# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2015 data_[Mn(bimb)3](ClO4)2.2H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H58 Cl2 Mn N12 O10' _chemical_formula_weight 1233.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 33.921(11) _cell_length_b 10.103(2) _cell_length_c 17.915(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6140(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 11.29 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 0.369 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8725 _exptl_absorpt_correction_T_max 0.9037 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.95 _diffrn_reflns_number 6423 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.2141 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5577 _reflns_number_gt 1798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00010(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(5) _refine_ls_number_reflns 5577 _refine_ls_number_parameters 767 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1827 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 0.722 _refine_ls_restrained_S_all 0.722 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.62626(6) 0.00009(18) 0.64470(18) 0.0461(3) Uani 1 1 d . . . Cl1 Cl 0.76450(17) -0.5083(4) 0.9608(3) 0.1078(17) Uani 1 1 d . . . Cl2 Cl 0.49534(15) 0.5127(4) 0.3201(2) 0.0843(13) Uani 1 1 d . . . O1 O 0.7713(3) -0.5691(10) 0.8913(6) 0.106(3) Uani 1 1 d . . . O2 O 0.7210(5) -0.5021(18) 0.9665(14) 0.291(12) Uani 1 1 d . . . O3 O 0.7757(4) -0.3765(8) 0.9629(7) 0.150(5) Uani 1 1 d . . . O4 O 0.7754(4) -0.5767(11) 1.0214(6) 0.150(5) Uani 1 1 d . . . O5 O 0.5348(3) 0.4956(10) 0.3032(8) 0.137(4) Uani 1 1 d . . . O6 O 0.4939(4) 0.5679(9) 0.3924(5) 0.137(4) Uani 1 1 d . . . O7 O 0.4792(3) 0.6052(12) 0.2706(6) 0.142(5) Uani 1 1 d . . . O8 O 0.4764(3) 0.3887(9) 0.3193(7) 0.125(4) Uani 1 1 d . . . O9W O 0.3567(4) 0.4333(17) 0.3583(8) 0.326(11) Uani 1 1 d . . . O10W O 0.6232(4) 0.566(2) 0.4232(7) 0.363(13) Uani 1 1 d . . . N1 N 0.6761(3) 0.1295(10) 0.6862(5) 0.046(3) Uani 1 1 d . . . N2 N 0.7336(2) 0.2313(9) 0.6886(6) 0.052(3) Uani 1 1 d . . . N3 N 1.0552(3) -0.0509(11) 0.8487(6) 0.055(3) Uani 1 1 d . . . N4 N 1.0990(3) -0.0071(10) 0.7622(6) 0.052(3) Uani 1 1 d . . . N5 N 0.5774(2) -0.1360(11) 0.6094(6) 0.053(3) Uani 1 1 d . . . N6 N 0.5224(3) -0.2493(9) 0.6071(6) 0.053(3) Uani 1 1 d . . . N7 N 0.1984(2) 0.0107(9) 0.4437(5) 0.038(2) Uani 1 1 d . . . N8 N 0.1530(3) -0.0070(9) 0.5325(6) 0.048(3) Uani 1 1 d . . . N9 N 0.5887(2) 0.1738(10) 0.6138(5) 0.045(3) Uani 1 1 d . . . N10 N 0.5434(3) 0.2898(11) 0.5544(6) 0.058(3) Uani 1 1 d . . . N11 N 0.2077(3) 0.3130(11) 0.7199(6) 0.061(3) Uani 1 1 d . . . N12 N 0.1622(3) 0.1810(10) 0.6718(6) 0.060(3) Uani 1 1 d . . . C1 C 0.6852(4) 0.1679(14) 0.7587(7) 0.064(4) Uani 1 1 d . . . H1 H 0.6694 0.1524 0.8001 0.077 Uiso 1 1 calc R . . C2 C 0.7206(4) 0.2312(12) 0.7606(8) 0.062(4) Uani 1 1 d . . . H2 H 0.7331 0.2668 0.8022 0.075 Uiso 1 1 calc R . . C3 C 0.7058(3) 0.1736(10) 0.6488(7) 0.053(3) Uani 1 1 d . . . H3 H 0.7075 0.1652 0.5972 0.063 Uiso 1 1 calc R . . C4 C 0.7721(3) 0.2894(11) 0.6621(7) 0.061(4) Uani 1 1 d . . . H4A H 0.7742 0.2771 0.6086 0.073 Uiso 1 1 calc R . . H4B H 0.7721 0.3838 0.6720 0.073 Uiso 1 1 calc R . . C5 C 0.8072(4) 0.2278(12) 0.6992(7) 0.051(3) Uani 1 1 d . . . C6 C 0.8133(4) 0.0921(12) 0.7041(7) 0.061(4) Uani 1 1 d . . . H6 H 0.7942 0.0347 0.6857 0.074 Uiso 1 1 calc R . . C7 C 0.8473(4) 0.0404(12) 0.7358(7) 0.059(4) Uani 1 1 d . . . H7 H 0.8511 -0.0507 0.7363 0.070 Uiso 1 1 calc R . . C8 C 0.8750(3) 0.1210(12) 0.7662(6) 0.044(3) Uani 1 1 d . . . C9 C 0.8689(3) 0.2537(12) 0.7650(7) 0.068(4) Uani 1 1 d . . . H9 H 0.8871 0.3116 0.7860 0.082 Uiso 1 1 calc R . . C10 C 0.8349(4) 0.3004(12) 0.7318(8) 0.069(4) Uani 1 1 d . . . H10 H 0.8310 0.3915 0.7323 0.083 Uiso 1 1 calc R . . C11 C 0.9115(4) 0.0620(13) 0.8009(7) 0.046(3) Uani 1 1 d . . . C12 C 0.9135(3) -0.0663(14) 0.8200(8) 0.058(4) Uani 1 1 d . . . H12 H 0.8917 -0.1212 0.8143 0.069 Uiso 1 1 calc R . . C13 C 0.9492(4) -0.1164(12) 0.8489(6) 0.058(4) Uani 1 1 d . . . H13 H 0.9501 -0.2042 0.8644 0.069 Uiso 1 1 calc R . . C14 C 0.9821(3) -0.0421(12) 0.8549(7) 0.043(3) Uani 1 1 d . . . C15 C 0.9790(3) 0.0908(12) 0.8375(7) 0.061(4) Uani 1 1 d . . . H15 H 1.0006 0.1462 0.8443 0.073 Uiso 1 1 calc R . . C16 C 0.9450(4) 0.1410(13) 0.8109(8) 0.078(5) Uani 1 1 d . . . H16 H 0.9438 0.2304 0.7988 0.094 Uiso 1 1 calc R . . C17 C 1.0193(3) -0.1010(10) 0.8859(6) 0.049(3) Uani 1 1 d . . . H17A H 1.0208 -0.0813 0.9388 0.059 Uiso 1 1 calc R . . H17B H 1.0182 -0.1964 0.8804 0.059 Uiso 1 1 calc R . . C18 C 1.0766(4) 0.0615(13) 0.8704(7) 0.069(4) Uani 1 1 d . . . H18 H 1.0732 0.1107 0.9138 0.083 Uiso 1 1 calc R . . C19 C 1.1032(3) 0.0840(12) 0.8157(7) 0.057(3) Uani 1 1 d . . . H19 H 1.1216 0.1522 0.8153 0.069 Uiso 1 1 calc R . . C20 C 1.0698(3) -0.0814(12) 0.7832(6) 0.044(3) Uani 1 1 d . . . H20 H 1.0602 -0.1506 0.7542 0.053 Uiso 1 1 calc R . . C21 C 0.5706(3) -0.1829(13) 0.5415(8) 0.060(4) Uani 1 1 d . . . H21 H 0.5875 -0.1686 0.5013 0.071 Uiso 1 1 calc R . . C22 C 0.5363(4) -0.2546(13) 0.5362(7) 0.060(4) Uani 1 1 d . . . H22 H 0.5254 -0.2960 0.4947 0.072 Uiso 1 1 calc R . . C23 C 0.5471(3) -0.1744(10) 0.6498(7) 0.053(3) Uani 1 1 d . . . H23 H 0.5431 -0.1536 0.6998 0.064 Uiso 1 1 calc R . . C24 C 0.4844(3) -0.3057(12) 0.6366(7) 0.073(4) Uani 1 1 d . . . H24A H 0.4827 -0.2896 0.6899 0.088 Uiso 1 1 calc R . . H24B H 0.4841 -0.4007 0.6287 0.088 Uiso 1 1 calc R . . C25 C 0.4480(3) -0.2413(13) 0.5965(9) 0.064(4) Uani 1 1 d . . . C26 C 0.4405(3) -0.1125(13) 0.6015(7) 0.056(4) Uani 1 1 d . . . H26 H 0.4577 -0.0577 0.6276 0.068 Uiso 1 1 calc R . . C27 C 0.4078(4) -0.0604(12) 0.5687(7) 0.055(3) Uani 1 1 d . . . H27 H 0.4033 0.0302 0.5724 0.066 Uiso 1 1 calc R . . C28 C 0.3808(4) -0.1384(13) 0.5298(8) 0.064(4) Uani 1 1 d . . . C29 C 0.3894(4) -0.2704(15) 0.5300(11) 0.144(9) Uani 1 1 d . . . H29 H 0.3716 -0.3287 0.5081 0.172 Uiso 1 1 calc R . . C30 C 0.4239(4) -0.3216(15) 0.5617(12) 0.143(9) Uani 1 1 d . . . H30 H 0.4296 -0.4114 0.5582 0.171 Uiso 1 1 calc R . . C31 C 0.3441(3) -0.0884(13) 0.4998(7) 0.054(4) Uani 1 1 d . . . C32 C 0.3361(4) 0.0454(14) 0.4841(11) 0.105(7) Uani 1 1 d . . . H32 H 0.3565 0.1049 0.4931 0.127 Uiso 1 1 calc R . . C33 C 0.3024(4) 0.0973(13) 0.4575(10) 0.096(6) Uani 1 1 d . . . H33 H 0.2995 0.1882 0.4515 0.115 Uiso 1 1 calc R . . C34 C 0.2712(4) 0.0082(11) 0.4390(7) 0.049(4) Uani 1 1 d . . . C35 C 0.2768(4) -0.1283(12) 0.4558(8) 0.074(4) Uani 1 1 d . . . H35 H 0.2566 -0.1892 0.4485 0.089 Uiso 1 1 calc R . . C36 C 0.3126(3) -0.1676(12) 0.4830(7) 0.065(4) Uani 1 1 d . . . H36 H 0.3158 -0.2579 0.4910 0.077 Uiso 1 1 calc R . . C37 C 0.2326(3) 0.0583(10) 0.4049(6) 0.062(4) Uani 1 1 d . . . H37A H 0.2325 0.1543 0.4058 0.074 Uiso 1 1 calc R . . H37B H 0.2312 0.0304 0.3532 0.074 Uiso 1 1 calc R . . C38 C 0.1792(4) -0.1019(14) 0.4291(7) 0.071(4) Uani 1 1 d . . . H38 H 0.1843 -0.1604 0.3902 0.085 Uiso 1 1 calc R . . C39 C 0.1505(3) -0.1142(12) 0.4834(7) 0.065(4) Uani 1 1 d . . . H39 H 0.1323 -0.1829 0.4866 0.078 Uiso 1 1 calc R . . C40 C 0.1821(3) 0.0650(12) 0.5051(7) 0.053(4) Uani 1 1 d . . . H40 H 0.1905 0.1445 0.5259 0.064 Uiso 1 1 calc R . . C41 C 0.5943(3) 0.3073(14) 0.6282(8) 0.078(5) Uani 1 1 d . . . H41 H 0.6145 0.3418 0.6574 0.094 Uiso 1 1 calc R . . C42 C 0.5653(4) 0.3825(14) 0.5927(7) 0.076(4) Uani 1 1 d . . . H42 H 0.5616 0.4736 0.5945 0.091 Uiso 1 1 calc R . . C43 C 0.5574(4) 0.1673(15) 0.5641(8) 0.068(4) Uani 1 1 d . . . H43 H 0.5478 0.0910 0.5415 0.082 Uiso 1 1 calc R . . C44 C 0.5091(3) 0.3179(14) 0.5038(7) 0.085(5) Uani 1 1 d . . . H44A H 0.5086 0.2535 0.4637 0.102 Uiso 1 1 calc R . . H44B H 0.5121 0.4051 0.4818 0.102 Uiso 1 1 calc R . . C45 C 0.4708(3) 0.3118(12) 0.5470(7) 0.054(3) Uani 1 1 d . . . C46 C 0.4669(4) 0.2936(14) 0.6226(7) 0.078(5) Uani 1 1 d . . . H46 H 0.4891 0.2777 0.6519 0.094 Uiso 1 1 calc R . . C47 C 0.4292(3) 0.2990(12) 0.6560(6) 0.063(4) Uani 1 1 d . . . H47 H 0.4273 0.2888 0.7074 0.076 Uiso 1 1 calc R . . C48 C 0.3955(3) 0.3187(11) 0.6158(6) 0.044(3) Uani 1 1 d . . . C49 C 0.3990(3) 0.3404(10) 0.5406(7) 0.043(3) Uani 1 1 d . . . H49 H 0.3768 0.3578 0.5117 0.052 Uiso 1 1 calc R . . C50 C 0.4364(3) 0.3361(11) 0.5078(7) 0.062(4) Uani 1 1 d . . . H50 H 0.4382 0.3503 0.4567 0.075 Uiso 1 1 calc R . . C51 C 0.3565(3) 0.3273(11) 0.6503(7) 0.044(3) Uani 1 1 d . . . C52 C 0.3518(3) 0.3314(10) 0.7286(8) 0.055(4) Uani 1 1 d . . . H52 H 0.3743 0.3280 0.7581 0.065 Uiso 1 1 calc R . . C53 C 0.3158(3) 0.3402(11) 0.7637(7) 0.052(4) Uani 1 1 d . . . H53 H 0.3144 0.3478 0.8154 0.062 Uiso 1 1 calc R . . C54 C 0.2808(3) 0.3375(11) 0.7207(8) 0.056(4) Uani 1 1 d . . . C55 C 0.2851(3) 0.3261(14) 0.6470(9) 0.082(5) Uani 1 1 d . . . H55 H 0.2626 0.3202 0.6176 0.099 Uiso 1 1 calc R . . C56 C 0.3217(3) 0.3227(13) 0.6122(7) 0.074(4) Uani 1 1 d . . . H56 H 0.3225 0.3171 0.5604 0.088 Uiso 1 1 calc R . . C57 C 0.2427(3) 0.3553(11) 0.7628(6) 0.059(4) Uani 1 1 d . . . H57A H 0.2439 0.3048 0.8088 0.071 Uiso 1 1 calc R . . H57B H 0.2398 0.4479 0.7760 0.071 Uiso 1 1 calc R . . C58 C 0.1856(4) 0.3870(12) 0.6679(7) 0.071(4) Uani 1 1 d . . . H58 H 0.1894 0.4747 0.6538 0.085 Uiso 1 1 calc R . . C59 C 0.1584(3) 0.3039(14) 0.6435(8) 0.067(4) Uani 1 1 d . . . H59 H 0.1386 0.3279 0.6103 0.080 Uiso 1 1 calc R . . C60 C 0.1931(3) 0.1908(12) 0.7160(7) 0.047(3) Uani 1 1 d . . . H60 H 0.2038 0.1193 0.7418 0.056 Uiso 1 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 Mn 0.0305(5) 0.0602(7) 0.0477(7) 0.0027(11) -0.0023(7) 0.0046(9) Cl1 0.181(5) 0.064(3) 0.078(3) 0.008(3) 0.012(3) -0.013(3) Cl2 0.108(3) 0.070(3) 0.075(3) 0.005(3) -0.009(3) 0.013(3) O1 0.152(8) 0.099(8) 0.068(7) -0.003(7) 0.003(7) -0.013(7) O2 0.158(12) 0.35(3) 0.36(3) 0.00(2) 0.020(19) -0.009(17) O3 0.250(14) 0.036(6) 0.163(12) -0.005(8) 0.008(11) -0.030(8) O4 0.288(16) 0.099(8) 0.062(7) 0.027(7) -0.016(9) 0.015(9) O5 0.114(8) 0.119(9) 0.177(11) 0.008(9) 0.001(8) 0.023(8) O6 0.284(13) 0.080(7) 0.047(6) -0.012(7) -0.001(8) -0.011(10) O7 0.167(11) 0.145(11) 0.116(10) 0.052(9) -0.035(9) 0.039(9) O8 0.172(11) 0.055(7) 0.149(11) -0.017(8) 0.022(10) -0.023(7) O9W 0.311(14) 0.47(2) 0.195(13) -0.228(15) -0.215(12) 0.297(16) O10W 0.219(12) 0.75(4) 0.121(11) 0.024(18) 0.087(10) 0.18(2) N1 0.030(5) 0.055(7) 0.053(7) -0.008(6) -0.001(5) 0.000(5) N2 0.030(5) 0.060(7) 0.068(8) -0.005(6) -0.010(6) 0.009(5) N3 0.047(7) 0.057(7) 0.059(8) -0.006(6) 0.007(6) -0.005(6) N4 0.044(6) 0.070(9) 0.041(7) -0.005(6) -0.006(6) -0.019(6) N5 0.031(6) 0.093(9) 0.035(6) -0.001(7) -0.007(5) -0.006(6) N6 0.056(6) 0.040(6) 0.064(7) -0.007(6) -0.004(6) -0.012(6) N7 0.029(5) 0.056(7) 0.029(5) -0.007(6) 0.002(4) 0.002(5) N8 0.033(6) 0.052(7) 0.060(7) -0.012(6) 0.001(6) -0.005(6) N9 0.029(5) 0.062(8) 0.044(6) -0.006(6) -0.003(5) 0.004(5) N10 0.032(6) 0.076(8) 0.065(8) 0.024(7) 0.004(5) 0.018(6) N11 0.064(7) 0.058(8) 0.060(7) -0.007(6) -0.012(6) -0.024(6) N12 0.050(6) 0.051(7) 0.081(9) 0.014(7) -0.010(6) -0.010(6) C1 0.047(8) 0.092(11) 0.054(9) -0.026(9) 0.004(7) 0.006(8) C2 0.053(8) 0.072(10) 0.061(10) -0.033(8) -0.005(8) 0.004(8) C3 0.042(6) 0.056(8) 0.061(8) -0.020(8) -0.017(8) -0.005(6) C4 0.071(8) 0.039(7) 0.073(10) 0.020(8) 0.000(8) -0.004(7) C5 0.064(8) 0.049(8) 0.041(8) -0.003(7) 0.010(7) -0.005(8) C6 0.067(9) 0.053(8) 0.065(9) -0.007(8) -0.003(8) -0.018(8) C7 0.055(8) 0.041(8) 0.080(10) -0.003(7) -0.010(7) 0.006(7) C8 0.022(6) 0.054(8) 0.056(8) -0.009(7) 0.010(6) -0.007(6) C9 0.050(8) 0.041(8) 0.114(11) -0.008(8) -0.026(8) -0.007(7) C10 0.063(8) 0.035(8) 0.109(12) -0.010(8) -0.027(9) -0.023(7) C11 0.046(8) 0.048(9) 0.043(8) -0.008(7) -0.001(7) 0.012(7) C12 0.042(8) 0.052(9) 0.079(10) -0.004(8) -0.022(7) 0.001(7) C13 0.086(10) 0.047(8) 0.041(8) 0.009(7) 0.016(7) 0.018(8) C14 0.049(8) 0.035(7) 0.043(8) 0.018(6) 0.000(7) -0.002(6) C15 0.036(7) 0.061(9) 0.086(10) 0.001(8) -0.011(7) -0.003(7) C16 0.047(8) 0.058(10) 0.129(14) -0.032(10) 0.018(9) -0.002(8) C17 0.059(7) 0.053(7) 0.035(7) 0.008(6) 0.015(6) -0.009(6) C18 0.066(9) 0.091(11) 0.052(9) -0.024(8) -0.005(7) -0.011(8) C19 0.046(7) 0.070(9) 0.056(8) -0.009(8) -0.005(7) -0.022(7) C20 0.037(7) 0.063(9) 0.033(8) -0.019(7) 0.002(6) 0.002(7) C21 0.034(7) 0.081(10) 0.063(10) 0.014(9) 0.015(7) -0.017(7) C22 0.055(8) 0.086(11) 0.040(8) -0.021(8) -0.014(7) 0.029(8) C23 0.060(8) 0.044(7) 0.056(8) 0.003(7) 0.020(8) -0.001(7) C24 0.050(7) 0.081(10) 0.089(11) -0.002(9) -0.009(8) -0.027(7) C25 0.032(7) 0.041(8) 0.119(13) 0.009(9) -0.017(8) -0.007(7) C26 0.052(8) 0.052(9) 0.065(9) -0.001(7) -0.016(7) -0.004(7) C27 0.059(9) 0.041(7) 0.065(9) -0.009(7) -0.006(7) -0.014(7) C28 0.050(8) 0.055(9) 0.088(11) -0.039(8) -0.012(7) 0.013(7) C29 0.053(8) 0.076(12) 0.30(3) -0.069(15) -0.083(12) 0.009(9) C30 0.077(11) 0.051(10) 0.30(3) -0.001(15) -0.071(15) 0.002(9) C31 0.031(7) 0.046(8) 0.084(10) -0.013(8) 0.007(7) -0.017(7) C32 0.041(9) 0.046(9) 0.23(2) -0.020(12) -0.023(11) 0.005(8) C33 0.048(9) 0.043(8) 0.195(17) -0.017(11) -0.020(11) -0.011(7) C34 0.050(7) 0.044(8) 0.053(9) 0.002(8) 0.016(6) 0.000(7) C35 0.056(8) 0.063(9) 0.104(12) 0.008(9) 0.014(9) -0.015(8) C36 0.040(7) 0.054(8) 0.100(11) 0.014(8) -0.016(7) 0.008(7) C37 0.051(7) 0.066(8) 0.069(9) 0.006(7) 0.023(7) -0.003(6) C38 0.061(9) 0.105(13) 0.046(9) -0.034(9) 0.004(7) 0.005(9) C39 0.072(9) 0.064(9) 0.060(9) -0.022(8) 0.007(8) -0.009(8) C40 0.038(7) 0.054(9) 0.067(10) -0.002(8) -0.003(7) -0.002(7) C41 0.068(9) 0.068(10) 0.098(12) 0.000(9) -0.010(8) 0.002(8) C42 0.068(9) 0.079(11) 0.081(11) 0.021(9) -0.016(8) 0.017(9) C43 0.051(8) 0.078(11) 0.077(11) 0.013(9) 0.015(8) 0.033(8) C44 0.054(8) 0.124(12) 0.075(9) 0.055(9) 0.002(7) 0.017(8) C45 0.046(7) 0.056(8) 0.060(9) -0.004(7) -0.010(7) 0.023(7) C46 0.076(10) 0.117(13) 0.043(9) 0.037(9) -0.008(8) 0.013(10) C47 0.042(6) 0.119(10) 0.028(7) -0.018(8) -0.003(6) 0.009(7) C48 0.051(7) 0.051(8) 0.031(7) -0.002(7) -0.011(6) 0.003(7) C49 0.039(6) 0.025(6) 0.065(9) 0.022(6) -0.014(6) -0.002(5) C50 0.056(8) 0.071(9) 0.061(9) -0.005(8) -0.005(7) 0.001(8) C51 0.042(6) 0.045(7) 0.043(7) -0.001(7) -0.014(7) -0.001(5) C52 0.040(7) 0.032(7) 0.091(11) 0.004(8) -0.009(8) -0.006(6) C53 0.053(8) 0.052(9) 0.051(8) -0.002(7) 0.005(7) -0.012(7) C54 0.034(7) 0.040(8) 0.094(11) 0.007(8) -0.007(8) -0.011(6) C55 0.038(7) 0.143(14) 0.066(9) -0.020(11) -0.008(8) -0.008(8) C56 0.049(7) 0.117(12) 0.055(8) -0.017(9) -0.005(7) 0.006(8) C57 0.047(7) 0.081(9) 0.050(8) -0.011(7) -0.020(6) -0.025(7) C58 0.070(8) 0.050(8) 0.094(12) 0.010(8) -0.033(8) -0.012(7) C59 0.034(6) 0.088(10) 0.078(10) 0.008(10) -0.006(8) -0.006(7) C60 0.035(7) 0.047(8) 0.059(9) 0.028(7) -0.009(7) 0.005(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 Mn N8 2.206(11) 3 ? Mn N9 2.238(10) . ? Mn N5 2.243(10) . ? Mn N12 2.252(10) 3 ? Mn N1 2.262(10) . ? Mn N4 2.301(11) 3_455 ? Cl1 O4 1.340(10) . ? Cl1 O3 1.384(9) . ? Cl1 O1 1.407(10) . ? Cl1 O2 1.480(15) . ? Cl2 O5 1.383(12) . ? Cl2 O7 1.400(10) . ? Cl2 O8 1.408(9) . ? Cl2 O6 1.412(10) . ? N1 C3 1.290(13) . ? N1 C1 1.391(14) . ? N2 C3 1.319(11) . ? N2 C2 1.364(13) . ? N2 C4 1.507(12) . ? N3 C20 1.312(13) . ? N3 C18 1.404(15) . ? N3 C17 1.477(12) . ? N4 C20 1.297(13) . ? N4 C19 1.336(14) . ? N4 Mn 2.301(11) 3 ? N5 C23 1.317(12) . ? N5 C21 1.326(14) . ? N6 C22 1.356(13) . ? N6 C23 1.362(13) . ? N6 C24 1.506(12) . ? N7 C38 1.335(14) . ? N7 C40 1.348(13) . ? N7 C37 1.435(11) . ? N8 C40 1.320(13) . ? N8 C39 1.399(13) . ? N8 Mn 2.206(11) 3_455 ? N9 C41 1.386(13) . ? N9 C43 1.388(14) . ? N10 C43 1.336(15) . ? N10 C42 1.378(14) . ? N10 C44 1.502(13) . ? N11 C60 1.332(13) . ? N11 C58 1.411(14) . ? N11 C57 1.476(12) . ? N12 C60 1.317(13) . ? N12 C59 1.347(14) . ? N12 Mn 2.252(10) 3_455 ? C1 C2 1.359(14) . ? C4 C5 1.498(14) . ? C5 C10 1.328(14) . ? C5 C6 1.389(14) . ? C6 C7 1.387(15) . ? C7 C8 1.358(14) . ? C8 C9 1.356(14) . ? C8 C11 1.508(14) . ? C9 C10 1.381(13) . ? C11 C12 1.342(17) . ? C11 C16 1.400(14) . ? C12 C13 1.411(14) . ? C13 C14 1.350(13) . ? C14 C15 1.382(14) . ? C14 C17 1.499(13) . ? C15 C16 1.346(14) . ? C18 C19 1.353(14) . ? C21 C22 1.376(15) . ? C24 C25 1.570(14) . ? C25 C30 1.310(17) . ? C25 C26 1.329(14) . ? C26 C27 1.362(14) . ? C27 C28 1.395(14) . ? C28 C29 1.365(16) . ? C28 C31 1.446(14) . ? C29 C30 1.400(17) . ? C31 C36 1.369(14) . ? C31 C32 1.408(18) . ? C32 C33 1.344(15) . ? C33 C34 1.428(14) . ? C34 C35 1.424(13) . ? C34 C37 1.534(13) . ? C35 C36 1.365(14) . ? C38 C39 1.383(15) . ? C41 C42 1.397(14) . ? C44 C45 1.514(14) . ? C45 C46 1.373(14) . ? C45 C50 1.385(13) . ? C46 C47 1.411(15) . ? C47 C48 1.367(13) . ? C48 C49 1.369(14) . ? C48 C51 1.464(11) . ? C49 C50 1.397(14) . ? C51 C56 1.364(13) . ? C51 C52 1.412(15) . ? C52 C53 1.377(13) . ? C53 C54 1.416(15) . ? C54 C55 1.332(17) . ? C54 C57 1.506(14) . ? C55 C56 1.389(14) . ? C58 C59 1.322(14) . ? 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 N8 Mn N9 89.1(3) 3 . ? N8 Mn N5 93.8(4) 3 . ? N9 Mn N5 89.5(4) . . ? N8 Mn N12 90.0(4) 3 3 ? N9 Mn N12 177.1(5) . 3 ? N5 Mn N12 87.9(4) . 3 ? N8 Mn N1 88.5(4) 3 . ? N9 Mn N1 93.1(4) . . ? N5 Mn N1 176.6(5) . . ? N12 Mn N1 89.6(4) 3 . ? N8 Mn N4 176.4(4) 3 3_455 ? N9 Mn N4 88.5(3) . 3_455 ? N5 Mn N4 88.8(4) . 3_455 ? N12 Mn N4 92.6(4) 3 3_455 ? N1 Mn N4 89.0(4) . 3_455 ? O4 Cl1 O3 113.5(9) . . ? O4 Cl1 O1 116.5(7) . . ? O3 Cl1 O1 113.5(8) . . ? O4 Cl1 O2 103.9(12) . . ? O3 Cl1 O2 103.3(10) . . ? O1 Cl1 O2 104.1(12) . . ? O5 Cl2 O7 108.9(8) . . ? O5 Cl2 O8 109.2(7) . . ? O7 Cl2 O8 114.2(8) . . ? O5 Cl2 O6 106.5(9) . . ? O7 Cl2 O6 107.7(7) . . ? O8 Cl2 O6 110.2(8) . . ? C3 N1 C1 102.4(10) . . ? C3 N1 Mn 127.8(9) . . ? C1 N1 Mn 129.4(9) . . ? C3 N2 C2 106.2(10) . . ? C3 N2 C4 128.4(11) . . ? C2 N2 C4 125.4(11) . . ? C20 N3 C18 104.0(10) . . ? C20 N3 C17 129.5(11) . . ? C18 N3 C17 125.4(11) . . ? C20 N4 C19 105.9(10) . . ? C20 N4 Mn 126.1(9) . 3 ? C19 N4 Mn 126.3(9) . 3 ? C23 N5 C21 105.2(10) . . ? C23 N5 Mn 127.1(9) . . ? C21 N5 Mn 127.3(8) . . ? C22 N6 C23 109.6(10) . . ? C22 N6 C24 127.6(12) . . ? C23 N6 C24 122.6(11) . . ? C38 N7 C40 107.9(10) . . ? C38 N7 C37 125.7(11) . . ? C40 N7 C37 126.1(10) . . ? C40 N8 C39 103.8(10) . . ? C40 N8 Mn 129.0(9) . 3_455 ? C39 N8 Mn 124.9(8) . 3_455 ? C41 N9 C43 105.7(11) . . ? C41 N9 Mn 129.7(8) . . ? C43 N9 Mn 123.9(9) . . ? C43 N10 C42 111.9(11) . . ? C43 N10 C44 121.9(13) . . ? C42 N10 C44 126.1(12) . . ? C60 N11 C58 105.0(10) . . ? C60 N11 C57 126.5(11) . . ? C58 N11 C57 128.1(11) . . ? C60 N12 C59 103.6(10) . . ? C60 N12 Mn 128.4(9) . 3_455 ? C59 N12 Mn 127.9(9) . 3_455 ? C2 C1 N1 110.6(12) . . ? C1 C2 N2 105.2(11) . . ? N1 C3 N2 115.5(12) . . ? C5 C4 N2 112.7(9) . . ? C10 C5 C6 114.3(13) . . ? C10 C5 C4 121.9(12) . . ? C6 C5 C4 123.8(12) . . ? C7 C6 C5 121.4(13) . . ? C8 C7 C6 121.0(12) . . ? C9 C8 C7 118.8(12) . . ? C9 C8 C11 121.4(12) . . ? C7 C8 C11 119.8(12) . . ? C8 C9 C10 118.1(12) . . ? C5 C10 C9 126.3(12) . . ? C12 C11 C16 118.4(12) . . ? C12 C11 C8 121.9(12) . . ? C16 C11 C8 119.6(12) . . ? C11 C12 C13 118.9(12) . . ? C14 C13 C12 122.7(12) . . ? C13 C14 C15 117.2(12) . . ? C13 C14 C17 120.3(11) . . ? C15 C14 C17 122.3(11) . . ? C16 C15 C14 120.9(12) . . ? C15 C16 C11 121.7(13) . . ? N3 C17 C14 113.0(9) . . ? C19 C18 N3 106.3(11) . . ? N4 C19 C18 109.4(11) . . ? N4 C20 N3 114.4(11) . . ? N5 C21 C22 113.5(11) . . ? N6 C22 C21 102.0(11) . . ? N5 C23 N6 109.6(11) . . ? N6 C24 C25 110.9(10) . . ? C30 C25 C26 121.3(13) . . ? C30 C25 C24 116.9(12) . . ? C26 C25 C24 121.7(12) . . ? C25 C26 C27 120.4(12) . . ? C26 C27 C28 122.2(12) . . ? C29 C28 C27 114.2(13) . . ? C29 C28 C31 121.7(12) . . ? C27 C28 C31 123.6(12) . . ? C28 C29 C30 122.7(14) . . ? C25 C30 C29 119.1(15) . . ? C36 C31 C32 111.5(12) . . ? C36 C31 C28 123.4(12) . . ? C32 C31 C28 125.1(12) . . ? C33 C32 C31 127.5(13) . . ? C32 C33 C34 117.8(13) . . ? C35 C34 C33 117.6(13) . . ? C35 C34 C37 121.2(11) . . ? C33 C34 C37 121.2(11) . . ? C36 C35 C34 118.4(12) . . ? C35 C36 C31 127.1(13) . . ? N7 C37 C34 112.8(9) . . ? N7 C38 C39 106.4(12) . . ? C38 C39 N8 109.2(12) . . ? N8 C40 N7 112.7(11) . . ? N9 C41 C42 110.3(12) . . ? N10 C42 C41 103.7(11) . . ? N10 C43 N9 108.2(13) . . ? N10 C44 C45 110.4(10) . . ? C46 C45 C50 116.3(12) . . ? C46 C45 C44 126.4(12) . . ? C50 C45 C44 117.2(11) . . ? C45 C46 C47 120.0(12) . . ? C48 C47 C46 122.8(12) . . ? C47 C48 C49 117.9(11) . . ? C47 C48 C51 122.9(10) . . ? C49 C48 C51 119.1(10) . . ? C48 C49 C50 119.2(11) . . ? C45 C50 C49 123.9(12) . . ? C56 C51 C52 113.7(12) . . ? C56 C51 C48 124.6(11) . . ? C52 C51 C48 121.5(10) . . ? C53 C52 C51 123.7(12) . . ? C52 C53 C54 119.7(12) . . ? C55 C54 C53 116.6(12) . . ? C55 C54 C57 126.9(11) . . ? C53 C54 C57 116.4(12) . . ? C54 C55 C56 123.1(13) . . ? C51 C56 C55 123.1(12) . . ? N11 C57 C54 113.2(9) . . ? C59 C58 N11 104.7(11) . . ? C58 C59 N12 113.1(12) . . ? N12 C60 N11 113.4(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Mn N1 C3 -1.9(10) 3 . . . ? N9 Mn N1 C3 -90.9(10) . . . . ? N5 Mn N1 C3 131(7) . . . . ? N12 Mn N1 C3 88.1(10) 3 . . . ? N4 Mn N1 C3 -179.3(10) 3_455 . . . ? N8 Mn N1 C1 -173.1(11) 3 . . . ? N9 Mn N1 C1 97.8(11) . . . . ? N5 Mn N1 C1 -41(8) . . . . ? N12 Mn N1 C1 -83.2(11) 3 . . . ? N4 Mn N1 C1 9.4(11) 3_455 . . . ? N8 Mn N5 C23 -173.8(10) 3 . . . ? N9 Mn N5 C23 -84.8(10) . . . . ? N12 Mn N5 C23 96.3(10) 3 . . . ? N1 Mn N5 C23 54(8) . . . . ? N4 Mn N5 C23 3.7(10) 3_455 . . . ? N8 Mn N5 C21 -2.0(11) 3 . . . ? N9 Mn N5 C21 87.1(11) . . . . ? N12 Mn N5 C21 -91.8(11) 3 . . . ? N1 Mn N5 C21 -134(7) . . . . ? N4 Mn N5 C21 175.6(11) 3_455 . . . ? N8 Mn N9 C41 -96.9(11) 3 . . . ? N5 Mn N9 C41 169.2(10) . . . . ? N12 Mn N9 C41 -168(8) 3 . . . ? N1 Mn N9 C41 -8.5(11) . . . . ? N4 Mn N9 C41 80.4(11) 3_455 . . . ? N8 Mn N9 C43 71.8(9) 3 . . . ? N5 Mn N9 C43 -22.0(9) . . . . ? N12 Mn N9 C43 1(9) 3 . . . ? N1 Mn N9 C43 160.3(9) . . . . ? N4 Mn N9 C43 -110.8(9) 3_455 . . . ? C3 N1 C1 C2 -1.1(15) . . . . ? Mn N1 C1 C2 171.8(8) . . . . ? N1 C1 C2 N2 -0.4(15) . . . . ? C3 N2 C2 C1 1.8(14) . . . . ? C4 N2 C2 C1 -179.3(10) . . . . ? C1 N1 C3 N2 2.4(14) . . . . ? Mn N1 C3 N2 -170.7(7) . . . . ? C2 N2 C3 N1 -2.8(14) . . . . ? C4 N2 C3 N1 178.3(10) . . . . ? C3 N2 C4 C5 -122.1(12) . . . . ? C2 N2 C4 C5 59.2(15) . . . . ? N2 C4 C5 C10 -128.3(13) . . . . ? N2 C4 C5 C6 50.3(16) . . . . ? C10 C5 C6 C7 -4.5(19) . . . . ? C4 C5 C6 C7 176.8(11) . . . . ? C5 C6 C7 C8 3(2) . . . . ? C6 C7 C8 C9 -0.1(19) . . . . ? C6 C7 C8 C11 179.5(11) . . . . ? C7 C8 C9 C10 -0.9(19) . . . . ? C11 C8 C9 C10 179.5(11) . . . . ? C6 C5 C10 C9 4(2) . . . . ? C4 C5 C10 C9 -177.5(12) . . . . ? C8 C9 C10 C5 -1(2) . . . . ? C9 C8 C11 C12 162.4(12) . . . . ? C7 C8 C11 C12 -17.2(18) . . . . ? C9 C8 C11 C16 -20.3(19) . . . . ? C7 C8 C11 C16 160.2(12) . . . . ? C16 C11 C12 C13 -0.4(19) . . . . ? C8 C11 C12 C13 177.0(11) . . . . ? C11 C12 C13 C14 -3(2) . . . . ? C12 C13 C14 C15 5(2) . . . . ? C12 C13 C14 C17 -179.8(11) . . . . ? C13 C14 C15 C16 -4(2) . . . . ? C17 C14 C15 C16 -179.0(12) . . . . ? C14 C15 C16 C11 1(2) . . . . ? C12 C11 C16 C15 1(2) . . . . ? C8 C11 C16 C15 -176.1(12) . . . . ? C20 N3 C17 C14 -76.4(15) . . . . ? C18 N3 C17 C14 89.3(14) . . . . ? C13 C14 C17 N3 143.6(12) . . . . ? C15 C14 C17 N3 -42.0(16) . . . . ? C20 N3 C18 C19 -2.1(13) . . . . ? C17 N3 C18 C19 -170.8(10) . . . . ? C20 N4 C19 C18 1.4(14) . . . . ? Mn N4 C19 C18 166.9(8) 3 . . . ? N3 C18 C19 N4 0.5(15) . . . . ? C19 N4 C20 N3 -2.9(14) . . . . ? Mn N4 C20 N3 -168.5(8) 3 . . . ? C18 N3 C20 N4 3.2(14) . . . . ? C17 N3 C20 N4 171.2(10) . . . . ? C23 N5 C21 C22 -1.1(15) . . . . ? Mn N5 C21 C22 -174.4(8) . . . . ? C23 N6 C22 C21 2.0(13) . . . . ? C24 N6 C22 C21 177.4(11) . . . . ? N5 C21 C22 N6 -0.5(15) . . . . ? C21 N5 C23 N6 2.4(13) . . . . ? Mn N5 C23 N6 175.6(7) . . . . ? C22 N6 C23 N5 -2.8(14) . . . . ? C24 N6 C23 N5 -178.6(10) . . . . ? C22 N6 C24 C25 -61.1(17) . . . . ? C23 N6 C24 C25 113.8(12) . . . . ? N6 C24 C25 C30 122.0(15) . . . . ? N6 C24 C25 C26 -62.3(18) . . . . ? C30 C25 C26 C27 -2(2) . . . . ? C24 C25 C26 C27 -177.2(11) . . . . ? C25 C26 C27 C28 1(2) . . . . ? C26 C27 C28 C29 2(2) . . . . ? C26 C27 C28 C31 174.6(12) . . . . ? C27 C28 C29 C30 -4(3) . . . . ? C31 C28 C29 C30 -177.1(16) . . . . ? C26 C25 C30 C29 -1(3) . . . . ? C24 C25 C30 C29 175.1(16) . . . . ? C28 C29 C30 C25 4(3) . . . . ? C29 C28 C31 C36 13(2) . . . . ? C27 C28 C31 C36 -158.8(13) . . . . ? C29 C28 C31 C32 -166.9(17) . . . . ? C27 C28 C31 C32 21(2) . . . . ? C36 C31 C32 C33 1(3) . . . . ? C28 C31 C32 C33 -178.6(17) . . . . ? C31 C32 C33 C34 -4(3) . . . . ? C32 C33 C34 C35 5(2) . . . . ? C32 C33 C34 C37 -177.0(15) . . . . ? C33 C34 C35 C36 -5(2) . . . . ? C37 C34 C35 C36 177.1(11) . . . . ? C34 C35 C36 C31 3(2) . . . . ? C32 C31 C36 C35 -1(2) . . . . ? C28 C31 C36 C35 178.8(13) . . . . ? C38 N7 C37 C34 -88.9(15) . . . . ? C40 N7 C37 C34 84.6(13) . . . . ? C35 C34 C37 N7 48.7(16) . . . . ? C33 C34 C37 N7 -129.0(13) . . . . ? C40 N7 C38 C39 0.6(14) . . . . ? C37 N7 C38 C39 175.0(10) . . . . ? N7 C38 C39 N8 -1.2(15) . . . . ? C40 N8 C39 C38 1.3(14) . . . . ? Mn N8 C39 C38 -162.7(8) 3_455 . . . ? C39 N8 C40 N7 -1.0(13) . . . . ? Mn N8 C40 N7 162.1(7) 3_455 . . . ? C38 N7 C40 N8 0.3(13) . . . . ? C37 N7 C40 N8 -174.1(10) . . . . ? C43 N9 C41 C42 4.3(15) . . . . ? Mn N9 C41 C42 174.6(8) . . . . ? C43 N10 C42 C41 -0.5(14) . . . . ? C44 N10 C42 C41 -177.3(10) . . . . ? N9 C41 C42 N10 -2.4(15) . . . . ? C42 N10 C43 N9 3.2(14) . . . . ? C44 N10 C43 N9 -179.8(9) . . . . ? C41 N9 C43 N10 -4.5(14) . . . . ? Mn N9 C43 N10 -175.5(7) . . . . ? C43 N10 C44 C45 91.2(15) . . . . ? C42 N10 C44 C45 -92.3(14) . . . . ? N10 C44 C45 C46 5(2) . . . . ? N10 C44 C45 C50 179.8(12) . . . . ? C50 C45 C46 C47 0(2) . . . . ? C44 C45 C46 C47 175.7(12) . . . . ? C45 C46 C47 C48 2(2) . . . . ? C46 C47 C48 C49 -3.3(19) . . . . ? C46 C47 C48 C51 -178.7(12) . . . . ? C47 C48 C49 C50 2.6(17) . . . . ? C51 C48 C49 C50 178.2(10) . . . . ? C46 C45 C50 C49 -1(2) . . . . ? C44 C45 C50 C49 -176.7(11) . . . . ? C48 C49 C50 C45 -0.5(18) . . . . ? C47 C48 C51 C56 -167.5(10) . . . . ? C49 C48 C51 C56 17(2) . . . . ? C47 C48 C51 C52 8(2) . . . . ? C49 C48 C51 C52 -167.6(9) . . . . ? C56 C51 C52 C53 -4.7(18) . . . . ? C48 C51 C52 C53 179.6(11) . . . . ? C51 C52 C53 C54 3.8(18) . . . . ? C52 C53 C54 C55 0.1(18) . . . . ? C52 C53 C54 C57 -176.7(10) . . . . ? C53 C54 C55 C56 -3(2) . . . . ? C57 C54 C55 C56 173.6(12) . . . . ? C52 C51 C56 C55 2.0(19) . . . . ? C48 C51 C56 C55 177.5(13) . . . . ? C54 C55 C56 C51 2(2) . . . . ? C60 N11 C57 C54 85.9(15) . . . . ? C58 N11 C57 C54 -85.7(15) . . . . ? C55 C54 C57 N11 20.6(18) . . . . ? C53 C54 C57 N11 -163.0(11) . . . . ? C60 N11 C58 C59 5.0(14) . . . . ? C57 N11 C58 C59 178.1(11) . . . . ? N11 C58 C59 N12 -3.5(16) . . . . ? C60 N12 C59 C58 0.5(16) . . . . ? Mn N12 C59 C58 -176.4(9) 3_455 . . . ? C59 N12 C60 N11 3.0(15) . . . . ? Mn N12 C60 N11 179.9(8) 3_455 . . . ? C58 N11 C60 N12 -5.2(15) . . . . ? C57 N11 C60 N12 -178.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.263 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.044 #===END data_bimb.2HClO4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cl N2 O4' _chemical_formula_weight 257.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.8950(10) _cell_length_b 15.164(2) _cell_length_c 14.904(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.210(10) _cell_angle_gamma 90.00 _cell_volume 1097.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 288(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 15.05 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.353 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8688 _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 288(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.03 _diffrn_reflns_number 2341 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1928 _reflns_number_gt 1162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1574P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1928 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2494 _refine_ls_wR_factor_gt 0.2276 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl 0.4160(3) 0.62473(10) 0.62495(10) 0.0664(6) Uani 1 1 d . . . N1 N -0.1209(8) 0.8014(2) 0.8571(3) 0.0400(9) Uani 1 1 d . . . N2 N 0.0321(12) 0.9323(3) 0.8505(3) 0.0616(14) Uani 1 1 d . . . C1 C -0.1137(12) 0.8791(3) 0.8949(4) 0.0528(13) Uani 1 1 d . . . H1 H -0.1982 0.8943 0.9453 0.063 Uiso 1 1 calc R . . C2 C 0.1235(13) 0.8885(4) 0.7827(4) 0.0615(15) Uani 1 1 d . . . H2 H 0.2318 0.9109 0.7410 0.074 Uiso 1 1 calc R . . C3 C 0.0295(12) 0.8063(4) 0.7860(4) 0.0587(15) Uani 1 1 d . . . H3 H 0.0606 0.7605 0.7471 0.070 Uiso 1 1 calc R . . C4 C -0.2472(10) 0.7211(3) 0.8895(4) 0.0535(13) Uani 1 1 d . . . H4A H -0.3723 0.6956 0.8407 0.064 Uiso 1 1 calc R . . H4B H -0.3522 0.7360 0.9383 0.064 Uiso 1 1 calc R . . C5 C -0.0258(10) 0.6544(3) 0.9225(3) 0.0425(11) Uani 1 1 d . . . C6 C 0.0442(12) 0.5882(4) 0.8673(4) 0.0651(16) Uani 1 1 d . . . H6 H -0.0453 0.5837 0.8087 0.078 Uiso 1 1 calc R . . C7 C 0.2484(12) 0.5276(4) 0.8982(4) 0.0609(15) Uani 1 1 d . . . H7 H 0.2895 0.4824 0.8599 0.073 Uiso 1 1 calc R . . C8 C 0.3907(9) 0.5326(3) 0.9836(3) 0.0385(11) Uani 1 1 d . . . C9 C 0.3247(12) 0.6017(3) 1.0374(3) 0.0562(14) Uani 1 1 d . . . H9 H 0.4222 0.6087 1.0946 0.067 Uiso 1 1 calc R . . C10 C 0.1160(11) 0.6611(3) 1.0079(3) 0.0553(14) Uani 1 1 d . . . H10 H 0.0720 0.7058 1.0464 0.066 Uiso 1 1 calc R . . O1 O 0.1189(8) 0.6199(3) 0.6212(4) 0.0932(16) Uani 1 1 d . . . O2 O 0.4922(11) 0.7063(3) 0.6618(4) 0.1065(18) Uani 1 1 d . . . O3 O 0.5232(10) 0.5573(3) 0.6821(4) 0.1022(17) Uani 1 1 d . . . O4 O 0.4681(14) 0.6172(6) 0.5387(4) 0.151(3) Uani 1 1 d . . . H0N H 0.045(11) 0.979(4) 0.856(4) 0.048(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl 0.0795(11) 0.0619(10) 0.0583(9) -0.0016(7) 0.0110(7) 0.0057(7) N1 0.043(2) 0.034(2) 0.043(2) 0.0070(17) 0.0070(17) 0.0046(17) N2 0.091(4) 0.034(3) 0.061(3) 0.002(2) 0.012(3) -0.006(3) C1 0.068(4) 0.043(3) 0.049(3) 0.001(2) 0.015(2) 0.001(3) C2 0.074(4) 0.054(3) 0.062(3) 0.018(3) 0.030(3) 0.004(3) C3 0.076(4) 0.049(3) 0.056(3) -0.003(2) 0.026(3) 0.002(3) C4 0.045(3) 0.049(3) 0.068(3) 0.011(2) 0.009(2) -0.002(2) C5 0.042(3) 0.033(2) 0.053(3) 0.009(2) 0.009(2) -0.009(2) C6 0.080(4) 0.049(3) 0.058(3) -0.010(3) -0.021(3) 0.009(3) C7 0.072(4) 0.044(3) 0.061(3) -0.018(2) -0.014(3) 0.010(3) C8 0.044(3) 0.032(2) 0.041(2) 0.0050(18) 0.011(2) -0.0075(19) C9 0.073(4) 0.057(3) 0.038(3) 0.003(2) 0.005(2) 0.013(3) C10 0.071(4) 0.048(3) 0.049(3) -0.003(2) 0.015(3) 0.013(3) O1 0.041(2) 0.102(4) 0.139(4) 0.035(3) 0.018(2) 0.008(2) O2 0.113(4) 0.064(3) 0.135(5) -0.019(3) -0.012(4) -0.001(3) O3 0.086(3) 0.078(3) 0.137(5) 0.034(3) -0.008(3) 0.020(3) O4 0.122(5) 0.274(9) 0.060(3) -0.041(4) 0.027(3) 0.005(5) _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 Cl O4 1.347(5) . ? Cl O2 1.385(5) . ? Cl O3 1.390(5) . ? Cl O1 1.450(5) . ? N1 C1 1.304(6) . ? N1 C3 1.366(6) . ? N1 C4 1.474(6) . ? N2 C1 1.311(7) . ? N2 C2 1.333(7) . ? C2 C3 1.331(8) . ? C4 C5 1.518(7) . ? C5 C6 1.368(7) . ? C5 C10 1.375(7) . ? C6 C7 1.393(7) . ? C7 C8 1.374(7) . ? C8 C9 1.383(7) . ? C8 C8 1.494(9) 3_667 ? C9 C10 1.390(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 O4 Cl O2 112.4(5) . . ? O4 Cl O3 114.9(5) . . ? O2 Cl O3 110.5(4) . . ? O4 Cl O1 105.5(4) . . ? O2 Cl O1 106.2(3) . . ? O3 Cl O1 106.7(3) . . ? C1 N1 C3 107.3(4) . . ? C1 N1 C4 126.5(4) . . ? C3 N1 C4 126.0(4) . . ? C1 N2 C2 109.4(5) . . ? N1 C1 N2 108.9(5) . . ? C3 C2 N2 106.7(5) . . ? C2 C3 N1 107.6(5) . . ? N1 C4 C5 110.2(4) . . ? C6 C5 C10 118.4(5) . . ? C6 C5 C4 121.0(5) . . ? C10 C5 C4 120.5(5) . . ? C5 C6 C7 120.6(5) . . ? C8 C7 C6 121.9(5) . . ? C7 C8 C9 116.8(4) . . ? C7 C8 C8 121.8(5) . 3_667 ? C9 C8 C8 121.4(5) . 3_667 ? C8 C9 C10 121.6(5) . . ? C5 C10 C9 120.6(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 C3 N1 C1 N2 0.5(6) . . . . ? C4 N1 C1 N2 175.6(5) . . . . ? C2 N2 C1 N1 -0.4(7) . . . . ? C1 N2 C2 C3 0.2(7) . . . . ? N2 C2 C3 N1 0.1(7) . . . . ? C1 N1 C3 C2 -0.4(7) . . . . ? C4 N1 C3 C2 -175.6(5) . . . . ? C1 N1 C4 C5 -111.5(6) . . . . ? C3 N1 C4 C5 62.8(7) . . . . ? N1 C4 C5 C6 -96.0(6) . . . . ? N1 C4 C5 C10 81.6(6) . . . . ? C10 C5 C6 C7 2.0(9) . . . . ? C4 C5 C6 C7 179.7(5) . . . . ? C5 C6 C7 C8 -1.4(9) . . . . ? C6 C7 C8 C9 -0.9(8) . . . . ? C6 C7 C8 C8 179.9(6) . . . 3_667 ? C7 C8 C9 C10 2.7(8) . . . . ? C8 C8 C9 C10 -178.2(5) 3_667 . . . ? C6 C5 C10 C9 -0.3(8) . . . . ? C4 C5 C10 C9 -178.0(5) . . . . ? C8 C9 C10 C5 -2.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.918 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.082 #===END