# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Stride, John' _publ_contact_author_email j.stride@unsw.edu.au _publ_section_title ; Four new coordination polymers constructed from benzene tricarboxylic acid: synthesis, crystal structure, thermal and magnetic properties ; loop_ _publ_author_name J.Stride M.Nadeem M.Bhadbhade data_arif48c2 _database_code_depnum_ccdc_archive 'CCDC 779475' #TrackingRef 'deposition_ARIF48C2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H14 Co1.50 F O12' _chemical_formula_weight 421.60 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' F F 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 17.4095(19) _cell_length_b 12.9460(10) _cell_length_c 6.5020(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.889(3) _cell_angle_gamma 90.00 _cell_volume 1359.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2123 _cell_measurement_theta_min 2.502 _cell_measurement_theta_max 28.129 _exptl_crystal_description 'Thin plates' _exptl_crystal_colour 'Light pink' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 854 _exptl_absorpt_coefficient_mu 1.932 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8199 _exptl_absorpt_correction_T_max 0.9355 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker kappa APEXII CCD Area Detector' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4416 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2325 _reflns_number_gt 2210 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_cell_refinement ; APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA) ; _computing_data_reduction ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_structure_solution 'SHELXS-97. Sheldrick, G. M. (2008)' _computing_structure_refinement 'SHELXL-97. Sheldrick, G. M. (2008)' _computing_molecular_graphics 'SHELXTL-Plus. Sheldrick, G. M. (2008)' _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^)+(0.1000P)^2^+0.5000P] 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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _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 2325 _refine_ls_number_parameters 236 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 0.781 _refine_ls_restrained_S_all 0.779 _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 -0.19923(7) 0.0000 0.0149(3) Uani 1 2 d S . . O1W O 0.2352(2) 0.5804(3) -0.0295(6) 0.0196(8) Uani 1 1 d D . . H1O1 H 0.187(3) 0.577(7) -0.174(6) 0.060 Uiso 1 1 d D . . H2O1 H 0.243(5) 0.656(7) -0.039(15) 0.060 Uiso 1 1 d . . . O2W O 0.2781(2) 0.4515(3) 0.6052(6) 0.0211(8) Uani 1 1 d . . . H2O2 H 0.3195 0.4800 0.7003 0.032 Uiso 1 1 calc R . . H1O2 H 0.258(4) 0.398(6) 0.626(10) 0.024(18) Uiso 1 1 d . . . O3W O 0.1778(2) 0.6196(3) 0.3415(7) 0.0158(8) Uani 1 1 d . . . H1O3 H 0.209(5) 0.661(7) 0.378(14) 0.05(3) Uiso 1 1 d . . . O4W O 0.3406(2) 0.4026(3) 0.2487(6) 0.0169(8) Uani 1 1 d D . . H1O4 H 0.374(4) 0.412(6) 0.154(9) 0.033(16) Uiso 1 1 d D . . H2O4 H 0.293(3) 0.354(5) 0.190(11) 0.05(2) Uiso 1 1 d D . . C1A C 0.4268(3) 0.7768(4) 0.4609(8) 0.0122(10) Uani 1 1 d . . . C2A C 0.4264(3) 0.8836(4) 0.4598(8) 0.0122(10) Uani 1 1 d . . . H2A H 0.3761 0.9201 0.4318 0.015 Uiso 1 1 calc R . . C3A C 0.5000 0.9376(6) 0.5000 0.0128(13) Uani 1 2 d SU . . C6A C 0.5000 0.7229(5) 0.5000 0.0121(13) Uani 1 2 d S . . H6A H 0.5000 0.6495 0.5000 0.015 Uiso 1 2 calc SR . . C7A C 0.3491(3) 0.7153(4) 0.4228(7) 0.0111(9) Uani 1 1 d . . . C8A C 0.5000 1.0536(6) 0.5000 0.0148(14) Uani 1 2 d SU . . O1A O 0.3534(2) 0.6189(3) 0.4024(6) 0.0160(8) Uani 1 1 d . . . O2A O 0.2851(2) 0.7621(3) 0.4177(6) 0.0184(8) Uani 1 1 d . . . O3A O 0.4314(3) 1.0999(3) 0.4369(7) 0.0253(10) Uani 1 1 d . . . Co2 Co 0.25834(4) 0.51368(5) 0.28599(10) 0.0119(2) Uani 1 1 d . . . O5 O 0.0572(2) -0.2044(3) 0.3510(6) 0.0222(8) Uani 1 1 d . . . O6W O 0.0844(3) -0.2950(4) -0.0380(7) 0.0317(11) Uani 1 1 d D . . H1O6 H 0.073(3) -0.326(4) -0.182(10) 0.012(14) Uiso 1 1 d . . . H2O6 H 0.098(5) -0.343(5) 0.091(9) 0.060 Uiso 1 1 d D . . C1B C 0.0742(3) 0.2690(4) 0.0429(8) 0.0143(11) Uani 1 1 d . . . C2B C 0.0731(3) 0.1617(4) 0.0393(8) 0.0111(10) Uani 1 1 d . . . H2B H 0.1230 0.1249 0.0639 0.013 Uiso 1 1 calc R . . C3B C 0.0000 0.1075(5) 0.0000 0.0136(15) Uani 1 2 d S . . C6B C 0.0000 0.3233(6) 0.0000 0.0131(14) Uani 1 2 d S . . H6B H 0.0000 0.3967 0.0000 0.016 Uiso 1 2 calc SR . . C7B C 0.1554(3) 0.3253(4) 0.0969(7) 0.0125(10) Uani 1 1 d . . . C8B C 0.0000 -0.0053(6) 0.0000 0.0145(16) Uani 1 2 d S . . O1B O 0.1574(2) 0.4185(3) 0.1476(6) 0.0151(8) Uani 1 1 d . . . O2B O 0.2161(2) 0.2742(3) 0.0895(6) 0.0180(8) Uani 1 1 d . . . O3B O 0.0656(2) -0.0564(3) 0.0233(6) 0.0166(8) 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 0.0140(5) 0.0084(5) 0.0222(5) 0.000 0.0064(4) 0.000 O1W 0.021(2) 0.016(2) 0.023(2) 0.0057(15) 0.0094(16) -0.0001(16) O2W 0.0155(19) 0.015(2) 0.025(2) 0.0064(16) -0.0018(15) -0.0048(18) O3W 0.0135(19) 0.011(2) 0.022(2) -0.0004(16) 0.0067(16) -0.0009(15) O4W 0.0136(18) 0.0119(19) 0.0262(19) -0.0024(16) 0.0084(15) 0.0003(15) C1A 0.011(3) 0.013(3) 0.012(2) 0.0028(18) 0.004(2) 0.0007(18) C2A 0.012(2) 0.012(3) 0.012(2) 0.000(2) 0.0038(19) 0.005(2) C3A 0.021(3) 0.007(3) 0.019(3) 0.000 0.017(2) 0.000 C6A 0.021(3) 0.002(3) 0.013(3) 0.000 0.007(3) 0.000 C7A 0.012(2) 0.010(2) 0.010(2) 0.0019(19) 0.0022(18) 0.003(2) C8A 0.025(3) 0.005(3) 0.021(3) 0.000 0.017(3) 0.000 O1A 0.0126(18) 0.0075(18) 0.025(2) -0.0031(15) 0.0030(16) -0.0035(13) O2A 0.0133(18) 0.0155(19) 0.029(2) -0.0032(15) 0.0113(16) -0.0013(14) O3A 0.031(2) 0.012(2) 0.045(3) 0.0076(18) 0.028(2) 0.0058(18) Co2 0.0100(3) 0.0078(3) 0.0174(3) 0.0000(3) 0.0046(2) -0.0008(3) O5 0.027(2) 0.0150(19) 0.0205(18) -0.0024(16) 0.0042(16) -0.0044(17) O6W 0.034(2) 0.035(3) 0.023(2) 0.000(2) 0.0066(19) 0.025(2) C1B 0.015(3) 0.016(3) 0.012(2) -0.0022(19) 0.004(2) -0.0013(19) C2B 0.010(3) 0.012(2) 0.012(2) 0.0017(18) 0.005(2) 0.0032(19) C3B 0.015(4) 0.009(4) 0.010(3) 0.000 -0.003(3) 0.000 C6B 0.019(4) 0.017(4) 0.003(3) 0.000 0.004(3) 0.000 C7B 0.016(2) 0.014(3) 0.008(2) 0.0000(18) 0.0040(18) -0.003(2) C8B 0.015(3) 0.017(4) 0.012(3) 0.000 0.006(3) 0.000 O1B 0.0124(18) 0.0097(19) 0.0218(18) -0.0045(15) 0.0049(15) -0.0025(14) O2B 0.0144(18) 0.0149(19) 0.028(2) -0.0065(15) 0.0110(16) -0.0035(14) O3B 0.0113(18) 0.0126(19) 0.028(2) -0.0005(16) 0.0095(16) -0.0004(15) _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 O6W 2.008(4) 2 ? Co1 O6W 2.008(4) . ? Co1 O5 2.124(4) 2 ? Co1 O5 2.124(4) . ? Co1 O3B 2.148(4) . ? Co1 O3B 2.148(4) 2 ? Co1 C8B 2.510(7) . ? O1W Co2 2.121(4) . ? O2W Co2 2.131(4) . ? O3W Co2 2.088(4) . ? O4W Co2 2.106(4) . ? C1A C2A 1.382(8) . ? C1A C6A 1.390(6) . ? C1A C7A 1.510(7) . ? C2A C3A 1.396(6) . ? C3A C2A 1.396(6) 2_656 ? C3A C8A 1.502(10) . ? C6A C1A 1.390(6) 2_656 ? C7A O2A 1.257(6) . ? C7A O1A 1.261(6) . ? C8A O3A 1.261(5) 2_656 ? C8A O3A 1.261(5) . ? O1A Co2 2.057(3) . ? Co2 O1B 2.058(4) . ? C1B C2B 1.389(7) . ? C1B C6B 1.404(6) . ? C1B C7B 1.511(7) . ? C2B C3B 1.392(6) . ? C3B C2B 1.392(6) 2 ? C3B C8B 1.461(10) . ? C6B C1B 1.404(6) 2 ? C7B O1B 1.247(7) . ? C7B O2B 1.263(6) . ? C8B O3B 1.279(5) 2 ? C8B O3B 1.279(5) . ? 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 O6W Co1 O6W 103.7(3) 2 . ? O6W Co1 O5 92.38(16) 2 2 ? O6W Co1 O5 85.40(16) . 2 ? O6W Co1 O5 85.40(16) 2 . ? O6W Co1 O5 92.38(16) . . ? O5 Co1 O5 176.4(2) 2 . ? O6W Co1 O3B 156.51(17) 2 . ? O6W Co1 O3B 98.37(18) . . ? O5 Co1 O3B 97.28(15) 2 . ? O5 Co1 O3B 85.82(15) . . ? O6W Co1 O3B 98.37(18) 2 2 ? O6W Co1 O3B 156.51(17) . 2 ? O5 Co1 O3B 85.82(15) 2 2 ? O5 Co1 O3B 97.28(15) . 2 ? O3B Co1 O3B 61.3(2) . 2 ? O6W Co1 C8B 128.14(15) 2 . ? O6W Co1 C8B 128.14(15) . . ? O5 Co1 C8B 91.80(11) 2 . ? O5 Co1 C8B 91.80(11) . . ? O3B Co1 C8B 30.64(10) . . ? O3B Co1 C8B 30.64(10) 2 . ? C2A C1A C6A 120.4(5) . . ? C2A C1A C7A 121.6(5) . . ? C6A C1A C7A 118.0(5) . . ? C1A C2A C3A 119.7(5) . . ? C2A C3A C2A 120.0(7) . 2_656 ? C2A C3A C8A 120.0(3) . . ? C2A C3A C8A 120.0(3) 2_656 . ? C1A C6A C1A 119.7(6) 2_656 . ? O2A C7A O1A 124.1(5) . . ? O2A C7A C1A 118.8(4) . . ? O1A C7A C1A 117.0(4) . . ? O3A C8A O3A 123.2(7) 2_656 . ? O3A C8A C3A 118.4(3) 2_656 . ? O3A C8A C3A 118.4(3) . . ? C7A O1A Co2 128.5(3) . . ? O1A Co2 O1B 174.68(16) . . ? O1A Co2 O3W 90.09(15) . . ? O1B Co2 O3W 87.13(15) . . ? O1A Co2 O4W 90.36(14) . . ? O1B Co2 O4W 92.69(15) . . ? O3W Co2 O4W 176.51(17) . . ? O1A Co2 O1W 85.59(15) . . ? O1B Co2 O1W 89.87(15) . . ? O3W Co2 O1W 90.14(15) . . ? O4W Co2 O1W 93.35(15) . . ? O1A Co2 O2W 94.35(15) . . ? O1B Co2 O2W 90.06(15) . . ? O3W Co2 O2W 87.37(15) . . ? O4W Co2 O2W 89.14(15) . . ? O1W Co2 O2W 177.51(16) . . ? C2B C1B C6B 119.4(5) . . ? C2B C1B C7B 119.4(5) . . ? C6B C1B C7B 121.1(5) . . ? C1B C2B C3B 120.8(5) . . ? C2B C3B C2B 119.4(7) . 2 ? C2B C3B C8B 120.3(3) . . ? C2B C3B C8B 120.3(3) 2 . ? C1B C6B C1B 120.0(7) 2 . ? O1B C7B O2B 125.1(5) . . ? O1B C7B C1B 117.4(4) . . ? O2B C7B C1B 117.5(5) . . ? O3B C8B O3B 117.7(6) 2 . ? O3B C8B C3B 121.2(3) 2 . ? O3B C8B C3B 121.2(3) . . ? O3B C8B Co1 58.8(3) 2 . ? O3B C8B Co1 58.8(3) . . ? C3B C8B Co1 180.0 . . ? C7B O1B Co2 129.1(3) . . ? C8B O3B Co1 90.5(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.873 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.095 # Attachment 'deposition_arif39c2byc.cif' data_arif39c2byc _database_code_depnum_ccdc_archive 'CCDC 779476' #TrackingRef 'deposition_arif39c2byc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H6 F2 Mn4 O12' _chemical_formula_weight 671.99 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' Mn Mn 0.3368 0.7283 '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' _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 10.7409(7) _cell_length_b 19.2474(12) _cell_length_c 5.2120(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.581(2) _cell_angle_gamma 90.00 _cell_volume 971.88(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2313 _cell_measurement_theta_min 3.809 _cell_measurement_theta_max 30.508 _exptl_crystal_description 'Triangle Plate' _exptl_crystal_colour 'Light Pink' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 2.631 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6968 _exptl_absorpt_correction_T_max 0.9324 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker kappa APEXII CCD Area Detector' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3531 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 857 _reflns_number_gt 800 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_cell_refinement ; APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA) ; _computing_data_reduction ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_structure_solution 'SHELXS-97. Sheldrick, G. M. (2008)' _computing_structure_refinement 'SHELXL-97. Sheldrick, G. M. (2008)' _computing_molecular_graphics 'SHELXTL-Plus. Sheldrick, G. M. (2008)' _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^)+(0.1000P)^2^+0.3444P] 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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 857 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 0.644 _refine_ls_restrained_S_all 0.644 _refine_ls_shift/su_max 0.001 _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 C5 C 1.0000 0.18137(15) 0.2500 0.0116(6) Uani 1 2 d S . . O1 O 1.07679(16) 0.15164(8) 0.4761(3) 0.0212(4) Uani 1 1 d . . . Mn1 Mn 0.65184(3) 0.445026(15) 0.12740(6) 0.00757(18) Uani 1 1 d . . . O3 O 0.74899(14) 0.45970(8) -0.1624(3) 0.0097(3) Uani 1 1 d . . . C6 C 0.80541(19) 0.40849(10) -0.2327(4) 0.0083(4) Uani 1 1 d . . . C1 C 1.0000 0.25961(15) 0.2500 0.0114(6) Uani 1 2 d S . . C4 C 1.0000 0.40384(15) 0.2500 0.0093(6) Uani 1 2 d S . . H4 H 1.0000 0.4532 0.2500 0.011 Uiso 1 2 calc SR . . C2 C 0.9112(2) 0.29567(11) 0.0077(4) 0.0101(4) Uani 1 1 d . . . H2 H 0.8534 0.2710 -0.1594 0.012 Uiso 1 1 calc R . . C3 C 0.9076(2) 0.36762(11) 0.0117(4) 0.0092(4) Uani 1 1 d . . . F1 F 0.5000 0.48691(9) 0.2500 0.0096(4) Uani 1 2 d S . . O2 O 0.78003(14) 0.39308(8) -0.4813(3) 0.0130(4) 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 C5 0.0118(14) 0.0102(15) 0.0119(14) 0.000 0.0042(12) 0.000 O1 0.0281(9) 0.0093(8) 0.0158(8) 0.0030(6) -0.0004(7) 0.0045(7) Mn1 0.0094(3) 0.0063(3) 0.0068(3) -0.00074(10) 0.00336(17) -0.00029(10) O3 0.0113(7) 0.0089(7) 0.0098(7) 0.0042(6) 0.0054(6) 0.0049(6) C6 0.0064(9) 0.0082(10) 0.0107(10) -0.0008(8) 0.0039(8) -0.0035(8) C1 0.0136(14) 0.0095(15) 0.0120(14) 0.000 0.0063(12) 0.000 C4 0.0094(14) 0.0085(14) 0.0108(13) 0.000 0.0052(11) 0.000 C2 0.0091(10) 0.0110(11) 0.0086(10) -0.0025(8) 0.0025(8) -0.0019(7) C3 0.0090(10) 0.0118(11) 0.0081(10) -0.0001(8) 0.0049(8) 0.0013(8) F1 0.0076(8) 0.0122(8) 0.0095(8) 0.000 0.0043(7) 0.000 O2 0.0165(8) 0.0127(8) 0.0078(7) 0.0005(6) 0.0032(6) 0.0038(6) _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 C5 O1 1.248(2) 2_755 ? C5 O1 1.248(2) . ? C5 C1 1.506(4) . ? O1 Mn1 2.0456(15) 8_556 ? Mn1 O1 2.0456(15) 8_455 ? Mn1 F1 2.1489(7) . ? Mn1 O2 2.1519(14) 1_556 ? Mn1 O3 2.1598(14) 6_566 ? Mn1 O3 2.1932(14) . ? Mn1 F1 2.3398(10) 5_665 ? O3 C6 1.290(2) . ? O3 Mn1 2.1598(14) 6_565 ? C6 O2 1.239(2) . ? C6 C3 1.496(3) . ? C1 C2 1.395(3) 2_755 ? C1 C2 1.395(3) . ? C4 C3 1.396(2) . ? C4 C3 1.396(2) 2_755 ? C4 H4 0.9500 . ? C2 C3 1.386(3) . ? C2 H2 0.9500 . ? F1 Mn1 2.1489(7) 2_655 ? F1 Mn1 2.3398(10) 6_566 ? F1 Mn1 2.3398(10) 5_665 ? O2 Mn1 2.1519(14) 1_554 ? 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 O1 C5 O1 125.4(3) 2_755 . ? O1 C5 C1 117.29(14) 2_755 . ? O1 C5 C1 117.29(14) . . ? C5 O1 Mn1 140.44(16) . 8_556 ? O1 Mn1 F1 103.45(6) 8_455 . ? O1 Mn1 O2 85.82(6) 8_455 1_556 ? F1 Mn1 O2 98.60(4) . 1_556 ? O1 Mn1 O3 172.51(6) 8_455 6_566 ? F1 Mn1 O3 78.06(5) . 6_566 ? O2 Mn1 O3 86.70(6) 1_556 6_566 ? O1 Mn1 O3 94.42(6) 8_455 . ? F1 Mn1 O3 143.54(5) . . ? O2 Mn1 O3 114.37(5) 1_556 . ? O3 Mn1 O3 88.32(5) 6_566 . ? O1 Mn1 F1 99.76(6) 8_455 5_665 ? F1 Mn1 F1 72.359(15) . 5_665 ? O2 Mn1 F1 170.21(5) 1_556 5_665 ? O3 Mn1 F1 87.70(5) 6_566 5_665 ? O3 Mn1 F1 73.45(4) . 5_665 ? C6 O3 Mn1 133.45(13) . 6_565 ? C6 O3 Mn1 121.25(13) . . ? Mn1 O3 Mn1 100.92(6) 6_565 . ? O2 C6 O3 124.17(18) . . ? O2 C6 C3 120.89(19) . . ? O3 C6 C3 114.93(17) . . ? C2 C1 C2 120.3(3) 2_755 . ? C2 C1 C5 119.84(13) 2_755 . ? C2 C1 C5 119.84(13) . . ? C3 C4 C3 120.1(3) . 2_755 ? C3 C4 H4 120.0 . . ? C3 C4 H4 120.0 2_755 . ? C3 C2 C1 119.75(19) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 119.91(19) . . ? C2 C3 C6 121.84(18) . . ? C4 C3 C6 118.24(19) . . ? Mn1 F1 Mn1 135.93(8) 2_655 . ? Mn1 F1 Mn1 107.641(15) 2_655 6_566 ? Mn1 F1 Mn1 96.721(16) . 6_566 ? Mn1 F1 Mn1 96.721(16) 2_655 5_665 ? Mn1 F1 Mn1 107.641(15) . 5_665 ? Mn1 F1 Mn1 111.90(7) 6_566 5_665 ? C6 O2 Mn1 129.90(14) . 1_554 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.343 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.068 # Attachment 'deposition_arif47c2byc.cif' data_arif47c2byc _database_code_depnum_ccdc_archive 'CCDC 779477' #TrackingRef 'deposition_arif47c2byc.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H6 Co4 F2 O12' _chemical_formula_weight 687.95 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' F F 0.0171 0.0103 '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 10.7409(6) _cell_length_b 18.8422(12) _cell_length_c 5.0778(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.932(2) _cell_angle_gamma 90.00 _cell_volume 924.19(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plates _exptl_crystal_colour Purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 3.623 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5180 _exptl_absorpt_correction_T_max 0.9085 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker kappa APEXII CCD Area Detector' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3276 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.97 _reflns_number_total 810 _reflns_number_gt 762 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_cell_refinement ; APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA) ; _computing_data_reduction ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_structure_solution 'SHELXS-97. Sheldrick, G. M. (2008)' _computing_structure_refinement 'SHELXL-97. Sheldrick, G. M. (2008)' _computing_molecular_graphics 'SHELXTL-Plus. Sheldrick, G. M. (2008)' _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^)+(0.1000P)^2^+0.1453P] 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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 810 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 0.689 _refine_ls_restrained_S_all 0.689 _refine_ls_shift/su_max 0.002 _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 0.14817(3) 1.051441(16) 0.11957(7) 0.0071(2) Uani 1 1 d . . . C1 C 0.5000 0.90356(19) 0.7500 0.0084(7) Uani 1 2 d S . . H1 H 0.5000 0.9540 0.7500 0.010 Uiso 1 2 calc SR . . C2 C 0.4060(2) 0.86704(13) 0.5073(5) 0.0075(5) Uani 1 1 d . . . C4 C 0.5000 0.75650(19) 0.7500 0.0098(7) Uani 1 2 d S . . C3 C 0.4093(2) 0.79337(13) 0.5031(5) 0.0094(5) Uani 1 1 d . . . H3 H 0.3498 0.7682 0.3320 0.011 Uiso 1 1 calc R . . O1 O 0.24314(19) 0.95991(9) 0.3359(4) 0.0095(4) Uani 1 1 d . . . O2 O 0.27830(17) 1.10380(9) 0.5023(4) 0.0116(4) Uani 1 1 d . . . O3 O 0.07314(19) 1.14678(9) -0.0127(4) 0.0177(4) Uani 1 1 d . . . C5 C 0.3022(2) 0.90933(13) 0.2584(5) 0.0065(5) Uani 1 1 d . . . C6 C 0.5000 0.67702(19) 0.7500 0.0100(8) Uani 1 2 d S . . F1 F 0.0000 1.01298(10) 0.2500 0.0091(5) Uani 1 2 d S . . 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 0.0094(3) 0.0049(3) 0.0051(3) 0.00108(11) 0.0013(2) 0.00037(11) C1 0.0136(17) 0.0069(18) 0.0071(17) 0.000 0.0068(15) 0.000 C2 0.0066(11) 0.0091(13) 0.0066(12) 0.0024(10) 0.0027(10) 0.0033(9) C4 0.0110(17) 0.0077(18) 0.0096(17) 0.000 0.0036(14) 0.000 C3 0.0098(12) 0.0088(13) 0.0066(12) -0.0026(10) 0.0007(10) -0.0024(9) O1 0.0121(9) 0.0071(9) 0.0095(10) 0.0034(7) 0.0047(8) 0.0042(7) O2 0.0153(9) 0.0102(10) 0.0061(9) 0.0006(7) 0.0018(7) -0.0023(7) O3 0.0254(10) 0.0050(9) 0.0119(10) 0.0012(7) -0.0017(8) 0.0043(8) C5 0.0067(11) 0.0035(12) 0.0085(13) -0.0016(10) 0.0028(10) -0.0027(9) C6 0.0081(16) 0.0106(19) 0.0102(18) 0.000 0.0031(15) 0.000 F1 0.0097(10) 0.0094(11) 0.0071(11) 0.000 0.0027(9) 0.000 _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 O3 1.9631(18) . ? Co1 O1 2.0597(17) . ? Co1 O2 2.0803(18) . ? Co1 F1 2.1020(7) . ? Co1 O1 2.1085(17) 6_575 ? Co1 F1 2.2171(11) 5_575 ? C1 C2 1.387(3) . ? C1 C2 1.387(3) 2_656 ? C1 H1 0.9500 . ? C2 C3 1.389(4) . ? C2 C5 1.497(3) . ? C4 C3 1.391(3) 2_656 ? C4 C3 1.391(3) . ? C4 C6 1.498(5) . ? C3 H3 0.9500 . ? O1 C5 1.298(3) . ? O1 Co1 2.1085(17) 6_576 ? O2 C5 1.236(3) 6_576 ? O3 C6 1.251(2) 3_454 ? C5 O2 1.236(3) 6_575 ? C6 O3 1.251(2) 4_545 ? C6 O3 1.251(2) 3_546 ? F1 Co1 2.1020(7) 2 ? F1 Co1 2.2171(11) 5_575 ? F1 Co1 2.2171(11) 6_576 ? 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 O3 Co1 O1 169.17(7) . . ? O3 Co1 O2 83.87(7) . . ? O1 Co1 O2 85.70(7) . . ? O3 Co1 F1 99.74(7) . . ? O1 Co1 F1 79.04(6) . . ? O2 Co1 F1 99.27(5) . . ? O3 Co1 O1 96.20(7) . 6_575 ? O1 Co1 O1 90.27(6) . 6_575 ? O2 Co1 O1 110.98(7) . 6_575 ? F1 Co1 O1 147.08(6) . 6_575 ? O3 Co1 F1 100.14(7) . 5_575 ? O1 Co1 F1 89.87(6) . 5_575 ? O2 Co1 F1 172.16(5) . 5_575 ? F1 Co1 F1 73.490(18) . 5_575 ? O1 Co1 F1 75.46(5) 6_575 5_575 ? C2 C1 C2 120.5(3) . 2_656 ? C2 C1 H1 119.7 . . ? C2 C1 H1 119.7 2_656 . ? C1 C2 C3 119.7(2) . . ? C1 C2 C5 118.0(2) . . ? C3 C2 C5 122.3(2) . . ? C3 C4 C3 120.1(3) 2_656 . ? C3 C4 C6 119.96(16) 2_656 . ? C3 C4 C6 119.96(16) . . ? C2 C3 C4 119.9(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 O1 Co1 130.32(15) . . ? C5 O1 Co1 125.42(15) . 6_576 ? Co1 O1 Co1 100.05(7) . 6_576 ? C5 O2 Co1 129.34(16) 6_576 . ? C6 O3 Co1 137.48(18) 3_454 . ? O2 C5 O1 124.2(2) 6_575 . ? O2 C5 C2 121.2(2) 6_575 . ? O1 C5 C2 114.7(2) . . ? O3 C6 O3 125.8(3) 4_545 3_546 ? O3 C6 C4 117.09(16) 4_545 . ? O3 C6 C4 117.09(16) 3_546 . ? Co1 F1 Co1 139.66(10) . 2 ? Co1 F1 Co1 106.510(19) . 5_575 ? Co1 F1 Co1 95.356(19) 2 5_575 ? Co1 F1 Co1 95.356(19) . 6_576 ? Co1 F1 Co1 106.510(19) 2 6_576 ? Co1 F1 Co1 113.61(9) 5_575 6_576 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.370 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.091 # Attachment 'deposition_arif50c2.cif' data_arif50c2 _database_code_depnum_ccdc_archive 'CCDC 779478' #TrackingRef 'deposition_arif50c2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H14 Fe1.50 O12' _chemical_formula_weight 397.98 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' Fe Fe 0.3463 0.8444 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 17.488(2) _cell_length_b 12.9304(17) _cell_length_c 6.5221(8) _cell_angle_alpha 90.00 _cell_angle_beta 111.523(5) _cell_angle_gamma 90.00 _cell_volume 1372.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1232 _cell_measurement_theta_min 2.504 _cell_measurement_theta_max 25.094 _exptl_crystal_description 'Thin needles' _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 1.673 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8506 _exptl_absorpt_correction_T_max 0.9835 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker kappa APEXII CCD Area Detector' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4878 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2304 _reflns_number_gt 2020 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_cell_refinement ; APEX2(Bruker, 2007, Bruker AXS Inc.,Madison, USA) ; _computing_data_reduction ; APEX2(Bruker, 2007, Bruker AXS Inc., Madison, USA) ; _computing_structure_solution 'SHELXS-97. Sheldrick, G. M. (2008)' _computing_structure_refinement 'SHELXL-97. Sheldrick, G. M. (2008)' _computing_molecular_graphics 'SHELXTL-Plus. Sheldrick, G. M. (2008)' _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^)+(0.1000P)^2^+1.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2304 _refine_ls_number_parameters 240 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1195 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.791 _refine_ls_restrained_S_all 0.786 _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 Fe1 Fe 0.0000 0.59664(8) 0.0000 0.0134(3) Uani 1 2 d S . . Fe2 Fe 0.25902(4) -0.11979(7) 0.28895(14) 0.0119(2) Uani 1 1 d . . . O1A O 0.3547(2) -0.2256(3) 0.4136(8) 0.0162(10) Uani 1 1 d . . . O2A O 0.2858(2) -0.3697(3) 0.4194(7) 0.0136(10) Uani 1 1 d . . . O3A O 0.4321(3) -0.7089(3) 0.4413(8) 0.0208(11) Uani 1 1 d . . . C1A C 0.4271(3) -0.3834(5) 0.4618(10) 0.0118(12) Uani 1 1 d U . . C2A C 0.4267(4) -0.4905(5) 0.4628(10) 0.0127(12) Uani 1 1 d U . . H2A H 0.3769 -0.5267 0.4385 0.015 Uiso 1 1 calc R . . C3A C 0.5000 -0.5459(7) 0.5000 0.0094(15) Uani 1 2 d SU . . C4A C 0.5000 -0.3301(7) 0.5000 0.0103(14) Uani 1 2 d SU . . H4A H 0.5000 -0.2566 0.5000 0.012 Uiso 1 2 calc SR . . C5A C 0.3505(4) -0.3219(5) 0.4279(10) 0.0137(13) Uani 1 1 d . . . C6A C 0.5000 -0.6613(7) 0.5000 0.0109(18) Uani 1 2 d S . . O1B O 0.1569(3) -0.0260(3) 0.1461(8) 0.0151(10) Uani 1 1 d . . . O2B O 0.2150(2) 0.1193(3) 0.0882(8) 0.0164(10) Uani 1 1 d . . . O3B O 0.0647(2) 0.4487(3) 0.0177(7) 0.0152(10) Uani 1 1 d . . . C1B C 0.0740(4) 0.1244(5) 0.0441(10) 0.0136(14) Uani 1 1 d . . . C2B C 0.0724(3) 0.2321(5) 0.0382(10) 0.0109(13) Uani 1 1 d . . . H2B H 0.1215 0.2697 0.0607 0.013 Uiso 1 1 calc R . . C3B C 0.0000 0.2840(6) 0.0000 0.0116(18) Uani 1 2 d S . . C4B C 0.0000 0.0702(7) 0.0000 0.0141(19) Uani 1 2 d S . . H4B H 0.0000 -0.0032 0.0000 0.017 Uiso 1 2 calc SR . . C5B C 0.1546(3) 0.0681(4) 0.0963(10) 0.0116(13) Uani 1 1 d . . . C6B C 0.0000 0.4001(6) 0.0000 0.013(2) Uani 1 2 d S . . O1W O 0.1785(3) -0.2276(3) 0.3476(8) 0.0150(10) Uani 1 1 d D . . H1W1 H 0.143(4) -0.219(6) 0.428(12) 0.062 Uiso 1 1 d D . . H2W1 H 0.209(5) -0.291(4) 0.391(13) 0.063 Uiso 1 1 d D . . O2W O 0.2370(3) -0.1861(3) -0.0315(7) 0.0170(10) Uani 1 1 d D . . H1W2 H 0.248(5) -0.2588(15) -0.030(13) 0.062 Uiso 1 1 d D . . H2W2 H 0.191(3) -0.167(5) -0.161(8) 0.062 Uiso 1 1 d D . . O3W O 0.2780(2) -0.0581(4) 0.6201(7) 0.0195(10) Uani 1 1 d D . . H2W3 H 0.325(4) -0.046(7) 0.753(9) 0.062 Uiso 1 1 d D . . O4W O 0.3417(3) -0.0063(3) 0.2510(8) 0.0162(10) Uani 1 1 d D . . H1W4 H 0.363(5) -0.034(6) 0.146(9) 0.062 Uiso 1 1 d D . . H2W4 H 0.302(4) 0.046(5) 0.186(11) 0.062 Uiso 1 1 d D . . O6W O -0.0564(3) 0.6002(4) -0.3512(7) 0.0191(10) Uani 1 1 d D . . H1W6 H -0.059(6) 0.648(4) -0.466(9) 0.062 Uiso 1 1 d D . . H2W6 H -0.043(6) 0.532(3) -0.385(13) 0.067 Uiso 1 1 d D . . O7W O -0.0871(3) 0.6902(4) 0.0385(8) 0.0259(11) Uani 1 1 d D . . H1W7 H -0.076(6) 0.734(5) 0.165(8) 0.063 Uiso 1 1 d D . . H2W7 H -0.109(6) 0.730(5) -0.095(7) 0.062 Uiso 1 1 d 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 Fe1 0.0132(6) 0.0077(6) 0.0203(7) 0.000 0.0074(5) 0.000 Fe2 0.0089(4) 0.0085(4) 0.0184(5) 0.0009(4) 0.0051(3) 0.0006(4) O1A 0.012(2) 0.009(2) 0.024(3) 0.0003(18) 0.0033(19) 0.0018(16) O2A 0.010(2) 0.009(2) 0.023(2) 0.0023(18) 0.0083(18) -0.0019(15) O3A 0.025(3) 0.011(2) 0.035(3) -0.002(2) 0.020(2) -0.0010(19) C1A 0.009(2) 0.015(3) 0.013(3) -0.001(2) 0.006(2) 0.0019(18) C2A 0.013(3) 0.013(3) 0.013(3) -0.001(2) 0.006(2) -0.001(2) C3A 0.015(3) 0.009(3) 0.009(3) 0.000 0.009(3) 0.000 C4A 0.013(3) 0.012(3) 0.009(3) 0.000 0.008(3) 0.000 C5A 0.019(3) 0.009(3) 0.013(3) -0.004(3) 0.007(3) -0.002(2) C6A 0.012(4) 0.009(4) 0.016(5) 0.000 0.010(4) 0.000 O1B 0.014(2) 0.010(2) 0.021(2) 0.0042(19) 0.0066(19) 0.0016(17) O2B 0.011(2) 0.014(2) 0.024(3) 0.0042(19) 0.0073(19) 0.0022(17) O3B 0.015(2) 0.007(2) 0.028(3) -0.002(2) 0.012(2) -0.0028(18) C1B 0.021(3) 0.013(3) 0.008(3) 0.000(2) 0.007(3) 0.000(2) C2B 0.010(3) 0.013(3) 0.013(3) -0.008(2) 0.008(3) -0.007(2) C3B 0.016(4) 0.012(5) 0.008(4) 0.000 0.007(4) 0.000 C4B 0.014(4) 0.024(5) 0.005(4) 0.000 0.004(3) 0.000 C5B 0.017(3) 0.008(3) 0.015(3) -0.001(2) 0.011(3) -0.001(2) C6B 0.014(4) 0.013(5) 0.014(4) 0.000 0.006(4) 0.000 O1W 0.015(2) 0.013(2) 0.022(3) 0.0014(19) 0.011(2) 0.0026(17) O2W 0.018(2) 0.012(2) 0.021(3) -0.0017(19) 0.0074(19) -0.0003(17) O3W 0.013(2) 0.020(2) 0.021(2) -0.001(2) 0.0008(19) 0.0031(19) O4W 0.019(2) 0.010(2) 0.019(2) 0.003(2) 0.0064(19) 0.0012(18) O6W 0.025(2) 0.014(2) 0.019(2) -0.002(2) 0.008(2) 0.002(2) O7W 0.028(3) 0.023(3) 0.021(3) 0.004(2) 0.002(2) 0.016(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 Fe1 O7W 2.032(5) 2 ? Fe1 O7W 2.032(5) . ? Fe1 O6W 2.136(5) 2 ? Fe1 O6W 2.136(5) . ? Fe1 O3B 2.204(4) 2 ? Fe1 O3B 2.204(4) . ? Fe2 O1B 2.076(4) . ? Fe2 O1A 2.082(4) . ? Fe2 O1W 2.114(4) . ? Fe2 O4W 2.137(4) . ? Fe2 O2W 2.159(5) . ? Fe2 O3W 2.210(5) . ? O1A C5A 1.253(8) . ? O2A C5A 1.272(7) . ? O3A C6A 1.266(6) . ? C1A C2A 1.384(9) . ? C1A C4A 1.389(7) . ? C1A C5A 1.503(8) . ? C2A C3A 1.410(8) . ? C3A C2A 1.410(8) 2_656 ? C3A C6A 1.492(12) . ? C4A C1A 1.389(7) 2_656 ? C6A O3A 1.266(6) 2_656 ? O1B C5B 1.256(7) . ? O2B C5B 1.264(7) . ? O3B C6B 1.261(6) . ? C1B C2B 1.393(8) . ? C1B C4B 1.406(8) . ? C1B C5B 1.510(8) . ? C2B C3B 1.373(7) . ? C3B C2B 1.373(7) 2 ? C3B C6B 1.502(12) . ? C4B C1B 1.406(8) 2 ? C6B O3B 1.261(6) 2 ? 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 O7W Fe1 O7W 106.9(3) 2 . ? O7W Fe1 O6W 92.75(19) 2 2 ? O7W Fe1 O6W 85.80(19) . 2 ? O7W Fe1 O6W 85.80(19) 2 . ? O7W Fe1 O6W 92.75(19) . . ? O6W Fe1 O6W 177.6(3) 2 . ? O7W Fe1 O3B 154.70(19) 2 2 ? O7W Fe1 O3B 97.47(19) . 2 ? O6W Fe1 O3B 95.78(17) 2 2 ? O6W Fe1 O3B 86.35(18) . 2 ? O7W Fe1 O3B 97.47(19) 2 . ? O7W Fe1 O3B 154.70(19) . . ? O6W Fe1 O3B 86.35(18) 2 . ? O6W Fe1 O3B 95.78(17) . . ? O3B Fe1 O3B 59.5(2) 2 . ? O1B Fe2 O1A 174.42(18) . . ? O1B Fe2 O1W 86.90(17) . . ? O1A Fe2 O1W 89.38(17) . . ? O1B Fe2 O4W 93.10(17) . . ? O1A Fe2 O4W 90.89(16) . . ? O1W Fe2 O4W 176.1(2) . . ? O1B Fe2 O2W 88.81(18) . . ? O1A Fe2 O2W 87.10(18) . . ? O1W Fe2 O2W 91.09(17) . . ? O4W Fe2 O2W 92.81(17) . . ? O1B Fe2 O3W 91.37(17) . . ? O1A Fe2 O3W 92.53(17) . . ? O1W Fe2 O3W 86.14(18) . . ? O4W Fe2 O3W 89.97(17) . . ? O2W Fe2 O3W 177.20(18) . . ? C5A O1A Fe2 128.4(4) . . ? C2A C1A C4A 120.1(6) . . ? C2A C1A C5A 121.6(5) . . ? C4A C1A C5A 118.2(6) . . ? C1A C2A C3A 120.2(6) . . ? C2A C3A C2A 118.9(8) 2_656 . ? C2A C3A C6A 120.6(4) 2_656 . ? C2A C3A C6A 120.6(4) . . ? C1A C4A C1A 120.5(8) . 2_656 ? O1A C5A O2A 123.7(5) . . ? O1A C5A C1A 117.6(5) . . ? O2A C5A C1A 118.7(5) . . ? O3A C6A O3A 121.8(8) . 2_656 ? O3A C6A C3A 119.1(4) . . ? O3A C6A C3A 119.1(4) 2_656 . ? C5B O1B Fe2 128.5(4) . . ? C6B O3B Fe1 90.1(4) . . ? C2B C1B C4B 119.0(6) . . ? C2B C1B C5B 119.7(5) . . ? C4B C1B C5B 121.2(6) . . ? C3B C2B C1B 120.1(6) . . ? C2B C3B C2B 121.5(8) 2 . ? C2B C3B C6B 119.2(4) 2 . ? C2B C3B C6B 119.2(4) . . ? C1B C4B C1B 120.2(8) . 2 ? O1B C5B O2B 124.8(5) . . ? O1B C5B C1B 117.6(5) . . ? O2B C5B C1B 117.6(5) . . ? O3B C6B O3B 120.3(7) . 2 ? O3B C6B C3B 119.9(4) . . ? O3B C6B C3B 119.9(4) 2 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.081 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.096