Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' #------------------------------------------------------------------ _audit_creation_date 2003-07-28 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; #------------------------------------------------------------------ _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Rabindranath Mukherjee' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Kanpur Kanpur Uttar Pradesh 208 016 INDIA ; _publ_contact_author_email RNM@IITK.AC.IN _publ_contact_author_fax '+91 (512) 2597437' _publ_contact_author_phone '+91 (512) 2597437' # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and properties of FeIII and CoIII complexes: structures of [(L2)FeIII(N3)3], [(L2)2FeIII2(mu-O)(mu-O2CMe)2][ClO4]2.2H2O and [(L2)2CoIII2(mu-OH)2(mu-O2CMe)][ClO4]3.MeCN [L2 = methyl[2- (2-pyridyl)ethyl](2-pyridylmethyl)amine] ; loop_ _publ_author_name _publ_author_address 'Jhumpa Mukherjee' ; Department of Chemistry Indian Institute of Technology Kanpur 208016 INDIA ; V.Balamurugan ; Department of Chemistry Indian Institute of Technology Kanpur 208016 INDIA ; 'Rajeev Gupta' ; Department of Chemistry Indian Institute of Technology Kanpur 208016 INDIA ; 'Rabindranath Mukherjee' ; Department of Chemistry Indian Institute of Technology Kanpur 208016 INDIA ; #================================================================= data_ironbala _database_code_CSD 209228 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 N12 Fe' _chemical_formula_sum 'C14 H17 Fe N12' _chemical_formula_weight 409.25 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pc2(1)n _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y, z+1/2' '-x, y+1/2, -z' _cell_length_a 8.526(5) _cell_length_b 14.119(5) _cell_length_c 15.250(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1835.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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_method 2\q/\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 1687 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1687 _reflns_number_gt 1130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_cell_refinement 'XSCANS (Siemens, 1994)' _computing_data_reduction 'XSCANS (Siemens, 1994)' _computing_structure_solution 'SIR92 (Altomare, et. al. 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0866P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(8) _refine_ls_number_reflns 1687 _refine_ls_number_parameters 244 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.005 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 C7 C 0.7278(12) 0.3590(8) 0.2848(7) 0.067(3) Uani 1 1 d . . . H7B H 0.6744 0.3407 0.3383 0.081 Uiso 1 1 calc R . . H7A H 0.6550 0.3527 0.2362 0.081 Uiso 1 1 calc R . . N12 N 1.4043(19) 0.4663(17) 0.261(2) 0.226(18) Uani 1 1 d . . . N8 N 1.281(2) 0.2045(13) 0.2693(11) 0.096(6) Uani 1 1 d . . . N7 N 1.165(2) 0.2173(11) 0.2993(12) 0.078(5) Uani 1 1 d . . . N9 N 1.393(2) 0.203(2) 0.221(2) 0.208(14) Uani 1 1 d . . . Fe Fe 1.06302(11) 0.3208(3) 0.36544(6) 0.0444(4) Uani 1 1 d . . . N3 N 0.9137(15) 0.2162(8) 0.4329(10) 0.043(4) Uani 1 1 d . . . C1 C 0.9280(17) 0.4468(12) 0.5202(9) 0.053(5) Uani 1 1 d . . . H1 H 0.9996 0.4140 0.5547 0.063 Uiso 1 1 calc R . . N5 N 1.3493(9) 0.3232(15) 0.4681(4) 0.0653(19) Uani 1 1 d . . . N6 N 1.4801(11) 0.315(3) 0.4732(6) 0.155(7) Uani 1 1 d . . . N4 N 1.2125(8) 0.3211(18) 0.4645(5) 0.078(3) Uani 1 1 d . . . C14 C 0.9328(17) 0.1962(10) 0.5153(13) 0.059(6) Uani 1 1 d . . . H14 H 1.0091 0.2306 0.5451 0.071 Uiso 1 1 calc R . . N1 N 0.9147(15) 0.4276(9) 0.4319(10) 0.048(4) Uani 1 1 d . . . N11 N 1.2884(14) 0.4392(8) 0.2689(13) 0.079(6) Uani 1 1 d . . . C5 C 0.8107(19) 0.4793(12) 0.3890(14) 0.062(5) Uani 1 1 d . . . C10 C 0.8049(17) 0.1685(11) 0.3848(12) 0.050(5) Uani 1 1 d . . . C2 C 0.834(2) 0.5149(13) 0.5560(13) 0.087(8) Uani 1 1 d . . . H2 H 0.8442 0.5264 0.6158 0.105 Uiso 1 1 calc R . . N10 N 1.1633(19) 0.4294(9) 0.2974(12) 0.071(5) Uani 1 1 d . . . C13 C 0.850(2) 0.1275(11) 0.5647(13) 0.067(5) Uani 1 1 d . . . H13 H 0.8686 0.1159 0.6238 0.080 Uiso 1 1 calc R . . C8 C 0.9210(10) 0.330(2) 0.1766(5) 0.075(3) Uani 1 1 d . . . H8C H 1.0215 0.3021 0.1647 0.113 Uiso 1 1 calc R . . H8A H 0.9294 0.3976 0.1739 0.113 Uiso 1 1 calc R . . H8B H 0.8465 0.3085 0.1337 0.113 Uiso 1 1 calc R . . C4 C 0.715(2) 0.5476(13) 0.4260(18) 0.084(7) Uani 1 1 d . . . H4 H 0.6422 0.5801 0.3923 0.101 Uiso 1 1 calc R . . C11 C 0.715(2) 0.0993(13) 0.425(2) 0.096(9) Uani 1 1 d . . . H11 H 0.6395 0.0658 0.3940 0.115 Uiso 1 1 calc R . . C9 C 0.811(3) 0.2008(10) 0.2886(16) 0.100(8) Uani 1 1 d D . . H9B H 0.8805 0.1580 0.2572 0.119 Uiso 1 1 calc R . . H9A H 0.7074 0.1934 0.2638 0.119 Uiso 1 1 calc R . . C12 C 0.741(3) 0.0804(14) 0.5169(19) 0.123(12) Uani 1 1 d . . . H12 H 0.6812 0.0341 0.5443 0.148 Uiso 1 1 calc R . . C6 C 0.787(2) 0.4615(10) 0.2916(13) 0.072(5) Uani 1 1 d . . . H6B H 0.8844 0.4691 0.2599 0.086 Uiso 1 1 calc R . . H6A H 0.7099 0.5051 0.2677 0.086 Uiso 1 1 calc R . . N2 N 0.8646(9) 0.2995(6) 0.2706(4) 0.057(3) Uani 1 1 d D . . C3 C 0.731(2) 0.5657(11) 0.5122(16) 0.076(6) Uani 1 1 d . . . H3 H 0.6721 0.6123 0.5398 0.091 Uiso 1 1 calc 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 C7 0.052(5) 0.091(9) 0.059(6) -0.011(5) -0.014(5) 0.008(5) N12 0.058(9) 0.17(2) 0.45(5) 0.21(3) 0.073(16) 0.015(10) N8 0.083(12) 0.140(14) 0.066(10) -0.048(10) 0.019(9) -0.022(10) N7 0.073(11) 0.089(11) 0.073(12) 0.011(9) 0.025(10) 0.003(9) N9 0.132(15) 0.25(3) 0.24(2) -0.18(2) 0.128(16) -0.099(16) Fe 0.0403(5) 0.0517(6) 0.0413(5) -0.0011(15) 0.0043(5) -0.0049(12) N3 0.051(9) 0.040(7) 0.037(9) 0.005(7) 0.001(7) 0.002(6) C1 0.063(11) 0.077(11) 0.019(6) -0.002(7) 0.020(6) -0.004(8) N5 0.056(4) 0.089(5) 0.051(4) 0.009(11) -0.004(3) 0.014(12) N6 0.055(5) 0.34(2) 0.074(6) -0.01(2) -0.015(5) 0.076(16) N4 0.045(4) 0.123(7) 0.066(5) 0.026(13) -0.003(3) 0.016(11) C14 0.056(11) 0.027(7) 0.094(14) -0.001(8) 0.002(9) 0.014(6) N1 0.048(9) 0.054(8) 0.042(10) 0.003(8) 0.006(7) -0.005(6) N11 0.040(8) 0.051(7) 0.147(15) 0.056(9) 0.012(9) -0.011(6) C5 0.057(11) 0.048(10) 0.080(13) 0.012(9) -0.027(8) 0.005(8) C10 0.045(10) 0.050(9) 0.055(10) -0.014(8) 0.019(7) 0.015(7) C2 0.106(16) 0.077(12) 0.079(13) -0.029(11) 0.069(13) -0.045(12) N10 0.079(11) 0.045(7) 0.089(13) 0.019(7) 0.028(10) -0.020(7) C13 0.090(12) 0.041(8) 0.070(11) 0.002(8) 0.012(9) -0.008(9) C8 0.066(5) 0.126(10) 0.034(4) -0.009(12) -0.003(4) 0.006(12) C4 0.066(14) 0.055(11) 0.13(2) 0.010(12) -0.014(13) -0.028(9) C11 0.051(12) 0.063(12) 0.17(3) -0.045(14) 0.021(13) -0.026(8) C9 0.131(16) 0.064(11) 0.104(17) -0.041(10) -0.048(13) 0.028(10) C12 0.16(2) 0.053(11) 0.16(2) 0.031(14) 0.118(19) 0.025(14) C6 0.114(13) 0.042(7) 0.060(10) 0.014(6) -0.040(9) -0.008(7) N2 0.057(4) 0.080(10) 0.034(4) -0.007(4) 0.006(3) 0.005(5) C3 0.051(9) 0.039(8) 0.137(18) 0.004(10) 0.013(10) 0.015(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 C7 N2 1.454(12) . ? C7 C6 1.535(19) . ? N12 N11 1.068(18) . ? N8 N7 1.10(2) . ? N8 N9 1.21(2) . ? N7 Fe 1.978(17) . ? Fe N4 1.977(7) . ? Fe N10 2.040(13) . ? Fe N3 2.204(13) . ? Fe N1 2.214(14) . ? Fe N2 2.246(8) . ? N3 C14 1.30(2) . ? N3 C10 1.36(2) . ? C1 C2 1.36(3) . ? C1 N1 1.38(2) . ? N5 N6 1.124(11) . ? N5 N4 1.168(9) . ? C14 C13 1.42(2) . ? N1 C5 1.322(19) . ? N11 N10 1.160(18) . ? C5 C4 1.38(3) . ? C5 C6 1.52(3) . ? C10 C11 1.39(3) . ? C10 C9 1.54(3) . ? C2 C3 1.32(3) . ? C13 C12 1.35(3) . ? C8 N2 1.572(14) . ? C4 C3 1.35(3) . ? C11 C12 1.44(3) . ? C9 N2 1.490(15) . ? 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 C7 C6 107.0(10) . . ? N7 N8 N9 165(3) . . ? N8 N7 Fe 136.7(16) . . ? N7 Fe N4 96.2(8) . . ? N7 Fe N10 96.4(3) . . ? N4 Fe N10 96.7(8) . . ? N7 Fe N3 89.9(6) . . ? N4 Fe N3 91.0(6) . . ? N10 Fe N3 169.5(6) . . ? N7 Fe N1 171.3(6) . . ? N4 Fe N1 91.0(6) . . ? N10 Fe N1 87.7(6) . . ? N3 Fe N1 85.01(19) . . ? N7 Fe N2 84.5(6) . . ? N4 Fe N2 168.0(6) . . ? N10 Fe N2 95.1(6) . . ? N3 Fe N2 77.0(4) . . ? N1 Fe N2 87.5(4) . . ? C14 N3 C10 120.0(14) . . ? C14 N3 Fe 121.7(11) . . ? C10 N3 Fe 118.3(12) . . ? C2 C1 N1 118.8(17) . . ? N6 N5 N4 173(3) . . ? N5 N4 Fe 132.8(6) . . ? N3 C14 C13 127.0(17) . . ? C5 N1 C1 115.5(15) . . ? C5 N1 Fe 122.2(13) . . ? C1 N1 Fe 122.3(11) . . ? N12 N11 N10 160(3) . . ? N1 C5 C4 125(2) . . ? N1 C5 C6 118.8(16) . . ? C4 C5 C6 115.8(17) . . ? N3 C10 C11 119.0(18) . . ? N3 C10 C9 110.1(15) . . ? C11 C10 C9 130.8(18) . . ? C3 C2 C1 124.9(18) . . ? N11 N10 Fe 131.7(12) . . ? C12 C13 C14 113.0(19) . . ? C3 C4 C5 118.2(19) . . ? C10 C11 C12 118.4(19) . . ? N2 C9 C10 117.6(15) . . ? C13 C12 C11 122.6(17) . . ? C5 C6 C7 105.5(13) . . ? C7 N2 C9 105.6(10) . . ? C7 N2 C8 102.9(10) . . ? C9 N2 C8 121.1(15) . . ? C7 N2 Fe 115.6(6) . . ? C9 N2 Fe 103.7(9) . . ? C8 N2 Fe 108.7(6) . . ? C2 C3 C4 117.3(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.390 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.073 #=END data_melfe1 _database_code_CSD 209229 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H40 N6 FE O5, 2[Cl O4], 2[H2 O]' _chemical_formula_sum 'C32 H44 Cl2 Fe2 N6 O15' _chemical_formula_weight 935.33 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)nb _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y+1/2, -z+1/2' 'x+1/2, -y, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.453(6) _cell_length_b 17.69(2) _cell_length_c 18.692(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4449(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Brownish-orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'CAD4 mach' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 90 _diffrn_standards_interval_time 'one hour' _diffrn_standards_decay_% ? _diffrn_reflns_number 11418 _diffrn_reflns_av_R_equivalents 0.2699 _diffrn_reflns_av_sigmaI/netI 0.1771 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 22.55 _reflns_number_total 2969 _reflns_number_gt 1237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR92 (Altomare, et. al. 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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. The asymmetric unit of the structure contains one complex dication, two ClO~4~^-^ anions and two molecules of water. Geometric and anisotropic displacement parameter restraints were applied in the least-squares refinement procedure. The distances between the following pairs of atoms C5-C6 C6 N2 C8-C9 C19-C20 C20-C21 C21-N5 N5-C23 C23-C24 were restrained using the DFIX command in SHELXL-97. During the anistropic refinement of oxygens, except solvent water oxygens, the anisotropic displacement parameters (Uij) of all oxygen atoms were restrained by means of the EADP restraint command. The pyridine ring carbons and nitrogens are also anisotropically refined and restrained using EADP command All H atoms were placed in calculated positions and refined using a riding model,except that H atoms of the solvent water molecules were not located. ; _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^)+(0.1725P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(16) _refine_ls_number_reflns 2969 _refine_ls_number_parameters 216 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.2369 _refine_ls_R_factor_gt 0.1010 _refine_ls_wR_factor_ref 0.3235 _refine_ls_wR_factor_gt 0.2328 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.2330(3) 0.1869(3) 0.2355(3) 0.0376(17) Uani 1 1 d . . . Fe2 Fe -0.0008(2) 0.1878(3) 0.2347(3) 0.0379(17) Uani 1 1 d . . . Cl1 Cl -0.1137(12) 0.1450(4) -0.0679(4) 0.062(2) Uani 1 1 d . . . Cl2 Cl -0.1153(11) -0.0239(4) 0.5907(3) 0.0558(17) Uani 1 1 d . . . O1 O -0.117(3) 0.1828(9) 0.1881(7) 0.050(2) Uani 1 1 d . . . O2 O -0.1979(19) 0.2828(14) 0.2926(12) 0.050(2) Uani 1 1 d . . . O3 O -0.0342(19) 0.2718(14) 0.3023(12) 0.050(2) Uani 1 1 d . . . O4 O -0.1993(18) 0.1034(13) 0.3051(12) 0.050(2) Uani 1 1 d . . . O5 O -0.0319(18) 0.1171(12) 0.3156(12) 0.050(2) Uani 1 1 d . . . O6 O -0.193(3) 0.176(2) -0.0317(19) 0.132(5) Uani 1 1 d . . . O7 O -0.117(4) 0.0653(16) -0.0459(14) 0.132(5) Uani 1 1 d . . . O8 O -0.113(4) 0.1366(15) -0.1395(15) 0.132(5) Uani 1 1 d . . . O9 O -0.012(3) 0.172(2) -0.0498(19) 0.132(5) Uani 1 1 d . . . O10 O -0.196(2) -0.0098(17) 0.5482(16) 0.090(4) Uani 1 1 d . . . O11 O -0.116(3) 0.0124(12) 0.6587(10) 0.090(4) Uani 1 1 d . . . O12 O -0.015(2) -0.0275(17) 0.5611(15) 0.090(4) Uani 1 1 d . . . O13 O -0.131(2) -0.1054(14) 0.6063(12) 0.090(4) Uani 1 1 d . . . N1 N -0.3046(15) 0.0989(10) 0.1756(11) 0.041(2) Uani 1 1 d G . . C1 C -0.2572(13) 0.0789(11) 0.1123(12) 0.054(5) Uani 1 1 d G . . H1 H -0.2060 0.1087 0.0945 0.064 Uiso 1 1 calc R . . C2 C -0.2863(16) 0.0142(12) 0.0756(9) 0.054(5) Uani 1 1 d G . . H2 H -0.2546 0.0008 0.0333 0.064 Uiso 1 1 calc R . . C3 C -0.3629(16) -0.0304(10) 0.1023(11) 0.054(5) Uani 1 1 d G . . H3 H -0.3824 -0.0737 0.0777 0.064 Uiso 1 1 calc R . . C4 C -0.4103(14) -0.0104(11) 0.1656(11) 0.054(5) Uani 1 1 d G . . H4 H -0.4615 -0.0403 0.1834 0.064 Uiso 1 1 calc R . . C5 C -0.3812(15) 0.0543(12) 0.2022(10) 0.054(5) Uani 1 1 d GD . . N3 N -0.3000(16) 0.2706(11) 0.1629(11) 0.041(2) Uani 1 1 d G . . C10 C -0.3752(16) 0.3216(13) 0.1794(9) 0.056(5) Uani 1 1 d G . . C11 C -0.3956(16) 0.3813(12) 0.1334(11) 0.056(5) Uani 1 1 d G . . H11 H -0.4459 0.4155 0.1445 0.067 Uiso 1 1 calc R . . C12 C -0.3410(18) 0.3900(12) 0.0708(10) 0.056(5) Uani 1 1 d G . . H12 H -0.3547 0.4300 0.0400 0.067 Uiso 1 1 calc R . . C13 C -0.2659(16) 0.3390(14) 0.0543(9) 0.056(5) Uani 1 1 d G . . H13 H -0.2293 0.3448 0.0124 0.067 Uiso 1 1 calc R . . C14 C -0.2454(15) 0.2793(12) 0.1003(11) 0.056(5) Uani 1 1 d G . . H14 H -0.1951 0.2452 0.0892 0.067 Uiso 1 1 calc R . . N4 N 0.0616(16) 0.2679(11) 0.1623(12) 0.041(2) Uani 1 1 d G . . C15 C 0.0193(15) 0.2822(12) 0.0957(12) 0.062(6) Uani 1 1 d G . . H15 H -0.0319 0.2517 0.0790 0.074 Uiso 1 1 calc R . . C16 C 0.0537(18) 0.3420(13) 0.0543(10) 0.062(6) Uani 1 1 d G . . H16 H 0.0254 0.3515 0.0098 0.074 Uiso 1 1 calc R . . C17 C 0.1303(18) 0.3875(11) 0.0794(13) 0.062(6) Uani 1 1 d G . . H17 H 0.1533 0.4275 0.0517 0.074 Uiso 1 1 calc R . . C18 C 0.1726(17) 0.3733(12) 0.1459(14) 0.062(6) Uani 1 1 d G . . H18 H 0.2238 0.4038 0.1627 0.074 Uiso 1 1 calc R . . C19 C 0.1382(18) 0.3135(13) 0.1874(10) 0.062(6) Uani 1 1 d GD . . N6 N 0.0623(14) 0.0986(10) 0.1757(12) 0.041(2) Uani 1 1 d G . . C24 C 0.1440(16) 0.0675(12) 0.2104(10) 0.061(5) Uani 1 1 d GD . . C25 C 0.1935(15) 0.0063(12) 0.1805(13) 0.061(5) Uani 1 1 d G . . H25 H 0.2482 -0.0145 0.2037 0.073 Uiso 1 1 calc R . . C26 C 0.1614(16) -0.0239(11) 0.1158(13) 0.061(5) Uani 1 1 d G . . H26 H 0.1945 -0.0649 0.0958 0.073 Uiso 1 1 calc R . . C27 C 0.0797(17) 0.0072(13) 0.0811(10) 0.061(5) Uani 1 1 d G . . H27 H 0.0581 -0.0129 0.0379 0.073 Uiso 1 1 calc R . . C28 C 0.0301(14) 0.0685(12) 0.1111(12) 0.061(5) Uani 1 1 d G . . H28 H -0.0246 0.0893 0.0879 0.073 Uiso 1 1 calc R . . C29 C -0.117(4) 0.3057(13) 0.3095(11) 0.042(5) Uiso 1 1 d . . . C30 C -0.117(5) 0.3844(18) 0.3424(18) 0.101(10) Uiso 1 1 d . . . H30A H -0.1838 0.4040 0.3430 0.152 Uiso 1 1 calc R . . H30B H -0.0756 0.4172 0.3146 0.152 Uiso 1 1 calc R . . H30C H -0.0923 0.3817 0.3905 0.152 Uiso 1 1 calc R . . C31 C -0.100(2) 0.0832(13) 0.3281(12) 0.040(7) Uiso 1 1 d . . . C32 C -0.103(4) 0.009(2) 0.3697(18) 0.107(13) Uiso 1 1 d . . . H32A H -0.1694 -0.0106 0.3695 0.160 Uiso 1 1 calc R . . H32B H -0.0821 0.0178 0.4181 0.160 Uiso 1 1 calc R . . H32C H -0.0589 -0.0268 0.3476 0.160 Uiso 1 1 calc R . . O1W O -0.060(3) 0.3566(18) 0.5558(13) 0.17(2) Uani 1 1 d . . . O2W O -0.193(3) 0.268(3) 0.5213(16) 0.23(3) Uani 1 1 d . . . C20 C 0.177(2) 0.3020(15) 0.2655(12) 0.061(9) Uiso 1 1 d D . . H20A H 0.2247 0.3407 0.2780 0.073 Uiso 1 1 calc R . . H20B H 0.1221 0.3039 0.2993 0.073 Uiso 1 1 calc R . . C6 C -0.404(3) 0.0989(16) 0.2741(14) 0.070 Uiso 1 1 d D . . H6A H -0.3714 0.0709 0.3120 0.084 Uiso 1 1 calc R . . H6B H -0.4749 0.0936 0.2823 0.084 Uiso 1 1 calc R . . N5 N 0.143(2) 0.1648(13) 0.2835(18) 0.074(5) Uiso 1 1 d D . . C23 C 0.2049(19) 0.0881(14) 0.2757(14) 0.050 Uiso 1 1 d D . . H23A H 0.2748 0.0960 0.2656 0.061 Uiso 1 1 calc R . . H23B H 0.1962 0.0535 0.3155 0.061 Uiso 1 1 calc R . . C21 C 0.225(2) 0.2233(14) 0.2655(19) 0.067 Uiso 1 1 d D . . H21A H 0.2780 0.2212 0.3010 0.080 Uiso 1 1 calc R . . H21B H 0.2541 0.2126 0.2190 0.080 Uiso 1 1 calc R . . C9 C -0.437(3) 0.2909(15) 0.2429(18) 0.061 Uiso 1 1 d D . . H9A H -0.4960 0.3217 0.2469 0.073 Uiso 1 1 calc R . . H9B H -0.3980 0.2990 0.2861 0.073 Uiso 1 1 calc R . . C22 C 0.145(3) 0.215(2) 0.361(2) 0.085(13) Uiso 1 1 d . . . H22A H 0.0957 0.1955 0.3935 0.128 Uiso 1 1 calc R . . H22B H 0.1306 0.2673 0.3513 0.128 Uiso 1 1 calc R . . H22C H 0.2095 0.2112 0.3828 0.128 Uiso 1 1 calc R . . C7 C -0.378(2) 0.1831(18) 0.3695(16) 0.046(8) Uiso 1 1 d . . . H7A H -0.3635 0.2318 0.3894 0.070 Uiso 1 1 calc R . . H7B H -0.3288 0.1474 0.3845 0.070 Uiso 1 1 calc R . . H7C H -0.4425 0.1668 0.3856 0.070 Uiso 1 1 calc R . . N2 N -0.378(2) 0.1884(14) 0.2885(17) 0.074(5) Uiso 1 1 d D . . C8 C -0.471(2) 0.2026(15) 0.2422(18) 0.065 Uiso 1 1 d D . . H8A H -0.5338 0.1929 0.2664 0.078 Uiso 1 1 calc R . . H8B H -0.4694 0.1789 0.1954 0.078 Uiso 1 1 calc 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 Fe1 0.028(3) 0.054(4) 0.031(3) -0.002(3) -0.002(3) -0.002(3) Fe2 0.026(3) 0.046(4) 0.042(4) -0.007(3) -0.012(3) 0.007(3) Cl1 0.061(5) 0.077(5) 0.049(4) -0.001(3) 0.016(8) -0.013(9) Cl2 0.044(4) 0.064(4) 0.059(4) -0.008(3) -0.014(8) -0.001(8) O1 0.050(4) 0.059(5) 0.041(4) -0.002(4) 0.005(7) 0.005(8) O2 0.050(4) 0.059(5) 0.041(4) -0.002(4) 0.005(7) 0.005(8) O3 0.050(4) 0.059(5) 0.041(4) -0.002(4) 0.005(7) 0.005(8) O4 0.050(4) 0.059(5) 0.041(4) -0.002(4) 0.005(7) 0.005(8) O5 0.050(4) 0.059(5) 0.041(4) -0.002(4) 0.005(7) 0.005(8) O6 0.123(12) 0.148(12) 0.123(12) 0.016(10) 0.069(13) 0.017(16) O7 0.123(12) 0.148(12) 0.123(12) 0.016(10) 0.069(13) 0.017(16) O8 0.123(12) 0.148(12) 0.123(12) 0.016(10) 0.069(13) 0.017(16) O9 0.123(12) 0.148(12) 0.123(12) 0.016(10) 0.069(13) 0.017(16) O10 0.072(8) 0.112(10) 0.087(8) -0.010(7) -0.007(10) 0.003(11) O11 0.072(8) 0.112(10) 0.087(8) -0.010(7) -0.007(10) 0.003(11) O12 0.072(8) 0.112(10) 0.087(8) -0.010(7) -0.007(10) 0.003(11) O13 0.072(8) 0.112(10) 0.087(8) -0.010(7) -0.007(10) 0.003(11) N1 0.030(5) 0.039(5) 0.054(5) 0.007(4) 0.004(11) -0.006(10) C1 0.051(10) 0.049(10) 0.060(11) 0.000(8) -0.019(8) -0.004(8) C2 0.051(10) 0.049(10) 0.060(11) 0.000(8) -0.019(8) -0.004(8) C3 0.051(10) 0.049(10) 0.060(11) 0.000(8) -0.019(8) -0.004(8) C4 0.051(10) 0.049(10) 0.060(11) 0.000(8) -0.019(8) -0.004(8) C5 0.051(10) 0.049(10) 0.060(11) 0.000(8) -0.019(8) -0.004(8) N3 0.030(5) 0.039(5) 0.054(5) 0.007(4) 0.004(11) -0.006(10) C10 0.049(10) 0.086(15) 0.031(9) 0.004(8) -0.008(8) 0.002(9) C11 0.049(10) 0.086(15) 0.031(9) 0.004(8) -0.008(8) 0.002(9) C12 0.049(10) 0.086(15) 0.031(9) 0.004(8) -0.008(8) 0.002(9) C13 0.049(10) 0.086(15) 0.031(9) 0.004(8) -0.008(8) 0.002(9) C14 0.049(10) 0.086(15) 0.031(9) 0.004(8) -0.008(8) 0.002(9) N4 0.030(5) 0.039(5) 0.054(5) 0.007(4) 0.004(11) -0.006(10) C15 0.057(12) 0.038(10) 0.090(15) 0.006(9) 0.009(10) 0.002(8) C16 0.057(12) 0.038(10) 0.090(15) 0.006(9) 0.009(10) 0.002(8) C17 0.057(12) 0.038(10) 0.090(15) 0.006(9) 0.009(10) 0.002(8) C18 0.057(12) 0.038(10) 0.090(15) 0.006(9) 0.009(10) 0.002(8) C19 0.057(12) 0.038(10) 0.090(15) 0.006(9) 0.009(10) 0.002(8) N6 0.030(5) 0.039(5) 0.054(5) 0.007(4) 0.004(11) -0.006(10) C24 0.062(11) 0.050(11) 0.070(12) 0.003(9) 0.016(9) 0.012(8) C25 0.062(11) 0.050(11) 0.070(12) 0.003(9) 0.016(9) 0.012(8) C26 0.062(11) 0.050(11) 0.070(12) 0.003(9) 0.016(9) 0.012(8) C27 0.062(11) 0.050(11) 0.070(12) 0.003(9) 0.016(9) 0.012(8) C28 0.062(11) 0.050(11) 0.070(12) 0.003(9) 0.016(9) 0.012(8) O1W 0.31(6) 0.15(3) 0.054(15) 0.063(17) -0.06(2) -0.17(3) O2W 0.21(4) 0.40(6) 0.07(2) 0.11(3) -0.08(2) -0.26(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 Fe1 O1 1.79(3) . ? Fe1 O4 2.02(2) . ? Fe1 O2 2.06(3) . ? Fe1 N1 2.146(15) . ? Fe1 N2 2.19(3) . ? Fe1 N3 2.202(16) . ? Fe2 O1 1.79(4) . ? Fe2 O3 2.00(3) . ? Fe2 O5 2.01(2) . ? Fe2 N6 2.103(15) . ? Fe2 N4 2.132(16) . ? Fe2 N5 2.17(3) . ? Cl1 O8 1.35(3) . ? Cl1 O6 1.37(3) . ? Cl1 O7 1.47(3) . ? Cl1 O9 1.49(4) . ? Cl2 O10 1.37(3) . ? Cl2 O11 1.425(19) . ? Cl2 O12 1.46(3) . ? Cl2 O13 1.49(2) . ? O2 C29 1.20(5) . ? O3 C29 1.28(5) . ? O4 C31 1.45(4) . ? O5 C31 1.12(3) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.589(18) . ? N3 C10 1.3900 . ? N3 C14 1.3900 . ? C10 C11 1.3900 . ? C10 C9 1.54(3) . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? N4 C15 1.3900 . ? N4 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.563(18) . ? N6 C24 1.3900 . ? N6 C28 1.3900 . ? C24 C25 1.3900 . ? C24 C23 1.514(18) . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C30 1.52(4) . ? C31 C32 1.52(4) . ? C20 C21 1.538(14) . ? C6 N2 1.643(19) . ? N5 C21 1.557(19) . ? N5 C23 1.601(19) . ? N5 C22 1.70(5) . ? C9 C8 1.631(19) . ? C7 N2 1.52(4) . ? N2 C8 1.543(19) . ? 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 Fe1 O4 95.4(9) . . ? O1 Fe1 O2 95.2(9) . . ? O4 Fe1 O2 102.5(9) . . ? O1 Fe1 N1 95.9(9) . . ? O4 Fe1 N1 84.7(9) . . ? O2 Fe1 N1 166.2(9) . . ? O1 Fe1 N2 176.9(11) . . ? O4 Fe1 N2 85.3(10) . . ? O2 Fe1 N2 87.7(10) . . ? N1 Fe1 N2 81.1(9) . . ? O1 Fe1 N3 94.5(9) . . ? O4 Fe1 N3 168.7(9) . . ? O2 Fe1 N3 81.9(9) . . ? N1 Fe1 N3 89.0(9) . . ? N2 Fe1 N3 84.6(9) . . ? O1 Fe2 O3 98.5(10) . . ? O1 Fe2 O5 98.8(10) . . ? O3 Fe2 O5 86.6(9) . . ? O1 Fe2 N6 93.5(9) . . ? O3 Fe2 N6 168.0(10) . . ? O5 Fe2 N6 90.6(9) . . ? O1 Fe2 N4 93.9(9) . . ? O3 Fe2 N4 89.8(9) . . ? O5 Fe2 N4 167.1(10) . . ? N6 Fe2 N4 90.4(9) . . ? O1 Fe2 N5 165.9(9) . . ? O3 Fe2 N5 94.2(10) . . ? O5 Fe2 N5 75.6(10) . . ? N6 Fe2 N5 73.8(10) . . ? N4 Fe2 N5 92.4(10) . . ? O8 Cl1 O6 123(3) . . ? O8 Cl1 O7 100.0(17) . . ? O6 Cl1 O7 103(2) . . ? O8 Cl1 O9 105(2) . . ? O6 Cl1 O9 118.4(19) . . ? O7 Cl1 O9 105(3) . . ? O10 Cl2 O11 116(2) . . ? O10 Cl2 O12 121.5(14) . . ? O11 Cl2 O12 111(2) . . ? O10 Cl2 O13 100.1(17) . . ? O11 Cl2 O13 105.1(14) . . ? O12 Cl2 O13 99.6(17) . . ? Fe1 O1 Fe2 121.1(8) . . ? C29 O2 Fe1 128(2) . . ? C29 O3 Fe2 128(2) . . ? C31 O4 Fe1 125.4(17) . . ? C31 O5 Fe2 131(2) . . ? C1 N1 C5 120.0 . . ? C1 N1 Fe1 115.0(11) . . ? C5 N1 Fe1 123.9(11) . . ? N1 C1 C2 120.0 . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 C6 140.5(17) . . ? N1 C5 C6 99.5(17) . . ? C10 N3 C14 120.0 . . ? C10 N3 Fe1 126.7(11) . . ? C14 N3 Fe1 112.1(11) . . ? N3 C10 C11 120.0 . . ? N3 C10 C9 109.3(18) . . ? C11 C10 C9 129.6(18) . . ? C12 C11 C10 120.0 . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 N3 120.0 . . ? C15 N4 C19 120.0 . . ? C15 N4 Fe2 121.8(12) . . ? C19 N4 Fe2 117.6(13) . . ? N4 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C19 120.0 . . ? C18 C19 N4 120.0 . . ? C18 C19 C20 120.6(19) . . ? N4 C19 C20 119.0(19) . . ? C24 N6 C28 120.0 . . ? C24 N6 Fe2 111.8(12) . . ? C28 N6 Fe2 128.1(12) . . ? C25 C24 N6 120.0 . . ? C25 C24 C23 104.6(16) . . ? N6 C24 C23 135.1(16) . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 N6 120.0 . . ? O2 C29 O3 127(2) . . ? O2 C29 C30 115(5) . . ? O3 C29 C30 118(5) . . ? O5 C31 O4 124(2) . . ? O5 C31 C32 126(3) . . ? O4 C31 C32 110(3) . . ? C21 C20 C19 105(2) . . ? C5 C6 N2 125(2) . . ? C21 N5 C23 100(2) . . ? C21 N5 C22 80(2) . . ? C23 N5 C22 121(3) . . ? C21 N5 Fe2 114.8(19) . . ? C23 N5 Fe2 125.7(19) . . ? C22 N5 Fe2 106(2) . . ? C24 C23 N5 89.7(17) . . ? C20 C21 N5 107(2) . . ? C10 C9 C8 119(3) . . ? C7 N2 C8 125(3) . . ? C7 N2 C6 96(2) . . ? C8 N2 C6 84(2) . . ? C7 N2 Fe1 116.8(19) . . ? C8 N2 Fe1 118(2) . . ? C6 N2 Fe1 95.9(18) . . ? N2 C8 C9 85(2) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 22.55 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.845 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.145 #=END data_ifn261m _database_code_CSD 209230 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H39 N6 Co2 O4, 3[Cl O4], C2 H3 N' _chemical_formula_sum 'C32 H42 Cl3 Co2 N7 O16' _chemical_formula_weight 1004.94 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.699(2) _cell_length_b 17.571(3) _cell_length_c 18.091(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4036.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.100 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart CCD diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 90 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25798 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9575 _reflns_number_gt 6479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SIR97 (Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0505P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.509(19) _refine_ls_number_reflns 9575 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 Cl1 Cl 0.23660(12) -0.11543(7) 0.43188(6) 0.0371(3) Uani 1 1 d . . . O8 O 0.2443(3) -0.04961(18) 0.38287(15) 0.0348(8) Uani 1 1 d . . . O7 O 0.2812(5) -0.1785(3) 0.3996(2) 0.105(2) Uani 1 1 d . . . O5 O 0.1250(4) -0.1316(3) 0.4417(3) 0.0879(18) Uani 1 1 d . . . O6 O 0.2763(4) -0.0967(2) 0.5008(2) 0.0707(16) Uani 1 1 d . . . C32 C 0.7417(5) 0.1288(3) 0.2313(3) 0.0453(13) Uani 1 1 d . . . C31 C 0.8061(5) 0.1957(4) 0.2427(3) 0.0564(17) Uani 1 1 d . . . H31A H 0.8803 0.1827 0.2348 0.085 Uiso 1 1 calc R . . H31B H 0.7965 0.2143 0.2933 0.085 Uiso 1 1 calc R . . H31C H 0.7852 0.2355 0.2076 0.085 Uiso 1 1 calc R . . Co2 Co 0.35585(4) 0.00142(3) 0.17822(3) 0.02065(14) Uani 1 1 d . . . Co1 Co 0.12974(4) 0.01216(3) 0.18125(3) 0.01997(14) Uani 1 1 d . . . O1 O 0.2487(2) 0.07589(15) 0.16067(13) 0.0205(6) Uani 1 1 d . . . H2O H 0.2531 0.1278 0.1463 0.025 Uiso 1 1 calc R . . O2 O 0.2388(2) -0.04722(15) 0.22560(14) 0.0215(6) Uani 1 1 d . . . H1O H 0.2360 -0.0879 0.2601 0.026 Uiso 1 1 calc R . . N6 N 0.4619(3) 0.0591(2) 0.1219(2) 0.0235(9) Uani 1 1 d . . . O3 O 0.1464(2) -0.04198(18) 0.09211(17) 0.0251(7) Uani 1 1 d . . . N1 N 0.0321(3) 0.0783(2) 0.1263(2) 0.0212(9) Uani 1 1 d . . . C10 C 0.0274(3) 0.0260(3) 0.3170(3) 0.0294(11) Uani 1 1 d . . . O4 O 0.3243(2) -0.04784(19) 0.08765(16) 0.0247(8) Uani 1 1 d . . . C11 C -0.0174(4) 0.0609(4) 0.3782(3) 0.0421(15) Uani 1 1 d . . . H11 H -0.0677 0.0346 0.4076 0.051 Uiso 1 1 calc R . . N2 N 0.0187(3) -0.0620(2) 0.2123(2) 0.0269(9) Uani 1 1 d . . . N5 N 0.4505(3) -0.0862(2) 0.2042(2) 0.0290(10) Uani 1 1 d . . . N3 N 0.0960(3) 0.0646(2) 0.2723(2) 0.0218(9) Uani 1 1 d . . . C24 C 0.5395(4) 0.0262(3) 0.0825(3) 0.0282(12) Uani 1 1 d . . . C25 C 0.6073(4) 0.0680(4) 0.0396(3) 0.0366(14) Uani 1 1 d . . . H25 H 0.6580 0.0433 0.0093 0.044 Uiso 1 1 calc R . . C19 C 0.4652(3) -0.0019(3) 0.3111(3) 0.0317(12) Uani 1 1 d . . . C17 C 0.5117(4) 0.0971(4) 0.3927(3) 0.0438(15) Uani 1 1 d . . . H17 H 0.5486 0.1152 0.4349 0.053 Uiso 1 1 calc R . . C26 C 0.6006(4) 0.1477(4) 0.0411(3) 0.0409(15) Uani 1 1 d . . . H26 H 0.6492 0.1779 0.0140 0.049 Uiso 1 1 calc R . . C7 C -0.0887(3) -0.0477(3) 0.1808(3) 0.0331(11) Uani 1 1 d . . . H7B H -0.1227 -0.0059 0.2088 0.040 Uiso 1 1 calc R . . H7A H -0.1323 -0.0939 0.1871 0.040 Uiso 1 1 calc R . . N4 N 0.4061(3) 0.0455(2) 0.2689(2) 0.0231(9) Uani 1 1 d . . . C2 C -0.0018(4) 0.2039(3) 0.0792(3) 0.0299(12) Uani 1 1 d . . . H2 H 0.0157 0.2565 0.0791 0.036 Uiso 1 1 calc R . . C1 C 0.0557(4) 0.1529(3) 0.1205(3) 0.0261(11) Uani 1 1 d . . . H1 H 0.1155 0.1713 0.1465 0.031 Uiso 1 1 calc R . . C23 C 0.5567(4) -0.0581(3) 0.0903(3) 0.0326(12) Uani 1 1 d . . . H23B H 0.6243 -0.0724 0.0669 0.039 Uiso 1 1 calc R . . H23A H 0.4995 -0.0858 0.0647 0.039 Uiso 1 1 calc R . . C28 C 0.4543(4) 0.1355(3) 0.1206(3) 0.0260(11) Uani 1 1 d . . . H28 H 0.3988 0.1591 0.1473 0.031 Uiso 1 1 calc R . . C14 C 0.1245(4) 0.1349(3) 0.2912(3) 0.0263(11) Uani 1 1 d . . . H14 H 0.1735 0.1612 0.2609 0.032 Uiso 1 1 calc R . . C13 C 0.0857(4) 0.1707(3) 0.3528(3) 0.0315(12) Uani 1 1 d . . . H13 H 0.1091 0.2202 0.3657 0.038 Uiso 1 1 calc R . . C4 C -0.1081(4) 0.1014(4) 0.0414(3) 0.0366(14) Uani 1 1 d . . . H4 H -0.1639 0.0818 0.0120 0.044 Uiso 1 1 calc R . . C16 C 0.4492(4) 0.1457(3) 0.3521(3) 0.0391(14) Uani 1 1 d . . . H16 H 0.4418 0.1975 0.3666 0.047 Uiso 1 1 calc R . . C6 C -0.0854(4) -0.0266(3) 0.0994(3) 0.0364(13) Uani 1 1 d . . . H6A H -0.0366 -0.0614 0.0734 0.044 Uiso 1 1 calc R . . H6B H -0.1564 -0.0336 0.0778 0.044 Uiso 1 1 calc R . . C29 C 0.2327(4) -0.0603(3) 0.0626(2) 0.0261(10) Uani 1 1 d . . . C9 C 0.0102(4) -0.0548(3) 0.2956(3) 0.0329(12) Uani 1 1 d . . . H9A H -0.0604 -0.0716 0.3121 0.040 Uiso 1 1 calc R . . H9B H 0.0635 -0.0875 0.3196 0.040 Uiso 1 1 calc R . . C3 C -0.0845(4) 0.1773(4) 0.0382(3) 0.0412(15) Uani 1 1 d . . . H3 H -0.1246 0.2108 0.0081 0.049 Uiso 1 1 calc R . . C18 C 0.5203(4) 0.0222(4) 0.3716(3) 0.0448(16) Uani 1 1 d . . . H18 H 0.5637 -0.0121 0.3985 0.054 Uiso 1 1 calc R . . C15 C 0.3968(4) 0.1185(3) 0.2899(3) 0.0294(12) Uani 1 1 d . . . H15 H 0.3540 0.1521 0.2618 0.035 Uiso 1 1 calc R . . C27 C 0.5238(4) 0.1809(3) 0.0819(3) 0.0331(13) Uani 1 1 d . . . H27 H 0.5179 0.2348 0.0839 0.040 Uiso 1 1 calc R . . C5 C -0.0513(4) 0.0523(3) 0.0873(3) 0.0288(12) Uani 1 1 d . . . C20 C 0.4601(4) -0.0840(3) 0.2864(3) 0.0382(13) Uani 1 1 d . . . H20B H 0.5245 -0.1112 0.3021 0.046 Uiso 1 1 calc R . . H20A H 0.3986 -0.1094 0.3093 0.046 Uiso 1 1 calc R . . C12 C 0.0118(4) 0.1334(3) 0.3957(3) 0.0389(14) Uani 1 1 d . . . H12 H -0.0185 0.1583 0.4372 0.047 Uiso 1 1 calc R . . Cl2 Cl 0.25898(10) 0.31186(6) 0.16498(6) 0.0320(3) Uani 1 1 d . . . O9 O 0.1639(3) 0.3003(2) 0.2046(2) 0.0536(11) Uani 1 1 d . . . O11 O 0.3456(3) 0.2839(2) 0.2076(2) 0.0596(12) Uani 1 1 d . . . O10 O 0.2537(3) 0.2684(2) 0.09779(17) 0.0515(10) Uani 1 1 d . . . O12 O 0.2726(4) 0.3910(2) 0.1499(3) 0.0762(14) Uani 1 1 d . . . Cl3 Cl 0.25301(11) 0.69080(7) 0.01350(6) 0.0347(3) Uani 1 1 d . . . O13 O 0.2469(3) 0.61088(19) 0.03202(18) 0.0443(8) Uani 1 1 d . . . O14 O 0.2350(6) 0.7340(3) 0.0773(2) 0.0937(18) Uani 1 1 d . . . O16 O 0.3532(4) 0.7089(3) -0.0119(3) 0.098(2) Uani 1 1 d . . . O15 O 0.1754(4) 0.7099(3) -0.0392(3) 0.0866(19) Uani 1 1 d . . . C21 C 0.4048(4) -0.1612(3) 0.1835(3) 0.0419(14) Uani 1 1 d . . . H21B H 0.3977 -0.1642 0.1296 0.063 Uiso 1 1 calc R . . H21A H 0.3353 -0.1668 0.2064 0.063 Uiso 1 1 calc R . . H21C H 0.4512 -0.2021 0.2008 0.063 Uiso 1 1 calc R . . C8 C 0.0490(4) -0.1428(3) 0.1939(3) 0.0375(13) Uani 1 1 d . . . H8C H 0.1196 -0.1534 0.2132 0.056 Uiso 1 1 calc R . . H8A H 0.0486 -0.1497 0.1402 0.056 Uiso 1 1 calc R . . H8B H -0.0017 -0.1779 0.2165 0.056 Uiso 1 1 calc R . . C30 C 0.2259(4) -0.1024(3) -0.0103(2) 0.0335(12) Uani 1 1 d . . . H30A H 0.1518 -0.1087 -0.0242 0.050 Uiso 1 1 calc R . . H30B H 0.2588 -0.1526 -0.0052 0.050 Uiso 1 1 calc R . . H30C H 0.2626 -0.0733 -0.0486 0.050 Uiso 1 1 calc R . . C22 C 0.5584(3) -0.0808(3) 0.1712(3) 0.0345(12) Uani 1 1 d . . . H22A H 0.5941 -0.1306 0.1761 0.041 Uiso 1 1 calc R . . H22B H 0.6000 -0.0429 0.1993 0.041 Uiso 1 1 calc R . . N7 N 0.6943(5) 0.0765(4) 0.2207(4) 0.085(2) 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 Cl1 0.0574(8) 0.0310(7) 0.0230(5) -0.0009(5) 0.0018(7) -0.0052(7) O8 0.047(2) 0.0327(19) 0.0246(15) 0.0034(13) -0.0030(19) -0.004(2) O7 0.217(7) 0.037(3) 0.062(3) -0.003(2) 0.052(4) 0.024(4) O5 0.064(3) 0.113(4) 0.087(4) 0.048(3) -0.018(3) -0.044(3) O6 0.135(5) 0.050(3) 0.0271(19) 0.0015(18) -0.017(2) -0.011(3) C32 0.048(3) 0.043(4) 0.045(3) -0.001(2) -0.005(3) -0.001(3) C31 0.065(4) 0.045(4) 0.059(4) 0.000(3) 0.005(3) -0.004(3) Co2 0.0192(3) 0.0225(3) 0.0202(3) 0.0000(3) 0.0004(2) 0.0004(3) Co1 0.0197(3) 0.0215(3) 0.0186(3) 0.0005(3) 0.0003(2) -0.0013(3) O1 0.0218(13) 0.0168(15) 0.0230(14) 0.0000(11) 0.0030(16) 0.0011(15) O2 0.0209(15) 0.0180(15) 0.0257(14) 0.0043(12) 0.0036(14) -0.0010(14) N6 0.0195(19) 0.029(2) 0.022(2) 0.0003(18) -0.0011(16) -0.0015(18) O3 0.0229(16) 0.0246(18) 0.0278(18) -0.0026(14) 0.0008(14) -0.0022(15) N1 0.0222(19) 0.022(2) 0.020(2) -0.0048(16) 0.0006(16) -0.0007(17) C10 0.024(2) 0.036(3) 0.028(3) 0.006(2) 0.001(2) 0.002(2) O4 0.0241(16) 0.0266(19) 0.0235(19) -0.0044(14) 0.0003(13) 0.0019(15) C11 0.036(3) 0.061(4) 0.029(3) 0.005(3) 0.008(2) 0.007(3) N2 0.025(2) 0.022(2) 0.033(2) -0.0006(18) 0.0016(17) -0.0043(17) N5 0.025(2) 0.028(2) 0.034(2) -0.0008(19) 0.0012(17) -0.0005(18) N3 0.0246(19) 0.025(2) 0.016(2) 0.0015(16) 0.0001(15) 0.0053(17) C24 0.018(2) 0.040(3) 0.026(3) -0.001(2) 0.0002(19) 0.005(2) C25 0.018(2) 0.062(4) 0.030(3) -0.001(3) 0.009(2) 0.004(3) C19 0.0204(19) 0.051(4) 0.024(3) 0.006(3) 0.0019(18) -0.003(2) C17 0.033(3) 0.072(5) 0.027(3) -0.001(3) -0.010(2) -0.006(3) C26 0.028(3) 0.057(4) 0.037(3) 0.015(3) 0.005(2) -0.012(3) C7 0.023(2) 0.036(3) 0.041(3) 0.006(3) -0.004(2) -0.008(2) N4 0.0214(19) 0.023(2) 0.025(2) 0.0018(17) 0.0036(16) -0.0004(17) C2 0.032(3) 0.032(3) 0.026(3) 0.008(2) -0.002(2) 0.004(2) C1 0.021(2) 0.031(3) 0.027(3) 0.002(2) 0.000(2) 0.003(2) C23 0.025(3) 0.034(3) 0.039(3) -0.009(2) 0.005(2) 0.006(2) C28 0.027(2) 0.034(3) 0.017(3) 0.004(2) -0.003(2) -0.001(2) C14 0.031(2) 0.025(3) 0.024(2) 0.001(2) -0.005(2) 0.006(2) C13 0.044(3) 0.030(3) 0.021(3) -0.001(2) -0.008(2) 0.007(2) C4 0.025(2) 0.061(4) 0.024(3) -0.003(3) -0.005(2) 0.002(3) C16 0.040(3) 0.046(4) 0.031(3) -0.004(3) 0.006(2) -0.016(3) C6 0.027(3) 0.047(4) 0.036(3) 0.000(3) -0.010(2) -0.002(2) C29 0.032(3) 0.023(2) 0.023(2) 0.0017(18) -0.004(2) -0.006(2) C9 0.030(3) 0.036(3) 0.033(3) 0.007(2) 0.001(2) -0.010(2) C3 0.034(3) 0.058(4) 0.031(3) 0.018(3) 0.003(2) 0.007(3) C18 0.034(3) 0.073(5) 0.027(3) 0.004(3) -0.007(2) -0.001(3) C15 0.034(3) 0.034(3) 0.020(3) -0.002(2) 0.006(2) -0.009(2) C27 0.032(3) 0.032(3) 0.035(3) 0.010(2) -0.007(2) -0.005(2) C5 0.023(2) 0.041(3) 0.023(3) -0.001(2) -0.001(2) -0.003(2) C20 0.035(3) 0.042(4) 0.037(3) 0.014(3) 0.002(2) 0.008(3) C12 0.037(3) 0.052(4) 0.028(3) -0.006(3) 0.001(2) 0.011(3) Cl2 0.0296(6) 0.0265(6) 0.0400(6) 0.0031(5) 0.0018(6) -0.0012(5) O9 0.052(2) 0.043(3) 0.066(3) -0.010(2) 0.030(2) 0.000(2) O11 0.062(3) 0.045(3) 0.072(3) -0.011(2) -0.040(2) 0.012(2) O10 0.054(2) 0.071(3) 0.0297(17) -0.0037(17) 0.004(2) -0.007(3) O12 0.063(3) 0.036(2) 0.130(4) 0.033(3) 0.004(3) -0.006(2) Cl3 0.0359(6) 0.0335(7) 0.0346(6) 0.0019(5) -0.0051(6) -0.0010(7) O13 0.051(2) 0.030(2) 0.052(2) 0.0118(16) -0.003(2) -0.005(2) O14 0.176(6) 0.055(3) 0.050(3) -0.017(2) 0.028(4) -0.025(4) O16 0.053(3) 0.088(4) 0.154(5) 0.080(4) 0.041(3) 0.013(3) O15 0.117(4) 0.038(3) 0.105(4) 0.008(3) -0.085(3) -0.004(3) C21 0.038(3) 0.022(3) 0.066(4) 0.010(3) 0.007(3) 0.004(2) C8 0.033(3) 0.026(3) 0.053(4) -0.002(3) 0.000(2) -0.005(2) C30 0.039(3) 0.035(3) 0.027(2) -0.010(2) 0.000(2) 0.005(2) C22 0.024(2) 0.032(3) 0.047(3) 0.000(3) 0.001(2) 0.006(2) N7 0.099(5) 0.065(4) 0.090(5) 0.005(4) -0.028(4) -0.032(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 Cl1 O7 1.375(4) . ? Cl1 O6 1.384(4) . ? Cl1 O5 1.457(5) . ? Cl1 O8 1.461(3) . ? C32 N7 1.115(7) . ? C32 C31 1.447(8) . ? Co2 O4 1.896(3) . ? Co2 O1 1.914(3) . ? Co2 O2 1.917(3) . ? Co2 N4 1.923(4) . ? Co2 N6 1.970(4) . ? Co2 N5 2.010(4) . ? Co2 Co1 2.8781(9) . ? Co1 O3 1.884(3) . ? Co1 O2 1.911(3) . ? Co1 O1 1.917(3) . ? Co1 N3 1.935(4) . ? Co1 N1 1.969(4) . ? Co1 N2 2.000(4) . ? N6 C24 1.346(6) . ? N6 C28 1.347(6) . ? O3 C29 1.261(5) . ? N1 C1 1.348(6) . ? N1 C5 1.352(6) . ? C10 N3 1.368(6) . ? C10 C11 1.388(7) . ? C10 C9 1.488(7) . ? O4 C29 1.268(5) . ? C11 C12 1.365(8) . ? N2 C7 1.499(5) . ? N2 C8 1.508(6) . ? N2 C9 1.516(6) . ? N5 C21 1.488(6) . ? N5 C20 1.492(6) . ? N5 C22 1.498(6) . ? N3 C14 1.332(6) . ? C24 C25 1.372(7) . ? C24 C23 1.504(7) . ? C25 C26 1.403(8) . ? C19 N4 1.358(6) . ? C19 C18 1.366(7) . ? C19 C20 1.511(8) . ? C17 C18 1.376(9) . ? C17 C16 1.377(8) . ? C26 C27 1.356(7) . ? C7 C6 1.519(7) . ? N4 C15 1.342(6) . ? C2 C3 1.368(7) . ? C2 C1 1.378(6) . ? C23 C22 1.517(7) . ? C28 C27 1.381(7) . ? C14 C13 1.371(6) . ? C13 C12 1.382(7) . ? C4 C3 1.369(8) . ? C4 C5 1.398(7) . ? C16 C15 1.393(7) . ? C6 C5 1.469(7) . ? C29 C30 1.514(6) . ? Cl2 O9 1.419(4) . ? Cl2 O12 1.428(4) . ? Cl2 O11 1.430(4) . ? Cl2 O10 1.437(3) . ? Cl3 O16 1.390(4) . ? Cl3 O14 1.400(4) . ? Cl3 O15 1.411(4) . ? Cl3 O13 1.446(3) . ? 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 O7 Cl1 O6 115.1(3) . . ? O7 Cl1 O5 107.2(4) . . ? O6 Cl1 O5 106.9(3) . . ? O7 Cl1 O8 110.6(2) . . ? O6 Cl1 O8 109.5(2) . . ? O5 Cl1 O8 107.1(3) . . ? N7 C32 C31 177.7(7) . . ? O4 Co2 O1 91.06(12) . . ? O4 Co2 O2 91.08(13) . . ? O1 Co2 O2 80.09(12) . . ? O4 Co2 N4 172.43(14) . . ? O1 Co2 N4 95.84(14) . . ? O2 Co2 N4 93.18(14) . . ? O4 Co2 N6 86.14(15) . . ? O1 Co2 N6 92.79(14) . . ? O2 Co2 N6 172.32(14) . . ? N4 Co2 N6 90.39(16) . . ? O4 Co2 N5 88.79(15) . . ? O1 Co2 N5 171.08(14) . . ? O2 Co2 N5 90.99(14) . . ? N4 Co2 N5 84.88(16) . . ? N6 Co2 N5 96.10(16) . . ? O4 Co2 Co1 80.53(9) . . ? O1 Co2 Co1 41.35(9) . . ? O2 Co2 Co1 41.17(9) . . ? N4 Co2 Co1 106.75(11) . . ? N6 Co2 Co1 131.19(12) . . ? N5 Co2 Co1 129.98(12) . . ? O3 Co1 O2 90.14(12) . . ? O3 Co1 O1 92.32(12) . . ? O2 Co1 O1 80.16(12) . . ? O3 Co1 N3 173.52(15) . . ? O2 Co1 N3 93.60(14) . . ? O1 Co1 N3 93.54(14) . . ? O3 Co1 N1 86.37(15) . . ? O2 Co1 N1 172.27(14) . . ? O1 Co1 N1 93.08(14) . . ? N3 Co1 N1 90.54(16) . . ? O3 Co1 N2 89.44(15) . . ? O2 Co1 N2 92.14(14) . . ? O1 Co1 N2 172.10(14) . . ? N3 Co1 N2 85.13(17) . . ? N1 Co1 N2 94.71(16) . . ? O3 Co1 Co2 80.73(9) . . ? O2 Co1 Co2 41.31(9) . . ? O1 Co1 Co2 41.26(8) . . ? N3 Co1 Co2 105.55(11) . . ? N1 Co1 Co2 131.12(11) . . ? N2 Co1 Co2 131.74(12) . . ? Co2 O1 Co1 97.39(12) . . ? Co1 O2 Co2 97.52(12) . . ? C24 N6 C28 118.1(4) . . ? C24 N6 Co2 123.6(4) . . ? C28 N6 Co2 118.2(3) . . ? C29 O3 Co1 126.1(3) . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Co1 118.2(3) . . ? C5 N1 Co1 123.9(3) . . ? N3 C10 C11 120.9(5) . . ? N3 C10 C9 114.3(4) . . ? C11 C10 C9 124.7(5) . . ? C29 O4 Co2 125.6(3) . . ? C12 C11 C10 119.1(5) . . ? C7 N2 C8 107.8(4) . . ? C7 N2 C9 107.4(4) . . ? C8 N2 C9 108.4(4) . . ? C7 N2 Co1 115.1(3) . . ? C8 N2 Co1 111.9(3) . . ? C9 N2 Co1 105.9(3) . . ? C21 N5 C20 107.9(4) . . ? C21 N5 C22 108.2(4) . . ? C20 N5 C22 108.7(4) . . ? C21 N5 Co2 112.7(3) . . ? C20 N5 Co2 105.2(3) . . ? C22 N5 Co2 113.9(3) . . ? C14 N3 C10 118.7(4) . . ? C14 N3 Co1 126.8(3) . . ? C10 N3 Co1 114.1(3) . . ? N6 C24 C25 121.9(5) . . ? N6 C24 C23 118.6(5) . . ? C25 C24 C23 119.3(5) . . ? C24 C25 C26 119.0(5) . . ? N4 C19 C18 122.9(5) . . ? N4 C19 C20 113.3(4) . . ? C18 C19 C20 123.7(5) . . ? C18 C17 C16 119.5(5) . . ? C27 C26 C25 118.9(5) . . ? N2 C7 C6 112.6(4) . . ? C15 N4 C19 118.4(4) . . ? C15 N4 Co2 126.7(4) . . ? C19 N4 Co2 114.6(3) . . ? C3 C2 C1 118.6(5) . . ? N1 C1 C2 123.8(5) . . ? C24 C23 C22 110.6(4) . . ? N6 C28 C27 122.6(5) . . ? N3 C14 C13 122.4(5) . . ? C14 C13 C12 118.9(5) . . ? C3 C4 C5 120.9(5) . . ? C17 C16 C15 119.5(5) . . ? C5 C6 C7 112.5(4) . . ? O3 C29 O4 127.0(4) . . ? O3 C29 C30 116.4(4) . . ? O4 C29 C30 116.6(4) . . ? C10 C9 N2 109.2(4) . . ? C2 C3 C4 118.6(5) . . ? C19 C18 C17 118.6(6) . . ? N4 C15 C16 121.0(5) . . ? C26 C27 C28 119.2(5) . . ? N1 C5 C4 120.4(5) . . ? N1 C5 C6 118.2(5) . . ? C4 C5 C6 121.3(5) . . ? N5 C20 C19 108.9(4) . . ? C11 C12 C13 119.8(5) . . ? O9 Cl2 O12 109.8(3) . . ? O9 Cl2 O11 109.4(2) . . ? O12 Cl2 O11 110.1(3) . . ? O9 Cl2 O10 108.2(3) . . ? O12 Cl2 O10 111.2(3) . . ? O11 Cl2 O10 108.0(3) . . ? O16 Cl3 O14 107.3(4) . . ? O16 Cl3 O15 111.2(3) . . ? O14 Cl3 O15 108.3(4) . . ? O16 Cl3 O13 110.3(3) . . ? O14 Cl3 O13 109.1(2) . . ? O15 Cl3 O13 110.5(3) . . ? N5 C22 C23 112.8(4) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.722 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.088 #=END