# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prasanta Ghosh' _publ_contact_author_email 'ghoshp chem@yahoo.co.in' loop_ _publ_author_name A.S.Roy M.K.Biswas T.Weyhermueller P.Ghosh data_CCDC668788 _database_code_depnum_ccdc_archive 'CCDC 668788' #TrackingRef '- CCDC668788 and CCDC770797.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Cl2 Fe N6 O4, 0.5(H2 O)' _chemical_formula_sum 'C24 H19 Cl2 Fe N6 O4.50' _chemical_formula_weight 590.20 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5743(9) _cell_length_b 14.0029(6) _cell_length_c 15.1688(10) _cell_angle_alpha 90.00 _cell_angle_beta 113.043(4) _cell_angle_gamma 90.00 _cell_volume 2457.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 38108 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.03 _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9451 _exptl_absorpt_correction_T_max 0.9826 _exptl_absorpt_process_details 'SADABS 2006/1, Bruker AXS (2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 70 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa-CCD' _diffrn_measurement_method '265 images at 1.0 deg. stewise rotation in omega and phi, 240 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12052 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4308 _reflns_number_gt 3217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0238P)^2^+2.3953P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4308 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.78496(4) 0.33210(3) 0.64751(3) 0.01882(12) Uani 1 1 d . . . N1 N 0.9684(2) 0.32322(15) 0.74298(15) 0.0180(5) Uani 1 1 d . . . C2 C 1.0504(3) 0.3886(2) 0.7520(2) 0.0235(7) Uani 1 1 d . . . H2 H 1.0286 0.4456 0.7154 0.028 Uiso 1 1 calc R . . C3 C 1.1651(3) 0.3765(2) 0.8122(2) 0.0267(7) Uani 1 1 d . . . H3 H 1.2201 0.4249 0.8172 0.032 Uiso 1 1 calc R . . C4 C 1.1988(3) 0.2942(2) 0.8647(2) 0.0268(7) Uani 1 1 d . . . H4 H 1.2772 0.2850 0.9067 0.032 Uiso 1 1 calc R . . C5 C 1.1170(3) 0.2246(2) 0.8556(2) 0.0256(7) Uani 1 1 d . . . H5 H 1.1385 0.1661 0.8897 0.031 Uiso 1 1 calc R . . C6 C 1.0026(3) 0.24214(19) 0.79545(19) 0.0195(7) Uani 1 1 d . . . C7 C 0.9109(3) 0.1740(2) 0.7868(2) 0.0211(7) Uani 1 1 d . . . H7 H 0.9291 0.1164 0.8227 0.025 Uiso 1 1 calc R . . N8 N 0.8060(2) 0.19166(15) 0.73101(17) 0.0197(6) Uani 1 1 d . . . C9 C 0.7180(3) 0.12728(19) 0.7311(2) 0.0205(7) Uani 1 1 d . . . C10 C 0.7244(3) 0.0756(2) 0.8122(2) 0.0230(7) Uani 1 1 d . . . H10 H 0.7900 0.0823 0.8707 0.028 Uiso 1 1 calc R . . C11 C 0.6352(3) 0.0147(2) 0.8075(2) 0.0260(7) Uani 1 1 d . . . H11 H 0.6407 -0.0204 0.8627 0.031 Uiso 1 1 calc R . . C12 C 0.5382(3) 0.0044(2) 0.7231(2) 0.0261(7) Uani 1 1 d . . . H12 H 0.4773 -0.0377 0.7193 0.031 Uiso 1 1 calc R . . C13 C 0.5332(3) 0.0574(2) 0.6446(2) 0.0227(7) Uani 1 1 d . . . C14 C 0.6205(3) 0.11900(19) 0.6466(2) 0.0216(7) Uani 1 1 d . . . H14 H 0.6137 0.1548 0.5915 0.026 Uiso 1 1 calc R . . N15 N 0.4310(2) 0.04838(18) 0.55405(18) 0.0265(6) Uani 1 1 d . . . O16 O 0.35372(19) -0.00725(15) 0.55063(16) 0.0344(6) Uani 1 1 d . . . O17 O 0.42843(18) 0.09653(15) 0.48495(15) 0.0291(5) Uani 1 1 d . . . N21 N 0.6200(2) 0.31959(16) 0.52455(16) 0.0213(6) Uani 1 1 d . . . C22 C 0.5247(3) 0.3692(2) 0.5134(2) 0.0272(8) Uani 1 1 d . . . H22 H 0.5211 0.4013 0.5674 0.033 Uiso 1 1 calc R . . C23 C 0.4306(3) 0.3757(2) 0.4259(2) 0.0311(8) Uani 1 1 d . . . H23 H 0.3649 0.4128 0.4201 0.037 Uiso 1 1 calc R . . C24 C 0.4344(3) 0.3276(2) 0.3481(2) 0.0303(8) Uani 1 1 d . . . H24 H 0.3712 0.3312 0.2877 0.036 Uiso 1 1 calc R . . C25 C 0.5311(3) 0.2740(2) 0.3584(2) 0.0270(8) Uani 1 1 d . . . H25 H 0.5346 0.2387 0.3062 0.032 Uiso 1 1 calc R . . C26 C 0.6228(3) 0.27307(19) 0.44707(19) 0.0200(7) Uani 1 1 d . . . C27 C 0.7315(3) 0.22377(19) 0.4629(2) 0.0214(7) Uani 1 1 d . . . H27 H 0.7378 0.1827 0.4153 0.026 Uiso 1 1 calc R . . N28 N 0.8179(2) 0.23732(16) 0.54242(16) 0.0202(6) Uani 1 1 d . . . C29 C 0.9251(3) 0.18892(19) 0.56059(19) 0.0202(7) Uani 1 1 d . . . C30 C 0.9345(3) 0.0910(2) 0.5813(2) 0.0245(7) Uani 1 1 d . . . H30 H 0.8684 0.0552 0.5769 0.029 Uiso 1 1 calc R . . C31 C 1.0417(3) 0.0467(2) 0.6083(2) 0.0260(7) Uani 1 1 d . . . H31 H 1.0485 -0.0194 0.6233 0.031 Uiso 1 1 calc R . . C32 C 1.1384(3) 0.0975(2) 0.6138(2) 0.0242(7) Uani 1 1 d . . . H32 H 1.2116 0.0673 0.6321 0.029 Uiso 1 1 calc R . . C33 C 1.1251(3) 0.1936(2) 0.5916(2) 0.0226(7) Uani 1 1 d . . . C34 C 1.0210(3) 0.2413(2) 0.56619(19) 0.0213(7) Uani 1 1 d . . . H34 H 1.0155 0.3078 0.5530 0.026 Uiso 1 1 calc R . . N35 N 1.2271(2) 0.24936(19) 0.59698(17) 0.0270(6) Uani 1 1 d . . . O36 O 1.3188(2) 0.20671(16) 0.61359(16) 0.0366(6) Uani 1 1 d . . . O37 O 1.2159(2) 0.33563(16) 0.58452(18) 0.0435(6) Uani 1 1 d . . . Cl40 Cl 0.81927(8) 0.47560(5) 0.57130(6) 0.0341(2) Uani 1 1 d . . . Cl50 Cl 0.70453(7) 0.39995(5) 0.74873(5) 0.02356(18) Uani 1 1 d . . . O40 O 1.0182(6) 0.5419(5) 0.5288(5) 0.083(2) Uani 0.50 1 d P . . 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 0.0191(3) 0.0186(2) 0.0185(2) -0.00108(17) 0.00708(18) 0.00314(19) N1 0.0206(15) 0.0180(12) 0.0163(12) -0.0007(10) 0.0081(11) 0.0014(11) C2 0.027(2) 0.0199(16) 0.0252(16) -0.0016(12) 0.0127(15) -0.0023(14) C3 0.023(2) 0.0310(18) 0.0280(17) -0.0066(13) 0.0120(15) -0.0091(15) C4 0.0185(19) 0.0289(17) 0.0300(17) -0.0053(13) 0.0061(15) 0.0004(14) C5 0.027(2) 0.0237(16) 0.0230(16) 0.0018(13) 0.0063(15) 0.0072(14) C6 0.0257(18) 0.0161(15) 0.0179(14) -0.0020(11) 0.0097(13) 0.0001(13) C7 0.029(2) 0.0163(15) 0.0204(15) 0.0003(12) 0.0119(14) 0.0008(14) N8 0.0205(16) 0.0165(13) 0.0249(13) -0.0036(10) 0.0119(12) -0.0018(11) C9 0.0220(18) 0.0159(15) 0.0284(16) -0.0041(12) 0.0148(14) 0.0012(13) C10 0.0228(18) 0.0229(16) 0.0239(16) -0.0010(12) 0.0098(14) 0.0024(14) C11 0.034(2) 0.0223(16) 0.0284(17) 0.0041(13) 0.0193(16) 0.0032(15) C12 0.0242(19) 0.0224(16) 0.0365(18) -0.0009(13) 0.0173(16) -0.0022(14) C13 0.0183(18) 0.0217(16) 0.0278(16) -0.0032(12) 0.0088(14) 0.0003(13) C14 0.0230(19) 0.0212(16) 0.0242(16) 0.0006(12) 0.0131(14) 0.0029(14) N15 0.0238(17) 0.0267(14) 0.0323(15) -0.0045(12) 0.0145(13) -0.0008(12) O16 0.0254(14) 0.0368(13) 0.0417(14) -0.0055(10) 0.0138(11) -0.0117(11) O17 0.0243(14) 0.0327(12) 0.0282(12) 0.0027(10) 0.0080(10) 0.0008(10) N21 0.0197(15) 0.0179(12) 0.0247(13) 0.0011(10) 0.0070(11) 0.0037(11) C22 0.024(2) 0.0222(16) 0.0335(18) -0.0014(13) 0.0097(16) 0.0008(14) C23 0.021(2) 0.0248(17) 0.042(2) 0.0053(15) 0.0064(16) 0.0047(14) C24 0.0214(19) 0.0364(18) 0.0250(17) 0.0094(14) 0.0002(14) -0.0063(16) C25 0.029(2) 0.0271(17) 0.0227(16) 0.0002(13) 0.0082(15) -0.0090(15) C26 0.0235(18) 0.0160(15) 0.0199(15) 0.0019(11) 0.0077(13) -0.0042(13) C27 0.031(2) 0.0155(15) 0.0206(15) 0.0015(12) 0.0129(15) -0.0003(14) N28 0.0231(16) 0.0187(13) 0.0209(13) 0.0006(10) 0.0108(12) 0.0024(11) C29 0.0258(19) 0.0209(16) 0.0161(14) -0.0020(11) 0.0105(13) 0.0040(13) C30 0.027(2) 0.0227(16) 0.0272(17) -0.0027(13) 0.0143(15) -0.0030(14) C31 0.034(2) 0.0184(16) 0.0310(17) 0.0014(13) 0.0180(16) 0.0027(14) C32 0.0253(19) 0.0259(16) 0.0251(16) 0.0016(13) 0.0140(14) 0.0046(14) C33 0.0266(19) 0.0265(17) 0.0177(15) -0.0019(12) 0.0120(14) -0.0020(14) C34 0.028(2) 0.0173(15) 0.0192(15) -0.0003(11) 0.0100(14) -0.0022(14) N35 0.0264(17) 0.0328(17) 0.0224(13) 0.0003(11) 0.0103(12) -0.0068(13) O36 0.0234(14) 0.0457(14) 0.0423(14) 0.0007(11) 0.0145(12) -0.0010(12) O37 0.0417(16) 0.0272(14) 0.0590(16) 0.0047(11) 0.0170(13) -0.0087(11) Cl40 0.0445(6) 0.0258(4) 0.0329(4) 0.0108(3) 0.0161(4) 0.0042(4) Cl50 0.0244(4) 0.0254(4) 0.0238(4) -0.0014(3) 0.0126(3) 0.0029(3) O40 0.079(5) 0.094(5) 0.073(4) -0.023(4) 0.026(4) -0.011(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 N21 2.187(2) . ? Fe1 N1 2.195(2) . ? Fe1 N28 2.234(2) . ? Fe1 N8 2.298(2) . ? Fe1 Cl50 2.3449(8) . ? Fe1 Cl40 2.4394(8) . ? N1 C2 1.345(4) . ? N1 C6 1.356(3) . ? C2 C3 1.383(4) . ? C3 C4 1.370(4) . ? C4 C5 1.385(4) . ? C5 C6 1.391(4) . ? C6 C7 1.462(4) . ? C7 N8 1.281(4) . ? N8 C9 1.428(4) . ? C9 C14 1.389(4) . ? C9 C10 1.403(4) . ? C10 C11 1.388(4) . ? C11 C12 1.388(4) . ? C12 C13 1.383(4) . ? C13 C14 1.387(4) . ? C13 N15 1.474(4) . ? N15 O16 1.231(3) . ? N15 O17 1.236(3) . ? N21 C22 1.337(4) . ? N21 C26 1.356(4) . ? C22 C23 1.393(4) . ? C23 C24 1.377(5) . ? C24 C25 1.385(5) . ? C25 C26 1.387(4) . ? C26 C27 1.465(4) . ? C27 N28 1.283(4) . ? N28 C29 1.435(4) . ? C29 C34 1.386(4) . ? C29 C30 1.401(4) . ? C30 C31 1.391(4) . ? C31 C32 1.383(4) . ? C32 C33 1.381(4) . ? C33 C34 1.383(4) . ? C33 N35 1.477(4) . ? N35 O37 1.222(3) . ? N35 O36 1.233(3) . ? O40 O40 1.427(12) 3_766 ? 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 N21 Fe1 N1 163.54(9) . . ? N21 Fe1 N28 73.90(9) . . ? N1 Fe1 N28 89.81(9) . . ? N21 Fe1 N8 105.54(9) . . ? N1 Fe1 N8 73.92(9) . . ? N28 Fe1 N8 82.60(8) . . ? N21 Fe1 Cl50 94.75(7) . . ? N1 Fe1 Cl50 101.65(6) . . ? N28 Fe1 Cl50 162.92(7) . . ? N8 Fe1 Cl50 88.40(6) . . ? N21 Fe1 Cl40 86.93(7) . . ? N1 Fe1 Cl40 91.39(6) . . ? N28 Fe1 Cl40 91.98(6) . . ? N8 Fe1 Cl40 164.29(7) . . ? Cl50 Fe1 Cl40 100.27(3) . . ? C2 N1 C6 117.1(2) . . ? C2 N1 Fe1 126.48(19) . . ? C6 N1 Fe1 116.41(19) . . ? N1 C2 C3 123.0(3) . . ? C4 C3 C2 119.5(3) . . ? C3 C4 C5 119.0(3) . . ? C4 C5 C6 118.6(3) . . ? N1 C6 C5 122.8(3) . . ? N1 C6 C7 115.8(3) . . ? C5 C6 C7 121.3(3) . . ? N8 C7 C6 120.3(3) . . ? C7 N8 C9 118.4(2) . . ? C7 N8 Fe1 113.31(19) . . ? C9 N8 Fe1 128.22(19) . . ? C14 C9 C10 119.5(3) . . ? C14 C9 N8 117.2(3) . . ? C10 C9 N8 123.3(3) . . ? C11 C10 C9 120.3(3) . . ? C12 C11 C10 120.8(3) . . ? C13 C12 C11 117.7(3) . . ? C12 C13 C14 123.1(3) . . ? C12 C13 N15 119.1(3) . . ? C14 C13 N15 117.8(3) . . ? C13 C14 C9 118.5(3) . . ? O16 N15 O17 123.5(3) . . ? O16 N15 C13 118.6(3) . . ? O17 N15 C13 117.9(3) . . ? C22 N21 C26 117.8(3) . . ? C22 N21 Fe1 124.7(2) . . ? C26 N21 Fe1 116.13(19) . . ? N21 C22 C23 122.6(3) . . ? C24 C23 C22 118.9(3) . . ? C23 C24 C25 119.4(3) . . ? C24 C25 C26 118.4(3) . . ? N21 C26 C25 122.9(3) . . ? N21 C26 C27 115.0(2) . . ? C25 C26 C27 122.1(3) . . ? N28 C27 C26 118.5(3) . . ? C27 N28 C29 119.8(2) . . ? C27 N28 Fe1 115.7(2) . . ? C29 N28 Fe1 124.46(17) . . ? C34 C29 C30 120.6(3) . . ? C34 C29 N28 119.4(2) . . ? C30 C29 N28 119.7(3) . . ? C31 C30 C29 119.3(3) . . ? C32 C31 C30 121.1(3) . . ? C33 C32 C31 117.8(3) . . ? C32 C33 C34 123.4(3) . . ? C32 C33 N35 118.8(3) . . ? C34 C33 N35 117.8(3) . . ? C33 C34 C29 117.9(3) . . ? O37 N35 O36 123.5(3) . . ? O37 N35 C33 118.0(3) . . ? O36 N35 C33 118.5(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.438 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.067 #===END data_CCDC770797 _database_code_depnum_ccdc_archive 'CCDC 770797' #TrackingRef '- CCDC668788 and CCDC770797.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 Cl2 Mn N6 O4, 0.5(H2 O)' _chemical_formula_sum 'C24 H19 Cl2 Mn N6 O4.50' _chemical_formula_weight 589.29 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5083(3) _cell_length_b 14.1086(4) _cell_length_c 15.2964(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.822(3) _cell_angle_gamma 90.00 _cell_volume 2488.10(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 38606 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 31.51 _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9109 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details 'SADABS 2006/1, Bruker AXS (2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '676 images at 1.0 deg. stepwise rotation in omega and phi, 90 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45198 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 31.53 _reflns_number_total 8287 _reflns_number_gt 6447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Collect Software' _computing_cell_refinement 'Bruker AXS Collect Software' _computing_data_reduction 'Bruker AXS Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0435P)^2^+2.2429P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8287 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.21123(2) 0.838345(19) 0.351979(19) 0.01895(7) Uani 1 1 d . . . Cl1 Cl 0.16979(6) 0.97896(4) 0.42742(4) 0.03970(13) Uani 1 1 d . . . Cl2 Cl 0.29992(4) 0.90154(3) 0.25059(3) 0.02462(9) Uani 1 1 d . . . N1 N 0.02119(13) 0.82497(10) 0.25340(11) 0.0186(3) Uani 1 1 d . . . C2 C -0.06119(16) 0.88877(13) 0.24555(14) 0.0232(3) Uani 1 1 d . . . H2 H -0.0399 0.9444 0.2834 0.028 Uiso 1 1 calc R . . C3 C -0.17698(16) 0.87737(14) 0.18431(15) 0.0261(4) Uani 1 1 d . . . H3 H -0.2327 0.9249 0.1799 0.031 Uiso 1 1 calc R . . C4 C -0.20927(16) 0.79605(14) 0.13034(14) 0.0260(4) Uani 1 1 d . . . H4 H -0.2874 0.7869 0.0877 0.031 Uiso 1 1 calc R . . C5 C -0.12545(16) 0.72750(13) 0.13947(14) 0.0240(4) Uani 1 1 d . . . H5 H -0.1457 0.6699 0.1048 0.029 Uiso 1 1 calc R . . C6 C -0.01151(15) 0.74519(12) 0.20048(12) 0.0184(3) Uani 1 1 d . . . C7 C 0.08004(15) 0.67666(12) 0.20797(13) 0.0197(3) Uani 1 1 d . . . H7 H 0.0608 0.6202 0.1713 0.024 Uiso 1 1 calc R . . N8 N 0.18564(12) 0.69227(10) 0.26353(11) 0.0186(3) Uani 1 1 d . . . C9 C 0.27326(15) 0.62768(12) 0.26396(13) 0.0193(3) Uani 1 1 d . . . C10 C 0.37112(15) 0.61969(12) 0.34788(13) 0.0201(3) Uani 1 1 d . . . H10 H 0.3778 0.6559 0.4021 0.024 Uiso 1 1 calc R . . C11 C 0.45843(15) 0.55791(13) 0.35069(13) 0.0210(3) Uani 1 1 d . . . C12 C 0.45394(16) 0.50466(13) 0.27294(14) 0.0242(4) Uani 1 1 d . . . H12 H 0.5151 0.4628 0.2769 0.029 Uiso 1 1 calc R . . C13 C 0.35682(17) 0.51478(13) 0.18913(14) 0.0246(4) Uani 1 1 d . . . H13 H 0.3517 0.4797 0.1347 0.029 Uiso 1 1 calc R . . C14 C 0.26684(16) 0.57567(13) 0.18386(13) 0.0220(3) Uani 1 1 d . . . H14 H 0.2011 0.5820 0.1260 0.026 Uiso 1 1 calc R . . N15 N 0.56046(13) 0.54948(11) 0.44035(12) 0.0235(3) Uani 1 1 d . . . O16 O 0.56243(11) 0.59738(10) 0.50810(10) 0.0268(3) Uani 1 1 d . . . O17 O 0.63789(12) 0.49391(11) 0.44384(11) 0.0325(3) Uani 1 1 d . . . N21 N 0.38277(14) 0.81974(11) 0.47913(11) 0.0232(3) Uani 1 1 d . . . C22 C 0.47836(17) 0.87027(14) 0.49141(15) 0.0282(4) Uani 1 1 d . . . H22 H 0.4831 0.9022 0.4383 0.034 Uiso 1 1 calc R . . C23 C 0.57109(17) 0.87784(15) 0.57887(16) 0.0325(4) Uani 1 1 d . . . H23 H 0.6368 0.9154 0.5856 0.039 Uiso 1 1 calc R . . C24 C 0.56568(18) 0.82987(17) 0.65533(16) 0.0348(5) Uani 1 1 d . . . H24 H 0.6277 0.8344 0.7157 0.042 Uiso 1 1 calc R . . C25 C 0.46847(18) 0.77450(15) 0.64374(14) 0.0291(4) Uani 1 1 d . . . H25 H 0.4641 0.7392 0.6951 0.035 Uiso 1 1 calc R . . C26 C 0.37847(16) 0.77264(13) 0.55487(13) 0.0221(3) Uani 1 1 d . . . C27 C 0.26935(17) 0.72139(13) 0.53812(13) 0.0231(3) Uani 1 1 d . . . H27 H 0.2637 0.6788 0.5843 0.028 Uiso 1 1 calc R . . N28 N 0.18260(13) 0.73554(11) 0.46014(11) 0.0212(3) Uani 1 1 d . . . C29 C 0.07638(16) 0.68635(12) 0.44100(12) 0.0205(3) Uani 1 1 d . . . C30 C -0.02062(16) 0.73880(12) 0.43466(13) 0.0218(3) Uani 1 1 d . . . H30 H -0.0151 0.8048 0.4479 0.026 Uiso 1 1 calc R . . C31 C -0.12566(16) 0.69126(13) 0.40838(13) 0.0222(3) Uani 1 1 d . . . C32 C -0.13897(17) 0.59567(14) 0.38603(14) 0.0254(4) Uani 1 1 d . . . H32 H -0.2125 0.5657 0.3672 0.030 Uiso 1 1 calc R . . C33 C -0.04072(18) 0.54509(13) 0.39211(15) 0.0279(4) Uani 1 1 d . . . H33 H -0.0472 0.4795 0.3769 0.033 Uiso 1 1 calc R . . C34 C 0.06692(17) 0.58951(13) 0.42026(14) 0.0246(4) Uani 1 1 d . . . H34 H 0.1337 0.5541 0.4253 0.030 Uiso 1 1 calc R . . N35 N -0.22859(15) 0.74650(13) 0.40196(12) 0.0276(3) Uani 1 1 d . . . O36 O -0.21788(16) 0.83220(12) 0.41416(14) 0.0437(4) Uani 1 1 d . . . O37 O -0.32031(13) 0.70394(13) 0.38562(12) 0.0378(4) Uani 1 1 d . . . O40 O 0.0145(6) 0.9503(5) 0.5231(6) 0.115(2) Uani 0.50 1 d P . . 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 0.01870(12) 0.01866(12) 0.01743(13) 0.00074(9) 0.00474(9) -0.00408(9) Cl1 0.0552(3) 0.0253(2) 0.0315(3) -0.01019(19) 0.0090(2) 0.0001(2) Cl2 0.0243(2) 0.0274(2) 0.0239(2) 0.00160(16) 0.01125(16) -0.00517(16) N1 0.0195(6) 0.0173(6) 0.0188(7) 0.0000(5) 0.0073(5) -0.0006(5) C2 0.0238(8) 0.0200(8) 0.0266(9) -0.0006(7) 0.0107(7) 0.0018(6) C3 0.0211(8) 0.0250(9) 0.0317(10) 0.0046(7) 0.0096(7) 0.0053(7) C4 0.0170(8) 0.0281(9) 0.0282(9) 0.0033(7) 0.0035(7) -0.0003(7) C5 0.0205(8) 0.0222(8) 0.0253(9) -0.0001(7) 0.0044(7) -0.0008(6) C6 0.0197(7) 0.0170(7) 0.0178(8) 0.0009(6) 0.0066(6) -0.0003(6) C7 0.0216(8) 0.0164(7) 0.0208(8) -0.0006(6) 0.0079(6) 0.0002(6) N8 0.0190(6) 0.0167(6) 0.0207(7) 0.0020(5) 0.0085(5) 0.0013(5) C9 0.0203(7) 0.0168(7) 0.0223(8) 0.0014(6) 0.0100(6) 0.0007(6) C10 0.0206(8) 0.0195(7) 0.0220(8) -0.0004(6) 0.0104(6) -0.0002(6) C11 0.0164(7) 0.0214(8) 0.0255(9) 0.0028(6) 0.0086(6) -0.0005(6) C12 0.0238(8) 0.0214(8) 0.0320(10) 0.0010(7) 0.0159(7) 0.0034(6) C13 0.0273(9) 0.0237(8) 0.0264(9) -0.0029(7) 0.0145(7) 0.0007(7) C14 0.0232(8) 0.0218(8) 0.0218(8) 0.0006(6) 0.0096(7) -0.0002(6) N15 0.0164(6) 0.0251(7) 0.0295(8) 0.0037(6) 0.0094(6) -0.0004(5) O16 0.0214(6) 0.0290(7) 0.0271(7) -0.0019(5) 0.0063(5) -0.0037(5) O17 0.0212(6) 0.0378(8) 0.0393(8) 0.0067(6) 0.0127(6) 0.0094(6) N21 0.0224(7) 0.0208(7) 0.0218(7) -0.0009(6) 0.0037(6) -0.0030(5) C22 0.0221(9) 0.0255(9) 0.0312(10) -0.0001(7) 0.0040(8) -0.0046(7) C23 0.0211(9) 0.0295(10) 0.0386(12) -0.0068(8) 0.0023(8) -0.0010(7) C24 0.0231(9) 0.0422(12) 0.0286(10) -0.0103(9) -0.0014(8) 0.0074(8) C25 0.0289(9) 0.0341(10) 0.0200(9) -0.0016(7) 0.0048(7) 0.0087(8) C26 0.0240(8) 0.0209(8) 0.0185(8) -0.0020(6) 0.0050(7) 0.0044(6) C27 0.0313(9) 0.0198(8) 0.0195(8) 0.0005(6) 0.0113(7) 0.0018(7) N28 0.0243(7) 0.0189(7) 0.0202(7) -0.0009(5) 0.0085(6) -0.0033(5) C29 0.0252(8) 0.0191(7) 0.0186(8) 0.0011(6) 0.0100(7) -0.0027(6) C30 0.0294(9) 0.0176(7) 0.0193(8) 0.0008(6) 0.0105(7) -0.0004(6) C31 0.0257(8) 0.0232(8) 0.0198(8) 0.0019(6) 0.0110(7) 0.0023(7) C32 0.0265(9) 0.0242(8) 0.0272(9) -0.0007(7) 0.0124(7) -0.0038(7) C33 0.0330(10) 0.0188(8) 0.0359(11) -0.0028(7) 0.0179(8) -0.0035(7) C34 0.0269(9) 0.0197(8) 0.0306(9) 0.0011(7) 0.0149(8) -0.0005(7) N35 0.0289(8) 0.0312(8) 0.0224(8) 0.0036(6) 0.0097(7) 0.0049(7) O36 0.0421(9) 0.0297(8) 0.0576(11) -0.0004(7) 0.0173(8) 0.0111(7) O37 0.0280(7) 0.0441(9) 0.0455(9) 0.0022(7) 0.0187(7) 0.0029(7) O40 0.100(5) 0.110(5) 0.144(6) 0.037(5) 0.055(5) 0.017(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 Mn1 N1 2.2759(15) . ? Mn1 N21 2.2843(16) . ? Mn1 N28 2.3300(15) . ? Mn1 Cl2 2.4012(5) . ? Mn1 N8 2.4176(15) . ? Mn1 Cl1 2.4496(6) . ? N1 C2 1.338(2) . ? N1 C6 1.354(2) . ? C2 C3 1.396(3) . ? C2 H2 0.9500 . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? C4 C5 1.393(3) . ? C4 H4 0.9500 . ? C5 C6 1.390(2) . ? C5 H5 0.9500 . ? C6 C7 1.469(2) . ? C7 N8 1.282(2) . ? C7 H7 0.9500 . ? N8 C9 1.423(2) . ? C9 C10 1.393(3) . ? C9 C14 1.403(3) . ? C10 C11 1.385(2) . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 N15 1.472(2) . ? C12 C13 1.390(3) . ? C12 H12 0.9500 . ? C13 C14 1.393(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? N15 O16 1.229(2) . ? N15 O17 1.231(2) . ? N21 C22 1.341(2) . ? N21 C26 1.355(2) . ? C22 C23 1.394(3) . ? C22 H22 0.9500 . ? C23 C24 1.375(3) . ? C23 H23 0.9500 . ? C24 C25 1.397(3) . ? C24 H24 0.9500 . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 C27 1.477(3) . ? C27 N28 1.279(2) . ? C27 H27 0.9500 . ? N28 C29 1.425(2) . ? C29 C30 1.392(3) . ? C29 C34 1.397(2) . ? C30 C31 1.388(3) . ? C30 H30 0.9500 . ? C31 C32 1.385(3) . ? C31 N35 1.475(2) . ? C32 C33 1.393(3) . ? C32 H32 0.9500 . ? C33 C34 1.393(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? N35 O36 1.223(2) . ? N35 O37 1.232(2) . ? O40 O40 1.550(13) 3_576 ? 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 N1 Mn1 N21 161.68(6) . . ? N1 Mn1 N28 90.58(5) . . ? N21 Mn1 N28 71.11(6) . . ? N1 Mn1 Cl2 103.20(4) . . ? N21 Mn1 Cl2 94.36(4) . . ? N28 Mn1 Cl2 157.90(4) . . ? N1 Mn1 N8 71.39(5) . . ? N21 Mn1 N8 104.79(5) . . ? N28 Mn1 N8 80.98(5) . . ? Cl2 Mn1 N8 87.08(4) . . ? N1 Mn1 Cl1 91.25(4) . . ? N21 Mn1 Cl1 89.57(4) . . ? N28 Mn1 Cl1 92.91(4) . . ? Cl2 Mn1 Cl1 103.82(2) . . ? N8 Mn1 Cl1 161.41(4) . . ? C2 N1 C6 117.52(15) . . ? C2 N1 Mn1 125.01(12) . . ? C6 N1 Mn1 117.44(11) . . ? N1 C2 C3 123.03(17) . . ? N1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C4 C3 C2 118.97(17) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.90(17) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 118.58(17) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? N1 C6 C5 122.95(16) . . ? N1 C6 C7 117.07(15) . . ? C5 C6 C7 119.96(16) . . ? N8 C7 C6 120.68(15) . . ? N8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 N8 C9 119.11(15) . . ? C7 N8 Mn1 113.32(11) . . ? C9 N8 Mn1 127.49(11) . . ? C10 C9 C14 119.64(16) . . ? C10 C9 N8 117.13(15) . . ? C14 C9 N8 123.19(16) . . ? C11 C10 C9 118.69(16) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 122.97(17) . . ? C10 C11 N15 117.92(16) . . ? C12 C11 N15 119.11(16) . . ? C11 C12 C13 117.69(16) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C12 C13 C14 120.94(17) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C9 120.04(17) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? O16 N15 O17 123.74(16) . . ? O16 N15 C11 117.88(15) . . ? O17 N15 C11 118.37(16) . . ? C22 N21 C26 118.03(16) . . ? C22 N21 Mn1 123.37(13) . . ? C26 N21 Mn1 116.67(12) . . ? N21 C22 C23 122.7(2) . . ? N21 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C24 C23 C22 118.8(2) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 119.65(19) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 118.0(2) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? N21 C26 C25 122.81(18) . . ? N21 C26 C27 115.63(16) . . ? C25 C26 C27 121.52(18) . . ? N28 C27 C26 118.56(16) . . ? N28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C27 N28 C29 120.11(16) . . ? C27 N28 Mn1 116.80(12) . . ? C29 N28 Mn1 123.04(11) . . ? C30 C29 C34 120.61(17) . . ? C30 C29 N28 118.25(16) . . ? C34 C29 N28 120.87(16) . . ? C31 C30 C29 117.69(16) . . ? C31 C30 H30 121.2 . . ? C29 C30 H30 121.2 . . ? C32 C31 C30 123.46(17) . . ? C32 C31 N35 118.66(17) . . ? C30 C31 N35 117.87(16) . . ? C31 C32 C33 117.63(17) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C32 C33 C34 120.81(18) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C33 C34 C29 119.78(18) . . ? C33 C34 H34 120.1 . . ? C29 C34 H34 120.1 . . ? O36 N35 O37 123.46(19) . . ? O36 N35 C31 118.10(18) . . ? O37 N35 C31 118.44(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.103 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.077 #===END