# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _audit_creation_method 'SHELXL-97 plus manual editing' _journal_coden_Cambridge 182 loop_ _publ_author_name 'Wright, Dominic S.' 'Alvarez, Carmen Soria' 'Bond, Andrew' 'Cave, Dale' 'Harron, Eilis A.' 'Layfield, Richard A.' 'McPartlin, M.' 'Mosquera, Marta E. G.' 'Rawson, J.' 'Wood, Paul' _publ_contact_author_name 'Andrew D. Bond' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK ; _publ_contact_author_email adb29@cam.ac.uk _publ_contact_author_fax '(01223) 336362' _publ_contact_author_phone '(01223) 336352' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Syntheses and Magnteic Properties of the Hexanuclear [Cp2Mn3(L1)4]2 and Octanuclear [Mn8(L2)12(mu4-O)2]. ; ############################### ## denoted 1.toluene in text ## ############################### data_dw0142 _database_code_CSD 188030 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H60 Mn6 N16, C7 H8' _chemical_formula_sum 'C67 H68 Mn6 N16' _chemical_formula_weight 1427.01 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 31.3272(6) _cell_length_b 33.1940(7) _cell_length_c 15.9032(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16537.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 29610 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5856 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Nonius KappaCCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 29610 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 9362 _reflns_number_gt 7482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+18.1019P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 9362 _refine_ls_number_parameters 340 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1778 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.503 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.102 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 0.15731(2) 0.04862(2) 0.86388(5) 0.0608(2) Uani 1 1 d . A . Mn2 Mn 0.10816(2) -0.043193(19) 0.90932(5) 0.0560(2) Uani 1 1 d . . . Mn3 Mn 0.060875(18) 0.044263(17) 0.93001(4) 0.04247(16) Uani 1 1 d . . . N1 N 0.12363(12) 0.04569(11) 0.9862(3) 0.0515(8) Uani 1 1 d . A . H1 H 0.1265 0.0710 1.0105 0.062 Uiso 1 1 calc R . . N2 N 0.14661(13) -0.01949(13) 1.0146(3) 0.0665(12) Uani 1 1 d . A . C21 C 0.14326(13) 0.01932(14) 1.0392(3) 0.0541(10) Uani 1 1 d . . . C22 C 0.15980(18) 0.03117(17) 1.1187(4) 0.0677(13) Uani 1 1 d . A . H22 H 0.1563 0.0582 1.1371 0.081 Uiso 1 1 calc R . . C23 C 0.1805(2) 0.0045(2) 1.1685(5) 0.090(2) Uani 1 1 d . . . H23 H 0.1920 0.0128 1.2209 0.108 Uiso 1 1 calc R A . C24 C 0.1846(3) -0.0348(2) 1.1424(6) 0.108(3) Uani 1 1 d . A . H24 H 0.1988 -0.0541 1.1764 0.129 Uiso 1 1 calc R . . C25 C 0.1679(2) -0.04530(18) 1.0671(6) 0.101(3) Uani 1 1 d . . . H25 H 0.1712 -0.0725 1.0494 0.121 Uiso 1 1 calc R A . N3 N 0.12869(15) 0.10157(15) 0.8232(3) 0.0727(12) Uani 1 1 d . . . H3 H 0.1422 0.1114 0.7792 0.087 Uiso 1 1 calc R A . N4 N 0.06458(12) 0.10934(11) 0.8959(3) 0.0568(9) Uani 1 1 d . A . C41 C 0.09591(17) 0.12507(16) 0.8442(3) 0.0623(12) Uani 1 1 d . A . C42 C 0.0919(2) 0.16593(18) 0.8187(4) 0.0794(16) Uani 1 1 d . . . H42 H 0.1135 0.1769 0.7835 0.095 Uiso 1 1 calc R A . C43 C 0.0602(2) 0.1893(2) 0.8408(6) 0.101(3) Uani 1 1 d . A . H43 H 0.0584 0.2163 0.8209 0.121 Uiso 1 1 calc R . . C44 C 0.0286(2) 0.17345(18) 0.8954(7) 0.103(3) Uani 1 1 d . . . H44 H 0.0056 0.1895 0.9154 0.124 Uiso 1 1 calc R A . C45 C 0.03277(17) 0.13414(16) 0.9177(5) 0.0779(16) Uani 1 1 d . A . H45 H 0.0110 0.1232 0.9523 0.094 Uiso 1 1 calc R . . N5 N 0.11949(13) -0.00167(13) 0.8066(3) 0.0625(10) Uani 1 1 d . A . H5 H 0.1382 -0.0149 0.7705 0.075 Uiso 1 1 calc R . . N6 N 0.05455(13) 0.03246(13) 0.7952(2) 0.0543(9) Uani 1 1 d . A . C61 C 0.08682(17) 0.01257(19) 0.7565(3) 0.0664(13) Uani 1 1 d . . . C62 C 0.0863(2) 0.0080(3) 0.6683(5) 0.113(3) Uani 1 1 d . A . H62 H 0.1080 -0.0073 0.6418 0.136 Uiso 1 1 calc R . . C63 C 0.0554(3) 0.0250(4) 0.6209(5) 0.152(5) Uani 1 1 d . . . H63 H 0.0555 0.0224 0.5614 0.182 Uiso 1 1 calc R A . C64 C 0.0232(3) 0.0467(3) 0.6622(6) 0.128(4) Uani 1 1 d . A . H64 H 0.0010 0.0594 0.6313 0.153 Uiso 1 1 calc R . . C65 C 0.02443(19) 0.0491(2) 0.7495(4) 0.0747(15) Uani 1 1 d . . . H65 H 0.0024 0.0636 0.7775 0.090 Uiso 1 1 calc R A . N7 N 0.04639(11) -0.02280(10) 0.9498(2) 0.0445(7) Uani 1 1 d . A . H7 H 0.0274 -0.0300 0.9075 0.053 Uiso 1 1 calc R . . N8 N -0.01054(13) -0.05433(12) 1.0241(3) 0.0593(10) Uani 1 1 d . . . C81 C 0.02891(15) -0.03714(14) 1.0242(3) 0.0553(11) Uani 1 1 d . . . C82 C 0.0515(2) -0.0335(2) 1.1009(4) 0.0833(19) Uani 1 1 d . A . H82 H 0.0787 -0.0208 1.1016 0.100 Uiso 1 1 calc R . . C83 C 0.0345(3) -0.0480(3) 1.1735(5) 0.120(4) Uani 1 1 d . . . H83 H 0.0498 -0.0457 1.2249 0.144 Uiso 1 1 calc R A . C84 C -0.0054(3) -0.0663(3) 1.1717(4) 0.115(3) Uani 1 1 d . A . H84 H -0.0177 -0.0771 1.2215 0.138 Uiso 1 1 calc R . . C85 C -0.02689(19) -0.0684(2) 1.0955(4) 0.087(2) Uani 1 1 d . . . H85 H -0.0544 -0.0803 1.0943 0.105 Uiso 1 1 calc R A . C1 C 0.1133(3) -0.1000(3) 0.7970(4) 0.0676(9) Uiso 0.473(5) 1 d PG A 1 H1A H 0.1158 -0.0927 0.7394 0.081 Uiso 0.473(5) 1 calc PR A 1 C2 C 0.14725(19) -0.1032(3) 0.8556(7) 0.0676(9) Uiso 0.473(5) 1 d PG A 1 H2 H 0.1766 -0.0983 0.8443 0.081 Uiso 0.473(5) 1 calc PR A 1 C3 C 0.1297(3) -0.1149(3) 0.9343(5) 0.0676(9) Uiso 0.473(5) 1 d PG A 1 H3A H 0.1453 -0.1192 0.9848 0.081 Uiso 0.473(5) 1 calc PR A 1 C4 C 0.0849(3) -0.1189(3) 0.9242(5) 0.0676(9) Uiso 0.473(5) 1 d PG A 1 H4 H 0.0652 -0.1264 0.9668 0.081 Uiso 0.473(5) 1 calc PR A 1 C5 C 0.0747(2) -0.1097(3) 0.8394(6) 0.0676(9) Uiso 0.473(5) 1 d PG A 1 H5A H 0.0470 -0.1100 0.8152 0.081 Uiso 0.473(5) 1 calc PR A 1 C1' C 0.0947(3) -0.1030(3) 0.7981(4) 0.0676(9) Uiso 0.527(5) 1 d PG A 2 H1' H 0.0802 -0.1002 0.7460 0.081 Uiso 0.527(5) 1 calc PR A 2 C2' C 0.1393(2) -0.0987(3) 0.8112(5) 0.0676(9) Uiso 0.527(5) 1 d PG A 2 H2' H 0.1599 -0.0925 0.7694 0.081 Uiso 0.527(5) 1 calc PR A 2 C3' C 0.14770(19) -0.1053(3) 0.8979(6) 0.0676(9) Uiso 0.527(5) 1 d PG A 2 H3' H 0.1749 -0.1043 0.9242 0.081 Uiso 0.527(5) 1 calc PR A 2 C4' C 0.1083(3) -0.1137(3) 0.9384(3) 0.0676(9) Uiso 0.527(5) 1 d PG A 2 H4' H 0.1045 -0.1192 0.9965 0.081 Uiso 0.527(5) 1 calc PR A 2 C5' C 0.07553(17) -0.1122(3) 0.8767(6) 0.0676(9) Uiso 0.527(5) 1 d PG A 2 H5' H 0.0460 -0.1167 0.8863 0.081 Uiso 0.527(5) 1 calc PR A 2 C11 C 0.22200(16) 0.0326(3) 0.7759(4) 0.130(4) Uani 1 1 d G . . H11 H 0.2179 0.0246 0.7192 0.156 Uiso 1 1 calc R A . C12 C 0.22916(16) 0.0725(3) 0.8046(6) 0.131(4) Uani 1 1 d G A . H12 H 0.2307 0.0959 0.7703 0.157 Uiso 1 1 calc R . . C13 C 0.23367(15) 0.0713(2) 0.8934(6) 0.121(3) Uani 1 1 d G A . H13 H 0.2387 0.0938 0.9290 0.145 Uiso 1 1 calc R . . C14 C 0.22929(14) 0.0307(3) 0.9196(4) 0.111(3) Uani 1 1 d G A . H14 H 0.2309 0.0212 0.9759 0.133 Uiso 1 1 calc R . . C15 C 0.22208(14) 0.00671(18) 0.8471(6) 0.124(3) Uani 1 1 d G A . H15 H 0.2180 -0.0217 0.8462 0.149 Uiso 1 1 calc R . . C1T C 0.1573(8) 0.0831(7) 0.5803(14) 0.231(6) Uiso 0.50 1 d PGD . . H1TA H 0.1478 0.0799 0.6367 0.277 Uiso 0.50 1 calc PR . . C2T C 0.1917(8) 0.0608(7) 0.5509(19) 0.231(6) Uiso 0.50 1 d PGD . . H2TA H 0.2058 0.0423 0.5872 0.277 Uiso 0.50 1 calc PR . . C3T C 0.2056(7) 0.0655(7) 0.468(2) 0.231(6) Uiso 0.50 1 d PGD . . H3TA H 0.2291 0.0502 0.4484 0.277 Uiso 0.50 1 calc PR . . C4T C 0.1850(8) 0.0925(8) 0.4154(16) 0.231(6) Uiso 0.50 1 d PGD . . H4TA H 0.1945 0.0957 0.3591 0.277 Uiso 0.50 1 calc PR . . C5T C 0.1506(8) 0.1148(7) 0.4448(16) 0.231(6) Uiso 0.50 1 d PGD . . H5TA H 0.1365 0.1333 0.4086 0.277 Uiso 0.50 1 calc PR . . C6T C 0.1367(7) 0.1101(7) 0.5273(16) 0.231(6) Uiso 0.50 1 d PGD . . C7T C 0.0972(9) 0.1317(10) 0.555(2) 0.231(6) Uiso 0.50 1 d PD . . H7TA H 0.0876 0.1499 0.5107 0.346 Uiso 0.50 1 calc PR . . H7TB H 0.1035 0.1473 0.6062 0.346 Uiso 0.50 1 calc PR . . H7TC H 0.0747 0.1120 0.5675 0.346 Uiso 0.50 1 calc PR . . 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 0.0428(3) 0.0650(5) 0.0746(5) -0.0044(4) 0.0103(3) 0.0002(3) Mn2 0.0463(3) 0.0445(3) 0.0772(5) -0.0119(3) -0.0088(3) 0.0085(3) Mn3 0.0384(3) 0.0386(3) 0.0504(3) -0.0014(2) 0.0025(2) 0.0005(2) N1 0.0471(18) 0.0457(19) 0.062(2) -0.0045(16) -0.0041(17) -0.0038(15) N2 0.053(2) 0.049(2) 0.098(3) -0.006(2) -0.029(2) 0.0026(17) C21 0.042(2) 0.048(2) 0.072(3) 0.001(2) -0.014(2) -0.0095(18) C22 0.071(3) 0.062(3) 0.070(3) -0.006(2) -0.015(3) -0.024(2) C23 0.090(4) 0.087(4) 0.092(4) 0.005(3) -0.048(4) -0.029(3) C24 0.113(5) 0.070(4) 0.140(7) 0.026(4) -0.075(5) -0.018(4) C25 0.098(5) 0.054(3) 0.150(7) 0.010(3) -0.077(5) -0.001(3) N3 0.067(3) 0.070(3) 0.082(3) 0.014(2) 0.021(2) -0.003(2) N4 0.0506(19) 0.0394(18) 0.081(3) -0.0006(17) -0.0026(18) -0.0018(15) C41 0.069(3) 0.057(3) 0.061(3) 0.009(2) -0.002(2) -0.006(2) C42 0.084(4) 0.059(3) 0.095(4) 0.021(3) -0.004(3) -0.006(3) C43 0.088(4) 0.054(3) 0.160(7) 0.031(4) -0.039(5) -0.004(3) C44 0.068(3) 0.050(3) 0.192(9) 0.014(4) -0.005(4) 0.006(3) C45 0.058(3) 0.053(3) 0.123(5) 0.005(3) -0.001(3) 0.002(2) N5 0.055(2) 0.062(2) 0.071(2) -0.015(2) 0.008(2) 0.0100(18) N6 0.056(2) 0.061(2) 0.0463(19) -0.0021(17) -0.0003(17) 0.0012(18) C61 0.067(3) 0.080(3) 0.052(3) -0.009(2) 0.005(2) 0.003(3) C62 0.093(5) 0.179(8) 0.068(4) -0.035(5) 0.003(4) 0.038(5) C63 0.115(7) 0.286(14) 0.054(4) -0.032(6) -0.010(4) 0.048(8) C64 0.115(7) 0.185(11) 0.082(5) 0.021(5) -0.043(5) 0.016(6) C65 0.069(4) 0.082(4) 0.073(4) 0.005(3) -0.009(3) 0.007(3) N7 0.0442(16) 0.0367(16) 0.053(2) 0.0006(14) -0.0105(15) -0.0012(13) N8 0.055(2) 0.048(2) 0.074(3) 0.0182(18) -0.0212(19) -0.0146(17) C81 0.051(2) 0.048(2) 0.067(3) 0.008(2) -0.016(2) -0.0106(19) C82 0.088(4) 0.097(4) 0.065(3) 0.019(3) -0.023(3) -0.041(3) C83 0.108(5) 0.183(9) 0.070(4) 0.049(5) -0.035(4) -0.075(5) C84 0.114(5) 0.166(8) 0.065(4) 0.052(5) -0.027(4) -0.073(6) C85 0.075(4) 0.099(5) 0.087(4) 0.050(4) -0.026(3) -0.039(3) C11 0.053(4) 0.215(12) 0.122(7) -0.048(8) 0.033(4) -0.004(6) C12 0.056(4) 0.146(9) 0.191(11) 0.030(8) 0.044(5) 0.000(4) C13 0.055(3) 0.149(9) 0.158(9) -0.051(7) 0.009(5) -0.002(4) C14 0.044(3) 0.168(9) 0.122(7) -0.011(7) 0.003(4) 0.007(4) C15 0.048(3) 0.121(7) 0.203(11) -0.023(8) 0.021(5) 0.009(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 N3 2.077(5) . ? Mn1 N1 2.215(4) . ? Mn1 N5 2.240(4) . ? Mn1 C15 2.475(5) . ? Mn1 C14 2.495(5) . ? Mn1 C11 2.519(5) . ? Mn1 C13 2.552(5) . ? Mn1 C12 2.566(5) . ? Mn1 Mn2 3.4901(11) . ? Mn1 Mn3 3.2021(9) . ? Mn2 N7 2.149(3) . ? Mn2 N5 2.166(5) . ? Mn2 N2 2.207(4) . ? Mn2 C4' 2.384(8) . ? Mn2 C3' 2.411(8) . ? Mn2 C2 2.488(9) . ? Mn2 C3 2.504(9) . ? Mn2 C5' 2.563(8) . ? Mn2 C1 2.603(9) . ? Mn2 C2' 2.603(8) . ? Mn2 C4 2.627(9) . ? Mn2 Mn3 3.2757(8) . ? Mn3 N1 2.160(4) . ? Mn3 N6 2.188(4) . ? Mn3 N8 2.200(4) 2 ? Mn3 N4 2.230(4) . ? Mn3 N7 2.293(3) . ? N1 C21 1.362(6) . ? N1 H1 0.9300 . ? N2 C21 1.351(6) . ? N2 C25 1.371(7) . ? C21 C22 1.422(7) . ? C22 C23 1.352(9) . ? C22 H22 0.9500 . ? C23 C24 1.374(10) . ? C23 H23 0.9500 . ? C24 C25 1.352(12) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? N3 C41 1.332(7) . ? N3 H3 0.8800 . ? N4 C45 1.339(7) . ? N4 C41 1.382(7) . ? C41 C42 1.421(8) . ? C42 C43 1.309(10) . ? C42 H42 0.9500 . ? C43 C44 1.419(12) . ? C43 H43 0.9500 . ? C44 C45 1.359(8) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? N5 C61 1.381(7) . ? N5 H5 0.9300 . ? N6 C65 1.313(7) . ? N6 C61 1.356(7) . ? C61 C62 1.410(9) . ? C62 C63 1.348(12) . ? C62 H62 0.9500 . ? C63 C64 1.404(14) . ? C63 H63 0.9500 . ? C64 C65 1.392(12) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? N7 C81 1.387(6) . ? N7 H7 0.9300 . ? N8 C85 1.329(7) . ? N8 C81 1.361(6) . ? N8 Mn3 2.200(4) 2 ? C81 C82 1.416(8) . ? C82 C83 1.360(10) . ? C82 H82 0.9500 . ? C83 C84 1.392(10) . ? C83 H83 0.9500 . ? C84 C85 1.388(9) . ? C84 H84 0.9500 . ? C85 H85 0.9500 . ? C1 C2 1.4200 . ? C1 C5 1.4200 . ? C1 H1A 0.9500 . ? C2 C3 1.4200 . ? C2 H2 0.9500 . ? C3 C4 1.4200 . ? C3 H3A 0.9500 . ? C4 C5 1.4200 . ? C4 H4 0.9500 . ? C5 H5A 0.9500 . ? C1' C2' 1.4200 . ? C1' C5' 1.4200 . ? C1' H1' 0.9500 . ? C2' C3' 1.4200 . ? C2' H2' 0.9500 . ? C3' C4' 1.4200 . ? C3' H3' 0.9500 . ? C4' C5' 1.4200 . ? C4' H4' 0.9500 . ? C5' H5' 0.9500 . ? C11 C12 1.4200 . ? C11 C15 1.4200 . ? C11 H11 0.9500 . ? C12 C13 1.4200 . ? C12 H12 0.9500 . ? C13 C14 1.4200 . ? C13 H13 0.9500 . ? C14 C15 1.4200 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C1T C2T 1.3900 . ? C1T C6T 1.3900 . ? C1T H1TA 0.9500 . ? C2T C3T 1.3900 . ? C2T H2TA 0.9500 . ? C3T C4T 1.3900 . ? C3T H3TA 0.9500 . ? C4T C5T 1.3900 . ? C4T H4TA 0.9500 . ? C5T C6T 1.3900 . ? C5T H5TA 0.9500 . ? C6T C7T 1.497(12) . ? C7T H7TA 0.9800 . ? C7T H7TB 0.9800 . ? C7T H7TC 0.9800 . ? 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 N3 Mn1 N1 96.03(17) . . ? N3 Mn1 N5 106.00(19) . . ? N1 Mn1 N5 94.14(15) . . ? N3 Mn1 C15 142.8(2) . . ? N1 Mn1 C15 117.4(3) . . ? N5 Mn1 C15 88.33(18) . . ? N3 Mn1 C14 134.7(3) . . ? N1 Mn1 C14 96.20(18) . . ? N5 Mn1 C14 116.4(3) . . ? C15 Mn1 C14 33.20(6) . . ? N3 Mn1 C11 110.7(3) . . ? N1 Mn1 C11 149.5(2) . . ? N5 Mn1 C11 92.4(2) . . ? C15 Mn1 C11 33.02(6) . . ? C14 Mn1 C11 54.54(6) . . ? N3 Mn1 C13 102.2(2) . . ? N1 Mn1 C13 107.3(2) . . ? N5 Mn1 C13 142.26(17) . . ? C15 Mn1 C13 54.37(6) . . ? C14 Mn1 C13 32.66(5) . . ? C11 Mn1 C13 53.88(6) . . ? N3 Mn1 C12 90.14(19) . . ? N1 Mn1 C12 139.0(3) . . ? N5 Mn1 C12 123.0(3) . . ? C15 Mn1 C12 54.19(6) . . ? C14 Mn1 C12 53.97(6) . . ? C11 Mn1 C12 32.41(6) . . ? C13 Mn1 C12 32.22(5) . . ? N3 Mn1 Mn3 74.53(12) . . ? N1 Mn1 Mn3 42.28(10) . . ? N5 Mn1 Mn3 66.47(10) . . ? C15 Mn1 Mn3 141.60(17) . . ? C14 Mn1 Mn3 136.48(15) . . ? C11 Mn1 Mn3 158.70(18) . . ? C13 Mn1 Mn3 146.87(17) . . ? C12 Mn1 Mn3 164.19(17) . . ? N7 Mn2 N5 99.96(14) . . ? N7 Mn2 N2 98.72(15) . . ? N5 Mn2 N2 104.80(17) . . ? N7 Mn2 C4' 104.6(2) . . ? N5 Mn2 C4' 140.36(18) . . ? N2 Mn2 C4' 101.7(2) . . ? N7 Mn2 C3' 139.0(2) . . ? N5 Mn2 C3' 113.8(2) . . ? N2 Mn2 C3' 94.68(19) . . ? C4' Mn2 C3' 34.44(10) . . ? N7 Mn2 C2 142.95(17) . . ? N5 Mn2 C2 99.8(2) . . ? N2 Mn2 C2 106.1(2) . . ? C4' Mn2 C2 44.01(19) . . ? C3' Mn2 C2 15.76(19) . . ? N7 Mn2 C3 119.6(3) . . ? N5 Mn2 C3 132.8(2) . . ? N2 Mn2 C3 94.08(18) . . ? C4' Mn2 C3 15.65(19) . . ? C3' Mn2 C3 20.22(19) . . ? C2 Mn2 C3 33.04(11) . . ? N7 Mn2 C5' 89.04(16) . . ? N5 Mn2 C5' 118.8(2) . . ? N2 Mn2 C5' 133.6(2) . . ? C4' Mn2 C5' 33.12(10) . . ? C3' Mn2 C5' 54.92(12) . . ? C2 Mn2 C5' 53.94(19) . . ? C3 Mn2 C5' 44.79(19) . . ? N7 Mn2 C1 119.3(2) . . ? N5 Mn2 C1 86.19(19) . . ? N2 Mn2 C1 138.2(2) . . ? C4' Mn2 C1 54.70(19) . . ? C3' Mn2 C1 45.38(19) . . ? C2 Mn2 C1 32.29(11) . . ? C3 Mn2 C1 53.43(13) . . ? C5' Mn2 C1 40.31(18) . . ? N7 Mn2 C2' 137.7(2) . . ? N5 Mn2 C2' 86.40(19) . . ? N2 Mn2 C2' 120.1(2) . . ? C4' Mn2 C2' 54.65(12) . . ? C3' Mn2 C2' 32.61(10) . . ? C2 Mn2 C2' 17.05(19) . . ? C3 Mn2 C2' 47.30(19) . . ? C5' Mn2 C2' 52.81(11) . . ? C1 Mn2 C2' 18.76(18) . . ? N7 Mn2 C4 91.40(19) . . ? N5 Mn2 C4 136.2(2) . . ? N2 Mn2 C4 115.1(2) . . ? C4' Mn2 C4 17.17(18) . . ? C3' Mn2 C4 48.07(19) . . ? C2 Mn2 C4 53.29(12) . . ? C3 Mn2 C4 32.01(10) . . ? C5' Mn2 C4 18.58(18) . . ? C1 Mn2 C4 52.12(12) . . ? C2' Mn2 C4 58.76(19) . . ? N1 Mn3 N6 119.43(15) . . ? N1 Mn3 N8 111.58(16) . 2 ? N6 Mn3 N8 128.97(16) . 2 ? N1 Mn3 N4 91.83(14) . . ? N6 Mn3 N4 86.56(16) . . ? N8 Mn3 N4 93.20(15) 2 . ? N1 Mn3 N7 98.31(13) . . ? N6 Mn3 N7 86.73(14) . . ? N8 Mn3 N7 84.95(14) 2 . ? N4 Mn3 N7 169.67(13) . . ? N1 Mn3 Mn1 43.62(11) . . ? N6 Mn3 Mn1 76.81(11) . . ? N8 Mn3 Mn1 153.24(12) 2 . ? N4 Mn3 Mn1 80.05(10) . . ? N7 Mn3 Mn1 106.00(9) . . ? C21 N1 Mn3 130.8(3) . . ? C21 N1 Mn1 110.9(3) . . ? Mn3 N1 Mn1 94.10(16) . . ? C21 N1 H1 106.2 . . ? Mn3 N1 H1 106.2 . . ? Mn1 N1 H1 106.2 . . ? C21 N2 C25 117.2(5) . . ? C21 N2 Mn2 121.2(3) . . ? C25 N2 Mn2 120.3(4) . . ? N2 C21 N1 117.9(4) . . ? N2 C21 C22 119.6(5) . . ? N1 C21 C22 122.5(5) . . ? C23 C22 C21 120.9(5) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.3(6) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 118.5(6) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C24 C25 N2 124.5(6) . . ? C24 C25 H25 117.8 . . ? N2 C25 H25 117.8 . . ? C41 N3 Mn1 138.6(4) . . ? C41 N3 H3 110.7 . . ? Mn1 N3 H3 110.7 . . ? C45 N4 C41 116.8(4) . . ? C45 N4 Mn3 119.6(3) . . ? C41 N4 Mn3 123.2(3) . . ? N3 C41 N4 118.4(4) . . ? N3 C41 C42 123.7(5) . . ? N4 C41 C42 117.9(5) . . ? C43 C42 C41 123.8(6) . . ? C43 C42 H42 118.1 . . ? C41 C42 H42 118.1 . . ? C42 C43 C44 118.3(6) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 116.7(6) . . ? C45 C44 H44 121.7 . . ? C43 C44 H44 121.7 . . ? N4 C45 C44 126.5(6) . . ? N4 C45 H45 116.7 . . ? C44 C45 H45 116.7 . . ? C61 N5 Mn2 122.1(4) . . ? C61 N5 Mn1 111.8(4) . . ? Mn2 N5 Mn1 104.74(19) . . ? C61 N5 H5 105.6 . . ? Mn2 N5 H5 105.6 . . ? Mn1 N5 H5 105.6 . . ? C65 N6 C61 119.3(5) . . ? C65 N6 Mn3 122.1(4) . . ? C61 N6 Mn3 117.7(3) . . ? N6 C61 N5 117.2(4) . . ? N6 C61 C62 119.7(6) . . ? N5 C61 C62 123.1(5) . . ? C63 C62 C61 121.3(7) . . ? C63 C62 H62 119.3 . . ? C61 C62 H62 119.3 . . ? C62 C63 C64 117.9(7) . . ? C62 C63 H63 121.0 . . ? C64 C63 H63 121.0 . . ? C65 C64 C63 118.5(7) . . ? C65 C64 H64 120.8 . . ? C63 C64 H64 120.8 . . ? N6 C65 C64 123.2(7) . . ? N6 C65 H65 118.4 . . ? C64 C65 H65 118.4 . . ? C81 N7 Mn2 120.2(3) . . ? C81 N7 Mn3 121.9(3) . . ? Mn2 N7 Mn3 94.96(13) . . ? C81 N7 H7 106.1 . . ? Mn2 N7 H7 106.1 . . ? Mn3 N7 H7 106.1 . . ? C85 N8 C81 119.8(4) . . ? C85 N8 Mn3 111.0(3) . 2 ? C81 N8 Mn3 126.0(3) . 2 ? N8 C81 N7 120.1(4) . . ? N8 C81 C82 119.4(5) . . ? N7 C81 C82 120.5(4) . . ? C83 C82 C81 120.3(5) . . ? C83 C82 H82 119.8 . . ? C81 C82 H82 119.8 . . ? C82 C83 C84 119.3(6) . . ? C82 C83 H83 120.3 . . ? C84 C83 H83 120.3 . . ? C85 C84 C83 118.4(6) . . ? C85 C84 H84 120.8 . . ? C83 C84 H84 120.8 . . ? N8 C85 C84 122.8(5) . . ? N8 C85 H85 118.6 . . ? C84 C85 H85 118.6 . . ? C2 C1 C5 108.0 . . ? C2 C1 Mn2 69.4(3) . . ? C5 C1 Mn2 77.7(3) . . ? C2 C1 H1A 126.0 . . ? C5 C1 H1A 126.0 . . ? Mn2 C1 H1A 118.7 . . ? C1 C2 C3 108.0 . . ? C1 C2 Mn2 78.3(3) . . ? C3 C2 Mn2 74.1(4) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Mn2 C2 H2 113.9 . . ? C4 C3 C2 108.0 . . ? C4 C3 Mn2 78.8(3) . . ? C2 C3 Mn2 72.9(4) . . ? C4 C3 H3A 126.0 . . ? C2 C3 H3A 126.0 . . ? Mn2 C3 H3A 114.6 . . ? C3 C4 C5 108.0 . . ? C3 C4 Mn2 69.2(3) . . ? C5 C4 Mn2 76.8(3) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Mn2 C4 H4 119.8 . . ? C4 C5 C1 108.0 . . ? C4 C5 H5A 126.0 . . ? C1 C5 H5A 126.0 . . ? C2' C1' C5' 108.0 . . ? C2' C1' H1' 126.0 . . ? C5' C1' H1' 126.0 . . ? C1' C2' C3' 108.0 . . ? C1' C2' Mn2 77.9(3) . . ? C3' C2' Mn2 66.2(3) . . ? C1' C2' H2' 126.0 . . ? C3' C2' H2' 126.0 . . ? Mn2 C2' H2' 121.4 . . ? C4' C3' C2' 108.0 . . ? C4' C3' Mn2 71.7(3) . . ? C2' C3' Mn2 81.2(3) . . ? C4' C3' H3' 126.0 . . ? C2' C3' H3' 126.0 . . ? Mn2 C3' H3' 113.4 . . ? C3' C4' C5' 108.0 . . ? C3' C4' Mn2 73.8(3) . . ? C5' C4' Mn2 80.4(3) . . ? C3' C4' H4' 126.0 . . ? C5' C4' H4' 126.0 . . ? Mn2 C4' H4' 112.3 . . ? C4' C5' C1' 108.0 . . ? C4' C5' Mn2 66.5(3) . . ? C1' C5' Mn2 79.4(3) . . ? C4' C5' H5' 126.0 . . ? C1' C5' H5' 126.0 . . ? Mn2 C5' H5' 119.7 . . ? C12 C11 C15 108.0 . . ? C12 C11 Mn1 75.6(2) . . ? C15 C11 Mn1 71.8(2) . . ? C12 C11 H11 126.0 . . ? C15 C11 H11 126.0 . . ? Mn1 C11 H11 118.5 . . ? C13 C12 C11 108.0 . . ? C13 C12 Mn1 73.33(19) . . ? C11 C12 Mn1 72.0(2) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? Mn1 C12 H12 120.5 . . ? C12 C13 C14 108.0 . . ? C12 C13 Mn1 74.5(2) . . ? C14 C13 Mn1 71.5(2) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Mn1 C13 H13 119.9 . . ? C15 C14 C13 108.0 . . ? C15 C14 Mn1 72.6(2) . . ? C13 C14 Mn1 75.9(2) . . ? C15 C14 H14 126.0 . . ? C13 C14 H14 126.0 . . ? Mn1 C14 H14 117.5 . . ? C14 C15 C11 108.0 . . ? C14 C15 Mn1 74.2(2) . . ? C11 C15 Mn1 75.2(2) . . ? C14 C15 H15 126.0 . . ? C11 C15 H15 126.0 . . ? Mn1 C15 H15 116.7 . . ? C2T C1T C6T 120.0 . . ? C2T C1T H1TA 120.0 . . ? C6T C1T H1TA 120.0 . . ? C3T C2T C1T 120.0 . . ? C3T C2T H2TA 120.0 . . ? C1T C2T H2TA 120.0 . . ? C2T C3T C4T 120.0 . . ? C2T C3T H3TA 120.0 . . ? C4T C3T H3TA 120.0 . . ? C5T C4T C3T 120.0 . . ? C5T C4T H4TA 120.0 . . ? C3T C4T H4TA 120.0 . . ? C6T C5T C4T 120.0 . . ? C6T C5T H5TA 120.0 . . ? C4T C5T H5TA 120.0 . . ? C5T C6T C1T 120.0 . . ? C5T C6T C7T 119.1(11) . . ? C1T C6T C7T 120.7(11) . . ? C6T C7T H7TA 109.5 . . ? C6T C7T H7TB 109.5 . . ? H7TA C7T H7TB 109.5 . . ? C6T C7T H7TC 109.5 . . ? H7TA C7T H7TC 109.5 . . ? H7TB C7T H7TC 109.5 . . ? #===END ############################ ## denoted 2.2thf in text ## ############################ data_dw0212 _database_code_CSD 188031 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H72 Br12 Mn8 N24 O2, 2(C4 H8 O)' _chemical_formula_sum 'C80 H88 Br12 Mn8 N24 O4' _chemical_formula_weight 2848.18 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' 'Br' 'Br' -0.2901 2.4595 '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 trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 15.8023(11) _cell_length_b 15.8023(11) _cell_length_c 34.803(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7526.4(9) _cell_formula_units_Z 3 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9167 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4164 _exptl_absorpt_coefficient_mu 5.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.508 _exptl_absorpt_correction_T_max 0.559 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Nonius KappaCCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 6760 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 25.02 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 2939 _reflns_number_gt 2006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97(Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+115.3428P] 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 2939 _refine_ls_number_parameters 200 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.828 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.112 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 0.20154(7) 0.54877(7) 0.20684(3) 0.0297(3) Uani 1 1 d . . . Mn2 Mn 0.3333 0.6667 0.27732(5) 0.0337(4) Uani 1 3 d S . . O1 O 0.3333 0.6667 0.21902(18) 0.0271(16) Uani 1 3 d S . . Br1 Br 0.02457(8) 0.58397(8) 0.35498(3) 0.0692(3) Uani 1 1 d . . . N1 N 0.0910(4) 0.5016(4) 0.25163(15) 0.0378(14) Uani 1 1 d . . . N2 N 0.1915(5) 0.6093(5) 0.29856(15) 0.0397(14) Uani 1 1 d D . . H2N H 0.186(5) 0.630(5) 0.3215(9) 0.034(19) Uiso 1 1 d D . . C1 C 0.1025(5) 0.5474(5) 0.28644(18) 0.0352(16) Uani 1 1 d . . . C2 C 0.0121(6) 0.5212(6) 0.3065(2) 0.048(2) Uani 1 1 d . . . C3 C -0.0831(6) 0.4554(6) 0.2911(2) 0.0466(19) Uiso 1 1 d . . . H3A H -0.1410 0.4438 0.3040 0.056 Uiso 1 1 calc R . . C4 C -0.0868(6) 0.4122(6) 0.2585(3) 0.055(2) Uani 1 1 d . . . C5 C -0.0003(6) 0.4363(6) 0.2388(2) 0.0473(19) Uani 1 1 d . . . H5A H -0.0057 0.4050 0.2149 0.057 Uiso 1 1 calc R . . C6 C -0.1841(6) 0.3394(7) 0.2417(3) 0.069(3) Uani 1 1 d . . . H6A H -0.2243 0.3700 0.2385 0.104 Uiso 1 1 calc R . . H6B H -0.2172 0.2831 0.2590 0.104 Uiso 1 1 calc R . . H6C H -0.1740 0.3175 0.2167 0.104 Uiso 1 1 calc R . . Br2 Br -0.00398(6) 0.24403(6) 0.15122(2) 0.0565(3) Uani 1 1 d . . . N3 N 0.1042(4) 0.5215(4) 0.10701(14) 0.0338(13) Uani 1 1 d . . . N4 N 0.1657(4) 0.4638(4) 0.15425(15) 0.0321(13) Uani 1 1 d D . . H4N H 0.160(6) 0.407(3) 0.161(2) 0.05(2) Uiso 1 1 d D . . C7 C 0.0960(5) 0.4453(5) 0.12766(17) 0.0309(15) Uani 1 1 d . . . C8 C 0.0172(5) 0.3500(5) 0.11905(19) 0.0400(17) Uani 1 1 d . . . C9 C -0.0439(6) 0.3349(6) 0.0889(2) 0.052(2) Uani 1 1 d . . . H9A H -0.0950 0.2707 0.0831 0.062 Uiso 1 1 calc R . . C10 C -0.0315(6) 0.4136(6) 0.0664(2) 0.050(2) Uani 1 1 d . . . C11 C 0.0418(5) 0.5043(6) 0.0777(2) 0.0424(18) Uani 1 1 d . . . H11A H 0.0492 0.5592 0.0637 0.051 Uiso 1 1 calc R . . C12 C -0.0943(7) 0.3975(7) 0.0317(3) 0.075(3) Uani 1 1 d . . . H12A H -0.0826 0.4607 0.0220 0.112 Uiso 1 1 calc R . . H12B H -0.1633 0.3571 0.0388 0.112 Uiso 1 1 calc R . . H12C H -0.0781 0.3643 0.0117 0.112 Uiso 1 1 calc R . . O1S O -0.263(2) 0.386(3) 0.0995(8) 0.170(10) Uiso 0.33 1 d PD A -1 C2S C -0.294(4) 0.284(4) 0.1093(13) 0.170(10) Uiso 0.33 1 d PD A -1 H2S1 H -0.3087 0.2441 0.0857 0.204 Uiso 0.33 1 calc PR A -1 H2S2 H -0.2424 0.2802 0.1238 0.204 Uiso 0.33 1 calc PR A -1 C3S C -0.382(4) 0.249(3) 0.1328(15) 0.170(10) Uiso 0.33 1 d PD A -1 H3S1 H -0.4413 0.2085 0.1171 0.204 Uiso 0.33 1 calc PR A -1 H3S2 H -0.3810 0.2084 0.1543 0.204 Uiso 0.33 1 calc PR A -1 C4S C -0.383(3) 0.334(4) 0.1475(11) 0.170(10) Uiso 0.33 1 d PD A -1 H4S1 H -0.3719 0.3398 0.1756 0.204 Uiso 0.33 1 calc PR A -1 H4S2 H -0.4477 0.3285 0.1425 0.204 Uiso 0.33 1 calc PR A -1 C5S C -0.307(5) 0.420(3) 0.1282(14) 0.170(10) Uiso 0.33 1 d PD A -1 H5S1 H -0.2566 0.4632 0.1469 0.204 Uiso 0.33 1 calc PR A -1 H5S2 H -0.3342 0.4569 0.1156 0.204 Uiso 0.33 1 calc PR A -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 0.0311(6) 0.0316(6) 0.0258(5) 0.0000(4) 0.0011(4) 0.0152(5) Mn2 0.0379(7) 0.0379(7) 0.0254(9) 0.000 0.000 0.0190(3) O1 0.030(3) 0.030(3) 0.021(4) 0.000 0.000 0.0151(13) Br1 0.0800(7) 0.0787(7) 0.0552(5) 0.0011(5) 0.0260(5) 0.0445(6) N1 0.036(3) 0.041(4) 0.034(3) 0.009(3) 0.005(3) 0.018(3) N2 0.047(4) 0.044(4) 0.029(3) 0.000(3) 0.005(3) 0.023(3) C1 0.043(4) 0.039(4) 0.028(3) 0.008(3) 0.008(3) 0.023(4) C2 0.067(6) 0.055(5) 0.035(4) 0.012(4) 0.018(4) 0.041(5) C4 0.041(5) 0.041(5) 0.073(6) 0.016(4) -0.006(4) 0.012(4) C5 0.045(5) 0.040(4) 0.046(4) 0.007(4) 0.002(4) 0.014(4) C6 0.044(5) 0.060(6) 0.092(7) 0.009(5) -0.003(5) 0.018(5) Br2 0.0560(5) 0.0337(4) 0.0655(5) 0.0040(4) -0.0050(4) 0.0117(4) N3 0.037(3) 0.035(3) 0.029(3) -0.004(3) -0.005(3) 0.018(3) N4 0.032(3) 0.031(3) 0.034(3) -0.006(3) -0.004(3) 0.016(3) C7 0.030(4) 0.039(4) 0.028(3) -0.005(3) -0.001(3) 0.021(3) C8 0.037(4) 0.036(4) 0.042(4) -0.001(3) 0.000(3) 0.014(4) C9 0.036(4) 0.044(5) 0.063(5) -0.014(4) -0.015(4) 0.010(4) C10 0.045(5) 0.050(5) 0.051(5) -0.006(4) -0.019(4) 0.020(4) C11 0.039(4) 0.050(5) 0.040(4) -0.003(4) -0.010(3) 0.023(4) C12 0.079(7) 0.076(7) 0.069(6) -0.011(5) -0.037(5) 0.039(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.0268(17) . ? Mn1 N4 2.171(5) . ? Mn1 N1 2.176(6) . ? Mn1 N4 2.317(6) 14_455 ? Mn1 N3 2.334(5) 15 ? Mn1 Mn2 3.1536(16) . ? Mn1 Mn1 3.4277(16) 15 ? Mn1 Mn1 3.4329(17) 2_665 ? Mn2 O1 2.029(7) . ? Mn2 N2 2.088(6) 3_565 ? Mn2 N2 2.088(6) . ? Mn2 N2 2.088(6) 2_665 ? Mn2 Mn1 3.1536(16) 3_565 ? Mn2 Mn1 3.1536(16) 2_665 ? O1 Mn1 2.0268(17) 3_565 ? O1 Mn1 2.0268(17) 2_665 ? Br1 C2 1.915(7) . ? N1 C5 1.362(9) . ? N1 C1 1.376(8) . ? N2 C1 1.318(9) . ? N2 H2N 0.88(1) . ? C1 C2 1.452(10) . ? C2 C3 1.439(11) . ? C3 C4 1.309(11) . ? C3 H3A 0.9500 . ? C4 C5 1.402(11) . ? C4 C6 1.504(11) . ? C5 H5A 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Br2 C8 1.900(7) . ? N3 C11 1.348(8) . ? N3 C7 1.351(8) . ? N3 Mn1 2.335(5) 14_455 ? N4 C7 1.354(8) . ? N4 Mn1 2.317(6) 15 ? N4 H4N 0.88(1) . ? C7 C8 1.425(10) . ? C8 C9 1.365(10) . ? C9 C10 1.397(11) . ? C9 H9A 0.9500 . ? C10 C11 1.375(10) . ? C10 C12 1.502(10) . ? C11 H11A 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O1S C5S 1.460(18) . ? O1S C2S 1.466(18) . ? C2S C3S 1.462(18) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.451(18) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.454(18) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 N4 125.1(2) . . ? O1 Mn1 N1 116.4(2) . . ? N4 Mn1 N1 118.4(2) . . ? O1 Mn1 N4 97.69(16) . 14_455 ? N4 Mn1 N4 86.96(9) . 14_455 ? N1 Mn1 N4 87.7(2) . 14_455 ? O1 Mn1 N3 93.49(15) . 15 ? N4 Mn1 N3 82.1(2) . 15 ? N1 Mn1 N3 92.3(2) . 15 ? N4 Mn1 N3 167.5(2) 14_455 15 ? O1 Mn1 Mn2 39.00(18) . . ? N4 Mn1 Mn2 155.80(15) . . ? N1 Mn1 Mn2 79.91(16) . . ? N4 Mn1 Mn2 110.75(14) 14_455 . ? N3 Mn1 Mn2 81.50(13) 15 . ? O1 Mn2 N2 110.73(16) . 3_565 ? O1 Mn2 N2 110.73(16) . . ? N2 Mn2 N2 108.19(17) 3_565 . ? O1 Mn2 N2 110.73(16) . 2_665 ? N2 Mn2 N2 108.19(17) 3_565 2_665 ? N2 Mn2 N2 108.19(17) . 2_665 ? O1 Mn2 Mn1 38.94(3) . . ? N2 Mn2 Mn1 142.03(17) 3_565 . ? N2 Mn2 Mn1 76.72(16) . . ? N2 Mn2 Mn1 105.49(16) 2_665 . ? O1 Mn2 Mn1 38.94(3) . 3_565 ? N2 Mn2 Mn1 76.72(16) 3_565 3_565 ? N2 Mn2 Mn1 105.49(16) . 3_565 ? N2 Mn2 Mn1 142.03(17) 2_665 3_565 ? Mn1 Mn2 Mn1 65.95(4) . 3_565 ? O1 Mn2 Mn1 38.94(3) . 2_665 ? N2 Mn2 Mn1 105.49(16) 3_565 2_665 ? N2 Mn2 Mn1 142.03(17) . 2_665 ? N2 Mn2 Mn1 76.72(16) 2_665 2_665 ? Mn1 Mn2 Mn1 65.95(4) . 2_665 ? Mn1 Mn2 Mn1 65.95(4) 3_565 2_665 ? Mn1 O1 Mn1 115.75(12) 3_565 . ? Mn1 O1 Mn1 115.75(12) 3_565 2_665 ? Mn1 O1 Mn1 115.75(12) . 2_665 ? Mn1 O1 Mn2 102.07(18) 3_565 . ? Mn1 O1 Mn2 102.07(18) . . ? Mn1 O1 Mn2 102.07(18) 2_665 . ? C5 N1 C1 119.8(6) . . ? C5 N1 Mn1 113.0(5) . . ? C1 N1 Mn1 125.4(5) . . ? C1 N2 Mn2 136.4(5) . . ? C1 N2 H2N 107(4) . . ? Mn2 N2 H2N 117(4) . . ? N2 C1 N1 118.9(6) . . ? N2 C1 C2 126.1(6) . . ? N1 C1 C2 115.0(7) . . ? C3 C2 C1 123.4(7) . . ? C3 C2 Br1 120.1(6) . . ? C1 C2 Br1 116.4(6) . . ? C4 C3 C2 117.2(7) . . ? C4 C3 H3A 121.4 . . ? C2 C3 H3A 121.4 . . ? C3 C4 C5 119.9(8) . . ? C3 C4 C6 119.9(8) . . ? C5 C4 C6 120.2(8) . . ? N1 C5 C4 124.5(7) . . ? N1 C5 H5A 117.8 . . ? C4 C5 H5A 117.8 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C11 N3 C7 119.2(6) . . ? C11 N3 Mn1 121.2(5) . 14_455 ? C7 N3 Mn1 119.3(4) . 14_455 ? C7 N4 Mn1 130.0(4) . . ? C7 N4 Mn1 111.3(4) . 15 ? Mn1 N4 Mn1 99.6(2) . 15 ? C7 N4 H4N 107(5) . . ? Mn1 N4 H4N 106(5) . . ? Mn1 N4 H4N 99(5) 15 . ? N3 C7 N4 117.8(6) . . ? N3 C7 C8 118.2(6) . . ? N4 C7 C8 123.9(6) . . ? C9 C8 C7 121.0(7) . . ? C9 C8 Br2 120.1(6) . . ? C7 C8 Br2 118.9(5) . . ? C8 C9 C10 120.2(7) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 115.9(7) . . ? C11 C10 C12 123.2(8) . . ? C9 C10 C12 120.8(7) . . ? N3 C11 C10 125.3(7) . . ? N3 C11 H11A 117.4 . . ? C10 C11 H11A 117.4 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5S O1S C2S 106.5(8) . . ? C3S C2S O1S 106.4(8) . . ? C3S C2S H2S1 110.5 . . ? O1S C2S H2S1 110.5 . . ? C3S C2S H2S2 110.5 . . ? O1S C2S H2S2 110.5 . . ? H2S1 C2S H2S2 108.6 . . ? C4S C3S C2S 107.2(7) . . ? C4S C3S H3S1 110.3 . . ? C2S C3S H3S1 110.3 . . ? C4S C3S H3S2 110.3 . . ? C2S C3S H3S2 110.3 . . ? H3S1 C3S H3S2 108.5 . . ? C3S C4S C5S 108.1(6) . . ? C3S C4S H4S1 110.1 . . ? C5S C4S H4S1 110.1 . . ? C3S C4S H4S2 110.1 . . ? C5S C4S H4S2 110.1 . . ? H4S1 C4S H4S2 108.4 . . ? C4S C5S O1S 107.5(6) . . ? C4S C5S H5S1 110.2 . . ? O1S C5S H5S1 110.2 . . ? C4S C5S H5S2 110.2 . . ? O1S C5S H5S2 110.2 . . ? H5S1 C5S H5S2 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Mn1 Mn2 O1 58.7(4) . . . . ? N1 Mn1 Mn2 O1 -159.68(16) . . . . ? N4 Mn1 Mn2 O1 -76.08(15) 14_455 . . . ? N3 Mn1 Mn2 O1 106.40(14) 15 . . . ? O1 Mn1 Mn2 N2 47.9(3) . . . 3_565 ? N4 Mn1 Mn2 N2 106.6(5) . . . 3_565 ? N1 Mn1 Mn2 N2 -111.8(3) . . . 3_565 ? N4 Mn1 Mn2 N2 -28.2(3) 14_455 . . 3_565 ? N3 Mn1 Mn2 N2 154.3(3) 15 . . 3_565 ? O1 Mn1 Mn2 N2 150.53(17) . . . . ? N4 Mn1 Mn2 N2 -150.7(4) . . . . ? N1 Mn1 Mn2 N2 -9.2(2) . . . . ? N4 Mn1 Mn2 N2 74.5(2) 14_455 . . . ? N3 Mn1 Mn2 N2 -103.1(2) 15 . . . ? O1 Mn1 Mn2 N2 -103.96(18) . . . 2_665 ? N4 Mn1 Mn2 N2 -45.2(4) . . . 2_665 ? N1 Mn1 Mn2 N2 96.4(2) . . . 2_665 ? N4 Mn1 Mn2 N2 180.0(2) 14_455 . . 2_665 ? N3 Mn1 Mn2 N2 2.4(2) 15 . . 2_665 ? O1 Mn1 Mn2 Mn1 36.585(10) . . . 3_565 ? N4 Mn1 Mn2 Mn1 95.3(4) . . . 3_565 ? N1 Mn1 Mn2 Mn1 -123.10(16) . . . 3_565 ? N4 Mn1 Mn2 Mn1 -39.49(15) 14_455 . . 3_565 ? N3 Mn1 Mn2 Mn1 142.99(14) 15 . . 3_565 ? O1 Mn1 Mn2 Mn1 -36.585(10) . . . 2_665 ? N4 Mn1 Mn2 Mn1 22.1(4) . . . 2_665 ? N1 Mn1 Mn2 Mn1 163.73(16) . . . 2_665 ? N4 Mn1 Mn2 Mn1 -112.66(14) 14_455 . . 2_665 ? N3 Mn1 Mn2 Mn1 69.81(14) 15 . . 2_665 ? N4 Mn1 O1 Mn1 95.5(3) . . . 3_565 ? N1 Mn1 O1 Mn1 -87.5(3) . . . 3_565 ? N4 Mn1 O1 Mn1 3.8(3) 14_455 . . 3_565 ? N3 Mn1 O1 Mn1 178.2(3) 15 . . 3_565 ? Mn2 Mn1 O1 Mn1 -109.9(3) . . . 3_565 ? N4 Mn1 O1 Mn1 -44.7(4) . . . 2_665 ? N1 Mn1 O1 Mn1 132.3(3) . . . 2_665 ? N4 Mn1 O1 Mn1 -136.4(3) 14_455 . . 2_665 ? N3 Mn1 O1 Mn1 38.0(3) 15 . . 2_665 ? Mn2 Mn1 O1 Mn1 109.9(3) . . . 2_665 ? N4 Mn1 O1 Mn2 -154.6(2) . . . . ? N1 Mn1 O1 Mn2 22.44(18) . . . . ? N4 Mn1 O1 Mn2 113.67(13) 14_455 . . . ? N3 Mn1 O1 Mn2 -71.91(13) 15 . . . ? N2 Mn2 O1 Mn1 -30.80(18) 3_565 . . 3_565 ? N2 Mn2 O1 Mn1 89.20(18) . . . 3_565 ? N2 Mn2 O1 Mn1 -150.80(18) 2_665 . . 3_565 ? Mn1 Mn2 O1 Mn1 120.0 . . . 3_565 ? Mn1 Mn2 O1 Mn1 -120.0 2_665 . . 3_565 ? N2 Mn2 O1 Mn1 -150.80(18) 3_565 . . . ? N2 Mn2 O1 Mn1 -30.80(18) . . . . ? N2 Mn2 O1 Mn1 89.20(18) 2_665 . . . ? Mn1 Mn2 O1 Mn1 -120.0 3_565 . . . ? Mn1 Mn2 O1 Mn1 120.0 2_665 . . . ? N2 Mn2 O1 Mn1 89.20(18) 3_565 . . 2_665 ? N2 Mn2 O1 Mn1 -150.80(18) . . . 2_665 ? N2 Mn2 O1 Mn1 -30.80(18) 2_665 . . 2_665 ? Mn1 Mn2 O1 Mn1 -120.0 . . . 2_665 ? Mn1 Mn2 O1 Mn1 120.0 3_565 . . 2_665 ? O1 Mn1 N1 C5 167.0(4) . . . . ? N4 Mn1 N1 C5 -15.8(6) . . . . ? N4 Mn1 N1 C5 69.5(5) 14_455 . . . ? N3 Mn1 N1 C5 -98.0(5) 15 . . . ? Mn2 Mn1 N1 C5 -178.9(5) . . . . ? O1 Mn1 N1 C1 2.7(6) . . . . ? N4 Mn1 N1 C1 180.0(5) . . . . ? N4 Mn1 N1 C1 -94.7(5) 14_455 . . . ? N3 Mn1 N1 C1 97.8(5) 15 . . . ? Mn2 Mn1 N1 C1 16.8(5) . . . . ? O1 Mn2 N2 C1 26.6(7) . . . . ? N2 Mn2 N2 C1 148.1(7) 3_565 . . . ? N2 Mn2 N2 C1 -94.9(8) 2_665 . . . ? Mn1 Mn2 N2 C1 7.3(7) . . . . ? Mn1 Mn2 N2 C1 67.3(7) 3_565 . . . ? Mn1 Mn2 N2 C1 -3.3(9) 2_665 . . . ? Mn2 N2 C1 N1 2.7(11) . . . . ? Mn2 N2 C1 C2 -177.5(5) . . . . ? C5 N1 C1 N2 179.1(6) . . . . ? Mn1 N1 C1 N2 -17.7(9) . . . . ? C5 N1 C1 C2 -0.8(9) . . . . ? Mn1 N1 C1 C2 162.5(5) . . . . ? N2 C1 C2 C3 177.8(7) . . . . ? N1 C1 C2 C3 -2.3(10) . . . . ? N2 C1 C2 Br1 0.6(10) . . . . ? N1 C1 C2 Br1 -179.6(5) . . . . ? C1 C2 C3 C4 5.2(11) . . . . ? Br1 C2 C3 C4 -177.7(6) . . . . ? C2 C3 C4 C5 -4.7(11) . . . . ? C2 C3 C4 C6 177.4(7) . . . . ? C1 N1 C5 C4 1.2(11) . . . . ? Mn1 N1 C5 C4 -164.0(6) . . . . ? C3 C4 C5 N1 1.8(12) . . . . ? C6 C4 C5 N1 179.7(7) . . . . ? O1 Mn1 N4 C7 -121.0(6) . . . . ? N1 Mn1 N4 C7 61.9(6) . . . . ? N4 Mn1 N4 C7 -23.8(6) 14_455 . . . ? N3 Mn1 N4 C7 150.3(6) 15 . . . ? Mn2 Mn1 N4 C7 -162.1(4) . . . . ? O1 Mn1 N4 Mn1 7.3(3) . . . 15 ? N1 Mn1 N4 Mn1 -169.7(2) . . . 15 ? N4 Mn1 N4 Mn1 104.58(14) 14_455 . . 15 ? N3 Mn1 N4 Mn1 -81.4(2) 15 . . 15 ? Mn2 Mn1 N4 Mn1 -33.8(5) . . . 15 ? C11 N3 C7 N4 173.3(6) . . . . ? Mn1 N3 C7 N4 -12.7(7) 14_455 . . . ? C11 N3 C7 C8 -4.0(9) . . . . ? Mn1 N3 C7 C8 170.0(5) 14_455 . . . ? Mn1 N4 C7 N3 65.5(8) . . . . ? Mn1 N4 C7 N3 -58.4(6) 15 . . . ? Mn1 N4 C7 C8 -117.3(7) . . . . ? Mn1 N4 C7 C8 118.8(6) 15 . . . ? N3 C7 C8 C9 5.0(10) . . . . ? N4 C7 C8 C9 -172.1(7) . . . . ? N3 C7 C8 Br2 -173.3(5) . . . . ? N4 C7 C8 Br2 9.5(9) . . . . ? C7 C8 C9 C10 -1.7(12) . . . . ? Br2 C8 C9 C10 176.6(6) . . . . ? C8 C9 C10 C11 -2.4(12) . . . . ? C8 C9 C10 C12 176.4(8) . . . . ? C7 N3 C11 C10 -0.1(11) . . . . ? Mn1 N3 C11 C10 -174.1(6) 14_455 . . . ? C9 C10 C11 N3 3.4(12) . . . . ? C12 C10 C11 N3 -175.3(8) . . . . ? C5S O1S C2S C3S 21(4) . . . . ? O1S C2S C3S C4S -19(5) . . . . ? C2S C3S C4S C5S 9(5) . . . . ? C3S C4S C5S O1S 4(5) . . . . ? C2S O1S C5S C4S -16(4) . . . . ? #===END