data_cpd3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H68 Cl4 Mn4 N4 O8' _chemical_formula_sum 'C52 H68 Cl4 Mn4 N4 O8' _chemical_formula_weight 1238.66 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' 'Mn' 'Mn' 0.3368 0.7283 '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 tetragonal _symmetry_space_group_name_H-M 'I -4' _symmetry_space_group_name_Hall 'I -4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.8213(8) _cell_length_b 15.8213(8) _cell_length_c 11.4105(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2856.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 17214 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 29.51 _exptl_crystal_description block _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.104 _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 153(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 'STOE IPDS' _diffrn_measurement_method 'omega oscillation' _diffrn_detector_area_resol_mean 0.716\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13058 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 29.51 _reflns_number_total 3963 _reflns_number_gt 3705 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+1.8854P] 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 SHELXL _refine_ls_extinction_coef 0.0046(6) _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 0.01(2) _refine_ls_number_reflns 3963 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.074354(18) 0.126208(18) 0.50130(3) 0.02955(10) Uani 1 1 d . . . Cl1 Cl -0.05317(4) 0.17638(4) 0.36077(5) 0.03690(13) Uani 1 1 d . . . O1 O 0.07668(12) 0.22745(11) 0.58285(16) 0.0372(4) Uani 1 1 d . . . O2 O 0.08632(10) 0.02359(10) 0.41053(15) 0.0292(3) Uani 1 1 d . . . N1 N 0.15834(12) 0.16984(12) 0.38609(17) 0.0293(4) Uani 1 1 d . . . C1 C 0.10641(14) 0.30138(14) 0.5502(2) 0.0302(4) Uani 1 1 d . . . C2 C 0.08275(18) 0.37236(16) 0.6158(2) 0.0381(5) Uani 1 1 d . . . H2A H 0.0470 0.3657 0.6799 0.046 Uiso 1 1 calc R . . C3 C 0.1113(2) 0.45127(17) 0.5875(2) 0.0443(6) Uani 1 1 d . . . H3A H 0.0938 0.4970 0.6325 0.053 Uiso 1 1 calc R . . C4 C 0.1655(2) 0.46552(16) 0.4937(3) 0.0493(6) Uani 1 1 d . . . C5 C 0.18968(19) 0.39553(17) 0.4289(2) 0.0428(6) Uani 1 1 d . . . H5A H 0.2267 0.4029 0.3664 0.051 Uiso 1 1 calc R . . C6 C 0.16046(14) 0.31416(15) 0.4541(2) 0.0313(4) Uani 1 1 d . . . C7 C 0.18503(14) 0.24579(14) 0.3786(2) 0.0303(4) Uani 1 1 d . . . H7A H 0.2236 0.2579 0.3194 0.036 Uiso 1 1 calc R . . C8 C 0.18801(15) 0.10327(15) 0.3061(2) 0.0337(5) Uani 1 1 d . . . H8B H 0.2380 0.0760 0.3377 0.040 Uiso 1 1 calc R . . H8A H 0.2019 0.1271 0.2302 0.040 Uiso 1 1 calc R . . C9 C 0.11637(15) 0.04016(14) 0.2947(2) 0.0324(4) Uani 1 1 d . . . H9B H 0.0714 0.0634 0.2467 0.039 Uiso 1 1 calc R . . H9A H 0.1364 -0.0116 0.2585 0.039 Uiso 1 1 calc R . . C10 C 0.1926(3) 0.5545(2) 0.4574(3) 0.0792(14) Uani 1 1 d . . . C11 C 0.1650(5) 0.6201(3) 0.5462(5) 0.155(4) Uani 1 1 d . . . H11A H 0.2005 0.6167 0.6143 0.233 Uiso 1 1 calc R . . H11B H 0.1074 0.6099 0.5684 0.233 Uiso 1 1 calc R . . H11C H 0.1696 0.6755 0.5123 0.233 Uiso 1 1 calc R . . C12 C 0.2880(4) 0.5578(3) 0.4444(5) 0.114(2) Uani 1 1 d . . . H12A H 0.3059 0.6157 0.4396 0.170 Uiso 1 1 calc R . . H12B H 0.3044 0.5285 0.3744 0.170 Uiso 1 1 calc R . . H12C H 0.3139 0.5314 0.5111 0.170 Uiso 1 1 calc R . . C13 C 0.1526(5) 0.5751(3) 0.3399(5) 0.118(3) Uani 1 1 d . . . H13A H 0.0922 0.5762 0.3480 0.178 Uiso 1 1 calc R . . H13B H 0.1683 0.5328 0.2836 0.178 Uiso 1 1 calc R . . H13C H 0.1721 0.6294 0.3138 0.178 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 Mn1 0.02920(16) 0.02702(15) 0.03244(16) 0.00101(15) 0.00475(15) -0.00185(10) Cl1 0.0367(3) 0.0350(3) 0.0391(3) 0.0069(2) 0.0047(2) 0.0052(2) O1 0.0435(9) 0.0308(8) 0.0373(9) -0.0013(7) 0.0132(7) -0.0081(7) O2 0.0300(7) 0.0268(7) 0.0309(8) 0.0030(6) 0.0000(6) 0.0041(5) N1 0.0267(8) 0.0312(9) 0.0299(9) 0.0040(7) 0.0045(7) 0.0022(6) C1 0.0316(10) 0.0285(10) 0.0306(10) 0.0012(8) -0.0003(8) -0.0036(8) C2 0.0492(14) 0.0366(11) 0.0285(11) -0.0051(9) 0.0084(9) -0.0110(10) C3 0.0685(18) 0.0327(11) 0.0318(12) -0.0053(10) 0.0061(12) -0.0101(11) C4 0.0771(18) 0.0345(11) 0.0363(12) -0.0007(12) 0.0103(15) -0.0168(11) C5 0.0528(15) 0.0391(12) 0.0365(13) 0.0008(10) 0.0101(11) -0.0132(11) C6 0.0310(10) 0.0323(10) 0.0307(10) 0.0005(8) 0.0006(8) -0.0035(8) C7 0.0266(9) 0.0341(10) 0.0303(11) 0.0058(8) 0.0027(8) -0.0005(7) C8 0.0340(10) 0.0321(10) 0.0351(11) 0.0026(9) 0.0078(9) 0.0057(8) C9 0.0373(11) 0.0298(10) 0.0300(11) 0.0003(8) 0.0015(9) 0.0060(8) C10 0.147(4) 0.0365(14) 0.0543(19) -0.0084(13) 0.047(2) -0.0328(19) C11 0.297(10) 0.046(2) 0.123(5) -0.039(3) 0.137(6) -0.073(4) C12 0.157(5) 0.085(3) 0.100(4) -0.022(3) 0.049(4) -0.080(4) C13 0.231(8) 0.043(2) 0.081(3) 0.021(2) 0.047(4) 0.007(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 Mn1 O1 1.8528(17) . ? Mn1 O2 1.9351(16) . ? Mn1 O2 1.9523(16) 4_556 ? Mn1 N1 1.9926(18) . ? Mn1 Cl1 2.5333(7) 3_556 ? Mn1 Cl1 2.6967(7) . ? Cl1 Mn1 2.5333(7) 4_556 ? O1 C1 1.315(3) . ? O2 C9 1.429(3) . ? O2 Mn1 1.9523(16) 3_556 ? N1 C7 1.277(3) . ? N1 C8 1.470(3) . ? C1 C2 1.401(3) . ? C1 C6 1.405(3) . ? C2 C3 1.366(3) . ? C2 H2A 0.9300 . ? C3 C4 1.390(4) . ? C3 H3A 0.9300 . ? C4 C5 1.385(4) . ? C4 C10 1.528(4) . ? C5 C6 1.398(3) . ? C5 H5A 0.9300 . ? C6 C7 1.436(3) . ? C7 H7A 0.9300 . ? C8 C9 1.516(3) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9A 0.9700 . ? C10 C11 1.515(5) . ? C10 C12 1.517(8) . ? C10 C13 1.518(8) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 Mn1 O2 172.84(7) . . ? O1 Mn1 O2 92.09(7) . 4_556 ? O2 Mn1 O2 94.72(10) . 4_556 ? O1 Mn1 N1 91.07(8) . . ? O2 Mn1 N1 82.67(7) . . ? O2 Mn1 N1 168.89(8) 4_556 . ? O1 Mn1 Cl1 93.99(7) . 3_556 ? O2 Mn1 Cl1 83.54(5) . 3_556 ? O2 Mn1 Cl1 92.19(5) 4_556 3_556 ? N1 Mn1 Cl1 98.22(6) . 3_556 ? O1 Mn1 Cl1 93.38(7) . . ? O2 Mn1 Cl1 90.11(5) . . ? O2 Mn1 Cl1 78.91(5) 4_556 . ? N1 Mn1 Cl1 90.27(6) . . ? Cl1 Mn1 Cl1 168.64(2) 3_556 . ? Mn1 Cl1 Mn1 77.544(19) 4_556 . ? C1 O1 Mn1 129.33(15) . . ? C9 O2 Mn1 111.94(13) . . ? C9 O2 Mn1 120.98(13) . 3_556 ? Mn1 O2 Mn1 114.95(8) . 3_556 ? C7 N1 C8 121.83(19) . . ? C7 N1 Mn1 126.20(16) . . ? C8 N1 Mn1 111.96(14) . . ? O1 C1 C2 117.8(2) . . ? O1 C1 C6 124.6(2) . . ? C2 C1 C6 117.7(2) . . ? C3 C2 C1 121.2(2) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 122.3(2) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C3 116.9(2) . . ? C5 C4 C10 121.0(3) . . ? C3 C4 C10 122.0(3) . . ? C4 C5 C6 122.4(2) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C7 118.7(2) . . ? C1 C6 C7 121.6(2) . . ? N1 C7 C6 125.4(2) . . ? N1 C7 H7A 117.3 . . ? C6 C7 H7A 117.3 . . ? N1 C8 C9 106.66(18) . . ? N1 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? N1 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? H8B C8 H8A 108.6 . . ? O2 C9 C8 106.8(2) . . ? O2 C9 H9B 110.4 . . ? C8 C9 H9B 110.4 . . ? O2 C9 H9A 110.4 . . ? C8 C9 H9A 110.4 . . ? H9B C9 H9A 108.6 . . ? C11 C10 C12 109.1(4) . . ? C11 C10 C13 108.9(5) . . ? C12 C10 C13 108.7(4) . . ? C11 C10 C4 111.7(3) . . ? C12 C10 C4 109.7(4) . . ? C13 C10 C4 108.7(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 Mn1 Cl1 Mn1 -105.51(5) . . . 4_556 ? O2 Mn1 Cl1 Mn1 80.74(5) . . . 4_556 ? O2 Mn1 Cl1 Mn1 -14.04(5) 4_556 . . 4_556 ? N1 Mn1 Cl1 Mn1 163.41(6) . . . 4_556 ? Cl1 Mn1 Cl1 Mn1 24.91(9) 3_556 . . 4_556 ? O2 Mn1 O1 C1 44.1(8) . . . . ? O2 Mn1 O1 C1 -154.0(2) 4_556 . . . ? N1 Mn1 O1 C1 15.4(2) . . . . ? Cl1 Mn1 O1 C1 113.7(2) 3_556 . . . ? Cl1 Mn1 O1 C1 -75.0(2) . . . . ? O1 Mn1 O2 C9 -51.8(7) . . . . ? O2 Mn1 O2 C9 146.33(16) 4_556 . . . ? N1 Mn1 O2 C9 -22.81(15) . . . . ? Cl1 Mn1 O2 C9 -122.00(14) 3_556 . . . ? Cl1 Mn1 O2 C9 67.44(14) . . . . ? O1 Mn1 O2 Mn1 91.2(7) . . . 3_556 ? O2 Mn1 O2 Mn1 -70.60(8) 4_556 . . 3_556 ? N1 Mn1 O2 Mn1 120.26(10) . . . 3_556 ? Cl1 Mn1 O2 Mn1 21.08(7) 3_556 . . 3_556 ? Cl1 Mn1 O2 Mn1 -149.48(8) . . . 3_556 ? O1 Mn1 N1 C7 -8.5(2) . . . . ? O2 Mn1 N1 C7 175.0(2) . . . . ? O2 Mn1 N1 C7 98.0(4) 4_556 . . . ? Cl1 Mn1 N1 C7 -102.69(19) 3_556 . . . ? Cl1 Mn1 N1 C7 84.89(19) . . . . ? O1 Mn1 N1 C8 171.72(16) . . . . ? O2 Mn1 N1 C8 -4.81(15) . . . . ? O2 Mn1 N1 C8 -81.8(4) 4_556 . . . ? Cl1 Mn1 N1 C8 77.53(15) 3_556 . . . ? Cl1 Mn1 N1 C8 -94.89(15) . . . . ? Mn1 O1 C1 C2 164.97(19) . . . . ? Mn1 O1 C1 C6 -15.2(4) . . . . ? O1 C1 C2 C3 179.8(3) . . . . ? C6 C1 C2 C3 0.0(4) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C2 C3 C4 C10 175.9(4) . . . . ? C3 C4 C5 C6 1.1(5) . . . . ? C10 C4 C5 C6 -174.7(4) . . . . ? C4 C5 C6 C1 -1.8(4) . . . . ? C4 C5 C6 C7 176.6(3) . . . . ? O1 C1 C6 C5 -178.6(3) . . . . ? C2 C1 C6 C5 1.2(4) . . . . ? O1 C1 C6 C7 3.0(4) . . . . ? C2 C1 C6 C7 -177.2(2) . . . . ? C8 N1 C7 C6 -178.9(2) . . . . ? Mn1 N1 C7 C6 1.3(3) . . . . ? C5 C6 C7 N1 -174.7(2) . . . . ? C1 C6 C7 N1 3.7(4) . . . . ? C7 N1 C8 C9 -150.8(2) . . . . ? Mn1 N1 C8 C9 29.0(2) . . . . ? Mn1 O2 C9 C8 44.43(19) . . . . ? Mn1 O2 C9 C8 -96.12(18) 3_556 . . . ? N1 C8 C9 O2 -46.5(2) . . . . ? C5 C4 C10 C11 -175.3(5) . . . . ? C3 C4 C10 C11 9.1(7) . . . . ? C5 C4 C10 C12 -54.1(5) . . . . ? C3 C4 C10 C12 130.3(4) . . . . ? C5 C4 C10 C13 64.6(5) . . . . ? C3 C4 C10 C13 -111.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.341 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.057