Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_cam127 _database_code_CSD 176424 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Wood, Paul' 'Bond, Andrew' 'Cave, Dale' 'Gascon, Jose-Miguel' 'Teat, Simon J.' _publ_contact_author_name 'Dr Paul Wood' _publ_contact_author_address ; University Chemical Laboratory Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email 'PTW22@CAM.AC.UK' _publ_section_title ; Layered metal organosulfides: Hydrothermal synthesis, structure and magnetic behaviour of the spin-canted metamagnet Co(1,2-(O2C)(S)C6H4 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C7 H4 O2 S2 2-, Co 2+' _chemical_formula_sum 'C7 H4 Co O2 S' _chemical_formula_weight 211.09 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 C2/c 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' '-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 27.890(2) _cell_length_b 7.6926(6) _cell_length_c 6.7497(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.895(2) _cell_angle_gamma 90.00 _cell_volume 1405.77(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3723 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 28.97 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 2.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7401 _exptl_absorpt_correction_T_max 0.9738 _exptl_absorpt_process_details ; Correction applied by SADABS - note that the transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). The numbers listed in the CIF are those calculated by SHELXL. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6904 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS, Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method 'Thin slice \w-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_reflns_number 4566 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.98 _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 28.98 _diffrn_measured_fraction_theta_full 0.910 _reflns_number_total 1865 _reflns_number_gt 1505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0597P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1865 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.370 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.264 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.222277(13) 0.94125(5) -0.00883(5) 0.01089(13) Uani 1 1 d . . . S1 S 0.16904(2) 1.06744(9) 0.17305(10) 0.01221(16) Uani 1 1 d . . . O1 O 0.22908(7) 0.7252(2) 0.1580(3) 0.0124(4) Uani 1 1 d . . . O2 O 0.21298(7) 0.5579(3) 0.4034(3) 0.0148(4) Uani 1 1 d . . . C1 C 0.14628(10) 0.7142(4) 0.2041(4) 0.0131(5) Uani 1 1 d . . . C2 C 0.12934(10) 0.8847(4) 0.1572(4) 0.0136(5) Uani 1 1 d . . . C3 C 0.07869(11) 0.9139(4) 0.0997(5) 0.0210(6) Uani 1 1 d . . . H3A H 0.0667 1.0284 0.0659 0.025 Uiso 1 1 calc R . . C4 C 0.04533(12) 0.7785(5) 0.0910(5) 0.0274(7) Uani 1 1 d . . . H4A H 0.0108 0.8006 0.0500 0.033 Uiso 1 1 calc R . . C5 C 0.06224(12) 0.6110(5) 0.1419(5) 0.0256(7) Uani 1 1 d . . . H5A H 0.0394 0.5186 0.1376 0.031 Uiso 1 1 calc R . . C6 C 0.11254(11) 0.5792(4) 0.1989(4) 0.0193(6) Uani 1 1 d . . . H6A H 0.1242 0.4646 0.2348 0.023 Uiso 1 1 calc R . . C7 C 0.19961(10) 0.6642(3) 0.2601(4) 0.0120(5) 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 Co1 0.0134(2) 0.00845(19) 0.01116(19) 0.00063(13) 0.00354(14) -0.00019(13) S1 0.0150(3) 0.0102(3) 0.0118(3) 0.0002(2) 0.0041(2) 0.0017(2) O1 0.0151(9) 0.0091(9) 0.0144(9) 0.0014(7) 0.0067(7) 0.0012(7) O2 0.0175(10) 0.0118(10) 0.0164(9) 0.0037(8) 0.0068(8) 0.0011(7) C1 0.0131(12) 0.0151(14) 0.0118(11) -0.0012(10) 0.0043(10) -0.0007(10) C2 0.0146(13) 0.0154(13) 0.0115(12) 0.0003(10) 0.0042(10) 0.0008(10) C3 0.0162(15) 0.0212(16) 0.0245(15) 0.0026(12) 0.0029(12) 0.0046(11) C4 0.0134(14) 0.0340(19) 0.0334(17) 0.0012(15) 0.0030(13) -0.0005(13) C5 0.0164(15) 0.0292(18) 0.0301(17) 0.0015(14) 0.0034(13) -0.0074(13) C6 0.0198(15) 0.0185(15) 0.0196(14) 0.0017(11) 0.0047(12) -0.0032(11) C7 0.0149(13) 0.0081(12) 0.0129(12) -0.0029(10) 0.0030(10) -0.0006(9) _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 O2 1.989(2) 4 ? Co1 O1 1.9906(19) . ? Co1 O1 2.2693(19) 7_565 ? Co1 S1 2.2996(7) 6_575 ? Co1 S1 2.3515(7) . ? S1 C2 1.777(3) . ? S1 Co1 2.2996(7) 6_576 ? O1 C7 1.282(3) . ? O1 Co1 2.2693(19) 7_565 ? O2 C7 1.253(3) . ? O2 Co1 1.989(2) 4_545 ? C1 C6 1.397(4) . ? C1 C2 1.404(4) . ? C1 C7 1.494(4) . ? C2 C3 1.390(4) . ? C3 C4 1.389(5) . ? C3 H3A 0.9500 . ? C4 C5 1.387(5) . ? C4 H4A 0.9500 . ? C5 C6 1.385(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? 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 Co1 O1 102.66(8) 4 . ? O2 Co1 O1 79.93(7) 4 7_565 ? O1 Co1 O1 78.10(8) . 7_565 ? O2 Co1 S1 132.41(6) 4 6_575 ? O1 Co1 S1 117.15(6) . 6_575 ? O1 Co1 S1 83.69(5) 7_565 6_575 ? O2 Co1 S1 105.06(6) 4 . ? O1 Co1 S1 92.05(6) . . ? O1 Co1 S1 169.82(5) 7_565 . ? S1 Co1 S1 98.77(3) 6_575 . ? C2 S1 Co1 106.66(9) . 6_576 ? C2 S1 Co1 95.99(9) . . ? Co1 S1 Co1 97.38(3) 6_576 . ? C7 O1 Co1 128.57(17) . . ? C7 O1 Co1 124.11(17) . 7_565 ? Co1 O1 Co1 101.90(8) . 7_565 ? C7 O2 Co1 130.33(18) . 4_545 ? C6 C1 C2 120.1(3) . . ? C6 C1 C7 116.0(3) . . ? C2 C1 C7 123.9(2) . . ? C3 C2 C1 118.6(3) . . ? C3 C2 S1 117.8(2) . . ? C1 C2 S1 123.7(2) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3A 119.5 . . ? C2 C3 H3A 119.5 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C6 C5 C4 119.7(3) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? O2 C7 O1 122.9(2) . . ? O2 C7 C1 117.2(2) . . ? O1 C7 C1 119.8(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 O2 Co1 S1 C2 -152.34(11) 4 . . . ? O1 Co1 S1 C2 -48.64(11) . . . . ? O1 Co1 S1 C2 -34.1(3) 7_565 . . . ? S1 Co1 S1 C2 69.23(9) 6_575 . . . ? O2 Co1 S1 Co1 -44.62(7) 4 . . 6_576 ? O1 Co1 S1 Co1 59.07(6) . . . 6_576 ? O1 Co1 S1 Co1 73.7(3) 7_565 . . 6_576 ? S1 Co1 S1 Co1 176.94(3) 6_575 . . 6_576 ? O2 Co1 O1 C7 129.0(2) 4 . . . ? O1 Co1 O1 C7 -154.3(3) 7_565 . . . ? S1 Co1 O1 C7 -77.8(2) 6_575 . . . ? S1 Co1 O1 C7 23.1(2) . . . . ? O2 Co1 O1 Co1 -76.68(9) 4 . . 7_565 ? O1 Co1 O1 Co1 0.0 7_565 . . 7_565 ? S1 Co1 O1 Co1 76.45(8) 6_575 . . 7_565 ? S1 Co1 O1 Co1 177.39(6) . . . 7_565 ? C6 C1 C2 C3 -2.0(4) . . . . ? C7 C1 C2 C3 177.6(3) . . . . ? C6 C1 C2 S1 176.3(2) . . . . ? C7 C1 C2 S1 -4.1(4) . . . . ? Co1 S1 C2 C3 127.5(2) 6_576 . . . ? Co1 S1 C2 C3 -132.9(2) . . . . ? Co1 S1 C2 C1 -50.8(2) 6_576 . . . ? Co1 S1 C2 C1 48.7(2) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? S1 C2 C3 C4 -177.7(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C4 C5 C6 C1 -0.5(5) . . . . ? C2 C1 C6 C5 1.9(4) . . . . ? C7 C1 C6 C5 -177.7(3) . . . . ? Co1 O2 C7 O1 -3.9(4) 4_545 . . . ? Co1 O2 C7 C1 173.69(17) 4_545 . . . ? Co1 O1 C7 O2 -159.0(2) . . . . ? Co1 O1 C7 O2 51.8(3) 7_565 . . . ? Co1 O1 C7 C1 23.5(3) . . . . ? Co1 O1 C7 C1 -125.7(2) 7_565 . . . ? C6 C1 C7 O2 -42.2(3) . . . . ? C2 C1 C7 O2 138.2(3) . . . . ? C6 C1 C7 O1 135.5(3) . . . . ? C2 C1 C7 O1 -44.1(4) . . . . ? #==END