# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1862 data_qv1-6d _audit_creation_method SHELXL-97 _chemical_name_systematic ; trtra hydrate bis-4,4'-biphenylenedicarboxylato di sodium one cobalt ; _publ_requested_journal 'Chem. Commun.' _publ_section_title ; The First Pillared 3D Structure Constructed by Carboxylate Ligands Bridging Heterometallic Tri-layers ; _publ_contact_author ; Li Jing Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; _publ_contact_author_email jingli@crab.rutgers.edu _publ_contact_author_fax '+1(856)225-6506' _publ_contact_author_phone '+1(856)225-6160' loop_ _publ_author_name _publ_author_address 'Pan Long' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Finkel Bruce S.' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Huang Xiaoying' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; 'Li Jing' ; Department of Chemistry, Rutgers University, Camden, NJ 08102, USA ; _chemical_name_common ? _chemical_formula_moiety Na2Co(bpdc)2(H2O)4 _chemical_formula_sum 'C28 H24 Co Na2 O12' _chemical_formula_weight 657.38 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' 'Na' 'Na' 0.0362 0.0249 '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 31.746(6) _cell_length_b 6.0830(10) _cell_length_c 13.363(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.35(3) _cell_angle_gamma 90.00 _cell_volume 2500.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.41 _cell_measurement_theta_max 10.46 _exptl_crystal_description block _exptl_crystal_colour redish _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 1.000 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 250 _diffrn_standards_decay_% +-4.0 _diffrn_reflns_number 5097 _diffrn_reflns_av_R_equivalents 0.1573 _diffrn_reflns_av_sigmaI/netI 0.2203 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.98 _reflns_number_total 2451 _reflns_number_gt 1096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4/PC' _computing_cell_refinement 'CAD4/PC' _computing_data_reduction 'XCAD4/PC' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Schakal 97(Keller, 1997)' _computing_publication_material 'Windows Word97' _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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1097 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1939 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.2500 0.2500 0.5000 0.0234(3) Uani 1 d S . . Na Na 0.18880(6) 0.1076(4) 0.26252(16) 0.0330(6) Uani 1 d . . . O1 O 0.19464(9) 0.0671(6) 0.4539(2) 0.0247(10) Uani 1 d . . . O2 O 0.20110(9) -0.1659(5) 0.5877(3) 0.0254(10) Uani 1 d . . . O3 O -0.16688(9) -0.2302(7) 0.2933(2) 0.0291(9) Uani 1 d . . . O4 O -0.15322(10) -0.5666(6) 0.2454(3) 0.0310(10) Uani 1 d . . . O5 O 0.26667(9) 0.1002(6) 0.3641(2) 0.0285(10) Uani 1 d . . . H1 H 0.2891 0.1735 0.3375 0.034 Uiso 1 d R . . H2 H 0.2800 -0.0311 0.3958 0.034 Uiso 1 d R . . O6 O 0.22062(9) 0.5115(6) 0.4144(2) 0.0320(10) Uani 1 d . . . H3 H 0.1958 0.4995 0.3727 0.038 Uiso 1 d R . . H4 H 0.2445 0.5539 0.3902 0.038 Uiso 1 d R . . C1 C 0.17979(15) -0.0754(9) 0.5054(4) 0.0207(13) Uani 1 d . . . C2 C 0.13253(15) -0.1342(10) 0.4658(4) 0.0203(14) Uani 1 d . . . C3 C 0.11700(15) -0.3355(9) 0.4862(4) 0.0249(15) Uani 1 d . . . H5 H 0.1369 -0.4453 0.5174 0.030 Uiso 1 d R . . C4 C 0.07305(14) -0.3812(9) 0.4542(3) 0.0242(14) Uani 1 d . . . H6 H 0.0610 -0.5073 0.4703 0.029 Uiso 1 d R . . C5 C 0.04387(13) -0.2210(11) 0.4049(3) 0.0212(14) Uani 1 d . . . C6 C 0.06052(14) -0.0202(9) 0.3837(4) 0.0225(13) Uani 1 d . . . H7 H 0.0382 0.1006 0.3572 0.027 Uiso 1 d R . . C7 C 0.10445(14) 0.0207(9) 0.4130(4) 0.0255(14) Uani 1 d . . . H8 H 0.1126 0.1541 0.3886 0.031 Uiso 1 d R . . C8 C -0.00357(14) -0.2654(11) 0.3775(3) 0.0183(11) Uani 1 d . . . C9 C -0.02030(15) -0.4694(9) 0.3457(4) 0.0226(14) Uani 1 d . . . H9 H -0.0025 -0.5756 0.3368 0.027 Uiso 1 d R . . C10 C -0.06420(14) -0.5075(10) 0.3127(4) 0.0254(14) Uani 1 d . . . H10 H -0.0760 -0.6494 0.2957 0.030 Uiso 1 d R . . C11 C -0.09354(16) -0.3416(9) 0.3149(4) 0.0206(14) Uani 1 d . . . C12 C -0.07767(14) -0.1404(10) 0.3506(4) 0.0225(14) Uani 1 d . . . H11 H -0.0959 -0.0205 0.3556 0.027 Uiso 1 d R . . C13 C -0.03290(15) -0.0978(9) 0.3804(4) 0.0252(14) Uani 1 d . . . H12 H -0.0234 0.0422 0.4063 0.030 Uiso 1 d R . . C14 C -0.14124(16) -0.3804(10) 0.2820(4) 0.0231(14) Uani 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 Co 0.0164(5) 0.0247(6) 0.0264(6) 0.0028(8) 0.0000(5) -0.0043(7) Na 0.0292(12) 0.0289(15) 0.0395(14) -0.0025(13) 0.0055(10) 0.0028(11) O1 0.0177(19) 0.025(2) 0.028(2) 0.003(2) -0.0007(17) -0.0072(18) O2 0.0193(19) 0.024(2) 0.030(2) 0.0072(19) 0.0018(17) -0.0033(16) O3 0.0161(17) 0.023(2) 0.049(2) 0.004(3) 0.0094(17) -0.002(2) O4 0.020(2) 0.029(3) 0.039(2) 0.000(2) -0.0033(17) -0.0065(19) O5 0.023(2) 0.026(2) 0.040(2) 0.005(2) 0.0129(17) -0.0001(17) O6 0.0136(17) 0.038(3) 0.039(2) 0.011(2) -0.0048(17) -0.0063(19) C1 0.025(3) 0.014(3) 0.025(3) -0.001(3) 0.010(3) 0.003(3) C2 0.017(3) 0.025(3) 0.020(3) 0.010(3) 0.006(2) 0.003(3) C3 0.018(3) 0.024(4) 0.028(3) 0.006(3) -0.001(3) -0.002(3) C4 0.018(3) 0.029(4) 0.024(3) 0.002(3) 0.004(2) -0.009(3) C5 0.013(2) 0.031(4) 0.019(3) -0.009(3) 0.002(2) 0.002(3) C6 0.015(3) 0.018(3) 0.035(3) -0.001(3) 0.007(2) 0.004(3) C7 0.019(3) 0.024(3) 0.036(4) 0.000(3) 0.013(3) -0.009(3) C8 0.018(2) 0.024(3) 0.014(3) -0.002(3) 0.007(2) 0.002(3) C9 0.026(3) 0.020(3) 0.023(3) -0.003(3) 0.008(3) 0.001(3) C10 0.022(3) 0.029(4) 0.023(3) -0.003(3) 0.002(2) -0.009(3) C11 0.022(3) 0.022(3) 0.017(3) -0.003(3) 0.003(3) -0.006(3) C12 0.016(3) 0.028(4) 0.026(3) -0.006(3) 0.010(2) 0.001(3) C13 0.023(3) 0.021(3) 0.030(4) -0.005(3) 0.005(3) -0.010(3) C14 0.022(3) 0.027(4) 0.018(3) 0.009(3) 0.001(2) 0.000(3) _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 Co O1 2.042(3) . ? Co O1 2.042(3) 7_556 ? Co O6 2.044(3) . ? Co O6 2.044(3) 7_556 ? Co O5 2.210(3) 7_556 ? Co O5 2.210(3) . ? Co Na 3.397(2) . ? Co Na 3.397(2) 7_556 ? Na O3 2.238(5) 2 ? Na O4 2.271(4) 2_565 ? Na O2 2.487(4) 6 ? Na O5 2.509(3) . ? Na O1 2.530(4) . ? O1 C1 1.268(5) . ? O2 C1 1.266(5) . ? O2 Na 2.487(4) 6_556 ? O3 C14 1.257(6) . ? O3 Na 2.238(5) 2 ? O4 C14 1.255(6) . ? O4 Na 2.271(4) 2_545 ? O5 H1 0.9790 . ? O5 H2 0.9526 . ? O6 H3 0.8478 . ? O6 H4 0.9307 . ? C1 C2 1.505(6) . ? C2 C7 1.367(6) . ? C2 C3 1.372(6) . ? C3 C4 1.382(6) . ? C3 H5 0.9433 . ? C4 C5 1.393(7) . ? C4 H6 0.9064 . ? C5 C6 1.388(8) . ? C5 C8 1.484(6) . ? C6 C7 1.374(6) . ? C6 H7 1.0208 . ? C7 H8 0.9338 . ? C8 C9 1.375(7) . ? C8 C13 1.388(7) . ? C9 C10 1.373(5) . ? C9 H9 0.8853 . ? C10 C11 1.379(7) . ? C10 H10 0.9458 . ? C11 C12 1.364(7) . ? C11 C14 1.487(6) . ? C12 C13 1.402(6) . ? C12 H11 0.9437 . ? C13 H12 0.9402 . ? 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 Co O1 180.0 . 7_556 ? O1 Co O6 90.92(13) . . ? O1 Co O6 89.08(13) 7_556 . ? O1 Co O6 89.08(13) . 7_556 ? O1 Co O6 90.92(13) 7_556 7_556 ? O6 Co O6 180.0 . 7_556 ? O1 Co O5 96.25(12) . 7_556 ? O1 Co O5 83.75(12) 7_556 7_556 ? O6 Co O5 88.28(13) . 7_556 ? O6 Co O5 91.72(13) 7_556 7_556 ? O1 Co O5 83.75(12) . . ? O1 Co O5 96.25(12) 7_556 . ? O6 Co O5 91.72(13) . . ? O6 Co O5 88.28(13) 7_556 . ? O5 Co O5 180.0 7_556 . ? O1 Co Na 47.87(10) . . ? O1 Co Na 132.13(10) 7_556 . ? O6 Co Na 66.39(10) . . ? O6 Co Na 113.61(10) 7_556 . ? O5 Co Na 132.43(8) 7_556 . ? O5 Co Na 47.57(8) . . ? O1 Co Na 132.13(10) . 7_556 ? O1 Co Na 47.87(10) 7_556 7_556 ? O6 Co Na 113.61(10) . 7_556 ? O6 Co Na 66.39(10) 7_556 7_556 ? O5 Co Na 47.57(8) 7_556 7_556 ? O5 Co Na 132.43(8) . 7_556 ? Na Co Na 180.0 . 7_556 ? O3 Na O4 132.54(14) 2 2_565 ? O3 Na O2 85.76(13) 2 6 ? O4 Na O2 91.38(14) 2_565 6 ? O3 Na O5 110.32(14) 2 . ? O4 Na O5 116.94(13) 2_565 . ? O2 Na O5 98.51(12) 6 . ? O3 Na O1 100.74(14) 2 . ? O4 Na O1 92.46(14) 2_565 . ? O2 Na O1 166.91(13) 6 . ? O5 Na O1 68.63(11) . . ? O3 Na Co 127.17(12) 2 . ? O4 Na Co 89.06(10) 2_565 . ? O2 Na Co 130.88(10) 6 . ? O5 Na Co 40.55(8) . . ? O1 Na Co 36.76(8) . . ? C1 O1 Co 128.1(3) . . ? C1 O1 Na 132.2(3) . . ? Co O1 Na 95.36(14) . . ? C1 O2 Na 125.4(3) . 6_556 ? C14 O3 Na 141.7(3) . 2 ? C14 O4 Na 154.8(4) . 2_545 ? Co O5 Na 91.88(11) . . ? Co O5 H1 117.1 . . ? Na O5 H1 120.2 . . ? Co O5 H2 98.7 . . ? Na O5 H2 121.7 . . ? H1 O5 H2 105.1 . . ? Co O6 H3 121.4 . . ? Co O6 H4 96.4 . . ? H3 O6 H4 120.0 . . ? O2 C1 O1 125.3(5) . . ? O2 C1 C2 118.3(5) . . ? O1 C1 C2 116.4(5) . . ? C7 C2 C3 119.8(5) . . ? C7 C2 C1 118.9(5) . . ? C3 C2 C1 121.2(5) . . ? C2 C3 C4 120.2(5) . . ? C2 C3 H5 119.0 . . ? C4 C3 H5 120.7 . . ? C3 C4 C5 120.5(5) . . ? C3 C4 H6 123.3 . . ? C5 C4 H6 115.7 . . ? C6 C5 C4 118.0(4) . . ? C6 C5 C8 121.6(5) . . ? C4 C5 C8 120.3(5) . . ? C7 C6 C5 120.8(5) . . ? C7 C6 H7 122.4 . . ? C5 C6 H7 116.0 . . ? C2 C7 C6 120.5(5) . . ? C2 C7 H8 125.3 . . ? C6 C7 H8 113.9 . . ? C9 C8 C13 117.5(4) . . ? C9 C8 C5 122.1(5) . . ? C13 C8 C5 120.4(6) . . ? C10 C9 C8 122.3(5) . . ? C10 C9 H9 117.7 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 120.5(5) . . ? C9 C10 H10 122.8 . . ? C11 C10 H10 116.3 . . ? C12 C11 C10 118.1(5) . . ? C12 C11 C14 120.5(5) . . ? C10 C11 C14 121.4(5) . . ? C11 C12 C13 121.7(5) . . ? C11 C12 H11 122.6 . . ? C13 C12 H11 115.7 . . ? C8 C13 C12 119.8(5) . . ? C8 C13 H12 121.3 . . ? C12 C13 H12 118.8 . . ? O4 C14 O3 124.1(5) . . ? O4 C14 C11 116.5(5) . . ? O3 C14 C11 119.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co Na O3 -51.36(18) . . . 2 ? O1 Co Na O3 128.64(18) 7_556 . . 2 ? O6 Co Na O3 -166.12(17) . . . 2 ? O6 Co Na O3 13.88(17) 7_556 . . 2 ? O5 Co Na O3 -102.47(18) 7_556 . . 2 ? O5 Co Na O3 77.53(18) . . . 2 ? Na Co Na O3 97(76) 7_556 . . 2 ? O1 Co Na O4 95.38(16) . . . 2_565 ? O1 Co Na O4 -84.62(16) 7_556 . . 2_565 ? O6 Co Na O4 -19.38(13) . . . 2_565 ? O6 Co Na O4 160.62(13) 7_556 . . 2_565 ? O5 Co Na O4 44.27(16) 7_556 . . 2_565 ? O5 Co Na O4 -135.73(16) . . . 2_565 ? Na Co Na O4 -116(76) 7_556 . . 2_565 ? O1 Co Na O2 -173.6(2) . . . 6 ? O1 Co Na O2 6.4(2) 7_556 . . 6 ? O6 Co Na O2 71.63(17) . . . 6 ? O6 Co Na O2 -108.37(17) 7_556 . . 6 ? O5 Co Na O2 135.28(18) 7_556 . . 6 ? O5 Co Na O2 -44.72(18) . . . 6 ? Na Co Na O2 -25(76) 7_556 . . 6 ? O1 Co Na O5 -128.89(18) . . . . ? O1 Co Na O5 51.11(18) 7_556 . . . ? O6 Co Na O5 116.35(16) . . . . ? O6 Co Na O5 -63.65(16) 7_556 . . . ? O5 Co Na O5 180.0 7_556 . . . ? Na Co Na O5 20(76) 7_556 . . . ? O1 Co Na O1 180.0 7_556 . . . ? O6 Co Na O1 -114.76(17) . . . . ? O6 Co Na O1 65.24(17) 7_556 . . . ? O5 Co Na O1 -51.11(18) 7_556 . . . ? O5 Co Na O1 128.89(18) . . . . ? Na Co Na O1 149(76) 7_556 . . . ? O1 Co O1 C1 134(100) 7_556 . . . ? O6 Co O1 C1 -145.2(4) . . . . ? O6 Co O1 C1 34.8(4) 7_556 . . . ? O5 Co O1 C1 -56.8(4) 7_556 . . . ? O5 Co O1 C1 123.2(4) . . . . ? Na Co O1 C1 158.5(4) . . . . ? Na Co O1 C1 -21.5(4) 7_556 . . . ? O1 Co O1 Na -24(100) 7_556 . . . ? O6 Co O1 Na 56.32(14) . . . . ? O6 Co O1 Na -123.68(14) 7_556 . . . ? O5 Co O1 Na 144.69(12) 7_556 . . . ? O5 Co O1 Na -35.31(12) . . . . ? Na Co O1 Na 180.0 7_556 . . . ? O3 Na O1 C1 -16.4(4) 2 . . . ? O4 Na O1 C1 117.8(4) 2_565 . . . ? O2 Na O1 C1 -135.3(6) 6 . . . ? O5 Na O1 C1 -124.2(4) . . . . ? Co Na O1 C1 -157.1(5) . . . . ? O3 Na O1 Co 140.69(13) 2 . . . ? O4 Na O1 Co -85.12(14) 2_565 . . . ? O2 Na O1 Co 21.8(7) 6 . . . ? O5 Na O1 Co 32.92(12) . . . . ? O1 Co O5 Na 35.50(13) . . . . ? O1 Co O5 Na -144.50(13) 7_556 . . . ? O6 Co O5 Na -55.23(13) . . . . ? O6 Co O5 Na 124.77(13) 7_556 . . . ? O5 Co O5 Na -151(82) 7_556 . . . ? Na Co O5 Na 180.0 7_556 . . . ? O3 Na O5 Co -123.94(14) 2 . . . ? O4 Na O5 Co 51.53(17) 2_565 . . . ? O2 Na O5 Co 147.46(13) 6 . . . ? O1 Na O5 Co -30.02(11) . . . . ? Na O2 C1 O1 111.4(5) 6_556 . . . ? Na O2 C1 C2 -66.6(6) 6_556 . . . ? Co O1 C1 O2 -16.2(7) . . . . ? Na O1 C1 O2 134.3(4) . . . . ? Co O1 C1 C2 161.8(3) . . . . ? Na O1 C1 C2 -47.7(6) . . . . ? O2 C1 C2 C7 148.8(5) . . . . ? O1 C1 C2 C7 -29.4(7) . . . . ? O2 C1 C2 C3 -28.0(8) . . . . ? O1 C1 C2 C3 153.8(5) . . . . ? C7 C2 C3 C4 -0.6(8) . . . . ? C1 C2 C3 C4 176.2(5) . . . . ? C2 C3 C4 C5 -2.7(8) . . . . ? C3 C4 C5 C6 3.7(8) . . . . ? C3 C4 C5 C8 -175.6(5) . . . . ? C4 C5 C6 C7 -1.6(8) . . . . ? C8 C5 C6 C7 177.6(4) . . . . ? C3 C2 C7 C6 2.6(8) . . . . ? C1 C2 C7 C6 -174.2(5) . . . . ? C5 C6 C7 C2 -1.5(8) . . . . ? C6 C5 C8 C9 144.9(5) . . . . ? C4 C5 C8 C9 -35.8(7) . . . . ? C6 C5 C8 C13 -33.2(7) . . . . ? C4 C5 C8 C13 146.0(5) . . . . ? C13 C8 C9 C10 3.3(7) . . . . ? C5 C8 C9 C10 -174.9(5) . . . . ? C8 C9 C10 C11 -3.1(8) . . . . ? C9 C10 C11 C12 0.1(8) . . . . ? C9 C10 C11 C14 -178.4(5) . . . . ? C10 C11 C12 C13 2.6(8) . . . . ? C14 C11 C12 C13 -178.8(5) . . . . ? C9 C8 C13 C12 -0.6(7) . . . . ? C5 C8 C13 C12 177.6(4) . . . . ? C11 C12 C13 C8 -2.4(8) . . . . ? Na O4 C14 O3 -56.2(11) 2_545 . . . ? Na O4 C14 C11 122.8(7) 2_545 . . . ? Na O3 C14 O4 -115.4(6) 2 . . . ? Na O3 C14 C11 65.6(8) 2 . . . ? C12 C11 C14 O4 176.6(5) . . . . ? C10 C11 C14 O4 -5.0(8) . . . . ? C12 C11 C14 O3 -4.3(8) . . . . ? C10 C11 C14 O3 174.1(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 O6 H4 O2 0.93 1.81 2.664(4) 150.9 7_556 O6 H3 O4 0.85 1.85 2.664(4) 160.5 2_565 O5 H1 O3 0.98 1.75 2.720(4) 172.0 3 O5 H2 O2 0.95 1.93 2.848(5) 160.2 7_546 _diffrn_measured_fraction_theta_max 0.453 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.453 _refine_diff_density_max 0.423 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.103 #=== END