# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1749 #Structure and magnetic behaviour of #[{Mn2(3-Et,4-Mepy)6(m1,1-N3)2(m1,3-N3)}n][PF6]n #and [{Mn2(3-ampy)4(m1,1-N3)2(m1,3-N3)(N3)(H2O)}n][(H2O)4]n, #two alternating #ferro-antiferromagnetic one-dimensional compounds. #Morsy Abu Youssef,a Albert Escuer,b Mohamed Goher,c #Franz A. Mautnera and Ramon Vicente.b data_mam26d _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Mn2(3-Et,4-Me-pyridine)6(N3)3](PF6)' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H66 F6 Mn2 N15 P' _chemical_formula_weight 1108.01 _chemical_melting_point ? _chemical_compound_source ? 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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.988(3) _cell_length_b 10.924(4) _cell_length_c 15.272(5) _cell_angle_alpha 99.50(3) _cell_angle_beta 106.81(3) _cell_angle_gamma 98.56(3) _cell_volume 1384.7(8) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 9.1 _cell_measurement_theta_max 14.8 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 1.32(3) _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'suspension method' _exptl_crystal_F_000 578 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.402 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle diffractometer' _diffrn_measurement_method 'Omega-scan; delta Omega: 1.30 deg.' _diffrn_standards_number '3 (0 2 0; -1 -3 2; -1 -1 3)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 17 _diffrn_reflns_number 5466 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4873 _reflns_number_observed 4145 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 68 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+5.6443P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4805 _refine_ls_number_parameters 443 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_obs 0.0881 _refine_ls_wR_factor_all 0.2356 _refine_ls_wR_factor_obs 0.2222 _refine_ls_goodness_of_fit_all 1.173 _refine_ls_goodness_of_fit_obs 1.234 _refine_ls_restrained_S_all 1.198 _refine_ls_restrained_S_obs 1.231 _refine_ls_shift/esd_max 0.352 _refine_ls_shift/esd_mean 0.012 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.16197(11) 0.58025(9) 0.97839(7) 0.0508(3) Uani 1 d . . N11 N 0.3745(8) 0.5191(7) 0.9658(5) 0.080(2) Uani 1 d . . N12 N 0.5000 0.5000 1.0000 0.067(2) Uani 1 d S . N21 N 0.0694(6) 0.3925(5) 1.0079(4) 0.0555(13) Uani 1 d . . N22 N 0.1636(7) 0.3354(5) 1.0464(4) 0.0600(14) Uani 1 d . . N23 N 0.2540(9) 0.2816(7) 1.0844(6) 0.102(2) Uani 1 d . . N1 N 0.2341(7) 0.7766(6) 0.9501(4) 0.069(2) Uani 1 d . . C1 C 0.3320(9) 0.7925(7) 0.8996(5) 0.070(2) Uani 1 d . . H1 H 0.3799(9) 0.7255(7) 0.8853(5) 0.084 Uiso 1 calc R . C2 C 0.3678(9) 0.8995(7) 0.8669(5) 0.070(2) Uani 1 d . . C3 C 0.3010(10) 1.0019(7) 0.8914(6) 0.078(2) Uani 1 d . . C4 C 0.2028(11) 0.9874(7) 0.9451(7) 0.091(3) Uani 1 d . . H4 H 0.1584(11) 1.0546(7) 0.9639(7) 0.109 Uiso 1 calc R . C5 C 0.1698(10) 0.8754(7) 0.9709(6) 0.076(2) Uani 1 d . . H5 H 0.0991(10) 0.8675(7) 1.0046(6) 0.091 Uiso 1 calc R . C6 C 0.4742(11) 0.9009(10) 0.8063(7) 0.103(3) Uani 1 d . . H6A H 0.5325(11) 0.9869(10) 0.8162(7) 0.124 Uiso 1 calc R . H6B H 0.5508(11) 0.8485(10) 0.8249(7) 0.124 Uiso 1 calc R . C7 C 0.3828(16) 0.8538(15) 0.7059(8) 0.166(6) Uani 1 d . . H7A H 0.3411(93) 0.7643(22) 0.6938(14) 0.200 Uiso 1 calc R . H7B H 0.4511(31) 0.8694(82) 0.6691(8) 0.200 Uiso 1 calc R . H7C H 0.2967(68) 0.8971(63) 0.6894(17) 0.200 Uiso 1 calc R . C8 C 0.3345(14) 1.1249(8) 0.8592(8) 0.119(4) Uani 1 d . . H8A H 0.2581(49) 1.1749(29) 0.8671(44) 0.142 Uiso 1 calc R . H8B H 0.3272(79) 1.1056(8) 0.7942(14) 0.142 Uiso 1 calc R . H8C H 0.4395(32) 1.1718(31) 0.8958(32) 0.142 Uiso 1 calc R . N2 N 0.0498(25) 0.5301(23) 0.8191(20) 0.059(4) Uani 0.50 d PD 1 C9 C -0.0280(23) 0.6096(16) 0.7749(17) 0.061(5) Uani 0.50 d PD 1 H9 H -0.0271(23) 0.6881(16) 0.8098(17) 0.073 Uiso 0.50 calc PR 1 C10 C -0.1097(20) 0.5797(21) 0.6797(17) 0.088(9) Uani 0.50 d PD 1 C11 C -0.1126(20) 0.4636(22) 0.6267(18) 0.081(7) Uani 0.50 d PD 1 C12 C -0.0335(21) 0.3841(22) 0.6723(18) 0.089(7) Uani 0.50 d PD 1 H12 H -0.0327(21) 0.3050(22) 0.6390(18) 0.106 Uiso 0.50 calc PR 1 C13 C 0.0470(22) 0.4201(21) 0.7689(18) 0.073(7) Uani 0.50 d PD 1 H13 H 0.1003(22) 0.3638(21) 0.7984(18) 0.087 Uiso 0.50 calc PR 1 C14 C -0.1931(30) 0.6680(34) 0.6337(22) 0.104(9) Uani 0.50 d PD 1 H14A H -0.1399(30) 0.6951(34) 0.5911(22) 0.124 Uiso 0.50 calc PR 1 H14B H -0.2999(30) 0.6228(34) 0.5961(22) 0.124 Uiso 0.50 calc PR 1 C15 C -0.2042(49) 0.7758(36) 0.6924(22) 0.189(18) Uani 0.50 d P 1 H15A H -0.2782(200) 0.8185(119) 0.6569(40) 0.226 Uiso 0.50 calc PR 1 H15B H -0.1017(71) 0.8317(101) 0.7193(120) 0.226 Uiso 0.50 calc PR 1 H15C H -0.2405(256) 0.7514(40) 0.7416(93) 0.226 Uiso 0.50 calc PR 1 C16 C -0.1952(27) 0.4156(26) 0.5229(16) 0.119(9) Uani 0.50 d PD 1 H16A H -0.3025(60) 0.4279(132) 0.5074(23) 0.143 Uiso 0.50 calc PR 1 H16B H -0.1958(159) 0.3269(42) 0.5059(24) 0.143 Uiso 0.50 calc PR 1 H16C H -0.1398(106) 0.4615(101) 0.4893(17) 0.143 Uiso 0.50 calc PR 1 N32 N 0.0629(25) 0.5021(22) 0.8211(20) 0.059(4) Uani 0.50 d PD 2 C39 C -0.0403(25) 0.5578(15) 0.7667(18) 0.066(6) Uani 0.50 d PD 2 H39 H -0.0699(25) 0.6278(15) 0.7954(18) 0.079 Uiso 0.50 calc PR 2 C40 C -0.1053(23) 0.5162(21) 0.6699(19) 0.089(9) Uani 0.50 d PD 2 C41 C -0.0632(20) 0.4135(17) 0.6265(15) 0.070(6) Uani 0.50 d PD 2 C42 C 0.0414(20) 0.3564(17) 0.6812(15) 0.077(6) Uani 0.50 d PD 2 H42 H 0.0722(20) 0.2863(17) 0.6536(15) 0.092 Uiso 0.50 calc PR 2 C43 C 0.1026(23) 0.4028(20) 0.7783(18) 0.066(6) Uani 0.50 d PD 2 H43 H 0.1738(23) 0.3623(20) 0.8140(18) 0.079 Uiso 0.50 calc PR 2 C44 C -0.2191(38) 0.5850(28) 0.6159(27) 0.222(27) Uani 0.50 d PD 2 H44A H -0.1694(38) 0.6115(28) 0.5716(27) 0.266 Uiso 0.50 calc PR 2 H44B H -0.3098(38) 0.5179(28) 0.5786(27) 0.266 Uiso 0.50 calc PR 2 C45 C -0.2712(87) 0.6617(74) 0.6343(45) 0.349(57) Uani 0.50 d P 2 H45A H -0.3485(490) 0.6727(347) 0.5794(81) 0.419 Uiso 0.50 calc PR 2 H45B H -0.1903(141) 0.7378(113) 0.6608(352) 0.419 Uiso 0.50 calc PR 2 H45C H -0.3222(539) 0.6445(227) 0.6795(291) 0.419 Uiso 0.50 calc PR 2 C46 C -0.1258(27) 0.3577(21) 0.5204(16) 0.101(8) Uani 0.50 d PD 2 H46A H -0.1070(133) 0.4233(35) 0.4877(16) 0.121 Uiso 0.50 calc PR 2 H46B H -0.2378(42) 0.3233(105) 0.5015(21) 0.121 Uiso 0.50 calc PR 2 H46C H -0.0718(112) 0.2917(86) 0.5056(20) 0.121 Uiso 0.50 calc PR 2 N3 N 0.2807(7) 0.6609(6) 1.1360(4) 0.071(2) Uani 1 d . . C17 C 0.2353(10) 0.7580(8) 1.1802(5) 0.082(2) Uani 1 d . . H17 H 0.1514(10) 0.7888(8) 1.1457(5) 0.099 Uiso 1 calc R 1 C18 C 0.3066(11) 0.8149(9) 1.2745(6) 0.091(3) Uani 0.50 d P 1 H18 H 0.2734(11) 0.8837(9) 1.3019(6) 0.109 Uiso 0.50 calc PR 1 C19 C 0.4279(12) 0.7671(11) 1.3267(6) 0.102(3) Uani 1 d . . C20A C 0.4715(10) 0.6672(10) 1.2831(6) 0.091(3) Uani 0.50 d P 2 H20A H 0.5512(10) 0.6316(10) 1.3169(6) 0.109 Uiso 0.50 calc PR 2 C21 C 0.3968(10) 0.6174(9) 1.1874(6) 0.087(2) Uani 1 d . . H21 H 0.4308(10) 0.5501(9) 1.1585(6) 0.104 Uiso 1 calc R 1 C18A C 0.3066(11) 0.8149(9) 1.2745(6) 0.091(3) Uani 0.50 d P 2 C32 C 0.2620(27) 0.9079(20) 1.3190(14) 0.105(6) Uani 0.50 d P 2 H32A H 0.3540(27) 0.9761(20) 1.3514(14) 0.126 Uiso 0.50 calc PR 2 H32B H 0.2217(27) 0.8783(20) 1.3659(14) 0.126 Uiso 0.50 calc PR 2 C33 C 0.1401(34) 0.9578(19) 1.2577(18) 0.137(10) Uani 0.50 d P 2 H33A H 0.1213(135) 1.0317(87) 1.2930(30) 0.165 Uiso 0.50 calc PR 2 H33B H 0.0436(62) 0.8943(55) 1.2320(86) 0.165 Uiso 0.50 calc PR 2 H33C H 0.1753(83) 0.9802(136) 1.2076(63) 0.165 Uiso 0.50 calc PR 2 C24 C 0.5041(15) 0.8303(13) 1.4294(7) 0.158(6) Uani 1 d . 2 H24A H 0.4230(15) 0.8378(78) 1.4581(16) 0.190 Uiso 1 calc R 2 H24B H 0.5646(89) 0.9132(35) 1.4355(7) 0.190 Uiso 1 calc R 2 H24C H 0.5732(81) 0.7801(45) 1.4599(14) 0.190 Uiso 1 calc R 2 C20 C 0.4715(10) 0.6672(10) 1.2831(6) 0.091(3) Uani 0.50 d P 1 C22 C 0.5893(27) 0.6191(21) 1.3429(13) 0.118(8) Uani 0.50 d P 1 H22A H 0.5633(27) 0.6138(21) 1.3997(13) 0.142 Uiso 0.50 calc PR 1 H22B H 0.6906(27) 0.6778(21) 1.3604(13) 0.142 Uiso 0.50 calc PR 1 C23 C 0.6047(26) 0.4942(21) 1.2998(15) 0.120(7) Uani 0.50 d P 1 H23A H 0.6848(116) 0.4655(60) 1.3436(36) 0.144 Uiso 0.50 calc PR 1 H23B H 0.6345(155) 0.4994(33) 1.2448(55) 0.144 Uiso 0.50 calc PR 1 H23C H 0.5050(52) 0.4354(35) 1.2827(86) 0.144 Uiso 0.50 calc PR 1 P1 P 0.0155(13) -0.0225(9) 0.4884(7) 0.097(2) Uani 0.50 d PD -1 F1 F 0.1138(37) 0.0326(31) 0.5906(15) 0.179(6) Uani 0.50 d PD -1 F2 F 0.0564(81) 0.0958(22) 0.4533(25) 0.197(11) Uani 0.50 d PD -1 F3 F 0.1603(32) -0.0690(29) 0.4758(29) 0.188(6) Uani 0.50 d PD -1 F4 F -0.0811(37) -0.0880(30) 0.3879(15) 0.179(6) Uani 0.50 d PD -1 F5 F -0.0613(81) -0.1452(23) 0.5046(26) 0.197(11) Uani 0.50 d PD -1 F6 F -0.1303(33) 0.0245(30) 0.5008(29) 0.188(6) Uani 0.50 d PD -1 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 0.0495(5) 0.0528(6) 0.0519(6) 0.0115(4) 0.0177(4) 0.0131(4) N11 0.064(4) 0.102(5) 0.091(5) 0.043(4) 0.031(4) 0.033(4) N12 0.057(5) 0.074(5) 0.087(6) 0.032(5) 0.036(5) 0.019(4) N21 0.056(3) 0.059(3) 0.051(3) 0.012(2) 0.013(2) 0.019(3) N22 0.065(4) 0.050(3) 0.061(3) 0.005(3) 0.015(3) 0.019(3) N23 0.097(5) 0.085(5) 0.123(6) 0.030(5) 0.017(5) 0.046(4) N1 0.071(4) 0.063(4) 0.086(4) 0.025(3) 0.038(3) 0.015(3) C1 0.076(5) 0.070(5) 0.075(5) 0.028(4) 0.031(4) 0.019(4) C2 0.063(4) 0.073(5) 0.076(5) 0.024(4) 0.021(4) 0.009(4) C3 0.086(5) 0.056(4) 0.085(5) 0.023(4) 0.019(4) 0.001(4) C4 0.113(7) 0.053(4) 0.117(7) 0.013(4) 0.055(6) 0.019(4) C5 0.085(5) 0.060(4) 0.093(6) 0.017(4) 0.043(5) 0.016(4) C6 0.099(7) 0.116(8) 0.118(8) 0.068(7) 0.049(6) 0.019(6) C7 0.155(12) 0.258(18) 0.087(8) 0.048(10) 0.042(8) 0.026(12) C8 0.158(10) 0.064(5) 0.130(9) 0.041(6) 0.042(7) -0.002(6) N2 0.062(4) 0.059(10) 0.062(4) 0.025(6) 0.019(4) 0.018(5) C9 0.068(10) 0.047(12) 0.061(11) 0.013(10) 0.011(8) 0.011(9) C10 0.088(15) 0.111(20) 0.057(12) 0.048(14) 0.008(10) -0.004(13) C11 0.083(15) 0.090(20) 0.070(16) 0.017(15) 0.029(13) 0.014(13) C12 0.092(18) 0.076(16) 0.084(18) -0.008(14) 0.026(17) 0.009(12) C13 0.087(15) 0.053(12) 0.073(13) -0.008(10) 0.025(12) 0.025(10) C14 0.110(17) 0.127(24) 0.080(16) 0.050(19) 0.011(12) 0.049(18) C15 0.292(41) 0.262(40) 0.150(27) 0.146(29) 0.140(29) 0.228(38) C16 0.119(21) 0.149(25) 0.063(12) 0.017(16) 0.012(13) -0.008(17) N32 0.062(4) 0.059(10) 0.062(4) 0.025(6) 0.019(4) 0.018(5) C39 0.083(12) 0.049(13) 0.067(12) 0.010(11) 0.025(10) 0.018(11) C40 0.084(15) 0.106(26) 0.068(18) 0.036(18) 0.004(12) 0.020(14) C41 0.092(15) 0.068(13) 0.043(11) 0.004(9) 0.015(11) 0.017(10) C42 0.094(15) 0.060(10) 0.061(10) -0.009(8) 0.019(12) 0.009(10) C43 0.088(15) 0.049(9) 0.073(12) 0.015(8) 0.033(12) 0.034(10) C44 0.345(61) 0.196(38) 0.118(25) 0.036(28) -0.008(30) 0.202(44) C45 0.490(114) 0.413(101) 0.225(56) 0.120(59) 0.057(67) 0.402(103) C46 0.138(23) 0.090(15) 0.055(10) -0.004(10) 0.012(12) 0.023(13) N3 0.063(4) 0.076(4) 0.065(4) 0.017(3) 0.014(3) -0.003(3) C17 0.085(6) 0.087(6) 0.063(5) 0.003(4) 0.020(4) 0.004(4) C18 0.089(6) 0.097(7) 0.071(5) 0.000(5) 0.026(5) -0.008(5) C19 0.098(7) 0.115(8) 0.055(5) -0.004(5) 0.012(5) -0.037(6) C20A 0.077(5) 0.111(7) 0.063(5) 0.019(5) 0.004(4) -0.008(5) C21 0.081(5) 0.090(6) 0.067(5) 0.022(4) 0.004(4) -0.011(5) C18A 0.089(6) 0.097(7) 0.071(5) 0.000(5) 0.026(5) -0.008(5) C32 0.127(17) 0.095(14) 0.097(14) -0.010(11) 0.052(13) 0.034(12) C33 0.204(28) 0.076(13) 0.154(22) -0.005(14) 0.114(22) 0.020(15) C24 0.156(11) 0.188(13) 0.063(6) -0.013(7) 0.000(6) -0.054(10) C20 0.077(5) 0.111(7) 0.063(5) 0.019(5) 0.004(4) -0.008(5) C22 0.130(17) 0.132(18) 0.065(11) -0.003(11) -0.009(11) 0.050(14) C23 0.120(17) 0.126(18) 0.097(15) 0.022(13) 0.004(12) 0.040(14) P1 0.083(5) 0.094(6) 0.115(6) 0.013(5) 0.037(4) 0.023(4) F1 0.182(14) 0.196(25) 0.115(11) -0.024(10) 0.000(10) 0.065(12) F2 0.245(12) 0.142(18) 0.196(30) 0.051(19) 0.083(28) -0.027(23) F3 0.115(11) 0.177(21) 0.257(22) -0.018(15) 0.057(10) 0.062(10) F4 0.182(14) 0.196(25) 0.115(11) -0.024(10) 0.000(10) 0.065(12) F5 0.245(12) 0.142(18) 0.196(30) 0.051(19) 0.083(28) -0.027(23) F6 0.115(11) 0.177(21) 0.257(22) -0.018(15) 0.057(10) 0.062(10) _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 N11 2.164(6) . yes Mn1 N21 2.207(5) 2_567 yes Mn1 N21 2.262(6) . yes Mn1 N2 2.28(3) . yes Mn1 N32 2.27(3) . yes Mn1 N3 2.290(6) . yes Mn1 N1 2.294(6) . yes N11 N12 1.163(6) . yes N12 N11 1.163(6) 2_667 yes N21 N22 1.200(7) . yes N21 Mn1 2.207(5) 2_567 yes N22 N23 1.152(8) . yes N1 C5 1.333(9) . ? N1 C1 1.339(9) . ? C1 C2 1.375(10) . ? C1 H1 0.93 . ? C2 C3 1.395(11) . ? C2 C6 1.511(11) . ? C3 C4 1.376(11) . ? C3 C8 1.524(10) . ? C4 C5 1.364(10) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? C6 C7 1.476(14) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? N2 C13 1.31(2) . ? N2 C9 1.34(2) . ? C9 C10 1.38(2) . ? C9 H9 0.93 . ? C10 C11 1.38(2) . ? C10 C14 1.46(4) . ? C11 C12 1.36(2) . ? C11 C16 1.51(3) . ? C12 C13 1.40(2) . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 C15 1.39(5) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 H15A 0.96 . ? C15 H15B 0.960(2) . ? C15 H15C 0.960(2) . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? N32 C43 1.32(2) . ? N32 C39 1.35(2) . ? C39 C40 1.39(2) . ? C39 H39 0.93 . ? C40 C41 1.37(2) . ? C40 C44 1.50(4) . ? C41 C42 1.36(2) . ? C41 C46 1.54(3) . ? C42 C43 1.40(2) . ? C42 H42 0.93 . ? C43 H43 0.93 . ? C44 C45 1.06(6) . ? C44 H44A 0.97 . ? C44 H44B 0.97 . ? C45 H45A 0.960(2) . ? C45 H45B 0.960(5) . ? C45 H45C 0.960(4) . ? C46 H46A 0.96 . ? C46 H46B 0.96 . ? C46 H46C 0.96 . ? N3 C21 1.315(10) . ? N3 C17 1.341(10) . ? C17 C18A 1.386(11) . ? C17 C18 1.386(11) . ? C17 H17 0.93 . ? C18 C19 1.379(14) . ? C18 H18 0.93 . ? C19 C20 1.352(14) . ? C19 C20A 1.352(14) . ? C19 C18A 1.379(14) . ? C19 C24 1.513(11) . ? C20A C21 1.395(11) . ? C20A H20A 0.93 . ? C21 C20 1.395(11) . ? C21 H21 0.93 . ? C18A C32 1.31(2) . ? C32 C33 1.46(3) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C33 H33A 0.9600(12) . ? C33 H33B 0.9600(14) . ? C33 H33C 0.960(2) . ? C24 H24A 0.96 . ? C24 H24B 0.9601(12) . ? C24 H24C 0.96 . ? C20 C22 1.41(2) . ? C22 C23 1.46(3) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 H23A 0.96 . ? C23 H23B 0.9600(12) . ? C23 H23C 0.960(2) . ? P1 F5 1.50(2) . ? P1 F2 1.52(2) . ? P1 F3 1.516(14) . ? P1 F4 1.52(2) . ? P1 F1 1.52(2) . ? P1 F6 1.527(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 N11 Mn1 N21 169.8(2) . 2_567 yes N11 Mn1 N21 91.4(2) . . yes N21 Mn1 N21 78.6(2) 2_567 . yes N11 Mn1 N2 90.4(6) . . yes N21 Mn1 N2 89.6(5) 2_567 . yes N21 Mn1 N2 98.3(6) . . yes N11 Mn1 N32 84.5(6) . . yes N21 Mn1 N32 94.3(6) 2_567 . yes N21 Mn1 N32 92.0(6) . . yes N11 Mn1 N3 91.5(3) . . yes N21 Mn1 N3 89.9(2) 2_567 . yes N21 Mn1 N3 89.8(2) . . yes N2 Mn1 N3 171.6(6) . . yes N32 Mn1 N3 175.7(5) . . yes N11 Mn1 N1 94.2(2) . . yes N21 Mn1 N1 95.8(2) 2_567 . yes N21 Mn1 N1 174.4(2) . . yes N2 Mn1 N1 81.8(6) . . yes N32 Mn1 N1 88.6(6) . . yes N3 Mn1 N1 89.9(2) . . yes N12 N11 Mn1 150.5(5) . . yes N11 N12 N11 180.000(5) . 2_667 yes N22 N21 Mn1 131.6(5) . 2_567 yes N22 N21 Mn1 118.5(4) . . yes Mn1 N21 Mn1 101.4(2) 2_567 . yes N23 N22 N21 179.1(7) . . yes C5 N1 C1 115.7(6) . . ? C5 N1 Mn1 124.2(5) . . ? C1 N1 Mn1 119.7(5) . . ? N1 C1 C2 125.6(7) . . ? N1 C1 H1 117.2(4) . . ? C2 C1 H1 117.2(5) . . ? C1 C2 C3 117.2(7) . . ? C1 C2 C6 119.6(7) . . ? C3 C2 C6 123.2(7) . . ? C4 C3 C2 117.6(7) . . ? C4 C3 C8 121.4(8) . . ? C2 C3 C8 121.1(8) . . ? C5 C4 C3 120.7(8) . . ? C5 C4 H4 119.7(5) . . ? C3 C4 H4 119.7(5) . . ? N1 C5 C4 123.2(8) . . ? N1 C5 H5 118.4(4) . . ? C4 C5 H5 118.4(5) . . ? C7 C6 C2 111.9(8) . . ? C7 C6 H6A 109.3(7) . . ? C2 C6 H6A 109.2(5) . . ? C7 C6 H6B 109.2(7) . . ? C2 C6 H6B 109.2(5) . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5(7) . . ? C6 C7 H7B 109.5(6) . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5(7) . . ? H7A C7 H7C 109.47(9) . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5(6) . . ? C3 C8 H8B 109.5(5) . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5(5) . . ? H8A C8 H8C 109.47(8) . . ? H8B C8 H8C 109.47(11) . . ? C13 N2 C9 117.7(22) . . ? C13 N2 Mn1 121.8(18) . . ? C9 N2 Mn1 120.2(18) . . ? N2 C9 C10 122.9(21) . . ? N2 C9 H9 118.6(14) . . ? C10 C9 H9 118.6(12) . . ? C11 C10 C9 119.4(20) . . ? C11 C10 C14 118.9(24) . . ? C9 C10 C14 121.6(23) . . ? C12 C11 C10 117.1(21) . . ? C12 C11 C16 116.4(22) . . ? C10 C11 C16 126.5(23) . . ? C11 C12 C13 120.7(20) . . ? C11 C12 H12 119.7(13) . . ? C13 C12 H12 119.7(12) . . ? N2 C13 C12 122.2(21) . . ? N2 C13 H13 118.9(15) . . ? C12 C13 H13 118.9(12) . . ? C15 C14 C10 116.1(23) . . ? C15 C14 H14A 108.3(17) . . ? C10 C14 H14A 108.3(9) . . ? C15 C14 H14B 108.2(20) . . ? C10 C14 H14B 108.3(11) . . ? H14A C14 H14B 107.4 . . ? C14 C15 H15A 109.5(16) . . ? C14 C15 H15B 109.5(20) . . ? H15A C15 H15B 109.5(3) . . ? C14 C15 H15C 109.5(16) . . ? H15A C15 H15C 109.47(13) . . ? H15B C15 H15C 109.5(2) . . ? C11 C16 H16A 109.5(10) . . ? C11 C16 H16B 109.4(14) . . ? H16A C16 H16B 109.47(8) . . ? C11 C16 H16C 109.5(7) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C43 N32 C39 116.8(22) . . ? C43 N32 Mn1 123.1(18) . . ? C39 N32 Mn1 120.1(18) . . ? N32 C39 C40 123.5(21) . . ? N32 C39 H39 118.2(14) . . ? C40 C39 H39 118.2(13) . . ? C41 C40 C39 119.0(19) . . ? C41 C40 C44 121.7(24) . . ? C39 C40 C44 119.3(25) . . ? C42 C41 C40 117.9(18) . . ? C42 C41 C46 117.7(18) . . ? C40 C41 C46 124.4(19) . . ? C41 C42 C43 120.4(17) . . ? C41 C42 H42 119.8(11) . . ? C43 C42 H42 119.8(11) . . ? N32 C43 C42 122.4(19) . . ? N32 C43 H43 118.8(14) . . ? C42 C43 H43 118.8(11) . . ? C45 C44 C40 134.5(53) . . ? C45 C44 H44A 103.5(47) . . ? C40 C44 H44A 103.6(11) . . ? C45 C44 H44B 103.6(54) . . ? C40 C44 H44B 103.5(12) . . ? H44A C44 H44B 105.3 . . ? C44 C45 H45A 109.5(44) . . ? C44 C45 H45B 109.5(53) . . ? H45A C45 H45B 109.5(6) . . ? C44 C45 H45C 109.4(47) . . ? H45A C45 H45C 109.5(4) . . ? H45B C45 H45C 109.5(4) . . ? C41 C46 H46A 109.5(8) . . ? C41 C46 H46B 109.5(7) . . ? H46A C46 H46B 109.5 . . ? C41 C46 H46C 109.4(11) . . ? H46A C46 H46C 109.47(6) . . ? H46B C46 H46C 109.47(10) . . ? C21 N3 C17 116.6(7) . . ? C21 N3 Mn1 122.8(6) . . ? C17 N3 Mn1 120.7(5) . . ? N3 C17 C18A 123.7(9) . . ? N3 C17 C18 123.7(9) . . ? N3 C17 H17 118.2(5) . . ? C18 C17 H17 118.2(6) . . ? C19 C18 C17 118.5(9) . . ? C19 C18 H18 120.7(6) . . ? C17 C18 H18 120.8(6) . . ? C20 C19 C18 118.2(8) . . ? C20A C19 C18A 118.2(8) . . ? C20A C19 C24 124.1(11) . . ? C18A C19 C24 117.7(11) . . ? C19 C20A C21 119.9(9) . . ? C19 C20A H20A 120.1(6) . . ? C21 C20A H20A 120.1(6) . . ? N3 C21 C20 123.2(10) . . ? N3 C21 C20A 123.2(10) . . ? N3 C21 H21 118.4(5) . . ? C20 C21 H21 118.4(6) . . ? C32 C18A C19 117.0(14) . . ? C32 C18A C17 124.4(14) . . ? C19 C18A C17 118.5(9) . . ? C18A C32 C33 113.4(17) . . ? C18A C32 H32A 108.9(11) . . ? C33 C32 H32A 108.9(13) . . ? C18A C32 H32B 108.9(11) . . ? C33 C32 H32B 108.9(13) . . ? H32A C32 H32B 107.7 . . ? C32 C33 H33A 109.5(11) . . ? C32 C33 H33B 109.5(13) . . ? H33A C33 H33B 109.5(3) . . ? C32 C33 H33C 109.5(13) . . ? H33A C33 H33C 109.5(2) . . ? H33B C33 H33C 109.5(2) . . ? C19 C24 H24A 109.5(6) . . ? C19 C24 H24B 109.5(6) . . ? H24A C24 H24B 109.47(11) . . ? C19 C24 H24C 109.5(8) . . ? H24A C24 H24C 109.47(7) . . ? H24B C24 H24C 109.5(2) . . ? C19 C20 C21 119.9(9) . . ? C19 C20 C22 114.5(12) . . ? C21 C20 C22 125.6(13) . . ? C20 C22 C23 112.9(15) . . ? C20 C22 H22A 109.0(11) . . ? C23 C22 H22A 109.0(13) . . ? C20 C22 H22B 109.0(11) . . ? C23 C22 H22B 109.0(14) . . ? H22A C22 H22B 107.79(10) . . ? C22 C23 H23A 109.5(10) . . ? C22 C23 H23B 109.5(14) . . ? H23A C23 H23B 109.47(12) . . ? C22 C23 H23C 109.4(14) . . ? H23A C23 H23C 109.5(2) . . ? H23B C23 H23C 109.47(14) . . ? F5 P1 F2 166.4(48) . . ? F5 P1 F3 95.4(30) . . ? F2 P1 F3 92.0(30) . . ? F5 P1 F4 80.5(24) . . ? F2 P1 F4 88.0(22) . . ? F3 P1 F4 90.5(17) . . ? F5 P1 F1 95.6(23) . . ? F2 P1 F1 96.1(24) . . ? F3 P1 F1 87.4(16) . . ? F4 P1 F1 175.4(24) . . ? F5 P1 F6 84.8(29) . . ? F2 P1 F6 87.8(31) . . ? F3 P1 F6 179.8(33) . . ? F4 P1 F6 89.4(16) . . ? F1 P1 F6 92.7(18) . . ? 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 N21 Mn1 N11 N12 -86.5(18) 2_567 . . . ? N21 Mn1 N11 N12 -78.1(10) . . . . ? N2 Mn1 N11 N12 -176.4(12) . . . . ? N32 Mn1 N11 N12 -170.0(12) . . . . ? N3 Mn1 N11 N12 11.8(10) . . . . ? N1 Mn1 N11 N12 101.8(10) . . . . ? Mn1 N11 N12 N11 -108.2(423) . . . 2_667 ? N11 Mn1 N21 N22 29.8(5) . . . . ? N21 Mn1 N21 N22 -151.7(6) 2_567 . . . ? N2 Mn1 N21 N22 120.4(7) . . . . ? N32 Mn1 N21 N22 114.3(7) . . . . ? N3 Mn1 N21 N22 -61.8(5) . . . . ? N1 Mn1 N21 N22 -149.0(20) . . . . ? N11 Mn1 N21 Mn1 -178.5(2) . . . 2_567 ? N21 Mn1 N21 Mn1 0.0 2_567 . . 2_567 ? N2 Mn1 N21 Mn1 -87.9(6) . . . 2_567 ? N32 Mn1 N21 Mn1 -93.9(6) . . . 2_567 ? N3 Mn1 N21 Mn1 90.0(2) . . . 2_567 ? N1 Mn1 N21 Mn1 2.8(23) . . . 2_567 ? Mn1 N21 N22 N23 -55.1(467) 2_567 . . . ? Mn1 N21 N22 N23 86.5(465) . . . . ? N11 Mn1 N1 C5 -162.4(7) . . . . ? N21 Mn1 N1 C5 19.1(7) 2_567 . . . ? N21 Mn1 N1 C5 16.3(26) . . . . ? N2 Mn1 N1 C5 107.8(8) . . . . ? N32 Mn1 N1 C5 113.2(8) . . . . ? N3 Mn1 N1 C5 -70.9(7) . . . . ? N11 Mn1 N1 C1 26.3(6) . . . . ? N21 Mn1 N1 C1 -152.3(6) 2_567 . . . ? N21 Mn1 N1 C1 -155.0(20) . . . . ? N2 Mn1 N1 C1 -63.5(8) . . . . ? N32 Mn1 N1 C1 -58.1(8) . . . . ? N3 Mn1 N1 C1 117.8(6) . . . . ? C5 N1 C1 C2 -1.3(12) . . . . ? Mn1 N1 C1 C2 170.8(6) . . . . ? N1 C1 C2 C3 2.5(12) . . . . ? N1 C1 C2 C6 -176.8(8) . . . . ? C1 C2 C3 C4 -1.0(12) . . . . ? C6 C2 C3 C4 178.4(8) . . . . ? C1 C2 C3 C8 179.6(8) . . . . ? C6 C2 C3 C8 -1.1(13) . . . . ? C2 C3 C4 C5 -1.6(13) . . . . ? C8 C3 C4 C5 177.9(9) . . . . ? C1 N1 C5 C4 -1.5(12) . . . . ? Mn1 N1 C5 C4 -173.2(7) . . . . ? C3 C4 C5 N1 3.0(14) . . . . ? C1 C2 C6 C7 89.0(11) . . . . ? C3 C2 C6 C7 -90.3(12) . . . . ? N11 Mn1 N2 C13 49.8(9) . . . . ? N21 Mn1 N2 C13 -120.1(9) 2_567 . . . ? N21 Mn1 N2 C13 -41.7(9) . . . . ? N32 Mn1 N2 C13 2.5(60) . . . . ? N3 Mn1 N2 C13 153.1(32) . . . . ? N1 Mn1 N2 C13 144.0(9) . . . . ? N11 Mn1 N2 C9 -136.1(8) . . . . ? N21 Mn1 N2 C9 54.1(8) 2_567 . . . ? N21 Mn1 N2 C9 132.5(8) . . . . ? N32 Mn1 N2 C9 176.7(71) . . . . ? N3 Mn1 N2 C9 -32.7(41) . . . . ? N1 Mn1 N2 C9 -41.9(8) . . . . ? C13 N2 C9 C10 0.0(2) . . . . ? Mn1 N2 C9 C10 -174.4(11) . . . . ? N2 C9 C10 C11 0.0(2) . . . . ? N2 C9 C10 C14 -180.0(2) . . . . ? C9 C10 C11 C12 0.0(2) . . . . ? C14 C10 C11 C12 -179.97(14) . . . . ? C9 C10 C11 C16 179.9(2) . . . . ? C14 C10 C11 C16 -0.1(3) . . . . ? C10 C11 C12 C13 0.0(2) . . . . ? C16 C11 C12 C13 -180.0(2) . . . . ? C9 N2 C13 C12 0.0(2) . . . . ? Mn1 N2 C13 C12 174.3(11) . . . . ? C11 C12 C13 N2 0.0(2) . . . . ? C11 C10 C14 C15 171.5(24) . . . . ? C9 C10 C14 C15 -8.5(24) . . . . ? N11 Mn1 N32 C43 33.0(9) . . . . ? N21 Mn1 N32 C43 -136.9(9) 2_567 . . . ? N21 Mn1 N32 C43 -58.2(9) . . . . ? N2 Mn1 N32 C43 165.4(71) . . . . ? N3 Mn1 N32 C43 57.2(84) . . . . ? N1 Mn1 N32 C43 127.4(9) . . . . ? N11 Mn1 N32 C39 -146.5(9) . . . . ? N21 Mn1 N32 C39 43.7(9) 2_567 . . . ? N21 Mn1 N32 C39 122.4(9) . . . . ? N2 Mn1 N32 C39 -14.0(60) . . . . ? N3 Mn1 N32 C39 -122.3(78) . . . . ? N1 Mn1 N32 C39 -52.1(9) . . . . ? C43 N32 C39 C40 0.0(2) . . . . ? Mn1 N32 C39 C40 179.5(11) . . . . ? N32 C39 C40 C41 0.0(2) . . . . ? N32 C39 C40 C44 -180.0(2) . . . . ? C39 C40 C41 C42 0.0(2) . . . . ? C44 C40 C41 C42 -179.99(14) . . . . ? C39 C40 C41 C46 180.0(2) . . . . ? C44 C40 C41 C46 0.0(3) . . . . ? C40 C41 C42 C43 0.0(2) . . . . ? C46 C41 C42 C43 -180.0(2) . . . . ? C39 N32 C43 C42 0.0(2) . . . . ? Mn1 N32 C43 C42 -179.5(12) . . . . ? C41 C42 C43 N32 0.0(2) . . . . ? C41 C40 C44 C45 176.8(79) . . . . ? C39 C40 C44 C45 -3.2(79) . . . . ? N11 Mn1 N3 C21 -26.7(6) . . . . ? N21 Mn1 N3 C21 143.3(6) 2_567 . . . ? N21 Mn1 N3 C21 64.7(6) . . . . ? N2 Mn1 N3 C21 -130.0(37) . . . . ? N32 Mn1 N3 C21 -50.8(82) . . . . ? N1 Mn1 N3 C21 -120.9(6) . . . . ? N11 Mn1 N3 C17 152.2(6) . . . . ? N21 Mn1 N3 C17 -37.8(6) 2_567 . . . ? N21 Mn1 N3 C17 -116.4(6) . . . . ? N2 Mn1 N3 C17 48.9(38) . . . . ? N32 Mn1 N3 C17 128.1(81) . . . . ? N1 Mn1 N3 C17 58.0(6) . . . . ? C21 N3 C17 C18A 1.8(12) . . . . ? Mn1 N3 C17 C18A -177.1(6) . . . . ? C21 N3 C17 C18 1.8(12) . . . . ? Mn1 N3 C17 C18 -177.1(6) . . . . ? N3 C17 C18 C19 -2.0(13) . . . . ? C18A C17 C18 C19 0.0(1000) . . . . ? C17 C18 C19 C20 0.2(13) . . . . ? C17 C18 C19 C20A 0.2(13) . . . . ? C17 C18 C19 C18A 101.2(1000) . . . . ? C17 C18 C19 C24 -179.9(8) . . . . ? C20 C19 C20A C21 0.0(1000) . . . . ? C18 C19 C20A C21 1.6(14) . . . . ? C18A C19 C20A C21 1.6(14) . . . . ? C24 C19 C20A C21 -178.3(9) . . . . ? C17 N3 C21 C20 0.0(11) . . . . ? Mn1 N3 C21 C20 179.0(6) . . . . ? C17 N3 C21 C20A 0.0(11) . . . . ? Mn1 N3 C21 C20A 179.0(6) . . . . ? C19 C20A C21 N3 -1.8(13) . . . . ? C19 C20A C21 C20 73.0(1000) . . . . ? C20 C19 C18A C32 177.2(14) . . . . ? C20A C19 C18A C32 177.2(14) . . . . ? C18 C19 C18A C32 0.0(1000) . . . . ? C24 C19 C18A C32 -3.0(18) . . . . ? C20 C19 C18A C17 0.2(13) . . . . ? C20A C19 C18A C17 0.2(13) . . . . ? C18 C19 C18A C17 0.0(1000) . . . . ? C24 C19 C18A C17 -179.9(8) . . . . ? N3 C17 C18A C32 -178.7(15) . . . . ? C18 C17 C18A C32 0.0(1000) . . . . ? N3 C17 C18A C19 -2.0(13) . . . . ? C18 C17 C18A C19 0.0(1000) . . . . ? C19 C18A C32 C33 176.5(15) . . . . ? C17 C18A C32 C33 -6.8(27) . . . . ? C20A C19 C20 C21 0.0(1000) . . . . ? C18 C19 C20 C21 1.6(14) . . . . ? C18A C19 C20 C21 1.6(14) . . . . ? C24 C19 C20 C21 -178.3(9) . . . . ? C20A C19 C20 C22 0.0(1000) . . . . ? C18 C19 C20 C22 -176.1(14) . . . . ? C18A C19 C20 C22 -176.1(14) . . . . ? C24 C19 C20 C22 4.0(18) . . . . ? N3 C21 C20 C19 -1.8(13) . . . . ? C20A C21 C20 C19 0.0(1000) . . . . ? N3 C21 C20 C22 175.6(15) . . . . ? C20A C21 C20 C22 0.0(1000) . . . . ? C19 C20 C22 C23 165.4(17) . . . . ? C21 C20 C22 C23 -12.1(29) . . . . ? _refine_diff_density_max 0.368 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.074 #===END data_alex1d _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[Mn2(3-aminopyridine)4(N3)4(H2O)](H2O)4' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H34 Mn2 N20 O5' _chemical_formula_weight 744.56 _chemical_melting_point ? _chemical_compound_source ? 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' 'Mn' 'Mn' 0.3368 0.7283 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.881(6) _cell_length_b 12.913(3) _cell_length_c 15.741(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.64(2) _cell_angle_gamma 90.00 _cell_volume 3287.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 7.2 _cell_measurement_theta_max 15.3 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 1.49(3) _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'suspension method' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'mod. STOE 4-circle diffractometer' _diffrn_measurement_method 'Omega-scan; delta Omega: 1.25 deg.' _diffrn_standards_number '3 (1 1 -3; -1 -3 2; 0 -4 0)' _diffrn_standards_interval_count 100 _diffrn_standards_interval_time '1 h' _diffrn_standards_decay_% 6 _diffrn_reflns_number 3293 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.48 _reflns_number_total 2670 _reflns_number_observed 2255 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _computing_publication_material 'SHELXTL/PC v.5.03 (Siemens Ind. Aut.)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.3217P] 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_number_reflns 2665 _refine_ls_number_parameters 283 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_obs 0.0373 _refine_ls_wR_factor_all 0.0875 _refine_ls_wR_factor_obs 0.0782 _refine_ls_goodness_of_fit_all 1.084 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.095 _refine_ls_restrained_S_obs 1.075 _refine_ls_shift/esd_max 0.454 _refine_ls_shift/esd_mean 0.031 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.00813(2) 0.11487(2) 0.44828(2) 0.03184(7) Uani 1 d . . N1 N -0.12854(9) 0.10961(13) 0.37321(11) 0.0401(4) Uani 1 d . . C1 C -0.15712(11) 0.0436(2) 0.30702(12) 0.0382(5) Uani 1 d . . H1 H -0.11912(11) 0.0048(2) 0.28774(12) 0.046 Uiso 1 calc R . C2 C -0.24073(12) 0.0290(2) 0.26485(13) 0.0418(5) Uani 1 d . . C3 C -0.29609(12) 0.0870(2) 0.2943(2) 0.0538(7) Uani 1 d . . H3 H -0.35264(12) 0.0792(2) 0.2684(2) 0.065 Uiso 1 calc R . C4 C -0.26728(13) 0.1560(2) 0.3620(2) 0.0564(7) Uani 1 d . . H4 H -0.30410(13) 0.1959(2) 0.3822(2) 0.068 Uiso 1 calc R . C5 C -0.18349(12) 0.1661(2) 0.40009(15) 0.0474(6) Uani 1 d . . H5 H -0.16438(12) 0.2135(2) 0.44586(15) 0.057 Uiso 1 calc R . N2 N -0.26664(11) -0.0390(2) 0.19372(12) 0.0548(6) Uani 1 d D . N3 N 0.14225(9) 0.13188(13) 0.52580(10) 0.0358(4) Uani 1 d . . C6 C 0.20100(11) 0.0928(2) 0.49364(13) 0.0373(5) Uani 1 d . . H6 H 0.18477(11) 0.0525(2) 0.44265(13) 0.045 Uiso 1 calc R . C7 C 0.28464(11) 0.1090(2) 0.53189(13) 0.0369(5) Uani 1 d . . C8 C 0.30790(12) 0.1705(2) 0.60650(13) 0.0434(6) Uani 1 d . . H8 H 0.36346(12) 0.1843(2) 0.63365(13) 0.052 Uiso 1 calc R . C9 C 0.24817(13) 0.2109(2) 0.64018(14) 0.0467(6) Uani 1 d . . H9 H 0.26292(13) 0.2524(2) 0.69055(14) 0.056 Uiso 1 calc R . C10 C 0.16648(13) 0.1899(2) 0.59918(13) 0.0412(5) Uani 1 d . . H10 H 0.12654(13) 0.2169(2) 0.62319(13) 0.049 Uiso 1 calc R . N4 N 0.34313(10) 0.0638(2) 0.49588(12) 0.0482(5) Uani 1 d D . N11 N -0.02158(9) 0.05903(13) 0.56857(10) 0.0375(4) Uani 1 d . . N12 N -0.05998(10) 0.09557(13) 0.61313(11) 0.0396(4) Uani 1 d . . N13 N -0.09713(13) 0.1297(2) 0.65723(14) 0.0721(6) Uani 1 d . . N21 N 0.03911(10) 0.14051(15) 0.32411(10) 0.0456(5) Uani 1 d . . N22 N 0.0000 0.1405(2) 0.2500 0.0338(6) Uani 1 d S . N31 N -0.0035(2) 0.2874(3) 0.4562(2) 0.0287(9) Uani 0.50 d P 1 N32 N -0.0294(2) 0.3326(3) 0.3889(3) 0.0510(11) Uani 0.50 d P 1 N33 N -0.0462(3) 0.3831(5) 0.3276(3) 0.085(2) Uani 0.50 d P 1 O3 O -0.0053(3) 0.2811(4) 0.4668(3) 0.069(2) Uani 0.50 d PD 2 O4 O -0.0453(3) 0.4084(4) 0.3107(3) 0.0677(14) Uani 0.50 d PD 2 H43 H -0.0219(13) 0.4053(23) 0.2717(11) 0.080(9) Uiso 0.50 d PD 2 H44 H -0.0265(22) 0.4594(15) 0.3416(15) 0.080(9) Uiso 0.50 d PD 2 H41 H -0.0116(20) 0.3087(25) 0.5119(9) 0.080(9) Uiso 0.50 d PD 2 H42 H -0.0168(32) 0.3235(18) 0.4269(11) 0.080(9) Uiso 0.50 d PD 2 O1 O 0.0000 0.3234(2) 0.7500 0.0989(11) Uani 1 d SD . O2 O -0.0444(2) 0.4049(2) 0.58516(15) 0.1172(9) Uani 1 d D . HN4A H 0.3868(9) 0.1033(14) 0.5026(15) 0.064(4) Uiso 1 d D . HN2A H -0.3148(8) -0.0659(17) 0.1932(14) 0.064(4) Uiso 1 d D . HN4B H 0.3232(13) 0.0351(16) 0.4415(9) 0.064(4) Uiso 1 d D . HN2B H -0.2282(9) -0.0797(15) 0.1848(14) 0.064(4) Uiso 1 d D . H21 H -0.0815(14) 0.3644(21) 0.5554(18) 0.067(8) Uiso 0.50 d PD . H22 H -0.0235(21) 0.3758(23) 0.6338(12) 0.067(8) Uiso 0.50 d PD . H23 H -0.0126(10) 0.3913(28) 0.5552(15) 0.067(8) Uiso 0.50 d PD . H24 H -0.0797(13) 0.4471(19) 0.5562(21) 0.067(8) Uiso 0.50 d PD . H11 H 0.0000 0.2598(11) 0.7500 0.240(29) Uiso 1 d SD . H12 H -0.0497(11) 0.3089(73) 0.7320(134) 0.240(29) Uiso 0.25 d PD . H13 H 0.0056(88) 0.3644(28) 0.7915(23) 0.240(29) Uiso 0.25 d PD . 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 0.03154(13) 0.0331(2) 0.03103(13) 0.00078(13) 0.00922(10) 0.00087(12) N1 0.0354(7) 0.0413(10) 0.0444(9) 0.0039(8) 0.0129(7) 0.0039(7) C1 0.0352(9) 0.0402(12) 0.0388(10) 0.0059(9) 0.0097(8) 0.0019(9) C2 0.0389(10) 0.0439(12) 0.0403(10) 0.0127(10) 0.0075(8) -0.0040(9) C3 0.0308(9) 0.061(2) 0.0677(14) 0.0122(13) 0.0115(10) 0.0025(10) C4 0.0420(10) 0.0544(15) 0.0780(15) 0.0042(13) 0.0253(10) 0.0120(11) C5 0.0422(10) 0.0424(13) 0.0589(12) -0.0008(11) 0.0167(9) 0.0048(10) N2 0.0448(10) 0.0659(14) 0.0479(10) 0.0028(10) 0.0040(9) -0.0109(10) N3 0.0361(8) 0.0362(10) 0.0336(8) 0.0029(7) 0.0077(7) -0.0027(7) C6 0.0352(9) 0.0369(12) 0.0365(10) -0.0015(9) 0.0048(8) -0.0011(8) C7 0.0353(9) 0.0321(11) 0.0405(10) 0.0092(9) 0.0065(8) 0.0011(8) C8 0.0371(10) 0.0385(12) 0.0449(12) 0.0035(10) -0.0038(9) -0.0063(9) C9 0.0565(12) 0.0354(12) 0.0405(11) -0.0026(10) 0.0015(10) -0.0045(10) C10 0.0477(10) 0.0382(12) 0.0371(10) -0.0005(9) 0.0113(9) 0.0029(9) N4 0.0354(8) 0.0542(12) 0.0528(10) -0.0003(9) 0.0094(8) 0.0008(8) N11 0.0423(8) 0.0370(10) 0.0380(8) 0.0013(8) 0.0189(7) 0.0045(7) N12 0.0465(8) 0.0323(10) 0.0436(9) -0.0004(8) 0.0187(7) -0.0010(7) N13 0.0922(12) 0.0583(14) 0.0879(12) -0.0116(11) 0.0611(10) 0.0056(11) N21 0.0443(9) 0.0605(12) 0.0317(8) 0.0020(8) 0.0107(7) -0.0053(9) N22 0.0341(10) 0.0337(13) 0.0354(11) 0.000 0.0127(9) 0.000 N31 0.040(2) 0.022(2) 0.025(2) -0.0053(14) 0.0114(13) 0.0043(14) N32 0.037(2) 0.052(2) 0.064(2) -0.018(2) 0.014(2) -0.004(2) N33 0.098(3) 0.102(4) 0.049(2) 0.044(3) 0.010(2) 0.049(3) O3 0.090(3) 0.057(3) 0.062(3) 0.014(2) 0.024(2) 0.002(2) O4 0.071(2) 0.082(3) 0.043(2) 0.010(2) 0.005(2) 0.020(2) O1 0.102(2) 0.075(2) 0.105(2) 0.000 0.006(2) 0.000 O2 0.153(2) 0.117(2) 0.0909(14) 0.0322(13) 0.0502(14) 0.063(2) _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 N21 2.188(2) . yes Mn1 O3 2.187(5) . yes Mn1 N11 2.214(2) . yes Mn1 N31 2.243(4) . yes Mn1 N3 2.254(2) . yes Mn1 N1 2.272(2) . yes Mn1 N11 2.280(2) 5_556 yes N1 C1 1.326(3) . ? N1 C5 1.340(3) . ? C1 C2 1.390(3) . ? C1 H1 0.93 . ? C2 C3 1.377(3) . ? C2 N2 1.391(3) . ? C3 C4 1.367(3) . ? C3 H3 0.93 . ? C4 C5 1.375(3) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? N2 HN2A 0.882(14) . ? N2 HN2B 0.878(14) . ? N3 C6 1.335(3) . ? N3 C10 1.339(2) . ? C6 C7 1.383(3) . ? C6 H6 0.93 . ? C7 C8 1.379(3) . ? C7 N4 1.399(3) . ? C8 C9 1.370(3) . ? C8 H8 0.93 . ? C9 C10 1.372(3) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? N4 HN4A 0.877(14) . ? N4 HN4B 0.904(13) . ? N11 N12 1.181(2) . ? N11 Mn1 2.280(2) 5_556 ? N12 N13 1.148(3) . ? N21 N22 1.164(2) . ? N22 N21 1.164(2) 2 ? N31 N32 1.179(5) . ? N31 H41 0.97(2) . ? N31 H42 0.65(2) . ? N32 N33 1.131(6) . ? N32 H42 0.59(2) . ? N33 H43 1.11(2) . ? N33 H44 1.04(2) . ? O3 H41 0.83(2) . ? O3 H42 0.81(2) . ? O4 H43 0.82(2) . ? O4 H44 0.83(2) . ? O1 H11 0.821(15) . ? O1 H12 0.83(2) . ? O1 H13 0.83(2) . ? O2 H21 0.85(2) . ? O2 H22 0.84(2) . ? O2 H23 0.83(2) . ? O2 H24 0.84(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 N21 Mn1 O3 91.78(14) . . yes N21 Mn1 N11 169.70(7) . . yes O3 Mn1 N11 98.52(14) . . yes N21 Mn1 N31 86.92(11) . . yes N11 Mn1 N31 103.37(10) . . yes N21 Mn1 N3 90.51(6) . . yes O3 Mn1 N3 87.61(13) . . yes N11 Mn1 N3 90.41(6) . . yes N31 Mn1 N3 87.91(9) . . yes N21 Mn1 N1 90.39(7) . . yes O3 Mn1 N1 88.30(13) . . yes N11 Mn1 N1 89.43(6) . . yes N31 Mn1 N1 88.08(9) . . yes N3 Mn1 N1 175.84(6) . . yes N21 Mn1 N11 89.31(7) . 5_556 yes O3 Mn1 N11 178.91(13) . 5_556 yes N11 Mn1 N11 80.40(6) . 5_556 yes N31 Mn1 N11 176.22(10) . 5_556 yes N3 Mn1 N11 92.35(6) . 5_556 yes N1 Mn1 N11 91.73(6) . 5_556 yes C1 N1 C5 118.0(2) . . ? C1 N1 Mn1 120.97(13) . . ? C5 N1 Mn1 120.74(13) . . ? N1 C1 C2 123.6(2) . . ? N1 C1 H1 118.20(11) . . ? C2 C1 H1 118.20(13) . . ? C3 C2 C1 117.4(2) . . ? C3 C2 N2 121.8(2) . . ? C1 C2 N2 120.8(2) . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 120.25(13) . . ? C2 C3 H3 120.25(12) . . ? C3 C4 C5 119.5(2) . . ? C3 C4 H4 120.23(13) . . ? C5 C4 H4 120.23(15) . . ? N1 C5 C4 122.0(2) . . ? N1 C5 H5 119.01(11) . . ? C4 C5 H5 119.01(15) . . ? C2 N2 HN2A 109.4(15) . . ? C2 N2 HN2B 115.5(12) . . ? HN2A N2 HN2B 119.0(20) . . ? C6 N3 C10 117.5(2) . . ? C6 N3 Mn1 119.87(12) . . ? C10 N3 Mn1 122.19(13) . . ? N3 C6 C7 123.7(2) . . ? N3 C6 H6 118.15(10) . . ? C7 C6 H6 118.15(12) . . ? C8 C7 C6 117.6(2) . . ? C8 C7 N4 121.6(2) . . ? C6 C7 N4 120.8(2) . . ? C9 C8 C7 119.2(2) . . ? C9 C8 H8 120.40(12) . . ? C7 C8 H8 120.40(12) . . ? C8 C9 C10 119.6(2) . . ? C8 C9 H9 120.18(12) . . ? C10 C9 H9 120.18(13) . . ? N3 C10 C9 122.3(2) . . ? N3 C10 H10 118.86(11) . . ? C9 C10 H10 118.86(13) . . ? C7 N4 HN4A 112.0(14) . . ? C7 N4 HN4B 116.1(14) . . ? HN4A N4 HN4B 115.1(21) . . ? N12 N11 Mn1 132.47(14) . . yes N12 N11 Mn1 123.52(14) . 5_556 yes Mn1 N11 Mn1 99.60(6) . 5_556 yes N13 N12 N11 178.9(2) . . yes N22 N21 Mn1 133.07(12) . . yes N21 N22 N21 180.0(3) 2 . yes N32 N31 Mn1 117.3(3) . . yes Mn1 N31 H41 111.7(19) . . ? Mn1 N31 H42 133.9(22) . . ? H41 N31 H42 109.3(29) . . ? N33 N32 N31 172.0(5) . . yes H43 N33 H44 75.9(17) . . ? Mn1 O3 H41 125.5(22) . . ? Mn1 O3 H42 124.6(18) . . ? H41 O3 H42 108.2(25) . . ? H43 O4 H44 107.1(25) . . ? H11 O1 H12 76.9(66) . . ? H11 O1 H13 130.0(32) . . ? H12 O1 H13 106.9(100) . . ? H21 O2 H22 106.3(27) . . ? H21 O2 H23 92.9(29) . . ? H22 O2 H23 104.6(32) . . ? H21 O2 H24 78.6(27) . . ? H22 O2 H24 147.1(35) . . ? H23 O2 H24 107.6(27) . . ? 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 N21 Mn1 N1 C1 55.8(2) . . . . ? O3 Mn1 N1 C1 147.6(2) . . . . ? N11 Mn1 N1 C1 -113.9(2) . . . . ? N31 Mn1 N1 C1 142.7(2) . . . . ? N3 Mn1 N1 C1 158.2(8) . . . . ? N11 Mn1 N1 C1 -33.5(2) 5_556 . . . ? N21 Mn1 N1 C5 -130.7(2) . . . . ? O3 Mn1 N1 C5 -38.9(2) . . . . ? N11 Mn1 N1 C5 59.6(2) . . . . ? N31 Mn1 N1 C5 -43.8(2) . . . . ? N3 Mn1 N1 C5 -28.3(9) . . . . ? N11 Mn1 N1 C5 140.0(2) 5_556 . . . ? C5 N1 C1 C2 -0.7(3) . . . . ? Mn1 N1 C1 C2 172.9(2) . . . . ? N1 C1 C2 C3 0.0(3) . . . . ? N1 C1 C2 N2 177.8(2) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? N2 C2 C3 C4 -177.2(2) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C1 N1 C5 C4 0.9(3) . . . . ? Mn1 N1 C5 C4 -172.8(2) . . . . ? C3 C4 C5 N1 -0.4(4) . . . . ? N21 Mn1 N3 C6 -38.4(2) . . . . ? O3 Mn1 N3 C6 -130.2(2) . . . . ? N11 Mn1 N3 C6 131.3(2) . . . . ? N31 Mn1 N3 C6 -125.3(2) . . . . ? N1 Mn1 N3 C6 -140.8(8) . . . . ? N11 Mn1 N3 C6 50.9(2) 5_556 . . . ? N21 Mn1 N3 C10 134.1(2) . . . . ? O3 Mn1 N3 C10 42.4(2) . . . . ? N11 Mn1 N3 C10 -56.2(2) . . . . ? N31 Mn1 N3 C10 47.2(2) . . . . ? N1 Mn1 N3 C10 31.7(9) . . . . ? N11 Mn1 N3 C10 -136.6(2) 5_556 . . . ? C10 N3 C6 C7 0.1(3) . . . . ? Mn1 N3 C6 C7 173.0(2) . . . . ? N3 C6 C7 C8 -1.2(3) . . . . ? N3 C6 C7 N4 178.6(2) . . . . ? C6 C7 C8 C9 1.2(3) . . . . ? N4 C7 C8 C9 -178.6(2) . . . . ? C7 C8 C9 C10 -0.1(3) . . . . ? C6 N3 C10 C9 1.0(3) . . . . ? Mn1 N3 C10 C9 -171.7(2) . . . . ? C8 C9 C10 N3 -1.0(3) . . . . ? N21 Mn1 N11 N12 -153.3(3) . . . . ? O3 Mn1 N11 N12 24.0(2) . . . . ? N31 Mn1 N11 N12 23.7(2) . . . . ? N3 Mn1 N11 N12 111.6(2) . . . . ? N1 Mn1 N11 N12 -64.2(2) . . . . ? N11 Mn1 N11 N12 -156.1(2) 5_556 . . . ? N21 Mn1 N11 Mn1 2.8(3) . . . 5_556 ? O3 Mn1 N11 Mn1 -179.96(13) . . . 5_556 ? N31 Mn1 N11 Mn1 179.74(9) . . . 5_556 ? N3 Mn1 N11 Mn1 -92.31(6) . . . 5_556 ? N1 Mn1 N11 Mn1 91.85(6) . . . 5_556 ? N11 Mn1 N11 Mn1 0.0 5_556 . . 5_556 ? Mn1 N11 N12 N13 175.8(1000) . . . . ? Mn1 N11 N12 N13 24.4(108) 5_556 . . . ? O3 Mn1 N21 N22 -94.9(3) . . . . ? N11 Mn1 N21 N22 82.4(4) . . . . ? N31 Mn1 N21 N22 -94.6(2) . . . . ? N3 Mn1 N21 N22 177.5(2) . . . . ? N1 Mn1 N21 N22 -6.6(2) . . . . ? N11 Mn1 N21 N22 85.2(2) 5_556 . . . ? Mn1 N21 N22 N21 101.5(1000) . . . 2 ? N21 Mn1 N31 N32 34.5(3) . . . . ? O3 Mn1 N31 N32 -148.5(22) . . . . ? N11 Mn1 N31 N32 -145.0(3) . . . . ? N3 Mn1 N31 N32 125.1(3) . . . . ? N1 Mn1 N31 N32 -56.0(3) . . . . ? N11 Mn1 N31 N32 31.2(16) 5_556 . . . ? Mn1 N31 N32 N33 -127.5(37) . . . . ? _refine_diff_density_max 0.287 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.045