# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 1999 # CCDC Number: 440/134 data_dw9819 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 Mn N8 S2' _chemical_formula_weight 581.70 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' 'S' 'S' 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 20.032(6) _cell_length_b 21.966(6) _cell_length_c 16.522(5) _cell_angle_alpha 112.11(4) _cell_angle_beta 113.73(4) _cell_angle_gamma 94.26(4) _cell_volume 5944(3) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_T_max 0.8666 _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 RAXIS-IIC _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22931 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.1788 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.10 _reflns_number_total 15828 _reflns_number_gt 6644 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1369P)^2^+63.9745P] 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 SHELXL _refine_ls_extinction_coef 0.0055(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15828 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2189 _refine_ls_R_factor_gt 0.1296 _refine_ls_wR_factor_ref 0.4033 _refine_ls_wR_factor_gt 0.3607 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.248 _refine_ls_shift/su_mean 0.057 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1_1 Mn 0.75462(16) 0.00548(13) 0.4917(2) 0.0484(8) Uani 1 d . . . S1_1 S 0.6357(3) -0.1077(3) 0.4121(4) 0.0543(13) Uani 1 d . . . S2_1 S 0.8716(3) 0.1183(2) 0.6349(3) 0.0425(11) Uani 1 d . . . N1_1 N 0.7810(8) -0.0654(6) 0.5574(10) 0.0390(9) Uiso 1 d . . . N2_1 N 0.7122(8) -0.1637(7) 0.5311(10) 0.0412(10) Uiso 1 d . . . H2_1 H 0.6723 -0.1975 0.5060 0.049 Uiso 1 calc R . . N3_1 N 0.7933(8) 0.1833(7) 0.7280(10) 0.0412(10) Uiso 1 d . . . H3_1 H 0.8302 0.2198 0.7750 0.049 Uiso 1 calc R . . N4_1 N 0.7299(8) 0.0830(6) 0.5927(10) 0.0390(9) Uiso 1 d . . . N5_1 N 0.6987(9) 0.0339(7) 0.3683(11) 0.0547(12) Uiso 1 d . . . N6_1 N 0.8208(9) -0.0281(7) 0.4000(11) 0.0547(12) Uiso 1 d . . . C1_1 C 0.7102(10) -0.1173(8) 0.5052(12) 0.0392(11) Uiso 1 d . . . C2_1 C 0.7818(9) -0.1577(8) 0.6020(12) 0.0395(8) Uiso 1 d . . . C3_1 C 0.8185(10) -0.1876(9) 0.6538(13) 0.0461(9) Uiso 1 d . . . H3_1 H 0.7911 -0.2312 0.6376 0.055 Uiso 1 calc R . . C4_1 C 0.8859(10) -0.1665(9) 0.7228(13) 0.0528(10) Uiso 1 d . . . H4_1 H 0.9051 -0.1917 0.7588 0.063 Uiso 1 calc R . . C5_1 C 0.9375(11) -0.0967(9) 0.7476(14) 0.0528(10) Uiso 1 d . . . H5_1 H 0.9888 -0.0789 0.7973 0.063 Uiso 1 calc R . . C6_1 C 0.9003(10) -0.0613(8) 0.6878(13) 0.0461(9) Uiso 1 d . . . H6_1 H 0.9274 -0.0196 0.6977 0.055 Uiso 1 calc R . . C7_1 C 0.8235(9) -0.0910(8) 0.6157(12) 0.0395(8) Uiso 1 d . . . C8_1 C 0.7986(9) 0.1303(8) 0.6541(12) 0.0392(11) Uiso 1 d . . . C9_1 C 0.7198(10) 0.1696(8) 0.7162(12) 0.0395(8) Uiso 1 d . . . C10_1 C 0.6905(9) 0.2070(8) 0.7729(13) 0.0461(9) Uiso 1 d . . . H10_1 H 0.7196 0.2481 0.8316 0.055 Uiso 1 calc R . . C11_1 C 0.6133(10) 0.1797(9) 0.7370(14) 0.0528(10) Uiso 1 d . . . H11_1 H 0.5884 0.2049 0.7709 0.063 Uiso 1 calc R . . C12_1 C 0.5724(10) 0.1198(9) 0.6572(13) 0.0528(10) Uiso 1 d . . . H12_1 H 0.5207 0.1045 0.6399 0.063 Uiso 1 calc R . . C13_1 C 0.6025(10) 0.0752(9) 0.5934(13) 0.0461(9) Uiso 1 d . . . H13_1 H 0.5750 0.0320 0.5383 0.055 Uiso 1 calc R . . C14_1 C 0.6753(9) 0.1070(8) 0.6278(12) 0.0395(8) Uiso 1 d . . . C15_1 C 0.6124(12) 0.0150(11) 0.3207(16) 0.0744(14) Uiso 1 d . . . H15A_1 H 0.5926 0.0331 0.2724 0.112 Uiso 1 calc R . . H15B_1 H 0.5965 0.0345 0.3718 0.112 Uiso 1 calc R . . H15C_1 H 0.5926 -0.0347 0.2875 0.112 Uiso 1 calc R . . C16_1 C 0.7195(12) 0.1071(10) 0.4095(16) 0.0744(14) Uiso 1 d . . . H16A_1 H 0.6951 0.1210 0.3571 0.112 Uiso 1 calc R . . H16B_1 H 0.7746 0.1240 0.4395 0.112 Uiso 1 calc R . . H16C_1 H 0.7030 0.1263 0.4600 0.112 Uiso 1 calc R . . C17_1 C 0.8011(12) -0.1116(10) 0.3577(16) 0.0744(14) Uiso 1 d . . . H17A_1 H 0.8271 -0.1300 0.3185 0.112 Uiso 1 calc R . . H17B_1 H 0.7463 -0.1313 0.3161 0.112 Uiso 1 calc R . . H17C_1 H 0.8180 -0.1232 0.4132 0.112 Uiso 1 calc R . . C18_1 C 0.9070(12) -0.0116(11) 0.4671(16) 0.0744(14) Uiso 1 d . . . H18A_1 H 0.9321 -0.0273 0.4259 0.112 Uiso 1 calc R . . H18B_1 H 0.9158 -0.0349 0.5093 0.112 Uiso 1 calc R . . H18C_1 H 0.9275 0.0377 0.5084 0.112 Uiso 1 calc R . . C19_1 C 0.7230(14) -0.0014(13) 0.2956(19) 0.094(2) Uiso 1 d . . . H19A_1 H 0.6925 -0.0495 0.2569 0.113 Uiso 1 calc R . . H19B_1 H 0.7124 0.0194 0.2495 0.113 Uiso 1 calc R . . C20_1 C 0.8018(14) -0.0002(13) 0.3362(19) 0.094(2) Uiso 1 d . . . H20A_1 H 0.8133 -0.0255 0.2817 0.113 Uiso 1 calc R . . H20B_1 H 0.8329 0.0476 0.3709 0.113 Uiso 1 calc R . . Mn1_2 Mn 0.75563(13) 0.49895(11) 0.99360(16) 0.0229(5) Uani 1 d . . . S1_2 S 0.6374(3) 0.3902(2) 0.9096(4) 0.0450(12) Uani 1 d . . . S2_2 S 0.8748(2) 0.6132(2) 1.1372(4) 0.0482(13) Uani 1 d . . . N1_2 N 0.7761(8) 0.4230(6) 1.0487(10) 0.0390(9) Uiso 1 d . . . N2_2 N 0.7088(8) 0.3300(7) 1.0307(10) 0.0412(10) Uiso 1 d . . . H2_2 H 0.6712 0.2949 1.0085 0.049 Uiso 1 calc R . . N3_2 N 0.7914(8) 0.6760(6) 1.2318(10) 0.0412(10) Uiso 1 d . . . H3_2 H 0.8292 0.7109 1.2814 0.049 Uiso 1 calc R . . N4_2 N 0.7266(8) 0.5755(6) 1.0960(10) 0.0390(9) Uiso 1 d . . . N5_2 N 0.6944(9) 0.5262(7) 0.8644(11) 0.0547(12) Uiso 1 d . . . N6_2 N 0.8204(9) 0.4598(7) 0.9080(11) 0.0547(12) Uiso 1 d . . . C1_2 C 0.7107(10) 0.3831(8) 0.9995(12) 0.0392(11) Uiso 1 d . . . C2_2 C 0.7862(9) 0.3502(8) 1.1088(12) 0.0395(8) Uiso 1 d . . . C3_2 C 0.8114(10) 0.3070(8) 1.1632(12) 0.0461(9) Uiso 1 d . . . H3_2 H 0.7824 0.2673 1.1561 0.055 Uiso 1 calc R . . C4_2 C 0.8963(10) 0.3443(9) 1.2334(13) 0.0528(10) Uiso 1 d . . . H4_2 H 0.9247 0.3261 1.2760 0.063 Uiso 1 calc R . . C5_2 C 0.9291(11) 0.3948(9) 1.2379(14) 0.0528(10) Uiso 1 d . . . H5_2 H 0.9813 0.4126 1.2841 0.063 Uiso 1 calc R . . C6_2 C 0.9016(10) 0.4268(8) 1.1877(13) 0.0461(9) Uiso 1 d . . . H6_2 H 0.9323 0.4657 1.1952 0.055 Uiso 1 calc R . . C7_2 C 0.8281(9) 0.4037(8) 1.1242(12) 0.0395(8) Uiso 1 d . . . C8_2 C 0.7935(9) 0.6222(8) 1.1579(12) 0.0392(11) Uiso 1 d . . . C9_2 C 0.7163(10) 0.6633(8) 1.2111(12) 0.0395(8) Uiso 1 d . . . C10_2 C 0.6750(9) 0.7036(8) 1.2587(12) 0.0461(9) Uiso 1 d . . . H10_2 H 0.6992 0.7483 1.3112 0.055 Uiso 1 calc R . . C11_2 C 0.5998(10) 0.6735(9) 1.2235(14) 0.0528(10) Uiso 1 d . . . H11_2 H 0.5726 0.6961 1.2557 0.063 Uiso 1 calc R . . C12_2 C 0.5611(11) 0.6062(9) 1.1363(13) 0.0528(10) Uiso 1 d . . . H12_2 H 0.5088 0.5858 1.1093 0.063 Uiso 1 calc R . . C13_2 C 0.6026(10) 0.5762(9) 1.0984(13) 0.0461(9) Uiso 1 d . . . H13_2 H 0.5774 0.5334 1.0417 0.055 Uiso 1 calc R . . C14_2 C 0.6833(9) 0.6013(8) 1.1336(12) 0.0395(8) Uiso 1 d . . . C15_2 C 0.6148(12) 0.5077(11) 0.8213(16) 0.0744(14) Uiso 1 d . . . H15A_2 H 0.5936 0.5183 0.7649 0.112 Uiso 1 calc R . . H15B_2 H 0.5990 0.5332 0.8702 0.112 Uiso 1 calc R . . H15C_2 H 0.5964 0.4587 0.7986 0.112 Uiso 1 calc R . . C16_2 C 0.7221(12) 0.6019(10) 0.9020(16) 0.0744(14) Uiso 1 d . . . H16A_2 H 0.7149 0.6121 0.8466 0.112 Uiso 1 calc R . . H16B_2 H 0.7760 0.6176 0.9497 0.112 Uiso 1 calc R . . H16C_2 H 0.6935 0.6254 0.9342 0.112 Uiso 1 calc R . . C17_2 C 0.7913(12) 0.3920(10) 0.8418(16) 0.0744(14) Uiso 1 d . . . H17A_2 H 0.8165 0.3805 0.8002 0.112 Uiso 1 calc R . . H17B_2 H 0.7369 0.3827 0.8003 0.112 Uiso 1 calc R . . H17C_2 H 0.7998 0.3642 0.8778 0.112 Uiso 1 calc R . . C18_2 C 0.8991(12) 0.4808(11) 0.9623(16) 0.0744(14) Uiso 1 d . . . H18A_2 H 0.9212 0.4595 0.9189 0.112 Uiso 1 calc R . . H18B_2 H 0.9151 0.4671 1.0158 0.112 Uiso 1 calc R . . H18C_2 H 0.9163 0.5305 0.9902 0.112 Uiso 1 calc R . . C19_2 C 0.7207(14) 0.4942(13) 0.7902(19) 0.094(2) Uiso 1 d . . . H19A_2 H 0.7135 0.5195 0.7501 0.113 Uiso 1 calc R . . H19B_2 H 0.6885 0.4469 0.7454 0.113 Uiso 1 calc R . . C20_2 C 0.8010(14) 0.4925(13) 0.8327(19) 0.094(2) Uiso 1 d . . . H20A_2 H 0.8339 0.5395 0.8674 0.113 Uiso 1 calc R . . H20B_2 H 0.8120 0.4658 0.7785 0.113 Uiso 1 calc R . . Mn1_3 Mn 0.73935(15) 0.51845(11) 0.5081(2) 0.0366(7) Uani 1 d . . . S1_3 S 0.6205(3) 0.4207(3) 0.4515(4) 0.0560(14) Uani 1 d . . . S2_3 S 0.8682(3) 0.6217(2) 0.6395(4) 0.0513(13) Uani 1 d . . . N1_3 N 0.7697(7) 0.4431(6) 0.5642(10) 0.0390(9) Uiso 1 d . . . N2_3 N 0.6982(8) 0.3424(7) 0.5311(10) 0.0412(10) Uiso 1 d . . . H2_3 H 0.6590 0.3082 0.5069 0.049 Uiso 1 calc R . . N3_3 N 0.8084(8) 0.6935(7) 0.7586(10) 0.0412(10) Uiso 1 d . . . H3_3 H 0.8514 0.7234 0.8063 0.049 Uiso 1 calc R . . N4_3 N 0.7307(7) 0.6025(6) 0.6219(10) 0.0390(9) Uiso 1 d . . . N5_3 N 0.6770(9) 0.5615(7) 0.3991(11) 0.0547(12) Uiso 1 d . . . N6_3 N 0.7749(8) 0.4790(7) 0.3861(11) 0.0547(12) Uiso 1 d . . . C1_3 C 0.6977(9) 0.4015(8) 0.5224(12) 0.0392(11) Uiso 1 d . . . C2_3 C 0.7737(9) 0.3474(8) 0.5862(12) 0.0395(8) Uiso 1 d . . . C3_3 C 0.8037(10) 0.3032(9) 0.6215(13) 0.0461(9) Uiso 1 d . . . H3_3 H 0.7715 0.2619 0.6054 0.055 Uiso 1 calc R . . C4_3 C 0.8732(10) 0.3171(9) 0.6747(13) 0.0528(10) Uiso 1 d . . . H4_3 H 0.8927 0.2847 0.6960 0.063 Uiso 1 calc R . . C5_3 C 0.9290(11) 0.3841(9) 0.7076(13) 0.0528(10) Uiso 1 d . . . H5_3 H 0.9811 0.3969 0.7536 0.063 Uiso 1 calc R . . C6_3 C 0.8915(10) 0.4283(8) 0.6582(12) 0.0461(9) Uiso 1 d . . . H6_3 H 0.9213 0.4682 0.6669 0.055 Uiso 1 calc R . . C7_3 C 0.8126(9) 0.4083(8) 0.6001(12) 0.0395(8) Uiso 1 d . . . C8_3 C 0.8034(9) 0.6411(8) 0.6736(12) 0.0392(11) Uiso 1 d . . . C9_3 C 0.7403(9) 0.6948(8) 0.7618(12) 0.0395(8) Uiso 1 d . . . C10_3 C 0.7154(10) 0.7332(9) 0.8198(13) 0.0461(9) Uiso 1 d . . . H10_3 H 0.7481 0.7750 0.8750 0.055 Uiso 1 calc R . . C11_3 C 0.6410(11) 0.7126(9) 0.8001(14) 0.0528(10) Uiso 1 d . . . H11_3 H 0.6236 0.7391 0.8440 0.063 Uiso 1 calc R . . C12_3 C 0.5944(11) 0.6563(9) 0.7204(14) 0.0528(10) Uiso 1 d . . . H12_3 H 0.5435 0.6458 0.7088 0.063 Uiso 1 calc R . . C13_3 C 0.6121(10) 0.6109(9) 0.6521(13) 0.0461(9) Uiso 1 d . . . H13_3 H 0.5766 0.5708 0.5961 0.055 Uiso 1 calc R . . C14_3 C 0.6865(9) 0.6302(8) 0.6740(12) 0.0395(8) Uiso 1 d . . . C15_3 C 0.5950(12) 0.5471(11) 0.3612(16) 0.0744(14) Uiso 1 d . . . H15A_3 H 0.5733 0.5624 0.3099 0.112 Uiso 1 calc R . . H15B_3 H 0.5834 0.5714 0.4152 0.112 Uiso 1 calc R . . H15C_3 H 0.5733 0.4980 0.3332 0.112 Uiso 1 calc R . . C16_3 C 0.7058(12) 0.6384(10) 0.4504(16) 0.0744(14) Uiso 1 d . . . H16A_3 H 0.6756 0.6571 0.4069 0.112 Uiso 1 calc R . . H16B_3 H 0.7589 0.6515 0.4659 0.112 Uiso 1 calc R . . H16C_3 H 0.7014 0.6563 0.5115 0.112 Uiso 1 calc R . . C17_3 C 0.7345(12) 0.4026(10) 0.3291(16) 0.0744(14) Uiso 1 d . . . H17A_3 H 0.7286 0.3852 0.2619 0.112 Uiso 1 calc R . . H17B_3 H 0.6845 0.3956 0.3262 0.112 Uiso 1 calc R . . H17C_3 H 0.7645 0.3782 0.3627 0.112 Uiso 1 calc R . . C18_3 C 0.8589(12) 0.4913(11) 0.4248(16) 0.0744(14) Uiso 1 d . . . H18A_3 H 0.8699 0.4646 0.3713 0.112 Uiso 1 calc R . . H18B_3 H 0.8796 0.4774 0.4779 0.112 Uiso 1 calc R . . H18C_3 H 0.8821 0.5398 0.4506 0.112 Uiso 1 calc R . . C19_3 C 0.6883(14) 0.5309(13) 0.3045(19) 0.094(2) Uiso 1 d . . . H19A_3 H 0.6459 0.4904 0.2517 0.113 Uiso 1 calc R . . H19B_3 H 0.6908 0.5651 0.2796 0.113 Uiso 1 calc R . . C20_3 C 0.7518(14) 0.5141(13) 0.3319(19) 0.094(2) Uiso 1 d . . . H20A_3 H 0.7919 0.5574 0.3682 0.113 Uiso 1 calc R . . H20B_3 H 0.7545 0.4881 0.2702 0.113 Uiso 1 calc R . . Mn1_4 Mn 0.74216(16) 0.01523(15) 0.0086(2) 0.0472(8) Uani 1 d . . . S1_4 S 0.6185(3) -0.0804(2) -0.0507(4) 0.0607(15) Uani 1 d . . . S2_4 S 0.8691(2) 0.1161(2) 0.1392(3) 0.0485(13) Uani 1 d . . . N1_4 N 0.7638(7) -0.0675(6) 0.0516(10) 0.0390(9) Uiso 1 d . . . N2_4 N 0.6947(8) -0.1587(7) 0.0323(10) 0.0412(10) Uiso 1 d . . . H2_4 H 0.6538 -0.1886 0.0151 0.049 Uiso 1 calc R . . N3_4 N 0.8128(8) 0.1931(7) 0.2626(10) 0.0412(10) Uiso 1 d . . . H3_4 H 0.8544 0.2262 0.3066 0.049 Uiso 1 calc R . . N4_4 N 0.7302(7) 0.0956(6) 0.1291(10) 0.0390(9) Uiso 1 d . . . N5_4 N 0.6704(9) 0.0542(8) -0.1087(11) 0.0547(12) Uiso 1 d . . . N6_4 N 0.7898(8) -0.0272(7) -0.1014(11) 0.0547(12) Uiso 1 d . . . C1_4 C 0.6958(9) -0.1060(8) 0.0101(12) 0.0392(11) Uiso 1 d . . . C2_4 C 0.7684(9) -0.1584(8) 0.0867(12) 0.0395(8) Uiso 1 d . . . C3_4 C 0.8028(10) -0.2042(8) 0.1247(12) 0.0461(9) Uiso 1 d . . . H3_4 H 0.7751 -0.2459 0.1143 0.055 Uiso 1 calc R . . C4_4 C 0.8912(10) -0.1765(9) 0.1849(13) 0.0528(10) Uiso 1 d . . . H4_4 H 0.9210 -0.2002 0.2166 0.063 Uiso 1 calc R . . C5_4 C 0.9225(11) -0.1201(9) 0.1902(13) 0.0528(10) Uiso 1 d . . . H5_4 H 0.9762 -0.1082 0.2203 0.063 Uiso 1 calc R . . C6_4 C 0.8942(10) -0.0819(9) 0.1635(12) 0.0461(9) Uiso 1 d . . . H6_4 H 0.9246 -0.0397 0.1798 0.055 Uiso 1 calc R . . C7_4 C 0.8171(9) -0.0984(8) 0.1086(12) 0.0395(8) Uiso 1 d . . . C8_4 C 0.8019(9) 0.1373(8) 0.1844(12) 0.0392(11) Uiso 1 d . . . C9_4 C 0.7401(9) 0.1856(8) 0.2566(12) 0.0395(8) Uiso 1 d . . . C10_4 C 0.7179(10) 0.2317(9) 0.3267(13) 0.0461(9) Uiso 1 d . . . H10_4 H 0.7533 0.2699 0.3861 0.055 Uiso 1 calc R . . C11_4 C 0.6429(11) 0.2157(9) 0.3003(14) 0.0528(10) Uiso 1 d . . . H11_4 H 0.6246 0.2468 0.3387 0.063 Uiso 1 calc R . . C12_4 C 0.5896(11) 0.1534(9) 0.2164(14) 0.0528(10) Uiso 1 d . . . H12_4 H 0.5384 0.1410 0.2028 0.063 Uiso 1 calc R . . C13_4 C 0.6181(10) 0.1116(9) 0.1555(13) 0.0461(9) Uiso 1 d . . . H13_4 H 0.5856 0.0703 0.0992 0.055 Uiso 1 calc R . . C14_4 C 0.6957(9) 0.1319(8) 0.1789(12) 0.0395(8) Uiso 1 d . . . C15_4 C 0.5893(12) 0.0426(11) -0.1278(16) 0.0744(14) Uiso 1 d . . . H15A_4 H 0.5565 0.0352 -0.1953 0.112 Uiso 1 calc R . . H15B_4 H 0.5836 0.0826 -0.0809 0.112 Uiso 1 calc R . . H15C_4 H 0.5751 0.0024 -0.1197 0.112 Uiso 1 calc R . . C16_4 C 0.7015(12) 0.1269(10) -0.0683(16) 0.0744(14) Uiso 1 d . . . H16A_4 H 0.6744 0.1427 -0.1174 0.112 Uiso 1 calc R . . H16B_4 H 0.7552 0.1364 -0.0512 0.112 Uiso 1 calc R . . H16C_4 H 0.6959 0.1507 -0.0089 0.112 Uiso 1 calc R . . C17_4 C 0.7541(12) -0.0947(10) -0.1657(16) 0.0744(14) Uiso 1 d . . . H17A_4 H 0.7787 -0.1118 -0.2072 0.112 Uiso 1 calc R . . H17B_4 H 0.7008 -0.0995 -0.2075 0.112 Uiso 1 calc R . . H17C_4 H 0.7572 -0.1209 -0.1283 0.112 Uiso 1 calc R . . C18_4 C 0.8667(12) -0.0196(11) -0.0559(16) 0.0744(14) Uiso 1 d . . . H18A_4 H 0.8855 -0.0285 -0.1045 0.112 Uiso 1 calc R . . H18B_4 H 0.8771 -0.0519 -0.0275 0.112 Uiso 1 calc R . . H18C_4 H 0.8922 0.0270 -0.0033 0.112 Uiso 1 calc R . . C19_4 C 0.6839(14) 0.0182(13) -0.1876(19) 0.094(2) Uiso 1 d . . . H19A_4 H 0.6682 0.0393 -0.2334 0.113 Uiso 1 calc R . . H19B_4 H 0.6509 -0.0288 -0.2235 0.113 Uiso 1 calc R . . C20_4 C 0.7667(14) 0.0139(13) -0.1630(19) 0.094(2) Uiso 1 d . . . H20A_4 H 0.7702 -0.0090 -0.2249 0.113 Uiso 1 calc R . . H20B_4 H 0.8014 0.0604 -0.1249 0.113 Uiso 1 calc R . . N7_5 N 0.5601(8) 0.2613(7) 0.4940(11) 0.0479(10) Uiso 1 d . . . N8_5 N 0.4313(8) 0.2283(7) 0.4966(11) 0.0479(10) Uiso 1 d . . . C21_5 C 0.4223(11) 0.2548(10) 0.4171(15) 0.0637(10) Uiso 1 d . . . H21A_5 H 0.3815 0.2213 0.3515 0.076 Uiso 1 calc R . . H21B_5 H 0.4085 0.2986 0.4350 0.076 Uiso 1 calc R . . C22_5 C 0.4959(11) 0.2644(10) 0.4134(15) 0.0637(10) Uiso 1 d . . . H22A_5 H 0.4893 0.2288 0.3501 0.076 Uiso 1 calc R . . H22B_5 H 0.5080 0.3092 0.4142 0.076 Uiso 1 calc R . . C23_5 C 0.4587(11) 0.1630(10) 0.4622(15) 0.0637(10) Uiso 1 d . . . H23A_5 H 0.4578 0.1377 0.5005 0.076 Uiso 1 calc R . . H23B_5 H 0.4247 0.1327 0.3914 0.076 Uiso 1 calc R . . C24_5 C 0.5408(11) 0.1850(10) 0.4790(15) 0.0637(10) Uiso 1 d . . . H24A_5 H 0.5458 0.1540 0.4213 0.076 Uiso 1 calc R . . H24B_5 H 0.5771 0.1815 0.5380 0.076 Uiso 1 calc R . . C25_5 C 0.4921(11) 0.2691(10) 0.5971(15) 0.0637(10) Uiso 1 d . . . H25A_5 H 0.5009 0.2416 0.6342 0.076 Uiso 1 calc R . . H25B_5 H 0.4771 0.3091 0.6312 0.076 Uiso 1 calc R . . C26_5 C 0.5630(11) 0.2927(10) 0.5956(14) 0.0637(10) Uiso 1 d . . . H26A_5 H 0.6048 0.2821 0.6414 0.076 Uiso 1 calc R . . H26B_5 H 0.5750 0.3429 0.6210 0.076 Uiso 1 calc R . . N7_6 N 0.5681(8) 0.2711(7) 1.0096(11) 0.0479(10) Uiso 1 d . . . N8_6 N 0.4435(8) 0.2449(7) 1.0075(11) 0.0479(10) Uiso 1 d . . . C21_6 C 0.5754(11) 0.2366(10) 1.0642(15) 0.0637(10) Uiso 1 d . . . H21A_6 H 0.6190 0.2634 1.1306 0.076 Uiso 1 calc R . . H21B_6 H 0.5856 0.1927 1.0325 0.076 Uiso 1 calc R . . C22_6 C 0.5011(11) 0.2222(10) 1.0749(15) 0.0637(10) Uiso 1 d . . . H22A_6 H 0.4827 0.1731 1.0545 0.076 Uiso 1 calc R . . H22B_6 H 0.5111 0.2484 1.1441 0.076 Uiso 1 calc R . . C23_6 C 0.5124(11) 0.2196(10) 0.9146(15) 0.0637(10) Uiso 1 d . . . H23A_6 H 0.5330 0.1802 0.8941 0.076 Uiso 1 calc R . . H23B_6 H 0.5012 0.2379 0.8656 0.076 Uiso 1 calc R . . C24_6 C 0.4363(11) 0.1949(10) 0.9157(14) 0.0637(10) Uiso 1 d . . . H24A_6 H 0.3917 0.1935 0.8589 0.076 Uiso 1 calc R . . H24B_6 H 0.4312 0.1490 0.9133 0.076 Uiso 1 calc R . . C25_6 C 0.5469(11) 0.3319(10) 1.0470(15) 0.0637(10) Uiso 1 d . . . H25A_6 H 0.5436 0.3568 1.0071 0.076 Uiso 1 calc R . . H25B_6 H 0.5851 0.3619 1.1161 0.076 Uiso 1 calc R . . C26_6 C 0.4694(11) 0.3121(10) 1.0417(15) 0.0637(10) Uiso 1 d . . . H26A_6 H 0.4737 0.3357 1.1085 0.076 Uiso 1 calc R . . H26B_6 H 0.4324 0.3278 0.9983 0.076 Uiso 1 calc R . . N7_7 N 1.0723(8) 0.7611(7) 1.0821(11) 0.0479(10) Uiso 1 d . . . N8_7 N 0.9526(8) 0.7516(7) 0.9317(11) 0.0479(10) Uiso 1 d . . . C21_7 C 1.0077(11) 0.7161(10) 1.0675(15) 0.0637(10) Uiso 1 d . . . H21A_7 H 1.0016 0.7339 1.1280 0.076 Uiso 1 calc R . . H21B_7 H 1.0166 0.6705 1.0555 0.076 Uiso 1 calc R . . C22_7 C 0.9364(11) 0.7096(10) 0.9814(15) 0.0637(10) Uiso 1 d . . . H22A_7 H 0.8996 0.7256 1.0047 0.076 Uiso 1 calc R . . H22B_7 H 0.9136 0.6611 0.9326 0.076 Uiso 1 calc R . . C23_7 C 1.0856(11) 0.7333(10) 0.9918(14) 0.0637(10) Uiso 1 d . . . H23A_7 H 1.1219 0.7688 0.9957 0.076 Uiso 1 calc R . . H23B_7 H 1.1067 0.6936 0.9884 0.076 Uiso 1 calc R . . C24_7 C 1.0106(11) 0.7125(10) 0.9020(15) 0.0637(10) Uiso 1 d . . . H24A_7 H 0.9890 0.6626 0.8717 0.076 Uiso 1 calc R . . H24B_7 H 1.0179 0.7237 0.8529 0.076 Uiso 1 calc R . . C25_7 C 1.0662(11) 0.8331(10) 1.0894(15) 0.0637(10) Uiso 1 d . . . H25A_7 H 1.0579 0.8595 1.1465 0.076 Uiso 1 calc R . . H25B_7 H 1.1130 0.8587 1.0973 0.076 Uiso 1 calc R . . C26_7 C 1.0003(11) 0.8209(10) 0.9952(14) 0.0637(10) Uiso 1 d . . . H26A_7 H 0.9682 0.8506 1.0114 0.076 Uiso 1 calc R . . H26B_7 H 1.0195 0.8356 0.9571 0.076 Uiso 1 calc R . . N7_8 N 1.0430(8) 0.7510(7) 0.5695(11) 0.0479(10) Uiso 1 d . . . N8_8 N 0.9261(8) 0.7424(7) 0.4173(11) 0.0479(10) Uiso 1 d . . . C21_8 C 1.0151(11) 0.6778(9) 0.4921(14) 0.0637(10) Uiso 1 d . . . H21A_8 H 1.0070 0.6459 0.5186 0.076 Uiso 1 calc R . . H21B_8 H 1.0503 0.6656 0.4642 0.076 Uiso 1 calc R . . C22_8 C 0.9311(11) 0.6795(10) 0.4068(15) 0.0637(10) Uiso 1 d . . . H22A_8 H 0.9248 0.6519 0.3398 0.076 Uiso 1 calc R . . H22B_8 H 0.8890 0.6578 0.4122 0.076 Uiso 1 calc R . . C23_8 C 1.0631(11) 0.7767(10) 0.5167(15) 0.0637(10) Uiso 1 d . . . H23A_8 H 1.1012 0.7553 0.5021 0.076 Uiso 1 calc R . . H23B_8 H 1.0870 0.8263 0.5577 0.076 Uiso 1 calc R . . C24_8 C 0.9956(11) 0.7650(10) 0.4187(15) 0.0637(10) Uiso 1 d . . . H24A_8 H 0.9970 0.8079 0.4120 0.076 Uiso 1 calc R . . H24B_8 H 0.9992 0.7303 0.3624 0.076 Uiso 1 calc R . . C25_8 C 0.9900(11) 0.7684(10) 0.5979(15) 0.0637(10) Uiso 1 d . . . H25A_8 H 1.0132 0.8071 0.6648 0.076 Uiso 1 calc R . . H25B_8 H 0.9617 0.7294 0.5977 0.076 Uiso 1 calc R . . C26_8 C 0.9303(11) 0.7918(10) 0.5082(14) 0.0637(10) Uiso 1 d . . . H26A_8 H 0.8796 0.7886 0.5049 0.076 Uiso 1 calc R . . H26B_8 H 0.9524 0.8388 0.5227 0.076 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1_1 0.0435(18) 0.0343(15) 0.058(2) 0.0197(14) 0.0170(16) 0.0072(13) S1_1 0.026(3) 0.062(3) 0.052(3) 0.017(3) 0.007(2) 0.001(2) S2_1 0.043(3) 0.040(2) 0.039(3) 0.015(2) 0.017(2) 0.013(2) Mn1_2 0.0304(13) 0.0276(12) 0.0191(12) 0.0127(10) 0.0167(11) 0.0100(10) S1_2 0.049(3) 0.048(3) 0.059(3) 0.040(2) 0.027(3) 0.017(2) S2_2 0.029(2) 0.052(3) 0.045(3) 0.007(2) 0.014(2) 0.012(2) Mn1_3 0.0442(16) 0.0167(11) 0.0442(16) 0.0097(11) 0.0192(14) 0.0119(11) S1_3 0.040(3) 0.063(3) 0.060(3) 0.032(3) 0.013(3) 0.016(3) S2_3 0.060(3) 0.031(2) 0.057(3) 0.011(2) 0.030(3) 0.012(2) Mn1_4 0.0388(17) 0.0609(18) 0.0368(16) 0.0284(14) 0.0096(14) -0.0026(13) S1_4 0.033(3) 0.054(3) 0.084(4) 0.048(3) 0.004(3) -0.004(2) S2_4 0.023(2) 0.062(3) 0.037(3) 0.005(2) 0.009(2) 0.008(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_1 N4_1 2.140(12) . ? Mn1_1 N1_1 2.192(14) . ? Mn1_1 N5_1 2.242(16) . ? Mn1_1 N6_1 2.349(15) . ? Mn1_1 S2_1 2.738(6) . ? Mn1_1 S1_1 2.779(6) . ? S1_1 C1_1 1.756(17) . ? S2_1 C8_1 1.637(16) . ? N1_1 C7_1 1.34(2) . ? N1_1 C1_1 1.45(2) . ? N2_1 C1_1 1.24(2) . ? N2_1 C2_1 1.37(2) . ? N3_1 C8_1 1.381(19) . ? N3_1 C9_1 1.40(2) . ? N4_1 C8_1 1.37(2) . ? N4_1 C14_1 1.474(19) . ? N5_1 C16_1 1.44(2) . ? N5_1 C19_1 1.45(3) . ? N5_1 C15_1 1.53(2) . ? N6_1 C20_1 1.35(3) . ? N6_1 C18_1 1.55(2) . ? N6_1 C17_1 1.65(2) . ? C2_1 C3_1 1.30(2) . ? C2_1 C7_1 1.52(2) . ? C3_1 C4_1 1.27(2) . ? C4_1 C5_1 1.59(2) . ? C5_1 C6_1 1.49(2) . ? C6_1 C7_1 1.41(2) . ? C9_1 C10_1 1.35(2) . ? C9_1 C14_1 1.44(2) . ? C10_1 C11_1 1.40(2) . ? C11_1 C12_1 1.34(2) . ? C12_1 C13_1 1.50(2) . ? C13_1 C14_1 1.35(2) . ? C19_1 C20_1 1.44(3) . ? Mn1_2 N1_2 2.174(13) . ? Mn1_2 N4_2 2.196(12) . ? Mn1_2 N6_2 2.269(15) . ? Mn1_2 N5_2 2.321(16) . ? Mn1_2 S1_2 2.694(6) . ? Mn1_2 S2_2 2.775(6) . ? S1_2 C1_2 1.685(17) . ? S2_2 C8_2 1.804(16) . ? N1_2 C1_2 1.26(2) . ? N1_2 C7_2 1.50(2) . ? N2_2 C1_2 1.45(2) . ? N2_2 C2_2 1.46(2) . ? N3_2 C8_2 1.361(19) . ? N3_2 C9_2 1.38(2) . ? N4_2 C14_2 1.305(19) . ? N4_2 C8_2 1.34(2) . ? N5_2 C15_2 1.41(2) . ? N5_2 C19_2 1.48(3) . ? N5_2 C16_2 1.51(2) . ? N6_2 C17_2 1.37(2) . ? N6_2 C18_2 1.40(2) . ? N6_2 C20_2 1.59(3) . ? C2_2 C7_2 1.27(2) . ? C2_2 C3_2 1.52(2) . ? C3_2 C4_2 1.55(2) . ? C4_2 C5_2 1.21(2) . ? C5_2 C6_2 1.27(2) . ? C6_2 C7_2 1.33(2) . ? C9_2 C14_2 1.34(2) . ? C9_2 C10_2 1.48(2) . ? C10_2 C11_2 1.38(2) . ? C11_2 C12_2 1.48(2) . ? C12_2 C13_2 1.31(2) . ? C13_2 C14_2 1.46(2) . ? C19_2 C20_2 1.48(3) . ? Mn1_3 N4_3 2.160(12) . ? Mn1_3 N1_3 2.196(13) . ? Mn1_3 N6_3 2.292(15) . ? Mn1_3 N5_3 2.312(16) . ? Mn1_3 S1_3 2.663(6) . ? Mn1_3 S2_3 2.726(6) . ? S1_3 C1_3 1.719(17) . ? S2_3 C8_3 1.635(16) . ? N1_3 C7_3 1.303(19) . ? N1_3 C1_3 1.39(2) . ? N2_3 C1_3 1.36(2) . ? N2_3 C2_3 1.38(2) . ? N3_3 C9_3 1.388(19) . ? N3_3 C8_3 1.399(19) . ? N4_3 C8_3 1.36(2) . ? N4_3 C14_3 1.481(19) . ? N5_3 C15_3 1.46(2) . ? N5_3 C16_3 1.51(2) . ? N5_3 C19_3 1.57(3) . ? N6_3 C20_3 1.36(3) . ? N6_3 C18_3 1.50(2) . ? N6_3 C17_3 1.53(2) . ? C2_3 C3_3 1.37(2) . ? C2_3 C7_3 1.38(2) . ? C3_3 C4_3 1.25(2) . ? C4_3 C5_3 1.54(2) . ? C5_3 C6_3 1.54(2) . ? C6_3 C7_3 1.40(2) . ? C9_3 C10_3 1.31(2) . ? C9_3 C14_3 1.50(2) . ? C10_3 C11_3 1.39(2) . ? C11_3 C12_3 1.32(2) . ? C12_3 C13_3 1.39(2) . ? C13_3 C14_3 1.37(2) . ? C19_3 C20_3 1.30(3) . ? Mn1_4 N1_4 2.199(13) . ? Mn1_4 N4_4 2.223(13) . ? Mn1_4 N6_4 2.309(15) . ? Mn1_4 N5_4 2.397(16) . ? Mn1_4 S2_4 2.679(6) . ? Mn1_4 S1_4 2.689(6) . ? S1_4 C1_4 1.740(17) . ? S2_4 C8_4 1.796(16) . ? N1_4 C1_4 1.297(19) . ? N1_4 C7_4 1.51(2) . ? N2_4 C1_4 1.34(2) . ? N2_4 C2_4 1.38(2) . ? N3_4 C8_4 1.327(19) . ? N3_4 C9_4 1.41(2) . ? N4_4 C14_4 1.356(18) . ? N4_4 C8_4 1.36(2) . ? N5_4 C19_4 1.39(3) . ? N5_4 C16_4 1.45(2) . ? N5_4 C15_4 1.51(2) . ? N6_4 C17_4 1.37(2) . ? N6_4 C18_4 1.38(2) . ? N6_4 C20_4 1.56(3) . ? C2_4 C7_4 1.41(2) . ? C2_4 C3_4 1.45(2) . ? C3_4 C4_4 1.57(2) . ? C4_4 C5_4 1.30(2) . ? C5_4 C6_4 1.17(2) . ? C6_4 C7_4 1.37(2) . ? C9_4 C14_4 1.27(2) . ? C9_4 C10_4 1.47(2) . ? C10_4 C11_4 1.36(2) . ? C11_4 C12_4 1.45(2) . ? C12_4 C13_4 1.42(2) . ? C13_4 C14_4 1.43(2) . ? C19_4 C20_4 1.56(3) . ? N7_5 C22_5 1.46(2) . ? N7_5 C26_5 1.53(2) . ? N7_5 C24_5 1.59(2) . ? N8_5 C25_5 1.46(2) . ? N8_5 C23_5 1.56(2) . ? N8_5 C21_5 1.58(2) . ? C21_5 C22_5 1.50(2) . ? C23_5 C24_5 1.56(3) . ? C25_5 C26_5 1.49(2) . ? N7_6 C21_6 1.36(2) . ? N7_6 C25_6 1.42(2) . ? N7_6 C23_6 1.43(2) . ? N8_6 C26_6 1.34(2) . ? N8_6 C24_6 1.44(2) . ? N8_6 C22_6 1.51(2) . ? C21_6 C22_6 1.59(3) . ? C23_6 C24_6 1.59(3) . ? C25_6 C26_6 1.54(2) . ? N7_7 C21_7 1.44(2) . ? N7_7 C23_7 1.53(2) . ? N7_7 C25_7 1.56(2) . ? N8_7 C26_7 1.45(2) . ? N8_7 C22_7 1.54(2) . ? N8_7 C24_7 1.62(2) . ? C21_7 C22_7 1.50(3) . ? C23_7 C24_7 1.50(3) . ? C25_7 C26_7 1.49(3) . ? N7_8 C25_8 1.35(2) . ? N7_8 C23_8 1.36(2) . ? N7_8 C21_8 1.51(2) . ? N8_8 C22_8 1.34(2) . ? N8_8 C24_8 1.43(2) . ? N8_8 C26_8 1.45(2) . ? C21_8 C22_8 1.72(3) . ? C23_8 C24_8 1.55(3) . ? C25_8 C26_8 1.77(3) . ? 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 N4_1 Mn1_1 N1_1 103.3(5) . . ? N4_1 Mn1_1 N5_1 94.3(5) . . ? N1_1 Mn1_1 N5_1 155.0(5) . . ? N4_1 Mn1_1 N6_1 150.9(5) . . ? N1_1 Mn1_1 N6_1 95.1(5) . . ? N5_1 Mn1_1 N6_1 76.6(5) . . ? N4_1 Mn1_1 S2_1 63.4(4) . . ? N1_1 Mn1_1 S2_1 99.9(4) . . ? N5_1 Mn1_1 S2_1 103.8(4) . . ? N6_1 Mn1_1 S2_1 91.7(4) . . ? N4_1 Mn1_1 S1_1 102.6(4) . . ? N1_1 Mn1_1 S1_1 65.1(4) . . ? N5_1 Mn1_1 S1_1 94.1(4) . . ? N6_1 Mn1_1 S1_1 105.5(4) . . ? S2_1 Mn1_1 S1_1 157.7(2) . . ? C1_1 S1_1 Mn1_1 75.6(6) . . ? C8_1 S2_1 Mn1_1 73.9(6) . . ? C7_1 N1_1 C1_1 99.1(13) . . ? C7_1 N1_1 Mn1_1 157.4(12) . . ? C1_1 N1_1 Mn1_1 103.4(10) . . ? C1_1 N2_1 C2_1 114.1(15) . . ? C8_1 N3_1 C9_1 109.1(13) . . ? C8_1 N4_1 C14_1 108.5(12) . . ? C8_1 N4_1 Mn1_1 102.2(9) . . ? C14_1 N4_1 Mn1_1 149.2(11) . . ? C16_1 N5_1 C19_1 115.5(18) . . ? C16_1 N5_1 C15_1 103.6(15) . . ? C19_1 N5_1 C15_1 110.1(17) . . ? C16_1 N5_1 Mn1_1 107.8(13) . . ? C19_1 N5_1 Mn1_1 105.6(13) . . ? C15_1 N5_1 Mn1_1 114.5(12) . . ? C20_1 N6_1 C18_1 114.8(18) . . ? C20_1 N6_1 C17_1 120.0(17) . . ? C18_1 N6_1 C17_1 97.9(14) . . ? C20_1 N6_1 Mn1_1 107.4(14) . . ? C18_1 N6_1 Mn1_1 112.2(11) . . ? C17_1 N6_1 Mn1_1 104.1(10) . . ? N2_1 C1_1 N1_1 114.5(16) . . ? N2_1 C1_1 S1_1 129.5(15) . . ? N1_1 C1_1 S1_1 115.9(12) . . ? C3_1 C2_1 N2_1 143.0(17) . . ? C3_1 C2_1 C7_1 119.1(15) . . ? N2_1 C2_1 C7_1 97.9(13) . . ? C4_1 C3_1 C2_1 128.9(19) . . ? C3_1 C4_1 C5_1 118.2(17) . . ? C6_1 C5_1 C4_1 115.7(16) . . ? C7_1 C6_1 C5_1 118.5(16) . . ? N1_1 C7_1 C6_1 126.4(15) . . ? N1_1 C7_1 C2_1 114.3(14) . . ? C6_1 C7_1 C2_1 119.3(14) . . ? N4_1 C8_1 N3_1 109.7(13) . . ? N4_1 C8_1 S2_1 120.4(11) . . ? N3_1 C8_1 S2_1 129.9(13) . . ? C10_1 C9_1 N3_1 128.8(16) . . ? C10_1 C9_1 C14_1 122.7(16) . . ? N3_1 C9_1 C14_1 108.5(13) . . ? C9_1 C10_1 C11_1 113.7(16) . . ? C12_1 C11_1 C10_1 123.8(18) . . ? C11_1 C12_1 C13_1 124.5(18) . . ? C14_1 C13_1 C12_1 108.4(15) . . ? C13_1 C14_1 C9_1 126.5(15) . . ? C13_1 C14_1 N4_1 129.0(15) . . ? C9_1 C14_1 N4_1 104.1(13) . . ? C20_1 C19_1 N5_1 115(2) . . ? N6_1 C20_1 C19_1 112(2) . . ? N1_2 Mn1_2 N4_2 104.7(5) . . ? N1_2 Mn1_2 N6_2 89.6(5) . . ? N4_2 Mn1_2 N6_2 156.3(5) . . ? N1_2 Mn1_2 N5_2 149.8(5) . . ? N4_2 Mn1_2 N5_2 94.6(5) . . ? N6_2 Mn1_2 N5_2 81.0(5) . . ? N1_2 Mn1_2 S1_2 64.0(4) . . ? N4_2 Mn1_2 S1_2 100.8(4) . . ? N6_2 Mn1_2 S1_2 102.5(4) . . ? N5_2 Mn1_2 S1_2 90.0(4) . . ? N1_2 Mn1_2 S2_2 104.0(4) . . ? N4_2 Mn1_2 S2_2 65.9(4) . . ? N6_2 Mn1_2 S2_2 92.6(4) . . ? N5_2 Mn1_2 S2_2 105.0(4) . . ? S1_2 Mn1_2 S2_2 160.30(17) . . ? C1_2 S1_2 Mn1_2 71.5(6) . . ? C8_2 S2_2 Mn1_2 71.5(5) . . ? C1_2 N1_2 C7_2 111.8(14) . . ? C1_2 N1_2 Mn1_2 99.5(11) . . ? C7_2 N1_2 Mn1_2 147.9(11) . . ? C1_2 N2_2 C2_2 101.1(13) . . ? C8_2 N3_2 C9_2 104.2(13) . . ? C14_2 N4_2 C8_2 102.3(13) . . ? C14_2 N4_2 Mn1_2 156.2(12) . . ? C8_2 N4_2 Mn1_2 101.4(9) . . ? C15_2 N5_2 C19_2 111.3(17) . . ? C15_2 N5_2 C16_2 109.0(16) . . ? C19_2 N5_2 C16_2 105.6(17) . . ? C15_2 N5_2 Mn1_2 114.9(13) . . ? C19_2 N5_2 Mn1_2 107.3(13) . . ? C16_2 N5_2 Mn1_2 108.3(12) . . ? C17_2 N6_2 C18_2 114.5(16) . . ? C17_2 N6_2 C20_2 99.5(16) . . ? C18_2 N6_2 C20_2 104.7(17) . . ? C17_2 N6_2 Mn1_2 114.0(13) . . ? C18_2 N6_2 Mn1_2 116.3(12) . . ? C20_2 N6_2 Mn1_2 105.3(12) . . ? N1_2 C1_2 N2_2 109.5(15) . . ? N1_2 C1_2 S1_2 124.8(13) . . ? N2_2 C1_2 S1_2 125.7(13) . . ? C7_2 C2_2 N2_2 115.0(15) . . ? C7_2 C2_2 C3_2 125.2(16) . . ? N2_2 C2_2 C3_2 119.9(14) . . ? C2_2 C3_2 C4_2 102.2(14) . . ? C5_2 C4_2 C3_2 124.8(19) . . ? C4_2 C5_2 C6_2 127(2) . . ? C5_2 C6_2 C7_2 117.2(18) . . ? C2_2 C7_2 C6_2 123.1(17) . . ? C2_2 C7_2 N1_2 102.5(15) . . ? C6_2 C7_2 N1_2 134.0(16) . . ? N4_2 C8_2 N3_2 113.4(14) . . ? N4_2 C8_2 S2_2 121.1(11) . . ? N3_2 C8_2 S2_2 125.5(12) . . ? C14_2 C9_2 N3_2 104.8(14) . . ? C14_2 C9_2 C10_2 123.3(16) . . ? N3_2 C9_2 C10_2 132.0(15) . . ? C11_2 C10_2 C9_2 117.2(16) . . ? C10_2 C11_2 C12_2 120.7(17) . . ? C13_2 C12_2 C11_2 116.6(18) . . ? C12_2 C13_2 C14_2 127.1(17) . . ? N4_2 C14_2 C9_2 115.0(16) . . ? N4_2 C14_2 C13_2 129.8(15) . . ? C9_2 C14_2 C13_2 114.9(15) . . ? N5_2 C19_2 C20_2 114(2) . . ? C19_2 C20_2 N6_2 113(2) . . ? N4_3 Mn1_3 N1_3 107.1(5) . . ? N4_3 Mn1_3 N6_3 149.9(5) . . ? N1_3 Mn1_3 N6_3 96.9(5) . . ? N4_3 Mn1_3 N5_3 88.1(5) . . ? N1_3 Mn1_3 N5_3 158.9(5) . . ? N6_3 Mn1_3 N5_3 74.4(5) . . ? N4_3 Mn1_3 S1_3 101.1(4) . . ? N1_3 Mn1_3 S1_3 66.6(4) . . ? N6_3 Mn1_3 S1_3 105.1(4) . . ? N5_3 Mn1_3 S1_3 96.7(4) . . ? N4_3 Mn1_3 S2_3 64.0(4) . . ? N1_3 Mn1_3 S2_3 98.5(4) . . ? N6_3 Mn1_3 S2_3 95.1(4) . . ? N5_3 Mn1_3 S2_3 101.3(4) . . ? S1_3 Mn1_3 S2_3 155.9(2) . . ? C1_3 S1_3 Mn1_3 74.8(6) . . ? C8_3 S2_3 Mn1_3 73.0(6) . . ? C7_3 N1_3 C1_3 102.4(13) . . ? C7_3 N1_3 Mn1_3 157.6(12) . . ? C1_3 N1_3 Mn1_3 98.6(10) . . ? C1_3 N2_3 C2_3 105.3(14) . . ? C9_3 N3_3 C8_3 114.9(14) . . ? C8_3 N4_3 C14_3 110.9(12) . . ? C8_3 N4_3 Mn1_3 99.8(9) . . ? C14_3 N4_3 Mn1_3 148.4(11) . . ? C15_3 N5_3 C16_3 105.4(15) . . ? C15_3 N5_3 C19_3 104.6(16) . . ? C16_3 N5_3 C19_3 110.7(16) . . ? C15_3 N5_3 Mn1_3 115.8(12) . . ? C16_3 N5_3 Mn1_3 109.3(12) . . ? C19_3 N5_3 Mn1_3 111.0(12) . . ? C20_3 N6_3 C18_3 107.2(17) . . ? C20_3 N6_3 C17_3 113.9(18) . . ? C18_3 N6_3 C17_3 111.5(14) . . ? C20_3 N6_3 Mn1_3 107.0(13) . . ? C18_3 N6_3 Mn1_3 113.4(12) . . ? C17_3 N6_3 Mn1_3 103.9(11) . . ? N2_3 C1_3 N1_3 112.8(15) . . ? N2_3 C1_3 S1_3 126.3(13) . . ? N1_3 C1_3 S1_3 120.1(12) . . ? C3_3 C2_3 N2_3 128.1(16) . . ? C3_3 C2_3 C7_3 127.3(16) . . ? N2_3 C2_3 C7_3 104.6(14) . . ? C4_3 C3_3 C2_3 120.0(18) . . ? C3_3 C4_3 C5_3 123.4(18) . . ? C4_3 C5_3 C6_3 113.0(16) . . ? C7_3 C6_3 C5_3 118.7(16) . . ? N1_3 C7_3 C2_3 114.7(15) . . ? N1_3 C7_3 C6_3 127.8(16) . . ? C2_3 C7_3 C6_3 117.1(15) . . ? N4_3 C8_3 N3_3 105.8(13) . . ? N4_3 C8_3 S2_3 123.1(12) . . ? N3_3 C8_3 S2_3 131.0(13) . . ? C10_3 C9_3 N3_3 137.9(17) . . ? C10_3 C9_3 C14_3 118.6(16) . . ? N3_3 C9_3 C14_3 103.4(13) . . ? C9_3 C10_3 C11_3 119.7(18) . . ? C12_3 C11_3 C10_3 120.3(18) . . ? C11_3 C12_3 C13_3 126.6(19) . . ? C14_3 C13_3 C12_3 112.9(17) . . ? C13_3 C14_3 N4_3 133.4(15) . . ? C13_3 C14_3 C9_3 121.9(15) . . ? N4_3 C14_3 C9_3 104.5(13) . . ? C20_3 C19_3 N5_3 106(2) . . ? C19_3 C20_3 N6_3 128(2) . . ? N1_4 Mn1_4 N4_4 106.4(5) . . ? N1_4 Mn1_4 N6_4 89.7(5) . . ? N4_4 Mn1_4 N6_4 155.4(5) . . ? N1_4 Mn1_4 N5_4 150.4(5) . . ? N4_4 Mn1_4 N5_4 92.0(5) . . ? N6_4 Mn1_4 N5_4 81.8(5) . . ? N1_4 Mn1_4 S2_4 103.2(4) . . ? N4_4 Mn1_4 S2_4 66.4(4) . . ? N6_4 Mn1_4 S2_4 92.2(4) . . ? N5_4 Mn1_4 S2_4 105.5(4) . . ? N1_4 Mn1_4 S1_4 64.5(4) . . ? N4_4 Mn1_4 S1_4 96.3(4) . . ? N6_4 Mn1_4 S1_4 107.5(4) . . ? N5_4 Mn1_4 S1_4 91.1(4) . . ? S2_4 Mn1_4 S1_4 156.1(2) . . ? C1_4 S1_4 Mn1_4 73.8(6) . . ? C8_4 S2_4 Mn1_4 75.0(5) . . ? C1_4 N1_4 C7_4 107.6(13) . . ? C1_4 N1_4 Mn1_4 101.5(10) . . ? C7_4 N1_4 Mn1_4 150.7(10) . . ? C1_4 N2_4 C2_4 108.7(14) . . ? C8_4 N3_4 C9_4 101.6(14) . . ? C14_4 N4_4 C8_4 100.2(13) . . ? C14_4 N4_4 Mn1_4 158.7(12) . . ? C8_4 N4_4 Mn1_4 100.7(9) . . ? C19_4 N5_4 C16_4 111.0(17) . . ? C19_4 N5_4 C15_4 117.1(17) . . ? C16_4 N5_4 C15_4 107.5(15) . . ? C19_4 N5_4 Mn1_4 101.4(13) . . ? C16_4 N5_4 Mn1_4 109.0(12) . . ? C15_4 N5_4 Mn1_4 110.6(12) . . ? C17_4 N6_4 C18_4 108.8(16) . . ? C17_4 N6_4 C20_4 107.0(17) . . ? C18_4 N6_4 C20_4 113.1(16) . . ? C17_4 N6_4 Mn1_4 112.0(13) . . ? C18_4 N6_4 Mn1_4 113.3(13) . . ? C20_4 N6_4 Mn1_4 102.6(11) . . ? N1_4 C1_4 N2_4 112.0(15) . . ? N1_4 C1_4 S1_4 120.0(12) . . ? N2_4 C1_4 S1_4 127.3(14) . . ? N2_4 C2_4 C7_4 108.4(14) . . ? N2_4 C2_4 C3_4 134.1(15) . . ? C7_4 C2_4 C3_4 117.5(15) . . ? C2_4 C3_4 C4_4 111.7(15) . . ? C5_4 C4_4 C3_4 118.1(17) . . ? C6_4 C5_4 C4_4 130(2) . . ? C5_4 C6_4 C7_4 119.8(19) . . ? C6_4 C7_4 C2_4 123.0(15) . . ? C6_4 C7_4 N1_4 134.0(15) . . ? C2_4 C7_4 N1_4 102.8(13) . . ? N3_4 C8_4 N4_4 115.5(14) . . ? N3_4 C8_4 S2_4 126.5(13) . . ? N4_4 C8_4 S2_4 117.7(11) . . ? C14_4 C9_4 N3_4 108.6(14) . . ? C14_4 C9_4 C10_4 124.8(16) . . ? N3_4 C9_4 C10_4 126.7(15) . . ? C11_4 C10_4 C9_4 115.1(16) . . ? C10_4 C11_4 C12_4 123.1(17) . . ? C13_4 C12_4 C11_4 116.3(17) . . ? C12_4 C13_4 C14_4 120.0(16) . . ? C9_4 C14_4 N4_4 114.0(15) . . ? C9_4 C14_4 C13_4 120.2(16) . . ? N4_4 C14_4 C13_4 125.6(15) . . ? N5_4 C19_4 C20_4 117(2) . . ? N6_4 C20_4 C19_4 109.2(19) . . ? C22_5 N7_5 C26_5 116.4(14) . . ? C22_5 N7_5 C24_5 105.3(14) . . ? C26_5 N7_5 C24_5 94.2(13) . . ? C25_5 N8_5 C23_5 101.9(14) . . ? C25_5 N8_5 C21_5 117.7(15) . . ? C23_5 N8_5 C21_5 103.3(14) . . ? C22_5 C21_5 N8_5 108.9(16) . . ? N7_5 C22_5 C21_5 114.8(17) . . ? C24_5 C23_5 N8_5 108.6(15) . . ? C23_5 C24_5 N7_5 110.5(14) . . ? N8_5 C25_5 C26_5 110.5(16) . . ? C25_5 C26_5 N7_5 114.8(16) . . ? C21_6 N7_6 C25_6 111.8(16) . . ? C21_6 N7_6 C23_6 100.0(15) . . ? C25_6 N7_6 C23_6 115.3(16) . . ? C26_6 N8_6 C24_6 123.8(16) . . ? C26_6 N8_6 C22_6 108.0(15) . . ? C24_6 N8_6 C22_6 97.2(13) . . ? N7_6 C21_6 C22_6 111.4(16) . . ? N8_6 C22_6 C21_6 105.4(15) . . ? N7_6 C23_6 C24_6 111.8(16) . . ? N8_6 C24_6 C23_6 104.5(15) . . ? N7_6 C25_6 C26_6 108.2(16) . . ? N8_6 C26_6 C25_6 112.7(16) . . ? C21_7 N7_7 C23_7 110.8(14) . . ? C21_7 N7_7 C25_7 117.8(14) . . ? C23_7 N7_7 C25_7 99.3(14) . . ? C26_7 N8_7 C22_7 117.6(15) . . ? C26_7 N8_7 C24_7 101.4(14) . . ? C22_7 N8_7 C24_7 96.5(13) . . ? N7_7 C21_7 C22_7 111.4(17) . . ? C21_7 C22_7 N8_7 111.2(16) . . ? C24_7 C23_7 N7_7 107.6(15) . . ? C23_7 C24_7 N8_7 110.4(15) . . ? C26_7 C25_7 N7_7 105.8(15) . . ? N8_7 C26_7 C25_7 116.9(16) . . ? C25_8 N7_8 C23_8 123.3(16) . . ? C25_8 N7_8 C21_8 110.3(15) . . ? C23_8 N7_8 C21_8 95.3(15) . . ? C22_8 N8_8 C24_8 98.1(15) . . ? C22_8 N8_8 C26_8 119.4(16) . . ? C24_8 N8_8 C26_8 105.7(15) . . ? N7_8 C21_8 C22_8 100.3(13) . . ? N8_8 C22_8 C21_8 113.9(16) . . ? N7_8 C23_8 C24_8 113.3(17) . . ? N8_8 C24_8 C23_8 109.7(16) . . ? N7_8 C25_8 C26_8 103.6(15) . . ? N8_8 C26_8 C25_8 103.2(13) . . ? _diffrn_measured_fraction_theta_max 0.748 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.748 _refine_diff_density_max 1.195 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.134 data_dw9811 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H21 Mn0.50 N4 S' _chemical_formula_weight 292.87 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' 'S' 'S' 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.851(5) _cell_length_b 18.442(5) _cell_length_c 7.695(5) _cell_angle_alpha 101.71(4) _cell_angle_beta 109.06(4) _cell_angle_gamma 78.18(4) _cell_volume 1539.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9215 _exptl_absorpt_correction_T_max 0.9430 _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 RAXIS-IIC _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7669 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.1593 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.19 _reflns_number_total 4885 _reflns_number_gt 2749 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.038(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4885 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.74926(7) 0.25064(5) 0.29685(10) 0.0368(3) Uani 1 d . . . S1 S 0.67569(12) 0.12017(8) 0.2802(2) 0.0486(4) Uani 1 d . . . S2 S 0.82203(12) 0.38075(8) 0.48628(19) 0.0494(4) Uani 1 d . . . N7 N 0.8726(3) 0.5440(2) 0.1011(6) 0.0434(11) Uani 1 d . . . N8 N 0.6277(4) -0.0429(3) 0.6871(6) 0.0442(11) Uani 1 d . . . N1 N 0.5848(3) 0.2606(2) 0.3790(5) 0.0367(10) Uani 1 d . . . N2 N 0.4622(4) 0.1803(3) 0.3588(6) 0.0419(11) Uani 1 d . . . N3 N 0.9131(3) 0.2394(2) 0.5329(5) 0.0402(11) Uani 1 d . . . N4 N 1.0362(3) 0.3185(3) 0.7178(5) 0.0416(11) Uani 1 d . . . H28 H 1.0625 0.3610 0.7741 0.050 Uiso 1 calc R . . N5 N 0.6299(3) 0.2989(3) 0.0216(5) 0.0442(11) Uani 1 d . . . N6 N 0.8673(3) 0.2048(3) 0.0943(5) 0.0452(12) Uani 1 d . . . C8 C 0.9287(4) 0.3108(3) 0.5853(6) 0.0393(13) Uani 1 d . . . C9 C 1.0965(4) 0.2480(3) 0.7484(6) 0.0377(12) Uani 1 d . . . C10 C 1.2090(5) 0.2241(4) 0.8652(7) 0.0531(16) Uani 1 d . . . H10 H 1.2611 0.2582 0.9440 0.064 Uiso 1 calc R . . C11 C 1.2407(5) 0.1472(4) 0.8596(8) 0.0581(17) Uani 1 d . . . H11 H 1.3176 0.1280 0.9357 0.070 Uiso 1 calc R . . C12 C 1.1639(5) 0.0969(4) 0.7466(8) 0.0613(17) Uani 1 d . . . H12 H 1.1891 0.0446 0.7472 0.074 Uiso 1 calc R . . C13 C 1.0506(5) 0.1227(3) 0.6332(7) 0.0513(15) Uani 1 d . . . H13 H 0.9971 0.0889 0.5578 0.062 Uiso 1 calc R . . C14 C 1.0183(4) 0.1990(3) 0.6335(7) 0.0393(13) Uani 1 d . . . C1 C 0.5707(4) 0.1881(3) 0.3429(6) 0.0368(12) Uani 1 d . . . C2 C 0.4027(4) 0.2512(3) 0.4033(6) 0.0395(13) Uani 1 d . . . C3 C 0.2911(5) 0.2754(4) 0.4320(7) 0.0537(15) Uani 1 d . . . H3 H 0.2392 0.2412 0.4250 0.064 Uiso 1 calc R . . C4 C 0.2587(5) 0.3514(4) 0.4712(8) 0.0610(17) Uani 1 d . . . H4 H 0.1814 0.3701 0.4877 0.073 Uiso 1 calc R . . C5 C 0.3357(5) 0.4020(4) 0.4875(7) 0.0551(16) Uani 1 d . . . H5 H 0.3104 0.4542 0.5165 0.066 Uiso 1 calc R . . C6 C 0.4485(5) 0.3773(3) 0.4621(7) 0.0512(15) Uani 1 d . . . H6 H 0.5016 0.4117 0.4755 0.061 Uiso 1 calc R . . C7 C 0.4816(4) 0.3014(3) 0.4168(7) 0.0412(13) Uani 1 d . . . C24 C 0.7568(5) -0.0626(4) 0.7075(8) 0.0633(18) Uani 1 d . . . H24A H 0.7974 -0.0859 0.8201 0.095 Uiso 1 calc R . . H24B H 0.7908 -0.0172 0.7173 0.095 Uiso 1 calc R . . H24C H 0.7688 -0.0978 0.5989 0.095 Uiso 1 calc R . . C25 C 0.6097(5) 0.0074(3) 0.8483(8) 0.0620(17) Uani 1 d . . . H25A H 0.6276 0.0568 0.8467 0.093 Uiso 1 calc R . . H25B H 0.6635 -0.0122 0.9609 0.093 Uiso 1 calc R . . H25C H 0.5256 0.0119 0.8472 0.093 Uiso 1 calc R . . C26 C 0.5683(4) -0.0086(4) 0.5187(8) 0.0544(16) Uani 1 d . . . H26A H 0.5871 -0.0429 0.4115 0.065 Uiso 1 calc R . . H26B H 0.6003 0.0384 0.5314 0.065 Uiso 1 calc R . . C21 C 0.8916(5) 0.4934(3) 0.2348(8) 0.0613(17) Uani 1 d . . . H21A H 0.8665 0.4453 0.1685 0.092 Uiso 1 calc R . . H21B H 0.8437 0.5155 0.3202 0.092 Uiso 1 calc R . . H21C H 0.9773 0.4854 0.3056 0.092 Uiso 1 calc R . . C22 C 0.7433(4) 0.5651(4) 0.0127(8) 0.0637(17) Uani 1 d . . . H22A H 0.7319 0.5981 -0.0786 0.096 Uiso 1 calc R . . H22B H 0.7046 0.5913 0.1074 0.096 Uiso 1 calc R . . H22C H 0.7069 0.5199 -0.0500 0.096 Uiso 1 calc R . . C23 C 0.9324(4) 0.5084(4) -0.0399(7) 0.0548(16) Uani 1 d . . . H23A H 0.9128 0.5416 -0.1351 0.066 Uiso 1 calc R . . H23B H 0.9006 0.4610 -0.1021 0.066 Uiso 1 calc R . . C15 C 0.5283(4) 0.2575(3) -0.0685(7) 0.0571(17) Uani 1 d . . . H15A H 0.4772 0.2650 0.0131 0.086 Uiso 1 calc R . . H15B H 0.5587 0.2041 -0.0931 0.086 Uiso 1 calc R . . H15C H 0.4809 0.2757 -0.1860 0.086 Uiso 1 calc R . . C16 C 0.5831(5) 0.3786(3) 0.0576(8) 0.0588(17) Uani 1 d . . . H16A H 0.6507 0.4070 0.1158 0.088 Uiso 1 calc R . . H16B H 0.5332 0.3858 0.1409 0.088 Uiso 1 calc R . . H16C H 0.5342 0.3962 -0.0600 0.088 Uiso 1 calc R . . C17 C 0.7105(5) 0.2888(4) -0.0970(7) 0.0562(16) Uani 1 d . . . H17A H 0.6607 0.2938 -0.2265 0.067 Uiso 1 calc R . . H17B H 0.7618 0.3290 -0.0531 0.067 Uiso 1 calc R . . C18 C 0.7884(5) 0.2156(4) -0.0946(7) 0.0609(18) Uani 1 d . . . H18A H 0.8391 0.2115 -0.1772 0.073 Uiso 1 calc R . . H18B H 0.7373 0.1754 -0.1439 0.073 Uiso 1 calc R . . C19 C 0.9703(4) 0.2452(4) 0.1463(7) 0.0591(17) Uani 1 d . . . H19A H 1.0230 0.2360 0.2701 0.089 Uiso 1 calc R . . H19B H 0.9413 0.2990 0.1478 0.089 Uiso 1 calc R . . H19C H 1.0157 0.2278 0.0558 0.089 Uiso 1 calc R . . C20 C 0.9146(5) 0.1246(4) 0.0955(8) 0.0598(17) Uani 1 d . . . H20A H 0.9607 0.1076 0.0058 0.090 Uiso 1 calc R . . H20B H 0.8472 0.0962 0.0612 0.090 Uiso 1 calc R . . H20C H 0.9673 0.1167 0.2201 0.090 Uiso 1 calc R . . H27 H 0.445(4) 0.132(3) 0.353(6) 0.045(15) Uiso 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 0.0247(4) 0.0526(6) 0.0328(5) 0.0072(4) 0.0069(3) -0.0070(3) S1 0.0410(8) 0.0490(10) 0.0607(10) 0.0027(7) 0.0249(7) -0.0068(7) S2 0.0414(8) 0.0512(10) 0.0466(9) 0.0110(7) -0.0019(7) -0.0084(7) N7 0.027(2) 0.055(3) 0.045(3) 0.001(2) 0.007(2) -0.010(2) N8 0.032(2) 0.061(3) 0.041(3) 0.009(2) 0.008(2) -0.013(2) N1 0.029(2) 0.046(3) 0.036(2) 0.005(2) 0.0121(18) -0.004(2) N2 0.034(2) 0.048(3) 0.046(3) 0.000(2) 0.018(2) -0.009(2) N3 0.032(2) 0.051(3) 0.034(2) 0.008(2) 0.0050(19) -0.006(2) N4 0.025(2) 0.064(3) 0.033(2) 0.010(2) -0.0028(18) -0.017(2) N5 0.027(2) 0.070(3) 0.036(2) 0.013(2) 0.0063(19) -0.009(2) N6 0.027(2) 0.073(4) 0.034(3) 0.010(2) 0.0092(19) -0.003(2) C8 0.036(3) 0.054(4) 0.031(3) 0.011(3) 0.010(2) -0.006(3) C9 0.027(3) 0.054(4) 0.031(3) 0.011(3) 0.007(2) -0.003(2) C10 0.034(3) 0.073(5) 0.052(4) 0.021(3) 0.006(3) -0.009(3) C11 0.039(3) 0.079(5) 0.052(4) 0.027(3) 0.008(3) 0.006(3) C12 0.060(4) 0.063(4) 0.056(4) 0.016(3) 0.017(3) 0.009(3) C13 0.048(3) 0.066(4) 0.040(3) 0.017(3) 0.008(3) -0.008(3) C14 0.032(3) 0.052(4) 0.033(3) 0.011(3) 0.006(2) -0.007(3) C1 0.032(3) 0.046(3) 0.035(3) 0.006(2) 0.013(2) -0.007(2) C2 0.032(3) 0.057(4) 0.026(3) 0.003(2) 0.003(2) -0.010(3) C3 0.030(3) 0.072(5) 0.055(4) 0.006(3) 0.009(3) -0.006(3) C4 0.040(3) 0.090(5) 0.051(4) 0.009(4) 0.018(3) -0.001(3) C5 0.050(4) 0.065(4) 0.046(4) 0.008(3) 0.016(3) 0.004(3) C6 0.052(4) 0.060(4) 0.043(3) 0.013(3) 0.019(3) 0.001(3) C7 0.035(3) 0.056(4) 0.032(3) 0.007(3) 0.009(2) -0.005(3) C24 0.037(3) 0.083(5) 0.075(4) 0.030(4) 0.014(3) -0.007(3) C25 0.070(4) 0.060(4) 0.048(4) 0.007(3) 0.008(3) -0.007(3) C26 0.040(3) 0.082(5) 0.047(3) 0.023(3) 0.008(3) -0.015(3) C21 0.063(4) 0.075(5) 0.058(4) 0.018(3) 0.026(3) -0.015(3) C22 0.030(3) 0.093(5) 0.062(4) 0.000(3) 0.011(3) -0.009(3) C23 0.027(3) 0.094(5) 0.041(4) 0.004(3) 0.010(3) -0.011(3) C15 0.034(3) 0.087(5) 0.044(4) 0.009(3) -0.004(3) -0.022(3) C16 0.034(3) 0.080(5) 0.060(4) 0.024(3) 0.005(3) -0.002(3) C17 0.041(3) 0.087(5) 0.042(3) 0.021(3) 0.009(3) -0.006(3) C18 0.037(3) 0.108(6) 0.035(3) 0.011(3) 0.009(3) -0.008(3) C19 0.034(3) 0.099(5) 0.048(4) 0.008(3) 0.010(3) -0.024(3) C20 0.043(3) 0.086(5) 0.048(4) 0.002(3) 0.016(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N3 2.190(4) . ? Mn1 N1 2.201(4) . ? Mn1 N6 2.347(4) . ? Mn1 N5 2.361(4) . ? Mn1 S1 2.6884(18) . ? Mn1 S2 2.690(2) . ? S1 C1 1.690(5) . ? S2 C8 1.716(5) . ? N7 C21 1.461(6) . ? N7 C23 1.460(7) . ? N7 C22 1.464(6) . ? N8 C25 1.438(7) . ? N8 C26 1.459(6) . ? N8 C24 1.461(6) . ? N1 C1 1.343(6) . ? N1 C7 1.384(6) . ? N2 C1 1.369(6) . ? N2 C2 1.386(6) . ? N3 C8 1.329(6) . ? N3 C14 1.390(6) . ? N4 C8 1.360(5) . ? N4 C9 1.374(6) . ? N5 C15 1.459(6) . ? N5 C16 1.464(7) . ? N5 C17 1.486(6) . ? N6 C19 1.463(6) . ? N6 C20 1.470(7) . ? N6 C18 1.476(6) . ? C9 C10 1.385(6) . ? C9 C14 1.393(7) . ? C10 C11 1.387(8) . ? C11 C12 1.396(8) . ? C12 C13 1.390(7) . ? C13 C14 1.380(7) . ? C2 C3 1.381(7) . ? C2 C7 1.411(7) . ? C3 C4 1.374(8) . ? C4 C5 1.395(8) . ? C5 C6 1.385(7) . ? C6 C7 1.379(7) . ? C26 C26 1.526(9) 2_656 ? C23 C23 1.507(9) 2_765 ? C17 C18 1.471(7) . ? 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 111.99(15) . . ? N3 Mn1 N6 89.23(15) . . ? N1 Mn1 N6 152.75(15) . . ? N3 Mn1 N5 152.82(15) . . ? N1 Mn1 N5 89.11(14) . . ? N6 Mn1 N5 77.10(14) . . ? N3 Mn1 S1 98.47(13) . . ? N1 Mn1 S1 64.83(12) . . ? N6 Mn1 S1 96.30(13) . . ? N5 Mn1 S1 106.22(12) . . ? N3 Mn1 S2 65.06(13) . . ? N1 Mn1 S2 98.33(13) . . ? N6 Mn1 S2 106.33(13) . . ? N5 Mn1 S2 96.07(13) . . ? S1 Mn1 S2 151.27(6) . . ? C1 S1 Mn1 74.05(18) . . ? C8 S2 Mn1 73.55(19) . . ? C21 N7 C23 110.2(5) . . ? C21 N7 C22 110.3(4) . . ? C23 N7 C22 110.0(4) . . ? C25 N8 C26 111.0(5) . . ? C25 N8 C24 109.7(5) . . ? C26 N8 C24 108.9(4) . . ? C1 N1 C7 107.2(4) . . ? C1 N1 Mn1 99.2(3) . . ? C7 N1 Mn1 152.1(4) . . ? C1 N2 C2 108.0(4) . . ? C8 N3 C14 105.3(4) . . ? C8 N3 Mn1 99.9(3) . . ? C14 N3 Mn1 152.8(4) . . ? C8 N4 C9 107.9(4) . . ? C15 N5 C16 108.8(4) . . ? C15 N5 C17 111.4(4) . . ? C16 N5 C17 109.2(4) . . ? C15 N5 Mn1 109.3(3) . . ? C16 N5 Mn1 112.2(3) . . ? C17 N5 Mn1 106.0(3) . . ? C19 N6 C20 107.8(4) . . ? C19 N6 C18 110.7(4) . . ? C20 N6 C18 108.6(4) . . ? C19 N6 Mn1 110.4(3) . . ? C20 N6 Mn1 112.4(3) . . ? C18 N6 Mn1 107.0(3) . . ? N3 C8 N4 111.7(4) . . ? N3 C8 S2 121.1(4) . . ? N4 C8 S2 127.3(4) . . ? N4 C9 C10 131.6(5) . . ? N4 C9 C14 105.4(4) . . ? C10 C9 C14 123.0(5) . . ? C9 C10 C11 115.6(5) . . ? C10 C11 C12 122.5(5) . . ? C13 C12 C11 120.5(6) . . ? C14 C13 C12 118.0(5) . . ? C13 C14 N3 129.9(5) . . ? C13 C14 C9 120.4(4) . . ? N3 C14 C9 109.7(5) . . ? N1 C1 N2 110.5(4) . . ? N1 C1 S1 121.6(4) . . ? N2 C1 S1 127.9(4) . . ? C3 C2 N2 132.0(5) . . ? C3 C2 C7 122.2(6) . . ? N2 C2 C7 105.8(5) . . ? C4 C3 C2 116.7(6) . . ? C3 C4 C5 122.0(6) . . ? C6 C5 C4 120.9(6) . . ? C7 C6 C5 118.1(6) . . ? C6 C7 N1 131.5(5) . . ? C6 C7 C2 119.9(5) . . ? N1 C7 C2 108.6(5) . . ? N8 C26 C26 111.8(5) . 2_656 ? N7 C23 C23 112.7(5) . 2_765 ? C18 C17 N5 112.5(5) . . ? C17 C18 N6 112.1(5) . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 0.335 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.091 data_dw9818 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H38 Mn N8 S2' _chemical_formula_weight 581.70 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 20.084(5) _cell_length_b 8.384(5) _cell_length_c 18.339(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.08(4) _cell_angle_gamma 90.00 _cell_volume 2952(2) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8314 _exptl_absorpt_correction_T_max 0.8658 _exptl_special_details ; High temperature form ; _diffrn_ambient_temperature 210(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 RAXIS-IIC _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4886 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.1147 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.13 _reflns_number_total 2575 _reflns_number_gt 1749 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0169P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0235(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2575 _refine_ls_number_parameters 201 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.131 _refine_ls_shift/su_mean 0.027 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.0000 0.22996(9) 0.7500 0.0345(2) Uani 1 d S . . S1 S 0.11216(4) 0.28697(12) 0.87230(3) 0.0450(3) Uani 1 d . . . N1 N 0.17781(12) 0.4953(3) 0.79959(10) 0.0365(6) Uani 1 d . . . H1 H 0.2127 0.5178 0.8392 0.044 Uiso 1 calc R . . C1 C 0.12405(14) 0.3959(4) 0.79855(12) 0.0336(7) Uani 1 d . . . N2 N 0.07800(12) 0.3880(3) 0.72824(10) 0.0366(6) Uani 1 d . . . C2 C 0.10452(15) 0.4871(4) 0.68288(13) 0.0352(7) Uani 1 d . . . N3 N -0.03467(17) 0.0169(4) 0.81031(15) 0.0681(9) Uani 1 d . . . C3 C 0.07714(17) 0.5237(4) 0.60515(13) 0.0476(9) Uani 1 d . . . H3 H 0.0346 0.4814 0.5752 0.057 Uiso 1 calc R . . C4 C 0.1166(2) 0.6260(5) 0.57513(16) 0.0568(10) Uani 1 d . . . H4 H 0.0997 0.6539 0.5233 0.068 Uiso 1 calc R . . C5 C 0.1791(2) 0.6885(5) 0.61759(17) 0.0569(10) Uani 1 d . . . H5 H 0.2042 0.7548 0.5938 0.068 Uiso 1 calc R . . C6 C 0.20623(16) 0.6559(4) 0.69529(14) 0.0465(8) Uani 1 d . . . H6 H 0.2485 0.7001 0.7249 0.056 Uiso 1 calc R . . C7 C 0.16724(15) 0.5549(4) 0.72612(13) 0.0354(7) Uani 1 d . . . C8 C -0.0041(5) -0.1236(7) 0.7865(3) 0.167(3) Uani 1 d . . . H8A H 0.0419 -0.1404 0.8232 0.200 Uiso 1 calc R . . H8B H -0.0329 -0.2157 0.7903 0.200 Uiso 1 calc R . . C9 C -0.1114(2) 0.0117(7) 0.7859(2) 0.108(2) Uani 1 d . . . H9A H -0.1269 -0.0809 0.8081 0.162 Uiso 1 calc R . . H9B H -0.1283 0.0049 0.7307 0.162 Uiso 1 calc R . . H9C H -0.1294 0.1077 0.8028 0.162 Uiso 1 calc R . . C10 C -0.0119(3) 0.0275(7) 0.89453(18) 0.117(2) Uani 1 d . . . H10A H -0.0284 -0.0652 0.9158 0.175 Uiso 1 calc R . . H10B H -0.0308 0.1234 0.9103 0.175 Uiso 1 calc R . . H10C H 0.0386 0.0312 0.9127 0.175 Uiso 1 calc R . . N4 N 0.25691(15) 0.8391(4) 1.05972(12) 0.0475(7) Uani 1 d D . . C11 C 0.3302(4) 0.8100(14) 1.0488(5) 0.074(3) Uani 0.50 d PD A -1 H11A H 0.3605 0.7564 1.0939 0.088 Uiso 0.50 calc PR A -1 H11B H 0.3516 0.9123 1.0427 0.088 Uiso 0.50 calc PR A -1 C12 C 0.3221(4) 0.7024(15) 0.9754(5) 0.079(3) Uani 0.50 d PD . -1 H12A H 0.3392 0.7602 0.9380 0.119 Uiso 0.50 calc PR . -1 H12B H 0.3494 0.6044 0.9895 0.119 Uiso 0.50 calc PR . -1 C13 C 0.2194(7) 0.9178(14) 0.9936(4) 0.086(4) Uani 0.50 d PD A -1 H13A H 0.2436 1.0161 0.9874 0.103 Uiso 0.50 calc PR A -1 H13B H 0.1732 0.9467 0.9973 0.103 Uiso 0.50 calc PR A -1 C14 C 0.2118(8) 0.8068(16) 0.9235(5) 0.119(6) Uani 0.50 d PD . -1 H14A H 0.1621 0.7903 0.8980 0.178 Uiso 0.50 calc PR . -1 H14B H 0.2316 0.8613 0.8874 0.178 Uiso 0.50 calc PR . -1 C15 C 0.2325(8) 0.6848(14) 1.0690(5) 0.108(6) Uani 0.50 d PD A -1 H15A H 0.1869 0.6934 1.0779 0.130 Uiso 0.50 calc PR A -1 H15B H 0.2646 0.6349 1.1141 0.130 Uiso 0.50 calc PR A -1 C16 C 0.2260(10) 0.5775(15) 0.9990(5) 0.114(6) Uani 0.50 d PD . -1 H16A H 0.2571 0.4855 1.0143 0.171 Uiso 0.50 calc PR . -1 H16B H 0.1782 0.5375 0.9800 0.171 Uiso 0.50 calc PR . -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 0.0331(4) 0.0360(5) 0.0322(3) 0.000 0.0063(2) 0.000 S1 0.0502(5) 0.0549(6) 0.0276(3) 0.0007(4) 0.0081(3) -0.0141(5) N1 0.0386(14) 0.0384(16) 0.0300(10) -0.0034(11) 0.0064(9) -0.0051(13) C1 0.0308(15) 0.042(2) 0.0288(12) -0.0041(13) 0.0107(11) -0.0021(15) N2 0.0376(14) 0.0436(17) 0.0288(10) -0.0040(11) 0.0098(10) -0.0050(13) C2 0.0371(17) 0.0411(19) 0.0309(12) -0.0028(14) 0.0155(12) 0.0052(16) N3 0.070(2) 0.057(2) 0.0657(16) 0.0207(17) 0.0018(16) -0.0198(19) C3 0.056(2) 0.056(2) 0.0313(13) 0.0010(15) 0.0137(14) 0.0060(19) C4 0.077(3) 0.059(3) 0.0388(15) 0.0105(18) 0.0246(17) 0.014(2) C5 0.075(3) 0.052(2) 0.0599(17) 0.0114(19) 0.0448(18) 0.008(2) C6 0.050(2) 0.041(2) 0.0549(16) 0.0005(16) 0.0245(16) -0.0008(18) C7 0.0406(17) 0.0333(18) 0.0362(13) -0.0016(13) 0.0176(13) 0.0012(16) C8 0.262(8) 0.045(4) 0.209(8) 0.043(4) 0.091(8) 0.009(6) C9 0.076(3) 0.125(5) 0.100(3) 0.049(3) -0.010(2) -0.057(4) C10 0.119(4) 0.142(5) 0.067(2) 0.056(3) -0.008(2) -0.064(4) N4 0.0593(18) 0.0448(19) 0.0347(11) -0.0039(13) 0.0081(12) -0.0151(16) C11 0.056(5) 0.083(8) 0.079(5) -0.036(5) 0.014(4) -0.013(6) C12 0.065(6) 0.085(8) 0.085(6) -0.045(6) 0.019(5) -0.019(6) C13 0.121(8) 0.081(9) 0.035(4) -0.011(5) -0.009(5) 0.048(9) C14 0.179(14) 0.099(12) 0.038(4) -0.017(6) -0.031(7) 0.079(11) C15 0.188(14) 0.096(10) 0.061(6) -0.037(6) 0.066(9) -0.102(12) C16 0.228(16) 0.081(9) 0.059(6) -0.027(6) 0.082(9) -0.081(12) _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 N2 2.176(3) . ? Mn1 N2 2.176(2) 2_556 ? Mn1 N3 2.313(3) . ? Mn1 N3 2.313(3) 2_556 ? Mn1 S1 2.7139(15) 2_556 ? Mn1 S1 2.7139(15) . ? S1 C1 1.706(3) . ? N1 C1 1.360(4) . ? N1 C7 1.394(3) . ? C1 N2 1.350(3) . ? N2 C2 1.388(3) . ? C2 C7 1.397(4) . ? C2 C3 1.403(3) . ? N3 C8 1.454(6) . ? N3 C9 1.473(5) . ? N3 C10 1.479(4) . ? C3 C4 1.387(4) . ? C4 C5 1.372(5) . ? C5 C6 1.395(4) . ? C6 C7 1.382(4) . ? C8 C8 1.396(9) 2_556 ? N4 C14 1.368(11) 7_567 ? N4 C13 1.392(8) . ? N4 C16 1.409(8) 7_567 ? N4 C15 1.411(9) . ? N4 C11 1.562(8) . ? N4 C12 1.567(8) 7_567 ? C11 C12 1.589(9) . ? C12 N4 1.567(8) 7_567 ? C13 C14 1.558(11) . ? C14 N4 1.368(11) 7_567 ? C15 C16 1.541(11) . ? C16 N4 1.409(8) 7_567 ? 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 N2 Mn1 N2 105.00(14) . 2_556 ? N2 Mn1 N3 153.10(10) . . ? N2 Mn1 N3 92.77(12) 2_556 . ? N2 Mn1 N3 92.76(12) . 2_556 ? N2 Mn1 N3 153.10(11) 2_556 2_556 ? N3 Mn1 N3 78.92(19) . 2_556 ? N2 Mn1 S1 102.04(6) . 2_556 ? N2 Mn1 S1 64.97(5) 2_556 2_556 ? N3 Mn1 S1 103.76(8) . 2_556 ? N3 Mn1 S1 91.96(8) 2_556 2_556 ? N2 Mn1 S1 64.97(5) . . ? N2 Mn1 S1 102.05(6) 2_556 . ? N3 Mn1 S1 91.96(8) . . ? N3 Mn1 S1 103.76(8) 2_556 . ? S1 Mn1 S1 159.71(5) 2_556 . ? C1 S1 Mn1 73.42(10) . . ? C1 N1 C7 108.2(2) . . ? N2 C1 N1 111.2(2) . . ? N2 C1 S1 121.0(2) . . ? N1 C1 S1 127.8(2) . . ? C1 N2 C2 105.5(2) . . ? C1 N2 Mn1 100.55(16) . . ? C2 N2 Mn1 153.90(17) . . ? N2 C2 C7 110.1(2) . . ? N2 C2 C3 129.4(3) . . ? C7 C2 C3 120.4(3) . . ? C8 N3 C9 112.4(5) . . ? C8 N3 C10 109.5(4) . . ? C9 N3 C10 107.2(3) . . ? C8 N3 Mn1 105.6(3) . . ? C9 N3 Mn1 108.2(3) . . ? C10 N3 Mn1 114.1(3) . . ? C4 C3 C2 116.1(3) . . ? C5 C4 C3 123.0(3) . . ? C4 C5 C6 121.5(3) . . ? C7 C6 C5 116.1(3) . . ? C6 C7 N1 132.2(3) . . ? C6 C7 C2 122.8(2) . . ? N1 C7 C2 105.0(2) . . ? C8 C8 N3 117.9(4) 2_556 . ? C14 N4 C13 135.6(5) 7_567 . ? C14 N4 C16 114.6(8) 7_567 7_567 ? C13 N4 C16 44.7(6) . 7_567 ? C14 N4 C15 46.1(7) 7_567 . ? C13 N4 C15 114.9(7) . . ? C16 N4 C15 135.9(5) 7_567 . ? C14 N4 C11 60.1(7) 7_567 . ? C13 N4 C11 104.6(6) . . ? C16 N4 C11 61.9(7) 7_567 . ? C15 N4 C11 104.2(7) . . ? C14 N4 C12 103.7(7) 7_567 7_567 ? C13 N4 C12 61.5(6) . 7_567 ? C16 N4 C12 103.9(7) 7_567 7_567 ? C15 N4 C12 60.0(6) . 7_567 ? C11 N4 C12 142.4(4) . 7_567 ? N4 C11 C12 109.4(6) . . ? N4 C12 C11 108.2(6) 7_567 . ? N4 C13 C14 109.4(7) . . ? N4 C14 C13 115.0(7) 7_567 . ? N4 C15 C16 112.5(6) . . ? N4 C16 C15 111.5(8) 7_567 . ? _diffrn_measured_fraction_theta_max 0.455 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.455 _refine_diff_density_max 0.254 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.063