# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Themistoklis Kabanos' 'George I Chilas' 'Maciej Kubicki' 'Nikolia Lalioti' 'Tiverios Vaimakis' _publ_contact_author_name 'Themistoklis Kabanos' _publ_contact_author_email TKAMPANO@CC.UOI.GR _publ_section_title ; Hydrothermal syntheses, crystal structures and physicochemical properties of 2-D and 3-D inorganic coordination cobalt(II)-sulfite polymers ; # Attachment 'combined.cif' #Hydrothermal syntheses, crystal structures and physicochemical properties #of 2-D and 3-D inorganic coordination cobalt(II)-sulfite polymers #by George I. Chilas, Nicolia Lalioti, Tiverios Vaimakis, #Maciej Kubicki, Themistoklis Kabanos* data_1 _database_code_depnum_ccdc_archive 'CCDC 750027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Co2 H3 O8 S2, Na' _chemical_formula_sum 'Co2 H3 Na O8 S2' _chemical_formula_weight 335.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' H H 0.0000 0.0000 '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 6.3214(15) _cell_length_b 7.827(2) _cell_length_c 8.898(2) _cell_angle_alpha 98.91(2) _cell_angle_beta 109.81(2) _cell_angle_gamma 112.61(2) _cell_volume 361.17(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2787 _cell_measurement_theta_min 4 _cell_measurement_theta_max 23 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 3.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 5.240 _exptl_absorpt_correction_T_min 0.542 _exptl_absorpt_correction_T_max 0.85500 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'KUMA KM4CCD four-circle diffractometer' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 4483 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.1203 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1264 _reflns_number_gt 645 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2006) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens (1989), Farrugia (1999)' _computing_publication_material 'SHELXL97 (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^)+(0.0200P)^2^+4.0000P] 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 1263 _refine_ls_number_parameters 121 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1580 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.397 _refine_ls_restrained_S_all 1.406 _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 0.1814(4) 0.6694(3) 0.1891(3) 0.0226(5) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 -0.5000 0.0224(7) Uani 1 2 d S . . Co3 Co 0.0000 0.5000 -0.5000 0.0231(7) Uani 1 2 d S . . Na1 Na 0.5553(12) 0.6753(9) -0.0910(7) 0.0380(16) Uani 1 1 d . . . S1 S 0.2367(7) 0.2459(5) -0.2965(5) 0.0249(9) Uani 1 1 d . . . O11 O 0.5095(17) 0.3212(15) -0.1586(12) 0.032(3) Uani 1 1 d U . . O12 O 0.1047(17) 0.2683(16) -0.1914(12) 0.034(3) Uani 1 1 d U . . O13 O 0.2699(15) 0.4183(12) -0.3703(11) 0.019(2) Uani 1 1 d U . . S2 S 0.0624(7) 0.7974(5) -0.1589(4) 0.0198(8) Uani 1 1 d . . . O21 O -0.2151(17) 0.7473(13) -0.2736(11) 0.022(2) Uani 1 1 d . . . O22 O 0.1777(16) 0.7513(13) -0.2770(11) 0.022(2) Uani 1 1 d . . . O23 O 0.0315(16) 0.6384(12) -0.0767(11) 0.021(2) Uani 1 1 d . . . O1 O 0.3954(18) 0.9810(14) 0.2900(12) 0.031(2) Uani 1 1 d . . . H1A H 0.3079 1.0589 0.2891 0.037 Uiso 1 1 d R . . H1B H 0.5256 1.0503 0.2553 0.037 Uiso 1 1 d R . . O2 O 0.2909(16) 0.6518(13) 0.4289(11) 0.018(2) Uani 1 1 d U . . H2A H 0.372(17) 0.761(8) 0.495(9) 0.080 Uiso 1 1 d R . . 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 0.0198(11) 0.0319(11) 0.0281(12) 0.0172(10) 0.0138(9) 0.0177(10) Co2 0.0192(15) 0.0332(16) 0.0282(18) 0.0186(14) 0.0154(13) 0.0172(14) Co3 0.0197(16) 0.0316(16) 0.0319(18) 0.0180(14) 0.0154(14) 0.0187(14) Na1 0.051(4) 0.038(4) 0.032(4) 0.013(3) 0.019(3) 0.024(3) S1 0.022(2) 0.030(2) 0.035(2) 0.0211(19) 0.0150(18) 0.0176(18) O11 0.024(5) 0.056(6) 0.033(6) 0.021(5) 0.016(4) 0.030(5) O12 0.023(5) 0.061(5) 0.038(5) 0.027(4) 0.023(4) 0.028(4) O13 0.018(5) 0.027(5) 0.029(5) 0.020(4) 0.019(4) 0.016(4) S2 0.024(2) 0.0267(19) 0.019(2) 0.0120(16) 0.0129(16) 0.0170(17) O21 0.025(5) 0.033(5) 0.023(6) 0.018(5) 0.015(5) 0.021(5) O22 0.015(5) 0.026(5) 0.027(6) 0.011(5) 0.011(4) 0.010(4) O23 0.014(5) 0.020(5) 0.021(6) 0.006(4) 0.001(4) 0.005(4) O1 0.039(6) 0.039(6) 0.042(7) 0.029(5) 0.025(5) 0.032(5) O2 0.016(4) 0.023(4) 0.024(5) 0.011(4) 0.010(4) 0.014(4) _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 O11 2.037(9) 2_665 ? Co1 O12 2.051(9) 2_565 ? Co1 O2 2.053(9) . ? Co1 O23 2.113(9) 2_565 ? Co1 O1 2.132(10) . ? Co1 O23 2.163(9) . ? Co2 O2 2.105(8) 1_554 ? Co2 O2 2.105(8) 2_665 ? Co2 O13 2.123(8) . ? Co2 O13 2.123(8) 2_664 ? Co2 O21 2.168(9) 1_655 ? Co2 O21 2.168(9) 2_564 ? Co2 Na1 3.531(6) . ? Co2 Na1 3.531(6) 2_664 ? Co3 O13 2.094(8) 2_564 ? Co3 O13 2.094(8) . ? Co3 O2 2.130(9) 2_565 ? Co3 O2 2.130(9) 1_554 ? Co3 O22 2.156(9) . ? Co3 O22 2.156(9) 2_564 ? Na1 O11 2.389(11) 2_665 ? Na1 O13 2.470(11) . ? Na1 O21 2.514(11) 1_655 ? Na1 O12 2.529(11) 2_665 ? Na1 O11 2.622(11) . ? Na1 O22 2.740(11) . ? Na1 S1 3.015(7) . ? Na1 S1 3.105(7) 2_665 ? Na1 S2 3.269(7) 1_655 ? Na1 Na1 3.363(12) 2_665 ? S1 O12 1.481(10) . ? S1 O11 1.545(10) . ? S1 O13 1.564(9) . ? S1 Na1 3.105(7) 2_665 ? O11 Co1 2.037(9) 2_665 ? O11 Na1 2.389(11) 2_665 ? O12 Co1 2.051(9) 2_565 ? O12 Na1 2.529(11) 2_665 ? S2 O23 1.521(9) . ? S2 O22 1.540(9) . ? S2 O21 1.551(9) . ? S2 Na1 3.269(7) 1_455 ? O21 Co2 2.168(9) 1_455 ? O21 Na1 2.514(11) 1_455 ? O23 Co1 2.113(9) 2_565 ? O1 H1A 0.9673 . ? O1 H1B 0.9735 . ? O2 Co2 2.105(8) 1_556 ? O2 Co3 2.130(9) 1_556 ? O2 H2A 0.801 . ? 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 O11 Co1 O12 162.1(4) 2_665 2_565 ? O11 Co1 O2 97.3(4) 2_665 . ? O12 Co1 O2 94.9(4) 2_565 . ? O11 Co1 O23 93.2(4) 2_665 2_565 ? O12 Co1 O23 99.3(4) 2_565 2_565 ? O2 Co1 O23 92.4(3) . 2_565 ? O11 Co1 O1 85.6(4) 2_665 . ? O12 Co1 O1 81.2(4) 2_565 . ? O2 Co1 O1 90.5(4) . . ? O23 Co1 O1 177.0(4) 2_565 . ? O11 Co1 O23 83.8(4) 2_665 . ? O12 Co1 O23 86.2(4) 2_565 . ? O2 Co1 O23 171.0(3) . . ? O23 Co1 O23 78.6(4) 2_565 . ? O1 Co1 O23 98.5(3) . . ? O2 Co2 O2 180.000(2) 1_554 2_665 ? O2 Co2 O13 81.0(3) 1_554 . ? O2 Co2 O13 99.0(3) 2_665 . ? O2 Co2 O13 99.0(3) 1_554 2_664 ? O2 Co2 O13 81.0(3) 2_665 2_664 ? O13 Co2 O13 180.000(2) . 2_664 ? O2 Co2 O21 91.1(3) 1_554 1_655 ? O2 Co2 O21 88.9(3) 2_665 1_655 ? O13 Co2 O21 88.3(3) . 1_655 ? O13 Co2 O21 91.7(3) 2_664 1_655 ? O2 Co2 O21 88.9(3) 1_554 2_564 ? O2 Co2 O21 91.1(3) 2_665 2_564 ? O13 Co2 O21 91.7(3) . 2_564 ? O13 Co2 O21 88.3(3) 2_664 2_564 ? O21 Co2 O21 180.0(4) 1_655 2_564 ? O2 Co2 Na1 85.6(3) 1_554 . ? O2 Co2 Na1 94.4(3) 2_665 . ? O13 Co2 Na1 43.5(3) . . ? O13 Co2 Na1 136.5(3) 2_664 . ? O21 Co2 Na1 44.9(3) 1_655 . ? O21 Co2 Na1 135.1(3) 2_564 . ? O2 Co2 Na1 94.4(3) 1_554 2_664 ? O2 Co2 Na1 85.6(3) 2_665 2_664 ? O13 Co2 Na1 136.5(3) . 2_664 ? O13 Co2 Na1 43.5(3) 2_664 2_664 ? O21 Co2 Na1 135.1(3) 1_655 2_664 ? O21 Co2 Na1 44.9(3) 2_564 2_664 ? Na1 Co2 Na1 180.0(2) . 2_664 ? O13 Co3 O13 180.000(1) 2_564 . ? O13 Co3 O2 81.1(3) 2_564 2_565 ? O13 Co3 O2 98.9(3) . 2_565 ? O13 Co3 O2 98.9(3) 2_564 1_554 ? O13 Co3 O2 81.1(3) . 1_554 ? O2 Co3 O2 180.000(1) 2_565 1_554 ? O13 Co3 O22 92.4(3) 2_564 . ? O13 Co3 O22 87.6(3) . . ? O2 Co3 O22 90.9(3) 2_565 . ? O2 Co3 O22 89.1(3) 1_554 . ? O13 Co3 O22 87.6(3) 2_564 2_564 ? O13 Co3 O22 92.4(3) . 2_564 ? O2 Co3 O22 89.1(3) 2_565 2_564 ? O2 Co3 O22 90.9(3) 1_554 2_564 ? O22 Co3 O22 180.0(5) . 2_564 ? O11 Na1 O13 125.4(4) 2_665 . ? O11 Na1 O21 159.3(4) 2_665 1_655 ? O13 Na1 O21 73.7(3) . 1_655 ? O11 Na1 O12 56.6(3) 2_665 2_665 ? O13 Na1 O12 139.4(4) . 2_665 ? O21 Na1 O12 104.5(4) 1_655 2_665 ? O11 Na1 O11 95.8(4) 2_665 . ? O13 Na1 O11 56.4(3) . . ? O21 Na1 O11 89.2(3) 1_655 . ? O12 Na1 O11 83.2(4) 2_665 . ? O11 Na1 O22 100.5(3) 2_665 . ? O13 Na1 O22 68.5(3) . . ? O21 Na1 O22 93.8(3) 1_655 . ? O12 Na1 O22 149.9(4) 2_665 . ? O11 Na1 O22 121.4(3) . . ? O11 Na1 S1 101.3(3) 2_665 . ? O13 Na1 S1 31.2(2) . . ? O21 Na1 S1 93.3(3) 1_655 . ? O12 Na1 S1 111.6(3) 2_665 . ? O11 Na1 S1 30.8(2) . . ? O22 Na1 S1 90.6(3) . . ? O11 Na1 S1 29.1(2) 2_665 2_665 ? O13 Na1 S1 144.1(3) . 2_665 ? O21 Na1 S1 130.7(3) 1_655 2_665 ? O12 Na1 S1 28.2(2) 2_665 2_665 ? O11 Na1 S1 93.9(3) . 2_665 ? O22 Na1 S1 124.7(3) . 2_665 ? S1 Na1 S1 113.4(2) . 2_665 ? O11 Na1 S2 133.1(3) 2_665 1_655 ? O13 Na1 S2 93.9(3) . 1_655 ? O21 Na1 S2 27.3(2) 1_655 1_655 ? O12 Na1 S2 77.1(3) 2_665 1_655 ? O11 Na1 S2 85.1(3) . 1_655 ? O22 Na1 S2 118.9(3) . 1_655 ? S1 Na1 S2 102.61(19) . 1_655 ? S1 Na1 S2 103.97(19) 2_665 1_655 ? O11 Na1 Na1 50.9(3) 2_665 2_665 ? O13 Na1 Na1 88.9(3) . 2_665 ? O21 Na1 Na1 130.8(4) 1_655 2_665 ? O12 Na1 Na1 61.1(3) 2_665 2_665 ? O11 Na1 Na1 45.0(2) . 2_665 ? O22 Na1 Na1 122.4(4) . 2_665 ? S1 Na1 Na1 57.96(19) . 2_665 ? S1 Na1 Na1 55.39(18) 2_665 2_665 ? S2 Na1 Na1 114.7(3) 1_655 2_665 ? O11 Na1 Co2 160.3(3) 2_665 . ? O13 Na1 Co2 36.3(2) . . ? O21 Na1 Co2 37.5(2) 1_655 . ? O12 Na1 Co2 128.6(3) 2_665 . ? O11 Na1 Co2 68.1(2) . . ? O22 Na1 Co2 79.8(2) . . ? S1 Na1 Co2 59.08(13) . . ? S1 Na1 Co2 155.3(2) 2_665 . ? S2 Na1 Co2 59.39(12) 1_655 . ? Na1 Na1 Co2 112.2(2) 2_665 . ? O12 S1 O11 100.9(6) . . ? O12 S1 O13 104.1(5) . . ? O11 S1 O13 101.7(5) . . ? O12 S1 Na1 78.3(5) . . ? O11 S1 Na1 60.4(4) . . ? O13 S1 Na1 54.8(4) . . ? O12 S1 Na1 53.7(4) . 2_665 ? O11 S1 Na1 48.8(4) . 2_665 ? O13 S1 Na1 121.0(4) . 2_665 ? Na1 S1 Na1 66.6(2) . 2_665 ? S1 O11 Co1 128.2(6) . 2_665 ? S1 O11 Na1 102.1(5) . 2_665 ? Co1 O11 Na1 127.2(5) 2_665 2_665 ? S1 O11 Na1 88.8(4) . . ? Co1 O11 Na1 109.1(4) 2_665 . ? Na1 O11 Na1 84.2(4) 2_665 . ? S1 O12 Co1 142.2(6) . 2_565 ? S1 O12 Na1 98.1(5) . 2_665 ? Co1 O12 Na1 117.3(4) 2_565 2_665 ? S1 O13 Co3 130.0(5) . . ? S1 O13 Co2 123.5(5) . . ? Co3 O13 Co2 97.1(3) . . ? S1 O13 Na1 94.0(4) . . ? Co3 O13 Na1 107.2(4) . . ? Co2 O13 Na1 100.2(4) . . ? O23 S2 O22 103.6(5) . . ? O23 S2 O21 104.0(5) . . ? O22 S2 O21 106.8(5) . . ? O23 S2 Na1 69.9(4) . 1_455 ? O22 S2 Na1 146.9(4) . 1_455 ? O21 S2 Na1 48.1(4) . 1_455 ? S2 O21 Co2 129.7(5) . 1_455 ? S2 O21 Na1 104.6(5) . 1_455 ? Co2 O21 Na1 97.7(4) 1_455 1_455 ? S2 O22 Co3 127.7(5) . . ? S2 O22 Na1 105.8(5) . . ? Co3 O22 Na1 96.7(3) . . ? S2 O23 Co1 129.7(5) . 2_565 ? S2 O23 Co1 128.8(5) . . ? Co1 O23 Co1 101.4(4) 2_565 . ? Co1 O1 H1A 119.7 . . ? Co1 O1 H1B 120.0 . . ? H1A O1 H1B 103.8 . . ? Co1 O2 Co2 119.3(4) . 1_556 ? Co1 O2 Co3 117.9(4) . 1_556 ? Co2 O2 Co3 96.6(4) 1_556 1_556 ? Co1 O2 H2A 108.18 . . ? Co2 O2 H2A 107.77 1_556 . ? Co3 O2 H2A 105.87 1_556 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.697 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.339 #===END======================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 750028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Co2 O12 S4, 4(Na)' _chemical_formula_sum 'Co2 Na4 O12 S4' _chemical_formula_weight 530.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.6497(7) _cell_length_b 10.2218(12) _cell_length_c 17.287(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1175.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 2840 _cell_measurement_theta_min 5 _cell_measurement_theta_max 24 _exptl_crystal_description needle _exptl_crystal_colour violet _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.996 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 3.745 _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'KUMA KM4CCD four-circle diffractometer' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 3225 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.88 _reflns_number_total 2124 _reflns_number_gt 1935 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2006) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens (1989), Farrugia (1999)' _computing_publication_material 'SHELXL97 (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^)+(0.0155P)^2^+1.3898P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2124 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0448 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.69534(8) 0.35759(5) 0.85237(3) 0.01521(13) Uani 1 1 d . . . Co2 Co 0.96547(7) 0.10488(5) 0.72277(3) 0.01086(11) Uani 1 1 d . . . Na1 Na 0.6919(2) 0.12327(15) 0.55910(8) 0.0201(3) Uani 1 1 d . . . Na2 Na 0.4279(2) 0.11511(16) 0.95039(8) 0.0214(4) Uani 1 1 d . . . Na3 Na 0.5186(2) -0.39387(17) 0.75469(9) 0.0186(3) Uani 1 1 d . . . Na4 Na 0.7171(2) -0.12247(15) 0.86016(8) 0.0160(3) Uani 1 1 d . . . S1 S 0.77989(14) -0.17565(9) 0.68142(5) 0.0106(2) Uani 1 1 d . . . O11 O 0.5757(4) -0.2272(3) 0.65202(16) 0.0152(6) Uani 1 1 d . . . O12 O 0.7353(4) -0.0377(2) 0.71007(16) 0.0167(6) Uani 1 1 d . . . O13 O 0.8086(4) -0.2563(3) 0.75601(15) 0.0154(6) Uani 1 1 d . . . S2 S 0.90472(13) 0.13390(10) 0.91897(5) 0.0135(2) Uani 1 1 d . . . O21 O 0.8369(4) 0.1298(3) 0.83300(14) 0.0206(6) Uani 1 1 d . . . O22 O 0.8153(4) 0.2679(3) 0.94348(15) 0.0189(6) Uani 1 1 d . . . O23 O 0.7749(4) 0.0346(3) 0.95803(15) 0.0226(7) Uani 1 1 d . . . S3 S 0.79389(13) 0.38511(9) 0.67469(5) 0.01074(18) Uani 1 1 d . . . O31 O 0.7318(4) 0.2436(2) 0.68878(15) 0.0156(6) Uani 1 1 d . . . O32 O 0.8196(4) 0.4415(2) 0.75925(14) 0.0135(6) Uani 1 1 d . . . O33 O 0.6092(4) 0.4543(3) 0.64612(16) 0.0177(6) Uani 1 1 d . . . S4 S 0.21248(13) 0.09336(10) 0.55341(5) 0.01382(19) Uani 1 1 d . . . O41 O 0.0300(4) 0.0987(3) 0.60665(15) 0.0245(7) Uani 1 1 d . . . O42 O 0.2817(5) 0.2290(3) 0.53953(17) 0.0291(7) Uani 1 1 d . . . O43 O 0.3803(4) 0.0343(3) 0.60535(16) 0.0180(6) 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 0.0169(2) 0.0153(3) 0.0135(2) 0.0019(2) -0.0010(2) -0.0034(2) Co2 0.0104(2) 0.0112(3) 0.0110(2) -0.0007(3) -0.00027(19) -0.0002(2) Na1 0.0192(7) 0.0247(9) 0.0164(7) -0.0025(8) 0.0011(6) -0.0055(8) Na2 0.0320(9) 0.0169(8) 0.0152(7) -0.0005(8) 0.0034(7) 0.0013(8) Na3 0.0160(6) 0.0152(8) 0.0248(7) 0.0001(8) 0.0061(6) -0.0013(7) Na4 0.0220(7) 0.0138(8) 0.0123(7) -0.0042(7) 0.0015(6) 0.0032(7) S1 0.0091(4) 0.0104(5) 0.0123(4) -0.0013(4) 0.0003(4) 0.0011(4) O11 0.0138(13) 0.0132(14) 0.0188(14) -0.0030(13) -0.0066(12) 0.0015(11) O12 0.0132(13) 0.0091(13) 0.0277(15) -0.0076(13) 0.0007(13) -0.0009(10) O13 0.0121(12) 0.0182(14) 0.0157(13) 0.0038(12) 0.0001(12) 0.0042(12) S2 0.0140(4) 0.0140(5) 0.0126(4) 0.0000(4) -0.0017(4) -0.0004(4) O21 0.0228(13) 0.0299(17) 0.0091(12) -0.0048(13) 0.0020(10) -0.0022(13) O22 0.0214(13) 0.0183(14) 0.0171(14) -0.0033(13) -0.0022(13) 0.0045(13) O23 0.0269(15) 0.0227(16) 0.0182(14) 0.0051(13) 0.0006(14) -0.0058(13) S3 0.0118(4) 0.0104(5) 0.0100(4) -0.0008(4) 0.0009(3) -0.0006(4) O31 0.0178(14) 0.0072(13) 0.0218(14) 0.0021(12) 0.0005(12) -0.0020(10) O32 0.0165(12) 0.0148(14) 0.0092(12) -0.0025(11) -0.0013(11) -0.0037(11) O33 0.0209(13) 0.0154(15) 0.0169(14) 0.0035(14) -0.0050(13) 0.0038(12) S4 0.0152(4) 0.0157(5) 0.0106(4) 0.0004(4) 0.0008(4) -0.0013(4) O41 0.0139(12) 0.046(2) 0.0138(12) 0.0021(15) -0.0003(11) 0.0038(15) O42 0.0392(17) 0.0185(15) 0.0298(16) 0.0080(14) -0.0044(16) -0.0053(14) O43 0.0146(12) 0.0188(15) 0.0207(14) 0.0027(13) 0.0005(12) 0.0021(12) _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 O22 1.989(3) . ? Co1 O11 2.001(2) 4_656 ? Co1 O32 2.002(3) . ? Co1 O43 2.013(3) 4_656 ? Co1 Na3 3.2692(17) 1_565 ? Co1 Na3 3.4720(17) 4_656 ? Co1 Na2 3.4897(16) . ? Co2 O41 2.054(3) 1_655 ? Co2 O13 2.099(3) 4_756 ? Co2 O21 2.104(2) . ? Co2 O12 2.125(2) . ? Co2 O31 2.184(3) . ? Co2 O32 2.220(3) 4_746 ? Co2 Na3 3.2422(15) 4_656 ? Co2 Na1 3.3688(15) . ? Co2 Na3 3.4531(15) 4_756 ? Na1 O42 2.355(3) 3_556 ? Na1 O23 2.388(3) 2_654 ? Na1 O43 2.400(3) . ? Na1 O41 2.407(3) 1_655 ? Na1 O31 2.571(3) . ? Na1 O42 2.954(4) . ? Na1 S4 3.2043(17) . ? Na1 Na4 3.492(2) 2_654 ? Na1 Na3 3.514(2) 4_656 ? Na1 Na2 3.983(2) 2_654 ? Na1 Na4 4.013(2) 4_656 ? Na2 O22 2.314(3) 3_457 ? Na2 O33 2.355(3) 4_646 ? Na2 O11 2.395(3) 4_656 ? Na2 O23 2.454(3) . ? Na2 S4 2.9297(18) 2 ? Na2 O22 3.015(3) . ? Na2 S2 3.2228(17) . ? Na2 Na4 3.468(2) . ? Na2 Na3 3.564(2) 4_656 ? Na2 Na1 3.983(2) 2_655 ? Na3 O12 2.320(3) 4_646 ? Na3 O13 2.387(3) . ? Na3 O31 2.388(3) 4_646 ? Na3 O11 2.490(3) . ? Na3 O33 2.509(3) 1_545 ? Na3 O43 2.616(3) 4_646 ? Na3 O32 2.616(3) 1_545 ? Na3 O21 2.819(3) 4_646 ? Na3 S1 3.0983(19) . ? Na3 S3 3.2201(18) 1_545 ? Na3 Co2 3.2422(15) 4_646 ? Na3 Co1 3.2692(17) 1_545 ? Na4 O42 2.305(3) 4_646 ? Na4 O33 2.310(3) 4_646 ? Na4 O13 2.342(3) . ? Na4 O23 2.364(3) . ? Na4 O21 2.739(3) . ? Na4 O12 2.738(3) . ? Na4 S2 3.0753(18) . ? Na4 S1 3.1650(16) . ? Na4 S4 3.2999(18) 4_646 ? Na4 S3 3.3079(17) 4_746 ? Na4 Na3 3.444(2) 4_656 ? S1 O12 1.523(2) . ? S1 O13 1.543(3) . ? S1 O11 1.543(3) . ? O11 Co1 2.001(2) 4_646 ? O11 Na2 2.395(3) 4_646 ? O12 Na3 2.320(3) 4_656 ? O13 Co2 2.099(3) 4_746 ? S2 O23 1.494(3) . ? S2 O22 1.552(3) . ? S2 O21 1.554(3) . ? O21 Na3 2.819(3) 4_656 ? O22 Na2 2.314(3) 3_557 ? O23 Na1 2.388(3) 2_655 ? S3 O33 1.501(3) . ? S3 O31 1.523(3) . ? S3 O32 1.581(3) . ? S3 Na3 3.2201(18) 1_565 ? S3 Na4 3.3079(17) 4_756 ? O31 Na3 2.388(3) 4_656 ? O32 Co2 2.220(3) 4_756 ? O32 Na3 2.616(3) 1_565 ? O33 Na4 2.310(3) 4_656 ? O33 Na2 2.355(3) 4_656 ? O33 Na3 2.509(3) 1_565 ? S4 O42 1.480(3) . ? S4 O41 1.524(3) . ? S4 O43 1.554(3) . ? S4 Na2 2.9297(18) 2_554 ? S4 Na4 3.2999(18) 4_656 ? O41 Co2 2.054(3) 1_455 ? O41 Na1 2.407(3) 1_455 ? O42 Na4 2.305(3) 4_656 ? O42 Na1 2.355(3) 3_456 ? O43 Co1 2.013(3) 4_646 ? O43 Na3 2.616(3) 4_656 ? 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 O22 Co1 O11 101.06(11) . 4_656 ? O22 Co1 O32 131.94(11) . . ? O11 Co1 O32 121.78(11) 4_656 . ? O22 Co1 O43 103.08(11) . 4_656 ? O11 Co1 O43 100.21(11) 4_656 4_656 ? O32 Co1 O43 90.61(11) . 4_656 ? O22 Co1 Na3 155.67(8) . 1_565 ? O11 Co1 Na3 89.60(8) 4_656 1_565 ? O32 Co1 Na3 53.15(8) . 1_565 ? O43 Co1 Na3 53.14(9) 4_656 1_565 ? O22 Co1 Na3 104.20(8) . 4_656 ? O11 Co1 Na3 44.79(8) 4_656 4_656 ? O32 Co1 Na3 93.31(8) . 4_656 ? O43 Co1 Na3 139.08(8) 4_656 4_656 ? Na3 Co1 Na3 98.782(16) 1_565 4_656 ? O22 Co1 Na2 59.52(8) . . ? O11 Co1 Na2 41.57(8) 4_656 . ? O32 Co1 Na2 154.81(8) . . ? O43 Co1 Na2 109.50(8) 4_656 . ? Na3 Co1 Na2 128.28(4) 1_565 . ? Na3 Co1 Na2 61.59(4) 4_656 . ? O41 Co2 O13 92.40(11) 1_655 4_756 ? O41 Co2 O21 166.87(10) 1_655 . ? O13 Co2 O21 92.92(10) 4_756 . ? O41 Co2 O12 91.64(12) 1_655 . ? O13 Co2 O12 175.85(11) 4_756 . ? O21 Co2 O12 83.33(10) . . ? O41 Co2 O31 84.58(11) 1_655 . ? O13 Co2 O31 96.75(10) 4_756 . ? O21 Co2 O31 82.88(10) . . ? O12 Co2 O31 84.56(9) . . ? O41 Co2 O32 88.82(11) 1_655 4_746 ? O13 Co2 O32 91.32(10) 4_756 4_746 ? O21 Co2 O32 103.04(10) . 4_746 ? O12 Co2 O32 87.83(10) . 4_746 ? O31 Co2 O32 169.76(10) . 4_746 ? O41 Co2 Na3 108.97(8) 1_655 4_656 ? O13 Co2 Na3 133.40(8) 4_756 4_656 ? O21 Co2 Na3 59.16(7) . 4_656 ? O12 Co2 Na3 45.58(7) . 4_656 ? O31 Co2 Na3 47.43(7) . 4_656 ? O32 Co2 Na3 128.70(8) 4_746 4_656 ? O41 Co2 Na1 45.06(7) 1_655 . ? O13 Co2 Na1 119.71(8) 4_756 . ? O21 Co2 Na1 122.31(8) . . ? O12 Co2 Na1 64.06(8) . . ? O31 Co2 Na1 49.74(7) . . ? O32 Co2 Na1 120.47(7) 4_746 . ? Na3 Co2 Na1 64.19(4) 4_656 . ? O41 Co2 Na3 84.42(7) 1_655 4_756 ? O13 Co2 Na3 42.81(8) 4_756 4_756 ? O21 Co2 Na3 107.52(8) . 4_756 ? O12 Co2 Na3 136.87(7) . 4_756 ? O31 Co2 Na3 137.29(8) . 4_756 ? O32 Co2 Na3 49.26(7) 4_746 4_756 ? Na3 Co2 Na3 166.61(5) 4_656 4_756 ? Na1 Co2 Na3 129.13(4) . 4_756 ? O42 Na1 O23 83.12(10) 3_556 2_654 ? O42 Na1 O43 134.68(12) 3_556 . ? O23 Na1 O43 93.86(11) 2_654 . ? O42 Na1 O41 94.43(12) 3_556 1_655 ? O23 Na1 O41 95.35(11) 2_654 1_655 ? O43 Na1 O41 130.79(11) . 1_655 ? O42 Na1 O31 107.36(11) 3_556 . ? O23 Na1 O31 162.12(11) 2_654 . ? O43 Na1 O31 88.85(10) . . ? O41 Na1 O31 69.87(10) 1_655 . ? O42 Na1 O42 85.21(8) 3_556 . ? O23 Na1 O42 104.39(10) 2_654 . ? O43 Na1 O42 51.64(9) . . ? O41 Na1 O42 160.04(11) 1_655 . ? O31 Na1 O42 91.14(9) . . ? O42 Na1 S4 106.93(10) 3_556 . ? O23 Na1 S4 90.28(8) 2_654 . ? O43 Na1 S4 27.75(7) . . ? O41 Na1 S4 158.43(9) 1_655 . ? O31 Na1 S4 100.08(7) . . ? O42 Na1 S4 27.43(6) . . ? O42 Na1 Co2 120.47(10) 3_556 . ? O23 Na1 Co2 121.80(9) 2_654 . ? O43 Na1 Co2 99.51(8) . . ? O41 Na1 Co2 37.16(6) 1_655 . ? O31 Na1 Co2 40.42(6) . . ? O42 Na1 Co2 127.97(8) . . ? S4 Na1 Co2 123.90(5) . . ? O42 Na1 Na4 40.92(8) 3_556 2_654 ? O23 Na1 Na4 42.44(7) 2_654 2_654 ? O43 Na1 Na4 118.47(9) . 2_654 ? O41 Na1 Na4 100.04(8) 1_655 2_654 ? O31 Na1 Na4 147.36(8) . 2_654 ? O42 Na1 Na4 92.75(7) . 2_654 ? S4 Na1 Na4 98.16(5) . 2_654 ? Co2 Na1 Na4 137.18(5) . 2_654 ? O42 Na1 Na3 142.77(10) 3_556 4_656 ? O23 Na1 Na3 132.31(9) 2_654 4_656 ? O43 Na1 Na3 48.10(8) . 4_656 ? O41 Na1 Na3 93.10(8) 1_655 4_656 ? O31 Na1 Na3 42.80(7) . 4_656 ? O42 Na1 Na3 75.84(7) . 4_656 ? S4 Na1 Na3 68.11(4) . 4_656 ? Co2 Na1 Na3 56.15(3) . 4_656 ? Na4 Na1 Na3 166.15(6) 2_654 4_656 ? O42 Na1 Na2 83.67(9) 3_556 2_654 ? O23 Na1 Na2 35.21(8) 2_654 2_654 ? O43 Na1 Na2 118.26(9) . 2_654 ? O41 Na1 Na2 60.29(8) 1_655 2_654 ? O31 Na1 Na2 129.71(8) . 2_654 ? O42 Na1 Na2 139.12(8) . 2_654 ? S4 Na1 Na2 123.97(5) . 2_654 ? Co2 Na1 Na2 91.11(4) . 2_654 ? Na4 Na1 Na2 54.82(4) 2_654 2_654 ? Na3 Na1 Na2 130.89(6) 4_656 2_654 ? O42 Na1 Na4 90.47(9) 3_556 4_656 ? O23 Na1 Na4 138.98(9) 2_654 4_656 ? O43 Na1 Na4 62.89(8) . 4_656 ? O41 Na1 Na4 125.58(9) 1_655 4_656 ? O31 Na1 Na4 57.08(7) . 4_656 ? O42 Na1 Na4 34.59(6) . 4_656 ? S4 Na1 Na4 52.99(4) . 4_656 ? Co2 Na1 Na4 96.32(4) . 4_656 ? Na4 Na1 Na4 117.48(5) 2_654 4_656 ? Na3 Na1 Na4 56.20(4) 4_656 4_656 ? Na2 Na1 Na4 172.19(5) 2_654 4_656 ? O22 Na2 O33 152.67(12) 3_457 4_646 ? O22 Na2 O11 103.59(11) 3_457 4_656 ? O33 Na2 O11 86.86(10) 4_646 4_656 ? O22 Na2 O23 115.77(11) 3_457 . ? O33 Na2 O23 84.40(10) 4_646 . ? O11 Na2 O23 105.96(10) 4_656 . ? O22 Na2 S4 77.93(8) 3_457 2 ? O33 Na2 S4 83.66(8) 4_646 2 ? O11 Na2 S4 159.39(8) 4_656 2 ? O23 Na2 S4 91.31(8) . 2 ? O22 Na2 O22 92.29(8) 3_457 . ? O33 Na2 O22 115.02(10) 4_646 . ? O11 Na2 O22 68.31(8) 4_656 . ? O23 Na2 O22 51.12(8) . . ? S4 Na2 O22 132.30(8) 2 . ? O22 Na2 S2 114.89(9) 3_457 . ? O33 Na2 S2 91.44(8) 4_646 . ? O11 Na2 S2 81.08(7) 4_656 . ? O23 Na2 S2 26.33(6) . . ? S4 Na2 S2 117.34(6) 2 . ? O22 Na2 S2 28.57(5) . . ? O22 Na2 Na4 153.85(9) 3_457 . ? O33 Na2 Na4 41.47(7) 4_646 . ? O11 Na2 Na4 98.30(8) 4_656 . ? O23 Na2 Na4 42.93(7) . . ? S4 Na2 Na4 86.60(5) 2 . ? O22 Na2 Na4 82.59(7) . . ? S2 Na2 Na4 54.57(4) . . ? O22 Na2 Co1 100.53(9) 3_457 . ? O33 Na2 Co1 101.84(8) 4_646 . ? O11 Na2 Co1 33.68(6) 4_656 . ? O23 Na2 Co1 77.59(7) . . ? S4 Na2 Co1 166.94(6) 2 . ? O22 Na2 Co1 34.65(5) . . ? S2 Na2 Co1 51.27(3) . . ? Na4 Na2 Co1 89.79(4) . . ? O22 Na2 Na3 146.52(10) 3_457 4_656 ? O33 Na2 Na3 44.59(8) 4_646 4_656 ? O11 Na2 Na3 44.19(7) 4_656 4_656 ? O23 Na2 Na3 87.19(8) . 4_656 ? S4 Na2 Na3 128.15(6) 2 4_656 ? O22 Na2 Na3 83.60(7) . 4_656 ? S2 Na2 Na3 74.67(4) . 4_656 ? Na4 Na2 Na3 58.62(4) . 4_656 ? Co1 Na2 Na3 58.96(4) . 4_656 ? O22 Na2 Na1 98.47(8) 3_457 2_655 ? O33 Na2 Na1 88.49(8) 4_646 2_655 ? O11 Na2 Na1 140.09(8) 4_656 2_655 ? O23 Na2 Na1 34.13(7) . 2_655 ? S4 Na2 Na1 58.02(4) 2 2_655 ? O22 Na2 Na1 78.06(6) . 2_655 ? S2 Na2 Na1 59.43(4) . 2_655 ? Na4 Na2 Na1 55.38(4) . 2_655 ? Co1 Na2 Na1 109.89(4) . 2_655 ? Na3 Na2 Na1 112.97(5) 4_656 2_655 ? O12 Na3 O13 163.49(12) 4_646 . ? O12 Na3 O31 76.02(9) 4_646 4_646 ? O13 Na3 O31 102.28(11) . 4_646 ? O12 Na3 O11 137.05(11) 4_646 . ? O13 Na3 O11 58.70(9) . . ? O31 Na3 O11 89.72(10) 4_646 . ? O12 Na3 O33 88.80(11) 4_646 1_545 ? O13 Na3 O33 100.22(10) . 1_545 ? O31 Na3 O33 146.90(11) 4_646 1_545 ? O11 Na3 O33 81.58(9) . 1_545 ? O12 Na3 O43 76.49(10) 4_646 4_646 ? O13 Na3 O43 87.06(10) . 4_646 ? O31 Na3 O43 88.05(10) 4_646 4_646 ? O11 Na3 O43 144.31(11) . 4_646 ? O33 Na3 O43 117.16(11) 1_545 4_646 ? O12 Na3 O32 98.12(10) 4_646 1_545 ? O13 Na3 O32 76.13(8) . 1_545 ? O31 Na3 O32 154.12(10) 4_646 1_545 ? O11 Na3 O32 110.18(9) . 1_545 ? O33 Na3 O32 56.00(9) 1_545 1_545 ? O43 Na3 O32 66.11(9) 4_646 1_545 ? O12 Na3 O21 65.50(9) 4_646 4_646 ? O13 Na3 O21 129.23(10) . 4_646 ? O31 Na3 O21 65.48(9) 4_646 4_646 ? O11 Na3 O21 71.69(9) . 4_646 ? O33 Na3 O21 81.49(9) 1_545 4_646 ? O43 Na3 O21 137.47(9) 4_646 4_646 ? O32 Na3 O21 135.48(10) 1_545 4_646 ? O12 Na3 S1 166.33(9) 4_646 . ? O13 Na3 S1 29.15(6) . . ? O31 Na3 S1 97.73(8) 4_646 . ? O11 Na3 S1 29.57(6) . . ? O33 Na3 S1 90.28(7) 1_545 . ? O43 Na3 S1 115.85(8) 4_646 . ? O32 Na3 S1 92.65(7) 1_545 . ? O21 Na3 S1 100.88(7) 4_646 . ? O12 Na3 S3 94.69(9) 4_646 1_545 ? O13 Na3 S3 87.59(8) . 1_545 ? O31 Na3 S3 170.11(9) 4_646 1_545 ? O11 Na3 S3 95.01(8) . 1_545 ? O33 Na3 S3 26.89(6) 1_545 1_545 ? O43 Na3 S3 93.10(8) 4_646 1_545 ? O32 Na3 S3 29.15(6) 1_545 1_545 ? O21 Na3 S3 107.82(8) 4_646 1_545 ? S1 Na3 S3 90.61(4) . 1_545 ? O12 Na3 Co2 40.85(6) 4_646 4_646 ? O13 Na3 Co2 143.45(9) . 4_646 ? O31 Na3 Co2 42.36(7) 4_646 4_646 ? O11 Na3 Co2 103.87(7) . 4_646 ? O33 Na3 Co2 109.02(8) 1_545 4_646 ? O43 Na3 Co2 98.22(7) 4_646 4_646 ? O32 Na3 Co2 138.89(8) 1_545 4_646 ? O21 Na3 Co2 39.86(5) 4_646 4_646 ? S1 Na3 Co2 127.50(6) . 4_646 ? S3 Na3 Co2 127.83(6) 1_545 4_646 ? O12 Na3 Co1 68.50(7) 4_646 1_545 ? O13 Na3 Co1 99.34(8) . 1_545 ? O31 Na3 Co1 119.78(8) 4_646 1_545 ? O11 Na3 Co1 147.71(8) . 1_545 ? O33 Na3 Co1 79.59(7) 1_545 1_545 ? O43 Na3 Co1 37.99(7) 4_646 1_545 ? O32 Na3 Co1 37.77(6) 1_545 1_545 ? O21 Na3 Co1 130.24(8) 4_646 1_545 ? S1 Na3 Co1 124.68(5) . 1_545 ? S3 Na3 Co1 58.14(3) 1_545 1_545 ? Co2 Na3 Co1 106.97(5) 4_646 1_545 ? O42 Na4 O33 105.21(12) 4_646 4_646 ? O42 Na4 O13 101.10(11) 4_646 . ? O33 Na4 O13 113.98(11) 4_646 . ? O42 Na4 O23 84.74(10) 4_646 . ? O33 Na4 O23 87.47(11) 4_646 . ? O13 Na4 O23 154.81(12) . . ? O42 Na4 O21 138.42(11) 4_646 . ? O33 Na4 O21 86.87(10) 4_646 . ? O13 Na4 O21 110.04(10) . . ? O23 Na4 O21 55.68(9) . . ? O42 Na4 O12 157.10(11) 4_646 . ? O33 Na4 O12 83.66(10) 4_646 . ? O13 Na4 O12 56.28(8) . . ? O23 Na4 O12 117.14(10) . . ? O21 Na4 O12 61.76(8) . . ? O42 Na4 S2 108.13(9) 4_646 . ? O33 Na4 S2 96.15(8) 4_646 . ? O13 Na4 S2 130.30(9) . . ? O23 Na4 S2 28.20(7) . . ? O21 Na4 S2 30.30(5) . . ? O12 Na4 S2 91.48(7) . . ? O42 Na4 S1 128.38(9) 4_646 . ? O33 Na4 S1 97.84(8) 4_646 . ? O13 Na4 S1 27.73(6) . . ? O23 Na4 S1 142.56(9) . . ? O21 Na4 S1 87.48(6) . . ? O12 Na4 S1 28.76(5) . . ? S2 Na4 S1 114.56(5) . . ? O42 Na4 S4 22.92(7) 4_646 4_646 ? O33 Na4 S4 116.97(9) 4_646 4_646 ? O13 Na4 S4 78.28(7) . 4_646 ? O23 Na4 S4 104.51(8) . 4_646 ? O21 Na4 S4 149.87(8) . 4_646 ? O12 Na4 S4 134.53(7) . 4_646 ? S2 Na4 S4 122.88(5) . 4_646 ? S1 Na4 S4 105.79(5) . 4_646 ? O42 Na4 S3 98.57(10) 4_646 4_746 ? O33 Na4 S3 155.08(9) 4_646 4_746 ? O13 Na4 S3 67.56(7) . 4_746 ? O23 Na4 S3 87.39(9) . 4_746 ? O21 Na4 S3 70.17(6) . 4_746 ? O12 Na4 S3 77.09(6) . 4_746 ? S2 Na4 S3 68.99(4) . 4_746 ? S1 Na4 S3 72.34(4) . 4_746 ? S4 Na4 S3 87.91(4) 4_646 4_746 ? O42 Na4 Na3 151.93(11) 4_646 4_656 ? O33 Na4 Na3 46.76(8) 4_646 4_656 ? O13 Na4 Na3 94.10(8) . 4_656 ? O23 Na4 Na3 91.48(9) . 4_656 ? O21 Na4 Na3 52.76(6) . 4_656 ? O12 Na4 Na3 42.19(6) . 4_656 ? S2 Na4 Na3 78.29(5) . 4_656 ? S1 Na4 Na3 67.28(4) . 4_656 ? S4 Na4 Na3 157.36(6) 4_646 4_656 ? S3 Na4 Na3 109.06(5) 4_746 4_656 ? O42 Na4 Na2 97.17(9) 4_646 . ? O33 Na4 Na2 42.47(7) 4_646 . ? O13 Na4 Na2 154.02(9) . . ? O23 Na4 Na2 44.99(8) . . ? O21 Na4 Na2 65.12(6) . . ? O12 Na4 Na2 103.25(7) . . ? S2 Na4 Na2 58.64(4) . . ? S1 Na4 Na2 129.23(5) . . ? S4 Na4 Na2 119.43(5) 4_646 . ? S3 Na4 Na2 127.63(5) 4_746 . ? Na3 Na4 Na2 62.08(4) 4_656 . ? O12 S1 O13 104.31(15) . . ? O12 S1 O11 104.58(14) . . ? O13 S1 O11 101.64(15) . . ? O12 S1 Na3 115.10(11) . . ? O13 S1 Na3 48.90(11) . . ? O11 S1 Na3 52.79(11) . . ? O12 S1 Na4 59.86(11) . . ? O13 S1 Na4 44.93(10) . . ? O11 S1 Na4 105.32(11) . . ? Na3 S1 Na4 69.55(4) . . ? S1 O11 Co1 131.11(16) . 4_646 ? S1 O11 Na2 118.82(14) . 4_646 ? Co1 O11 Na2 104.75(11) 4_646 4_646 ? S1 O11 Na3 97.64(13) . . ? Co1 O11 Na3 100.72(11) 4_646 . ? Na2 O11 Na3 93.71(10) 4_646 . ? S1 O12 Co2 121.89(14) . . ? S1 O12 Na3 144.44(15) . 4_656 ? Co2 O12 Na3 93.57(10) . 4_656 ? S1 O12 Na4 91.37(12) . . ? Co2 O12 Na4 98.68(10) . . ? Na3 O12 Na4 85.39(10) 4_656 . ? S1 O13 Co2 126.59(15) . 4_746 ? S1 O13 Na4 107.34(14) . . ? Co2 O13 Na4 116.52(12) 4_746 . ? S1 O13 Na3 101.95(14) . . ? Co2 O13 Na3 100.49(11) 4_746 . ? Na4 O13 Na3 98.14(11) . . ? O23 S2 O22 104.79(16) . . ? O23 S2 O21 104.25(16) . . ? O22 S2 O21 100.03(15) . . ? O23 S2 Na4 48.39(11) . . ? O22 S2 Na4 133.39(12) . . ? O21 S2 Na4 62.79(11) . . ? O23 S2 Na2 46.76(12) . . ? O22 S2 Na2 68.28(11) . . ? O21 S2 Na2 82.77(10) . . ? Na4 S2 Na2 66.78(4) . . ? S2 O21 Co2 138.74(16) . . ? S2 O21 Na4 86.91(12) . . ? Co2 O21 Na4 99.19(11) . . ? S2 O21 Na3 139.48(14) . 4_656 ? Co2 O21 Na3 80.98(8) . 4_656 ? Na4 O21 Na3 76.56(8) . 4_656 ? S2 O22 Co1 110.12(14) . . ? S2 O22 Na2 123.27(16) . 3_557 ? Co1 O22 Na2 121.28(13) . 3_557 ? S2 O22 Na2 83.16(11) . . ? Co1 O22 Na2 85.83(10) . . ? Na2 O22 Na2 120.83(11) 3_557 . ? S2 O23 Na4 103.41(14) . . ? S2 O23 Na1 137.44(17) . 2_655 ? Na4 O23 Na1 94.58(11) . 2_655 ? S2 O23 Na2 106.91(15) . . ? Na4 O23 Na2 92.08(11) . . ? Na1 O23 Na2 110.66(12) 2_655 . ? O33 S3 O31 106.14(15) . . ? O33 S3 O32 102.77(15) . . ? O31 S3 O32 103.16(14) . . ? O33 S3 Na3 49.12(11) . 1_565 ? O31 S3 Na3 116.31(11) . 1_565 ? O32 S3 Na3 53.73(10) . 1_565 ? O33 S3 Na4 139.07(12) . 4_756 ? O31 S3 Na4 105.87(11) . 4_756 ? O32 S3 Na4 94.05(11) . 4_756 ? Na3 S3 Na4 130.81(5) 1_565 4_756 ? S3 O31 Co2 117.80(14) . . ? S3 O31 Na3 144.40(16) . 4_656 ? Co2 O31 Na3 90.21(10) . 4_656 ? S3 O31 Na1 110.05(14) . . ? Co2 O31 Na1 89.84(10) . . ? Na3 O31 Na1 90.19(10) 4_656 . ? S3 O32 Co1 122.86(15) . . ? S3 O32 Co2 118.26(14) . 4_756 ? Co1 O32 Co2 118.38(11) . 4_756 ? S3 O32 Na3 97.12(12) . 1_565 ? Co1 O32 Na3 89.08(10) . 1_565 ? Co2 O32 Na3 90.74(9) 4_756 1_565 ? S3 O33 Na4 128.62(16) . 4_656 ? S3 O33 Na2 130.36(16) . 4_656 ? Na4 O33 Na2 96.06(10) 4_656 4_656 ? S3 O33 Na3 103.99(14) . 1_565 ? Na4 O33 Na3 91.13(11) 4_656 1_565 ? Na2 O33 Na3 94.18(11) 4_656 1_565 ? O42 S4 O41 108.15(18) . . ? O42 S4 O43 103.54(17) . . ? O41 S4 O43 103.70(14) . . ? O42 S4 Na2 132.98(13) . 2_554 ? O41 S4 Na2 98.03(13) . 2_554 ? O43 S4 Na2 107.30(12) . 2_554 ? O42 S4 Na1 66.82(13) . . ? O41 S4 Na1 140.37(11) . . ? O43 S4 Na1 45.97(10) . . ? Na2 S4 Na1 113.89(5) 2_554 . ? O42 S4 Na4 37.33(12) . 4_656 ? O41 S4 Na4 78.91(13) . 4_656 ? O43 S4 Na4 88.76(11) . 4_656 ? Na2 S4 Na4 163.88(5) 2_554 4_656 ? Na1 S4 Na4 76.17(4) . 4_656 ? S4 O41 Co2 139.27(16) . 1_455 ? S4 O41 Na1 122.77(15) . 1_455 ? Co2 O41 Na1 97.78(10) 1_455 1_455 ? S4 O42 Na4 119.74(17) . 4_656 ? S4 O42 Na1 129.73(18) . 3_456 ? Na4 O42 Na1 97.08(12) 4_656 3_456 ? S4 O42 Na1 85.75(13) . . ? Na4 O42 Na1 98.72(12) 4_656 . ? Na1 O42 Na1 123.49(13) 3_456 . ? S4 O43 Co1 112.26(15) . 4_646 ? S4 O43 Na1 106.28(14) . . ? Co1 O43 Na1 132.60(13) 4_646 . ? S4 O43 Na3 127.57(15) . 4_656 ? Co1 O43 Na3 88.87(11) 4_646 4_656 ? Na1 O43 Na3 88.84(10) . 4_656 ? _diffrn_measured_fraction_theta_max 0.883 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.334 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.084 #===END======================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 750029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Co3 H18 N6 O18 S6, 2(H2 O), 4(H4 N)' _chemical_formula_sum 'Co3 H38 N10 O20 S6' _chemical_formula_weight 867.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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' 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 trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 9.9242(5) _cell_length_b 9.9242(5) _cell_length_c 30.2127(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2577.0(2) _cell_formula_units_Z 3 _cell_measurement_temperature 295(1) _cell_measurement_reflns_used 8379 _cell_measurement_theta_min 3 _cell_measurement_theta_max 22 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1335 _exptl_absorpt_coefficient_mu 1.873 _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_T_max 0.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'KUMA KM4CCD four-circle diffractometer' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 8406 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0102 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1012 _reflns_number_gt 982 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2006) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens (1989), Farrugia (1999)' _computing_publication_material 'SHELXL97 (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^)+(0.1821P)^2^+3.4752P] 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 1012 _refine_ls_number_parameters 67 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.2307 _refine_ls_wR_factor_gt 0.2255 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.242 _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 0.12823(3) 0.0195(5) Uani 1 3 d S . . Co2 Co 0.0000 0.0000 0.0000 0.0206(6) Uani 1 6 d S . . S1 S 0.21406(11) 0.13441(12) 0.08802(3) 0.0263(6) Uani 1 1 d . . . O11 O 0.2625(5) 0.3012(4) 0.09062(14) 0.0569(12) Uani 1 1 d . . . O12 O 0.3407(4) 0.1134(5) 0.10585(12) 0.0471(11) Uani 1 1 d . . . O13 O 0.1954(3) 0.0867(4) 0.04038(9) 0.0337(9) Uani 1 1 d . . . N1 N 0.1117(5) -0.0756(4) 0.16704(13) 0.0319(9) Uani 1 1 d . . . H11 H 0.1759 0.0007 0.1850 0.038 Uiso 1 1 calc R . . H12 H 0.1662 -0.1053 0.1503 0.038 Uiso 1 1 calc R . . H13 H 0.0428 -0.1560 0.1830 0.038 Uiso 1 1 calc R . . N1A N 0.2581(18) 0.4582(12) 0.0163(4) 0.110(5) Uani 0.66667 1 d PU A 1 H3A H 0.1782 0.4714 0.0244 0.132 Uiso 0.66667 1 d PR A 1 H4A H 0.3330 0.5484 0.0048 0.132 Uiso 0.66667 1 d PR A 1 H1A H 0.2954 0.4333 0.0401 0.132 Uiso 0.66667 1 d PR A 1 H2A H 0.2255 0.3828 -0.0044 0.132 Uiso 0.66667 1 d PR A 1 O1B O 0.1439(18) 0.4443(12) 0.0232(4) 0.091(5) Uani 0.33333 1 d PRU A 2 H1B H 0.1794 0.4186 0.0483 0.109 Uiso 0.33333 1 d PR A 2 H2B H 0.1108 0.3644 0.0027 0.109 Uiso 0.33333 1 d PR A 2 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 0.0232(6) 0.0232(6) 0.0120(8) 0.000 0.000 0.0116(3) Co2 0.0246(7) 0.0246(7) 0.0125(8) 0.000 0.000 0.0123(3) S1 0.0221(7) 0.0323(8) 0.0169(8) -0.0014(4) -0.0003(3) 0.0079(5) O11 0.063(3) 0.0310(19) 0.051(2) -0.0020(17) 0.0199(19) 0.0038(19) O12 0.0295(19) 0.078(3) 0.029(2) 0.0045(16) -0.0036(14) 0.0238(19) O13 0.0266(15) 0.051(2) 0.0147(16) -0.0012(14) 0.0004(11) 0.0130(15) N1 0.038(2) 0.038(2) 0.020(2) 0.0055(14) -0.0045(14) 0.0199(18) N1A 0.134(9) 0.076(7) 0.100(7) -0.012(5) -0.006(7) 0.037(6) O1B 0.109(10) 0.074(8) 0.087(8) 0.009(7) -0.017(7) 0.043(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 N1 2.000(4) 2 ? Co1 N1 2.000(4) 3 ? Co1 N1 2.000(4) . ? Co1 S1 2.2213(11) 2 ? Co1 S1 2.2213(11) 3 ? Co1 S1 2.2213(11) . ? Co2 O13 2.079(3) 10 ? Co2 O13 2.079(3) 11 ? Co2 O13 2.079(3) . ? Co2 O13 2.079(3) 2 ? Co2 O13 2.079(3) 12 ? Co2 O13 2.079(3) 3 ? S1 O12 1.474(4) . ? S1 O11 1.477(4) . ? S1 O13 1.498(3) . ? N1 H11 0.8900 . ? N1 H12 0.8900 . ? N1 H13 0.8900 . ? N1A H3A 0.9001 . ? N1A H4A 0.8999 . ? N1A H1A 0.9008 . ? N1A H2A 0.9004 . ? O1B H1B 0.9241 . ? O1B H2B 0.9272 . ? 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 N1 Co1 N1 89.11(17) 2 3 ? N1 Co1 N1 89.11(17) 2 . ? N1 Co1 N1 89.11(17) 3 . ? N1 Co1 S1 90.16(12) 2 2 ? N1 Co1 S1 87.74(12) 3 2 ? N1 Co1 S1 176.78(12) . 2 ? N1 Co1 S1 176.78(12) 2 3 ? N1 Co1 S1 90.16(12) 3 3 ? N1 Co1 S1 87.74(12) . 3 ? S1 Co1 S1 92.95(4) 2 3 ? N1 Co1 S1 87.74(12) 2 . ? N1 Co1 S1 176.78(12) 3 . ? N1 Co1 S1 90.16(12) . . ? S1 Co1 S1 92.95(4) 2 . ? S1 Co1 S1 92.95(4) 3 . ? O13 Co2 O13 89.04(11) 10 11 ? O13 Co2 O13 180.00(13) 10 . ? O13 Co2 O13 90.96(11) 11 . ? O13 Co2 O13 90.96(11) 10 2 ? O13 Co2 O13 180.0(2) 11 2 ? O13 Co2 O13 89.04(11) . 2 ? O13 Co2 O13 89.04(11) 10 12 ? O13 Co2 O13 89.04(11) 11 12 ? O13 Co2 O13 90.96(11) . 12 ? O13 Co2 O13 90.96(11) 2 12 ? O13 Co2 O13 90.96(11) 10 3 ? O13 Co2 O13 90.96(11) 11 3 ? O13 Co2 O13 89.04(11) . 3 ? O13 Co2 O13 89.04(11) 2 3 ? O13 Co2 O13 180.00(19) 12 3 ? O12 S1 O11 108.4(3) . . ? O12 S1 O13 106.6(2) . . ? O11 S1 O13 109.0(2) . . ? O12 S1 Co1 110.00(16) . . ? O11 S1 Co1 108.77(17) . . ? O13 S1 Co1 113.94(13) . . ? S1 O13 Co2 129.59(19) . . ? Co1 N1 H11 109.5 . . ? Co1 N1 H12 109.5 . . ? H11 N1 H12 109.5 . . ? Co1 N1 H13 109.5 . . ? H11 N1 H13 109.5 . . ? H12 N1 H13 109.5 . . ? H3A N1A H4A 108.1 . . ? H3A N1A H1A 109.5 . . ? H4A N1A H1A 109.5 . . ? H3A N1A H2A 109.5 . . ? H4A N1A H2A 109.5 . . ? H1A N1A H2A 110.6 . . ? H1B O1B H2B 109.5 . . ? 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 N1A H1A O11 0.90 1.93 2.747(12) 150.1 . O1B H1B O11 0.92 2.15 3.037(14) 159.9 . N1A H2A O13 0.90 1.96 2.839(12) 166.0 12 O1B H2B O13 0.93 2.11 3.008(13) 161.4 12 N1 H13 O12 0.89 2.08 2.968(5) 172.7 15_445 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.840 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.345