# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1-eb2225 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 C43 H41 Mn2 N9 O3 2+, 4 Cl O4 -, H2 O' _chemical_formula_sum 'C86 H84 Cl4 Mn4 N18 O23' _chemical_formula_weight 2099.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 '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 10.7837(3) _cell_length_b 11.6961(4) _cell_length_c 18.9210(6) _cell_angle_alpha 73.692(3) _cell_angle_beta 80.838(3) _cell_angle_gamma 88.509(3) _cell_volume 2260.79(12) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11341 _cell_measurement_theta_min 3.9354 _cell_measurement_theta_max 73.8253 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1078 _exptl_absorpt_coefficient_mu 6.248 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.4623 _exptl_absorpt_correction_T_max 0.8063 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21d (release 25-05-2012 CrysAlis171 .NET) (compiled May 25 2012,16:20:25) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Agilent Technologies SuperNova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_reflns_number 25644 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 73.99 _reflns_number_total 8930 _reflns_number_gt 7758 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2011)' _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2011)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2011)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and local programs' _refine_special_details ; The asymmetric unit of eb2225 contains one dimanganese (III) complex, two perchlorate counterions and one molecule of water, which was refined as disordered over an inversion centre with occupancy fixed to 0.5 and restrained O--H distances. 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^)+(0.0445P)^2^+1.3099P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary charge-flipping _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8930 _refine_ls_number_parameters 621 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Mn1 Mn 0.31485(3) 0.92514(3) 0.722905(18) 0.02242(8) Uani 1 1 d . . . Mn2 Mn 0.25674(3) 0.65121(3) 0.789149(17) 0.01977(8) Uani 1 1 d . . . O1 O 0.14912(14) 0.51995(13) 0.80193(8) 0.0258(3) Uani 1 1 d . . . O2 O 0.17362(14) 0.87081(13) 0.69168(9) 0.0285(3) Uani 1 1 d . . . O3 O 0.34941(13) 0.78260(13) 0.78163(8) 0.0246(3) Uani 1 1 d . . . N1 N 0.15230(16) 0.74966(15) 0.71479(10) 0.0229(3) Uani 1 1 d . . . N2 N 0.46058(17) 1.01757(16) 0.75295(10) 0.0272(4) Uani 1 1 d . . . N3 N 0.21348(18) 0.98942(16) 0.81852(10) 0.0279(4) Uani 1 1 d . . . N4 N 0.48703(17) 0.91884(15) 0.63963(10) 0.0258(4) Uani 1 1 d . . . N5 N 0.27902(17) 1.09578(15) 0.66254(10) 0.0259(4) Uani 1 1 d . . . N6 N 0.40509(15) 0.53567(15) 0.84202(9) 0.0223(3) Uani 1 1 d . . . N7 N 0.39241(16) 0.60643(15) 0.69330(9) 0.0229(3) Uani 1 1 d . . . N8 N 0.19688(16) 0.62913(15) 0.91002(10) 0.0228(3) Uani 1 1 d . . . O8 O 0.7929(2) 1.36538(16) 0.51888(11) 0.0482(5) Uani 1 1 d . . . N9 N 0.56187(19) 0.30482(18) 0.81760(13) 0.0378(5) Uani 1 1 d . . . C1 C 0.07948(19) 0.49750(18) 0.75592(12) 0.0234(4) Uani 1 1 d . . . C2 C 0.0404(2) 0.3791(2) 0.76635(13) 0.0282(4) Uani 1 1 d . . . H2 H 0.0656 0.3175 0.8057 0.034 Uiso 1 1 calc R . . C3 C -0.0340(2) 0.3513(2) 0.72034(14) 0.0320(5) Uani 1 1 d . . . H3 H -0.0591 0.2707 0.7286 0.038 Uiso 1 1 calc R . . C4 C -0.0728(2) 0.4392(2) 0.66195(14) 0.0337(5) Uani 1 1 d . . . H4 H -0.1232 0.4192 0.6301 0.040 Uiso 1 1 calc R . . C5 C -0.0366(2) 0.5562(2) 0.65125(14) 0.0320(5) Uani 1 1 d . . . H5 H -0.0629 0.6168 0.6117 0.038 Uiso 1 1 calc R . . C6 C 0.03823(19) 0.58740(19) 0.69765(12) 0.0251(4) Uani 1 1 d . . . C7 C 0.0721(2) 0.71200(19) 0.68243(12) 0.0262(4) Uani 1 1 d . . . H7 H 0.0331 0.7690 0.6467 0.031 Uiso 1 1 calc R . . C8 C 0.4284(2) 1.0076(2) 0.83386(13) 0.0326(5) Uani 1 1 d . . . H8A H 0.4799 1.0659 0.8463 0.039 Uiso 1 1 calc R . . H8B H 0.4487 0.9268 0.8631 0.039 Uiso 1 1 calc R . . C9 C 0.2912(2) 1.03011(19) 0.85515(12) 0.0301(5) Uani 1 1 d . . . C10 C 0.2465(3) 1.0824(2) 0.91147(13) 0.0364(5) Uani 1 1 d . . . H10 H 0.3029 1.1109 0.9368 0.044 Uiso 1 1 calc R . . C11 C 0.1184(3) 1.0920(2) 0.92988(15) 0.0440(6) Uani 1 1 d . . . H11 H 0.0854 1.1279 0.9679 0.053 Uiso 1 1 calc R . . C12 C 0.0386(3) 1.0490(2) 0.89258(15) 0.0437(6) Uani 1 1 d . . . H12 H -0.0499 1.0540 0.9051 0.052 Uiso 1 1 calc R . . C13 C 0.0893(2) 0.9988(2) 0.83669(14) 0.0352(5) Uani 1 1 d . . . H13 H 0.0346 0.9701 0.8105 0.042 Uiso 1 1 calc R . . C14 C 0.5811(2) 0.9581(2) 0.73851(13) 0.0295(5) Uani 1 1 d . . . H14A H 0.5852 0.8844 0.7795 0.035 Uiso 1 1 calc R . . H14B H 0.6517 1.0114 0.7373 0.035 Uiso 1 1 calc R . . C15 C 0.5939(2) 0.92770(18) 0.66542(12) 0.0272(4) Uani 1 1 d . . . C16 C 0.7103(2) 0.9052(2) 0.62924(14) 0.0345(5) Uani 1 1 d . . . H16 H 0.7850 0.9131 0.6483 0.041 Uiso 1 1 calc R . . C17 C 0.7149(2) 0.8708(2) 0.56467(15) 0.0385(6) Uani 1 1 d . . . H17 H 0.7932 0.8548 0.5386 0.046 Uiso 1 1 calc R . . C18 C 0.6046(2) 0.8602(2) 0.53844(13) 0.0346(5) Uani 1 1 d . . . H18 H 0.6061 0.8356 0.4945 0.042 Uiso 1 1 calc R . . C19 C 0.4925(2) 0.88551(18) 0.57666(12) 0.0287(5) Uani 1 1 d . . . H19 H 0.4169 0.8793 0.5581 0.034 Uiso 1 1 calc R . . C20 C 0.4674(2) 1.1441(2) 0.70556(13) 0.0316(5) Uani 1 1 d . . . H20A H 0.5424 1.1548 0.6664 0.038 Uiso 1 1 calc R . . H20B H 0.4785 1.1969 0.7369 0.038 Uiso 1 1 calc R . . C21 C 0.3539(2) 1.18183(19) 0.66901(12) 0.0282(5) Uani 1 1 d . . . C22 C 0.3296(2) 1.3017(2) 0.63967(14) 0.0340(5) Uani 1 1 d . . . H22 H 0.3824 1.3614 0.6451 0.041 Uiso 1 1 calc R . . C23 C 0.2282(2) 1.3332(2) 0.60260(14) 0.0360(5) Uani 1 1 d . . . H23 H 0.2106 1.4147 0.5822 0.043 Uiso 1 1 calc R . . C24 C 0.1522(2) 1.2445(2) 0.59542(13) 0.0334(5) Uani 1 1 d . . . H24 H 0.0826 1.2643 0.5695 0.040 Uiso 1 1 calc R . . C25 C 0.1798(2) 1.1271(2) 0.62664(12) 0.0291(5) Uani 1 1 d . . . H25 H 0.1269 1.0662 0.6227 0.035 Uiso 1 1 calc R . . C26 C 0.52298(19) 0.57513(19) 0.78891(12) 0.0250(4) Uani 1 1 d . . . H26A H 0.5919 0.5216 0.8052 0.030 Uiso 1 1 calc R . . H26B H 0.5463 0.6568 0.7882 0.030 Uiso 1 1 calc R . . C27 C 0.50579(19) 0.57347(18) 0.71184(12) 0.0238(4) Uani 1 1 d . . . C28 C 0.6019(2) 0.5428(2) 0.66292(13) 0.0294(5) Uani 1 1 d . . . H28 H 0.6803 0.5176 0.6782 0.035 Uiso 1 1 calc R . . C29 C 0.5816(2) 0.5497(2) 0.59133(13) 0.0316(5) Uani 1 1 d . . . H29 H 0.6460 0.5295 0.5566 0.038 Uiso 1 1 calc R . . C30 C 0.4663(2) 0.58633(19) 0.57125(12) 0.0288(5) Uani 1 1 d . . . H30 H 0.4507 0.5931 0.5222 0.035 Uiso 1 1 calc R . . C31 C 0.3740(2) 0.61295(18) 0.62356(12) 0.0259(4) Uani 1 1 d . . . H31 H 0.2943 0.6368 0.6097 0.031 Uiso 1 1 calc R . . C32 C 0.40987(19) 0.5630(2) 0.91316(12) 0.0272(4) Uani 1 1 d . . . H32A H 0.4578 0.6385 0.9031 0.033 Uiso 1 1 calc R . . H32B H 0.4543 0.4989 0.9453 0.033 Uiso 1 1 calc R . . C33 C 0.27957(19) 0.57454(19) 0.95349(12) 0.0247(4) Uani 1 1 d . . . C34 C 0.2493(2) 0.5370(2) 1.03046(12) 0.0319(5) Uani 1 1 d . . . H34 H 0.3081 0.4947 1.0601 0.038 Uiso 1 1 calc R . . C35 C 0.1317(2) 0.5622(2) 1.06350(13) 0.0341(5) Uani 1 1 d . . . H35 H 0.1089 0.5380 1.1162 0.041 Uiso 1 1 calc R . . C36 C 0.0483(2) 0.6227(2) 1.01897(13) 0.0321(5) Uani 1 1 d . . . H36 H -0.0317 0.6434 1.0406 0.038 Uiso 1 1 calc R . . C37 C 0.0826(2) 0.65294(19) 0.94221(12) 0.0271(4) Uani 1 1 d . . . H37 H 0.0237 0.6916 0.9114 0.033 Uiso 1 1 calc R . . C38 C 0.3759(2) 0.40619(19) 0.85461(13) 0.0269(4) Uani 1 1 d . . . H38A H 0.3512 0.3953 0.8087 0.032 Uiso 1 1 calc R . . H38B H 0.3031 0.3822 0.8950 0.032 Uiso 1 1 calc R . . C39 C 0.4836(2) 0.3248(2) 0.87503(14) 0.0305(5) Uani 1 1 d . . . C40 C 0.5002(3) 0.2752(3) 0.94830(16) 0.0481(7) Uani 1 1 d . . . H40 H 0.4423 0.2893 0.9882 0.058 Uiso 1 1 calc R . . C41 C 0.6035(4) 0.2044(3) 0.9618(2) 0.0708(10) Uani 1 1 d . . . H41 H 0.6180 0.1700 1.0115 0.085 Uiso 1 1 calc R . . C42 C 0.6837(3) 0.1843(3) 0.9043(3) 0.0716(11) Uani 1 1 d . . . H42 H 0.7549 0.1359 0.9129 0.086 Uiso 1 1 calc R . . C43 C 0.6601(3) 0.2352(3) 0.8331(2) 0.0557(9) Uani 1 1 d . . . H43 H 0.7164 0.2203 0.7928 0.067 Uiso 1 1 calc R . . Cl1 Cl -0.23305(6) 0.80800(5) 0.88745(4) 0.03978(14) Uani 1 1 d . . . O4 O -0.19657(18) 0.7577(2) 0.95976(11) 0.0519(5) Uani 1 1 d . . . O5 O -0.34492(17) 0.74880(18) 0.88269(11) 0.0481(5) Uani 1 1 d . . . O6 O -0.1347(2) 0.7920(3) 0.83176(12) 0.0701(7) Uani 1 1 d . . . O7 O -0.2570(3) 0.9311(2) 0.8781(2) 0.1023(12) Uani 1 1 d . . . Cl2 Cl 0.78287(5) 1.23861(5) 0.54920(3) 0.03484(13) Uani 1 1 d . . . O9 O 0.7936(2) 1.2033(2) 0.62529(12) 0.0703(7) Uani 1 1 d . . . O10 O 0.6680(2) 1.1950(2) 0.53914(12) 0.0636(7) Uani 1 1 d . . . O11 O 0.8844(3) 1.1904(3) 0.5095(2) 0.1233(15) Uani 1 1 d . . . O12 O 1.0064(5) 0.9793(5) 0.5512(3) 0.0643(12) Uani 0.50 1 d PD A -1 H1O H 0.968(7) 1.038(6) 0.527(5) 0.09(3) Uiso 0.50 1 d PD B -1 H2O H 1.054(11) 0.954(10) 0.519(4) 0.19(8) Uiso 0.50 1 d PD C -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 0.02470(17) 0.01822(16) 0.02440(17) -0.00651(13) -0.00255(13) -0.00279(12) Mn2 0.02086(16) 0.01853(16) 0.02030(16) -0.00539(12) -0.00419(12) -0.00144(12) O1 0.0268(7) 0.0248(7) 0.0260(7) -0.0059(6) -0.0060(6) -0.0045(6) O2 0.0324(8) 0.0177(7) 0.0352(8) -0.0030(6) -0.0121(7) -0.0018(6) O3 0.0246(7) 0.0240(7) 0.0263(7) -0.0074(6) -0.0060(6) -0.0026(6) N1 0.0238(8) 0.0193(8) 0.0259(9) -0.0060(7) -0.0051(7) -0.0009(6) N2 0.0294(9) 0.0263(9) 0.0258(9) -0.0094(7) 0.0003(7) -0.0048(7) N3 0.0309(9) 0.0240(9) 0.0272(9) -0.0081(7) 0.0028(8) -0.0035(7) N4 0.0292(9) 0.0214(9) 0.0251(9) -0.0059(7) -0.0002(7) -0.0025(7) N5 0.0283(9) 0.0209(9) 0.0267(9) -0.0073(7) 0.0027(7) -0.0018(7) N6 0.0206(8) 0.0247(9) 0.0220(8) -0.0072(7) -0.0037(7) 0.0001(6) N7 0.0259(9) 0.0198(8) 0.0227(9) -0.0067(7) -0.0010(7) -0.0010(7) N8 0.0221(8) 0.0225(8) 0.0241(9) -0.0069(7) -0.0033(7) -0.0001(6) O8 0.0630(12) 0.0303(9) 0.0505(11) -0.0049(8) -0.0170(10) -0.0086(8) N9 0.0301(10) 0.0293(10) 0.0543(13) -0.0164(9) 0.0012(9) 0.0004(8) C1 0.0201(9) 0.0253(10) 0.0256(10) -0.0109(8) 0.0014(8) -0.0016(8) C2 0.0266(10) 0.0246(11) 0.0324(12) -0.0096(9) 0.0021(9) -0.0038(8) C3 0.0262(11) 0.0309(12) 0.0422(13) -0.0201(10) 0.0042(10) -0.0065(9) C4 0.0250(11) 0.0407(13) 0.0448(14) -0.0256(11) -0.0080(10) -0.0015(9) C5 0.0265(11) 0.0373(13) 0.0363(12) -0.0151(10) -0.0089(9) 0.0013(9) C6 0.0211(10) 0.0270(11) 0.0294(11) -0.0114(9) -0.0035(8) -0.0013(8) C7 0.0254(10) 0.0256(11) 0.0281(11) -0.0067(8) -0.0070(8) 0.0015(8) C8 0.0346(12) 0.0375(13) 0.0281(11) -0.0145(10) -0.0005(9) -0.0094(10) C9 0.0391(12) 0.0223(10) 0.0256(11) -0.0052(8) 0.0037(9) -0.0076(9) C10 0.0510(15) 0.0280(12) 0.0282(12) -0.0101(9) 0.0047(11) -0.0074(10) C11 0.0577(17) 0.0332(13) 0.0357(14) -0.0115(11) 0.0115(12) 0.0039(12) C12 0.0411(14) 0.0433(15) 0.0393(14) -0.0076(11) 0.0072(11) 0.0062(11) C13 0.0338(12) 0.0315(12) 0.0348(13) -0.0042(10) 0.0012(10) 0.0006(9) C14 0.0268(11) 0.0323(12) 0.0306(11) -0.0102(9) -0.0047(9) -0.0032(9) C15 0.0299(11) 0.0202(10) 0.0292(11) -0.0053(8) -0.0004(9) -0.0037(8) C16 0.0301(12) 0.0315(12) 0.0406(13) -0.0109(10) -0.0001(10) 0.0004(9) C17 0.0375(13) 0.0327(12) 0.0416(14) -0.0128(11) 0.0089(11) -0.0012(10) C18 0.0483(14) 0.0260(11) 0.0261(11) -0.0075(9) 0.0052(10) -0.0019(10) C19 0.0398(12) 0.0193(10) 0.0243(11) -0.0027(8) -0.0031(9) -0.0033(9) C20 0.0339(12) 0.0242(11) 0.0357(12) -0.0099(9) 0.0014(10) -0.0070(9) C21 0.0322(11) 0.0242(11) 0.0259(11) -0.0097(9) 0.0073(9) -0.0034(9) C22 0.0379(13) 0.0230(11) 0.0367(13) -0.0076(9) 0.0070(10) -0.0059(9) C23 0.0412(13) 0.0233(11) 0.0364(13) -0.0047(9) 0.0079(10) 0.0022(9) C24 0.0358(12) 0.0297(12) 0.0297(12) -0.0058(9) 0.0051(10) 0.0039(9) C25 0.0315(11) 0.0255(11) 0.0273(11) -0.0062(9) 0.0018(9) 0.0000(9) C26 0.0210(10) 0.0275(11) 0.0268(11) -0.0086(9) -0.0026(8) -0.0002(8) C27 0.0244(10) 0.0202(10) 0.0250(10) -0.0058(8) 0.0005(8) -0.0026(8) C28 0.0263(10) 0.0301(11) 0.0303(11) -0.0090(9) 0.0014(9) -0.0009(8) C29 0.0364(12) 0.0289(11) 0.0285(11) -0.0111(9) 0.0044(9) -0.0038(9) C30 0.0398(12) 0.0222(10) 0.0243(11) -0.0084(8) -0.0007(9) -0.0040(9) C31 0.0329(11) 0.0196(10) 0.0259(11) -0.0076(8) -0.0043(9) -0.0024(8) C32 0.0229(10) 0.0365(12) 0.0251(11) -0.0117(9) -0.0073(8) 0.0044(9) C33 0.0241(10) 0.0267(10) 0.0248(10) -0.0088(8) -0.0052(8) 0.0014(8) C34 0.0301(11) 0.0405(13) 0.0245(11) -0.0068(10) -0.0073(9) 0.0043(9) C35 0.0326(12) 0.0447(14) 0.0232(11) -0.0091(10) 0.0007(9) -0.0013(10) C36 0.0257(11) 0.0381(13) 0.0336(12) -0.0154(10) 0.0013(9) 0.0015(9) C37 0.0242(10) 0.0264(11) 0.0301(11) -0.0070(9) -0.0038(9) 0.0015(8) C38 0.0250(10) 0.0246(10) 0.0292(11) -0.0056(9) -0.0026(9) -0.0007(8) C39 0.0262(11) 0.0253(11) 0.0382(13) -0.0060(9) -0.0050(9) -0.0008(8) C40 0.0536(17) 0.0403(15) 0.0434(15) 0.0022(12) -0.0130(13) 0.0063(12) C41 0.077(2) 0.0488(19) 0.083(3) 0.0030(18) -0.044(2) 0.0154(17) C42 0.0462(18) 0.0452(18) 0.132(4) -0.026(2) -0.041(2) 0.0206(14) C43 0.0293(13) 0.0357(14) 0.105(3) -0.0302(16) -0.0008(15) 0.0025(11) Cl1 0.0364(3) 0.0355(3) 0.0536(4) -0.0141(3) -0.0228(3) 0.0041(2) O4 0.0391(10) 0.0789(15) 0.0467(11) -0.0256(10) -0.0216(9) 0.0175(10) O5 0.0371(10) 0.0564(12) 0.0510(11) -0.0078(9) -0.0189(9) -0.0082(8) O6 0.0465(12) 0.115(2) 0.0450(12) -0.0163(13) -0.0040(10) -0.0114(13) O7 0.129(2) 0.0427(13) 0.173(3) -0.0448(17) -0.111(2) 0.0289(14) Cl2 0.0388(3) 0.0282(3) 0.0368(3) -0.0091(2) -0.0030(2) -0.0038(2) O9 0.0952(18) 0.0612(14) 0.0516(13) 0.0070(11) -0.0387(13) -0.0322(13) O10 0.0768(15) 0.0546(13) 0.0560(13) 0.0063(10) -0.0349(12) -0.0305(11) O11 0.129(3) 0.0625(18) 0.146(3) -0.0283(19) 0.068(2) 0.0180(18) O12 0.047(3) 0.081(4) 0.066(3) -0.022(3) -0.012(2) 0.013(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 Mn2 3.1350(4) . ? Mn1 O2 1.9026(15) . ? Mn1 O3 1.7923(15) . ? Mn1 N2 2.1632(18) . ? Mn1 N3 2.2637(18) . ? Mn1 N4 2.2499(18) . ? Mn1 N5 2.0634(18) . ? Mn2 O1 1.8860(14) . ? Mn2 O3 1.8145(14) . ? Mn2 N1 2.0252(18) . ? Mn2 N6 2.2415(17) . ? Mn2 N7 2.3136(17) . ? Mn2 N8 2.2183(17) . ? O1 C1 1.318(2) . ? O2 N1 1.374(2) . ? N1 C7 1.287(3) . ? N2 C8 1.487(3) . ? N2 C14 1.481(3) . ? N2 C20 1.496(3) . ? N3 C9 1.342(3) . ? N3 C13 1.338(3) . ? N4 C15 1.339(3) . ? N4 C19 1.346(3) . ? N5 C21 1.350(3) . ? N5 C25 1.346(3) . ? N6 C26 1.484(3) . ? N6 C32 1.477(3) . ? N6 C38 1.499(3) . ? N7 C27 1.343(3) . ? N7 C31 1.346(3) . ? N8 C33 1.337(3) . ? N8 C37 1.343(3) . ? O8 Cl2 1.4319(19) . ? N9 C39 1.337(3) . ? N9 C43 1.338(4) . ? C1 C2 1.409(3) . ? C1 C6 1.414(3) . ? C2 H2 0.950 . ? C2 C3 1.379(3) . ? C3 H3 0.950 . ? C3 C4 1.393(4) . ? C4 H4 0.950 . ? C4 C5 1.383(3) . ? C5 H5 0.950 . ? C5 C6 1.406(3) . ? C6 C7 1.449(3) . ? C7 H7 0.950 . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C8 C9 1.507(3) . ? C9 C10 1.389(3) . ? C10 H10 0.950 . ? C10 C11 1.379(4) . ? C11 H11 0.950 . ? C11 C12 1.381(4) . ? C12 H12 0.950 . ? C12 C13 1.383(4) . ? C13 H13 0.950 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.507(3) . ? C15 C16 1.387(3) . ? C16 H16 0.950 . ? C16 C17 1.382(4) . ? C17 H17 0.950 . ? C17 C18 1.381(4) . ? C18 H18 0.950 . ? C18 C19 1.377(3) . ? C19 H19 0.950 . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.498(3) . ? C21 C22 1.390(3) . ? C22 H22 0.950 . ? C22 C23 1.378(4) . ? C23 H23 0.950 . ? C23 C24 1.387(4) . ? C24 H24 0.950 . ? C24 C25 1.379(3) . ? C25 H25 0.950 . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C26 C27 1.504(3) . ? C27 C28 1.386(3) . ? C28 H28 0.950 . ? C28 C29 1.386(3) . ? C29 H29 0.950 . ? C29 C30 1.380(3) . ? C30 H30 0.950 . ? C30 C31 1.382(3) . ? C31 H31 0.950 . ? C32 H32A 0.990 . ? C32 H32B 0.990 . ? C32 C33 1.510(3) . ? C33 C34 1.385(3) . ? C34 H34 0.950 . ? C34 C35 1.385(3) . ? C35 H35 0.950 . ? C35 C36 1.376(3) . ? C36 H36 0.950 . ? C36 C37 1.385(3) . ? C37 H37 0.950 . ? C38 H38A 0.990 . ? C38 H38B 0.990 . ? C38 C39 1.510(3) . ? C39 C40 1.383(4) . ? C40 H40 0.950 . ? C40 C41 1.385(4) . ? C41 H41 0.950 . ? C41 C42 1.349(6) . ? C42 H42 0.950 . ? C42 C43 1.373(5) . ? C43 H43 0.950 . ? Cl1 O4 1.442(2) . ? Cl1 O5 1.4339(18) . ? Cl1 O6 1.419(2) . ? Cl1 O7 1.422(2) . ? Cl2 O9 1.405(2) . ? Cl2 O10 1.413(2) . ? Cl2 O11 1.424(3) . ? O12 H1O 0.846(10) . ? O12 H2O 0.843(10) . ? 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 Mn2 Mn1 O2 65.75(4) . . ? Mn2 Mn1 O3 29.84(4) . . ? Mn2 Mn1 N2 123.66(5) . . ? Mn2 Mn1 N3 99.24(5) . . ? Mn2 Mn1 N4 99.27(5) . . ? Mn2 Mn1 N5 154.08(5) . . ? O2 Mn1 O3 95.57(6) . . ? O2 Mn1 N2 169.86(7) . . ? O2 Mn1 N3 99.04(7) . . ? O2 Mn1 N4 108.76(7) . . ? O2 Mn1 N5 88.42(7) . . ? O3 Mn1 N2 93.84(7) . . ? O3 Mn1 N3 94.16(7) . . ? O3 Mn1 N4 90.96(7) . . ? O3 Mn1 N5 174.85(7) . . ? N2 Mn1 N3 76.46(7) . . ? N2 Mn1 N4 74.81(7) . . ? N2 Mn1 N5 81.98(7) . . ? N3 Mn1 N4 151.08(7) . . ? N3 Mn1 N5 81.97(7) . . ? N4 Mn1 N5 90.84(7) . . ? Mn1 Mn2 O1 148.79(5) . . ? Mn1 Mn2 O3 29.44(5) . . ? Mn1 Mn2 N1 60.92(5) . . ? Mn1 Mn2 N6 118.14(4) . . ? Mn1 Mn2 N7 92.33(4) . . ? Mn1 Mn2 N8 103.73(5) . . ? O1 Mn2 O3 175.03(7) . . ? O1 Mn2 N1 88.34(7) . . ? O1 Mn2 N6 92.84(6) . . ? O1 Mn2 N7 93.12(6) . . ? O1 Mn2 N8 86.15(6) . . ? O3 Mn2 N1 90.35(7) . . ? O3 Mn2 N6 89.76(6) . . ? O3 Mn2 N7 91.68(6) . . ? O3 Mn2 N8 90.34(6) . . ? N1 Mn2 N6 163.77(7) . . ? N1 Mn2 N7 90.27(7) . . ? N1 Mn2 N8 119.67(7) . . ? N6 Mn2 N7 73.50(6) . . ? N6 Mn2 N8 76.56(6) . . ? N7 Mn2 N8 149.98(6) . . ? Mn2 O1 C1 129.81(14) . . ? Mn1 O2 N1 115.48(12) . . ? Mn1 O3 Mn2 120.73(8) . . ? Mn2 N1 O2 117.35(12) . . ? Mn2 N1 C7 127.72(15) . . ? O2 N1 C7 114.79(17) . . ? Mn1 N2 C8 107.78(13) . . ? Mn1 N2 C14 108.17(13) . . ? Mn1 N2 C20 108.27(14) . . ? C8 N2 C14 109.73(18) . . ? C8 N2 C20 112.52(17) . . ? C14 N2 C20 110.23(17) . . ? Mn1 N3 C9 113.43(15) . . ? Mn1 N3 C13 126.96(16) . . ? C9 N3 C13 119.4(2) . . ? Mn1 N4 C15 112.78(14) . . ? Mn1 N4 C19 127.10(15) . . ? C15 N4 C19 118.77(19) . . ? Mn1 N5 C21 115.07(15) . . ? Mn1 N5 C25 125.15(15) . . ? C21 N5 C25 119.19(19) . . ? Mn2 N6 C26 104.57(12) . . ? Mn2 N6 C32 106.46(12) . . ? Mn2 N6 C38 111.36(12) . . ? C26 N6 C32 110.84(16) . . ? C26 N6 C38 112.06(16) . . ? C32 N6 C38 111.22(17) . . ? Mn2 N7 C27 112.65(13) . . ? Mn2 N7 C31 129.32(14) . . ? C27 N7 C31 117.99(18) . . ? Mn2 N8 C33 114.82(13) . . ? Mn2 N8 C37 125.80(14) . . ? C33 N8 C37 118.91(18) . . ? C39 N9 C43 117.5(3) . . ? O1 C1 C2 118.9(2) . . ? O1 C1 C6 123.10(18) . . ? C2 C1 C6 117.98(19) . . ? C1 C2 H2 119.4 . . ? C1 C2 C3 121.1(2) . . ? H2 C2 C3 119.4 . . ? C2 C3 H3 119.4 . . ? C2 C3 C4 121.1(2) . . ? H3 C3 C4 119.4 . . ? C3 C4 H4 120.7 . . ? C3 C4 C5 118.7(2) . . ? H4 C4 C5 120.7 . . ? C4 C5 H5 119.3 . . ? C4 C5 C6 121.5(2) . . ? H5 C5 C6 119.3 . . ? C1 C6 C5 119.6(2) . . ? C1 C6 C7 122.49(19) . . ? C5 C6 C7 117.9(2) . . ? N1 C7 C6 123.5(2) . . ? N1 C7 H7 118.2 . . ? C6 C7 H7 118.2 . . ? N2 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? N2 C8 C9 111.43(19) . . ? H8A C8 H8B 108.0 . . ? H8A C8 C9 109.3 . . ? H8B C8 C9 109.3 . . ? N3 C9 C8 114.93(19) . . ? N3 C9 C10 121.8(2) . . ? C8 C9 C10 123.1(2) . . ? C9 C10 H10 120.7 . . ? C9 C10 C11 118.5(2) . . ? H10 C10 C11 120.7 . . ? C10 C11 H11 120.2 . . ? C10 C11 C12 119.5(2) . . ? H11 C11 C12 120.2 . . ? C11 C12 H12 120.5 . . ? C11 C12 C13 119.0(3) . . ? H12 C12 C13 120.5 . . ? N3 C13 C12 121.7(2) . . ? N3 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? N2 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? N2 C14 C15 110.88(18) . . ? H14A C14 H14B 108.1 . . ? H14A C14 C15 109.5 . . ? H14B C14 C15 109.5 . . ? N4 C15 C14 116.32(19) . . ? N4 C15 C16 122.5(2) . . ? C14 C15 C16 121.1(2) . . ? C15 C16 H16 120.9 . . ? C15 C16 C17 118.3(2) . . ? H16 C16 C17 120.9 . . ? C16 C17 H17 120.3 . . ? C16 C17 C18 119.4(2) . . ? H17 C17 C18 120.3 . . ? C17 C18 H18 120.4 . . ? C17 C18 C19 119.2(2) . . ? H18 C18 C19 120.4 . . ? N4 C19 C18 121.9(2) . . ? N4 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? N2 C20 H20A 108.8 . . ? N2 C20 H20B 108.8 . . ? N2 C20 C21 113.82(18) . . ? H20A C20 H20B 107.7 . . ? H20A C20 C21 108.8 . . ? H20B C20 C21 108.8 . . ? N5 C21 C20 117.85(19) . . ? N5 C21 C22 121.1(2) . . ? C20 C21 C22 121.0(2) . . ? C21 C22 H22 120.3 . . ? C21 C22 C23 119.4(2) . . ? H22 C22 C23 120.3 . . ? C22 C23 H23 120.3 . . ? C22 C23 C24 119.3(2) . . ? H23 C23 C24 120.3 . . ? C23 C24 H24 120.7 . . ? C23 C24 C25 118.7(2) . . ? H24 C24 C25 120.7 . . ? N5 C25 C24 122.3(2) . . ? N5 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? N6 C26 H26A 109.6 . . ? N6 C26 H26B 109.6 . . ? N6 C26 C27 110.15(16) . . ? H26A C26 H26B 108.1 . . ? H26A C26 C27 109.6 . . ? H26B C26 C27 109.6 . . ? N7 C27 C26 115.45(18) . . ? N7 C27 C28 122.6(2) . . ? C26 C27 C28 121.97(19) . . ? C27 C28 H28 120.6 . . ? C27 C28 C29 118.8(2) . . ? H28 C28 C29 120.6 . . ? C28 C29 H29 120.5 . . ? C28 C29 C30 119.0(2) . . ? H29 C29 C30 120.5 . . ? C29 C30 H30 120.5 . . ? C29 C30 C31 119.0(2) . . ? H30 C30 C31 120.5 . . ? N7 C31 C30 122.7(2) . . ? N7 C31 H31 118.7 . . ? C30 C31 H31 118.7 . . ? N6 C32 H32A 109.4 . . ? N6 C32 H32B 109.4 . . ? N6 C32 C33 111.31(16) . . ? H32A C32 H32B 108.0 . . ? H32A C32 C33 109.4 . . ? H32B C32 C33 109.4 . . ? N8 C33 C32 115.40(18) . . ? N8 C33 C34 122.1(2) . . ? C32 C33 C34 122.42(19) . . ? C33 C34 H34 120.6 . . ? C33 C34 C35 118.8(2) . . ? H34 C34 C35 120.6 . . ? C34 C35 H35 120.4 . . ? C34 C35 C36 119.1(2) . . ? H35 C35 C36 120.4 . . ? C35 C36 H36 120.5 . . ? C35 C36 C37 119.1(2) . . ? H36 C36 C37 120.5 . . ? N8 C37 C36 121.9(2) . . ? N8 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? N6 C38 H38A 108.7 . . ? N6 C38 H38B 108.7 . . ? N6 C38 C39 114.15(17) . . ? H38A C38 H38B 107.6 . . ? H38A C38 C39 108.7 . . ? H38B C38 C39 108.7 . . ? N9 C39 C38 115.6(2) . . ? N9 C39 C40 122.4(2) . . ? C38 C39 C40 122.0(2) . . ? C39 C40 H40 120.9 . . ? C39 C40 C41 118.1(3) . . ? H40 C40 C41 120.9 . . ? C40 C41 H41 120.0 . . ? C40 C41 C42 120.0(3) . . ? H41 C41 C42 120.0 . . ? C41 C42 H42 120.7 . . ? C41 C42 C43 118.6(3) . . ? H42 C42 C43 120.7 . . ? N9 C43 C42 123.4(3) . . ? N9 C43 H43 118.3 . . ? C42 C43 H43 118.3 . . ? O4 Cl1 O5 109.74(12) . . ? O4 Cl1 O6 108.97(13) . . ? O4 Cl1 O7 108.66(16) . . ? O5 Cl1 O6 109.26(14) . . ? O5 Cl1 O7 109.32(15) . . ? O6 Cl1 O7 110.9(2) . . ? O8 Cl2 O9 111.68(13) . . ? O8 Cl2 O10 110.78(13) . . ? O8 Cl2 O11 106.55(16) . . ? O9 Cl2 O10 109.64(13) . . ? O9 Cl2 O11 108.7(2) . . ? O10 Cl2 O11 109.5(2) . . ? H1O O12 H2O 106(3) . . ? 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 O2 Mn1 Mn2 O1 -7.23(11) . . . . ? O2 Mn1 Mn2 O3 -178.01(11) . . . . ? O2 Mn1 Mn2 N1 3.68(8) . . . . ? O2 Mn1 Mn2 N6 165.20(7) . . . . ? O2 Mn1 Mn2 N7 92.69(7) . . . . ? O2 Mn1 Mn2 N8 -112.89(7) . . . . ? O3 Mn1 Mn2 O1 170.79(13) . . . . ? O3 Mn1 Mn2 N1 -178.31(11) . . . . ? O3 Mn1 Mn2 N6 -16.79(11) . . . . ? O3 Mn1 Mn2 N7 -89.30(10) . . . . ? O3 Mn1 Mn2 N8 65.13(10) . . . . ? N2 Mn1 Mn2 O1 168.42(11) . . . . ? N2 Mn1 Mn2 O3 -2.37(11) . . . . ? N2 Mn1 Mn2 N1 179.32(8) . . . . ? N2 Mn1 Mn2 N6 -19.16(8) . . . . ? N2 Mn1 Mn2 N7 -91.67(7) . . . . ? N2 Mn1 Mn2 N8 62.76(7) . . . . ? N3 Mn1 Mn2 O1 88.59(10) . . . . ? N3 Mn1 Mn2 O3 -82.19(11) . . . . ? N3 Mn1 Mn2 N1 99.50(8) . . . . ? N3 Mn1 Mn2 N6 -98.98(7) . . . . ? N3 Mn1 Mn2 N7 -171.49(7) . . . . ? N3 Mn1 Mn2 N8 -17.07(7) . . . . ? N4 Mn1 Mn2 O1 -113.72(10) . . . . ? N4 Mn1 Mn2 O3 75.49(11) . . . . ? N4 Mn1 Mn2 N1 -102.82(7) . . . . ? N4 Mn1 Mn2 N6 58.70(7) . . . . ? N4 Mn1 Mn2 N7 -13.81(7) . . . . ? N4 Mn1 Mn2 N8 140.62(7) . . . . ? N5 Mn1 Mn2 O1 -2.03(15) . . . . ? N5 Mn1 Mn2 O3 -172.81(15) . . . . ? N5 Mn1 Mn2 N1 8.88(13) . . . . ? N5 Mn1 Mn2 N6 170.40(12) . . . . ? N5 Mn1 Mn2 N7 97.89(12) . . . . ? N5 Mn1 Mn2 N8 -107.68(12) . . . . ? Mn1 Mn2 O1 C1 35.0(2) . . . . ? O3 Mn2 O1 C1 100.2(8) . . . . ? N1 Mn2 O1 C1 25.48(17) . . . . ? N6 Mn2 O1 C1 -138.32(17) . . . . ? N7 Mn2 O1 C1 -64.70(17) . . . . ? N8 Mn2 O1 C1 145.37(17) . . . . ? Mn2 Mn1 O2 N1 -5.25(11) . . . . ? O3 Mn1 O2 N1 -6.24(14) . . . . ? N2 Mn1 O2 N1 -164.2(3) . . . . ? N3 Mn1 O2 N1 -101.37(13) . . . . ? N4 Mn1 O2 N1 86.68(14) . . . . ? N5 Mn1 O2 N1 177.02(14) . . . . ? O2 Mn1 O3 Mn2 1.82(10) . . . . ? N2 Mn1 O3 Mn2 178.02(9) . . . . ? N3 Mn1 O3 Mn2 101.34(9) . . . . ? N4 Mn1 O3 Mn2 -107.14(9) . . . . ? N5 Mn1 O3 Mn2 142.5(7) . . . . ? O1 Mn2 O3 Mn1 -73.2(8) . . . . ? N1 Mn2 O3 Mn1 1.48(10) . . . . ? N6 Mn2 O3 Mn1 165.24(9) . . . . ? N7 Mn2 O3 Mn1 91.76(9) . . . . ? N8 Mn2 O3 Mn1 -118.20(9) . . . . ? Mn1 O2 N1 Mn2 8.36(18) . . . . ? Mn1 O2 N1 C7 -167.69(15) . . . . ? Mn1 Mn2 N1 O2 -5.23(11) . . . . ? Mn1 Mn2 N1 C7 170.2(2) . . . . ? O1 Mn2 N1 O2 169.14(14) . . . . ? O1 Mn2 N1 C7 -15.39(19) . . . . ? O3 Mn2 N1 O2 -6.06(14) . . . . ? O3 Mn2 N1 C7 169.40(19) . . . . ? N6 Mn2 N1 O2 -96.4(3) . . . . ? N6 Mn2 N1 C7 79.1(3) . . . . ? N7 Mn2 N1 O2 -97.74(14) . . . . ? N7 Mn2 N1 C7 77.72(19) . . . . ? N8 Mn2 N1 O2 84.53(15) . . . . ? N8 Mn2 N1 C7 -100.00(19) . . . . ? Mn2 Mn1 N2 C8 -62.77(15) . . . . ? Mn2 Mn1 N2 C14 55.81(15) . . . . ? Mn2 Mn1 N2 C20 175.26(11) . . . . ? O2 Mn1 N2 C8 94.1(4) . . . . ? O2 Mn1 N2 C14 -147.3(4) . . . . ? O2 Mn1 N2 C20 -27.9(5) . . . . ? O3 Mn1 N2 C8 -63.96(15) . . . . ? O3 Mn1 N2 C14 54.62(14) . . . . ? O3 Mn1 N2 C20 174.08(13) . . . . ? N3 Mn1 N2 C8 29.41(14) . . . . ? N3 Mn1 N2 C14 147.99(15) . . . . ? N3 Mn1 N2 C20 -92.56(14) . . . . ? N4 Mn1 N2 C8 -153.91(16) . . . . ? N4 Mn1 N2 C14 -35.33(13) . . . . ? N4 Mn1 N2 C20 84.12(14) . . . . ? N5 Mn1 N2 C8 113.02(15) . . . . ? N5 Mn1 N2 C14 -128.40(14) . . . . ? N5 Mn1 N2 C20 -8.95(13) . . . . ? Mn2 Mn1 N3 C9 110.73(15) . . . . ? Mn2 Mn1 N3 C13 -74.88(19) . . . . ? O2 Mn1 N3 C9 177.43(15) . . . . ? O2 Mn1 N3 C13 -8.2(2) . . . . ? O3 Mn1 N3 C9 81.11(16) . . . . ? O3 Mn1 N3 C13 -104.50(19) . . . . ? N2 Mn1 N3 C9 -11.85(15) . . . . ? N2 Mn1 N3 C13 162.5(2) . . . . ? N4 Mn1 N3 C9 -18.5(2) . . . . ? N4 Mn1 N3 C13 155.92(17) . . . . ? N5 Mn1 N3 C9 -95.47(16) . . . . ? N5 Mn1 N3 C13 78.92(19) . . . . ? Mn2 Mn1 N4 C15 -97.53(14) . . . . ? Mn2 Mn1 N4 C19 68.91(17) . . . . ? O2 Mn1 N4 C15 -164.94(14) . . . . ? O2 Mn1 N4 C19 1.49(19) . . . . ? O3 Mn1 N4 C15 -68.73(15) . . . . ? O3 Mn1 N4 C19 97.71(18) . . . . ? N2 Mn1 N4 C15 24.99(14) . . . . ? N2 Mn1 N4 C19 -168.58(19) . . . . ? N3 Mn1 N4 C15 31.7(2) . . . . ? N3 Mn1 N4 C19 -161.90(16) . . . . ? N5 Mn1 N4 C15 106.44(15) . . . . ? N5 Mn1 N4 C19 -87.12(18) . . . . ? Mn2 Mn1 N5 C21 170.89(10) . . . . ? Mn2 Mn1 N5 C25 -0.2(3) . . . . ? O2 Mn1 N5 C21 175.63(15) . . . . ? O2 Mn1 N5 C25 4.54(17) . . . . ? O3 Mn1 N5 C21 34.8(8) . . . . ? O3 Mn1 N5 C25 -136.3(7) . . . . ? N2 Mn1 N5 C21 -1.09(15) . . . . ? N2 Mn1 N5 C25 -172.18(18) . . . . ? N3 Mn1 N5 C21 76.27(15) . . . . ? N3 Mn1 N5 C25 -94.83(17) . . . . ? N4 Mn1 N5 C21 -75.62(15) . . . . ? N4 Mn1 N5 C25 113.29(17) . . . . ? Mn1 Mn2 N6 C26 -45.57(13) . . . . ? Mn1 Mn2 N6 C32 71.83(13) . . . . ? Mn1 Mn2 N6 C38 -166.78(11) . . . . ? O1 Mn2 N6 C26 130.51(12) . . . . ? O1 Mn2 N6 C32 -112.10(13) . . . . ? O1 Mn2 N6 C38 9.29(13) . . . . ? O3 Mn2 N6 C26 -53.73(12) . . . . ? O3 Mn2 N6 C32 63.67(13) . . . . ? O3 Mn2 N6 C38 -174.94(13) . . . . ? N1 Mn2 N6 C26 36.7(3) . . . . ? N1 Mn2 N6 C32 154.1(2) . . . . ? N1 Mn2 N6 C38 -84.5(3) . . . . ? N7 Mn2 N6 C26 38.10(12) . . . . ? N7 Mn2 N6 C32 155.49(14) . . . . ? N7 Mn2 N6 C38 -83.12(13) . . . . ? N8 Mn2 N6 C26 -144.14(13) . . . . ? N8 Mn2 N6 C32 -26.74(13) . . . . ? N8 Mn2 N6 C38 94.65(13) . . . . ? Mn1 Mn2 N7 C27 97.47(13) . . . . ? Mn1 Mn2 N7 C31 -80.09(17) . . . . ? O1 Mn2 N7 C27 -113.26(14) . . . . ? O1 Mn2 N7 C31 69.17(17) . . . . ? O3 Mn2 N7 C27 68.03(14) . . . . ? O3 Mn2 N7 C31 -109.54(17) . . . . ? N1 Mn2 N7 C27 158.38(14) . . . . ? N1 Mn2 N7 C31 -19.18(17) . . . . ? N6 Mn2 N7 C27 -21.22(13) . . . . ? N6 Mn2 N7 C31 161.21(18) . . . . ? N8 Mn2 N7 C27 -25.6(2) . . . . ? N8 Mn2 N7 C31 156.86(16) . . . . ? Mn1 Mn2 N8 C33 -108.41(14) . . . . ? Mn1 Mn2 N8 C37 79.58(17) . . . . ? O1 Mn2 N8 C33 101.59(15) . . . . ? O1 Mn2 N8 C37 -70.42(17) . . . . ? O3 Mn2 N8 C33 -81.93(15) . . . . ? O3 Mn2 N8 C37 106.06(17) . . . . ? N1 Mn2 N8 C33 -172.53(14) . . . . ? N1 Mn2 N8 C37 15.46(19) . . . . ? N6 Mn2 N8 C33 7.74(14) . . . . ? N6 Mn2 N8 C37 -164.27(18) . . . . ? N7 Mn2 N8 C33 12.0(2) . . . . ? N7 Mn2 N8 C37 -159.98(15) . . . . ? Mn2 O1 C1 C2 158.97(15) . . . . ? Mn2 O1 C1 C6 -23.2(3) . . . . ? O1 C1 C2 C3 179.13(19) . . . . ? C6 C1 C2 C3 1.2(3) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C2 C3 C4 C5 -0.7(3) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C4 C5 C6 C1 1.0(3) . . . . ? C4 C5 C6 C7 179.9(2) . . . . ? O1 C1 C6 C5 -179.55(19) . . . . ? O1 C1 C6 C7 1.7(3) . . . . ? C2 C1 C6 C5 -1.7(3) . . . . ? C2 C1 C6 C7 179.53(19) . . . . ? Mn2 N1 C7 C6 3.2(3) . . . . ? O2 N1 C7 C6 178.74(19) . . . . ? C1 C6 C7 N1 7.7(3) . . . . ? C5 C6 C7 N1 -171.1(2) . . . . ? Mn1 N2 C8 C9 -44.1(2) . . . . ? C14 N2 C8 C9 -161.69(18) . . . . ? C20 N2 C8 C9 75.2(2) . . . . ? Mn1 N3 C9 C8 -9.1(2) . . . . ? Mn1 N3 C9 C10 174.57(17) . . . . ? C13 N3 C9 C8 176.0(2) . . . . ? C13 N3 C9 C10 -0.3(3) . . . . ? N2 C8 C9 N3 36.0(3) . . . . ? N2 C8 C9 C10 -147.8(2) . . . . ? N3 C9 C10 C11 0.1(4) . . . . ? C8 C9 C10 C11 -175.8(2) . . . . ? C9 C10 C11 C12 0.5(4) . . . . ? C10 C11 C12 C13 -0.9(4) . . . . ? Mn1 N3 C13 C12 -174.29(18) . . . . ? C9 N3 C13 C12 -0.2(3) . . . . ? C11 C12 C13 N3 0.8(4) . . . . ? Mn1 N2 C14 C15 42.4(2) . . . . ? C8 N2 C14 C15 159.75(17) . . . . ? C20 N2 C14 C15 -75.8(2) . . . . ? Mn1 N4 C15 C14 -8.8(2) . . . . ? Mn1 N4 C15 C16 168.43(17) . . . . ? C19 N4 C15 C14 -176.43(19) . . . . ? C19 N4 C15 C16 0.8(3) . . . . ? N2 C14 C15 N4 -22.3(3) . . . . ? N2 C14 C15 C16 160.5(2) . . . . ? N4 C15 C16 C17 -0.8(3) . . . . ? C14 C15 C16 C17 176.2(2) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? C16 C17 C18 C19 0.9(4) . . . . ? Mn1 N4 C19 C18 -165.55(16) . . . . ? C15 N4 C19 C18 0.2(3) . . . . ? C17 C18 C19 N4 -1.0(3) . . . . ? Mn1 N2 C20 C21 17.1(2) . . . . ? C8 N2 C20 C21 -101.9(2) . . . . ? C14 N2 C20 C21 135.21(19) . . . . ? Mn1 N5 C21 C20 11.6(2) . . . . ? Mn1 N5 C21 C22 -171.27(16) . . . . ? C25 N5 C21 C20 -176.72(19) . . . . ? C25 N5 C21 C22 0.4(3) . . . . ? N2 C20 C21 N5 -19.8(3) . . . . ? N2 C20 C21 C22 163.06(19) . . . . ? N5 C21 C22 C23 -0.8(3) . . . . ? C20 C21 C22 C23 176.3(2) . . . . ? C21 C22 C23 C24 0.1(3) . . . . ? C22 C23 C24 C25 0.8(3) . . . . ? Mn1 N5 C25 C24 171.39(16) . . . . ? C21 N5 C25 C24 0.6(3) . . . . ? C23 C24 C25 N5 -1.2(3) . . . . ? Mn2 N6 C26 C27 -52.42(17) . . . . ? C32 N6 C26 C27 -166.76(17) . . . . ? C38 N6 C26 C27 68.3(2) . . . . ? Mn2 N7 C27 C26 -1.5(2) . . . . ? Mn2 N7 C27 C28 -179.88(16) . . . . ? C31 N7 C27 C26 176.40(17) . . . . ? C31 N7 C27 C28 -2.0(3) . . . . ? N6 C26 C27 N7 36.9(2) . . . . ? N6 C26 C27 C28 -144.6(2) . . . . ? N7 C27 C28 C29 1.9(3) . . . . ? C26 C27 C28 C29 -176.4(2) . . . . ? C27 C28 C29 C30 -0.3(3) . . . . ? C28 C29 C30 C31 -1.1(3) . . . . ? Mn2 N7 C31 C30 177.97(15) . . . . ? C27 N7 C31 C30 0.5(3) . . . . ? C29 C30 C31 N7 1.1(3) . . . . ? Mn2 N6 C32 C33 42.2(2) . . . . ? C26 N6 C32 C33 155.34(18) . . . . ? C38 N6 C32 C33 -79.3(2) . . . . ? Mn2 N8 C33 C32 13.7(2) . . . . ? Mn2 N8 C33 C34 -169.61(17) . . . . ? C37 N8 C33 C32 -173.70(18) . . . . ? C37 N8 C33 C34 3.0(3) . . . . ? N6 C32 C33 N8 -38.9(3) . . . . ? N6 C32 C33 C34 144.4(2) . . . . ? N8 C33 C34 C35 -3.3(3) . . . . ? C32 C33 C34 C35 173.2(2) . . . . ? C33 C34 C35 C36 0.5(4) . . . . ? C34 C35 C36 C37 2.3(4) . . . . ? Mn2 N8 C37 C36 171.78(16) . . . . ? C33 N8 C37 C36 0.1(3) . . . . ? C35 C36 C37 N8 -2.7(3) . . . . ? Mn2 N6 C38 C39 167.99(15) . . . . ? C26 N6 C38 C39 51.3(2) . . . . ? C32 N6 C38 C39 -73.4(2) . . . . ? C43 N9 C39 C38 178.6(2) . . . . ? C43 N9 C39 C40 -0.9(4) . . . . ? N6 C38 C39 N9 -89.2(2) . . . . ? N6 C38 C39 C40 90.3(3) . . . . ? N9 C39 C40 C41 1.3(4) . . . . ? C38 C39 C40 C41 -178.2(3) . . . . ? C39 C40 C41 C42 -0.8(5) . . . . ? C40 C41 C42 C43 0.0(5) . . . . ? C39 N9 C43 C42 0.0(4) . . . . ? C41 C42 C43 N9 0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.674 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.052 _database_code_depnum_ccdc_archive 'CCDC 950511' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2-eb2176 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H43 Mn2 N9 O3 2+, 2 Cl O4 -, 0.32 H2 O' _chemical_formula_sum 'C44 H43.64 Cl2 Mn2 N9 O11.32' _chemical_formula_weight 1060.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 '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 10.7046(4) _cell_length_b 11.6206(4) _cell_length_c 19.4847(6) _cell_angle_alpha 74.968(3) _cell_angle_beta 79.750(3) _cell_angle_gamma 89.644(3) _cell_volume 2301.46(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13389 _cell_measurement_theta_min 3.9390 _cell_measurement_theta_max 73.7687 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1090 _exptl_absorpt_coefficient_mu 6.141 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.3146 _exptl_absorpt_correction_T_max 0.6110 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21c (release 23-05-2012 CrysAlis171 .NET) (compiled May 23 2012,12:53:54) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Agilent Technologies SuperNova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_reflns_number 36643 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 73.93 _reflns_number_total 9143 _reflns_number_gt 7880 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2011)' _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2011)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2011)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and local programs' _refine_special_details ; One of the perchlorate anions (atoms Cl2 to C11) was refined using a two-part disorder model with occupancy ratio 0.511:0.489(16) and the geometry of the anion was restrained to be similar to that of the ordered perchlorate (Cl1 to O7). When the model was complete a large residual peak of ~2.3 e.A-3 was identified. This has been modelled as 1/3 of a water molecule. Water H atoms were added using the CALC-OH routine of WinGX and refined with restrained O-H and H...H distances. 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^)+(0.0667P)^2^+2.1610P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary charge-flipping _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00073(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9143 _refine_ls_number_parameters 677 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _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 Mn1 Mn 0.31501(4) 0.40714(4) 0.22848(2) 0.03165(13) Uani 1 1 d . . . Mn2 Mn 0.26067(4) 0.13431(4) 0.29512(2) 0.02948(12) Uani 1 1 d . . . O1 O 0.15099(19) 0.00011(18) 0.31516(11) 0.0369(4) Uani 1 1 d . . . O2 O 0.16586(19) 0.34538(17) 0.20757(11) 0.0367(4) Uani 1 1 d . . . O3 O 0.35747(18) 0.26863(18) 0.28277(10) 0.0342(4) Uani 1 1 d . . . N1 N 0.1475(2) 0.2233(2) 0.22716(13) 0.0325(5) Uani 1 1 d . . . N2 N 0.4654(2) 0.5062(2) 0.25217(13) 0.0377(6) Uani 1 1 d . . . N3 N 0.4807(2) 0.4067(2) 0.14016(13) 0.0343(5) Uani 1 1 d . . . N4 N 0.2204(2) 0.4734(2) 0.32344(13) 0.0379(6) Uani 1 1 d . . . N5 N 0.2776(2) 0.5752(2) 0.17123(13) 0.0372(5) Uani 1 1 d . . . N6 N 0.4098(2) 0.0239(2) 0.34558(12) 0.0314(5) Uani 1 1 d . . . N7 N 0.2018(2) 0.1248(2) 0.41135(13) 0.0326(5) Uani 1 1 d . . . N8 N 0.3943(2) 0.0861(2) 0.20260(13) 0.0334(5) Uani 1 1 d . . . N9 N 0.5665(2) -0.2106(2) 0.32681(15) 0.0449(6) Uani 1 1 d . . . C1 C 0.0823(3) -0.0305(3) 0.27156(16) 0.0341(6) Uani 1 1 d . . . C2 C 0.0544(3) -0.1529(3) 0.28277(18) 0.0403(7) Uani 1 1 d . . . H2 H 0.0868 -0.2095 0.3193 0.048 Uiso 1 1 calc R . . C3 C -0.0195(3) -0.1917(3) 0.2412(2) 0.0479(8) Uani 1 1 d . . . H3 H -0.0384 -0.2746 0.2498 0.057 Uiso 1 1 calc R . . C4 C -0.0659(3) -0.1109(3) 0.1873(2) 0.0508(9) Uani 1 1 d . . . H4 H -0.1152 -0.1379 0.1581 0.061 Uiso 1 1 calc R . . C5 C -0.0404(3) 0.0098(3) 0.17610(19) 0.0445(7) Uani 1 1 d . . . H5 H -0.0729 0.0650 0.1390 0.053 Uiso 1 1 calc R . . C6 C 0.0325(3) 0.0531(3) 0.21817(16) 0.0347(6) Uani 1 1 d . . . C7 C 0.0544(3) 0.1831(3) 0.20408(15) 0.0342(6) Uani 1 1 d . . . C8 C -0.0273(3) 0.2682(3) 0.16348(18) 0.0445(7) Uani 1 1 d . . . H8A H 0.0161 0.2988 0.1132 0.067 Uiso 1 1 calc R . . H8B H -0.0441 0.3347 0.1857 0.067 Uiso 1 1 calc R . . H8C H -0.1078 0.2274 0.1647 0.067 Uiso 1 1 calc R . . C9 C 0.5870(3) 0.4531(3) 0.22962(17) 0.0414(7) Uani 1 1 d . . . H9A H 0.5957 0.3775 0.2659 0.050 Uiso 1 1 calc R . . H9B H 0.6586 0.5082 0.2273 0.050 Uiso 1 1 calc R . . C10 C 0.5927(3) 0.4290(3) 0.15712(16) 0.0368(6) Uani 1 1 d . . . C11 C 0.7066(3) 0.4256(3) 0.11169(18) 0.0438(7) Uani 1 1 d . . . H11 H 0.7843 0.4462 0.1236 0.053 Uiso 1 1 calc R . . C12 C 0.7063(3) 0.3920(3) 0.04869(18) 0.0485(8) Uani 1 1 d . . . H12 H 0.7839 0.3864 0.0175 0.058 Uiso 1 1 calc R . . C13 C 0.5911(3) 0.3666(3) 0.03171(17) 0.0436(7) Uani 1 1 d . . . H13 H 0.5883 0.3425 -0.0110 0.052 Uiso 1 1 calc R . . C14 C 0.4803(3) 0.3769(3) 0.07803(16) 0.0374(6) Uani 1 1 d . . . H14 H 0.4011 0.3624 0.0655 0.045 Uiso 1 1 calc R . . C15 C 0.4405(3) 0.4909(3) 0.33119(16) 0.0431(7) Uani 1 1 d . . . H15A H 0.4967 0.5472 0.3433 0.052 Uiso 1 1 calc R . . H15B H 0.4597 0.4088 0.3560 0.052 Uiso 1 1 calc R . . C16 C 0.3033(3) 0.5138(3) 0.35714(16) 0.0399(7) Uani 1 1 d . . . C17 C 0.2644(4) 0.5678(3) 0.41222(17) 0.0466(8) Uani 1 1 d . . . H17 H 0.3245 0.5955 0.4353 0.056 Uiso 1 1 calc R . . C18 C 0.1347(4) 0.5807(3) 0.43311(18) 0.0514(9) Uani 1 1 d . . . H18 H 0.1052 0.6180 0.4706 0.062 Uiso 1 1 calc R . . C19 C 0.0495(3) 0.5389(3) 0.39877(18) 0.0482(8) Uani 1 1 d . . . H19 H -0.0393 0.5466 0.4124 0.058 Uiso 1 1 calc R . . C20 C 0.0957(3) 0.4854(3) 0.34410(17) 0.0417(7) Uani 1 1 d . . . H20 H 0.0373 0.4563 0.3205 0.050 Uiso 1 1 calc R . . C21 C 0.4663(3) 0.6340(3) 0.21078(17) 0.0427(7) Uani 1 1 d . . . H21A H 0.5450 0.6527 0.1738 0.051 Uiso 1 1 calc R . . H21B H 0.4686 0.6847 0.2443 0.051 Uiso 1 1 calc R . . C22 C 0.3541(3) 0.6653(3) 0.17406(16) 0.0390(7) Uani 1 1 d . . . C23 C 0.3323(4) 0.7824(3) 0.1422(2) 0.0518(9) Uani 1 1 d . . . H23 H 0.3870 0.8447 0.1446 0.062 Uiso 1 1 calc R . . C24 C 0.2315(4) 0.8087(3) 0.1070(2) 0.0545(9) Uani 1 1 d . . . H24 H 0.2160 0.8891 0.0847 0.065 Uiso 1 1 calc R . . C25 C 0.1522(3) 0.7162(3) 0.10434(19) 0.0489(8) Uani 1 1 d . . . H25 H 0.0815 0.7322 0.0805 0.059 Uiso 1 1 calc R . . C26 C 0.1783(3) 0.6015(3) 0.13679(17) 0.0416(7) Uani 1 1 d . . . H26 H 0.1243 0.5381 0.1350 0.050 Uiso 1 1 calc R . . C27 C 0.4153(3) 0.0575(3) 0.41283(16) 0.0376(6) Uani 1 1 d . . . H27A H 0.4651 0.1338 0.4012 0.045 Uiso 1 1 calc R . . H27B H 0.4593 -0.0042 0.4442 0.045 Uiso 1 1 calc R . . C28 C 0.2835(3) 0.0708(3) 0.45326(15) 0.0344(6) Uani 1 1 d . . . C29 C 0.2508(3) 0.0368(3) 0.52761(17) 0.0435(7) Uani 1 1 d . . . H29 H 0.3081 -0.0057 0.5560 0.052 Uiso 1 1 calc R . . C30 C 0.1331(3) 0.0655(3) 0.56030(17) 0.0465(8) Uani 1 1 d . . . H30 H 0.1091 0.0442 0.6115 0.056 Uiso 1 1 calc R . . C31 C 0.0517(3) 0.1252(3) 0.51744(17) 0.0420(7) Uani 1 1 d . . . H31 H -0.0284 0.1480 0.5386 0.050 Uiso 1 1 calc R . . C32 C 0.0879(3) 0.1517(3) 0.44324(17) 0.0377(6) Uani 1 1 d . . . H32 H 0.0301 0.1903 0.4138 0.045 Uiso 1 1 calc R . . C33 C 0.5287(3) 0.0617(3) 0.29169(16) 0.0359(6) Uani 1 1 d . . . H33A H 0.5971 0.0081 0.3061 0.043 Uiso 1 1 calc R . . H33B H 0.5552 0.1436 0.2907 0.043 Uiso 1 1 calc R . . C34 C 0.5099(3) 0.0583(3) 0.21775(16) 0.0355(6) Uani 1 1 d . . . C35 C 0.6071(3) 0.0328(3) 0.16724(18) 0.0432(7) Uani 1 1 d . . . H35 H 0.6872 0.0103 0.1798 0.052 Uiso 1 1 calc R . . C36 C 0.5857(3) 0.0408(3) 0.09818(18) 0.0465(8) Uani 1 1 d . . . H36 H 0.6510 0.0243 0.0625 0.056 Uiso 1 1 calc R . . C37 C 0.4688(3) 0.0727(3) 0.08201(17) 0.0419(7) Uani 1 1 d . . . H37 H 0.4524 0.0806 0.0347 0.050 Uiso 1 1 calc R . . C38 C 0.3752(3) 0.0933(3) 0.13551(16) 0.0371(6) Uani 1 1 d . . . H38 H 0.2937 0.1134 0.1243 0.045 Uiso 1 1 calc R . . C39 C 0.3794(3) -0.1066(3) 0.35962(16) 0.0371(6) Uani 1 1 d . . . H39A H 0.3576 -0.1216 0.3153 0.045 Uiso 1 1 calc R . . H39B H 0.3033 -0.1287 0.3982 0.045 Uiso 1 1 calc R . . C40 C 0.4849(3) -0.1864(3) 0.38169(17) 0.0390(7) Uani 1 1 d . . . C41 C 0.4968(4) -0.2304(3) 0.45295(19) 0.0523(8) Uani 1 1 d . . . H41 H 0.4373 -0.2118 0.4905 0.063 Uiso 1 1 calc R . . C42 C 0.5965(4) -0.3020(4) 0.4689(3) 0.0712(12) Uani 1 1 d . . . H42 H 0.6065 -0.3330 0.5177 0.085 Uiso 1 1 calc R . . C43 C 0.6795(4) -0.3274(4) 0.4150(3) 0.0695(12) Uani 1 1 d . . . H43 H 0.7485 -0.3768 0.4251 0.083 Uiso 1 1 calc R . . C44 C 0.6629(3) -0.2806(3) 0.3445(2) 0.0569(10) Uani 1 1 d . . . H44 H 0.7223 -0.2987 0.3067 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.77475(7) 0.30956(7) 0.38022(4) 0.04509(19) Uani 1 1 d D . . O4 O 0.8697(3) 0.2653(3) 0.33462(15) 0.0726(8) Uani 1 1 d D . . O5 O 0.8037(2) 0.2753(3) 0.45193(15) 0.0735(9) Uani 1 1 d D . . O6 O 0.7727(4) 0.4346(3) 0.3567(3) 0.1126(16) Uani 1 1 d D . . O7 O 0.6531(2) 0.2585(3) 0.38028(14) 0.0595(7) Uani 1 1 d D . . Cl2 Cl 0.7663(3) 0.7527(3) 0.0371(2) 0.0367(10) Uani 0.511(16) 1 d PD A 1 O8 O 0.6310(6) 0.7455(10) 0.0532(5) 0.066(3) Uani 0.511(16) 1 d PD A 1 O9 O 0.7957(7) 0.6929(8) -0.0177(4) 0.064(2) Uani 0.511(16) 1 d PD A 1 O10 O 0.821(2) 0.8690(12) 0.0034(9) 0.220(11) Uani 0.511(16) 1 d PD A 1 O11 O 0.8170(12) 0.7037(8) 0.0985(5) 0.071(3) Uani 0.511(16) 1 d PD A 1 Cl2' Cl 0.7785(8) 0.7485(6) 0.0394(4) 0.097(2) Uani 0.489(16) 1 d PD A 2 O8' O 0.6526(17) 0.7160(17) 0.0345(11) 0.185(10) Uani 0.489(16) 1 d PD A 2 O9' O 0.860(2) 0.6823(12) 0.0060(14) 0.229(12) Uani 0.489(16) 1 d PD A 2 O10' O 0.7994(6) 0.8771(5) 0.0097(5) 0.051(2) Uani 0.489(16) 1 d PD A 2 O11' O 0.7770(19) 0.7146(17) 0.1140(7) 0.152(9) Uani 0.489(16) 1 d PD A 2 O12 O 0.9162(8) 0.0673(7) 0.0157(5) 0.058(3) Uani 0.320(8) 1 d PD . . H1O H 0.996(2) 0.075(10) 0.011(8) 0.070 Uiso 0.320(8) 1 d PD . . H2O H 0.899(10) -0.004(4) 0.017(8) 0.070 Uiso 0.320(8) 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0347(2) 0.0253(2) 0.0341(2) -0.01127(18) 0.00137(17) -0.00579(17) Mn2 0.0292(2) 0.0259(2) 0.0333(2) -0.01081(17) -0.00103(16) -0.00481(16) O1 0.0372(10) 0.0312(11) 0.0417(11) -0.0100(9) -0.0042(8) -0.0078(8) O2 0.0387(10) 0.0259(10) 0.0453(11) -0.0107(9) -0.0053(9) -0.0039(8) O3 0.0343(10) 0.0324(11) 0.0363(10) -0.0125(8) -0.0026(8) -0.0051(8) N1 0.0337(11) 0.0284(12) 0.0363(12) -0.0144(10) 0.0000(9) -0.0030(9) N2 0.0419(13) 0.0338(13) 0.0356(12) -0.0131(10) 0.0035(10) -0.0105(10) N3 0.0371(12) 0.0292(12) 0.0348(12) -0.0101(10) 0.0007(9) -0.0027(10) N4 0.0446(13) 0.0293(13) 0.0371(13) -0.0125(10) 0.0059(10) -0.0072(10) N5 0.0431(13) 0.0290(13) 0.0362(12) -0.0119(10) 0.0067(10) -0.0047(10) N6 0.0264(11) 0.0323(13) 0.0357(12) -0.0123(10) -0.0013(9) -0.0013(9) N7 0.0293(11) 0.0300(12) 0.0380(12) -0.0110(10) -0.0014(9) -0.0033(9) N8 0.0360(12) 0.0283(12) 0.0362(12) -0.0132(10) 0.0003(9) -0.0026(9) N9 0.0408(14) 0.0364(15) 0.0542(16) -0.0147(12) 0.0043(12) -0.0019(11) C1 0.0287(13) 0.0329(15) 0.0419(15) -0.0174(12) 0.0023(11) -0.0074(11) C2 0.0349(14) 0.0344(16) 0.0510(17) -0.0182(14) 0.0043(13) -0.0055(12) C3 0.0413(16) 0.0384(18) 0.068(2) -0.0305(17) 0.0039(15) -0.0080(14) C4 0.0387(16) 0.053(2) 0.071(2) -0.0373(19) -0.0071(15) -0.0057(15) C5 0.0339(15) 0.051(2) 0.0576(19) -0.0296(16) -0.0078(13) -0.0017(13) C6 0.0280(13) 0.0362(16) 0.0432(15) -0.0193(13) -0.0017(11) -0.0015(11) C7 0.0280(13) 0.0394(16) 0.0371(14) -0.0164(12) -0.0017(11) -0.0021(11) C8 0.0406(16) 0.0451(19) 0.0520(18) -0.0175(15) -0.0122(14) 0.0014(13) C9 0.0366(15) 0.0455(18) 0.0415(16) -0.0145(14) -0.0007(12) -0.0101(13) C10 0.0392(15) 0.0288(15) 0.0394(15) -0.0097(12) 0.0019(12) -0.0047(12) C11 0.0398(16) 0.0450(19) 0.0442(17) -0.0123(14) -0.0004(13) -0.0006(13) C12 0.0472(18) 0.049(2) 0.0453(18) -0.0146(15) 0.0066(14) 0.0044(15) C13 0.0579(19) 0.0353(17) 0.0360(15) -0.0138(13) 0.0019(13) 0.0043(14) C14 0.0476(16) 0.0260(14) 0.0373(15) -0.0095(12) -0.0024(12) -0.0012(12) C15 0.0504(18) 0.0431(18) 0.0360(15) -0.0159(13) 0.0003(13) -0.0161(14) C16 0.0526(18) 0.0283(15) 0.0341(14) -0.0089(12) 0.0056(13) -0.0107(13) C17 0.069(2) 0.0323(16) 0.0352(15) -0.0129(13) 0.0041(14) -0.0122(15) C18 0.073(2) 0.0342(17) 0.0396(17) -0.0126(14) 0.0128(16) 0.0027(16) C19 0.0561(19) 0.0365(18) 0.0441(17) -0.0083(14) 0.0077(15) 0.0051(14) C20 0.0466(17) 0.0316(16) 0.0407(16) -0.0082(13) 0.0068(13) -0.0033(13) C21 0.0517(18) 0.0320(16) 0.0414(16) -0.0134(13) 0.0055(13) -0.0148(13) C22 0.0463(16) 0.0286(15) 0.0375(15) -0.0134(12) 0.0118(12) -0.0047(12) C23 0.060(2) 0.0306(17) 0.057(2) -0.0135(15) 0.0142(16) -0.0060(15) C24 0.066(2) 0.0306(17) 0.056(2) -0.0070(15) 0.0108(17) 0.0035(16) C25 0.0549(19) 0.0363(18) 0.0481(18) -0.0096(14) 0.0073(15) 0.0078(14) C26 0.0456(16) 0.0360(17) 0.0409(16) -0.0147(13) 0.0050(13) 0.0006(13) C27 0.0316(14) 0.0465(18) 0.0383(15) -0.0186(13) -0.0041(11) -0.0003(12) C28 0.0311(13) 0.0364(16) 0.0371(14) -0.0128(12) -0.0049(11) -0.0020(11) C29 0.0387(16) 0.051(2) 0.0397(16) -0.0135(14) -0.0035(12) 0.0002(14) C30 0.0386(16) 0.061(2) 0.0377(16) -0.0153(15) 0.0036(12) -0.0054(15) C31 0.0340(14) 0.0441(18) 0.0467(17) -0.0177(14) 0.0041(12) -0.0010(13) C32 0.0321(14) 0.0337(16) 0.0465(16) -0.0148(13) 0.0009(12) -0.0010(11) C33 0.0288(13) 0.0355(16) 0.0422(15) -0.0138(13) 0.0023(11) -0.0038(11) C34 0.0349(14) 0.0278(14) 0.0413(15) -0.0107(12) 0.0019(11) -0.0033(11) C35 0.0379(15) 0.0407(18) 0.0480(17) -0.0146(14) 0.0044(13) -0.0015(13) C36 0.0510(18) 0.0411(18) 0.0425(17) -0.0156(14) 0.0109(14) -0.0007(14) C37 0.0588(19) 0.0284(15) 0.0365(15) -0.0130(12) 0.0034(13) -0.0047(13) C38 0.0483(16) 0.0265(14) 0.0362(14) -0.0112(12) -0.0024(12) -0.0028(12) C39 0.0338(14) 0.0344(16) 0.0401(15) -0.0084(12) -0.0007(11) -0.0043(12) C40 0.0349(14) 0.0342(16) 0.0442(16) -0.0087(13) 0.0004(12) -0.0051(12) C41 0.055(2) 0.053(2) 0.0450(18) -0.0071(16) -0.0072(15) 0.0052(16) C42 0.073(3) 0.068(3) 0.070(3) -0.005(2) -0.024(2) 0.018(2) C43 0.053(2) 0.054(2) 0.104(4) -0.017(2) -0.028(2) 0.0135(18) C44 0.0369(17) 0.043(2) 0.088(3) -0.0218(19) 0.0037(17) 0.0000(14) Cl1 0.0375(4) 0.0457(4) 0.0578(5) -0.0227(4) -0.0101(3) 0.0011(3) O4 0.0575(16) 0.109(3) 0.0575(16) -0.0389(17) -0.0012(13) 0.0137(16) O5 0.0479(14) 0.134(3) 0.0547(15) -0.0480(18) -0.0182(12) 0.0107(16) O6 0.104(3) 0.0475(18) 0.212(5) -0.036(2) -0.094(3) 0.0063(18) O7 0.0408(12) 0.0820(19) 0.0554(14) -0.0154(13) -0.0111(11) -0.0131(12) Cl2 0.0359(15) 0.0342(17) 0.0402(18) -0.0175(13) 0.0043(10) -0.0032(11) O8 0.037(4) 0.089(6) 0.052(4) 0.005(3) 0.013(3) -0.003(3) O9 0.058(4) 0.083(5) 0.060(4) -0.043(3) -0.003(3) -0.006(3) O10 0.34(2) 0.160(14) 0.120(11) 0.000(10) 0.001(12) -0.183(16) O11 0.096(6) 0.056(4) 0.075(6) -0.010(4) -0.061(6) -0.009(4) Cl2' 0.130(5) 0.082(4) 0.074(4) -0.017(3) -0.010(3) -0.051(3) O8' 0.239(18) 0.137(13) 0.174(14) 0.054(10) -0.160(14) -0.106(13) O9' 0.209(18) 0.104(9) 0.30(2) -0.077(13) 0.185(17) -0.011(11) O10' 0.038(3) 0.030(4) 0.079(5) -0.008(3) -0.003(3) 0.007(3) O11' 0.165(15) 0.200(17) 0.078(7) -0.020(8) -0.009(8) -0.122(12) O12 0.063(5) 0.048(5) 0.057(5) -0.002(4) -0.014(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Mn2 3.1136(6) . ? Mn1 O2 1.905(2) . ? Mn1 O3 1.788(2) . ? Mn1 N2 2.166(2) . ? Mn1 N3 2.242(2) . ? Mn1 N4 2.260(2) . ? Mn1 N5 2.058(3) . ? Mn2 O1 1.8726(19) . ? Mn2 O3 1.8179(19) . ? Mn2 N1 2.034(3) . ? Mn2 N6 2.245(2) . ? Mn2 N7 2.214(2) . ? Mn2 N8 2.282(2) . ? O1 C1 1.331(3) . ? O2 N1 1.376(3) . ? N1 C7 1.299(4) . ? N2 C9 1.482(4) . ? N2 C15 1.478(4) . ? N2 C21 1.494(4) . ? N3 C10 1.342(4) . ? N3 C14 1.344(4) . ? N4 C16 1.346(4) . ? N4 C20 1.341(4) . ? N5 C22 1.351(4) . ? N5 C26 1.349(4) . ? N6 C27 1.472(4) . ? N6 C33 1.486(3) . ? N6 C39 1.495(4) . ? N7 C28 1.344(4) . ? N7 C32 1.341(4) . ? N8 C34 1.341(4) . ? N8 C38 1.340(4) . ? N9 C40 1.344(4) . ? N9 C44 1.348(5) . ? C1 C2 1.408(4) . ? C1 C6 1.406(4) . ? C2 H2 0.950 . ? C2 C3 1.380(5) . ? C3 H3 0.950 . ? C3 C4 1.379(5) . ? C4 H4 0.950 . ? C4 C5 1.383(5) . ? C5 H5 0.950 . ? C5 C6 1.407(4) . ? C6 C7 1.476(4) . ? C7 C8 1.483(4) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.500(4) . ? C10 C11 1.381(4) . ? C11 H11 0.950 . ? C11 C12 1.382(5) . ? C12 H12 0.950 . ? C12 C13 1.385(5) . ? C13 H13 0.950 . ? C13 C14 1.382(4) . ? C14 H14 0.950 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.512(5) . ? C16 C17 1.381(4) . ? C17 H17 0.950 . ? C17 C18 1.393(5) . ? C18 H18 0.950 . ? C18 C19 1.382(5) . ? C19 H19 0.950 . ? C19 C20 1.385(4) . ? C20 H20 0.950 . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C21 C22 1.501(5) . ? C22 C23 1.380(5) . ? C23 H23 0.950 . ? C23 C24 1.371(6) . ? C24 H24 0.950 . ? C24 C25 1.391(5) . ? C25 H25 0.950 . ? C25 C26 1.369(5) . ? C26 H26 0.950 . ? C27 H27A 0.990 . ? C27 H27B 0.990 . ? C27 C28 1.517(4) . ? C28 C29 1.379(4) . ? C29 H29 0.950 . ? C29 C30 1.388(4) . ? C30 H30 0.950 . ? C30 C31 1.374(5) . ? C31 H31 0.950 . ? C31 C32 1.381(4) . ? C32 H32 0.950 . ? C33 H33A 0.990 . ? C33 H33B 0.990 . ? C33 C34 1.500(4) . ? C34 C35 1.386(4) . ? C35 H35 0.950 . ? C35 C36 1.385(5) . ? C36 H36 0.950 . ? C36 C37 1.370(5) . ? C37 H37 0.950 . ? C37 C38 1.379(4) . ? C38 H38 0.950 . ? C39 H39A 0.990 . ? C39 H39B 0.990 . ? C39 C40 1.507(4) . ? C40 C41 1.378(5) . ? C41 H41 0.950 . ? C41 C42 1.378(5) . ? C42 H42 0.950 . ? C42 C43 1.344(6) . ? C43 H43 0.950 . ? C43 C44 1.382(6) . ? C44 H44 0.950 . ? Cl1 O4 1.413(3) . ? Cl1 O5 1.439(3) . ? Cl1 O6 1.407(3) . ? Cl1 O7 1.434(2) . ? Cl2 O8 1.424(6) . ? Cl2 O9 1.409(7) . ? Cl2 O10 1.420(10) . ? Cl2 O11 1.387(6) . ? Cl2' O8' 1.427(11) . ? Cl2' O9' 1.353(10) . ? Cl2' O10' 1.459(8) . ? Cl2' O11' 1.402(11) . ? O12 H1O 0.840(10) . ? O12 H2O 0.840(10) . ? 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 Mn2 Mn1 O2 65.32(6) . . ? Mn2 Mn1 O3 30.56(6) . . ? Mn2 Mn1 N2 123.18(7) . . ? Mn2 Mn1 N3 100.60(6) . . ? Mn2 Mn1 N4 99.17(6) . . ? Mn2 Mn1 N5 154.99(7) . . ? O2 Mn1 O3 95.87(9) . . ? O2 Mn1 N2 169.60(10) . . ? O2 Mn1 N3 109.92(9) . . ? O2 Mn1 N4 97.62(9) . . ? O2 Mn1 N5 89.69(9) . . ? O3 Mn1 N2 92.70(9) . . ? O3 Mn1 N3 91.60(9) . . ? O3 Mn1 N4 94.72(9) . . ? O3 Mn1 N5 174.05(10) . . ? N2 Mn1 N3 75.62(9) . . ? N2 Mn1 N4 75.77(9) . . ? N2 Mn1 N5 81.55(10) . . ? N3 Mn1 N4 150.94(9) . . ? N3 Mn1 N5 88.49(9) . . ? N4 Mn1 N5 82.40(9) . . ? Mn1 Mn2 O1 149.14(7) . . ? Mn1 Mn2 O3 30.00(7) . . ? Mn1 Mn2 N1 61.93(7) . . ? Mn1 Mn2 N6 119.26(6) . . ? Mn1 Mn2 N7 101.65(6) . . ? Mn1 Mn2 N8 93.14(6) . . ? O1 Mn2 O3 174.51(9) . . ? O1 Mn2 N1 88.06(9) . . ? O1 Mn2 N6 91.58(9) . . ? O1 Mn2 N7 85.02(9) . . ? O1 Mn2 N8 94.98(9) . . ? O3 Mn2 N1 91.87(9) . . ? O3 Mn2 N6 89.83(9) . . ? O3 Mn2 N7 90.13(9) . . ? O3 Mn2 N8 90.52(8) . . ? N1 Mn2 N6 165.83(9) . . ? N1 Mn2 N7 117.05(9) . . ? N1 Mn2 N8 91.88(9) . . ? N6 Mn2 N7 77.00(9) . . ? N6 Mn2 N8 74.04(9) . . ? N7 Mn2 N8 151.03(9) . . ? Mn2 O1 C1 127.85(19) . . ? Mn1 O2 N1 116.68(16) . . ? Mn1 O3 Mn2 119.44(11) . . ? Mn2 N1 O2 114.75(16) . . ? Mn2 N1 C7 129.7(2) . . ? O2 N1 C7 115.3(2) . . ? Mn1 N2 C9 107.40(17) . . ? Mn1 N2 C15 106.93(17) . . ? Mn1 N2 C21 109.43(19) . . ? C9 N2 C15 110.4(3) . . ? C9 N2 C21 110.2(2) . . ? C15 N2 C21 112.3(2) . . ? Mn1 N3 C10 113.08(19) . . ? Mn1 N3 C14 127.8(2) . . ? C10 N3 C14 118.8(3) . . ? Mn1 N4 C16 113.42(19) . . ? Mn1 N4 C20 127.2(2) . . ? C16 N4 C20 119.1(3) . . ? Mn1 N5 C22 116.1(2) . . ? Mn1 N5 C26 124.9(2) . . ? C22 N5 C26 118.8(3) . . ? Mn2 N6 C27 106.36(17) . . ? Mn2 N6 C33 104.16(17) . . ? Mn2 N6 C39 111.42(16) . . ? C27 N6 C33 111.4(2) . . ? C27 N6 C39 111.7(2) . . ? C33 N6 C39 111.5(2) . . ? Mn2 N7 C28 114.61(18) . . ? Mn2 N7 C32 126.0(2) . . ? C28 N7 C32 118.7(3) . . ? Mn2 N8 C34 113.05(19) . . ? Mn2 N8 C38 128.5(2) . . ? C34 N8 C38 118.1(3) . . ? C40 N9 C44 116.7(3) . . ? O1 C1 C2 117.2(3) . . ? O1 C1 C6 123.3(3) . . ? C2 C1 C6 119.5(3) . . ? C1 C2 H2 119.6 . . ? C1 C2 C3 120.8(3) . . ? H2 C2 C3 119.6 . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 120.4(3) . . ? H3 C3 C4 119.8 . . ? C3 C4 H4 120.2 . . ? C3 C4 C5 119.6(3) . . ? H4 C4 C5 120.2 . . ? C4 C5 H5 119.1 . . ? C4 C5 C6 121.9(3) . . ? H5 C5 C6 119.1 . . ? C1 C6 C5 118.0(3) . . ? C1 C6 C7 123.0(3) . . ? C5 C6 C7 119.0(3) . . ? N1 C7 C6 119.3(3) . . ? N1 C7 C8 119.6(3) . . ? C6 C7 C8 121.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 H9A 109.4 . . ? N2 C9 H9B 109.4 . . ? N2 C9 C10 111.0(3) . . ? H9A C9 H9B 108.0 . . ? H9A C9 C10 109.4 . . ? H9B C9 C10 109.4 . . ? N3 C10 C9 116.1(2) . . ? N3 C10 C11 121.9(3) . . ? C9 C10 C11 121.9(3) . . ? C10 C11 H11 120.4 . . ? C10 C11 C12 119.2(3) . . ? H11 C11 C12 120.4 . . ? C11 C12 H12 120.5 . . ? C11 C12 C13 118.9(3) . . ? H12 C12 C13 120.5 . . ? C12 C13 H13 120.6 . . ? C12 C13 C14 118.8(3) . . ? H13 C13 C14 120.6 . . ? N3 C14 C13 122.2(3) . . ? N3 C14 H14 118.9 . . ? C13 C14 H14 118.9 . . ? N2 C15 H15A 109.6 . . ? N2 C15 H15B 109.6 . . ? N2 C15 C16 110.4(3) . . ? H15A C15 H15B 108.1 . . ? H15A C15 C16 109.6 . . ? H15B C15 C16 109.6 . . ? N4 C16 C15 114.2(3) . . ? N4 C16 C17 122.2(3) . . ? C15 C16 C17 123.5(3) . . ? C16 C17 H17 120.8 . . ? C16 C17 C18 118.4(3) . . ? H17 C17 C18 120.8 . . ? C17 C18 H18 120.3 . . ? C17 C18 C19 119.4(3) . . ? H18 C18 C19 120.3 . . ? C18 C19 H19 120.6 . . ? C18 C19 C20 118.8(3) . . ? H19 C19 C20 120.6 . . ? N4 C20 C19 122.1(3) . . ? N4 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? N2 C21 H21A 108.8 . . ? N2 C21 H21B 108.8 . . ? N2 C21 C22 114.0(2) . . ? H21A C21 H21B 107.6 . . ? H21A C21 C22 108.8 . . ? H21B C21 C22 108.8 . . ? N5 C22 C21 118.1(3) . . ? N5 C22 C23 121.1(3) . . ? C21 C22 C23 120.8(3) . . ? C22 C23 H23 120.1 . . ? C22 C23 C24 119.8(3) . . ? H23 C23 C24 120.1 . . ? C23 C24 H24 120.4 . . ? C23 C24 C25 119.1(3) . . ? H24 C24 C25 120.4 . . ? C24 C25 H25 120.7 . . ? C24 C25 C26 118.6(4) . . ? H25 C25 C26 120.7 . . ? N5 C26 C25 122.4(3) . . ? N5 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? N6 C27 H27A 109.3 . . ? N6 C27 H27B 109.3 . . ? N6 C27 C28 111.5(2) . . ? H27A C27 H27B 108.0 . . ? H27A C27 C28 109.3 . . ? H27B C27 C28 109.3 . . ? N7 C28 C27 114.9(2) . . ? N7 C28 C29 121.9(3) . . ? C27 C28 C29 123.1(3) . . ? C28 C29 H29 120.5 . . ? C28 C29 C30 119.1(3) . . ? H29 C29 C30 120.5 . . ? C29 C30 H30 120.6 . . ? C29 C30 C31 118.9(3) . . ? H30 C30 C31 120.6 . . ? C30 C31 H31 120.4 . . ? C30 C31 C32 119.1(3) . . ? H31 C31 C32 120.4 . . ? N7 C32 C31 122.2(3) . . ? N7 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? N6 C33 H33A 109.5 . . ? N6 C33 H33B 109.5 . . ? N6 C33 C34 110.9(2) . . ? H33A C33 H33B 108.0 . . ? H33A C33 C34 109.5 . . ? H33B C33 C34 109.5 . . ? N8 C34 C33 115.7(2) . . ? N8 C34 C35 122.0(3) . . ? C33 C34 C35 122.2(3) . . ? C34 C35 H35 120.5 . . ? C34 C35 C36 119.0(3) . . ? H35 C35 C36 120.5 . . ? C35 C36 H36 120.5 . . ? C35 C36 C37 119.0(3) . . ? H36 C36 C37 120.5 . . ? C36 C37 H37 120.5 . . ? C36 C37 C38 119.0(3) . . ? H37 C37 C38 120.5 . . ? N8 C38 C37 122.8(3) . . ? N8 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? N6 C39 H39A 108.6 . . ? N6 C39 H39B 108.6 . . ? N6 C39 C40 114.7(2) . . ? H39A C39 H39B 107.6 . . ? H39A C39 C40 108.6 . . ? H39B C39 C40 108.6 . . ? N9 C40 C39 115.1(3) . . ? N9 C40 C41 122.6(3) . . ? C39 C40 C41 122.3(3) . . ? C40 C41 H41 120.5 . . ? C40 C41 C42 119.0(4) . . ? H41 C41 C42 120.5 . . ? C41 C42 H42 120.2 . . ? C41 C42 C43 119.5(4) . . ? H42 C42 C43 120.2 . . ? C42 C43 H43 120.5 . . ? C42 C43 C44 119.0(4) . . ? H43 C43 C44 120.5 . . ? N9 C44 C43 123.1(4) . . ? N9 C44 H44 118.4 . . ? C43 C44 H44 118.4 . . ? O4 Cl1 O5 107.62(17) . . ? O4 Cl1 O6 110.8(3) . . ? O4 Cl1 O7 109.48(18) . . ? O5 Cl1 O6 109.6(2) . . ? O5 Cl1 O7 109.90(17) . . ? O6 Cl1 O7 109.40(19) . . ? O8 Cl2 O9 103.4(5) . . ? O8 Cl2 O10 115.1(10) . . ? O8 Cl2 O11 111.1(7) . . ? O9 Cl2 O10 103.2(8) . . ? O9 Cl2 O11 114.4(6) . . ? O10 Cl2 O11 109.4(9) . . ? O8' Cl2' O9' 108.1(11) . . ? O8' Cl2' O10' 108.8(8) . . ? O8' Cl2' O11' 102.9(10) . . ? O9' Cl2' O10' 114.6(8) . . ? O9' Cl2' O11' 110.2(12) . . ? O10' Cl2' O11' 111.5(9) . . ? H1O O12 H2O 107(3) . . ? 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 O2 Mn1 Mn2 O1 -8.67(14) . . . . ? O2 Mn1 Mn2 O3 -177.94(14) . . . . ? O2 Mn1 Mn2 N1 6.01(10) . . . . ? O2 Mn1 Mn2 N6 169.91(10) . . . . ? O2 Mn1 Mn2 N7 -108.59(9) . . . . ? O2 Mn1 Mn2 N8 96.47(9) . . . . ? O3 Mn1 Mn2 O1 169.27(18) . . . . ? O3 Mn1 Mn2 N1 -176.05(14) . . . . ? O3 Mn1 Mn2 N6 -12.15(14) . . . . ? O3 Mn1 Mn2 N7 69.36(14) . . . . ? O3 Mn1 Mn2 N8 -85.59(14) . . . . ? N2 Mn1 Mn2 O1 164.49(15) . . . . ? N2 Mn1 Mn2 O3 -4.79(14) . . . . ? N2 Mn1 Mn2 N1 179.17(11) . . . . ? N2 Mn1 Mn2 N6 -16.93(10) . . . . ? N2 Mn1 Mn2 N7 64.57(10) . . . . ? N2 Mn1 Mn2 N8 -90.38(10) . . . . ? N3 Mn1 Mn2 O1 -115.85(14) . . . . ? N3 Mn1 Mn2 O3 74.87(14) . . . . ? N3 Mn1 Mn2 N1 -101.17(10) . . . . ? N3 Mn1 Mn2 N6 62.72(9) . . . . ? N3 Mn1 Mn2 N7 144.23(9) . . . . ? N3 Mn1 Mn2 N8 -10.72(9) . . . . ? N4 Mn1 Mn2 O1 85.55(15) . . . . ? N4 Mn1 Mn2 O3 -83.72(14) . . . . ? N4 Mn1 Mn2 N1 100.23(10) . . . . ? N4 Mn1 Mn2 N6 -95.87(10) . . . . ? N4 Mn1 Mn2 N7 -14.37(9) . . . . ? N4 Mn1 Mn2 N8 -169.31(9) . . . . ? N5 Mn1 Mn2 O1 -6.1(2) . . . . ? N5 Mn1 Mn2 O3 -175.4(2) . . . . ? N5 Mn1 Mn2 N1 8.57(17) . . . . ? N5 Mn1 Mn2 N6 172.47(17) . . . . ? N5 Mn1 Mn2 N7 -106.03(17) . . . . ? N5 Mn1 Mn2 N8 99.02(17) . . . . ? Mn1 Mn2 O1 C1 43.4(3) . . . . ? O3 Mn2 O1 C1 119.8(10) . . . . ? N1 Mn2 O1 C1 30.5(2) . . . . ? N6 Mn2 O1 C1 -135.3(2) . . . . ? N7 Mn2 O1 C1 147.9(2) . . . . ? N8 Mn2 O1 C1 -61.2(2) . . . . ? Mn2 Mn1 O2 N1 -8.79(15) . . . . ? O3 Mn1 O2 N1 -9.85(18) . . . . ? N2 Mn1 O2 N1 -155.2(4) . . . . ? N3 Mn1 O2 N1 84.01(18) . . . . ? N4 Mn1 O2 N1 -105.43(18) . . . . ? N5 Mn1 O2 N1 172.29(18) . . . . ? O2 Mn1 O3 Mn2 1.88(13) . . . . ? N2 Mn1 O3 Mn2 175.99(12) . . . . ? N3 Mn1 O3 Mn2 -108.33(12) . . . . ? N4 Mn1 O3 Mn2 100.05(12) . . . . ? N5 Mn1 O3 Mn2 160.9(8) . . . . ? O1 Mn2 O3 Mn1 -85.7(10) . . . . ? N1 Mn2 O3 Mn1 3.49(13) . . . . ? N6 Mn2 O3 Mn1 169.42(12) . . . . ? N7 Mn2 O3 Mn1 -113.58(12) . . . . ? N8 Mn2 O3 Mn1 95.39(12) . . . . ? Mn1 O2 N1 Mn2 13.5(2) . . . . ? Mn1 O2 N1 C7 -171.48(19) . . . . ? Mn1 Mn2 N1 O2 -8.34(14) . . . . ? Mn1 Mn2 N1 C7 177.6(3) . . . . ? O1 Mn2 N1 O2 164.19(18) . . . . ? O1 Mn2 N1 C7 -9.9(2) . . . . ? O3 Mn2 N1 O2 -10.32(18) . . . . ? O3 Mn2 N1 C7 175.6(2) . . . . ? N6 Mn2 N1 O2 -107.0(4) . . . . ? N6 Mn2 N1 C7 78.9(4) . . . . ? N7 Mn2 N1 O2 80.78(18) . . . . ? N7 Mn2 N1 C7 -93.3(3) . . . . ? N8 Mn2 N1 O2 -100.90(17) . . . . ? N8 Mn2 N1 C7 85.0(2) . . . . ? Mn2 Mn1 N2 C9 59.7(2) . . . . ? Mn2 Mn1 N2 C15 -58.8(2) . . . . ? Mn2 Mn1 N2 C21 179.29(15) . . . . ? O2 Mn1 N2 C9 -157.2(4) . . . . ? O2 Mn1 N2 C15 84.3(5) . . . . ? O2 Mn1 N2 C21 -37.6(6) . . . . ? O3 Mn1 N2 C9 57.22(19) . . . . ? O3 Mn1 N2 C15 -61.2(2) . . . . ? O3 Mn1 N2 C21 176.86(18) . . . . ? N3 Mn1 N2 C9 -33.75(18) . . . . ? N3 Mn1 N2 C15 -152.2(2) . . . . ? N3 Mn1 N2 C21 85.90(19) . . . . ? N4 Mn1 N2 C9 151.4(2) . . . . ? N4 Mn1 N2 C15 33.0(2) . . . . ? N4 Mn1 N2 C21 -88.95(19) . . . . ? N5 Mn1 N2 C9 -124.4(2) . . . . ? N5 Mn1 N2 C15 117.2(2) . . . . ? N5 Mn1 N2 C21 -4.71(18) . . . . ? Mn2 Mn1 N3 C10 -101.5(2) . . . . ? Mn2 Mn1 N3 C14 71.9(2) . . . . ? O2 Mn1 N3 C10 -169.0(2) . . . . ? O2 Mn1 N3 C14 4.5(3) . . . . ? O3 Mn1 N3 C10 -72.1(2) . . . . ? O3 Mn1 N3 C14 101.4(2) . . . . ? N2 Mn1 N3 C10 20.3(2) . . . . ? N2 Mn1 N3 C14 -166.3(3) . . . . ? N4 Mn1 N3 C10 30.6(3) . . . . ? N4 Mn1 N3 C14 -155.9(2) . . . . ? N5 Mn1 N3 C10 101.9(2) . . . . ? N5 Mn1 N3 C14 -84.6(3) . . . . ? Mn2 Mn1 N4 C16 107.6(2) . . . . ? Mn2 Mn1 N4 C20 -78.6(2) . . . . ? O2 Mn1 N4 C16 173.7(2) . . . . ? O2 Mn1 N4 C20 -12.4(3) . . . . ? O3 Mn1 N4 C16 77.1(2) . . . . ? O3 Mn1 N4 C20 -109.0(3) . . . . ? N2 Mn1 N4 C16 -14.4(2) . . . . ? N2 Mn1 N4 C20 159.4(3) . . . . ? N3 Mn1 N4 C16 -24.8(3) . . . . ? N3 Mn1 N4 C20 149.1(2) . . . . ? N5 Mn1 N4 C16 -97.6(2) . . . . ? N5 Mn1 N4 C20 76.2(3) . . . . ? Mn2 Mn1 N5 C22 171.08(14) . . . . ? Mn2 Mn1 N5 C26 -3.5(3) . . . . ? O2 Mn1 N5 C22 173.4(2) . . . . ? O2 Mn1 N5 C26 -1.2(2) . . . . ? O3 Mn1 N5 C22 14.3(10) . . . . ? O3 Mn1 N5 C26 -160.3(8) . . . . ? N2 Mn1 N5 C22 -1.0(2) . . . . ? N2 Mn1 N5 C26 -175.5(2) . . . . ? N3 Mn1 N5 C22 -76.7(2) . . . . ? N3 Mn1 N5 C26 108.8(2) . . . . ? N4 Mn1 N5 C22 75.7(2) . . . . ? N4 Mn1 N5 C26 -98.9(2) . . . . ? Mn1 Mn2 N6 C27 70.61(17) . . . . ? Mn1 Mn2 N6 C33 -47.13(18) . . . . ? Mn1 Mn2 N6 C39 -167.42(15) . . . . ? O1 Mn2 N6 C27 -110.12(18) . . . . ? O1 Mn2 N6 C33 132.14(17) . . . . ? O1 Mn2 N6 C39 11.85(18) . . . . ? O3 Mn2 N6 C27 64.57(17) . . . . ? O3 Mn2 N6 C33 -53.17(17) . . . . ? O3 Mn2 N6 C39 -173.46(18) . . . . ? N1 Mn2 N6 C27 161.5(3) . . . . ? N1 Mn2 N6 C33 43.8(4) . . . . ? N1 Mn2 N6 C39 -76.5(4) . . . . ? N7 Mn2 N6 C27 -25.60(17) . . . . ? N7 Mn2 N6 C33 -143.34(18) . . . . ? N7 Mn2 N6 C39 96.37(18) . . . . ? N8 Mn2 N6 C27 155.16(18) . . . . ? N8 Mn2 N6 C33 37.42(16) . . . . ? N8 Mn2 N6 C39 -82.87(18) . . . . ? Mn1 Mn2 N7 C28 -112.20(19) . . . . ? Mn1 Mn2 N7 C32 77.8(2) . . . . ? O1 Mn2 N7 C28 98.3(2) . . . . ? O1 Mn2 N7 C32 -71.7(2) . . . . ? O3 Mn2 N7 C28 -84.3(2) . . . . ? O3 Mn2 N7 C32 105.7(2) . . . . ? N1 Mn2 N7 C28 -176.47(18) . . . . ? N1 Mn2 N7 C32 13.5(3) . . . . ? N6 Mn2 N7 C28 5.49(19) . . . . ? N6 Mn2 N7 C32 -164.5(2) . . . . ? N8 Mn2 N7 C28 7.0(3) . . . . ? N8 Mn2 N7 C32 -163.0(2) . . . . ? Mn1 Mn2 N8 C34 97.14(19) . . . . ? Mn1 Mn2 N8 C38 -76.0(2) . . . . ? O1 Mn2 N8 C34 -112.7(2) . . . . ? O1 Mn2 N8 C38 74.2(2) . . . . ? O3 Mn2 N8 C34 67.2(2) . . . . ? O3 Mn2 N8 C38 -105.9(2) . . . . ? N1 Mn2 N8 C34 159.1(2) . . . . ? N1 Mn2 N8 C38 -14.0(2) . . . . ? N6 Mn2 N8 C34 -22.43(19) . . . . ? N6 Mn2 N8 C38 164.5(3) . . . . ? N7 Mn2 N8 C34 -24.0(3) . . . . ? N7 Mn2 N8 C38 162.9(2) . . . . ? Mn2 O1 C1 C2 151.7(2) . . . . ? Mn2 O1 C1 C6 -31.4(4) . . . . ? O1 C1 C2 C3 178.1(3) . . . . ? C6 C1 C2 C3 1.0(4) . . . . ? C1 C2 C3 C4 0.8(5) . . . . ? C2 C3 C4 C5 -1.4(5) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? O1 C1 C6 C5 -179.0(3) . . . . ? O1 C1 C6 C7 1.6(4) . . . . ? C2 C1 C6 C5 -2.2(4) . . . . ? C2 C1 C6 C7 178.5(3) . . . . ? C4 C5 C6 C1 1.6(5) . . . . ? C4 C5 C6 C7 -179.0(3) . . . . ? Mn2 N1 C7 C6 -10.0(4) . . . . ? Mn2 N1 C7 C8 170.6(2) . . . . ? O2 N1 C7 C6 176.0(2) . . . . ? O2 N1 C7 C8 -3.5(4) . . . . ? C1 C6 C7 N1 18.3(4) . . . . ? C1 C6 C7 C8 -162.3(3) . . . . ? C5 C6 C7 N1 -161.0(3) . . . . ? C5 C6 C7 C8 18.4(4) . . . . ? Mn1 N2 C9 C10 44.1(3) . . . . ? C15 N2 C9 C10 160.3(2) . . . . ? C21 N2 C9 C10 -75.1(3) . . . . ? Mn1 N3 C10 C9 -1.6(3) . . . . ? Mn1 N3 C10 C11 176.1(2) . . . . ? C14 N3 C10 C9 -175.7(3) . . . . ? C14 N3 C10 C11 1.9(4) . . . . ? N2 C9 C10 N3 -28.6(4) . . . . ? N2 C9 C10 C11 153.8(3) . . . . ? N3 C10 C11 C12 -3.6(5) . . . . ? C9 C10 C11 C12 173.9(3) . . . . ? C10 C11 C12 C13 2.2(5) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? Mn1 N3 C14 C13 -172.1(2) . . . . ? C10 N3 C14 C13 1.1(4) . . . . ? C12 C13 C14 N3 -2.3(5) . . . . ? Mn1 N2 C15 C16 -48.2(3) . . . . ? C9 N2 C15 C16 -164.7(2) . . . . ? C21 N2 C15 C16 71.9(3) . . . . ? Mn1 N4 C16 C15 -7.9(3) . . . . ? Mn1 N4 C16 C17 174.1(2) . . . . ? C20 N4 C16 C15 177.7(3) . . . . ? C20 N4 C16 C17 -0.3(5) . . . . ? N2 C15 C16 N4 37.8(4) . . . . ? N2 C15 C16 C17 -144.2(3) . . . . ? N4 C16 C17 C18 -0.1(5) . . . . ? C15 C16 C17 C18 -178.0(3) . . . . ? C16 C17 C18 C19 0.4(5) . . . . ? C17 C18 C19 C20 -0.3(5) . . . . ? Mn1 N4 C20 C19 -173.1(2) . . . . ? C16 N4 C20 C19 0.5(5) . . . . ? C18 C19 C20 N4 -0.2(5) . . . . ? Mn1 N2 C21 C22 9.3(3) . . . . ? C9 N2 C21 C22 127.2(3) . . . . ? C15 N2 C21 C22 -109.3(3) . . . . ? Mn1 N5 C22 C21 6.8(3) . . . . ? Mn1 N5 C22 C23 -175.2(2) . . . . ? C26 N5 C22 C21 -178.3(3) . . . . ? C26 N5 C22 C23 -0.3(4) . . . . ? N2 C21 C22 N5 -11.0(4) . . . . ? N2 C21 C22 C23 171.0(3) . . . . ? N5 C22 C23 C24 0.1(5) . . . . ? C21 C22 C23 C24 178.0(3) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? Mn1 N5 C26 C25 174.7(2) . . . . ? C22 N5 C26 C25 0.2(4) . . . . ? C24 C25 C26 N5 0.1(5) . . . . ? Mn2 N6 C27 C28 42.0(3) . . . . ? C33 N6 C27 C28 154.8(3) . . . . ? C39 N6 C27 C28 -79.8(3) . . . . ? Mn2 N7 C28 C27 16.3(3) . . . . ? Mn2 N7 C28 C29 -167.2(2) . . . . ? C32 N7 C28 C27 -172.8(3) . . . . ? C32 N7 C28 C29 3.6(4) . . . . ? N6 C27 C28 N7 -40.7(4) . . . . ? N6 C27 C28 C29 142.9(3) . . . . ? N7 C28 C29 C30 -4.0(5) . . . . ? C27 C28 C29 C30 172.2(3) . . . . ? C28 C29 C30 C31 1.1(5) . . . . ? C29 C30 C31 C32 1.9(5) . . . . ? Mn2 N7 C32 C31 169.3(2) . . . . ? C28 N7 C32 C31 -0.4(4) . . . . ? C30 C31 C32 N7 -2.4(5) . . . . ? Mn2 N6 C33 C34 -50.1(3) . . . . ? C27 N6 C33 C34 -164.4(2) . . . . ? C39 N6 C33 C34 70.1(3) . . . . ? Mn2 N8 C34 C33 1.2(3) . . . . ? Mn2 N8 C34 C35 -176.4(2) . . . . ? C38 N8 C34 C33 175.0(2) . . . . ? C38 N8 C34 C35 -2.5(4) . . . . ? N6 C33 C34 N8 34.0(4) . . . . ? N6 C33 C34 C35 -148.5(3) . . . . ? N8 C34 C35 C36 2.5(5) . . . . ? C33 C34 C35 C36 -174.8(3) . . . . ? C34 C35 C36 C37 -0.5(5) . . . . ? C35 C36 C37 C38 -1.5(5) . . . . ? Mn2 N8 C38 C37 173.2(2) . . . . ? C34 N8 C38 C37 0.4(4) . . . . ? C36 C37 C38 N8 1.6(5) . . . . ? Mn2 N6 C39 C40 170.2(2) . . . . ? C27 N6 C39 C40 -71.0(3) . . . . ? C33 N6 C39 C40 54.3(3) . . . . ? C44 N9 C40 C39 179.2(3) . . . . ? C44 N9 C40 C41 -0.3(5) . . . . ? N6 C39 C40 N9 -89.7(3) . . . . ? N6 C39 C40 C41 89.9(4) . . . . ? N9 C40 C41 C42 0.2(6) . . . . ? C39 C40 C41 C42 -179.3(4) . . . . ? C40 C41 C42 C43 -0.2(7) . . . . ? C41 C42 C43 C44 0.2(7) . . . . ? C40 N9 C44 C43 0.4(5) . . . . ? C42 C43 C44 N9 -0.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 73.93 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.969 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.067 _vrf_PLAT077_2-eb2176 ; PROBLEM: Unitcell contains non-integer number of atoms .. ? RESPONSE: Please see _refine_special_details for a discussion on the refinement of a partly occupied water molecule. ; _vrf_PLAT221_2-eb2176 ; PROBLEM: Large Solvent/Anion O Ueq(max)/Ueq(min) ... 4.5 Ratio RESPONSE: Please see _refine_special_details for a discussion on the refinement of a partly occupied water molecule. ; _vrf_PLAT029_2-eb2176 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.977 RESPONSE: Insignificant. ; _vrf_PLAT002_2-eb2176 ; PROBLEM: Number of Distance or Angle Restraints on AtSite 18 RESPONSE: Please see _refine_special_details for a discussion on the refinement of a disordered perchlorate anion. ; _database_code_depnum_ccdc_archive 'CCDC 950512' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3-eb2089 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H45 Mn2 N9 O3, 2(Cl O4)' _chemical_formula_sum 'C45 H45 Cl2 Mn2 N9 O11' _chemical_formula_weight 1068.68 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0368(4) _cell_length_b 11.5272(6) _cell_length_c 19.2934(10) _cell_angle_alpha 74.555(5) _cell_angle_beta 81.387(4) _cell_angle_gamma 84.794(4) _cell_volume 2335.92(19) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 6471 _cell_measurement_theta_min 2.9861 _cell_measurement_theta_max 23.2067 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.8619 _exptl_absorpt_correction_T_max 0.9496 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; Despite using a crystal of reasonable dimensions no diffraction was observed beyond a resolution of 0.9 \%A and so the data set was truncated at this resolution. H atoms were all placed geometrically. The two perchlorate ions were refined using a two part whole molecule disorder model, with occupancy ratios of 0.599:0.401(13) and 0.698:0.302(12) for the perchlorate ions containing Cl1 and Cl2 respectively. ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Agilent Technologies XCalibur' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1042 _diffrn_reflns_number 28621 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6699 _reflns_number_gt 5042 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2011)' _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2011)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2011)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and local programs' _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^)+(0.0282P)^2^+0.4651P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary charge-flipping _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6699 _refine_ls_number_parameters 715 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Mn1 Mn 0.26107(4) 0.84600(4) 0.20396(2) 0.02909(14) Uani 1 1 d . . . Mn2 Mn 0.22763(4) 0.57034(4) 0.26860(2) 0.03163(15) Uani 1 1 d . . . O1 O 0.35577(19) 0.97925(18) 0.18871(11) 0.0395(6) Uani 1 1 d . . . O2 O 0.37178(18) 0.62663(17) 0.28844(11) 0.0384(6) Uani 1 1 d . . . O3 O 0.17846(17) 0.71202(17) 0.21301(10) 0.0325(5) Uani 1 1 d . . . N1 N 0.3828(2) 0.7495(2) 0.26955(13) 0.0305(6) Uani 1 1 d . . . N2 N 0.1044(2) 0.9608(2) 0.15424(12) 0.0300(6) Uani 1 1 d . . . N3 N 0.3107(2) 0.8655(2) 0.08585(13) 0.0317(6) Uani 1 1 d . . . N4 N 0.1342(2) 0.8981(2) 0.29689(13) 0.0334(6) Uani 1 1 d . . . N5 N -0.0545(3) 1.2032(3) 0.17883(16) 0.0528(8) Uani 1 1 d . . . N6 N 0.0807(2) 0.4752(2) 0.24903(13) 0.0353(7) Uani 1 1 d . . . N7 N 0.0742(2) 0.5844(2) 0.35820(13) 0.0347(7) Uani 1 1 d . . . N8 N 0.3101(3) 0.4937(2) 0.17436(14) 0.0381(7) Uani 1 1 d . . . N9 N 0.2715(2) 0.4007(2) 0.33250(13) 0.0321(6) Uani 1 1 d . . . C1 C 0.4282(3) 1.0034(3) 0.23126(16) 0.0306(8) Uani 1 1 d . . . C2 C 0.4472(3) 1.1258(3) 0.22378(17) 0.0375(8) Uani 1 1 d . . . H2 H 0.4056 1.1865 0.1905 0.045 Uiso 1 1 calc R . . C3 C 0.5244(3) 1.1584(3) 0.26348(19) 0.0482(10) Uani 1 1 d . . . H3 H 0.5370 1.2413 0.2570 0.058 Uiso 1 1 calc R . . C4 C 0.5845(3) 1.0716(3) 0.3132(2) 0.0586(11) Uani 1 1 d . . . H4 H 0.6365 1.0946 0.3417 0.070 Uiso 1 1 calc R . . C5 C 0.5680(3) 0.9524(3) 0.32066(19) 0.0493(10) Uani 1 1 d . . . H5 H 0.6106 0.8933 0.3542 0.059 Uiso 1 1 calc R . . C6 C 0.4904(3) 0.9142(3) 0.28055(16) 0.0319(8) Uani 1 1 d . . . C7 C 0.4752(3) 0.7847(3) 0.29205(15) 0.0306(8) Uani 1 1 d . . . C8 C 0.5608(3) 0.6920(3) 0.33328(16) 0.0393(9) Uani 1 1 d . . . H8A H 0.6414 0.7267 0.3283 0.047 Uiso 1 1 calc R . . H8B H 0.5733 0.6219 0.3119 0.047 Uiso 1 1 calc R . . C9 C 0.5118(3) 0.6492(3) 0.41360(17) 0.0584(11) Uani 1 1 d . . . H9A H 0.5668 0.5842 0.4375 0.088 Uiso 1 1 calc R . . H9B H 0.4297 0.6194 0.4188 0.088 Uiso 1 1 calc R . . H9C H 0.5074 0.7165 0.4361 0.088 Uiso 1 1 calc R . . C10 C -0.0055(3) 0.9256(3) 0.20807(15) 0.0337(8) Uani 1 1 d . . . H10A H -0.0256 0.8429 0.2097 0.040 Uiso 1 1 calc R . . H10B H -0.0765 0.9809 0.1935 0.040 Uiso 1 1 calc R . . C11 C 0.0186(3) 0.9308(3) 0.28206(16) 0.0322(8) Uani 1 1 d . . . C12 C -0.0716(3) 0.9633(3) 0.33174(18) 0.0454(9) Uani 1 1 d . . . H12 H -0.1519 0.9879 0.3194 0.054 Uiso 1 1 calc R . . C13 C -0.0439(4) 0.9597(3) 0.39999(19) 0.0502(10) Uani 1 1 d . . . H13 H -0.1052 0.9807 0.4354 0.060 Uiso 1 1 calc R . . C14 C 0.0730(4) 0.9255(3) 0.41568(17) 0.0441(9) Uani 1 1 d . . . H14 H 0.0939 0.9215 0.4623 0.053 Uiso 1 1 calc R . . C15 C 0.1596(3) 0.8969(3) 0.36294(17) 0.0373(8) Uani 1 1 d . . . H15 H 0.2412 0.8754 0.3737 0.045 Uiso 1 1 calc R . . C16 C 0.1280(3) 1.0920(3) 0.14056(17) 0.0372(8) Uani 1 1 d . . . H16A H 0.1958 1.1121 0.1003 0.045 Uiso 1 1 calc R . . H16B H 0.1561 1.1043 0.1843 0.045 Uiso 1 1 calc R . . C17 C 0.0195(3) 1.1793(3) 0.12200(18) 0.0404(9) Uani 1 1 d . . . C18 C 0.0020(4) 1.2340(3) 0.0517(2) 0.0607(11) Uani 1 1 d . . . H18 H 0.0555 1.2149 0.0125 0.073 Uiso 1 1 calc R . . C19 C -0.0951(5) 1.3170(4) 0.0393(3) 0.0900(16) Uani 1 1 d . . . H19 H -0.1088 1.3564 -0.0090 0.108 Uiso 1 1 calc R . . C20 C -0.1702(4) 1.3427(4) 0.0951(3) 0.0876(16) Uani 1 1 d . . . H20 H -0.2372 1.4003 0.0870 0.105 Uiso 1 1 calc R . . C21 C -0.1484(4) 1.2841(4) 0.1641(3) 0.0666(12) Uani 1 1 d . . . H21 H -0.2027 1.3016 0.2036 0.080 Uiso 1 1 calc R . . C22 C 0.0962(3) 0.9274(3) 0.08655(15) 0.0354(8) Uani 1 1 d . . . H22A H 0.0451 0.9896 0.0561 0.043 Uiso 1 1 calc R . . H22B H 0.0562 0.8498 0.0981 0.043 Uiso 1 1 calc R . . C23 C 0.2220(3) 0.9158(3) 0.04499(16) 0.0327(8) Uani 1 1 d . . . C24 C 0.2455(3) 0.9514(3) -0.02983(17) 0.0469(9) Uani 1 1 d . . . H24 H 0.1819 0.9890 -0.0577 0.056 Uiso 1 1 calc R . . C25 C 0.3612(3) 0.9320(3) -0.06356(19) 0.0515(10) Uani 1 1 d . . . H25 H 0.3784 0.9550 -0.1150 0.062 Uiso 1 1 calc R . . C26 C 0.4513(3) 0.8791(3) -0.02219(19) 0.0459(9) Uani 1 1 d . . . H26 H 0.5320 0.8642 -0.0443 0.055 Uiso 1 1 calc R . . C27 C 0.4232(3) 0.8478(3) 0.05206(18) 0.0393(8) Uani 1 1 d . . . H27 H 0.4864 0.8121 0.0806 0.047 Uiso 1 1 calc R . . C28 C -0.0372(3) 0.5331(3) 0.27270(17) 0.0423(9) Uani 1 1 d . . . H28A H -0.1037 0.4779 0.2782 0.051 Uiso 1 1 calc R . . H28B H -0.0547 0.6073 0.2350 0.051 Uiso 1 1 calc R . . C29 C -0.0362(3) 0.5647(3) 0.34361(17) 0.0349(8) Uani 1 1 d . . . C30 C -0.1425(3) 0.5795(3) 0.38778(19) 0.0441(9) Uani 1 1 d . . . H30 H -0.2188 0.5606 0.3775 0.053 Uiso 1 1 calc R . . C31 C -0.1370(4) 0.6224(3) 0.44744(19) 0.0514(10) Uani 1 1 d . . . H31 H -0.2100 0.6365 0.4777 0.062 Uiso 1 1 calc R . . C32 C -0.0249(4) 0.6447(3) 0.46267(18) 0.0477(10) Uani 1 1 d . . . H32 H -0.0189 0.6747 0.5033 0.057 Uiso 1 1 calc R . . C33 C 0.0782(3) 0.6223(3) 0.41768(17) 0.0395(9) Uani 1 1 d . . . H33 H 0.1560 0.6342 0.4293 0.047 Uiso 1 1 calc R . . C34 C 0.0924(3) 0.3454(3) 0.29019(19) 0.0485(10) Uani 1 1 d . . . H34A H 0.0140 0.3237 0.3217 0.058 Uiso 1 1 calc R . . H34B H 0.1054 0.2950 0.2551 0.058 Uiso 1 1 calc R . . C35 C 0.1942(3) 0.3154(3) 0.33622(17) 0.0359(8) Uani 1 1 d . . . C36 C 0.2090(4) 0.2011(3) 0.3808(2) 0.0523(10) Uani 1 1 d . . . H36 H 0.1519 0.1422 0.3842 0.063 Uiso 1 1 calc R . . C37 C 0.3062(4) 0.1722(3) 0.4203(2) 0.0588(11) Uani 1 1 d . . . H37 H 0.3172 0.0936 0.4510 0.071 Uiso 1 1 calc R . . C38 C 0.3874(3) 0.2590(3) 0.41461(18) 0.0475(9) Uani 1 1 d . . . H38 H 0.4563 0.2407 0.4406 0.057 Uiso 1 1 calc R . . C39 C 0.3676(3) 0.3724(3) 0.37096(16) 0.0378(8) Uani 1 1 d . . . H39 H 0.4229 0.4327 0.3677 0.045 Uiso 1 1 calc R . . C40 C 0.0950(3) 0.4887(3) 0.16937(16) 0.0427(9) Uani 1 1 d . . . H40A H 0.0692 0.5721 0.1446 0.051 Uiso 1 1 calc R . . H40B H 0.0411 0.4332 0.1587 0.051 Uiso 1 1 calc R . . C41 C 0.2255(3) 0.4616(3) 0.14070(17) 0.0388(9) Uani 1 1 d . . . C42 C 0.2579(4) 0.4110(3) 0.08264(18) 0.0478(10) Uani 1 1 d . . . H42 H 0.1966 0.3882 0.0599 0.057 Uiso 1 1 calc R . . C43 C 0.3796(4) 0.3943(3) 0.0584(2) 0.0574(11) Uani 1 1 d . . . H43 H 0.4038 0.3604 0.0183 0.069 Uiso 1 1 calc R . . C44 C 0.4669(4) 0.4272(3) 0.0927(2) 0.0598(11) Uani 1 1 d . . . H44 H 0.5518 0.4158 0.0768 0.072 Uiso 1 1 calc R . . C45 C 0.4291(3) 0.4767(3) 0.15023(19) 0.0495(10) Uani 1 1 d . . . H45 H 0.4892 0.4997 0.1737 0.059 Uiso 1 1 calc R . . Cl1 Cl 0.7512(5) 0.2593(3) 0.4223(3) 0.0293(13) Uani 0.599(13) 1 d P A 1 O4 O 0.6999(18) 0.1478(17) 0.4595(10) 0.097(7) Uani 0.599(13) 1 d P A 1 O6 O 0.7127(9) 0.3104(7) 0.3583(5) 0.096(4) Uani 0.599(13) 1 d P A 1 O5 O 0.7224(8) 0.3290(6) 0.4741(4) 0.095(4) Uani 0.599(13) 1 d P A 1 O7 O 0.8826(8) 0.2397(9) 0.4166(5) 0.081(3) Uani 0.599(13) 1 d P A 1 Cl1' Cl 0.7468(12) 0.2571(11) 0.4241(7) 0.094(4) Uani 0.401(13) 1 d P A 2 O4' O 0.697(2) 0.142(2) 0.4597(12) 0.058(8) Uani 0.401(13) 1 d P A 2 O5' O 0.8503(14) 0.2898(11) 0.4441(8) 0.091(7) Uani 0.401(13) 1 d P A 2 O6' O 0.6552(8) 0.3584(8) 0.4137(8) 0.090(6) Uani 0.401(13) 1 d P A 2 O7' O 0.7870(14) 0.2481(14) 0.3486(7) 0.101(5) Uani 0.401(13) 1 d P A 2 Cl2 Cl 0.7488(7) 0.6989(7) 0.1218(3) 0.0848(19) Uani 0.698(12) 1 d P B 1 O8 O 0.7135(11) 0.7166(12) 0.0569(6) 0.112(4) Uani 0.698(12) 1 d P B 1 O9 O 0.8667(5) 0.7278(8) 0.1224(3) 0.070(3) Uani 0.698(12) 1 d P B 1 O10 O 0.6642(6) 0.7674(6) 0.1608(3) 0.093(3) Uani 0.698(12) 1 d P B 1 O11 O 0.7184(13) 0.5988(11) 0.1486(8) 0.231(8) Uani 0.698(12) 1 d P B 1 Cl2' Cl 0.7481(9) 0.7001(8) 0.1234(4) 0.021(2) Uani 0.302(12) 1 d PU B 2 O8' O 0.720(2) 0.7751(14) 0.0407(14) 0.057(4) Uani 0.302(12) 1 d P B 2 O9' O 0.860(2) 0.636(3) 0.1023(10) 0.192(14) Uani 0.302(12) 1 d P B 2 O10' O 0.777(4) 0.7755(14) 0.1571(13) 0.210(18) Uani 0.302(12) 1 d P B 2 O11' O 0.7219(10) 0.5664(10) 0.1812(7) 0.050(4) Uani 0.302(12) 1 d P B 2 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 0.0297(3) 0.0263(3) 0.0322(3) -0.0049(2) -0.0104(2) -0.0039(2) Mn2 0.0324(3) 0.0260(3) 0.0371(3) -0.0057(2) -0.0080(2) -0.0061(2) O1 0.0444(14) 0.0330(13) 0.0427(14) -0.0020(10) -0.0186(11) -0.0120(11) O2 0.0381(14) 0.0232(13) 0.0537(14) -0.0012(11) -0.0180(11) -0.0070(11) O3 0.0312(13) 0.0291(12) 0.0382(12) -0.0055(10) -0.0111(10) -0.0062(10) N1 0.0320(16) 0.0241(15) 0.0354(15) -0.0036(12) -0.0095(12) -0.0054(13) N2 0.0291(16) 0.0328(16) 0.0287(15) -0.0088(12) -0.0028(12) -0.0033(13) N3 0.0276(16) 0.0285(15) 0.0391(16) -0.0085(13) -0.0054(13) -0.0006(13) N4 0.0399(18) 0.0282(15) 0.0314(16) -0.0057(12) -0.0068(13) -0.0014(13) N5 0.051(2) 0.047(2) 0.059(2) -0.0178(16) -0.0005(17) 0.0030(17) N6 0.0334(17) 0.0360(17) 0.0391(17) -0.0119(13) -0.0047(13) -0.0091(14) N7 0.0336(17) 0.0327(16) 0.0368(17) -0.0055(13) -0.0054(13) -0.0059(13) N8 0.0366(18) 0.0342(17) 0.0411(17) -0.0059(13) -0.0012(14) -0.0069(14) N9 0.0348(17) 0.0275(15) 0.0342(16) -0.0099(12) 0.0005(13) -0.0044(13) C1 0.0239(19) 0.035(2) 0.0326(19) -0.0088(16) 0.0015(15) -0.0080(16) C2 0.039(2) 0.033(2) 0.040(2) -0.0097(16) -0.0010(16) -0.0090(17) C3 0.049(2) 0.039(2) 0.062(3) -0.022(2) -0.001(2) -0.0089(19) C4 0.063(3) 0.051(3) 0.077(3) -0.028(2) -0.032(2) -0.010(2) C5 0.050(2) 0.044(2) 0.062(2) -0.0168(19) -0.0273(19) -0.0027(19) C6 0.0298(19) 0.034(2) 0.0356(19) -0.0114(16) -0.0074(15) -0.0052(16) C7 0.0300(19) 0.032(2) 0.0315(18) -0.0083(15) -0.0079(15) -0.0055(16) C8 0.032(2) 0.039(2) 0.048(2) -0.0071(17) -0.0154(17) -0.0019(17) C9 0.063(3) 0.069(3) 0.041(2) -0.002(2) -0.021(2) -0.002(2) C10 0.030(2) 0.035(2) 0.0348(19) -0.0072(15) -0.0045(15) -0.0007(16) C11 0.038(2) 0.0236(18) 0.0327(19) -0.0052(15) -0.0002(16) -0.0044(16) C12 0.045(2) 0.042(2) 0.045(2) -0.0111(18) 0.0045(18) -0.0031(18) C13 0.069(3) 0.040(2) 0.039(2) -0.0154(18) 0.013(2) -0.007(2) C14 0.076(3) 0.031(2) 0.027(2) -0.0086(16) -0.006(2) -0.010(2) C15 0.054(2) 0.0242(19) 0.035(2) -0.0055(16) -0.0113(18) -0.0069(17) C16 0.037(2) 0.037(2) 0.0355(19) -0.0052(16) -0.0046(16) -0.0032(17) C17 0.037(2) 0.039(2) 0.044(2) -0.0057(18) -0.0086(18) -0.0042(18) C18 0.067(3) 0.058(3) 0.050(3) -0.003(2) -0.017(2) 0.014(2) C19 0.099(4) 0.082(4) 0.084(4) -0.008(3) -0.041(3) 0.029(3) C20 0.065(4) 0.072(3) 0.131(5) -0.023(4) -0.052(4) 0.026(3) C21 0.040(3) 0.054(3) 0.105(4) -0.030(3) 0.005(2) 0.006(2) C22 0.029(2) 0.049(2) 0.0294(18) -0.0118(16) -0.0074(15) 0.0027(17) C23 0.031(2) 0.034(2) 0.033(2) -0.0095(16) -0.0051(16) -0.0017(16) C24 0.044(2) 0.063(3) 0.031(2) -0.0088(18) -0.0075(17) 0.002(2) C25 0.050(3) 0.064(3) 0.037(2) -0.0149(19) 0.0071(19) -0.001(2) C26 0.038(2) 0.045(2) 0.054(3) -0.0202(19) 0.0090(19) -0.0015(19) C27 0.031(2) 0.035(2) 0.052(2) -0.0122(17) -0.0081(17) 0.0034(17) C28 0.030(2) 0.050(2) 0.048(2) -0.0115(18) -0.0064(16) -0.0097(18) C29 0.035(2) 0.0298(19) 0.037(2) -0.0034(16) -0.0041(17) -0.0026(17) C30 0.036(2) 0.037(2) 0.054(2) -0.0048(18) -0.0033(18) 0.0003(18) C31 0.056(3) 0.040(2) 0.049(2) -0.0091(19) 0.011(2) 0.007(2) C32 0.071(3) 0.031(2) 0.039(2) -0.0066(17) -0.005(2) 0.000(2) C33 0.053(2) 0.027(2) 0.037(2) -0.0029(17) -0.0118(18) -0.0058(18) C34 0.054(3) 0.036(2) 0.057(2) -0.0087(18) -0.0085(19) -0.0184(19) C35 0.038(2) 0.029(2) 0.039(2) -0.0084(16) 0.0029(16) -0.0063(17) C36 0.059(3) 0.025(2) 0.065(3) 0.0004(19) -0.001(2) -0.0099(19) C37 0.067(3) 0.032(2) 0.063(3) 0.0075(19) -0.001(2) 0.004(2) C38 0.044(2) 0.044(2) 0.048(2) -0.0048(19) -0.0036(18) 0.006(2) C39 0.039(2) 0.034(2) 0.038(2) -0.0052(17) -0.0062(17) -0.0023(17) C40 0.047(2) 0.046(2) 0.041(2) -0.0168(17) -0.0086(17) -0.0118(18) C41 0.049(2) 0.0278(19) 0.036(2) -0.0030(16) -0.0022(18) -0.0096(18) C42 0.070(3) 0.033(2) 0.040(2) -0.0083(17) -0.005(2) -0.009(2) C43 0.084(3) 0.040(2) 0.040(2) -0.0078(18) 0.009(2) 0.005(2) C44 0.056(3) 0.055(3) 0.053(3) -0.003(2) 0.012(2) 0.008(2) C45 0.047(3) 0.043(2) 0.051(2) -0.0006(19) -0.0016(19) -0.003(2) Cl1 0.032(3) 0.021(2) 0.032(2) -0.0071(17) 0.0083(19) -0.0103(18) O4 0.103(13) 0.055(9) 0.114(12) 0.034(8) -0.029(9) -0.056(9) O6 0.126(10) 0.091(6) 0.069(6) 0.017(5) -0.061(6) -0.034(6) O5 0.109(7) 0.094(5) 0.094(6) -0.062(4) 0.028(5) -0.024(5) O7 0.064(5) 0.080(6) 0.085(5) -0.004(4) 0.014(4) -0.014(4) Cl1' 0.079(8) 0.126(9) 0.092(9) -0.033(7) -0.032(6) -0.029(7) O4' 0.056(14) 0.063(15) 0.058(12) -0.018(12) -0.010(10) -0.013(11) O5' 0.101(13) 0.068(8) 0.117(12) 0.000(6) -0.080(11) -0.037(8) O6' 0.047(6) 0.051(5) 0.143(14) 0.008(6) 0.015(6) 0.010(4) O7' 0.119(11) 0.113(10) 0.078(7) -0.058(7) 0.049(7) -0.055(8) Cl2 0.061(2) 0.093(3) 0.117(3) -0.047(2) -0.0357(19) 0.0131(16) O8 0.066(5) 0.213(12) 0.076(7) -0.065(8) -0.046(5) 0.034(8) O9 0.034(3) 0.122(7) 0.057(3) -0.016(3) -0.017(2) -0.023(3) O10 0.087(5) 0.133(5) 0.048(3) -0.030(3) 0.004(3) 0.055(4) O11 0.342(16) 0.134(9) 0.215(14) 0.037(8) -0.095(11) -0.147(10) Cl2' 0.020(2) 0.022(2) 0.022(2) -0.0062(11) -0.0028(10) 0.0000(10) O8' 0.057(8) 0.059(8) 0.054(9) -0.007(7) -0.025(6) 0.013(7) O9' 0.166(18) 0.21(2) 0.103(13) 0.045(14) 0.043(12) 0.138(18) O10' 0.46(5) 0.052(10) 0.17(2) 0.003(10) -0.21(3) -0.06(2) O11' 0.045(7) 0.012(5) 0.080(8) 0.014(5) -0.013(5) 0.002(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 Mn1 Mn2 3.1230(6) . ? Mn1 O1 1.8700(19) . ? Mn1 O3 1.8196(18) . ? Mn1 N1 2.032(2) . ? Mn1 N2 2.250(2) . ? Mn1 N3 2.218(2) . ? Mn1 N4 2.281(3) . ? Mn2 O2 1.8976(19) . ? Mn2 O3 1.7868(19) . ? Mn2 N6 2.168(2) . ? Mn2 N7 2.259(3) . ? Mn2 N8 2.264(3) . ? Mn2 N9 2.074(2) . ? O1 C1 1.323(3) . ? O2 N1 1.378(3) . ? N1 C7 1.302(3) . ? N2 C10 1.484(3) . ? N2 C16 1.505(4) . ? N2 C22 1.473(3) . ? N3 C23 1.341(4) . ? N3 C27 1.338(4) . ? N4 C11 1.348(4) . ? N4 C15 1.342(4) . ? N5 C17 1.341(4) . ? N5 C21 1.340(4) . ? N6 C28 1.474(4) . ? N6 C34 1.500(4) . ? N6 C40 1.488(4) . ? N7 C29 1.342(4) . ? N7 C33 1.340(4) . ? N8 C41 1.343(4) . ? N8 C45 1.341(4) . ? N9 C35 1.340(4) . ? N9 C39 1.351(4) . ? C1 C2 1.411(4) . ? C1 C6 1.408(4) . ? C2 H2 0.950 . ? C2 C3 1.364(4) . ? C3 H3 0.950 . ? C3 C4 1.386(5) . ? C4 H4 0.950 . ? C4 C5 1.369(4) . ? C5 H5 0.950 . ? C5 C6 1.405(4) . ? C6 C7 1.470(4) . ? C7 C8 1.502(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C8 C9 1.526(4) . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.508(4) . ? C11 C12 1.374(4) . ? C12 H12 0.950 . ? C12 C13 1.385(4) . ? C13 H13 0.950 . ? C13 C14 1.369(5) . ? C14 H14 0.950 . ? C14 C15 1.374(4) . ? C15 H15 0.950 . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.514(4) . ? C17 C18 1.369(4) . ? C18 H18 0.950 . ? C18 C19 1.374(5) . ? C19 H19 0.950 . ? C19 C20 1.338(6) . ? C20 H20 0.950 . ? C20 C21 1.369(6) . ? C21 H21 0.950 . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C22 C23 1.509(4) . ? C23 C24 1.382(4) . ? C24 H24 0.950 . ? C24 C25 1.371(4) . ? C25 H25 0.950 . ? C25 C26 1.366(4) . ? C26 H26 0.950 . ? C26 C27 1.375(4) . ? C27 H27 0.950 . ? C28 H28A 0.990 . ? C28 H28B 0.990 . ? C28 C29 1.509(4) . ? C29 C30 1.369(4) . ? C30 H30 0.950 . ? C30 C31 1.379(5) . ? C31 H31 0.950 . ? C31 C32 1.374(5) . ? C32 H32 0.950 . ? C32 C33 1.373(4) . ? C33 H33 0.950 . ? C34 H34A 0.990 . ? C34 H34B 0.990 . ? C34 C35 1.496(4) . ? C35 C36 1.379(4) . ? C36 H36 0.950 . ? C36 C37 1.374(5) . ? C37 H37 0.950 . ? C37 C38 1.375(5) . ? C38 H38 0.950 . ? C38 C39 1.373(4) . ? C39 H39 0.950 . ? C40 H40A 0.990 . ? C40 H40B 0.990 . ? C40 C41 1.500(4) . ? C41 C42 1.383(4) . ? C42 H42 0.950 . ? C42 C43 1.369(5) . ? C43 H43 0.950 . ? C43 C44 1.378(5) . ? C44 H44 0.950 . ? C44 C45 1.374(5) . ? C45 H45 0.950 . ? Cl1 O4 1.417(19) . ? Cl1 O6 1.332(9) . ? Cl1 O5 1.426(9) . ? Cl1 O7 1.440(11) . ? Cl1' O4' 1.43(3) . ? Cl1' O5' 1.373(17) . ? Cl1' O6' 1.465(12) . ? Cl1' O7' 1.485(14) . ? Cl2 O8 1.324(12) . ? Cl2 O9 1.374(8) . ? Cl2 O10 1.427(8) . ? Cl2 O11 1.189(11) . ? Cl2' O8' 1.66(2) . ? Cl2' O9' 1.44(2) . ? Cl2' O10' 1.30(2) . ? Cl2' O11' 1.665(12) . ? 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 Mn2 Mn1 O1 149.19(6) . . ? Mn2 Mn1 O3 29.71(6) . . ? Mn2 Mn1 N1 61.73(7) . . ? Mn2 Mn1 N2 118.25(6) . . ? Mn2 Mn1 N3 104.13(6) . . ? Mn2 Mn1 N4 93.64(6) . . ? O1 Mn1 O3 175.07(10) . . ? O1 Mn1 N1 87.75(9) . . ? O1 Mn1 N2 92.43(9) . . ? O1 Mn1 N3 85.11(9) . . ? O1 Mn1 N4 92.38(9) . . ? O3 Mn1 N1 91.43(9) . . ? O3 Mn1 N2 89.44(8) . . ? O3 Mn1 N3 90.92(9) . . ? O3 Mn1 N4 92.53(9) . . ? N1 Mn1 N2 167.31(10) . . ? N1 Mn1 N3 116.77(10) . . ? N1 Mn1 N4 93.69(10) . . ? N2 Mn1 N3 75.87(9) . . ? N2 Mn1 N4 73.62(9) . . ? N3 Mn1 N4 149.25(9) . . ? Mn1 Mn2 O2 65.21(6) . . ? Mn1 Mn2 O3 30.31(6) . . ? Mn1 Mn2 N6 124.04(7) . . ? Mn1 Mn2 N7 97.56(6) . . ? Mn1 Mn2 N8 102.13(6) . . ? Mn1 Mn2 N9 154.14(7) . . ? O2 Mn2 O3 95.34(8) . . ? O2 Mn2 N6 169.82(9) . . ? O2 Mn2 N7 108.68(9) . . ? O2 Mn2 N8 99.11(10) . . ? O2 Mn2 N9 89.21(9) . . ? O3 Mn2 N6 93.75(9) . . ? O3 Mn2 N7 91.31(9) . . ? O3 Mn2 N8 94.89(9) . . ? O3 Mn2 N9 175.42(9) . . ? N6 Mn2 N7 75.65(9) . . ? N6 Mn2 N8 75.50(10) . . ? N6 Mn2 N9 81.76(10) . . ? N7 Mn2 N8 150.81(9) . . ? N7 Mn2 N9 86.72(9) . . ? N8 Mn2 N9 84.88(9) . . ? Mn1 O1 C1 129.32(18) . . ? Mn2 O2 N1 116.99(15) . . ? Mn1 O3 Mn2 119.98(10) . . ? Mn1 N1 O2 114.88(16) . . ? Mn1 N1 C7 130.1(2) . . ? O2 N1 C7 114.8(2) . . ? Mn1 N2 C10 104.87(16) . . ? Mn1 N2 C16 109.86(17) . . ? Mn1 N2 C22 106.46(18) . . ? C10 N2 C16 112.2(2) . . ? C10 N2 C22 111.1(2) . . ? C16 N2 C22 111.9(2) . . ? Mn1 N3 C23 115.3(2) . . ? Mn1 N3 C27 125.9(2) . . ? C23 N3 C27 118.1(3) . . ? Mn1 N4 C11 113.6(2) . . ? Mn1 N4 C15 128.5(2) . . ? C11 N4 C15 117.8(3) . . ? C17 N5 C21 116.9(3) . . ? Mn2 N6 C28 108.20(18) . . ? Mn2 N6 C34 109.00(18) . . ? Mn2 N6 C40 106.44(18) . . ? C28 N6 C34 111.4(2) . . ? C28 N6 C40 110.1(2) . . ? C34 N6 C40 111.5(3) . . ? Mn2 N7 C29 113.2(2) . . ? Mn2 N7 C33 128.5(2) . . ? C29 N7 C33 117.8(3) . . ? Mn2 N8 C41 113.3(2) . . ? Mn2 N8 C45 128.2(2) . . ? C41 N8 C45 118.6(3) . . ? Mn2 N9 C35 115.5(2) . . ? Mn2 N9 C39 125.3(2) . . ? C35 N9 C39 119.2(3) . . ? O1 C1 C2 117.3(3) . . ? O1 C1 C6 123.6(3) . . ? C2 C1 C6 119.0(3) . . ? C1 C2 H2 119.5 . . ? C1 C2 C3 121.1(3) . . ? H2 C2 C3 119.5 . . ? C2 C3 H3 119.7 . . ? C2 C3 C4 120.5(3) . . ? H3 C3 C4 119.7 . . ? C3 C4 H4 120.4 . . ? C3 C4 C5 119.2(3) . . ? H4 C4 C5 120.4 . . ? C4 C5 H5 118.8 . . ? C4 C5 C6 122.5(3) . . ? H5 C5 C6 118.8 . . ? C1 C6 C5 117.7(3) . . ? C1 C6 C7 122.6(3) . . ? C5 C6 C7 119.7(3) . . ? N1 C7 C6 119.7(3) . . ? N1 C7 C8 119.3(3) . . ? C6 C7 C8 120.9(3) . . ? C7 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C7 C8 C9 112.3(3) . . ? H8A C8 H8B 107.9 . . ? H8A C8 C9 109.2 . . ? H8B C8 C9 109.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.7 . . ? N2 C10 H10B 109.7 . . ? N2 C10 C11 110.0(2) . . ? H10A C10 H10B 108.2 . . ? H10A C10 C11 109.7 . . ? H10B C10 C11 109.7 . . ? N4 C11 C10 115.3(3) . . ? N4 C11 C12 122.2(3) . . ? C10 C11 C12 122.5(3) . . ? C11 C12 H12 120.5 . . ? C11 C12 C13 119.1(3) . . ? H12 C12 C13 120.5 . . ? C12 C13 H13 120.5 . . ? C12 C13 C14 119.0(3) . . ? H13 C13 C14 120.5 . . ? C13 C14 H14 120.5 . . ? C13 C14 C15 118.9(3) . . ? H14 C14 C15 120.5 . . ? N4 C15 C14 122.9(3) . . ? N4 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N2 C16 H16A 108.4 . . ? N2 C16 H16B 108.4 . . ? N2 C16 C17 115.6(2) . . ? H16A C16 H16B 107.4 . . ? H16A C16 C17 108.4 . . ? H16B C16 C17 108.4 . . ? N5 C17 C16 115.5(3) . . ? N5 C17 C18 122.6(3) . . ? C16 C17 C18 121.9(3) . . ? C17 C18 H18 120.8 . . ? C17 C18 C19 118.4(4) . . ? H18 C18 C19 120.8 . . ? C18 C19 H19 119.9 . . ? C18 C19 C20 120.2(5) . . ? H19 C19 C20 119.9 . . ? C19 C20 H20 120.7 . . ? C19 C20 C21 118.6(5) . . ? H20 C20 C21 120.7 . . ? N5 C21 C20 123.3(4) . . ? N5 C21 H21 118.3 . . ? C20 C21 H21 118.3 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? N2 C22 C23 110.9(2) . . ? H22A C22 H22B 108.0 . . ? H22A C22 C23 109.5 . . ? H22B C22 C23 109.5 . . ? N3 C23 C22 115.2(3) . . ? N3 C23 C24 121.6(3) . . ? C22 C23 C24 123.2(3) . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 119.5(3) . . ? H24 C24 C25 120.2 . . ? C24 C25 H25 120.5 . . ? C24 C25 C26 119.1(3) . . ? H25 C25 C26 120.5 . . ? C25 C26 H26 120.6 . . ? C25 C26 C27 118.9(3) . . ? H26 C26 C27 120.6 . . ? N3 C27 C26 122.9(3) . . ? N3 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? N6 C28 H28A 109.2 . . ? N6 C28 H28B 109.2 . . ? N6 C28 C29 112.0(2) . . ? H28A C28 H28B 107.9 . . ? H28A C28 C29 109.2 . . ? H28B C28 C29 109.2 . . ? N7 C29 C28 115.8(3) . . ? N7 C29 C30 122.5(3) . . ? C28 C29 C30 121.6(3) . . ? C29 C30 H30 120.6 . . ? C29 C30 C31 118.9(3) . . ? H30 C30 C31 120.6 . . ? C30 C31 H31 120.3 . . ? C30 C31 C32 119.4(4) . . ? H31 C31 C32 120.3 . . ? C31 C32 H32 120.9 . . ? C31 C32 C33 118.3(3) . . ? H32 C32 C33 120.9 . . ? N7 C33 C32 123.1(3) . . ? N7 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? N6 C34 H34A 108.6 . . ? N6 C34 H34B 108.6 . . ? N6 C34 C35 114.6(3) . . ? H34A C34 H34B 107.6 . . ? H34A C34 C35 108.6 . . ? H34B C34 C35 108.6 . . ? N9 C35 C34 118.9(3) . . ? N9 C35 C36 120.9(3) . . ? C34 C35 C36 120.2(3) . . ? C35 C36 H36 120.0 . . ? C35 C36 C37 120.0(3) . . ? H36 C36 C37 120.0 . . ? C36 C37 H37 120.5 . . ? C36 C37 C38 118.9(3) . . ? H37 C37 C38 120.5 . . ? C37 C38 H38 120.4 . . ? C37 C38 C39 119.1(3) . . ? H38 C38 C39 120.4 . . ? N9 C39 C38 121.8(3) . . ? N9 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? N6 C40 H40A 109.4 . . ? N6 C40 H40B 109.4 . . ? N6 C40 C41 111.1(3) . . ? H40A C40 H40B 108.0 . . ? H40A C40 C41 109.4 . . ? H40B C40 C41 109.4 . . ? N8 C41 C40 114.8(3) . . ? N8 C41 C42 121.8(3) . . ? C40 C41 C42 123.3(3) . . ? C41 C42 H42 120.5 . . ? C41 C42 C43 119.1(4) . . ? H42 C42 C43 120.5 . . ? C42 C43 H43 120.3 . . ? C42 C43 C44 119.4(4) . . ? H43 C43 C44 120.3 . . ? C43 C44 H44 120.5 . . ? C43 C44 C45 118.9(4) . . ? H44 C44 C45 120.5 . . ? N8 C45 C44 122.2(4) . . ? N8 C45 H45 118.9 . . ? C44 C45 H45 118.9 . . ? O4 Cl1 O6 114.7(10) . . ? O4 Cl1 O5 102.8(8) . . ? O4 Cl1 O7 107.3(10) . . ? O6 Cl1 O5 114.4(5) . . ? O6 Cl1 O7 112.4(6) . . ? O5 Cl1 O7 104.1(5) . . ? O4' Cl1' O5' 120.5(15) . . ? O4' Cl1' O6' 114.4(13) . . ? O4' Cl1' O7' 103.4(12) . . ? O5' Cl1' O6' 110.3(12) . . ? O5' Cl1' O7' 103.3(12) . . ? O6' Cl1' O7' 102.2(13) . . ? O8 Cl2 O9 115.9(8) . . ? O8 Cl2 O10 107.1(8) . . ? O8 Cl2 O11 100.0(12) . . ? O9 Cl2 O10 109.8(7) . . ? O9 Cl2 O11 120.1(10) . . ? O10 Cl2 O11 102.5(10) . . ? O8' Cl2' O9' 97.3(12) . . ? O8' Cl2' O10' 109.2(11) . . ? O8' Cl2' O11' 138.6(11) . . ? O9' Cl2' O10' 107.2(16) . . ? O9' Cl2' O11' 81.7(12) . . ? O10' Cl2' O11' 110.6(10) . . ? 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 O1 Mn1 Mn2 O2 2.85(16) . . . . ? O1 Mn1 Mn2 O3 -170.45(19) . . . . ? O1 Mn1 Mn2 N6 -172.26(16) . . . . ? O1 Mn1 Mn2 N7 109.99(15) . . . . ? O1 Mn1 Mn2 N8 -91.69(15) . . . . ? O1 Mn1 Mn2 N9 11.9(2) . . . . ? O3 Mn1 Mn2 O2 173.30(15) . . . . ? O3 Mn1 Mn2 N6 -1.82(15) . . . . ? O3 Mn1 Mn2 N7 -79.57(15) . . . . ? O3 Mn1 Mn2 N8 78.76(15) . . . . ? O3 Mn1 Mn2 N9 -177.7(2) . . . . ? N1 Mn1 Mn2 O2 -5.73(11) . . . . ? N1 Mn1 Mn2 O3 -179.03(15) . . . . ? N1 Mn1 Mn2 N6 179.16(12) . . . . ? N1 Mn1 Mn2 N7 101.40(10) . . . . ? N1 Mn1 Mn2 N8 -100.27(11) . . . . ? N1 Mn1 Mn2 N9 3.28(18) . . . . ? N2 Mn1 Mn2 O2 -171.32(10) . . . . ? N2 Mn1 Mn2 O3 15.39(15) . . . . ? N2 Mn1 Mn2 N6 13.57(11) . . . . ? N2 Mn1 Mn2 N7 -64.18(10) . . . . ? N2 Mn1 Mn2 N8 94.14(10) . . . . ? N2 Mn1 Mn2 N9 -162.31(17) . . . . ? N3 Mn1 Mn2 O2 107.35(10) . . . . ? N3 Mn1 Mn2 O3 -65.95(15) . . . . ? N3 Mn1 Mn2 N6 -67.77(11) . . . . ? N3 Mn1 Mn2 N7 -145.52(9) . . . . ? N3 Mn1 Mn2 N8 12.80(10) . . . . ? N3 Mn1 Mn2 N9 116.35(18) . . . . ? N4 Mn1 Mn2 O2 -97.97(10) . . . . ? N4 Mn1 Mn2 O3 88.73(15) . . . . ? N4 Mn1 Mn2 N6 86.92(11) . . . . ? N4 Mn1 Mn2 N7 9.16(9) . . . . ? N4 Mn1 Mn2 N8 167.49(10) . . . . ? N4 Mn1 Mn2 N9 -88.96(17) . . . . ? Mn2 Mn1 O1 C1 -34.3(3) . . . . ? O3 Mn1 O1 C1 -107.3(10) . . . . ? N1 Mn1 O1 C1 -26.7(3) . . . . ? N2 Mn1 O1 C1 140.6(3) . . . . ? N3 Mn1 O1 C1 -143.8(3) . . . . ? N4 Mn1 O1 C1 66.9(3) . . . . ? Mn1 Mn2 O2 N1 8.37(16) . . . . ? O3 Mn2 O2 N1 11.8(2) . . . . ? N6 Mn2 O2 N1 164.8(5) . . . . ? N7 Mn2 O2 N1 -81.44(19) . . . . ? N8 Mn2 O2 N1 107.60(19) . . . . ? N9 Mn2 O2 N1 -167.71(19) . . . . ? O2 Mn2 O3 Mn1 -6.11(14) . . . . ? N6 Mn2 O3 Mn1 178.49(13) . . . . ? N7 Mn2 O3 Mn1 102.79(13) . . . . ? N8 Mn2 O3 Mn1 -105.76(13) . . . . ? N9 Mn2 O3 Mn1 167.3(12) . . . . ? O1 Mn1 O3 Mn2 81.3(10) . . . . ? N1 Mn1 O3 Mn2 0.86(13) . . . . ? N2 Mn1 O3 Mn2 -166.48(13) . . . . ? N3 Mn1 O3 Mn2 117.66(13) . . . . ? N4 Mn1 O3 Mn2 -92.91(13) . . . . ? Mn2 O2 N1 Mn1 -12.9(2) . . . . ? Mn2 O2 N1 C7 172.0(2) . . . . ? Mn2 Mn1 N1 O2 7.91(15) . . . . ? Mn2 Mn1 N1 C7 -177.9(3) . . . . ? O1 Mn1 N1 O2 -167.70(19) . . . . ? O1 Mn1 N1 C7 6.5(3) . . . . ? O3 Mn1 N1 O2 7.43(19) . . . . ? O3 Mn1 N1 C7 -178.4(3) . . . . ? N2 Mn1 N1 O2 101.2(4) . . . . ? N2 Mn1 N1 C7 -84.6(5) . . . . ? N3 Mn1 N1 O2 -84.33(19) . . . . ? N3 Mn1 N1 C7 89.8(3) . . . . ? N4 Mn1 N1 O2 100.06(19) . . . . ? N4 Mn1 N1 C7 -85.8(3) . . . . ? Mn2 Mn1 N2 C10 47.63(19) . . . . ? Mn2 Mn1 N2 C16 168.38(16) . . . . ? Mn2 Mn1 N2 C22 -70.23(18) . . . . ? O1 Mn1 N2 C10 -129.38(18) . . . . ? O1 Mn1 N2 C16 -8.64(19) . . . . ? O1 Mn1 N2 C22 112.76(18) . . . . ? O3 Mn1 N2 C10 55.19(18) . . . . ? O3 Mn1 N2 C16 175.93(18) . . . . ? O3 Mn1 N2 C22 -62.67(18) . . . . ? N1 Mn1 N2 C10 -38.8(5) . . . . ? N1 Mn1 N2 C16 81.9(4) . . . . ? N1 Mn1 N2 C22 -156.7(4) . . . . ? N3 Mn1 N2 C10 146.28(19) . . . . ? N3 Mn1 N2 C16 -92.97(19) . . . . ? N3 Mn1 N2 C22 28.43(17) . . . . ? N4 Mn1 N2 C10 -37.61(17) . . . . ? N4 Mn1 N2 C16 83.13(19) . . . . ? N4 Mn1 N2 C22 -155.47(19) . . . . ? Mn2 Mn1 N3 C23 106.6(2) . . . . ? Mn2 Mn1 N3 C27 -83.5(2) . . . . ? O1 Mn1 N3 C23 -103.3(2) . . . . ? O1 Mn1 N3 C27 66.7(2) . . . . ? O3 Mn1 N3 C23 79.7(2) . . . . ? O3 Mn1 N3 C27 -110.4(2) . . . . ? N1 Mn1 N3 C23 171.73(19) . . . . ? N1 Mn1 N3 C27 -18.3(3) . . . . ? N2 Mn1 N3 C23 -9.5(2) . . . . ? N2 Mn1 N3 C27 160.5(3) . . . . ? N4 Mn1 N3 C23 -16.9(3) . . . . ? N4 Mn1 N3 C27 153.1(2) . . . . ? Mn2 Mn1 N4 C11 -97.07(19) . . . . ? Mn2 Mn1 N4 C15 81.0(2) . . . . ? O1 Mn1 N4 C11 113.2(2) . . . . ? O1 Mn1 N4 C15 -68.8(2) . . . . ? O3 Mn1 N4 C11 -67.3(2) . . . . ? O3 Mn1 N4 C15 110.7(2) . . . . ? N1 Mn1 N4 C11 -158.9(2) . . . . ? N1 Mn1 N4 C15 19.1(2) . . . . ? N2 Mn1 N4 C11 21.33(19) . . . . ? N2 Mn1 N4 C15 -160.6(3) . . . . ? N3 Mn1 N4 C11 28.7(3) . . . . ? N3 Mn1 N4 C15 -153.2(2) . . . . ? Mn1 Mn2 N6 C28 -57.3(2) . . . . ? Mn1 Mn2 N6 C34 -178.58(17) . . . . ? Mn1 Mn2 N6 C40 61.0(2) . . . . ? O2 Mn2 N6 C28 148.6(5) . . . . ? O2 Mn2 N6 C34 27.4(6) . . . . ? O2 Mn2 N6 C40 -93.0(5) . . . . ? O3 Mn2 N6 C28 -58.2(2) . . . . ? O3 Mn2 N6 C34 -179.5(2) . . . . ? O3 Mn2 N6 C40 60.1(2) . . . . ? N7 Mn2 N6 C28 32.16(18) . . . . ? N7 Mn2 N6 C34 -89.1(2) . . . . ? N7 Mn2 N6 C40 150.5(2) . . . . ? N8 Mn2 N6 C28 -152.3(2) . . . . ? N8 Mn2 N6 C34 86.4(2) . . . . ? N8 Mn2 N6 C40 -33.99(19) . . . . ? N9 Mn2 N6 C28 120.9(2) . . . . ? N9 Mn2 N6 C34 -0.4(2) . . . . ? N9 Mn2 N6 C40 -120.8(2) . . . . ? Mn1 Mn2 N7 C29 103.82(19) . . . . ? Mn1 Mn2 N7 C33 -67.8(2) . . . . ? O2 Mn2 N7 C29 170.14(19) . . . . ? O2 Mn2 N7 C33 -1.5(3) . . . . ? O3 Mn2 N7 C29 74.0(2) . . . . ? O3 Mn2 N7 C33 -97.6(2) . . . . ? N6 Mn2 N7 C29 -19.5(2) . . . . ? N6 Mn2 N7 C33 168.9(3) . . . . ? N8 Mn2 N7 C29 -28.4(3) . . . . ? N8 Mn2 N7 C33 159.9(2) . . . . ? N9 Mn2 N7 C29 -101.8(2) . . . . ? N9 Mn2 N7 C33 86.5(2) . . . . ? Mn1 Mn2 N8 C41 -104.35(19) . . . . ? Mn1 Mn2 N8 C45 76.4(3) . . . . ? O2 Mn2 N8 C41 -170.8(2) . . . . ? O2 Mn2 N8 C45 9.9(3) . . . . ? O3 Mn2 N8 C41 -74.6(2) . . . . ? O3 Mn2 N8 C45 106.2(3) . . . . ? N6 Mn2 N8 C41 18.1(2) . . . . ? N6 Mn2 N8 C45 -161.2(3) . . . . ? N7 Mn2 N8 C41 27.0(3) . . . . ? N7 Mn2 N8 C45 -152.3(2) . . . . ? N9 Mn2 N8 C41 100.8(2) . . . . ? N9 Mn2 N8 C45 -78.4(3) . . . . ? Mn1 Mn2 N9 C35 173.89(16) . . . . ? Mn1 Mn2 N9 C39 -4.1(4) . . . . ? O2 Mn2 N9 C35 -177.9(2) . . . . ? O2 Mn2 N9 C39 4.0(3) . . . . ? O3 Mn2 N9 C35 8.6(13) . . . . ? O3 Mn2 N9 C39 -169.4(11) . . . . ? N6 Mn2 N9 C35 -2.7(2) . . . . ? N6 Mn2 N9 C39 179.3(3) . . . . ? N7 Mn2 N9 C35 73.3(2) . . . . ? N7 Mn2 N9 C39 -104.7(3) . . . . ? N8 Mn2 N9 C35 -78.7(2) . . . . ? N8 Mn2 N9 C39 103.3(3) . . . . ? Mn1 O1 C1 C2 -153.5(2) . . . . ? Mn1 O1 C1 C6 29.4(4) . . . . ? O1 C1 C2 C3 -177.4(3) . . . . ? C6 C1 C2 C3 -0.1(5) . . . . ? C1 C2 C3 C4 -1.1(5) . . . . ? C2 C3 C4 C5 1.7(6) . . . . ? C3 C4 C5 C6 -1.1(6) . . . . ? C4 C5 C6 C1 -0.1(5) . . . . ? C4 C5 C6 C7 -179.0(3) . . . . ? O1 C1 C6 C5 177.8(3) . . . . ? O1 C1 C6 C7 -3.3(5) . . . . ? C2 C1 C6 C5 0.7(5) . . . . ? C2 C1 C6 C7 179.6(3) . . . . ? Mn1 N1 C7 C6 11.0(4) . . . . ? Mn1 N1 C7 C8 -172.5(2) . . . . ? O2 N1 C7 C6 -174.9(2) . . . . ? O2 N1 C7 C8 1.6(4) . . . . ? C1 C6 C7 N1 -15.9(5) . . . . ? C1 C6 C7 C8 167.6(3) . . . . ? C5 C6 C7 N1 162.9(3) . . . . ? C5 C6 C7 C8 -13.5(5) . . . . ? N1 C7 C8 C9 -82.8(4) . . . . ? C6 C7 C8 C9 93.6(3) . . . . ? Mn1 N2 C10 C11 50.9(3) . . . . ? C16 N2 C10 C11 -68.3(3) . . . . ? C22 N2 C10 C11 165.5(2) . . . . ? Mn1 N4 C11 C10 0.6(3) . . . . ? Mn1 N4 C11 C12 178.9(2) . . . . ? C15 N4 C11 C10 -177.7(2) . . . . ? C15 N4 C11 C12 0.7(4) . . . . ? N2 C10 C11 N4 -35.4(3) . . . . ? N2 C10 C11 C12 146.2(3) . . . . ? N4 C11 C12 C13 -1.6(5) . . . . ? C10 C11 C12 C13 176.6(3) . . . . ? C11 C12 C13 C14 0.9(5) . . . . ? C12 C13 C14 C15 0.7(5) . . . . ? Mn1 N4 C15 C14 -176.9(2) . . . . ? C11 N4 C15 C14 1.1(4) . . . . ? C13 C14 C15 N4 -1.7(5) . . . . ? Mn1 N2 C16 C17 -167.7(2) . . . . ? C10 N2 C16 C17 -51.5(3) . . . . ? C22 N2 C16 C17 74.2(3) . . . . ? C21 N5 C17 C16 177.3(3) . . . . ? C21 N5 C17 C18 0.1(5) . . . . ? N2 C16 C17 N5 87.6(3) . . . . ? N2 C16 C17 C18 -95.2(4) . . . . ? N5 C17 C18 C19 0.4(6) . . . . ? C16 C17 C18 C19 -176.6(4) . . . . ? C17 C18 C19 C20 -0.3(7) . . . . ? C18 C19 C20 C21 -0.3(8) . . . . ? C17 N5 C21 C20 -0.8(6) . . . . ? C19 C20 C21 N5 0.9(7) . . . . ? Mn1 N2 C22 C23 -43.6(3) . . . . ? C10 N2 C22 C23 -157.3(2) . . . . ? C16 N2 C22 C23 76.4(3) . . . . ? Mn1 N3 C23 C22 -12.1(3) . . . . ? Mn1 N3 C23 C24 169.4(2) . . . . ? C27 N3 C23 C22 177.1(3) . . . . ? C27 N3 C23 C24 -1.4(4) . . . . ? N2 C22 C23 N3 38.7(4) . . . . ? N2 C22 C23 C24 -142.8(3) . . . . ? N3 C23 C24 C25 1.8(5) . . . . ? C22 C23 C24 C25 -176.6(3) . . . . ? C23 C24 C25 C26 -0.8(5) . . . . ? C24 C25 C26 C27 -0.5(5) . . . . ? Mn1 N3 C27 C26 -169.7(2) . . . . ? C23 N3 C27 C26 0.0(5) . . . . ? C25 C26 C27 N3 0.9(5) . . . . ? Mn2 N6 C28 C29 -42.0(3) . . . . ? C34 N6 C28 C29 77.8(3) . . . . ? C40 N6 C28 C29 -158.0(2) . . . . ? Mn2 N7 C29 C28 2.0(3) . . . . ? Mn2 N7 C29 C30 -174.0(2) . . . . ? C33 N7 C29 C28 174.7(3) . . . . ? C33 N7 C29 C30 -1.4(4) . . . . ? N6 C28 C29 N7 26.8(4) . . . . ? N6 C28 C29 C30 -157.1(3) . . . . ? N7 C29 C30 C31 3.6(5) . . . . ? C28 C29 C30 C31 -172.3(3) . . . . ? C29 C30 C31 C32 -2.5(5) . . . . ? C30 C31 C32 C33 -0.4(5) . . . . ? Mn2 N7 C33 C32 169.5(2) . . . . ? C29 N7 C33 C32 -1.8(4) . . . . ? C31 C32 C33 N7 2.7(5) . . . . ? Mn2 N6 C34 C35 3.1(3) . . . . ? C28 N6 C34 C35 -116.2(3) . . . . ? C40 N6 C34 C35 120.3(3) . . . . ? Mn2 N9 C35 C34 5.4(4) . . . . ? Mn2 N9 C35 C36 -175.6(3) . . . . ? C39 N9 C35 C34 -176.5(3) . . . . ? C39 N9 C35 C36 2.5(5) . . . . ? N6 C34 C35 N9 -5.7(5) . . . . ? N6 C34 C35 C36 175.3(3) . . . . ? N9 C35 C36 C37 -2.2(5) . . . . ? C34 C35 C36 C37 176.8(3) . . . . ? C35 C36 C37 C38 0.2(6) . . . . ? C36 C37 C38 C39 1.4(6) . . . . ? Mn2 N9 C39 C38 177.1(2) . . . . ? C35 N9 C39 C38 -0.9(5) . . . . ? C37 C38 C39 N9 -1.1(5) . . . . ? Mn2 N6 C40 C41 47.5(3) . . . . ? C28 N6 C40 C41 164.5(3) . . . . ? C34 N6 C40 C41 -71.3(3) . . . . ? Mn2 N8 C41 C40 3.1(3) . . . . ? Mn2 N8 C41 C42 -178.9(2) . . . . ? C45 N8 C41 C40 -177.6(3) . . . . ? C45 N8 C41 C42 0.5(4) . . . . ? N6 C40 C41 N8 -34.1(4) . . . . ? N6 C40 C41 C42 147.9(3) . . . . ? N8 C41 C42 C43 -0.6(5) . . . . ? C40 C41 C42 C43 177.2(3) . . . . ? C41 C42 C43 C44 0.6(5) . . . . ? C42 C43 C44 C45 -0.4(5) . . . . ? Mn2 N8 C45 C44 178.9(2) . . . . ? C41 N8 C45 C44 -0.3(5) . . . . ? C43 C44 C45 N8 0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.334 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.050 _vrf_THETM01_3-eb2089 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Diffraction was weak, and the data set was truncated at 0.9A resolution. ; _vrf_PLAT221_3-eb2089 ; PROBLEM: Large Solvent/Anion O Ueq(max)/Ueq(min) ... 4.3 Ratio RESPONSE: Both perchlorate ions are refined as completely disordered. ; _database_code_depnum_ccdc_archive 'CCDC 950513' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4-eb2190 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 C49 H45 Mn2 N9 O3 2+, 4 Cl O4 -, C H4 O' _chemical_formula_sum 'C99 H94 Cl4 Mn4 N18 O23' _chemical_formula_weight 2265.48 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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.3801(2) _cell_length_b 22.7282(4) _cell_length_c 19.6458(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.4164(16) _cell_angle_gamma 90.00 _cell_volume 5038.87(16) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 13281 _cell_measurement_theta_min 2.8318 _cell_measurement_theta_max 28.6998 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2332 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.8585 _exptl_absorpt_correction_T_max 0.8819 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21d (release 25-05-2012 CrysAlis171 .NET) (compiled May 25 2012,16:20:25) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Agilent Technologies SuperNova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3147 _diffrn_reflns_number 41286 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 28.76 _reflns_number_total 11501 _reflns_number_gt 8573 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2011)' _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2011)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2011)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 2008) and local programs' _refine_special_details ; Two perchlorate counterions are present in the asymmetric unit. Each was refined using a two part disorder model with occupancy ratios of 0.692:0.308(7) for perchlorate including Cl1, and 0.553:0.447(6) for perchlorate including Cl2. The geometry of all four perchlorates was restrained to be similar. One molecule of methanol solvate is present in the asymmetric unit, disordered over an inversion centre. Thus the complete chemical formula is 2 C49H45Mn2N9O32+ 4 ClO6 CH3OH. 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^)+(0.0363P)^2^+3.0460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary charge-flipping _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11501 _refine_ls_number_parameters 769 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Mn1 Mn 0.35615(3) 0.627924(15) 0.302766(17) 0.02191(9) Uani 1 1 d . . . Mn2 Mn 0.08718(3) 0.649441(15) 0.255162(17) 0.02226(9) Uani 1 1 d . . . O1 O 0.49484(14) 0.58462(7) 0.29788(8) 0.0300(4) Uani 1 1 d . . . O2 O 0.15262(13) 0.58358(7) 0.21511(8) 0.0283(4) Uani 1 1 d . . . O3 O 0.22069(13) 0.66927(7) 0.30779(8) 0.0259(4) Uani 1 1 d . . . N1 N 0.26899(15) 0.56841(8) 0.23869(9) 0.0226(4) Uani 1 1 d . . . N2 N 0.45294(16) 0.69854(8) 0.36493(9) 0.0222(4) Uani 1 1 d . . . N3 N 0.36028(17) 0.59737(9) 0.40970(10) 0.0277(4) Uani 1 1 d . . . N4 N 0.68840(17) 0.77868(9) 0.38099(10) 0.0289(5) Uani 1 1 d . . . N5 N 0.41067(16) 0.68961(9) 0.22369(9) 0.0251(4) Uani 1 1 d . . . N6 N -0.01648(16) 0.71902(8) 0.29297(10) 0.0260(4) Uani 1 1 d . . . N7 N 0.00818(17) 0.60771(9) 0.34392(10) 0.0301(5) Uani 1 1 d . . . N8 N -0.07490(16) 0.62657(8) 0.20289(9) 0.0240(4) Uani 1 1 d . . . N9 N 0.09587(17) 0.72444(9) 0.18104(10) 0.0306(5) Uani 1 1 d . . . C1 C 0.5137(2) 0.53235(10) 0.27167(11) 0.0228(5) Uani 1 1 d . . . C2 C 0.6286(2) 0.50880(11) 0.28566(12) 0.0283(5) Uani 1 1 d . . . H2 H 0.6869 0.5296 0.3153 0.034 Uiso 1 1 calc R . . C3 C 0.6581(2) 0.45650(11) 0.25745(13) 0.0325(6) Uani 1 1 d . . . H3 H 0.7366 0.4417 0.2673 0.039 Uiso 1 1 calc R . . C4 C 0.5744(2) 0.42512(11) 0.21474(14) 0.0373(6) Uani 1 1 d . . . H4 H 0.5953 0.3892 0.1947 0.045 Uiso 1 1 calc R . . C5 C 0.4609(2) 0.44637(11) 0.20167(13) 0.0313(6) Uani 1 1 d . . . H5 H 0.4032 0.4242 0.1732 0.038 Uiso 1 1 calc R . . C6 C 0.4275(2) 0.50006(10) 0.22926(11) 0.0231(5) Uani 1 1 d . . . C7 C 0.3050(2) 0.52024(10) 0.21206(11) 0.0220(5) Uani 1 1 d . . . C8 C 0.2174(2) 0.48776(10) 0.16251(11) 0.0227(5) Uani 1 1 d . . . C9 C 0.1278(2) 0.45453(10) 0.18571(12) 0.0264(5) Uani 1 1 d . . . H9 H 0.1269 0.4486 0.2335 0.032 Uiso 1 1 calc R . . C10 C 0.1306(2) 0.47084(11) 0.04623(12) 0.0341(6) Uani 1 1 d . . . H10 H 0.1316 0.4762 -0.0016 0.041 Uiso 1 1 calc R . . C11 C 0.0410(2) 0.43830(11) 0.06931(13) 0.0349(6) Uani 1 1 d . . . H11 H -0.0196 0.4216 0.0374 0.042 Uiso 1 1 calc R . . C12 C 0.0400(2) 0.43013(11) 0.13885(13) 0.0318(6) Uani 1 1 d . . . H12 H -0.0214 0.4076 0.1547 0.038 Uiso 1 1 calc R . . C13 C 0.2192(2) 0.49577(11) 0.09283(12) 0.0293(5) Uani 1 1 d . . . H13 H 0.2807 0.5182 0.0769 0.035 Uiso 1 1 calc R . . C14 C 0.3952(2) 0.70138(11) 0.42859(11) 0.0275(5) Uani 1 1 d . . . H14A H 0.3162 0.7199 0.4184 0.033 Uiso 1 1 calc R . . H14B H 0.4437 0.7257 0.4634 0.033 Uiso 1 1 calc R . . C15 C 0.3822(2) 0.64021(11) 0.45649(12) 0.0276(5) Uani 1 1 d . . . C16 C 0.3905(2) 0.62842(13) 0.52604(13) 0.0398(7) Uani 1 1 d . . . H16 H 0.4046 0.6594 0.5586 0.048 Uiso 1 1 calc R . . C17 C 0.3779(3) 0.57132(14) 0.54763(15) 0.0497(8) Uani 1 1 d . . . H17 H 0.3845 0.5624 0.5952 0.060 Uiso 1 1 calc R . . C18 C 0.3559(3) 0.52742(13) 0.49940(15) 0.0452(7) Uani 1 1 d . . . H18 H 0.3462 0.4878 0.5131 0.054 Uiso 1 1 calc R . . C19 C 0.3481(2) 0.54196(12) 0.43086(14) 0.0368(6) Uani 1 1 d . . . H19 H 0.3335 0.5117 0.3975 0.044 Uiso 1 1 calc R . . C20 C 0.58271(19) 0.68599(10) 0.38061(11) 0.0232(5) Uani 1 1 d . . . H20A H 0.6150 0.6789 0.3369 0.028 Uiso 1 1 calc R . . H20B H 0.5932 0.6493 0.4079 0.028 Uiso 1 1 calc R . . C21 C 0.6539(2) 0.73420(10) 0.41926(11) 0.0239(5) Uani 1 1 d . . . C22 C 0.6824(2) 0.73210(11) 0.48968(12) 0.0302(5) Uani 1 1 d . . . H22 H 0.6582 0.6996 0.5150 0.036 Uiso 1 1 calc R . . C23 C 0.7461(3) 0.77764(12) 0.52305(13) 0.0398(7) Uani 1 1 d . . . H23 H 0.7670 0.7769 0.5714 0.048 Uiso 1 1 calc R . . C24 C 0.7789(3) 0.82422(12) 0.48487(14) 0.0421(7) Uani 1 1 d . . . H24 H 0.8213 0.8566 0.5065 0.050 Uiso 1 1 calc R . . C25 C 0.7489(2) 0.82281(12) 0.41463(13) 0.0357(6) Uani 1 1 d . . . H25 H 0.7723 0.8549 0.3886 0.043 Uiso 1 1 calc R . . C26 C 0.4301(2) 0.75248(10) 0.32263(11) 0.0251(5) Uani 1 1 d . . . H26A H 0.4815 0.7848 0.3429 0.030 Uiso 1 1 calc R . . H26B H 0.3465 0.7647 0.3220 0.030 Uiso 1 1 calc R . . C27 C 0.4551(2) 0.74067(10) 0.25036(11) 0.0244(5) Uani 1 1 d . . . C28 C 0.5157(2) 0.77921(11) 0.21329(12) 0.0303(5) Uani 1 1 d . . . H28 H 0.5483 0.8146 0.2334 0.036 Uiso 1 1 calc R . . C29 C 0.5279(2) 0.76503(12) 0.14566(12) 0.0341(6) Uani 1 1 d . . . H29 H 0.5707 0.7904 0.1193 0.041 Uiso 1 1 calc R . . C30 C 0.4777(2) 0.71406(12) 0.11703(12) 0.0323(6) Uani 1 1 d . . . H30 H 0.4821 0.7046 0.0703 0.039 Uiso 1 1 calc R . . C31 C 0.4208(2) 0.67709(11) 0.15800(12) 0.0284(5) Uani 1 1 d . . . H31 H 0.3876 0.6414 0.1389 0.034 Uiso 1 1 calc R . . C32 C -0.0154(2) 0.71016(12) 0.36795(12) 0.0339(6) Uani 1 1 d . . . H32A H -0.0783 0.7345 0.3842 0.041 Uiso 1 1 calc R . . H32B H 0.0618 0.7234 0.3922 0.041 Uiso 1 1 calc R . . C33 C -0.0348(2) 0.64667(12) 0.38527(12) 0.0330(6) Uani 1 1 d . . . C34 C -0.0884(2) 0.62874(15) 0.44140(14) 0.0475(8) Uani 1 1 d . . . H34 H -0.1197 0.6569 0.4700 0.057 Uiso 1 1 calc R . . C35 C -0.0954(3) 0.56916(17) 0.45507(16) 0.0582(9) Uani 1 1 d . . . H35 H -0.1307 0.5560 0.4936 0.070 Uiso 1 1 calc R . . C36 C -0.0513(3) 0.52934(15) 0.41286(16) 0.0530(8) Uani 1 1 d . . . H36 H -0.0558 0.4883 0.4214 0.064 Uiso 1 1 calc R . . C37 C -0.0001(2) 0.54992(12) 0.35764(14) 0.0390(6) Uani 1 1 d . . . H37 H 0.0304 0.5223 0.3281 0.047 Uiso 1 1 calc R . . C38 C -0.1397(2) 0.71606(11) 0.25533(12) 0.0267(5) Uani 1 1 d . . . H38A H -0.1503 0.7484 0.2214 0.032 Uiso 1 1 calc R . . H38B H -0.1971 0.7222 0.2885 0.032 Uiso 1 1 calc R . . C39 C -0.1670(2) 0.65874(10) 0.21881(11) 0.0249(5) Uani 1 1 d . . . C40 C -0.2825(2) 0.64063(11) 0.19879(12) 0.0295(5) Uani 1 1 d . . . H40 H -0.3468 0.6630 0.2113 0.035 Uiso 1 1 calc R . . C41 C -0.3036(2) 0.58989(12) 0.16064(12) 0.0328(6) Uani 1 1 d . . . H41 H -0.3825 0.5773 0.1463 0.039 Uiso 1 1 calc R . . C42 C -0.2088(2) 0.55758(11) 0.14344(12) 0.0303(5) Uani 1 1 d . . . H42 H -0.2215 0.5228 0.1167 0.036 Uiso 1 1 calc R . . C43 C -0.0953(2) 0.57692(11) 0.16599(12) 0.0286(5) Uani 1 1 d . . . H43 H -0.0298 0.5545 0.1551 0.034 Uiso 1 1 calc R . . C44 C 0.0394(2) 0.77592(11) 0.27924(14) 0.0353(6) Uani 1 1 d . . . H44A H 0.1100 0.7822 0.3135 0.042 Uiso 1 1 calc R . . H44B H -0.0172 0.8083 0.2839 0.042 Uiso 1 1 calc R . . C45 C 0.0753(2) 0.77698(11) 0.20855(14) 0.0355(6) Uani 1 1 d . . . C46 C 0.0892(3) 0.82924(14) 0.17427(19) 0.0564(9) Uani 1 1 d . . . H46 H 0.0735 0.8659 0.1945 0.068 Uiso 1 1 calc R . . C47 C 0.1261(3) 0.82701(17) 0.1103(2) 0.0713(11) Uani 1 1 d . . . H47 H 0.1371 0.8623 0.0860 0.086 Uiso 1 1 calc R . . C48 C 0.1471(3) 0.77318(16) 0.08171(17) 0.0584(9) Uani 1 1 d . . . H48 H 0.1725 0.7709 0.0376 0.070 Uiso 1 1 calc R . . C49 C 0.1307(2) 0.72281(14) 0.11819(13) 0.0397(6) Uani 1 1 d . . . H49 H 0.1444 0.6857 0.0984 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.2320(4) 0.38934(19) 0.37325(19) 0.0315(6) Uani 0.692(7) 1 d PD A 1 O4 O 0.2902(4) 0.39642(17) 0.44288(19) 0.0448(10) Uani 0.692(7) 1 d PD A 1 O5 O 0.1265(11) 0.4253(5) 0.3642(7) 0.045(3) Uani 0.692(7) 1 d PD A 1 O6 O 0.2027(4) 0.3287(2) 0.3616(2) 0.0438(11) Uani 0.692(7) 1 d PD A 1 O7 O 0.3128(3) 0.40859(18) 0.32734(18) 0.0606(15) Uani 0.692(7) 1 d PD A 1 Cl1' Cl 0.2219(9) 0.3768(4) 0.3615(4) 0.046(2) Uani 0.308(7) 1 d PD A 2 O4' O 0.3258(8) 0.3902(4) 0.4076(7) 0.062(3) Uani 0.308(7) 1 d PD A 2 O5' O 0.144(2) 0.4274(11) 0.3593(14) 0.041(5) Uani 0.308(7) 1 d PD A 2 O6' O 0.1635(10) 0.3269(5) 0.3881(7) 0.062(3) Uani 0.308(7) 1 d PD A 2 O7' O 0.2445(10) 0.3631(4) 0.2945(4) 0.081(4) Uani 0.308(7) 1 d PD A 2 Cl2 Cl 0.7311(6) 0.1402(3) 0.5621(4) 0.0490(17) Uani 0.447(6) 1 d PD B 1 O8 O 0.7685(4) 0.1485(3) 0.6334(3) 0.061(2) Uani 0.447(6) 1 d PD B 1 O9 O 0.6055(9) 0.1527(8) 0.5471(9) 0.050(5) Uani 0.447(6) 1 d PD B 1 O10 O 0.7583(5) 0.0829(3) 0.5441(4) 0.068(3) Uani 0.447(6) 1 d PD B 1 O11 O 0.7962(11) 0.1803(5) 0.5272(7) 0.164(7) Uani 0.447(6) 1 d PD B 1 Cl2' Cl 0.7268(6) 0.1416(3) 0.5506(3) 0.0426(12) Uani 0.553(6) 1 d PD B 2 O8' O 0.7548(5) 0.0941(4) 0.5954(4) 0.122(4) Uani 0.553(6) 1 d PD B 2 O9' O 0.6022(7) 0.1557(6) 0.5502(8) 0.051(4) Uani 0.553(6) 1 d PD B 2 O10' O 0.7452(4) 0.1233(2) 0.4831(2) 0.0656(17) Uani 0.553(6) 1 d PD B 2 O11' O 0.7971(4) 0.1911(3) 0.5658(4) 0.086(3) Uani 0.553(6) 1 d PD B 2 O12 O -0.5207(4) 0.5589(2) 0.0491(2) 0.0728(15) Uani 0.50 1 d P C -1 H12O H -0.5684 0.5754 0.0189 0.087 Uiso 0.50 1 calc PR C -1 C50 C -0.4724(6) 0.5164(3) 0.0232(3) 0.0529(17) Uani 0.50 1 d P C -1 H50A H -0.4032 0.5304 0.0029 0.079 Uiso 0.50 1 calc PR C -1 H50B H -0.5289 0.4983 -0.0125 0.079 Uiso 0.50 1 calc PR C -1 H50C H -0.4471 0.4873 0.0589 0.079 Uiso 0.50 1 calc PR C -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 0.01958(18) 0.02212(19) 0.02451(18) -0.00399(14) 0.00467(13) 0.00156(14) Mn2 0.01926(17) 0.02109(19) 0.02701(19) -0.00270(14) 0.00519(13) 0.00246(14) O1 0.0232(8) 0.0295(9) 0.0369(9) -0.0099(7) 0.0024(7) 0.0046(7) O2 0.0198(8) 0.0282(9) 0.0363(9) -0.0084(7) 0.0013(7) 0.0042(7) O3 0.0219(8) 0.0255(9) 0.0308(9) -0.0055(7) 0.0053(7) 0.0018(7) N1 0.0186(9) 0.0235(10) 0.0259(10) -0.0020(8) 0.0034(7) 0.0031(8) N2 0.0223(9) 0.0223(10) 0.0233(9) -0.0012(8) 0.0075(7) 0.0021(8) N3 0.0258(10) 0.0278(11) 0.0301(11) 0.0015(8) 0.0066(8) -0.0018(9) N4 0.0272(11) 0.0315(12) 0.0282(10) 0.0038(9) 0.0048(8) -0.0038(9) N5 0.0209(10) 0.0287(11) 0.0259(10) -0.0011(8) 0.0041(8) 0.0020(8) N6 0.0229(10) 0.0249(11) 0.0305(10) -0.0021(8) 0.0054(8) 0.0029(8) N7 0.0249(10) 0.0335(12) 0.0323(11) 0.0053(9) 0.0050(8) 0.0026(9) N8 0.0234(10) 0.0225(10) 0.0265(10) 0.0015(8) 0.0046(8) 0.0027(8) N9 0.0237(10) 0.0330(12) 0.0361(12) 0.0050(9) 0.0071(9) 0.0033(9) C1 0.0256(12) 0.0228(12) 0.0215(11) 0.0026(9) 0.0090(9) 0.0031(10) C2 0.0260(12) 0.0302(14) 0.0293(12) 0.0041(10) 0.0055(10) 0.0039(11) C3 0.0273(13) 0.0310(14) 0.0408(14) 0.0073(11) 0.0101(11) 0.0106(11) C4 0.0369(15) 0.0245(14) 0.0524(16) -0.0019(12) 0.0134(12) 0.0076(12) C5 0.0318(13) 0.0256(13) 0.0375(14) -0.0041(10) 0.0079(11) 0.0012(11) C6 0.0256(12) 0.0217(12) 0.0238(11) 0.0036(9) 0.0101(9) 0.0021(10) C7 0.0254(12) 0.0197(12) 0.0222(11) 0.0016(9) 0.0076(9) 0.0005(10) C8 0.0269(12) 0.0165(11) 0.0251(11) -0.0024(9) 0.0047(9) 0.0038(10) C9 0.0308(13) 0.0212(12) 0.0282(12) 0.0033(9) 0.0070(10) 0.0018(10) C10 0.0423(15) 0.0347(15) 0.0241(12) -0.0016(10) 0.0001(11) 0.0073(12) C11 0.0339(14) 0.0290(14) 0.0385(14) -0.0050(11) -0.0078(11) 0.0034(12) C12 0.0294(13) 0.0233(13) 0.0424(15) 0.0022(11) 0.0039(11) -0.0019(11) C13 0.0344(13) 0.0263(13) 0.0286(13) 0.0023(10) 0.0091(10) 0.0030(11) C14 0.0288(12) 0.0310(13) 0.0243(12) -0.0060(10) 0.0097(10) -0.0028(11) C15 0.0242(12) 0.0332(14) 0.0268(12) -0.0015(10) 0.0081(9) -0.0038(10) C16 0.0462(16) 0.0472(17) 0.0281(13) -0.0023(12) 0.0129(12) -0.0098(14) C17 0.0554(19) 0.062(2) 0.0331(15) 0.0146(14) 0.0109(13) -0.0057(16) C18 0.0465(17) 0.0417(17) 0.0488(17) 0.0174(14) 0.0116(13) -0.0050(14) C19 0.0361(15) 0.0320(15) 0.0434(15) 0.0054(12) 0.0089(12) -0.0036(12) C20 0.0223(11) 0.0226(12) 0.0255(11) -0.0006(9) 0.0061(9) 0.0032(10) C21 0.0248(12) 0.0246(12) 0.0229(11) 0.0003(9) 0.0060(9) 0.0045(10) C22 0.0378(14) 0.0273(13) 0.0258(12) 0.0023(10) 0.0059(10) 0.0008(11) C23 0.0583(18) 0.0354(15) 0.0245(13) -0.0023(11) 0.0006(12) -0.0051(13) C24 0.0538(18) 0.0320(15) 0.0385(15) -0.0046(12) -0.0013(13) -0.0100(13) C25 0.0393(15) 0.0310(14) 0.0367(14) 0.0049(11) 0.0044(11) -0.0073(12) C26 0.0233(11) 0.0218(12) 0.0305(12) -0.0012(10) 0.0050(9) 0.0017(10) C27 0.0207(11) 0.0250(12) 0.0271(12) 0.0015(9) 0.0017(9) 0.0044(10) C28 0.0291(13) 0.0278(13) 0.0338(13) 0.0059(10) 0.0031(10) 0.0014(11) C29 0.0309(13) 0.0401(16) 0.0313(13) 0.0123(11) 0.0048(11) -0.0023(12) C30 0.0278(13) 0.0473(16) 0.0218(12) 0.0045(11) 0.0030(10) 0.0023(12) C31 0.0230(12) 0.0362(14) 0.0258(12) -0.0025(10) 0.0023(9) 0.0025(11) C32 0.0328(14) 0.0425(16) 0.0267(12) -0.0073(11) 0.0048(10) 0.0136(12) C33 0.0215(12) 0.0489(17) 0.0289(13) 0.0049(11) 0.0042(10) 0.0096(12) C34 0.0326(15) 0.078(2) 0.0337(15) 0.0112(14) 0.0103(12) 0.0191(15) C35 0.0395(17) 0.086(3) 0.0508(19) 0.0358(18) 0.0135(14) 0.0094(17) C36 0.0450(17) 0.056(2) 0.058(2) 0.0269(16) 0.0082(15) 0.0015(16) C37 0.0345(14) 0.0390(16) 0.0430(15) 0.0117(12) 0.0028(12) 0.0016(12) C38 0.0215(11) 0.0288(13) 0.0307(12) 0.0015(10) 0.0058(9) 0.0061(10) C39 0.0239(12) 0.0306(13) 0.0214(11) 0.0080(9) 0.0071(9) 0.0038(10) C40 0.0229(12) 0.0397(15) 0.0262(12) 0.0037(11) 0.0048(10) 0.0046(11) C41 0.0256(12) 0.0448(16) 0.0280(13) 0.0017(11) 0.0035(10) -0.0055(12) C42 0.0313(13) 0.0324(14) 0.0272(12) -0.0006(10) 0.0030(10) -0.0046(11) C43 0.0271(12) 0.0285(13) 0.0307(13) 0.0012(10) 0.0050(10) 0.0037(11) C44 0.0307(14) 0.0221(13) 0.0541(17) -0.0075(11) 0.0090(12) 0.0016(11) C45 0.0228(12) 0.0281(14) 0.0567(17) 0.0061(12) 0.0092(12) 0.0034(11) C46 0.0464(18) 0.0341(17) 0.095(3) 0.0179(17) 0.0323(18) 0.0071(14) C47 0.066(2) 0.056(2) 0.100(3) 0.043(2) 0.038(2) 0.0161(19) C48 0.0489(19) 0.075(3) 0.056(2) 0.0321(18) 0.0243(15) 0.0116(17) C49 0.0295(14) 0.0534(18) 0.0372(15) 0.0078(13) 0.0081(11) 0.0037(13) Cl1 0.0352(9) 0.0310(11) 0.0302(11) 0.0085(9) 0.0118(9) 0.0034(7) O4 0.057(2) 0.0369(19) 0.037(2) -0.0003(15) -0.0031(16) -0.0033(16) O5 0.041(3) 0.032(4) 0.062(5) 0.006(3) 0.010(3) 0.010(2) O6 0.051(3) 0.019(2) 0.058(3) -0.0081(18) -0.0044(18) 0.0043(18) O7 0.050(2) 0.083(3) 0.053(2) 0.028(2) 0.0276(16) 0.0045(19) Cl1' 0.049(3) 0.053(5) 0.036(3) 0.009(3) 0.005(2) 0.024(3) O4' 0.038(5) 0.033(4) 0.102(9) 0.010(5) -0.035(5) -0.007(4) O5' 0.043(9) 0.047(10) 0.031(7) 0.002(6) 0.004(6) 0.017(7) O6' 0.046(6) 0.055(6) 0.078(8) 0.026(6) -0.013(5) -0.011(5) O7' 0.119(9) 0.088(8) 0.038(4) 0.011(4) 0.015(5) 0.065(7) Cl2 0.048(3) 0.032(2) 0.075(4) -0.004(2) 0.038(3) 0.004(2) O8 0.033(3) 0.082(4) 0.068(4) -0.045(3) 0.006(2) -0.007(3) O9 0.046(8) 0.063(9) 0.039(7) -0.001(6) -0.004(5) 0.041(6) O10 0.068(4) 0.042(4) 0.090(5) -0.039(4) -0.009(4) 0.021(3) O11 0.185(11) 0.121(11) 0.220(14) 0.093(10) 0.153(11) 0.026(8) Cl2' 0.053(2) 0.0436(19) 0.0305(10) -0.0005(9) 0.0031(10) 0.0202(14) O8' 0.062(3) 0.167(9) 0.144(7) 0.133(7) 0.044(4) 0.061(4) O9' 0.046(7) 0.045(6) 0.061(8) -0.012(5) 0.005(5) -0.003(5) O10' 0.076(3) 0.077(4) 0.048(3) -0.023(2) 0.027(2) -0.007(2) O11' 0.031(2) 0.081(4) 0.140(6) -0.067(5) -0.011(3) -0.003(3) O12 0.054(3) 0.094(4) 0.062(3) 0.017(3) -0.024(2) -0.027(3) C50 0.043(4) 0.066(5) 0.054(4) -0.001(3) 0.026(3) 0.033(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 Mn2 3.1215(5) . ? Mn1 O1 1.8729(16) . ? Mn1 O3 1.8190(15) . ? Mn1 N1 2.0188(18) . ? Mn1 N2 2.2211(19) . ? Mn1 N3 2.2074(19) . ? Mn1 N5 2.239(2) . ? Mn2 O2 1.8883(16) . ? Mn2 O3 1.7819(15) . ? Mn2 N6 2.1612(19) . ? Mn2 N7 2.270(2) . ? Mn2 N8 2.0586(19) . ? Mn2 N9 2.252(2) . ? O1 C1 1.323(3) . ? O2 N1 1.389(2) . ? N1 C7 1.302(3) . ? N2 C14 1.488(3) . ? N2 C20 1.497(3) . ? N2 C26 1.485(3) . ? N3 C15 1.340(3) . ? N3 C19 1.339(3) . ? N4 C21 1.348(3) . ? N4 C25 1.341(3) . ? N5 C27 1.345(3) . ? N5 C31 1.341(3) . ? N6 C32 1.485(3) . ? N6 C38 1.500(3) . ? N6 C44 1.481(3) . ? N7 C33 1.336(3) . ? N7 C37 1.347(3) . ? N8 C39 1.347(3) . ? N8 C43 1.345(3) . ? N9 C45 1.343(3) . ? N9 C49 1.345(3) . ? C1 C2 1.406(3) . ? C1 C6 1.408(3) . ? C2 C3 1.372(3) . ? C3 C4 1.383(4) . ? C4 C5 1.373(4) . ? C5 C6 1.407(3) . ? C6 C7 1.465(3) . ? C7 C8 1.496(3) . ? C8 C9 1.392(3) . ? C8 C13 1.384(3) . ? C9 C12 1.384(3) . ? C10 C11 1.382(4) . ? C10 C13 1.392(3) . ? C11 C12 1.380(4) . ? C14 C15 1.509(3) . ? C15 C16 1.384(3) . ? C16 C17 1.378(4) . ? C17 C18 1.377(4) . ? C18 C19 1.378(4) . ? C20 C21 1.508(3) . ? C21 C22 1.380(3) . ? C22 C23 1.380(4) . ? C23 C24 1.376(4) . ? C24 C25 1.378(4) . ? C26 C27 1.508(3) . ? C27 C28 1.380(3) . ? C28 C29 1.392(3) . ? C29 C30 1.379(4) . ? C30 C31 1.381(3) . ? C32 C33 1.505(4) . ? C33 C34 1.388(4) . ? C34 C35 1.385(5) . ? C35 C36 1.366(5) . ? C36 C37 1.377(4) . ? C38 C39 1.500(3) . ? C39 C40 1.385(3) . ? C40 C41 1.380(4) . ? C41 C42 1.382(4) . ? C42 C43 1.382(3) . ? C44 C45 1.498(4) . ? C45 C46 1.384(4) . ? C46 C47 1.377(5) . ? C47 C48 1.380(5) . ? C48 C49 1.376(4) . ? Cl1 O4 1.450(5) . ? Cl1 O5 1.444(7) . ? Cl1 O6 1.430(5) . ? Cl1 O7 1.437(4) . ? Cl1' O4' 1.427(10) . ? Cl1' O5' 1.453(12) . ? Cl1' O6' 1.444(10) . ? Cl1' O7' 1.408(9) . ? Cl2 O8 1.422(8) . ? Cl2 O9 1.449(9) . ? Cl2 O10 1.395(8) . ? Cl2 O11 1.407(9) . ? Cl2' O8' 1.404(7) . ? Cl2' O9' 1.453(8) . ? Cl2' O10' 1.430(7) . ? Cl2' O11' 1.391(7) . ? O12 C50 1.252(8) . ? 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 Mn2 Mn1 O1 150.13(5) . . ? Mn2 Mn1 O3 29.56(5) . . ? Mn2 Mn1 N1 62.24(5) . . ? Mn2 Mn1 N2 116.68(5) . . ? Mn2 Mn1 N3 103.53(5) . . ? Mn2 Mn1 N5 92.46(5) . . ? O1 Mn1 O3 179.39(8) . . ? O1 Mn1 N1 88.02(7) . . ? O1 Mn1 N2 92.67(7) . . ? O1 Mn1 N3 88.22(7) . . ? O1 Mn1 N5 89.01(7) . . ? O3 Mn1 N1 91.63(7) . . ? O3 Mn1 N2 87.73(7) . . ? O3 Mn1 N3 91.43(7) . . ? O3 Mn1 N5 91.54(7) . . ? N1 Mn1 N2 174.77(7) . . ? N1 Mn1 N3 109.33(8) . . ? N1 Mn1 N5 98.32(7) . . ? N2 Mn1 N3 75.87(7) . . ? N2 Mn1 N5 76.52(7) . . ? N3 Mn1 N5 152.08(7) . . ? Mn1 Mn2 O2 64.94(5) . . ? Mn1 Mn2 O3 30.24(5) . . ? Mn1 Mn2 N6 124.70(5) . . ? Mn1 Mn2 N7 100.06(5) . . ? Mn1 Mn2 N8 152.96(5) . . ? Mn1 Mn2 N9 100.90(5) . . ? O2 Mn2 O3 95.15(7) . . ? O2 Mn2 N6 170.21(7) . . ? O2 Mn2 N7 101.85(7) . . ? O2 Mn2 N8 88.17(7) . . ? O2 Mn2 N9 106.14(8) . . ? O3 Mn2 N6 94.46(7) . . ? O3 Mn2 N7 93.01(7) . . ? O3 Mn2 N8 174.44(7) . . ? O3 Mn2 N9 94.50(7) . . ? N6 Mn2 N7 75.75(7) . . ? N6 Mn2 N8 82.10(7) . . ? N6 Mn2 N9 74.92(7) . . ? N7 Mn2 N8 81.92(7) . . ? N7 Mn2 N9 150.18(7) . . ? N8 Mn2 N9 88.85(7) . . ? Mn1 O1 C1 132.21(14) . . ? Mn2 O2 N1 117.91(12) . . ? Mn1 O3 Mn2 120.19(9) . . ? Mn1 N1 O2 114.35(13) . . ? Mn1 N1 C7 131.22(15) . . ? O2 N1 C7 114.26(17) . . ? Mn1 N2 C14 104.60(13) . . ? Mn1 N2 C20 112.43(13) . . ? Mn1 N2 C26 104.50(13) . . ? C14 N2 C20 111.50(17) . . ? C14 N2 C26 111.74(17) . . ? C20 N2 C26 111.66(17) . . ? Mn1 N3 C15 113.79(15) . . ? Mn1 N3 C19 126.94(17) . . ? C15 N3 C19 119.2(2) . . ? C21 N4 C25 117.0(2) . . ? Mn1 N5 C27 113.21(14) . . ? Mn1 N5 C31 126.93(16) . . ? C27 N5 C31 118.9(2) . . ? Mn2 N6 C32 107.85(14) . . ? Mn2 N6 C38 108.35(13) . . ? Mn2 N6 C44 108.06(14) . . ? C32 N6 C38 111.75(18) . . ? C32 N6 C44 110.50(19) . . ? C38 N6 C44 110.20(18) . . ? Mn2 N7 C33 113.74(17) . . ? Mn2 N7 C37 127.32(18) . . ? C33 N7 C37 118.9(2) . . ? Mn2 N8 C39 114.89(15) . . ? Mn2 N8 C43 124.20(16) . . ? C39 N8 C43 119.7(2) . . ? Mn2 N9 C45 112.84(16) . . ? Mn2 N9 C49 127.97(18) . . ? C45 N9 C49 118.7(2) . . ? O1 C1 C2 117.3(2) . . ? O1 C1 C6 124.2(2) . . ? C2 C1 C6 118.4(2) . . ? C1 C2 C3 121.4(2) . . ? C2 C3 C4 120.4(2) . . ? C3 C4 C5 119.3(2) . . ? C4 C5 C6 121.8(2) . . ? C1 C6 C5 118.6(2) . . ? C1 C6 C7 122.9(2) . . ? C5 C6 C7 118.6(2) . . ? N1 C7 C6 120.7(2) . . ? N1 C7 C8 117.27(19) . . ? C6 C7 C8 122.04(19) . . ? C7 C8 C9 120.7(2) . . ? C7 C8 C13 119.0(2) . . ? C9 C8 C13 120.0(2) . . ? C8 C9 C12 119.7(2) . . ? C11 C10 C13 120.3(2) . . ? C10 C11 C12 119.9(2) . . ? C9 C12 C11 120.4(2) . . ? C8 C13 C10 119.6(2) . . ? N2 C14 C15 109.88(18) . . ? N3 C15 C14 116.0(2) . . ? N3 C15 C16 121.3(2) . . ? C14 C15 C16 122.7(2) . . ? C15 C16 C17 119.3(3) . . ? C16 C17 C18 119.2(3) . . ? C17 C18 C19 118.8(3) . . ? N3 C19 C18 122.2(3) . . ? N2 C20 C21 114.64(18) . . ? N4 C21 C20 116.11(19) . . ? N4 C21 C22 122.5(2) . . ? C20 C21 C22 121.4(2) . . ? C21 C22 C23 119.4(2) . . ? C22 C23 C24 118.7(2) . . ? C23 C24 C25 118.6(2) . . ? N4 C25 C24 123.8(2) . . ? N2 C26 C27 109.84(18) . . ? N5 C27 C26 114.4(2) . . ? N5 C27 C28 122.1(2) . . ? C26 C27 C28 123.5(2) . . ? C27 C28 C29 118.4(2) . . ? C28 C29 C30 119.8(2) . . ? C29 C30 C31 118.3(2) . . ? N5 C31 C30 122.5(2) . . ? N6 C32 C33 111.8(2) . . ? N7 C33 C32 114.9(2) . . ? N7 C33 C34 121.4(3) . . ? C32 C33 C34 123.6(2) . . ? C33 C34 C35 118.9(3) . . ? C34 C35 C36 119.7(3) . . ? C35 C36 C37 118.6(3) . . ? N7 C37 C36 122.4(3) . . ? N6 C38 C39 113.40(18) . . ? N8 C39 C38 117.6(2) . . ? N8 C39 C40 120.7(2) . . ? C38 C39 C40 121.6(2) . . ? C39 C40 C41 119.7(2) . . ? C40 C41 C42 119.3(2) . . ? C41 C42 C43 118.6(2) . . ? N8 C43 C42 121.9(2) . . ? N6 C44 C45 111.0(2) . . ? N9 C45 C44 116.2(2) . . ? N9 C45 C46 122.0(3) . . ? C44 C45 C46 121.8(3) . . ? C45 C46 C47 118.7(3) . . ? C46 C47 C48 119.5(3) . . ? C47 C48 C49 118.9(3) . . ? N9 C49 C48 122.1(3) . . ? O4 Cl1 O5 108.9(6) . . ? O4 Cl1 O6 109.1(3) . . ? O4 Cl1 O7 107.9(3) . . ? O5 Cl1 O6 110.7(6) . . ? O5 Cl1 O7 109.9(7) . . ? O6 Cl1 O7 110.4(4) . . ? O4' Cl1' O5' 107.7(12) . . ? O4' Cl1' O6' 108.7(8) . . ? O4' Cl1' O7' 113.8(10) . . ? O5' Cl1' O6' 108.9(15) . . ? O5' Cl1' O7' 109.4(13) . . ? O6' Cl1' O7' 108.2(9) . . ? O8 Cl2 O9 109.6(9) . . ? O8 Cl2 O10 108.9(6) . . ? O8 Cl2 O11 106.5(7) . . ? O9 Cl2 O10 112.2(9) . . ? O9 Cl2 O11 110.0(9) . . ? O10 Cl2 O11 109.4(8) . . ? O8' Cl2' O9' 108.3(7) . . ? O8' Cl2' O10' 108.0(6) . . ? O8' Cl2' O11' 114.1(7) . . ? O9' Cl2' O10' 108.6(7) . . ? O9' Cl2' O11' 110.9(7) . . ? O10' Cl2' O11' 106.7(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 O1 Mn1 Mn2 O2 1.89(13) . . . . ? O1 Mn1 Mn2 O3 178.93(15) . . . . ? O1 Mn1 Mn2 N6 179.92(13) . . . . ? O1 Mn1 Mn2 N7 100.37(12) . . . . ? O1 Mn1 Mn2 N8 8.44(17) . . . . ? O1 Mn1 Mn2 N9 -100.96(12) . . . . ? O3 Mn1 Mn2 O2 -177.04(12) . . . . ? O3 Mn1 Mn2 N6 0.99(12) . . . . ? O3 Mn1 Mn2 N7 -78.56(12) . . . . ? O3 Mn1 Mn2 N8 -170.49(16) . . . . ? O3 Mn1 Mn2 N9 80.11(12) . . . . ? N1 Mn1 Mn2 O2 -3.93(8) . . . . ? N1 Mn1 Mn2 O3 173.10(12) . . . . ? N1 Mn1 Mn2 N6 174.10(9) . . . . ? N1 Mn1 Mn2 N7 94.54(8) . . . . ? N1 Mn1 Mn2 N8 2.62(13) . . . . ? N1 Mn1 Mn2 N9 -106.79(8) . . . . ? N2 Mn1 Mn2 O2 170.31(8) . . . . ? N2 Mn1 Mn2 O3 -12.65(12) . . . . ? N2 Mn1 Mn2 N6 -11.66(8) . . . . ? N2 Mn1 Mn2 N7 -91.21(8) . . . . ? N2 Mn1 Mn2 N8 176.86(13) . . . . ? N2 Mn1 Mn2 N9 67.46(8) . . . . ? N3 Mn1 Mn2 O2 -108.89(8) . . . . ? N3 Mn1 Mn2 O3 68.14(12) . . . . ? N3 Mn1 Mn2 N6 69.14(8) . . . . ? N3 Mn1 Mn2 N7 -10.42(8) . . . . ? N3 Mn1 Mn2 N8 -102.34(13) . . . . ? N3 Mn1 Mn2 N9 148.25(8) . . . . ? N5 Mn1 Mn2 O2 94.18(8) . . . . ? N5 Mn1 Mn2 O3 -88.78(11) . . . . ? N5 Mn1 Mn2 N6 -87.79(8) . . . . ? N5 Mn1 Mn2 N7 -167.34(7) . . . . ? N5 Mn1 Mn2 N8 100.73(13) . . . . ? N5 Mn1 Mn2 N9 -8.68(7) . . . . ? Mn2 Mn1 O1 C1 -14.9(3) . . . . ? O3 Mn1 O1 C1 45(7) . . . . ? N1 Mn1 O1 C1 -9.8(2) . . . . ? N2 Mn1 O1 C1 175.4(2) . . . . ? N3 Mn1 O1 C1 99.7(2) . . . . ? N5 Mn1 O1 C1 -108.1(2) . . . . ? Mn1 Mn2 O2 N1 5.73(12) . . . . ? O3 Mn2 O2 N1 4.23(15) . . . . ? N6 Mn2 O2 N1 -164.7(4) . . . . ? N7 Mn2 O2 N1 -89.95(15) . . . . ? N8 Mn2 O2 N1 -171.30(15) . . . . ? N9 Mn2 O2 N1 100.43(15) . . . . ? O2 Mn2 O3 Mn1 2.70(11) . . . . ? N6 Mn2 O3 Mn1 -179.18(10) . . . . ? N7 Mn2 O3 Mn1 104.89(10) . . . . ? N8 Mn2 O3 Mn1 129.2(7) . . . . ? N9 Mn2 O3 Mn1 -103.99(10) . . . . ? O1 Mn1 O3 Mn2 -61(7) . . . . ? N1 Mn1 O3 Mn2 -6.10(11) . . . . ? N2 Mn1 O3 Mn2 168.71(10) . . . . ? N3 Mn1 O3 Mn2 -115.49(10) . . . . ? N5 Mn1 O3 Mn2 92.27(10) . . . . ? Mn2 O2 N1 Mn1 -8.83(18) . . . . ? Mn2 O2 N1 C7 175.45(15) . . . . ? Mn2 Mn1 N1 O2 5.32(11) . . . . ? Mn2 Mn1 N1 C7 -179.9(2) . . . . ? O1 Mn1 N1 O2 -171.78(14) . . . . ? O1 Mn1 N1 C7 3.0(2) . . . . ? O3 Mn1 N1 O2 8.72(14) . . . . ? O3 Mn1 N1 C7 -176.5(2) . . . . ? N2 Mn1 N1 O2 -74.1(8) . . . . ? N2 Mn1 N1 C7 100.7(8) . . . . ? N3 Mn1 N1 O2 100.81(14) . . . . ? N3 Mn1 N1 C7 -84.4(2) . . . . ? N5 Mn1 N1 O2 -83.07(14) . . . . ? N5 Mn1 N1 C7 91.7(2) . . . . ? Mn2 Mn1 N2 C14 63.14(14) . . . . ? Mn2 Mn1 N2 C20 -175.71(12) . . . . ? Mn2 Mn1 N2 C26 -54.42(13) . . . . ? O1 Mn1 N2 C14 -122.60(14) . . . . ? O1 Mn1 N2 C20 -1.45(14) . . . . ? O1 Mn1 N2 C26 119.83(13) . . . . ? O3 Mn1 N2 C14 56.93(14) . . . . ? O3 Mn1 N2 C20 178.09(14) . . . . ? O3 Mn1 N2 C26 -60.63(13) . . . . ? N1 Mn1 N2 C14 140.0(7) . . . . ? N1 Mn1 N2 C20 -98.9(8) . . . . ? N1 Mn1 N2 C26 22.4(8) . . . . ? N3 Mn1 N2 C14 -35.12(13) . . . . ? N3 Mn1 N2 C20 86.04(14) . . . . ? N3 Mn1 N2 C26 -152.68(14) . . . . ? N5 Mn1 N2 C14 149.06(14) . . . . ? N5 Mn1 N2 C20 -89.79(14) . . . . ? N5 Mn1 N2 C26 31.49(13) . . . . ? Mn2 Mn1 N3 C15 -95.54(16) . . . . ? Mn2 Mn1 N3 C19 87.2(2) . . . . ? O1 Mn1 N3 C15 112.23(17) . . . . ? O1 Mn1 N3 C19 -65.0(2) . . . . ? O3 Mn1 N3 C15 -68.27(17) . . . . ? O3 Mn1 N3 C19 114.5(2) . . . . ? N1 Mn1 N3 C15 -160.50(16) . . . . ? N1 Mn1 N3 C19 22.3(2) . . . . ? N2 Mn1 N3 C15 19.02(16) . . . . ? N2 Mn1 N3 C19 -158.2(2) . . . . ? N5 Mn1 N3 C15 27.7(3) . . . . ? N5 Mn1 N3 C19 -149.51(19) . . . . ? Mn2 Mn1 N5 C27 107.07(15) . . . . ? Mn2 Mn1 N5 C31 -84.41(18) . . . . ? O1 Mn1 N5 C27 -102.77(16) . . . . ? O1 Mn1 N5 C31 65.75(18) . . . . ? O3 Mn1 N5 C27 77.51(15) . . . . ? O3 Mn1 N5 C31 -113.97(18) . . . . ? N1 Mn1 N5 C27 169.38(15) . . . . ? N1 Mn1 N5 C31 -22.11(19) . . . . ? N2 Mn1 N5 C27 -9.79(15) . . . . ? N2 Mn1 N5 C31 158.73(19) . . . . ? N3 Mn1 N5 C27 -18.5(2) . . . . ? N3 Mn1 N5 C31 150.06(18) . . . . ? Mn1 Mn2 N6 C32 -61.34(16) . . . . ? Mn1 Mn2 N6 C38 177.54(12) . . . . ? Mn1 Mn2 N6 C44 58.14(16) . . . . ? O2 Mn2 N6 C32 108.1(4) . . . . ? O2 Mn2 N6 C38 -13.0(5) . . . . ? O2 Mn2 N6 C44 -132.4(4) . . . . ? O3 Mn2 N6 C32 -60.83(16) . . . . ? O3 Mn2 N6 C38 178.04(14) . . . . ? O3 Mn2 N6 C44 58.64(16) . . . . ? N7 Mn2 N6 C32 31.15(15) . . . . ? N7 Mn2 N6 C38 -89.98(15) . . . . ? N7 Mn2 N6 C44 150.63(16) . . . . ? N8 Mn2 N6 C32 114.77(16) . . . . ? N8 Mn2 N6 C38 -6.36(14) . . . . ? N8 Mn2 N6 C44 -125.76(16) . . . . ? N9 Mn2 N6 C32 -154.30(16) . . . . ? N9 Mn2 N6 C38 84.58(15) . . . . ? N9 Mn2 N6 C44 -34.82(15) . . . . ? Mn1 Mn2 N7 C33 107.65(16) . . . . ? Mn1 Mn2 N7 C37 -73.1(2) . . . . ? O2 Mn2 N7 C33 173.93(16) . . . . ? O2 Mn2 N7 C37 -6.9(2) . . . . ? O3 Mn2 N7 C33 78.02(17) . . . . ? O3 Mn2 N7 C37 -102.8(2) . . . . ? N6 Mn2 N7 C33 -15.82(16) . . . . ? N6 Mn2 N7 C37 163.4(2) . . . . ? N8 Mn2 N7 C33 -99.67(17) . . . . ? N8 Mn2 N7 C37 79.6(2) . . . . ? N9 Mn2 N7 C33 -26.4(2) . . . . ? N9 Mn2 N7 C37 152.78(19) . . . . ? Mn1 Mn2 N8 C39 167.52(11) . . . . ? Mn1 Mn2 N8 C43 0.4(3) . . . . ? O2 Mn2 N8 C39 173.45(16) . . . . ? O2 Mn2 N8 C43 6.33(18) . . . . ? O3 Mn2 N8 C39 46.7(8) . . . . ? O3 Mn2 N8 C43 -120.4(7) . . . . ? N6 Mn2 N8 C39 -5.42(16) . . . . ? N6 Mn2 N8 C43 -172.55(19) . . . . ? N7 Mn2 N8 C39 71.20(16) . . . . ? N7 Mn2 N8 C43 -95.92(19) . . . . ? N9 Mn2 N8 C39 -80.36(16) . . . . ? N9 Mn2 N8 C43 112.52(19) . . . . ? Mn1 Mn2 N9 C45 -100.18(16) . . . . ? Mn1 Mn2 N9 C49 72.0(2) . . . . ? O2 Mn2 N9 C45 -167.02(16) . . . . ? O2 Mn2 N9 C49 5.1(2) . . . . ? O3 Mn2 N9 C45 -70.33(17) . . . . ? O3 Mn2 N9 C49 101.8(2) . . . . ? N6 Mn2 N9 C45 23.09(16) . . . . ? N6 Mn2 N9 C49 -164.7(2) . . . . ? N7 Mn2 N9 C45 33.7(3) . . . . ? N7 Mn2 N9 C49 -154.09(19) . . . . ? N8 Mn2 N9 C45 105.21(17) . . . . ? N8 Mn2 N9 C49 -82.6(2) . . . . ? Mn1 O1 C1 C2 -170.85(16) . . . . ? Mn1 O1 C1 C6 11.2(3) . . . . ? O1 C1 C2 C3 -176.2(2) . . . . ? C6 C1 C2 C3 1.8(3) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C3 C4 C5 C6 1.5(4) . . . . ? C4 C5 C6 C1 -0.3(4) . . . . ? C4 C5 C6 C7 179.1(2) . . . . ? O1 C1 C6 C5 176.6(2) . . . . ? O1 C1 C6 C7 -2.8(3) . . . . ? C2 C1 C6 C5 -1.3(3) . . . . ? C2 C1 C6 C7 179.3(2) . . . . ? Mn1 N1 C7 C6 2.1(3) . . . . ? Mn1 N1 C7 C8 -176.45(15) . . . . ? O2 N1 C7 C6 176.96(18) . . . . ? O2 N1 C7 C8 -1.6(3) . . . . ? C1 C6 C7 N1 -3.5(3) . . . . ? C1 C6 C7 C8 175.0(2) . . . . ? C5 C6 C7 N1 177.1(2) . . . . ? C5 C6 C7 C8 -4.3(3) . . . . ? N1 C7 C8 C9 -75.5(3) . . . . ? N1 C7 C8 C13 98.2(3) . . . . ? C6 C7 C8 C9 105.9(3) . . . . ? C6 C7 C8 C13 -80.4(3) . . . . ? C7 C8 C9 C12 172.9(2) . . . . ? C13 C8 C9 C12 -0.7(3) . . . . ? C13 C10 C11 C12 -0.5(4) . . . . ? C10 C11 C12 C9 0.3(4) . . . . ? C8 C9 C12 C11 0.3(4) . . . . ? C7 C8 C13 C10 -173.2(2) . . . . ? C9 C8 C13 C10 0.5(3) . . . . ? C11 C10 C13 C8 0.1(4) . . . . ? Mn1 N2 C14 C15 47.3(2) . . . . ? C20 N2 C14 C15 -74.4(2) . . . . ? C26 N2 C14 C15 159.82(19) . . . . ? Mn1 N3 C15 C14 2.4(3) . . . . ? Mn1 N3 C15 C16 -178.6(2) . . . . ? C19 N3 C15 C14 179.8(2) . . . . ? C19 N3 C15 C16 -1.1(4) . . . . ? N2 C14 C15 N3 -34.8(3) . . . . ? N2 C14 C15 C16 146.1(2) . . . . ? N3 C15 C16 C17 1.2(4) . . . . ? C14 C15 C16 C17 -179.8(3) . . . . ? C15 C16 C17 C18 -0.9(4) . . . . ? C16 C17 C18 C19 0.6(4) . . . . ? Mn1 N3 C19 C18 177.9(2) . . . . ? C15 N3 C19 C18 0.8(4) . . . . ? C17 C18 C19 N3 -0.6(4) . . . . ? Mn1 N2 C20 C21 176.64(14) . . . . ? C14 N2 C20 C21 -66.2(2) . . . . ? C26 N2 C20 C21 59.5(2) . . . . ? C25 N4 C21 C20 178.1(2) . . . . ? C25 N4 C21 C22 -2.4(3) . . . . ? N2 C20 C21 N4 -83.6(2) . . . . ? N2 C20 C21 C22 96.9(3) . . . . ? N4 C21 C22 C23 1.5(4) . . . . ? C20 C21 C22 C23 -179.0(2) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C22 C23 C24 C25 -1.4(4) . . . . ? C21 N4 C25 C24 1.4(4) . . . . ? C23 C24 C25 N4 0.5(4) . . . . ? Mn1 N2 C26 C27 -49.54(19) . . . . ? C14 N2 C26 C27 -162.09(18) . . . . ? C20 N2 C26 C27 72.3(2) . . . . ? Mn1 N5 C27 C26 -15.2(2) . . . . ? Mn1 N5 C27 C28 166.37(18) . . . . ? C31 N5 C27 C26 175.27(19) . . . . ? C31 N5 C27 C28 -3.2(3) . . . . ? N2 C26 C27 N5 45.1(3) . . . . ? N2 C26 C27 C28 -136.5(2) . . . . ? N5 C27 C28 C29 1.7(3) . . . . ? C26 C27 C28 C29 -176.6(2) . . . . ? C27 C28 C29 C30 1.4(4) . . . . ? C28 C29 C30 C31 -2.9(4) . . . . ? Mn1 N5 C31 C30 -166.40(17) . . . . ? C27 N5 C31 C30 1.5(3) . . . . ? C29 C30 C31 N5 1.5(4) . . . . ? Mn2 N6 C32 C33 -44.1(2) . . . . ? C38 N6 C32 C33 74.9(2) . . . . ? C44 N6 C32 C33 -162.0(2) . . . . ? Mn2 N7 C33 C32 -3.9(3) . . . . ? Mn2 N7 C33 C34 178.78(19) . . . . ? C37 N7 C33 C32 176.8(2) . . . . ? C37 N7 C33 C34 -0.5(4) . . . . ? N6 C32 C33 N7 32.2(3) . . . . ? N6 C32 C33 C34 -150.6(2) . . . . ? N7 C33 C34 C35 1.0(4) . . . . ? C32 C33 C34 C35 -176.1(3) . . . . ? C33 C34 C35 C36 -0.9(4) . . . . ? C34 C35 C36 C37 0.3(5) . . . . ? Mn2 N7 C37 C36 -179.3(2) . . . . ? C33 N7 C37 C36 -0.1(4) . . . . ? C35 C36 C37 N7 0.2(4) . . . . ? Mn2 N6 C38 C39 16.2(2) . . . . ? C32 N6 C38 C39 -102.5(2) . . . . ? C44 N6 C38 C39 134.2(2) . . . . ? Mn2 N8 C39 C38 16.8(2) . . . . ? Mn2 N8 C39 C40 -166.43(17) . . . . ? C43 N8 C39 C38 -175.4(2) . . . . ? C43 N8 C39 C40 1.3(3) . . . . ? N6 C38 C39 N8 -22.6(3) . . . . ? N6 C38 C39 C40 160.7(2) . . . . ? N8 C39 C40 C41 -1.7(3) . . . . ? C38 C39 C40 C41 174.9(2) . . . . ? C39 C40 C41 C42 0.5(4) . . . . ? C40 C41 C42 C43 0.9(4) . . . . ? Mn2 N8 C43 C42 166.68(17) . . . . ? C39 N8 C43 C42 0.1(3) . . . . ? C41 C42 C43 N8 -1.2(4) . . . . ? Mn2 N6 C44 C45 43.4(2) . . . . ? C32 N6 C44 C45 161.2(2) . . . . ? C38 N6 C44 C45 -74.8(2) . . . . ? Mn2 N9 C45 C44 -5.7(3) . . . . ? Mn2 N9 C45 C46 172.8(2) . . . . ? C49 N9 C45 C44 -178.7(2) . . . . ? C49 N9 C45 C46 -0.1(4) . . . . ? N6 C44 C45 N9 -25.0(3) . . . . ? N6 C44 C45 C46 156.5(3) . . . . ? N9 C45 C46 C47 -0.6(5) . . . . ? C44 C45 C46 C47 177.9(3) . . . . ? C45 C46 C47 C48 0.7(5) . . . . ? C46 C47 C48 C49 -0.1(5) . . . . ? Mn2 N9 C49 C48 -171.0(2) . . . . ? C45 N9 C49 C48 0.7(4) . . . . ? C47 C48 C49 N9 -0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.588 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.063 _vrf_PLAT420_4-eb2190 ; PROBLEM: Without Acceptor *O12 - *H12O ... ? RESPONSE: Atom H12O forms part of a disordered MeOH. The atom was added geometrically, without considering H-bonding acceptors, since the disorder makes discussion of H-bonding interaction moot. The atom was added to the model more for the sake of completeness. ; _vrf_PLAT214_4-eb2190 ; PROBLEM: Atom O8' (Anion/Solvent) ADP max/min Ratio 4.1 prola RESPONSE: This is part of a disordered perchlorate, which is discussed in _refine_special_details. ; _vrf_PLAT002_4-eb2190 ; PROBLEM: Number of Distance or Angle Restraints on AtSite 20 RESPONSE: Two perchlorate anions were refined using disorder models. See _refine_special_details. ; #################### ## END OF CIF _database_code_depnum_ccdc_archive 'CCDC 950514'