Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Schroder, Martin' 'Blake, A.' 'Tei, Lorenzo' 'Wilson, Claire' _publ_contact_author_name 'Prof Martin Schroder' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'M.Schroder@nottingham.ac.uk' _publ_section_title ; Synthesis of asymmetric derivatives of 1,4,7-triazacyclononane and trigonal prismatic Mn(II) complexes ; data_MNNOAM _database_code_CSD 173798 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H30 Cl Mn N5 O7' _chemical_formula_weight 458.81 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' 'Mn' 'Mn' 0.3368 0.7283 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7577(9) _cell_length_b 14.199(2) _cell_length_c 15.771(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.543(2) _cell_angle_gamma 90.00 _cell_volume 1959.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5810 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.67 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.737 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS' _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 area detector' _diffrn_measurement_method 'omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18071 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.00 _reflns_number_total 4742 _reflns_number_gt 3565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'DeltaF synthesis for MeOH H, others placed geometrically' _refine_ls_hydrogen_treatment 'rotating rigid body for MeOH, others riding on parent atom' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4742 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.012 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.65535(3) 0.355231(19) 0.052724(19) 0.01621(9) Uani 1 1 d . . . N1 N 0.8433(2) 0.25497(12) 0.00989(11) 0.0224(4) Uani 1 1 d . . . C2 C 0.7926(3) 0.15992(14) 0.03653(15) 0.0276(5) Uani 1 1 d . . . H2A H 0.8730 0.1133 0.0247 0.033 Uiso 1 1 calc R . . H2B H 0.6989 0.1422 0.0029 0.033 Uiso 1 1 calc R . . C3 C 0.7605(3) 0.15719(14) 0.13046(14) 0.0263(5) Uani 1 1 d . . . H3A H 0.7102 0.0969 0.1437 0.032 Uiso 1 1 calc R . . H3B H 0.8583 0.1604 0.1643 0.032 Uiso 1 1 calc R . . N4 N 0.66093(19) 0.23652(11) 0.15447(11) 0.0222(4) Uani 1 1 d . . . C5 C 0.7196(3) 0.28438(15) 0.23313(13) 0.0261(5) Uani 1 1 d . . . H5A H 0.7333 0.2373 0.2792 0.031 Uiso 1 1 calc R . . H5B H 0.6434 0.3312 0.2508 0.031 Uiso 1 1 calc R . . C6 C 0.8705(3) 0.33367(15) 0.22052(14) 0.0262(5) Uani 1 1 d . . . H6A H 0.8979 0.3728 0.2709 0.031 Uiso 1 1 calc R . . H6B H 0.9520 0.2862 0.2143 0.031 Uiso 1 1 calc R . . N7 N 0.85944(19) 0.39427(11) 0.14360(11) 0.0209(4) Uani 1 1 d . . . C8 C 0.9895(2) 0.38092(15) 0.08743(15) 0.0268(5) Uani 1 1 d . . . H8A H 1.0864 0.3932 0.1202 0.032 Uiso 1 1 calc R . . H8B H 0.9811 0.4271 0.0405 0.032 Uiso 1 1 calc R . . C9 C 0.9935(2) 0.28181(15) 0.05050(14) 0.0261(5) Uani 1 1 d . . . H9A H 1.0730 0.2786 0.0079 0.031 Uiso 1 1 calc R . . H9B H 1.0212 0.2364 0.0963 0.031 Uiso 1 1 calc R . . C1A C 0.8473(3) 0.26263(16) -0.08366(14) 0.0275(5) Uani 1 1 d . . . H1A1 H 0.9029 0.2079 -0.1060 0.033 Uiso 1 1 calc R . . H1A2 H 0.9035 0.3204 -0.0985 0.033 Uiso 1 1 calc R . . C2A C 0.6872(3) 0.26599(15) -0.12503(14) 0.0286(5) Uani 1 1 d . . . H2A1 H 0.6931 0.2778 -0.1867 0.034 Uiso 1 1 calc R . . H2A2 H 0.6354 0.2048 -0.1174 0.034 Uiso 1 1 calc R . . N3A N 0.5995(2) 0.34166(12) -0.08586(11) 0.0264(4) Uani 1 1 d . . . H3A1 H 0.4967 0.3295 -0.0942 0.032 Uiso 1 1 calc R . . H3A2 H 0.6199 0.3978 -0.1121 0.032 Uiso 1 1 calc R . . C1B C 0.5009(2) 0.20478(14) 0.16100(15) 0.0278(5) Uani 1 1 d . . . H1B1 H 0.4925 0.1669 0.2133 0.033 Uiso 1 1 calc R . . H1B2 H 0.4726 0.1639 0.1119 0.033 Uiso 1 1 calc R . . C2B C 0.3907(2) 0.28688(15) 0.16299(14) 0.0268(5) Uani 1 1 d . . . H2B1 H 0.2845 0.2632 0.1574 0.032 Uiso 1 1 calc R . . H2B2 H 0.4037 0.3199 0.2181 0.032 Uiso 1 1 calc R . . N3B N 0.4180(2) 0.35324(12) 0.09359(12) 0.0254(4) Uani 1 1 d . . . H3B1 H 0.3923 0.4129 0.1108 0.031 Uiso 1 1 calc R . . H3B2 H 0.3543 0.3379 0.0477 0.031 Uiso 1 1 calc R . . C1C C 0.8415(3) 0.49457(14) 0.16466(14) 0.0255(5) Uani 1 1 d . . . H1C1 H 0.9436 0.5225 0.1772 0.031 Uiso 1 1 calc R . . H1C2 H 0.7820 0.5001 0.2163 0.031 Uiso 1 1 calc R . . C2C C 0.7609(2) 0.54960(14) 0.09269(14) 0.0224(4) Uani 1 1 d . . . O3C O 0.76992(19) 0.63722(10) 0.09511(11) 0.0318(4) Uani 1 1 d . . . O4C O 0.68611(17) 0.50283(10) 0.03685(10) 0.0276(4) Uani 1 1 d . . . C1M C 0.7271(4) 0.89829(18) 0.04409(19) 0.0507(7) Uani 1 1 d . . . H1M1 H 0.6548 0.9508 0.0381 0.076 Uiso 1 1 calc R . . H1M2 H 0.7906 0.8961 -0.0055 0.076 Uiso 1 1 calc R . . H1M3 H 0.7924 0.9072 0.0955 0.076 Uiso 1 1 calc R . . O1M O 0.6458(2) 0.81327(13) 0.05007(13) 0.0473(5) Uani 1 1 d . . . H1M H 0.7064 0.7699 0.0650 0.071 Uiso 1 1 calc R . . Cl Cl -0.15565(7) -0.01720(4) 0.78886(4) 0.03258(15) Uani 1 1 d . . . O1 O -0.1456(2) -0.11207(11) 0.81816(12) 0.0418(4) Uani 1 1 d . . . O2 O -0.2380(2) -0.01251(13) 0.70949(12) 0.0539(5) Uani 1 1 d . . . O3 O -0.2318(5) 0.0379(2) 0.84581(17) 0.1419(17) Uani 1 1 d . . . O4 O -0.0088(3) 0.0175(2) 0.7777(3) 0.1497(18) 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 Mn1 0.01767(16) 0.01627(14) 0.01468(16) 0.00094(11) 0.00050(11) -0.00125(11) N1 0.0241(9) 0.0232(8) 0.0201(9) -0.0004(7) 0.0034(7) -0.0002(7) C2 0.0326(12) 0.0206(10) 0.0298(13) -0.0007(9) 0.0029(10) 0.0023(9) C3 0.0295(12) 0.0208(10) 0.0284(12) 0.0053(9) 0.0013(9) 0.0026(8) N4 0.0226(9) 0.0204(8) 0.0234(10) 0.0026(7) 0.0004(7) 0.0010(7) C5 0.0329(12) 0.0284(11) 0.0170(11) 0.0045(9) 0.0008(9) 0.0018(9) C6 0.0289(12) 0.0287(11) 0.0204(11) 0.0013(9) -0.0070(9) 0.0012(9) N7 0.0217(9) 0.0202(8) 0.0206(9) 0.0007(7) -0.0015(7) 0.0008(7) C8 0.0206(11) 0.0279(11) 0.0320(13) 0.0023(9) 0.0002(9) -0.0007(9) C9 0.0207(11) 0.0287(11) 0.0291(12) 0.0026(9) 0.0028(9) 0.0037(9) C1A 0.0293(12) 0.0321(11) 0.0217(11) -0.0021(9) 0.0070(9) 0.0008(9) C2A 0.0378(13) 0.0290(11) 0.0189(11) -0.0035(9) 0.0014(10) -0.0008(10) N3A 0.0266(10) 0.0301(10) 0.0224(10) 0.0008(7) -0.0002(8) 0.0009(8) C1B 0.0262(12) 0.0232(10) 0.0342(13) 0.0077(9) 0.0039(10) -0.0032(9) C2B 0.0252(11) 0.0278(11) 0.0276(12) 0.0033(9) 0.0042(9) -0.0020(9) N3B 0.0265(10) 0.0262(9) 0.0238(10) 0.0052(8) 0.0027(8) 0.0036(7) C1C 0.0289(12) 0.0238(10) 0.0234(12) -0.0049(9) -0.0041(9) -0.0017(9) C2C 0.0207(10) 0.0229(10) 0.0240(11) 0.0000(8) 0.0064(9) 0.0003(8) O3C 0.0389(9) 0.0190(7) 0.0377(10) -0.0019(7) 0.0032(8) -0.0009(6) O4C 0.0325(9) 0.0219(7) 0.0277(9) 0.0040(6) -0.0075(7) -0.0026(6) C1M 0.068(2) 0.0373(14) 0.0468(18) -0.0016(13) 0.0020(15) -0.0082(14) O1M 0.0485(12) 0.0381(10) 0.0550(13) 0.0062(9) -0.0015(10) -0.0018(8) Cl 0.0458(4) 0.0225(3) 0.0288(3) 0.0037(2) -0.0063(3) -0.0047(2) O1 0.0453(11) 0.0277(8) 0.0513(12) 0.0141(8) -0.0076(9) -0.0033(8) O2 0.0657(14) 0.0517(11) 0.0424(12) 0.0019(9) -0.0198(10) 0.0128(10) O3 0.305(5) 0.0699(17) 0.0532(17) -0.0114(14) 0.031(2) 0.076(2) O4 0.0611(17) 0.112(2) 0.269(5) 0.132(3) -0.061(2) -0.0485(17) _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 2.3000(17) . y Mn1 N4 2.3263(17) . y Mn1 N7 2.3084(17) . y Mn1 N3A 2.2268(18) . y Mn1 N3B 2.2037(18) . y Mn1 O4C 2.1292(14) . y N1 C1A 1.481(3) . ? N1 C9 1.487(3) . ? N1 C2 1.487(2) . ? C2 C3 1.521(3) . ? C3 N4 1.484(3) . ? N4 C1B 1.480(3) . ? N4 C5 1.486(3) . ? C5 C6 1.517(3) . ? C6 N7 1.487(3) . ? N7 C1C 1.472(2) . ? N7 C8 1.486(3) . ? C8 C9 1.524(3) . ? C1A C2A 1.521(3) . ? C2A N3A 1.473(3) . ? C1B C2B 1.515(3) . ? C2B N3B 1.472(3) . ? C1C C2C 1.525(3) . ? C2C O3C 1.247(2) . ? C2C O4C 1.262(2) . ? C1M O1M 1.407(3) . ? Cl O3 1.384(3) . ? Cl O4 1.396(3) . ? Cl O2 1.4183(19) . ? Cl O1 1.4256(16) . ? 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 N4 76.16(6) . . y N1 Mn1 N7 77.68(6) . . y N7 Mn1 N4 75.74(6) . . y O4C Mn1 N1 118.60(6) . . y N3B Mn1 N1 140.76(6) . . y N3A Mn1 N1 77.71(6) . . y O4C Mn1 N4 142.70(6) . . y N3B Mn1 N4 77.31(6) . . y N3A Mn1 N4 127.68(6) . . y O4C Mn1 N7 74.82(6) . . y N3B Mn1 N7 122.41(7) . . y N3A Mn1 N7 139.51(7) . . y N3B Mn1 N3A 96.71(7) . . y O4C Mn1 N3B 99.96(6) . . y O4C Mn1 N3A 89.61(6) . . y C1A N1 C9 110.51(17) . . ? C1A N1 C2 111.63(17) . . ? C9 N1 C2 112.34(17) . . ? C1A N1 Mn1 107.23(13) . . ? C9 N1 Mn1 110.23(12) . . ? C2 N1 Mn1 104.62(12) . . ? N1 C2 C3 111.65(17) . . ? N4 C3 C2 111.45(17) . . ? C1B N4 C3 110.82(16) . . ? C1B N4 C5 111.98(17) . . ? C3 N4 C5 112.03(17) . . ? C1B N4 Mn1 106.12(12) . . ? C3 N4 Mn1 111.63(12) . . ? C5 N4 Mn1 103.91(12) . . ? N4 C5 C6 111.86(17) . . ? N7 C6 C5 110.38(17) . . ? C1C N7 C8 110.49(16) . . ? C1C N7 C6 112.30(16) . . ? C8 N7 C6 112.87(16) . . ? C1C N7 Mn1 106.56(12) . . ? C8 N7 Mn1 101.07(12) . . ? C6 N7 Mn1 112.85(12) . . ? N7 C8 C9 112.15(17) . . ? N1 C9 C8 111.47(16) . . ? N1 C1A C2A 111.55(18) . . ? N3A C2A C1A 109.35(17) . . ? C2A N3A Mn1 112.26(13) . . ? N4 C1B C2B 111.91(17) . . ? N3B C2B C1B 110.67(17) . . ? C2B N3B Mn1 114.32(13) . . ? N7 C1C C2C 112.21(17) . . ? O3C C2C O4C 125.2(2) . . ? O3C C2C C1C 117.49(19) . . ? O4C C2C C1C 117.28(17) . . ? C2C O4C Mn1 120.01(13) . . ? O3 Cl O4 110.8(3) . . ? O3 Cl O2 107.78(18) . . ? O4 Cl O2 107.93(19) . . ? O3 Cl O1 110.39(15) . . ? O4 Cl O1 109.28(14) . . ? O2 Cl O1 110.62(11) . . ? 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 O4C Mn1 N1 C1A -66.10(14) . . . . ? N3B Mn1 N1 C1A 102.17(15) . . . . ? N3A Mn1 N1 C1A 16.63(13) . . . . ? N7 Mn1 N1 C1A -130.98(14) . . . . ? N4 Mn1 N1 C1A 150.90(14) . . . . ? O4C Mn1 N1 C9 54.25(14) . . . . ? N3B Mn1 N1 C9 -137.49(13) . . . . ? N3A Mn1 N1 C9 136.97(14) . . . . ? N7 Mn1 N1 C9 -10.63(13) . . . . ? N4 Mn1 N1 C9 -88.76(13) . . . . ? O4C Mn1 N1 C2 175.23(12) . . . . ? N3B Mn1 N1 C2 -16.50(18) . . . . ? N3A Mn1 N1 C2 -102.04(13) . . . . ? N7 Mn1 N1 C2 110.35(13) . . . . ? N4 Mn1 N1 C2 32.23(13) . . . . ? C1A N1 C2 C3 -169.58(18) . . . . ? C9 N1 C2 C3 65.6(2) . . . . ? Mn1 N1 C2 C3 -53.94(19) . . . . ? N1 C2 C3 N4 49.2(2) . . . . ? C2 C3 N4 C1B 100.8(2) . . . . ? C2 C3 N4 C5 -133.36(19) . . . . ? C2 C3 N4 Mn1 -17.3(2) . . . . ? O4C Mn1 N4 C1B 111.38(14) . . . . ? N3B Mn1 N4 C1B 21.56(13) . . . . ? N3A Mn1 N4 C1B -67.14(15) . . . . ? N1 Mn1 N4 C1B -129.27(14) . . . . ? N7 Mn1 N4 C1B 150.18(14) . . . . ? O4C Mn1 N4 C3 -127.78(14) . . . . ? N3B Mn1 N4 C3 142.40(14) . . . . ? N3A Mn1 N4 C3 53.70(16) . . . . ? N1 Mn1 N4 C3 -8.43(13) . . . . ? N7 Mn1 N4 C3 -88.98(14) . . . . ? O4C Mn1 N4 C5 -6.85(18) . . . . ? N3B Mn1 N4 C5 -96.67(13) . . . . ? N3A Mn1 N4 C5 174.63(12) . . . . ? N1 Mn1 N4 C5 112.49(13) . . . . ? N7 Mn1 N4 C5 31.94(12) . . . . ? C1B N4 C5 C6 -168.66(16) . . . . ? C3 N4 C5 C6 66.1(2) . . . . ? Mn1 N4 C5 C6 -54.55(18) . . . . ? N4 C5 C6 N7 50.5(2) . . . . ? C5 C6 N7 C1C 102.1(2) . . . . ? C5 C6 N7 C8 -132.16(18) . . . . ? C5 C6 N7 Mn1 -18.3(2) . . . . ? O4C Mn1 N7 C1C 25.40(13) . . . . ? N3B Mn1 N7 C1C -66.89(15) . . . . ? N3A Mn1 N7 C1C 96.21(15) . . . . ? N1 Mn1 N7 C1C 149.95(14) . . . . ? N4 Mn1 N7 C1C -131.43(14) . . . . ? O4C Mn1 N7 C8 -90.08(12) . . . . ? N3B Mn1 N7 C8 177.63(11) . . . . ? N3A Mn1 N7 C8 -19.27(16) . . . . ? N1 Mn1 N7 C8 34.46(11) . . . . ? N4 Mn1 N7 C8 113.09(12) . . . . ? O4C Mn1 N7 C6 149.11(14) . . . . ? N3B Mn1 N7 C6 56.82(15) . . . . ? N3A Mn1 N7 C6 -140.08(13) . . . . ? N1 Mn1 N7 C6 -86.35(14) . . . . ? N4 Mn1 N7 C6 -7.72(13) . . . . ? C1C N7 C8 C9 -169.09(17) . . . . ? C6 N7 C8 C9 64.2(2) . . . . ? Mn1 N7 C8 C9 -56.56(18) . . . . ? C1A N1 C9 C8 102.4(2) . . . . ? C2 N1 C9 C8 -132.24(19) . . . . ? Mn1 N1 C9 C8 -16.0(2) . . . . ? N7 C8 C9 N1 51.6(2) . . . . ? C9 N1 C1A C2A -162.16(17) . . . . ? C2 N1 C1A C2A 72.0(2) . . . . ? Mn1 N1 C1A C2A -41.99(19) . . . . ? N1 C1A C2A N3A 53.5(2) . . . . ? C1A C2A N3A Mn1 -36.5(2) . . . . ? O4C Mn1 N3A C2A 130.44(14) . . . . ? N3B Mn1 N3A C2A -129.58(14) . . . . ? N1 Mn1 N3A C2A 11.00(14) . . . . ? N7 Mn1 N3A C2A 64.73(17) . . . . ? N4 Mn1 N3A C2A -50.46(17) . . . . ? C3 N4 C1B C2B -165.37(18) . . . . ? C5 N4 C1B C2B 68.7(2) . . . . ? Mn1 N4 C1B C2B -44.0(2) . . . . ? N4 C1B C2B N3B 49.5(3) . . . . ? C1B C2B N3B Mn1 -28.2(2) . . . . ? O4C Mn1 N3B C2B -138.48(14) . . . . ? N3A Mn1 N3B C2B 130.74(14) . . . . ? N1 Mn1 N3B C2B 51.97(19) . . . . ? N7 Mn1 N3B C2B -60.22(16) . . . . ? N4 Mn1 N3B C2B 3.55(14) . . . . ? C8 N7 C1C C2C 78.8(2) . . . . ? C6 N7 C1C C2C -154.24(17) . . . . ? Mn1 N7 C1C C2C -30.2(2) . . . . ? N7 C1C C2C O3C -164.16(18) . . . . ? N7 C1C C2C O4C 18.1(3) . . . . ? O3C C2C O4C Mn1 -170.67(16) . . . . ? C1C C2C O4C Mn1 6.9(2) . . . . ? N3B Mn1 O4C C2C 102.38(16) . . . . ? N3A Mn1 O4C C2C -160.87(16) . . . . ? N1 Mn1 O4C C2C -85.12(17) . . . . ? N7 Mn1 O4C C2C -18.69(15) . . . . ? N4 Mn1 O4C C2C 20.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.661 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.067 data_MN3DAM _database_code_CSD 173799 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H25 Mn N7 O6' _chemical_formula_weight 394.31 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' 'Mn' 'Mn' 0.3368 0.7283 '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) 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 7.8382(7) _cell_length_b 14.3920(10) _cell_length_c 14.6130(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1648.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5495 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 28.70 _exptl_crystal_description 'column' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.436 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS' _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 area detector' _diffrn_measurement_method 'omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10415 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.84 _reflns_number_total 3918 _reflns_number_gt 3533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier map' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _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 0.008(15) _refine_ls_number_reflns 3918 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.89395(4) 0.96398(2) 0.057176(19) 0.01850(9) Uani 1 1 d . . . N1 N 1.1156(3) 0.89015(11) 0.13650(11) 0.0198(4) Uani 1 1 d . . . C2 C 1.2724(3) 0.94765(15) 0.14387(15) 0.0233(5) Uani 1 1 d . . . H2A H 1.3553 0.9281 0.0965 0.028 Uiso 1 1 calc R . . H2B H 1.3255 0.9379 0.2046 0.028 Uiso 1 1 calc R . . C3 C 1.2307(3) 1.04991(15) 0.13154(14) 0.0239(5) Uani 1 1 d . . . H3A H 1.1628 1.0718 0.1844 0.029 Uiso 1 1 calc R . . H3B H 1.3379 1.0862 0.1297 0.029 Uiso 1 1 calc R . . N4 N 1.1333(2) 1.06600(12) 0.04605(11) 0.0223(4) Uani 1 1 d . . . C5 C 1.2354(3) 1.04271(16) -0.03603(14) 0.0275(5) Uani 1 1 d . . . H5A H 1.3396 1.0089 -0.0171 0.033 Uiso 1 1 calc R . . H5B H 1.2710 1.1008 -0.0669 0.033 Uiso 1 1 calc R . . C6 C 1.1347(3) 0.98325(15) -0.10248(14) 0.0256(5) Uani 1 1 d . . . H6A H 1.0454 1.0217 -0.1319 0.031 Uiso 1 1 calc R . . H6B H 1.2119 0.9602 -0.1510 0.031 Uiso 1 1 calc R . . N7 N 1.0532(2) 0.90274(12) -0.05558(12) 0.0215(4) Uani 1 1 d . . . H7 H 0.9807 0.8735 -0.0969 0.026 Uiso 1 1 calc R . . C8 C 1.1772(3) 0.83284(15) -0.02079(14) 0.0249(5) Uani 1 1 d . . . H8A H 1.2942 0.8584 -0.0253 0.030 Uiso 1 1 calc R . . H8B H 1.1716 0.7764 -0.0594 0.030 Uiso 1 1 calc R . . C9 C 1.1404(3) 0.80665(14) 0.07851(14) 0.0235(5) Uani 1 1 d . . . H9A H 1.0365 0.7676 0.0810 0.028 Uiso 1 1 calc R . . H9B H 1.2367 0.7696 0.1029 0.028 Uiso 1 1 calc R . . C1A C 1.0532(3) 0.86466(15) 0.22883(14) 0.0257(5) Uani 1 1 d . . . H1A1 H 1.0655 0.9188 0.2701 0.031 Uiso 1 1 calc R . . H1A2 H 1.1248 0.8138 0.2535 0.031 Uiso 1 1 calc R . . C2A C 0.8704(3) 0.83415(15) 0.22812(14) 0.0281(5) Uani 1 1 d . . . H2A1 H 0.8587 0.7752 0.1937 0.034 Uiso 1 1 calc R . . H2A2 H 0.8302 0.8237 0.2915 0.034 Uiso 1 1 calc R . . N3A N 0.7669(3) 0.90820(14) 0.18386(12) 0.0275(4) Uani 1 1 d . . . H3A1 H 0.7504 0.9560 0.2247 0.033 Uiso 1 1 calc R . . H3A2 H 0.6616 0.8846 0.1686 0.033 Uiso 1 1 calc R . . C1B C 1.0677(3) 1.16248(15) 0.04248(16) 0.0316(6) Uani 1 1 d . . . H1B1 H 1.0412 1.1790 -0.0217 0.038 Uiso 1 1 calc R . . H1B2 H 1.1568 1.2056 0.0648 0.038 Uiso 1 1 calc R . . C2B C 0.9096(4) 1.17351(15) 0.09995(16) 0.0308(5) Uani 1 1 d . . . H2B1 H 0.9384 1.1643 0.1653 0.037 Uiso 1 1 calc R . . H2B2 H 0.8636 1.2371 0.0925 0.037 Uiso 1 1 calc R . . N3B N 0.7799(3) 1.10504(13) 0.07185(13) 0.0317(5) Uani 1 1 d . . . H3B1 H 0.7327 1.1230 0.0170 0.038 Uiso 1 1 calc R . . H3B2 H 0.6942 1.1032 0.1148 0.038 Uiso 1 1 calc R . . N1N N 0.9644(3) 0.78430(14) -0.26134(13) 0.0274(4) Uani 1 1 d . . . O1 O 0.9156(3) 0.86680(11) -0.25458(12) 0.0373(4) Uani 1 1 d . . . O2 O 0.9928(2) 0.73863(12) -0.19002(12) 0.0352(4) Uani 1 1 d . . . O3 O 0.9855(3) 0.74921(15) -0.33773(13) 0.0565(6) Uani 1 1 d . . . N2N N 0.6394(2) 0.94738(13) -0.09645(12) 0.0245(4) Uani 1 1 d . . . O4 O 0.6599(2) 0.91063(11) -0.01739(10) 0.0261(4) Uani 1 1 d . . . O5 O 0.7248(2) 1.01761(11) -0.11658(11) 0.0343(4) Uani 1 1 d . . . O6 O 0.5357(2) 0.91327(13) -0.15054(11) 0.0332(4) 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 Mn 0.02275(16) 0.02011(14) 0.01265(14) -0.00112(12) 0.00042(12) 0.00175(13) N1 0.0249(9) 0.0201(8) 0.0144(8) 0.0003(6) -0.0014(8) 0.0004(8) C2 0.0256(11) 0.0265(12) 0.0179(10) -0.0010(8) -0.0040(8) 0.0004(9) C3 0.0270(12) 0.0249(12) 0.0198(11) -0.0021(8) -0.0006(8) -0.0038(9) N4 0.0324(10) 0.0210(8) 0.0136(8) 0.0004(6) 0.0007(8) -0.0014(7) C5 0.0352(12) 0.0278(11) 0.0195(11) 0.0005(9) 0.0057(9) -0.0052(10) C6 0.0314(13) 0.0305(12) 0.0148(10) 0.0006(8) 0.0041(9) 0.0012(9) N7 0.0256(9) 0.0242(8) 0.0146(8) -0.0022(7) 0.0004(8) 0.0000(7) C8 0.0283(11) 0.0262(11) 0.0203(10) -0.0047(9) 0.0018(9) 0.0019(9) C9 0.0278(12) 0.0201(9) 0.0225(11) -0.0019(8) -0.0019(8) 0.0018(9) C1A 0.0373(14) 0.0258(11) 0.0142(10) 0.0043(8) -0.0021(9) -0.0012(9) C2A 0.0380(14) 0.0300(11) 0.0163(10) 0.0032(8) 0.0024(10) -0.0029(11) N3A 0.0291(11) 0.0357(11) 0.0179(10) -0.0029(8) 0.0000(8) -0.0014(9) C1B 0.0519(16) 0.0200(10) 0.0228(11) 0.0018(8) -0.0007(10) -0.0012(10) C2B 0.0479(15) 0.0211(10) 0.0235(11) -0.0031(8) -0.0045(11) 0.0075(11) N3B 0.0394(12) 0.0300(10) 0.0256(11) -0.0080(8) -0.0029(9) 0.0102(9) N1N 0.0256(11) 0.0336(10) 0.0230(10) -0.0049(8) -0.0022(8) -0.0006(9) O1 0.0502(12) 0.0299(9) 0.0318(9) -0.0060(7) -0.0091(9) 0.0084(8) O2 0.0377(11) 0.0372(9) 0.0306(9) 0.0067(7) -0.0003(8) 0.0029(8) O3 0.0777(17) 0.0644(14) 0.0275(10) -0.0238(9) -0.0134(10) 0.0254(13) N2N 0.0263(11) 0.0276(10) 0.0195(9) -0.0016(7) 0.0004(7) 0.0054(8) O4 0.0317(9) 0.0319(8) 0.0148(7) 0.0022(6) -0.0029(6) -0.0012(7) O5 0.0446(11) 0.0320(10) 0.0264(9) 0.0051(7) 0.0006(8) -0.0073(8) O6 0.0301(9) 0.0450(10) 0.0246(9) -0.0039(7) -0.0095(7) 0.0014(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 Mn N1 2.3434(19) . y Mn N4 2.3879(19) . y Mn N7 2.2470(18) . y Mn N3A 2.2504(19) . y Mn N3B 2.2285(19) . y Mn O4 2.2676(16) . y N1 C1A 1.481(3) . ? N1 C9 1.483(3) . ? N1 C2 1.486(3) . ? C2 C3 1.518(3) . ? C3 N4 1.482(3) . ? N4 C5 1.480(3) . ? N4 C1B 1.482(3) . ? C5 C6 1.516(3) . ? C6 N7 1.490(3) . ? N7 C8 1.489(3) . ? C8 C9 1.527(3) . ? C1A C2A 1.499(4) . ? C2A N3A 1.487(3) . ? C1B C2B 1.505(4) . ? C2B N3B 1.474(3) . ? N1N O3 1.236(3) . ? N1N O1 1.251(3) . ? N1N O2 1.252(3) . ? N2N O6 1.236(2) . ? N2N O5 1.247(2) . ? N2N O4 1.281(2) . ? 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 Mn N4 74.33(6) . . y N7 Mn N1 76.88(6) . . y N7 Mn N4 75.81(6) . . y N3A Mn N1 76.08(7) . . y N3B Mn N1 131.52(7) . . y O4 Mn N1 133.15(6) . . y N3A Mn N4 128.55(6) . . y N3B Mn N4 76.21(7) . . y O4 Mn N4 144.20(6) . . y N7 Mn N3A 135.17(7) . . y N3B Mn N7 130.59(7) . . y N7 Mn O4 87.94(6) . . y N3B Mn N3A 93.91(7) . . y N3B Mn O4 91.73(7) . . y N3A Mn O4 85.20(6) . . y C1A N1 C9 111.29(16) . . ? C1A N1 C2 110.18(17) . . ? C9 N1 C2 112.60(18) . . ? C1A N1 Mn 108.55(14) . . ? C9 N1 Mn 100.49(12) . . ? C2 N1 Mn 113.36(12) . . ? N1 C2 C3 110.68(19) . . ? N4 C3 C2 111.24(17) . . ? C5 N4 C1B 111.80(17) . . ? C5 N4 C3 111.68(17) . . ? C1B N4 C3 110.79(17) . . ? C5 N4 Mn 109.91(13) . . ? C1B N4 Mn 107.80(14) . . ? C3 N4 Mn 104.54(12) . . ? N4 C5 C6 111.44(19) . . ? N7 C6 C5 111.57(17) . . ? C8 N7 C6 113.73(17) . . ? C8 N7 Mn 112.18(13) . . ? C6 N7 Mn 105.69(12) . . ? N7 C8 C9 111.59(18) . . ? N1 C9 C8 111.58(17) . . ? N1 C1A C2A 112.45(18) . . ? N3A C2A C1A 108.34(18) . . ? C2A N3A Mn 111.83(14) . . ? N4 C1B C2B 111.42(18) . . ? N3B C2B C1B 109.98(18) . . ? C2B N3B Mn 111.05(15) . . ? O3 N1N O1 120.0(2) . . ? O3 N1N O2 120.9(2) . . ? O1 N1N O2 119.13(19) . . ? O6 N2N O5 121.61(18) . . ? O6 N2N O4 119.71(18) . . ? O5 N2N O4 118.67(18) . . ? N2N O4 Mn 113.28(13) . . ? 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 N3B Mn N1 C1A 73.18(16) . . . . ? N7 Mn N1 C1A -153.50(14) . . . . ? N3A Mn N1 C1A -9.61(13) . . . . ? O4 Mn N1 C1A -79.10(14) . . . . ? N4 Mn N1 C1A 127.80(14) . . . . ? N3B Mn N1 C9 -169.97(12) . . . . ? N7 Mn N1 C9 -36.65(12) . . . . ? N3A Mn N1 C9 107.24(13) . . . . ? O4 Mn N1 C9 37.74(15) . . . . ? N4 Mn N1 C9 -115.35(13) . . . . ? N3B Mn N1 C2 -49.59(17) . . . . ? N7 Mn N1 C2 83.72(14) . . . . ? N3A Mn N1 C2 -132.39(14) . . . . ? O4 Mn N1 C2 158.12(12) . . . . ? N4 Mn N1 C2 5.03(13) . . . . ? C1A N1 C2 C3 -100.2(2) . . . . ? C9 N1 C2 C3 134.94(17) . . . . ? Mn N1 C2 C3 21.7(2) . . . . ? N1 C2 C3 N4 -52.7(2) . . . . ? C2 C3 N4 C5 -64.4(2) . . . . ? C2 C3 N4 C1B 170.22(19) . . . . ? C2 C3 N4 Mn 54.36(19) . . . . ? N3B Mn N4 C5 -129.61(15) . . . . ? N7 Mn N4 C5 9.25(13) . . . . ? N3A Mn N4 C5 146.46(14) . . . . ? O4 Mn N4 C5 -56.30(18) . . . . ? N1 Mn N4 C5 89.33(14) . . . . ? N3B Mn N4 C1B -7.53(13) . . . . ? N7 Mn N4 C1B 131.33(14) . . . . ? N3A Mn N4 C1B -91.46(15) . . . . ? O4 Mn N4 C1B 65.78(17) . . . . ? N1 Mn N4 C1B -148.59(14) . . . . ? N3B Mn N4 C3 110.39(14) . . . . ? N7 Mn N4 C3 -110.75(13) . . . . ? N3A Mn N4 C3 26.46(16) . . . . ? O4 Mn N4 C3 -176.29(12) . . . . ? N1 Mn N4 C3 -30.66(12) . . . . ? C1B N4 C5 C6 -102.7(2) . . . . ? C3 N4 C5 C6 132.5(2) . . . . ? Mn N4 C5 C6 17.0(2) . . . . ? N4 C5 C6 N7 -49.5(3) . . . . ? C5 C6 N7 C8 -67.5(2) . . . . ? C5 C6 N7 Mn 55.9(2) . . . . ? N3B Mn N7 C8 148.43(14) . . . . ? N3A Mn N7 C8 -39.95(18) . . . . ? O4 Mn N7 C8 -121.05(14) . . . . ? N1 Mn N7 C8 14.27(14) . . . . ? N4 Mn N7 C8 91.15(14) . . . . ? N3B Mn N7 C6 23.97(17) . . . . ? N3A Mn N7 C6 -164.41(13) . . . . ? O4 Mn N7 C6 114.49(13) . . . . ? N1 Mn N7 C6 -110.19(14) . . . . ? N4 Mn N7 C6 -33.31(13) . . . . ? C6 N7 C8 C9 131.32(19) . . . . ? Mn N7 C8 C9 11.4(2) . . . . ? C1A N1 C9 C8 170.97(19) . . . . ? C2 N1 C9 C8 -64.7(2) . . . . ? Mn N1 C9 C8 56.18(19) . . . . ? N7 C8 C9 N1 -48.5(2) . . . . ? C9 N1 C1A C2A -72.8(2) . . . . ? C2 N1 C1A C2A 161.55(18) . . . . ? Mn N1 C1A C2A 36.9(2) . . . . ? N1 C1A C2A N3A -54.2(2) . . . . ? C1A C2A N3A Mn 43.5(2) . . . . ? N3B Mn N3A C2A -150.27(15) . . . . ? N7 Mn N3A C2A 36.10(19) . . . . ? O4 Mn N3A C2A 118.31(15) . . . . ? N1 Mn N3A C2A -18.40(14) . . . . ? N4 Mn N3A C2A -74.81(16) . . . . ? C5 N4 C1B C2B 155.3(2) . . . . ? C3 N4 C1B C2B -79.4(2) . . . . ? Mn N4 C1B C2B 34.4(2) . . . . ? N4 C1B C2B N3B -55.0(3) . . . . ? C1B C2B N3B Mn 46.6(2) . . . . ? N7 Mn N3B C2B -77.76(17) . . . . ? N3A Mn N3B C2B 108.15(16) . . . . ? O4 Mn N3B C2B -166.54(15) . . . . ? N1 Mn N3B C2B 33.30(19) . . . . ? N4 Mn N3B C2B -20.63(14) . . . . ? O6 N2N O4 Mn 167.30(15) . . . . ? O5 N2N O4 Mn -13.1(2) . . . . ? N3B Mn O4 N2N 67.48(14) . . . . ? N7 Mn O4 N2N -63.09(13) . . . . ? N3A Mn O4 N2N 161.26(14) . . . . ? N1 Mn O4 N2N -132.91(13) . . . . ? N4 Mn O4 N2N -1.07(19) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.274 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.056