# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Anthony Cheetham' _publ_contact_author_email AKC30@CAM.AC.UK _publ_section_title ; A Hybrid Cobalt Disulfonate with a Novel Inorganic Layer Architecture Exhibiting a Field-Induced Magnetic Transition ; loop_ _publ_author_name 'A. Cheetham' 'Russell Feller' 'Paul M. Forster' 'Brent C. Melot' # Attachment 'Feller_et_al.CIF' data_sulfonate _database_code_depnum_ccdc_archive 'CCDC 702928' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H8 Co3 O10 S2' _chemical_formula_weight 432.99 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' O O 0.0106 0.0060 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9462(6) _cell_length_b 5.2818(4) _cell_length_c 10.1259(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.297(2) _cell_angle_gamma 90.00 _cell_volume 477.68(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 426 _exptl_absorpt_coefficient_mu 5.630 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3847 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.09 _reflns_number_total 1005 _reflns_number_gt 935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0365P)^2^+0.7181P] 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 0.047(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1005 _refine_ls_number_parameters 94 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Co1 Co 0.0000 0.0000 0.0000 0.01136(19) Uani 1 2 d S . . Co2 Co -0.08008(4) -0.47867(7) 0.14015(3) 0.01213(18) Uani 1 1 d . . . S1 S -0.32076(7) -0.00118(11) 0.15381(6) 0.0125(2) Uani 1 1 d . . . C1 C -0.4973(3) 0.0502(6) 0.0700(3) 0.0161(5) Uani 1 1 d D . . O1 O -0.2902(2) -0.2734(4) 0.15142(19) 0.0197(4) Uani 1 1 d . . . O2 O -0.2120(2) 0.1445(4) 0.07906(18) 0.0170(4) Uani 1 1 d . . . O3 O -0.3333(2) 0.0935(4) 0.28740(18) 0.0205(4) Uani 1 1 d . . . O4 O -0.0571(2) 0.1543(4) -0.18207(16) 0.0140(4) Uani 1 1 d . . . O5 O -0.0916(2) -0.3375(3) -0.05125(18) 0.0144(4) Uani 1 1 d . . . H1 H -0.506(4) 0.235(6) 0.070(3) 0.031(7) Uiso 1 1 d D . . H2 H -0.558(4) -0.037(6) 0.134(3) 0.031(7) Uiso 1 1 d D . . H3 H -0.141(4) 0.216(7) -0.174(3) 0.030(7) Uiso 1 1 d . . . H4 H -0.171(4) -0.341(7) -0.092(3) 0.030(7) Uiso 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 Co1 0.0132(3) 0.0108(3) 0.0099(3) 0.00022(15) -0.0007(2) 0.00006(16) Co2 0.0131(3) 0.0132(2) 0.0100(2) 0.00104(11) 0.00031(15) 0.00066(12) S1 0.0093(3) 0.0157(4) 0.0121(4) -0.0002(2) -0.0009(2) 0.0005(2) C1 0.0095(12) 0.0220(13) 0.0164(14) -0.0022(11) -0.0021(10) 0.0011(10) O1 0.0168(9) 0.0150(9) 0.0272(10) 0.0027(8) 0.0017(7) 0.0019(7) O2 0.0145(9) 0.0176(10) 0.0191(9) 0.0012(7) 0.0016(7) -0.0008(7) O3 0.0168(9) 0.0294(11) 0.0153(9) -0.0036(8) 0.0006(7) -0.0002(8) O4 0.0140(9) 0.0145(9) 0.0132(9) -0.0006(6) -0.0020(7) 0.0026(7) O5 0.0130(9) 0.0160(9) 0.0140(8) -0.0012(7) -0.0018(7) 0.0005(7) _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 Co1 O5 2.0171(18) . ? Co1 O5 2.0171(18) 3 ? Co1 O4 2.0532(17) 3 ? Co1 O4 2.0532(17) . ? Co1 O2 2.2349(18) . ? Co1 O2 2.2349(18) 3 ? Co2 O4 2.0250(17) 4_556 ? Co2 O5 2.0667(18) 3_545 ? Co2 O5 2.0736(19) . ? Co2 O4 2.1362(19) 3 ? Co2 O1 2.1787(19) . ? Co2 O2 2.3774(19) 1_545 ? S1 O3 1.4526(19) . ? S1 O1 1.464(2) . ? S1 O2 1.4822(19) . ? S1 C1 1.771(3) . ? C1 C1 1.512(5) 3_455 ? C1 H1 0.98(3) . ? C1 H2 0.99(3) . ? O2 Co2 2.3774(19) 1_565 ? O4 Co2 2.0250(17) 4 ? O4 Co2 2.1362(19) 3 ? O4 H3 0.83(4) . ? O5 Co2 2.0667(18) 3_545 ? O5 H4 0.80(4) . ? 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 O5 Co1 O5 180.00(11) . 3 ? O5 Co1 O4 87.53(7) . 3 ? O5 Co1 O4 92.47(7) 3 3 ? O5 Co1 O4 92.47(7) . . ? O5 Co1 O4 87.53(7) 3 . ? O4 Co1 O4 180.00(11) 3 . ? O5 Co1 O2 93.06(7) . . ? O5 Co1 O2 86.94(7) 3 . ? O4 Co1 O2 89.23(7) 3 . ? O4 Co1 O2 90.77(7) . . ? O5 Co1 O2 86.94(7) . 3 ? O5 Co1 O2 93.06(7) 3 3 ? O4 Co1 O2 90.77(7) 3 3 ? O4 Co1 O2 89.23(7) . 3 ? O2 Co1 O2 180.00(9) . 3 ? O4 Co2 O5 97.60(7) 4_556 3_545 ? O4 Co2 O5 173.06(7) 4_556 . ? O5 Co2 O5 76.12(8) 3_545 . ? O4 Co2 O4 99.38(4) 4_556 3 ? O5 Co2 O4 91.75(7) 3_545 3 ? O5 Co2 O4 83.93(7) . 3 ? O4 Co2 O1 103.00(7) 4_556 . ? O5 Co2 O1 157.17(8) 3_545 . ? O5 Co2 O1 82.72(7) . . ? O4 Co2 O1 94.48(7) 3 . ? O4 Co2 O2 82.61(7) 4_556 1_545 ? O5 Co2 O2 82.15(7) 3_545 1_545 ? O5 Co2 O2 93.48(7) . 1_545 ? O4 Co2 O2 173.80(7) 3 1_545 ? O1 Co2 O2 90.76(7) . 1_545 ? O3 S1 O1 112.21(12) . . ? O3 S1 O2 112.65(12) . . ? O1 S1 O2 111.89(11) . . ? O3 S1 C1 106.19(12) . . ? O1 S1 C1 107.76(13) . . ? O2 S1 C1 105.63(12) . . ? C1 C1 S1 112.0(2) 3_455 . ? C1 C1 H1 110.6(19) 3_455 . ? S1 C1 H1 103(2) . . ? C1 C1 H2 118(2) 3_455 . ? S1 C1 H2 97(2) . . ? H1 C1 H2 115(3) . . ? S1 O1 Co2 130.69(11) . . ? S1 O2 Co1 126.95(11) . . ? S1 O2 Co2 129.23(11) . 1_565 ? Co1 O2 Co2 87.73(6) . 1_565 ? Co2 O4 Co1 128.59(10) 4 . ? Co2 O4 Co2 124.87(9) 4 3 ? Co1 O4 Co2 91.68(7) . 3 ? Co2 O4 H3 103(2) 4 . ? Co1 O4 H3 104(2) . . ? Co2 O4 H3 100(3) 3 . ? Co1 O5 Co2 103.08(8) . 3_545 ? Co1 O5 Co2 94.58(8) . . ? Co2 O5 Co2 103.88(8) 3_545 . ? Co1 O5 H4 119(3) . . ? Co2 O5 H4 115(2) 3_545 . ? Co2 O5 H4 118(2) . . ? 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 O3 S1 C1 C1 -177.6(3) . . . 3_455 ? O1 S1 C1 C1 -57.2(3) . . . 3_455 ? O2 S1 C1 C1 62.6(3) . . . 3_455 ? O3 S1 O1 Co2 -97.11(16) . . . . ? O2 S1 O1 Co2 30.65(19) . . . . ? C1 S1 O1 Co2 146.34(15) . . . . ? O4 Co2 O1 S1 113.78(15) 4_556 . . . ? O5 Co2 O1 S1 -92.3(2) 3_545 . . . ? O5 Co2 O1 S1 -70.22(16) . . . . ? O4 Co2 O1 S1 13.07(16) 3 . . . ? O2 Co2 O1 S1 -163.63(16) 1_545 . . . ? O3 S1 O2 Co1 116.79(14) . . . . ? O1 S1 O2 Co1 -10.74(17) . . . . ? C1 S1 O2 Co1 -127.72(14) . . . . ? O3 S1 O2 Co2 -6.59(18) . . . 1_565 ? O1 S1 O2 Co2 -134.11(13) . . . 1_565 ? C1 S1 O2 Co2 108.91(15) . . . 1_565 ? O5 Co1 O2 S1 38.04(14) . . . . ? O5 Co1 O2 S1 -141.96(14) 3 . . . ? O4 Co1 O2 S1 -49.44(14) 3 . . . ? O4 Co1 O2 S1 130.56(14) . . . . ? O2 Co1 O2 S1 -169(100) 3 . . . ? O5 Co1 O2 Co2 177.70(6) . . . 1_565 ? O5 Co1 O2 Co2 -2.30(6) 3 . . 1_565 ? O4 Co1 O2 Co2 90.22(7) 3 . . 1_565 ? O4 Co1 O2 Co2 -89.78(7) . . . 1_565 ? O2 Co1 O2 Co2 -29(100) 3 . . 1_565 ? O5 Co1 O4 Co2 -29.56(12) . . . 4 ? O5 Co1 O4 Co2 150.44(12) 3 . . 4 ? O4 Co1 O4 Co2 53(46) 3 . . 4 ? O2 Co1 O4 Co2 -122.66(12) . . . 4 ? O2 Co1 O4 Co2 57.34(12) 3 . . 4 ? O5 Co1 O4 Co2 -168.60(7) . . . 3 ? O5 Co1 O4 Co2 11.40(7) 3 . . 3 ? O4 Co1 O4 Co2 -86(46) 3 . . 3 ? O2 Co1 O4 Co2 98.30(7) . . . 3 ? O2 Co1 O4 Co2 -81.70(7) 3 . . 3 ? O5 Co1 O5 Co2 46(100) 3 . . 3_545 ? O4 Co1 O5 Co2 -93.62(9) 3 . . 3_545 ? O4 Co1 O5 Co2 86.38(9) . . . 3_545 ? O2 Co1 O5 Co2 177.28(7) . . . 3_545 ? O2 Co1 O5 Co2 -2.72(7) 3 . . 3_545 ? O5 Co1 O5 Co2 152(100) 3 . . . ? O4 Co1 O5 Co2 11.78(8) 3 . . . ? O4 Co1 O5 Co2 -168.22(8) . . . . ? O2 Co1 O5 Co2 -77.31(7) . . . . ? O2 Co1 O5 Co2 102.69(7) 3 . . . ? O4 Co2 O5 Co1 -130.3(6) 4_556 . . . ? O5 Co2 O5 Co1 -104.69(10) 3_545 . . . ? O4 Co2 O5 Co1 -11.37(7) 3 . . . ? O1 Co2 O5 Co1 83.96(8) . . . . ? O2 Co2 O5 Co1 174.28(7) 1_545 . . . ? O4 Co2 O5 Co2 -25.6(7) 4_556 . . 3_545 ? O5 Co2 O5 Co2 0.0 3_545 . . 3_545 ? O4 Co2 O5 Co2 93.32(8) 3 . . 3_545 ? O1 Co2 O5 Co2 -171.35(9) . . . 3_545 ? O2 Co2 O5 Co2 -81.03(8) 1_545 . . 3_545 ? 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 O4 H3 O3 0.83(4) 2.01(4) 2.809(3) 161(3) 4_565 O5 H4 O3 0.80(4) 2.27(4) 2.961(3) 144(4) 4 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.521 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.131