data_s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Co N19 Na O' _chemical_formula_weight 596.42 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' 'N' 'N' 0.0061 0.0033 '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' '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' _symmetry_cell_setting 'Trigonal' _symmetry_space_group_name_H-M 'P-31c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 10.4089(15) _cell_length_b 10.4089(15) _cell_length_c 14.028(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1316.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1289 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.71 _exptl_crystal_description 'prism-shaped crystal' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8995 _exptl_absorpt_correction_T_max 0.9314 _exptl_absorpt_process_details 'SADABS' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5921 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.99 _reflns_number_total 793 _reflns_number_gt 644 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 793 _refine_ls_number_parameters 77 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.134 _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 Na1 Na 0.3333 0.6667 0.2500 0.0544(8) Uani 1 6 d S . . Co1 Co 0.6667 0.3333 0.2500 0.0383(4) Uani 1 6 d S . . N1 N 0.6400(3) 0.4923(3) 0.16777(18) 0.0514(7) Uani 1 1 d . . . N4 N 0.5166(3) 0.6234(3) 0.1606(2) 0.0596(8) Uani 1 1 d . . . C1 C 0.5423(4) 0.5273(4) 0.2056(2) 0.0530(9) Uani 1 1 d D A . N2 N 0.6786(13) 0.5713(15) 0.0961(7) 0.056(2) Uani 0.50 1 d PD A 1 N3 N 0.6081(10) 0.6473(9) 0.0906(6) 0.064(2) Uani 0.50 1 d PD A 1 C2 C 0.7172(18) 0.5592(19) 0.0746(10) 0.066(3) Uani 0.50 1 d PD A 2 H2A H 0.7839 0.5347 0.0477 0.079 Uiso 0.50 1 calc PR A 2 C3 C 0.6846(11) 0.6578(10) 0.0312(7) 0.084(3) Uani 0.50 1 d PD A 2 H3A H 0.7307 0.7013 -0.0261 0.101 Uiso 0.50 1 calc PR A 2 C4 C 0.5846(13) 0.6939(12) 0.0710(7) 0.072(3) Uani 0.50 1 d PD A 2 H4A H 0.5623 0.7603 0.0414 0.086 Uiso 0.50 1 calc 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 Na1 0.0420(10) 0.0420(10) 0.079(2) 0.000 0.000 0.0210(5) Co1 0.0395(4) 0.0395(4) 0.0360(6) 0.000 0.000 0.0197(2) N1 0.0559(16) 0.0519(15) 0.0483(16) 0.0040(12) 0.0015(12) 0.0285(13) N4 0.0670(19) 0.0622(17) 0.0580(17) 0.0111(14) 0.0105(15) 0.0386(15) C1 0.0528(19) 0.0497(18) 0.063(2) -0.0110(14) -0.0087(15) 0.0309(17) N2 0.066(6) 0.072(5) 0.045(5) 0.028(4) 0.022(4) 0.045(4) N3 0.083(5) 0.076(5) 0.055(5) 0.023(4) 0.020(4) 0.055(4) C2 0.076(9) 0.073(6) 0.048(6) 0.022(5) 0.025(5) 0.037(6) C3 0.107(7) 0.103(7) 0.046(5) 0.040(4) 0.029(4) 0.055(6) C4 0.093(7) 0.072(6) 0.056(5) 0.026(4) 0.013(4) 0.046(5) _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 Na1 N4 2.504(3) 2_665 ? Na1 N4 2.504(3) 3_565 ? Na1 N4 2.504(3) 6_565 ? Na1 N4 2.504(3) 5 ? Na1 N4 2.504(3) . ? Na1 N4 2.504(3) 4_665 ? Co1 N1 2.146(3) 3_665 ? Co1 N1 2.146(3) 2_655 ? Co1 N1 2.146(3) 6 ? Co1 N1 2.146(3) 5_655 ? Co1 N1 2.146(3) . ? Co1 N1 2.146(3) 4_665 ? N1 N2 1.232(10) . ? N1 C1 1.348(4) . ? N1 C2 1.510(12) . ? N4 N3 1.303(8) . ? N4 C1 1.319(4) . ? N4 C4 1.450(10) . ? C1 C1 1.441(7) 4_665 ? C1 N3 1.943(8) . ? N2 N3 1.323(12) . ? C2 C3 1.373(15) . ? C2 H2A 0.9300 . ? C3 C4 1.389(13) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? 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 N4 Na1 N4 97.11(9) 2_665 3_565 ? N4 Na1 N4 70.78(13) 2_665 6_565 ? N4 Na1 N4 162.10(14) 3_565 6_565 ? N4 Na1 N4 97.46(14) 2_665 5 ? N4 Na1 N4 70.78(13) 3_565 5 ? N4 Na1 N4 97.11(9) 6_565 5 ? N4 Na1 N4 97.11(9) 2_665 . ? N4 Na1 N4 97.11(9) 3_565 . ? N4 Na1 N4 97.46(14) 6_565 . ? N4 Na1 N4 162.10(14) 5 . ? N4 Na1 N4 162.10(14) 2_665 4_665 ? N4 Na1 N4 97.46(14) 3_565 4_665 ? N4 Na1 N4 97.11(9) 6_565 4_665 ? N4 Na1 N4 97.11(9) 5 4_665 ? N4 Na1 N4 70.78(13) . 4_665 ? N1 Co1 N1 93.82(10) 3_665 2_655 ? N1 Co1 N1 96.21(14) 3_665 6 ? N1 Co1 N1 77.51(14) 2_655 6 ? N1 Co1 N1 77.51(14) 3_665 5_655 ? N1 Co1 N1 167.13(14) 2_655 5_655 ? N1 Co1 N1 93.82(10) 6 5_655 ? N1 Co1 N1 93.82(10) 3_665 . ? N1 Co1 N1 93.82(10) 2_655 . ? N1 Co1 N1 167.13(14) 6 . ? N1 Co1 N1 96.21(14) 5_655 . ? N1 Co1 N1 167.13(14) 3_665 4_665 ? N1 Co1 N1 96.21(14) 2_655 4_665 ? N1 Co1 N1 93.82(10) 6 4_665 ? N1 Co1 N1 93.82(10) 5_655 4_665 ? N1 Co1 N1 77.51(14) . 4_665 ? N2 N1 C1 100.4(5) . . ? N2 N1 C2 20.8(7) . . ? C1 N1 C2 121.0(6) . . ? N2 N1 Co1 145.9(4) . . ? C1 N1 Co1 113.7(2) . . ? C2 N1 Co1 125.2(5) . . ? N3 N4 C1 95.7(4) . . ? N3 N4 C4 28.8(4) . . ? C1 N4 C4 124.5(5) . . ? N3 N4 Na1 153.3(4) . . ? C1 N4 Na1 111.0(2) . . ? C4 N4 Na1 124.5(5) . . ? N4 C1 N1 118.9(3) . . ? N4 C1 C1 123.59(19) . 4_665 ? N1 C1 C1 117.52(18) . 4_665 ? N4 C1 N3 41.8(3) . . ? N1 C1 N3 77.0(3) . . ? C1 C1 N3 165.4(3) 4_665 . ? N1 N2 N3 110.6(6) . . ? N4 N3 N2 114.5(7) . . ? N4 N3 C1 42.5(3) . . ? N2 N3 C1 72.0(5) . . ? C3 C2 N1 117.1(9) . . ? C3 C2 H2A 121.5 . . ? N1 C2 H2A 121.5 . . ? C2 C3 C4 121.5(8) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C3 C4 N4 117.0(8) . . ? C3 C4 H4A 121.5 . . ? N4 C4 H4A 121.5 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.188 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.046