# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name L.Thompson _publ_contact_author_address ; Department of Chemistry Memorial University of St John's Newfoundland A1B 3X7 CANADA ; _publ_section_title ; A self-assembled hexa-decanuclear 4 x [2x2] Mn(II)16 square grid from a pyridazine bis hydrazone ligand synthesis, structure and magnetism ; _publ_contact_author_email LTHOMP@MUN.CA loop_ _publ_author_name L.Thompson L.N.Dawe S.Dey # Attachment 'SD186Anew.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 616858' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H96 Mn16 N66 O30' _chemical_formula_weight 4109.91 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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 40.32(2) _cell_length_b 12.990(6) _cell_length_c 22.830(12) _cell_angle_alpha 90.00 _cell_angle_beta 117.670(8) _cell_angle_gamma 90.00 _cell_volume 10590(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 17290 _cell_measurement_theta_min 1.7957 _cell_measurement_theta_max 30.7747 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4124 _exptl_absorpt_coefficient_mu 0.988 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7257 _exptl_absorpt_correction_T_max 0.9074 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 35421 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16847 _reflns_number_gt 14242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 843.2 electrons per unit cell in three voids (3573.1 A^3), that is 422 electrons per asymmetric unit. Disordered solvent waters appeared to be present prior to the application of Squeeze, though a good point atom model could not be achieved for these. The application of squeeze gave a good improvement in the data statistics and allowed for a full refinement of the framework structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.144 0.084 0.514 3557.6 837.6 2 0.500 0.317 0.500 7.2 2.8 3 0.000 0.817 0.500 7.2 2.8 _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^)+(0.1376P)^2^+23.7401P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00121(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.16(3) _refine_ls_number_reflns 16847 _refine_ls_number_parameters 1130 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.2446 _refine_ls_wR_factor_gt 0.2330 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.28503(4) 0.25204(17) -0.18776(8) 0.0783(5) Uani 1 1 d . . . Mn2 Mn 0.35436(4) 0.39582(13) -0.01973(7) 0.0611(4) Uani 1 1 d . . . Mn3 Mn 0.42467(4) 0.40964(11) 0.15521(6) 0.0561(3) Uani 1 1 d . . . Mn4 Mn 0.49459(4) 0.29032(11) 0.32911(7) 0.0603(4) Uani 1 1 d . . . Mn5 Mn 0.36097(4) 0.14326(13) -0.23095(7) 0.0627(4) Uani 1 1 d . . . Mn6 Mn 0.42737(3) 0.27020(11) -0.06557(6) 0.0554(3) Uani 1 1 d . . . Mn7 Mn 0.49727(4) 0.27456(10) 0.11107(6) 0.0531(3) Uani 1 1 d . . . Mn8 Mn 0.56354(4) 0.15501(10) 0.27781(6) 0.0542(3) Uani 1 1 d . . . O1 O 0.32149(18) 0.2619(7) -0.0791(3) 0.074(2) Uani 1 1 d . . . O2 O 0.44582(18) 0.2881(5) 0.2321(3) 0.0582(14) Uani 1 1 d . . . O3 O 0.38559(16) 0.1544(6) -0.1200(3) 0.0617(15) Uani 1 1 d . . . O4 O 0.50686(16) 0.1644(5) 0.1889(3) 0.0560(14) Uani 1 1 d . . . O5 O 0.54446(17) 0.2868(5) 0.3129(3) 0.0616(15) Uani 1 1 d . . . O6 O 0.67829(18) 0.2625(7) 0.2325(3) 0.0710(18) Uani 1 1 d . . . O7 O 0.48131(16) 0.3960(5) 0.1592(3) 0.0610(16) Uani 1 1 d . . . O8 O 0.61462(17) 0.3871(6) 0.0783(3) 0.0643(16) Uani 1 1 d . . . O9 O 0.3969(2) 0.4687(8) 0.0609(3) 0.091(3) Uani 1 1 d . . . O10 O 0.4706(2) 0.3422(6) 0.0183(3) 0.082(2) Uani 1 1 d . . . O11 O 0.58800(19) 0.0971(7) 0.2237(3) 0.079(2) Uani 1 1 d . . . O12 O 0.5357(2) 0.1894(5) 0.0918(4) 0.075(2) Uani 1 1 d . . . O13 O 0.3219(4) 0.2476(13) 0.1425(7) 0.158(5) Uiso 1 1 d . . . O14 O 0.2758(4) 0.3359(11) 0.1279(7) 0.149(5) Uiso 1 1 d . . . O15 O 0.3136(6) 0.275(2) 0.2275(12) 0.254(10) Uiso 1 1 d . . . N1 N 0.2460(3) 0.1477(12) -0.2688(5) 0.093(3) Uani 1 1 d . . . N2 N 0.2831(2) 0.1174(13) -0.1459(5) 0.134(6) Uani 1 1 d . . . N3 N 0.3022(2) 0.1018(9) -0.0775(5) 0.081(3) Uani 1 1 d . . . N4 N 0.36496(17) 0.2641(6) 0.0490(3) 0.0528(17) Uani 1 1 d . . . N5 N 0.39034(19) 0.2668(6) 0.1116(4) 0.0557(17) Uani 1 1 d . . . N6 N 0.4380(2) 0.1212(7) 0.2552(4) 0.071(2) Uani 1 1 d . . . N7 N 0.4694(2) 0.1421(6) 0.3159(4) 0.066(2) Uani 1 1 d . . . N8 N 0.5265(2) 0.1936(9) 0.4232(4) 0.075(3) Uani 1 1 d . . . N9 N 0.3173(2) 0.0546(7) -0.3182(4) 0.066(2) Uani 1 1 d . . . N10 N 0.3456(2) 0.0108(7) -0.1916(4) 0.068(2) Uani 1 1 d . . . N11 N 0.36473(19) -0.0097(7) -0.1245(4) 0.0608(19) Uani 1 1 d . . . N12 N 0.42767(17) 0.1436(6) 0.0067(4) 0.0544(17) Uani 1 1 d . . . N13 N 0.45290(17) 0.1475(6) 0.0694(3) 0.0518(16) Uani 1 1 d . . . N14 N 0.4987(2) -0.0034(6) 0.2123(4) 0.0582(18) Uani 1 1 d . . . N15 N 0.5296(2) 0.0194(6) 0.2705(4) 0.0589(17) Uani 1 1 d . . . N16 N 0.5932(2) 0.0690(7) 0.3743(4) 0.066(2) Uani 1 1 d . . . N17 N 0.4629(2) 0.3886(6) 0.3676(4) 0.067(2) Uani 1 1 d . . . N18 N 0.5255(3) 0.4335(7) 0.3652(4) 0.076(2) Uani 1 1 d . . . N19 N 0.5576(2) 0.4497(6) 0.3610(4) 0.069(2) Uani 1 1 d . . . N20 N 0.6039(2) 0.2900(8) 0.2971(3) 0.070(2) Uani 1 1 d . . . N21 N 0.63100(19) 0.2841(7) 0.2799(3) 0.0596(18) Uani 1 1 d . . . N22 N 0.6985(2) 0.4316(8) 0.2596(5) 0.085(3) Uani 1 1 d . . . N23 N 0.7200(2) 0.4032(9) 0.2310(5) 0.088(3) Uani 1 1 d . . . N24 N 0.7612(2) 0.3351(8) 0.1754(4) 0.076(3) Uani 1 1 d D . . N25 N 0.3941(2) 0.4999(7) 0.1994(4) 0.067(2) Uani 1 1 d . . . N26 N 0.4616(2) 0.5370(6) 0.2130(4) 0.0559(17) Uani 1 1 d . . . N27 N 0.4954(2) 0.5494(6) 0.2132(4) 0.063(2) Uani 1 1 d . . . N28 N 0.54291(19) 0.3986(6) 0.1490(3) 0.0493(15) Uani 1 1 d . . . N29 N 0.56980(18) 0.3979(6) 0.1315(3) 0.0542(16) Uani 1 1 d . . . N30 N 0.6390(2) 0.5463(7) 0.1197(4) 0.068(2) Uani 1 1 d . . . N31 N 0.6600(2) 0.5266(7) 0.0865(4) 0.067(2) Uani 1 1 d . . . N32 N 0.6963(2) 0.4798(8) 0.0214(4) 0.074(2) Uani 1 1 d . . . N33 N 0.3001(5) 0.2773(16) 0.1640(9) 0.146(5) Uiso 1 1 d . . . C1 C 0.2271(4) 0.1602(12) -0.3330(6) 0.113(5) Uani 1 1 d . . . H1 H 0.2304 0.2241 -0.3498 0.136 Uiso 1 1 calc R . . C2 C 0.2041(4) 0.0945(17) -0.3767(6) 0.125(6) Uani 1 1 d . . . H2 H 0.1924 0.1104 -0.4226 0.150 Uiso 1 1 calc R . . C3 C 0.1970(5) 0.0007(19) -0.3545(8) 0.149(8) Uani 1 1 d . . . H3 H 0.1787 -0.0461 -0.3836 0.179 Uiso 1 1 calc R . . C4 C 0.2177(4) -0.0195(18) -0.2896(7) 0.135(7) Uani 1 1 d . . . H4 H 0.2160 -0.0851 -0.2728 0.161 Uiso 1 1 calc R . . C5 C 0.2422(3) 0.0574(12) -0.2455(6) 0.086(4) Uani 1 1 d . . . C6 C 0.2622(3) 0.0352(9) -0.1760(5) 0.070(3) Uani 1 1 d . . . H5 H 0.2609 -0.0268 -0.1552 0.084 Uiso 1 1 calc R . . C7 C 0.3231(2) 0.1782(7) -0.0498(4) 0.056(2) Uani 1 1 d . . . C8 C 0.3473(3) 0.1707(7) 0.0231(5) 0.062(2) Uani 1 1 d . . . C9 C 0.3535(3) 0.0891(8) 0.0608(5) 0.063(2) Uani 1 1 d . . . H6 H 0.3396 0.0276 0.0434 0.075 Uiso 1 1 calc R . . C10 C 0.3798(3) 0.0939(10) 0.1240(5) 0.073(3) Uani 1 1 d . . . H7 H 0.3854 0.0339 0.1507 0.087 Uiso 1 1 calc R . . C11 C 0.3989(2) 0.1837(8) 0.1512(5) 0.059(2) Uani 1 1 d . . . C12 C 0.4296(2) 0.1996(6) 0.2179(4) 0.0501(19) Uani 1 1 d . . . C13 C 0.4812(4) 0.0774(12) 0.3633(6) 0.097(4) Uani 1 1 d . . . H8 H 0.4679 0.0156 0.3602 0.116 Uiso 1 1 calc R . . C14 C 0.5155(4) 0.1012(9) 0.4219(6) 0.084(3) Uani 1 1 d . . . C15 C 0.5316(4) 0.0286(10) 0.4692(7) 0.127(7) Uani 1 1 d . . . H9 H 0.5213 -0.0383 0.4653 0.152 Uiso 1 1 calc R . . C16 C 0.5644(5) 0.0591(11) 0.5237(8) 0.115(5) Uani 1 1 d . . . H10 H 0.5778 0.0107 0.5578 0.138 Uiso 1 1 calc R . . C17 C 0.5782(5) 0.1601(19) 0.5296(7) 0.137(8) Uani 1 1 d . . . H11 H 0.6000 0.1833 0.5673 0.165 Uiso 1 1 calc R . . C18 C 0.5582(4) 0.2198(11) 0.4784(5) 0.095(4) Uani 1 1 d . . . H12 H 0.5670 0.2883 0.4803 0.114 Uiso 1 1 calc R . . C19 C 0.3001(3) 0.0794(11) -0.3819(6) 0.088(3) Uani 1 1 d . . . H13 H 0.3094 0.1390 -0.3935 0.105 Uiso 1 1 calc R . . C20 C 0.2730(5) 0.034(2) -0.4297(5) 0.166(10) Uani 1 1 d . . . H14 H 0.2585 0.0650 -0.4717 0.199 Uiso 1 1 calc R . . C21 C 0.2665(4) -0.0712(17) -0.4125(5) 0.132(7) Uani 1 1 d . . . H15 H 0.2501 -0.1153 -0.4470 0.159 Uiso 1 1 calc R . . C22 C 0.2844(4) -0.1110(14) -0.3438(7) 0.123(6) Uani 1 1 d . . . H16 H 0.2803 -0.1780 -0.3317 0.147 Uiso 1 1 calc R . . C23 C 0.3087(3) -0.0365(9) -0.2982(5) 0.067(3) Uani 1 1 d . . . C24 C 0.3253(3) -0.0650(8) -0.2304(5) 0.066(2) Uani 1 1 d . . . H17 H 0.3222 -0.1303 -0.2148 0.079 Uiso 1 1 calc R . . C25 C 0.3852(2) 0.0724(8) -0.0951(5) 0.060(2) Uani 1 1 d . . . C26 C 0.4101(3) 0.0626(8) -0.0200(4) 0.061(2) Uani 1 1 d . . . C27 C 0.4155(3) -0.0287(9) 0.0143(5) 0.067(3) Uani 1 1 d . . . H18 H 0.4024 -0.0899 -0.0067 0.080 Uiso 1 1 calc R . . C28 C 0.4404(3) -0.0262(8) 0.0800(5) 0.065(2) Uani 1 1 d . . . H19 H 0.4444 -0.0844 0.1077 0.078 Uiso 1 1 calc R . . C29 C 0.4599(2) 0.0660(7) 0.1046(4) 0.055(2) Uani 1 1 d . . . C30 C 0.4908(2) 0.0798(7) 0.1743(5) 0.056(2) Uani 1 1 d . . . C31 C 0.5450(3) -0.0546(7) 0.3128(5) 0.074(3) Uani 1 1 d . . . H20 H 0.5346 -0.1220 0.3044 0.088 Uiso 1 1 calc R . . C32 C 0.5786(3) -0.0308(9) 0.3733(6) 0.085(3) Uani 1 1 d . . . C33 C 0.5971(4) -0.0996(12) 0.4216(6) 0.121(6) Uani 1 1 d . . . H21 H 0.5874 -0.1667 0.4198 0.145 Uiso 1 1 calc R . . C34 C 0.6324(4) -0.0686(9) 0.4764(5) 0.089(4) Uani 1 1 d . . . H22 H 0.6464 -0.1157 0.5110 0.107 Uiso 1 1 calc R . . C35 C 0.6442(3) 0.0218(8) 0.4776(5) 0.084(3) Uani 1 1 d . . . H23 H 0.6661 0.0440 0.5155 0.101 Uiso 1 1 calc R . . C36 C 0.6261(3) 0.0902(9) 0.4249(5) 0.076(3) Uani 1 1 d . . . H24 H 0.6379 0.1539 0.4255 0.091 Uiso 1 1 calc R . . C37 C 0.4296(3) 0.3667(12) 0.3656(7) 0.095(4) Uani 1 1 d . . . H25 H 0.4177 0.3033 0.3467 0.114 Uiso 1 1 calc R . . C38 C 0.4125(4) 0.4318(12) 0.3895(6) 0.094(4) Uani 1 1 d . . . H26 H 0.3889 0.4143 0.3862 0.113 Uiso 1 1 calc R . . C39 C 0.4290(5) 0.5214(13) 0.4180(8) 0.123(6) Uani 1 1 d . . . H27 H 0.4175 0.5669 0.4356 0.147 Uiso 1 1 calc R . . C40 C 0.4635(5) 0.5455(15) 0.4209(7) 0.120(6) Uani 1 1 d . . . H28 H 0.4757 0.6081 0.4409 0.144 Uiso 1 1 calc R . . C41 C 0.4803(4) 0.4788(10) 0.3947(5) 0.086(3) Uani 1 1 d . . . C42 C 0.5155(4) 0.5003(9) 0.3934(6) 0.087(3) Uani 1 1 d . . . H29 H 0.5298 0.5605 0.4127 0.104 Uiso 1 1 calc R . . C43 C 0.5645(3) 0.3720(10) 0.3325(4) 0.075(3) Uani 1 1 d . . . C44 C 0.5971(3) 0.3773(8) 0.3198(5) 0.066(2) Uani 1 1 d . . . C45 C 0.6183(3) 0.4666(8) 0.3272(5) 0.076(3) Uani 1 1 d . . . H30 H 0.6133 0.5289 0.3435 0.091 Uiso 1 1 calc R . . C46 C 0.6464(3) 0.4603(9) 0.3101(5) 0.082(3) Uani 1 1 d . . . H31 H 0.6625 0.5170 0.3158 0.099 Uiso 1 1 calc R . . C47 C 0.6504(2) 0.3697(8) 0.2846(5) 0.062(2) Uani 1 1 d . . . C48 C 0.6765(3) 0.3527(9) 0.2562(4) 0.067(3) Uani 1 1 d . . . C49 C 0.7450(3) 0.4615(12) 0.2303(8) 0.101(4) Uani 1 1 d . . . H32 H 0.7491 0.5272 0.2507 0.121 Uiso 1 1 calc R . . C50 C 0.7661(3) 0.4316(12) 0.2007(7) 0.101(4) Uani 1 1 d D . . C51 C 0.7910(4) 0.4978(15) 0.1951(8) 0.127(6) Uani 1 1 d D . . H33 H 0.7911 0.5687 0.2055 0.152 Uiso 1 1 calc R . . C52 C 0.8168(9) 0.459(3) 0.1735(14) 0.205(13) Uiso 1 1 d D . . H34 H 0.8401 0.4916 0.1863 0.246 Uiso 1 1 calc R . . C53 C 0.8062(5) 0.366(2) 0.1307(11) 0.165(10) Uani 1 1 d D . . H35 H 0.8142 0.3482 0.0989 0.199 Uiso 1 1 calc R . . C54 C 0.7794(4) 0.3026(17) 0.1483(9) 0.134(7) Uani 1 1 d D . . H36 H 0.7767 0.2316 0.1371 0.161 Uiso 1 1 calc R . . C55 C 0.3593(3) 0.4870(9) 0.1918(6) 0.072(3) Uani 1 1 d . . . H37 H 0.3458 0.4283 0.1676 0.087 Uiso 1 1 calc R . . C56 C 0.3419(3) 0.5496(10) 0.2154(6) 0.080(3) Uani 1 1 d . . . H38 H 0.3164 0.5385 0.2046 0.096 Uiso 1 1 calc R . . C57 C 0.3605(3) 0.6255(11) 0.2530(6) 0.089(4) Uani 1 1 d . . . H39 H 0.3490 0.6666 0.2729 0.106 Uiso 1 1 calc R . . C58 C 0.3979(3) 0.6492(12) 0.2655(6) 0.093(4) Uani 1 1 d . . . H40 H 0.4116 0.7056 0.2923 0.112 Uiso 1 1 calc R . . C59 C 0.4127(3) 0.5836(7) 0.2355(5) 0.064(2) Uani 1 1 d . . . C60 C 0.4505(3) 0.5997(10) 0.2393(6) 0.079(3) Uani 1 1 d . . . H41 H 0.4654 0.6575 0.2617 0.095 Uiso 1 1 calc R . . C61 C 0.5012(3) 0.4782(7) 0.1809(4) 0.0533(19) Uani 1 1 d . . . C62 C 0.5353(2) 0.4860(8) 0.1724(4) 0.054(2) Uani 1 1 d . . . C63 C 0.5547(3) 0.5761(7) 0.1787(5) 0.066(2) Uani 1 1 d . . . H42 H 0.5497 0.6369 0.1966 0.079 Uiso 1 1 calc R . . C64 C 0.5815(3) 0.5731(7) 0.1577(5) 0.068(3) Uani 1 1 d . . . H43 H 0.5957 0.6328 0.1598 0.081 Uiso 1 1 calc R . . C65 C 0.5875(2) 0.4839(8) 0.1339(5) 0.063(2) Uani 1 1 d . . . C66 C 0.6154(3) 0.4717(7) 0.1084(4) 0.052(2) Uani 1 1 d . . . C67 C 0.6842(4) 0.5907(13) 0.0898(7) 0.101(4) Uani 1 1 d . . . H44 H 0.6899 0.6501 0.1171 0.121 Uiso 1 1 calc R . . C68 C 0.7031(3) 0.5699(9) 0.0500(6) 0.077(3) Uani 1 1 d . . . C69 C 0.7294(5) 0.6402(15) 0.0496(8) 0.126(6) Uani 1 1 d . . . H45 H 0.7347 0.7034 0.0731 0.152 Uiso 1 1 calc R . . C70 C 0.7470(5) 0.6127(19) 0.0136(9) 0.155(9) Uani 1 1 d . . . H46 H 0.7644 0.6594 0.0109 0.186 Uiso 1 1 calc R . . C71 C 0.7409(3) 0.5219(13) -0.0184(6) 0.093(4) Uani 1 1 d . . . H47 H 0.7531 0.5049 -0.0441 0.111 Uiso 1 1 calc R . . C72 C 0.7155(3) 0.4528(12) -0.0122(6) 0.089(4) Uani 1 1 d . . . H48 H 0.7118 0.3865 -0.0318 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0606(8) 0.1122(15) 0.0616(8) -0.0225(9) 0.0279(7) -0.0134(8) Mn2 0.0484(6) 0.0833(10) 0.0560(7) -0.0124(7) 0.0279(6) -0.0033(6) Mn3 0.0588(7) 0.0576(8) 0.0526(7) -0.0142(6) 0.0265(6) -0.0108(6) Mn4 0.0702(8) 0.0554(8) 0.0545(7) -0.0077(6) 0.0283(6) -0.0088(6) Mn5 0.0556(7) 0.0762(10) 0.0500(7) -0.0038(7) 0.0193(6) 0.0052(7) Mn6 0.0514(6) 0.0600(8) 0.0542(7) -0.0038(6) 0.0239(6) 0.0034(6) Mn7 0.0588(7) 0.0497(7) 0.0553(7) -0.0026(6) 0.0302(6) -0.0025(5) Mn8 0.0620(7) 0.0529(7) 0.0491(6) 0.0028(6) 0.0270(6) -0.0117(6) O1 0.061(4) 0.100(6) 0.061(4) -0.023(4) 0.028(3) -0.036(4) O2 0.078(4) 0.047(3) 0.048(3) -0.001(2) 0.028(3) -0.009(3) O3 0.057(3) 0.064(4) 0.053(3) -0.009(3) 0.016(3) -0.010(3) O4 0.063(3) 0.048(3) 0.045(3) 0.003(2) 0.015(3) -0.014(3) O5 0.063(3) 0.058(4) 0.058(3) -0.006(3) 0.023(3) -0.023(3) O6 0.060(3) 0.099(6) 0.054(3) 0.005(4) 0.026(3) -0.001(4) O7 0.059(3) 0.072(4) 0.063(3) -0.035(3) 0.038(3) -0.015(3) O8 0.063(3) 0.077(5) 0.062(3) -0.002(3) 0.037(3) -0.011(3) O9 0.068(4) 0.142(8) 0.050(4) -0.012(4) 0.016(3) -0.032(5) O10 0.089(5) 0.076(5) 0.044(3) 0.007(3) -0.002(3) -0.015(4) O11 0.068(4) 0.108(6) 0.074(4) -0.038(4) 0.044(4) -0.031(4) O12 0.101(5) 0.037(3) 0.114(6) -0.014(3) 0.072(5) -0.014(3) N1 0.065(5) 0.150(11) 0.066(5) -0.020(7) 0.032(4) -0.015(6) N2 0.042(4) 0.254(17) 0.095(7) -0.118(10) 0.022(4) -0.015(7) N3 0.060(5) 0.109(7) 0.075(6) -0.029(5) 0.032(4) -0.026(5) N4 0.047(3) 0.077(5) 0.036(3) -0.020(3) 0.021(3) -0.023(3) N5 0.059(4) 0.057(5) 0.066(4) -0.011(4) 0.042(4) -0.006(3) N6 0.057(4) 0.083(6) 0.065(5) -0.008(4) 0.021(4) -0.028(4) N7 0.087(5) 0.053(5) 0.079(5) 0.000(4) 0.056(5) -0.014(4) N8 0.070(5) 0.108(8) 0.058(5) 0.010(5) 0.038(4) 0.002(5) N9 0.056(4) 0.072(5) 0.053(4) -0.016(4) 0.011(4) -0.012(4) N10 0.059(4) 0.080(6) 0.071(5) -0.026(4) 0.036(4) -0.024(4) N11 0.045(3) 0.077(5) 0.063(4) -0.011(4) 0.027(3) -0.012(3) N12 0.038(3) 0.067(5) 0.067(4) -0.010(4) 0.032(3) -0.005(3) N13 0.039(3) 0.064(4) 0.051(4) -0.012(4) 0.019(3) -0.012(3) N14 0.054(4) 0.057(4) 0.054(4) 0.008(3) 0.018(3) -0.016(3) N15 0.073(4) 0.051(4) 0.061(4) 0.005(3) 0.038(4) -0.004(3) N16 0.077(5) 0.067(5) 0.047(4) 0.014(3) 0.022(4) -0.004(4) N17 0.079(5) 0.059(5) 0.052(4) -0.006(4) 0.020(4) -0.002(4) N18 0.077(5) 0.076(6) 0.066(5) -0.015(4) 0.027(4) -0.016(4) N19 0.074(5) 0.063(5) 0.051(4) -0.025(4) 0.012(4) -0.008(4) N20 0.059(4) 0.101(7) 0.038(3) 0.011(4) 0.011(3) -0.006(4) N21 0.051(4) 0.074(5) 0.049(4) 0.017(4) 0.019(3) 0.004(4) N22 0.070(5) 0.090(7) 0.105(7) 0.012(6) 0.050(5) -0.022(5) N23 0.063(5) 0.103(7) 0.100(7) 0.020(6) 0.040(5) -0.009(5) N24 0.074(5) 0.100(8) 0.064(5) 0.030(5) 0.041(4) 0.013(5) N25 0.066(4) 0.076(6) 0.060(4) 0.006(4) 0.031(4) 0.010(4) N26 0.072(4) 0.047(4) 0.068(4) -0.004(3) 0.049(4) -0.006(3) N27 0.064(4) 0.065(5) 0.060(4) -0.028(4) 0.030(4) -0.021(4) N28 0.060(4) 0.051(4) 0.039(3) 0.000(3) 0.026(3) -0.012(3) N29 0.049(3) 0.061(4) 0.047(3) -0.002(3) 0.018(3) -0.005(3) N30 0.070(5) 0.069(5) 0.072(5) -0.005(4) 0.039(4) -0.016(4) N31 0.057(4) 0.068(5) 0.075(5) 0.028(4) 0.031(4) -0.012(4) N32 0.082(5) 0.084(7) 0.071(5) 0.034(5) 0.048(5) 0.007(5) C1 0.114(10) 0.096(10) 0.075(7) -0.027(7) -0.002(7) -0.019(8) C2 0.095(10) 0.190(18) 0.050(6) -0.027(9) -0.001(7) -0.003(11) C3 0.106(11) 0.22(2) 0.086(10) -0.079(13) 0.013(9) -0.083(14) C4 0.100(10) 0.21(2) 0.074(8) -0.078(11) 0.026(7) -0.026(11) C5 0.086(7) 0.119(11) 0.073(7) -0.039(7) 0.054(6) -0.024(7) C6 0.070(6) 0.074(7) 0.068(6) -0.010(5) 0.034(5) -0.021(5) C7 0.050(4) 0.060(6) 0.060(5) -0.030(4) 0.027(4) -0.021(4) C8 0.082(6) 0.043(5) 0.101(7) -0.012(5) 0.075(6) -0.029(4) C9 0.064(5) 0.056(5) 0.081(6) -0.017(5) 0.044(5) -0.016(4) C10 0.072(6) 0.085(7) 0.073(6) -0.016(5) 0.044(5) -0.029(5) C11 0.060(5) 0.060(6) 0.075(6) -0.022(5) 0.047(5) -0.017(4) C12 0.063(5) 0.036(4) 0.067(5) -0.008(4) 0.043(4) -0.001(3) C13 0.091(8) 0.105(10) 0.085(8) 0.018(7) 0.033(7) -0.029(7) C14 0.107(9) 0.055(6) 0.092(8) 0.029(6) 0.049(7) 0.007(6) C15 0.114(10) 0.066(7) 0.114(10) 0.043(7) -0.019(8) -0.046(7) C16 0.153(14) 0.067(8) 0.125(12) 0.036(8) 0.064(11) 0.011(9) C17 0.115(11) 0.21(2) 0.071(8) -0.004(11) 0.028(8) 0.066(14) C18 0.110(9) 0.100(9) 0.049(5) 0.008(6) 0.015(6) -0.001(7) C19 0.077(7) 0.091(9) 0.089(8) -0.032(7) 0.033(6) -0.010(6) C20 0.139(13) 0.29(3) 0.032(5) -0.016(9) 0.009(7) -0.121(17) C21 0.106(10) 0.23(2) 0.040(5) -0.038(9) 0.014(6) -0.063(12) C22 0.109(10) 0.134(13) 0.091(9) -0.067(9) 0.017(8) 0.000(9) C23 0.055(5) 0.077(7) 0.068(6) -0.018(5) 0.028(5) 0.003(4) C24 0.070(5) 0.062(6) 0.075(6) -0.021(5) 0.042(5) -0.015(4) C25 0.058(5) 0.066(6) 0.066(5) -0.008(5) 0.037(4) 0.000(4) C26 0.058(5) 0.068(6) 0.057(5) -0.005(4) 0.027(4) -0.007(4) C27 0.060(5) 0.082(7) 0.061(5) -0.009(5) 0.031(4) -0.031(5) C28 0.063(5) 0.074(6) 0.062(5) 0.010(5) 0.032(4) -0.013(4) C29 0.070(5) 0.054(5) 0.052(4) 0.012(4) 0.039(4) -0.012(4) C30 0.062(5) 0.046(5) 0.074(6) -0.001(4) 0.043(5) -0.014(4) C31 0.077(6) 0.041(5) 0.066(5) 0.027(4) 0.002(5) -0.011(4) C32 0.087(7) 0.069(7) 0.077(7) 0.035(6) 0.020(6) -0.008(5) C33 0.092(8) 0.100(9) 0.087(8) 0.038(8) -0.029(7) -0.002(8) C34 0.112(9) 0.069(7) 0.062(6) 0.018(5) 0.019(6) -0.008(6) C35 0.092(7) 0.052(6) 0.072(7) 0.006(5) 0.008(6) 0.006(5) C36 0.079(6) 0.074(7) 0.057(5) -0.002(5) 0.016(5) -0.014(5) C37 0.077(7) 0.120(11) 0.112(9) 0.006(8) 0.064(7) 0.003(7) C38 0.094(8) 0.114(11) 0.068(7) -0.015(7) 0.033(6) 0.016(8) C39 0.169(15) 0.095(11) 0.126(12) 0.007(9) 0.086(12) 0.073(11) C40 0.134(13) 0.151(16) 0.088(9) 0.003(9) 0.064(9) 0.050(12) C41 0.092(8) 0.079(8) 0.066(6) -0.004(5) 0.019(6) 0.021(6) C42 0.110(9) 0.062(7) 0.093(8) -0.034(6) 0.052(7) -0.017(6) C43 0.067(6) 0.103(9) 0.034(4) 0.014(5) 0.006(4) 0.007(6) C44 0.084(6) 0.056(6) 0.057(5) -0.015(4) 0.033(5) -0.017(5) C45 0.095(7) 0.058(6) 0.071(6) -0.024(5) 0.036(6) -0.041(5) C46 0.086(7) 0.073(7) 0.073(6) -0.014(5) 0.025(6) -0.047(6) C47 0.052(5) 0.068(6) 0.066(5) 0.011(5) 0.029(4) -0.005(4) C48 0.066(5) 0.084(7) 0.044(4) 0.011(5) 0.021(4) -0.021(5) C49 0.070(7) 0.092(9) 0.129(11) 0.011(8) 0.036(7) -0.014(6) C50 0.083(8) 0.106(11) 0.128(11) 0.020(9) 0.060(8) -0.033(7) C51 0.120(12) 0.129(14) 0.154(15) -0.031(12) 0.083(12) -0.054(10) C53 0.100(11) 0.24(3) 0.19(2) 0.11(2) 0.102(13) 0.037(14) C54 0.105(10) 0.148(15) 0.170(16) 0.040(13) 0.080(12) 0.056(11) C55 0.055(5) 0.075(7) 0.094(7) -0.008(6) 0.041(5) -0.019(5) C56 0.062(6) 0.084(8) 0.110(9) 0.015(7) 0.053(6) 0.019(5) C57 0.079(7) 0.091(9) 0.101(8) -0.034(7) 0.046(7) -0.006(6) C58 0.093(8) 0.105(10) 0.107(9) -0.036(8) 0.068(7) -0.011(7) C59 0.068(5) 0.050(5) 0.075(6) -0.004(4) 0.036(5) 0.014(4) C60 0.058(5) 0.090(8) 0.097(8) -0.047(7) 0.043(5) -0.009(5) C61 0.066(5) 0.041(4) 0.061(5) -0.014(4) 0.036(4) -0.012(4) C62 0.055(4) 0.070(6) 0.044(4) -0.003(4) 0.030(4) -0.010(4) C63 0.080(6) 0.047(5) 0.084(6) -0.018(4) 0.049(5) -0.013(4) C64 0.083(6) 0.047(5) 0.098(7) -0.019(5) 0.063(6) -0.031(4) C65 0.048(4) 0.071(6) 0.063(5) -0.017(5) 0.021(4) -0.009(4) C66 0.074(5) 0.045(5) 0.041(4) 0.003(3) 0.029(4) -0.020(4) C67 0.100(9) 0.111(10) 0.114(10) 0.001(8) 0.067(8) -0.032(8) C68 0.072(6) 0.055(6) 0.110(8) 0.011(6) 0.049(6) 0.000(5) C69 0.144(13) 0.132(14) 0.141(13) 0.003(11) 0.099(12) -0.047(11) C70 0.132(13) 0.24(2) 0.146(15) -0.069(16) 0.106(13) -0.096(16) C71 0.091(8) 0.137(12) 0.081(7) 0.014(8) 0.066(7) -0.003(8) C72 0.060(5) 0.133(11) 0.086(7) 0.015(7) 0.044(6) 0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N2 2.012(18) . ? Mn1 O6 2.156(7) 2_655 ? Mn1 N23 2.164(12) 2_655 ? Mn1 O1 2.224(7) . ? Mn1 N1 2.242(11) . ? Mn1 N24 2.283(9) 2_655 ? Mn2 O9 2.072(7) . ? Mn2 N31 2.174(10) 2_655 ? Mn2 O8 2.218(6) 2_655 ? Mn2 N4 2.224(8) . ? Mn2 O1 2.225(7) . ? Mn2 N32 2.302(9) 2_655 ? Mn3 O9 2.059(8) . ? Mn3 N26 2.207(7) . ? Mn3 O2 2.217(6) . ? Mn3 O7 2.250(6) . ? Mn3 N5 2.251(8) . ? Mn3 N25 2.252(8) . ? Mn4 N7 2.133(8) . ? Mn4 O2 2.174(6) . ? Mn4 N18 2.176(9) . ? Mn4 O5 2.207(6) . ? Mn4 N17 2.255(9) . ? Mn4 N8 2.298(9) . ? Mn5 O11 2.075(6) 2_655 ? Mn5 N10 2.162(9) . ? Mn5 O6 2.204(8) 2_655 ? Mn5 N21 2.245(9) 2_655 ? Mn5 O3 2.255(6) . ? Mn5 N9 2.267(7) . ? Mn6 O10 2.116(6) . ? Mn6 O12 2.121(7) 2_655 ? Mn6 O3 2.168(6) . ? Mn6 O8 2.191(7) 2_655 ? Mn6 N29 2.279(8) 2_655 ? Mn6 N12 2.325(8) . ? Mn7 O10 2.073(6) . ? Mn7 O12 2.111(7) . ? Mn7 O4 2.171(6) . ? Mn7 O7 2.183(6) . ? Mn7 N13 2.291(7) . ? Mn7 N28 2.292(7) . ? Mn8 O11 2.048(7) . ? Mn8 O5 2.177(7) . ? Mn8 N15 2.190(8) . ? Mn8 O4 2.247(6) . ? Mn8 N16 2.254(7) . ? Mn8 N20 2.293(9) . ? O1 C7 1.261(13) . ? O2 C12 1.289(10) . ? O3 C25 1.212(12) . ? O4 C30 1.240(10) . ? O5 C43 1.321(14) . ? O6 C48 1.307(14) . ? O6 Mn1 2.157(7) 2_655 ? O6 Mn5 2.204(8) 2_655 ? O7 C61 1.288(10) . ? O8 C66 1.288(11) . ? O8 Mn6 2.191(7) 2_655 ? O8 Mn2 2.218(6) 2_655 ? O11 Mn5 2.075(6) 2_655 ? O12 Mn6 2.121(7) 2_655 ? O13 N33 1.251(19) . ? O14 N33 1.21(2) . ? O15 N33 1.29(2) . ? N1 C1 1.311(16) . ? N1 C5 1.327(19) . ? N2 C6 1.336(16) . ? N2 N3 1.399(15) . ? N3 C7 1.265(12) . ? N4 N5 1.317(9) . ? N4 C8 1.392(11) . ? N5 C11 1.347(13) . ? N6 C12 1.269(12) . ? N6 N7 1.402(11) . ? N7 C13 1.274(15) . ? N8 C14 1.274(15) . ? N8 C18 1.357(15) . ? N9 C19 1.328(15) . ? N9 C23 1.370(14) . ? N10 C24 1.321(12) . ? N10 N11 1.384(11) . ? N11 C25 1.325(12) . ? N12 C26 1.256(12) . ? N12 N13 1.317(9) . ? N13 C29 1.279(11) . ? N14 C30 1.328(12) . ? N14 N15 1.367(10) . ? N15 C31 1.299(11) . ? N16 C36 1.323(12) . ? N16 C32 1.420(14) . ? N17 C37 1.351(13) . ? N17 C41 1.359(15) . ? N18 C42 1.254(14) . ? N18 N19 1.358(12) . ? N19 C43 1.300(14) . ? N20 N21 1.322(10) . ? N20 C44 1.327(14) . ? N21 C47 1.336(13) . ? N21 Mn5 2.245(9) 2_655 ? N22 C48 1.335(13) . ? N22 N23 1.356(14) . ? N23 C49 1.265(15) . ? N23 Mn1 2.164(12) 2_655 ? N24 C54 1.232(17) . ? N24 C50 1.354(18) . ? N24 Mn1 2.282(9) 2_655 ? N25 C55 1.340(12) . ? N25 C59 1.360(13) . ? N26 C60 1.214(12) . ? N26 N27 1.369(10) . ? N27 C61 1.270(11) . ? N28 N29 1.318(9) . ? N28 C62 1.349(12) . ? N29 C65 1.313(12) . ? N29 Mn6 2.279(8) 2_655 ? N30 C66 1.297(11) . ? N30 N31 1.398(11) . ? N31 C67 1.257(14) . ? N31 Mn2 2.174(10) 2_655 ? N32 C68 1.305(15) . ? N32 C72 1.365(14) . ? N32 Mn2 2.302(9) 2_655 ? C1 C2 1.31(2) . ? C2 C3 1.40(3) . ? C3 C4 1.35(2) . ? C4 C5 1.436(19) . ? C5 C6 1.437(16) . ? C7 C8 1.490(14) . ? C8 C9 1.314(14) . ? C9 C10 1.337(14) . ? C10 C11 1.377(13) . ? C11 C12 1.463(13) . ? C13 C14 1.442(17) . ? C14 C15 1.350(15) . ? C15 C16 1.39(2) . ? C16 C17 1.41(3) . ? C17 C18 1.32(2) . ? C19 C20 1.273(17) . ? C20 C21 1.48(3) . ? C21 C22 1.48(2) . ? C22 C23 1.426(16) . ? C23 C24 1.421(14) . ? C25 C26 1.538(13) . ? C26 C27 1.383(15) . ? C27 C28 1.364(13) . ? C28 C29 1.399(13) . ? C29 C30 1.507(12) . ? C31 C32 1.450(14) . ? C32 C33 1.344(15) . ? C33 C34 1.447(16) . ? C34 C35 1.264(16) . ? C35 C36 1.397(15) . ? C37 C38 1.354(18) . ? C38 C39 1.35(2) . ? C39 C40 1.40(2) . ? C40 C41 1.394(18) . ? C41 C42 1.459(18) . ? C43 C44 1.473(15) . ? C44 C45 1.404(13) . ? C45 C46 1.360(17) . ? C46 C47 1.356(16) . ? C47 C48 1.484(14) . ? C49 C50 1.37(2) . ? C50 C51 1.370(17) . ? C51 C52 1.44(3) . ? C52 C53 1.49(4) . ? C53 C54 1.55(2) . ? C55 C56 1.340(15) . ? C56 C57 1.294(17) . ? C57 C58 1.434(16) . ? C58 C59 1.388(14) . ? C59 C60 1.503(13) . ? C61 C62 1.478(11) . ? C62 C63 1.379(13) . ? C63 C64 1.375(13) . ? C64 C65 1.346(14) . ? C65 C66 1.498(13) . ? C67 C68 1.456(17) . ? C68 C69 1.406(17) . ? C69 C70 1.36(2) . ? C70 C71 1.35(3) . ? C71 C72 1.415(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mn1 O6 117.8(3) . 2_655 ? N2 Mn1 N23 171.5(3) . 2_655 ? O6 Mn1 N23 70.5(3) 2_655 2_655 ? N2 Mn1 O1 70.8(3) . . ? O6 Mn1 O1 106.3(2) 2_655 . ? N23 Mn1 O1 109.3(4) 2_655 . ? N2 Mn1 N1 72.5(4) . . ? O6 Mn1 N1 91.1(3) 2_655 . ? N23 Mn1 N1 106.9(4) 2_655 . ? O1 Mn1 N1 143.3(4) . . ? N2 Mn1 N24 98.0(4) . 2_655 ? O6 Mn1 N24 143.9(4) 2_655 2_655 ? N23 Mn1 N24 73.6(4) 2_655 2_655 ? O1 Mn1 N24 89.4(3) . 2_655 ? N1 Mn1 N24 95.0(3) . 2_655 ? O9 Mn2 N31 96.1(3) . 2_655 ? O9 Mn2 O8 95.3(3) . 2_655 ? N31 Mn2 O8 70.0(3) 2_655 2_655 ? O9 Mn2 N4 85.2(3) . . ? N31 Mn2 N4 175.5(3) 2_655 . ? O8 Mn2 N4 114.1(3) 2_655 . ? O9 Mn2 O1 155.7(4) . . ? N31 Mn2 O1 107.2(3) 2_655 . ? O8 Mn2 O1 86.4(3) 2_655 . ? N4 Mn2 O1 72.1(3) . . ? O9 Mn2 N32 99.2(3) . 2_655 ? N31 Mn2 N32 70.9(3) 2_655 2_655 ? O8 Mn2 N32 139.4(3) 2_655 2_655 ? N4 Mn2 N32 104.8(3) . 2_655 ? O1 Mn2 N32 95.0(3) . 2_655 ? O9 Mn3 N26 103.6(3) . . ? O9 Mn3 O2 156.4(3) . . ? N26 Mn3 O2 98.9(3) . . ? O9 Mn3 O7 96.9(3) . . ? N26 Mn3 O7 69.1(2) . . ? O2 Mn3 O7 84.4(3) . . ? O9 Mn3 N5 85.4(3) . . ? N26 Mn3 N5 171.0(3) . . ? O2 Mn3 N5 72.2(3) . . ? O7 Mn3 N5 110.9(2) . . ? O9 Mn3 N25 97.5(3) . . ? N26 Mn3 N25 72.6(3) . . ? O2 Mn3 N25 96.0(3) . . ? O7 Mn3 N25 141.2(3) . . ? N5 Mn3 N25 106.0(3) . . ? N7 Mn4 O2 72.4(3) . . ? N7 Mn4 N18 167.6(3) . . ? O2 Mn4 N18 119.0(3) . . ? N7 Mn4 O5 111.7(3) . . ? O2 Mn4 O5 107.0(2) . . ? N18 Mn4 O5 71.0(3) . . ? N7 Mn4 N17 104.3(3) . . ? O2 Mn4 N17 89.8(3) . . ? N18 Mn4 N17 72.4(3) . . ? O5 Mn4 N17 143.4(3) . . ? N7 Mn4 N8 70.2(3) . . ? O2 Mn4 N8 142.5(3) . . ? N18 Mn4 N8 98.0(4) . . ? O5 Mn4 N8 89.2(3) . . ? N17 Mn4 N8 96.8(3) . . ? O11 Mn5 N10 101.7(3) 2_655 . ? O11 Mn5 O6 152.0(3) 2_655 2_655 ? N10 Mn5 O6 102.9(3) . 2_655 ? O11 Mn5 N21 84.7(3) 2_655 2_655 ? N10 Mn5 N21 172.6(3) . 2_655 ? O6 Mn5 N21 71.8(3) 2_655 2_655 ? O11 Mn5 O3 91.5(3) 2_655 . ? N10 Mn5 O3 69.3(3) . . ? O6 Mn5 O3 84.9(2) 2_655 . ? N21 Mn5 O3 114.6(3) 2_655 . ? O11 Mn5 N9 105.1(3) 2_655 . ? N10 Mn5 N9 72.8(3) . . ? O6 Mn5 N9 94.8(3) 2_655 . ? N21 Mn5 N9 102.1(3) 2_655 . ? O3 Mn5 N9 141.0(3) . . ? O10 Mn6 O12 94.8(3) . 2_655 ? O10 Mn6 O3 156.8(3) . . ? O12 Mn6 O3 87.4(3) 2_655 . ? O10 Mn6 O8 94.2(3) . 2_655 ? O12 Mn6 O8 154.9(3) 2_655 2_655 ? O3 Mn6 O8 93.3(3) . 2_655 ? O10 Mn6 N29 90.2(3) . 2_655 ? O12 Mn6 N29 85.2(3) 2_655 2_655 ? O3 Mn6 N29 113.0(3) . 2_655 ? O8 Mn6 N29 71.3(2) 2_655 2_655 ? O10 Mn6 N12 86.5(3) . . ? O12 Mn6 N12 94.4(2) 2_655 . ? O3 Mn6 N12 70.3(3) . . ? O8 Mn6 N12 109.5(2) 2_655 . ? N29 Mn6 N12 176.7(3) 2_655 . ? O10 Mn7 O12 95.3(3) . . ? O10 Mn7 O4 157.8(3) . . ? O12 Mn7 O4 87.5(3) . . ? O10 Mn7 O7 94.2(3) . . ? O12 Mn7 O7 154.2(2) . . ? O4 Mn7 O7 92.7(3) . . ? O10 Mn7 N13 86.9(3) . . ? O12 Mn7 N13 92.5(3) . . ? O4 Mn7 N13 70.9(2) . . ? O7 Mn7 N13 111.9(2) . . ? O10 Mn7 N28 91.9(3) . . ? O12 Mn7 N28 84.8(3) . . ? O4 Mn7 N28 110.3(2) . . ? O7 Mn7 N28 71.0(2) . . ? N13 Mn7 N28 176.9(2) . . ? O11 Mn8 O5 149.6(3) . . ? O11 Mn8 N15 96.8(3) . . ? O5 Mn8 N15 110.2(3) . . ? O11 Mn8 O4 92.7(3) . . ? O5 Mn8 O4 84.6(2) . . ? N15 Mn8 O4 68.7(2) . . ? O11 Mn8 N16 102.8(3) . . ? O5 Mn8 N16 98.5(3) . . ? N15 Mn8 N16 72.9(3) . . ? O4 Mn8 N16 139.9(3) . . ? O11 Mn8 N20 84.2(3) . . ? O5 Mn8 N20 70.6(3) . . ? N15 Mn8 N20 173.5(3) . . ? O4 Mn8 N20 117.7(2) . . ? N16 Mn8 N20 100.6(3) . . ? C7 O1 Mn1 112.7(5) . . ? C7 O1 Mn2 118.8(5) . . ? Mn1 O1 Mn2 128.5(4) . . ? C12 O2 Mn4 112.5(5) . . ? C12 O2 Mn3 118.2(5) . . ? Mn4 O2 Mn3 129.1(3) . . ? C25 O3 Mn6 121.1(6) . . ? C25 O3 Mn5 112.1(6) . . ? Mn6 O3 Mn5 120.5(3) . . ? C30 O4 Mn7 119.5(6) . . ? C30 O4 Mn8 112.3(6) . . ? Mn7 O4 Mn8 119.7(3) . . ? C43 O5 Mn8 121.2(7) . . ? C43 O5 Mn4 112.9(7) . . ? Mn8 O5 Mn4 125.7(3) . . ? C48 O6 Mn1 115.8(6) . 2_655 ? C48 O6 Mn5 117.3(6) . 2_655 ? Mn1 O6 Mn5 126.4(4) 2_655 2_655 ? C61 O7 Mn7 121.1(5) . . ? C61 O7 Mn3 112.9(5) . . ? Mn7 O7 Mn3 124.6(3) . . ? C66 O8 Mn6 119.3(5) . 2_655 ? C66 O8 Mn2 113.4(5) . 2_655 ? Mn6 O8 Mn2 124.9(3) 2_655 2_655 ? Mn3 O9 Mn2 125.6(5) . . ? Mn7 O10 Mn6 123.8(4) . . ? Mn8 O11 Mn5 125.7(3) . 2_655 ? Mn7 O12 Mn6 118.6(3) . 2_655 ? C1 N1 C5 116.2(12) . . ? C1 N1 Mn1 132.0(12) . . ? C5 N1 Mn1 111.8(7) . . ? C6 N2 N3 110.3(14) . . ? C6 N2 Mn1 127.2(9) . . ? N3 N2 Mn1 122.2(9) . . ? C7 N3 N2 109.7(11) . . ? N5 N4 C8 118.1(8) . . ? N5 N4 Mn2 122.8(6) . . ? C8 N4 Mn2 118.6(6) . . ? N4 N5 C11 122.4(8) . . ? N4 N5 Mn3 120.7(6) . . ? C11 N5 Mn3 116.7(6) . . ? C12 N6 N7 110.3(8) . . ? C13 N7 N6 121.5(9) . . ? C13 N7 Mn4 120.6(8) . . ? N6 N7 Mn4 117.8(6) . . ? C14 N8 C18 115.1(11) . . ? C14 N8 Mn4 117.1(8) . . ? C18 N8 Mn4 127.4(9) . . ? C19 N9 C23 119.4(9) . . ? C19 N9 Mn5 129.5(8) . . ? C23 N9 Mn5 111.0(6) . . ? C24 N10 N11 116.9(9) . . ? C24 N10 Mn5 121.5(7) . . ? N11 N10 Mn5 119.5(5) . . ? C25 N11 N10 107.7(8) . . ? C26 N12 N13 122.4(8) . . ? C26 N12 Mn6 115.6(6) . . ? N13 N12 Mn6 119.4(5) . . ? C29 N13 N12 119.1(7) . . ? C29 N13 Mn7 115.7(5) . . ? N12 N13 Mn7 122.6(6) . . ? C30 N14 N15 107.0(7) . . ? C31 N15 N14 117.9(8) . . ? C31 N15 Mn8 118.2(6) . . ? N14 N15 Mn8 120.3(5) . . ? C36 N16 C32 116.4(9) . . ? C36 N16 Mn8 127.8(7) . . ? C32 N16 Mn8 114.1(6) . . ? C37 N17 C41 119.5(11) . . ? C37 N17 Mn4 127.0(8) . . ? C41 N17 Mn4 113.5(8) . . ? C42 N18 N19 118.2(9) . . ? C42 N18 Mn4 121.4(8) . . ? N19 N18 Mn4 120.2(7) . . ? C43 N19 N18 110.4(9) . . ? N21 N20 C44 121.0(9) . . ? N21 N20 Mn8 120.6(7) . . ? C44 N20 Mn8 118.1(7) . . ? N20 N21 C47 117.6(9) . . ? N20 N21 Mn5 121.7(7) . 2_655 ? C47 N21 Mn5 120.2(6) . 2_655 ? C48 N22 N23 108.8(10) . . ? C49 N23 N22 122.2(13) . . ? C49 N23 Mn1 116.4(10) . 2_655 ? N22 N23 Mn1 121.3(7) . 2_655 ? C54 N24 C50 121.8(14) . . ? C54 N24 Mn1 127.6(13) . 2_655 ? C50 N24 Mn1 110.6(7) . 2_655 ? C55 N25 C59 115.3(9) . . ? C55 N25 Mn3 129.3(8) . . ? C59 N25 Mn3 115.2(6) . . ? C60 N26 N27 121.0(8) . . ? C60 N26 Mn3 119.8(6) . . ? N27 N26 Mn3 119.0(5) . . ? C61 N27 N26 111.3(7) . . ? N29 N28 C62 119.8(7) . . ? N29 N28 Mn7 120.7(5) . . ? C62 N28 Mn7 116.7(5) . . ? C65 N29 N28 119.3(8) . . ? C65 N29 Mn6 117.0(6) . 2_655 ? N28 N29 Mn6 120.4(5) . 2_655 ? C66 N30 N31 109.2(8) . . ? C67 N31 N30 119.6(11) . . ? C67 N31 Mn2 120.5(9) . 2_655 ? N30 N31 Mn2 119.5(6) . 2_655 ? C68 N32 C72 118.1(11) . . ? C68 N32 Mn2 114.2(7) . 2_655 ? C72 N32 Mn2 126.9(9) . 2_655 ? O14 N33 O13 114.8(19) . . ? O14 N33 O15 125(2) . . ? O13 N33 O15 115(2) . . ? N1 C1 C2 127.5(17) . . ? C1 C2 C3 118.7(14) . . ? C4 C3 C2 116.3(14) . . ? C3 C4 C5 121(2) . . ? N1 C5 C4 120.4(13) . . ? N1 C5 C6 120.6(10) . . ? C4 C5 C6 119.0(15) . . ? N2 C6 C5 107.7(12) . . ? O1 C7 N3 123.6(9) . . ? O1 C7 C8 119.6(7) . . ? N3 C7 C8 116.4(10) . . ? C9 C8 N4 121.3(9) . . ? C9 C8 C7 127.7(8) . . ? N4 C8 C7 110.9(8) . . ? C8 C9 C10 119.0(9) . . ? C9 C10 C11 121.6(11) . . ? N5 C11 C10 117.4(9) . . ? N5 C11 C12 114.5(8) . . ? C10 C11 C12 127.9(10) . . ? N6 C12 O2 126.9(8) . . ? N6 C12 C11 114.8(8) . . ? O2 C12 C11 118.3(8) . . ? N7 C13 C14 117.8(11) . . ? N8 C14 C15 127.4(13) . . ? N8 C14 C13 113.3(10) . . ? C15 C14 C13 119.2(11) . . ? C14 C15 C16 114.8(11) . . ? C15 C16 C17 121.5(13) . . ? C18 C17 C16 114.3(16) . . ? C17 C18 N8 126.8(16) . . ? C20 C19 N9 129.0(15) . . ? C19 C20 C21 112.8(15) . . ? C22 C21 C20 122.9(12) . . ? C23 C22 C21 111.6(16) . . ? N9 C23 C24 121.6(9) . . ? N9 C23 C22 122.5(11) . . ? C24 C23 C22 115.8(12) . . ? N10 C24 C23 111.6(10) . . ? O3 C25 N11 127.6(9) . . ? O3 C25 C26 116.9(9) . . ? N11 C25 C26 115.5(9) . . ? N12 C26 C27 122.7(9) . . ? N12 C26 C25 113.6(9) . . ? C27 C26 C25 123.5(9) . . ? C28 C27 C26 116.3(9) . . ? C27 C28 C29 116.9(9) . . ? N13 C29 C28 122.4(8) . . ? N13 C29 C30 113.5(7) . . ? C28 C29 C30 124.1(7) . . ? O4 C30 N14 127.5(9) . . ? O4 C30 C29 117.5(8) . . ? N14 C30 C29 115.0(7) . . ? N15 C31 C32 117.6(8) . . ? C33 C32 N16 121.7(11) . . ? C33 C32 C31 123.8(11) . . ? N16 C32 C31 114.0(8) . . ? C32 C33 C34 118.2(13) . . ? C35 C34 C33 119.1(11) . . ? C34 C35 C36 122.1(11) . . ? N16 C36 C35 122.1(10) . . ? N17 C37 C38 122.5(14) . . ? C39 C38 C37 120.3(15) . . ? C38 C39 C40 118.3(13) . . ? C41 C40 C39 120.8(17) . . ? N17 C41 C40 118.6(14) . . ? N17 C41 C42 117.3(10) . . ? C40 C41 C42 124.1(14) . . ? N18 C42 C41 115.2(10) . . ? N19 C43 O5 125.5(10) . . ? N19 C43 C44 118.7(11) . . ? O5 C43 C44 115.8(10) . . ? N20 C44 C45 121.9(10) . . ? N20 C44 C43 113.7(9) . . ? C45 C44 C43 124.3(10) . . ? C46 C45 C44 117.2(10) . . ? C47 C46 C45 117.3(9) . . ? N21 C47 C46 125.0(9) . . ? N21 C47 C48 110.4(9) . . ? C46 C47 C48 124.6(9) . . ? O6 C48 N22 123.2(10) . . ? O6 C48 C47 120.1(9) . . ? N22 C48 C47 116.6(11) . . ? N23 C49 C50 121.2(15) . . ? N24 C50 C49 118.1(11) . . ? N24 C50 C51 120.7(15) . . ? C49 C50 C51 121.2(16) . . ? C50 C51 C52 119(2) . . ? C51 C52 C53 119(3) . . ? C52 C53 C54 106(2) . . ? N24 C54 C53 127(2) . . ? C56 C55 N25 125.6(10) . . ? C57 C56 C55 118.7(10) . . ? C56 C57 C58 121.8(11) . . ? C59 C58 C57 114.9(11) . . ? N25 C59 C58 123.3(10) . . ? N25 C59 C60 113.9(8) . . ? C58 C59 C60 122.8(10) . . ? N26 C60 C59 118.5(9) . . ? N27 C61 O7 125.3(8) . . ? N27 C61 C62 117.3(7) . . ? O7 C61 C62 117.1(7) . . ? N28 C62 C63 122.2(7) . . ? N28 C62 C61 113.1(7) . . ? C63 C62 C61 124.2(8) . . ? C64 C63 C62 116.1(8) . . ? C65 C64 C63 118.8(8) . . ? N29 C65 C64 123.6(8) . . ? N29 C65 C66 112.7(8) . . ? C64 C65 C66 123.6(8) . . ? O8 C66 N30 125.3(8) . . ? O8 C66 C65 117.4(7) . . ? N30 C66 C65 117.3(8) . . ? N31 C67 C68 117.0(14) . . ? N32 C68 C69 124.1(13) . . ? N32 C68 C67 115.6(10) . . ? C69 C68 C67 120.0(13) . . ? C70 C69 C68 116.3(17) . . ? C71 C70 C69 122.8(15) . . ? C70 C71 C72 117.4(11) . . ? N32 C72 C71 121.2(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.808 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.105