes N1 . S12 . 1.680(5) yes N1 . F1 . 1.384(6) yes S11 . C21 . 1.832(7) yes S11 . O11 . 1.401(6) yes S11 . O21 . 1.401(6) yes S12 . C22 . 1.837(7) yes S12 . O12 . 1.419(5) yes S12 . O22 . 1.403(5) yes C21 . F11 . 1.298(8) yes C21 . F21 . 1.312(8) yes C21 . F31 . 1.312(8) yes C22 . F12 . 1.308(9) yes C22 . F22 . 1.319(9) yes C22 . F32 . 1.29(1) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S11 . N1 . S12 . 128.0(3) no S11 . N1 . F1 . 110.6(4) no S12 . N1 . F1 . 111.6(4) no N1 . S11 . C21 . 98.5(3) no N1 . S11 . O11 . 106.8(3) no C21 . S11 . O11 . 108.0(4) no N1 . S11 . O21 . 108.0(4) no C21 . S11 . O21 . 108.0(4) no O11 . S11 . O21 . 124.5(5) no N1 . S12 . C22 . 103.8(3) no N1 . S12 . O12 . 105.2(3) no C22 . S12 . O12 . 107.3(3) no N1 . S12 . O22 . 106.3(3) no C22 . S12 . O22 . 107.4(3) no O12 . S12 . O22 . 125.0(3) no S11 . C21 . F11 . 110.5(5) no S11 . C21 . F21 . 110.2(5) no F11 . C21 . F21 . 109.6(6) no S11 . C21 . F31 . 106.8(5) no F11 . C21 . F31 . 109.9(6) no F21 . C21 . F31 . 109.9(6) no S12 . C22 . F12 . 108.7(6) no S12 . C22 . F22 . 109.5(5) no F12 . C22 . F22 . 107.1(7) no S12 . C22 . F32 . 110.7(5) no F12 . C22 . F32 . 108.8(7) no F22 . C22 . F32 . 111.9(8) no