# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1875 data_s #Crystal data for [C12N6H6]*2H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 N6 O2' _chemical_formula_weight 270.26 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 6.9260(14) _cell_length_b 9.242(2) _cell_length_c 18.158(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.04(3) _cell_angle_gamma 90.00 _cell_volume 1162.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8715 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.1338 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.33 _reflns_number_total 4374 _reflns_number_gt 2601 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Giacovazzo et al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0085(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -2(2) _refine_ls_number_reflns 4374 _refine_ls_number_parameters 424 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 0.786 _refine_ls_restrained_S_all 0.786 _refine_ls_shift/su_max 0.173 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.5201(6) 0.6830(5) 0.3404(2) 0.0230(10) Uani 1 1 d . . . N2 N -0.6627(6) 0.3986(5) 0.3444(2) 0.0251(11) Uani 1 1 d . . . N3 N -0.7381(5) 0.2528(4) 0.2160(3) 0.0247(12) Uani 1 1 d . . . N4 N -0.6582(6) 0.3897(5) 0.0790(2) 0.0256(11) Uani 1 1 d . . . N5 N -0.5413(6) 0.6739(5) 0.0751(2) 0.0226(11) Uani 1 1 d . . . N6 N -0.4654(6) 0.8224(4) 0.2077(3) 0.0229(10) Uani 1 1 d . . . N21 N -0.1592(6) 0.3896(5) 0.3350(2) 0.0236(10) Uani 1 1 d . . . N22 N -0.2366(5) 0.2528(4) 0.1985(3) 0.0220(11) Uani 1 1 d . . . N23 N -0.1625(6) 0.3988(5) 0.0691(2) 0.0251(11) Uani 1 1 d . . . N24 N -0.0202(6) 0.6836(5) 0.0737(2) 0.0220(10) Uani 1 1 d . . . N25 N 0.0335(6) 0.8223(4) 0.2054(3) 0.0232(10) Uani 1 1 d . . . N26 N -0.0427(6) 0.6743(4) 0.3388(3) 0.0225(11) Uani 1 1 d . . . C1 C -0.5628(7) 0.6105(5) 0.2772(3) 0.0207(12) Uani 1 1 d . . . C2 C -0.6321(7) 0.4670(5) 0.2799(3) 0.0195(13) Uani 1 1 d . . . C3 C -0.6679(7) 0.3909(5) 0.2113(3) 0.0195(11) Uani 1 1 d . . . C4 C -0.6336(7) 0.4598(5) 0.1442(3) 0.0203(13) Uani 1 1 d . . . C5 C -0.5675(7) 0.6092(5) 0.1415(3) 0.0193(12) Uani 1 1 d . . . C6 C -0.5317(7) 0.6822(5) 0.2072(4) 0.0179(11) Uani 1 1 d . . . C7 C -0.5481(7) 0.6146(6) 0.4032(3) 0.0243(12) Uani 1 1 d . . . C8 C -0.6210(8) 0.4719(6) 0.4058(3) 0.0243(14) Uani 1 1 d . . . C9 C -0.7624(7) 0.1871(6) 0.1515(3) 0.0246(13) Uani 1 1 d . . . C10 C -0.7229(7) 0.2543(6) 0.0841(3) 0.0250(14) Uani 1 1 d . . . C11 C -0.4819(7) 0.8094(6) 0.0775(3) 0.0248(13) Uani 1 1 d . . . C12 C -0.4408(7) 0.8840(6) 0.1428(3) 0.0241(13) Uani 1 1 d . . . C21 C -0.1322(7) 0.4596(6) 0.2701(3) 0.0187(12) Uani 1 1 d . . . C22 C -0.1699(7) 0.3906(5) 0.2029(3) 0.0186(10) Uani 1 1 d . . . C23 C -0.1319(7) 0.4669(5) 0.1346(3) 0.0196(13) Uani 1 1 d . . . C24 C -0.0634(7) 0.6105(5) 0.1361(3) 0.0196(12) Uani 1 1 d . . . C25 C -0.0312(7) 0.6821(5) 0.2063(3) 0.0172(11) Uani 1 1 d . . . C26 C -0.0682(7) 0.6098(5) 0.2721(3) 0.0198(12) Uani 1 1 d . . . C27 C -0.2221(8) 0.2540(6) 0.3301(3) 0.0279(14) Uani 1 1 d . . . C28 C -0.2611(7) 0.1873(6) 0.2620(3) 0.0232(13) Uani 1 1 d . . . C29 C -0.1205(8) 0.4730(6) 0.0084(3) 0.0243(14) Uani 1 1 d . . . C30 C -0.0481(7) 0.6129(6) 0.0109(3) 0.0259(13) Uani 1 1 d . . . C31 C 0.0579(7) 0.8823(6) 0.2717(3) 0.0227(12) Uani 1 1 d . . . C32 C 0.0183(7) 0.8098(6) 0.3372(3) 0.0255(13) Uani 1 1 d . . . O1 O -0.2620(6) 0.1095(4) 0.0217(2) 0.0354(10) Uani 1 1 d . . . O2 O 0.0875(6) 0.9658(5) 0.0266(2) 0.0367(11) Uani 1 1 d . . . O3 O -0.7610(6) 0.1098(4) 0.3927(2) 0.0353(10) Uani 1 1 d . . . O4 O -0.4128(6) 0.9648(4) 0.3873(2) 0.0355(10) Uani 1 1 d . . . H7 H -0.522(6) 0.653(5) 0.458(3) 0.031(4) Uiso 1 1 d . . . H8 H -0.621(7) 0.427(5) 0.455(3) 0.031(4) Uiso 1 1 d . . . H9 H -0.800(7) 0.070(5) 0.164(3) 0.031(4) Uiso 1 1 d . . . H10 H -0.729(7) 0.193(5) 0.045(3) 0.031(4) Uiso 1 1 d . . . H11 H -0.439(7) 0.852(5) 0.031(3) 0.031(4) Uiso 1 1 d . . . H12 H -0.376(7) 0.994(5) 0.136(3) 0.031(4) Uiso 1 1 d . . . H27 H -0.251(7) 0.201(5) 0.382(3) 0.031(4) Uiso 1 1 d . . . H28 H -0.315(7) 0.082(5) 0.262(3) 0.031(4) Uiso 1 1 d . . . H29 H -0.122(7) 0.414(5) -0.034(3) 0.031(4) Uiso 1 1 d . . . H30 H -0.023(6) 0.658(5) -0.033(3) 0.031(4) Uiso 1 1 d . . . H31 H 0.118(7) 0.995(5) 0.277(3) 0.031(4) Uiso 1 1 d . . . H32 H 0.039(7) 0.856(5) 0.388(3) 0.031(4) Uiso 1 1 d . . . H1W H -0.121(10) 1.059(7) 0.020(4) 0.084(8) Uiso 1 1 d . . . H2W H -0.263(10) 1.204(7) 0.051(4) 0.084(8) Uiso 1 1 d . . . H3W H 0.046(10) 0.874(8) 0.061(4) 0.084(8) Uiso 1 1 d . . . H4W H -0.875(11) 0.937(8) -0.013(4) 0.084(8) Uiso 1 1 d . . . H5W H -0.634(10) 0.062(7) 0.385(4) 0.084(8) Uiso 1 1 d . . . H6W H -0.713(10) 0.800(8) -0.120(4) 0.084(8) Uiso 1 1 d . . . H7W H -0.362(10) 0.059(8) -0.071(4) 0.084(8) Uiso 1 1 d . . . H8W H -0.494(10) 0.878(7) 0.364(4) 0.084(8) Uiso 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 N1 0.022(2) 0.027(3) 0.020(3) -0.002(2) -0.001(2) 0.0028(19) N2 0.022(2) 0.036(3) 0.017(2) 0.006(2) 0.0004(19) 0.002(2) N3 0.020(3) 0.027(3) 0.027(3) -0.004(2) 0.004(2) -0.002(2) N4 0.022(2) 0.028(3) 0.026(3) -0.003(2) 0.002(2) 0.001(2) N5 0.021(3) 0.030(3) 0.018(3) 0.001(2) 0.000(2) 0.000(2) N6 0.019(2) 0.027(2) 0.023(2) 0.003(2) 0.001(2) 0.0039(19) N21 0.027(2) 0.024(2) 0.020(3) 0.001(2) -0.001(2) -0.002(2) N22 0.019(2) 0.025(2) 0.022(3) 0.001(2) -0.008(2) -0.0024(19) N23 0.025(2) 0.033(3) 0.017(2) -0.003(2) 0.000(2) 0.004(2) N24 0.021(2) 0.028(3) 0.016(2) 0.001(2) -0.0013(19) 0.0046(19) N25 0.022(2) 0.028(2) 0.020(2) -0.001(2) 0.001(2) 0.0018(19) N26 0.025(3) 0.022(2) 0.021(3) 0.000(2) -0.002(2) 0.001(2) C1 0.013(3) 0.027(3) 0.022(3) -0.004(3) -0.003(2) 0.004(2) C2 0.015(3) 0.025(3) 0.019(3) 0.000(2) 0.003(2) 0.002(2) C3 0.016(2) 0.025(2) 0.018(3) -0.002(3) 0.002(2) 0.002(2) C4 0.015(3) 0.023(3) 0.023(3) -0.009(2) -0.001(2) 0.002(2) C5 0.016(3) 0.025(3) 0.017(3) 0.000(2) -0.001(2) 0.002(2) C6 0.014(2) 0.022(2) 0.017(3) 0.000(3) 0.002(2) 0.000(2) C7 0.026(3) 0.029(3) 0.018(3) -0.003(2) 0.006(2) -0.003(2) C8 0.025(3) 0.032(4) 0.016(3) -0.001(3) -0.002(2) 0.001(2) C9 0.026(3) 0.032(3) 0.016(3) -0.002(3) 0.002(2) 0.003(2) C10 0.026(3) 0.027(3) 0.022(3) -0.005(3) 0.003(3) -0.002(2) C11 0.021(3) 0.030(3) 0.023(3) 0.005(3) 0.003(2) 0.003(2) C12 0.021(3) 0.030(3) 0.021(3) 0.001(3) 0.000(2) 0.004(2) C21 0.012(3) 0.026(3) 0.018(3) 0.002(2) -0.001(2) -0.001(2) C22 0.013(2) 0.025(2) 0.017(3) 0.002(3) 0.000(2) 0.003(2) C23 0.020(3) 0.024(3) 0.015(3) -0.001(2) 0.001(2) 0.001(2) C24 0.015(3) 0.028(3) 0.016(3) 0.004(2) 0.000(2) 0.006(2) C25 0.015(2) 0.021(2) 0.016(3) -0.002(3) 0.001(2) -0.001(2) C26 0.017(3) 0.025(3) 0.018(3) 0.003(2) 0.003(2) 0.002(2) C27 0.030(3) 0.031(3) 0.023(3) 0.000(3) 0.002(3) -0.001(3) C28 0.029(3) 0.019(3) 0.022(3) 0.006(2) 0.003(2) 0.002(2) C29 0.023(3) 0.034(4) 0.016(3) 0.001(3) 0.005(2) 0.000(2) C30 0.025(3) 0.036(3) 0.017(3) 0.001(3) -0.001(2) 0.001(3) C31 0.024(3) 0.023(3) 0.021(3) -0.003(3) 0.000(2) -0.003(2) C32 0.024(3) 0.030(3) 0.023(3) -0.004(3) -0.007(2) 0.003(2) O1 0.045(3) 0.031(2) 0.030(3) -0.0012(19) -0.007(2) -0.0054(19) O2 0.044(3) 0.031(2) 0.034(3) -0.001(2) 0.006(2) -0.0023(19) O3 0.041(3) 0.032(2) 0.033(3) 0.000(2) 0.004(2) -0.0060(19) O4 0.042(3) 0.028(2) 0.036(3) 0.000(2) -0.008(2) -0.0078(19) _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 N1 C7 1.318(7) . ? N1 C1 1.361(6) . ? N2 C8 1.335(7) . ? N2 C2 1.347(6) . ? N3 C9 1.330(7) . ? N3 C3 1.369(6) . ? N4 C10 1.332(7) . ? N4 C4 1.361(6) . ? N5 C11 1.318(7) . ? N5 C5 1.358(6) . ? N6 C12 1.321(7) . ? N6 C6 1.375(5) . ? N21 C27 1.330(7) . ? N21 C21 1.359(6) . ? N22 C28 1.313(7) . ? N22 C22 1.357(5) . ? N23 C29 1.330(7) . ? N23 C23 1.362(6) . ? N24 C30 1.330(7) . ? N24 C24 1.352(6) . ? N25 C31 1.337(7) . ? N25 C25 1.371(5) . ? N26 C32 1.321(6) . ? N26 C26 1.362(6) . ? C1 C2 1.412(7) . ? C1 C6 1.450(7) . ? C2 C3 1.452(7) . ? C3 C4 1.394(7) . ? C4 C5 1.455(7) . ? C5 C6 1.393(7) . ? C7 C8 1.413(8) . ? C9 C10 1.400(8) . ? C11 C12 1.399(7) . ? C21 C22 1.400(7) . ? C21 C26 1.457(7) . ? C22 C23 1.452(7) . ? C23 C24 1.409(7) . ? C24 C25 1.453(7) . ? C25 C26 1.394(7) . ? C27 C28 1.408(8) . ? C29 C30 1.388(8) . ? C31 C32 1.392(7) . ? 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 C7 N1 C1 117.5(5) . . ? C8 N2 C2 117.0(5) . . ? C9 N3 C3 114.6(5) . . ? C10 N4 C4 115.4(5) . . ? C11 N5 C5 115.5(5) . . ? C12 N6 C6 116.3(5) . . ? C27 N21 C21 115.8(5) . . ? C28 N22 C22 115.1(5) . . ? C29 N23 C23 116.8(5) . . ? C30 N24 C24 116.2(5) . . ? C31 N25 C25 115.0(5) . . ? C32 N26 C26 115.8(5) . . ? N1 C1 C2 120.5(5) . . ? N1 C1 C6 118.8(5) . . ? C2 C1 C6 120.7(5) . . ? N2 C2 C1 121.6(5) . . ? N2 C2 C3 119.5(5) . . ? C1 C2 C3 118.8(5) . . ? N3 C3 C4 122.8(5) . . ? N3 C3 C2 117.3(5) . . ? C4 C3 C2 120.0(5) . . ? N4 C4 C3 121.4(5) . . ? N4 C4 C5 117.5(5) . . ? C3 C4 C5 121.1(5) . . ? N5 C5 C6 121.5(5) . . ? N5 C5 C4 119.4(5) . . ? C6 C5 C4 119.1(5) . . ? N6 C6 C5 121.5(5) . . ? N6 C6 C1 118.3(5) . . ? C5 C6 C1 120.2(4) . . ? N1 C7 C8 121.9(5) . . ? N2 C8 C7 121.5(5) . . ? N3 C9 C10 122.8(5) . . ? N4 C10 C9 122.9(5) . . ? N5 C11 C12 124.0(5) . . ? N6 C12 C11 121.2(5) . . ? N21 C21 C22 120.9(5) . . ? N21 C21 C26 118.3(5) . . ? C22 C21 C26 120.9(5) . . ? N22 C22 C21 122.8(5) . . ? N22 C22 C23 117.9(5) . . ? C21 C22 C23 119.2(5) . . ? N23 C23 C24 120.3(5) . . ? N23 C23 C22 119.5(5) . . ? C24 C23 C22 120.2(5) . . ? N24 C24 C23 121.9(5) . . ? N24 C24 C25 118.2(5) . . ? C23 C24 C25 119.8(4) . . ? N25 C25 C26 121.6(5) . . ? N25 C25 C24 118.0(5) . . ? C26 C25 C24 120.4(4) . . ? N26 C26 C25 122.0(5) . . ? N26 C26 C21 118.6(4) . . ? C25 C26 C21 119.4(5) . . ? N21 C27 C28 122.3(5) . . ? N22 C28 C27 123.0(5) . . ? N23 C29 C30 122.2(5) . . ? N24 C30 C29 122.5(5) . . ? N25 C31 C32 123.0(5) . . ? N26 C32 C31 122.6(5) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.280 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.063 #===END data_s2 #Crystal data for [Co(HAT)Cl2]4*25H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H78 Cl8 Co4 N24 O27' _chemical_formula_weight 1942.64 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y, -z+1/2' '-y+1/2, -x+1/2, -z' 'y, x, -z' 'y, -x+1/2, z+1/2' '-y+1/2, x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y, z-1/2' 'y-1/2, x-1/2, z' '-y, -x, z' '-y, x-1/2, -z-1/2' 'y-1/2, -x, -z-1/2' _cell_length_a 17.663(3) _cell_length_b 17.663(3) _cell_length_c 12.171(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3797.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1988 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32898 _diffrn_reflns_av_R_equivalents 0.0925 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.25 _reflns_number_total 2469 _reflns_number_gt 783 _reflns_threshold_expression >4sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 4sigma(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^)+(0.1420P)^2^+13.9602P] 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 SHELXL _refine_ls_extinction_coef 0.0000(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2469 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2417 _refine_ls_R_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.4082 _refine_ls_wR_factor_gt 0.2057 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 1.535 _refine_ls_shift/su_mean 0.132 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.7500 -0.03446(13) 0.2500 0.0867(10) Uani 1 2 d S . . Cl Cl 0.6601(2) -0.1243(2) 0.3191(3) 0.1187(15) Uani 1 1 d . . . N1 N 0.8318(5) 0.0556(5) 0.2212(6) 0.086(3) Uani 1 1 d . . . N2 N 0.8022(6) -0.0227(5) 0.4083(7) 0.083(3) Uani 1 1 d . . . N3 N 0.8903(6) -0.0023(6) 0.5987(6) 0.095(3) Uani 1 1 d . . . C1 C 0.8723(6) 0.0719(6) 0.3142(7) 0.083(3) Uani 1 1 d . . . C2 C 0.8588(7) 0.0290(7) 0.4107(8) 0.082(3) Uani 1 1 d . . . C3 C 0.9018(6) 0.0389(6) 0.5088(8) 0.086(3) Uani 1 1 d . . . C4 C 0.8481(7) 0.0964(7) 0.1324(8) 0.089(3) Uani 1 1 d . . . H4 H 0.8213 0.0874 0.0679 0.050 Uiso 1 1 calc . . . C5 C 0.7895(7) -0.0615(6) 0.5010(10) 0.084(3) Uani 1 1 d . . . H5 H 0.7500 -0.0963 0.5033 0.050 Uiso 1 1 calc . . . C6 C 0.8334(9) -0.0511(7) 0.5928(9) 0.099(4) Uani 1 1 d . . . H6 H 0.8226 -0.0800 0.6547 0.050 Uiso 1 1 calc . . . O1 O 0.7270(16) 0.0827(15) 0.651(2) 0.112(7) Uiso 0.50 1 d P . . O2 O 0.690(2) 0.084(2) 0.640(3) 0.089(11) Uiso 0.25 1 d P . . O3 O 0.7500 0.2500 0.1969(15) 0.122(6) Uiso 1 4 d S . . O4 O 0.7500 -0.2500 0.397(5) 0.19(3) Uiso 0.50 2 d SP . . O5 O 0.773(4) 0.160(4) 0.585(5) 0.172(19) Uiso 0.25 1 d P . . O6 O 0.730(3) 0.126(3) 0.624(4) 0.124(15) Uiso 0.25 1 d P . . O7 O 0.7001(19) -0.2346(18) 0.363(3) 0.098(9) Uiso 0.25 1 d P . . O8 O 0.4980(13) 0.0292(13) 0.6935(19) 0.079(8) Uiso 0.25 1 d P . . O9 O 0.7032(13) 0.2032(13) 0.031(3) 0.113(8) Uiso 0.50 2 d SP . . O10 O 0.730(3) -0.251(3) 0.432(4) 0.121(16) Uiso 0.25 1 d P . . O11 O 0.819(2) 0.181(2) 0.527(5) 0.065(14) Uiso 0.25 2 d SP . . O12 O 0.734(7) 0.100(6) 0.712(9) 0.16(5) Uiso 0.13 1 d P . . O13 O 0.571(3) 0.071(3) 0.677(5) 0.15(2) Uiso 0.25 2 d SP . . O14 O 1.017(5) 0.380(5) 0.591(8) 0.16(3) Uiso 0.13 1 d P . . O15 O 0.454(3) 0.046(3) 0.5000 0.17(2) Uiso 0.25 2 d SP . . O16 O 0.800(5) 0.200(5) 0.549(10) 0.19(5) Uiso 0.25 2 d SP . . 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 0.0999(17) 0.0983(17) 0.0619(13) 0.000 -0.0075(11) 0.000 Cl 0.118(3) 0.149(3) 0.089(2) 0.008(2) -0.0187(19) 0.001(2) N1 0.113(7) 0.091(6) 0.054(5) -0.001(4) -0.005(5) 0.006(5) N2 0.102(7) 0.084(6) 0.064(5) 0.002(5) -0.002(5) -0.001(6) N3 0.111(8) 0.116(8) 0.057(5) 0.017(5) -0.005(5) -0.006(7) C1 0.108(8) 0.091(7) 0.051(5) 0.001(5) -0.003(5) 0.001(6) C2 0.095(8) 0.092(8) 0.059(6) 0.000(5) -0.001(6) 0.002(7) C3 0.096(8) 0.099(8) 0.064(6) 0.006(6) -0.011(6) -0.004(6) C4 0.109(8) 0.106(8) 0.050(5) 0.001(5) -0.011(5) -0.002(6) C5 0.095(8) 0.085(8) 0.073(6) 0.007(6) -0.005(6) -0.009(6) C6 0.137(12) 0.089(9) 0.072(7) 0.018(6) -0.010(8) 0.003(8) _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 N2 2.145(9) . ? Co N2 2.145(9) 4_655 ? Co N1 2.177(10) 4_655 ? Co N1 2.177(10) . ? Co Cl 2.397(4) . ? Co Cl 2.397(4) 4_655 ? N1 C1 1.369(12) . ? N1 C4 1.331(12) . ? N2 C5 1.339(14) . ? N2 C2 1.355(14) . ? N3 C3 1.330(13) . ? N3 C6 1.326(16) . ? C1 C1 1.39(2) 14_665 ? C1 C2 1.419(14) . ? C2 C3 1.426(14) . ? C3 C3 1.48(2) 14_665 ? C4 C4 1.39(2) 14_665 ? C4 H4 0.9301 . ? C5 C6 1.372(17) . ? C5 H5 0.9294 . ? C6 H6 0.9306 . ? 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 N2 Co N2 168.9(5) . 4_655 ? N2 Co N1 94.0(3) . 4_655 ? N2 Co N1 77.8(3) 4_655 4_655 ? N2 Co N1 77.8(3) . . ? N2 Co N1 94.0(3) 4_655 . ? N1 Co N1 86.2(5) 4_655 . ? N2 Co Cl 91.9(3) . . ? N2 Co Cl 95.4(3) 4_655 . ? N1 Co Cl 89.3(3) 4_655 . ? N1 Co Cl 168.4(2) . . ? N2 Co Cl 95.4(3) . 4_655 ? N2 Co Cl 91.9(3) 4_655 4_655 ? N1 Co Cl 168.4(2) 4_655 4_655 ? N1 Co Cl 89.3(3) . 4_655 ? Cl Co Cl 97.1(2) . 4_655 ? C1 N1 C4 116.4(10) . . ? C1 N1 Co 111.6(7) . . ? C4 N1 Co 132.1(7) . . ? C5 N2 C2 116.7(9) . . ? C5 N2 Co 129.5(8) . . ? C2 N2 Co 113.7(7) . . ? C3 N3 C6 115.3(10) . . ? N1 C1 C1 121.2(6) . 14_665 ? N1 C1 C2 119.0(10) . . ? C1 C1 C2 119.8(6) 14_665 . ? N2 C2 C3 119.6(10) . . ? N2 C2 C1 117.8(10) . . ? C3 C2 C1 122.6(11) . . ? N3 C3 C2 122.7(10) . . ? N3 C3 C3 119.7(7) . 14_665 ? C2 C3 C3 117.6(7) . 14_665 ? N1 C4 C4 122.4(6) . 14_665 ? N1 C4 H4 118.8 . . ? C4 C4 H4 118.9 14_665 . ? N2 C5 C6 121.6(11) . . ? N2 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? N3 C6 C5 124.0(11) . . ? N3 C6 H6 118.1 . . ? C5 C6 H6 117.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.742 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.121