# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jie Zhang' _publ_contact_author_email ZHANGJIE@FJIRSM.AC.CN _publ_section_title ; A Series of Manganese-Carboxylate Coordination Polymers Exhibiting Diverse Magnetic Properties ; loop_ _publ_author_name 'Jie Zhang.' 'Hong-Peng Jia.' 'Zhan-Feng Ju.' 'Wei Li.' # Attachment 'compound1-3.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 679474' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H7 Mn N3 O8' _chemical_formula_sum 'C14 H7 Mn N3 O8' _chemical_formula_weight 400.17 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Iba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, z+1/2' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 18.3259(15) _cell_length_b 25.300(2) _cell_length_c 7.5240(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3488.5(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3194 _cell_measurement_theta_min 2.2233 _cell_measurement_theta_max 27.4835 _exptl_crystal_description needle _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details '(R.H. Blessing, 1995&1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13311 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3860 _reflns_number_gt 3194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku Corp.,2000)' _computing_cell_refinement 'CrystalClear(Rigaku Corp.,2000)' _computing_data_reduction 'CrystalClear(Rigaku Corp.,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 3860 _refine_ls_number_parameters 239 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1890 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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 0.90073(3) 0.51713(2) 0.26448(13) 0.0216(2) Uani 1 1 d . . . C1 C 0.7510(3) 0.3890(2) 0.0834(8) 0.0317(12) Uani 1 1 d . . . C2 C 0.7102(3) 0.3905(2) 0.2385(9) 0.0386(14) Uani 1 1 d . . . H2 H 0.7226 0.4149 0.3297 0.046 Uiso 1 1 calc R . . C3 C 0.6516(3) 0.3566(2) 0.2613(10) 0.0365(12) Uani 1 1 d . . . C4 C 0.6307(3) 0.3187(2) 0.1325(8) 0.0267(11) Uani 1 1 d . . . C5 C 0.6761(3) 0.3185(2) -0.0200(9) 0.0333(13) Uani 1 1 d . . . C6 C 0.7337(3) 0.3523(2) -0.0448(9) 0.0355(13) Uani 1 1 d . . . H6 H 0.7618 0.3504 -0.1507 0.043 Uiso 1 1 calc R . . C7 C 0.8109(3) 0.4293(2) 0.0538(8) 0.0331(12) Uani 1 1 d . . . C8 C 0.5531(3) 0.12791(18) -0.0208(7) 0.0212(10) Uani 1 1 d . . . C9 C 0.6204(3) 0.1468(2) 0.0368(8) 0.0289(12) Uani 1 1 d . . . H9 H 0.6614 0.1238 0.0394 0.035 Uiso 1 1 calc R . . C10 C 0.6282(3) 0.1989(2) 0.0903(9) 0.0306(12) Uani 1 1 d . . . H10 H 0.6746 0.2116 0.1272 0.037 Uiso 1 1 calc R . . C11 C 0.5679(3) 0.23306(19) 0.0902(8) 0.0274(11) Uani 1 1 d . . . C12 C 0.5002(4) 0.21417(16) 0.0315(9) 0.0259(10) Uani 1 1 d . . . H12 H 0.4590 0.2370 0.0307 0.031 Uiso 1 1 calc R . . C13 C 0.4932(3) 0.16269(18) -0.0252(7) 0.0244(11) Uani 1 1 d . . . H13 H 0.4474 0.1505 -0.0678 0.029 Uiso 1 1 calc R . . C14 C 0.5448(3) 0.07331(18) -0.0785(7) 0.0215(10) Uani 1 1 d . . . H17 H 0.536(3) 0.289(3) 0.233(9) 0.07(3) Uiso 1 1 d D . . N1 N 0.6099(4) 0.3623(2) 0.4267(9) 0.061(2) Uani 1 1 d . . . N2 N 0.6559(4) 0.2866(2) -0.1768(8) 0.0481(16) Uani 1 1 d . . . N3 N 0.5734(3) 0.28460(18) 0.1558(7) 0.0305(11) Uani 1 1 d D . . O1 O 0.6439(5) 0.3795(3) 0.5557(8) 0.109(3) Uani 1 1 d . . . O2 O 0.5469(4) 0.3490(2) 0.4302(9) 0.076(2) Uani 1 1 d . . . O3 O 0.5925(3) 0.2859(2) -0.2212(9) 0.0604(15) Uani 1 1 d . . . O4 O 0.7051(4) 0.2637(3) -0.2539(11) 0.091(3) Uani 1 1 d . . . O5 O 0.8383(2) 0.42900(16) -0.0990(7) 0.0425(11) Uani 1 1 d . . . O6 O 0.8269(3) 0.4594(2) 0.1785(6) 0.0492(13) Uani 1 1 d . . . O7 O 0.5856(2) 0.03760(14) -0.0096(5) 0.0257(8) Uani 1 1 d . . . O8 O 0.5010(2) 0.06133(12) -0.2012(5) 0.0333(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0255(4) 0.0188(3) 0.0204(4) 0.0006(3) -0.0010(4) -0.0026(2) C1 0.036(3) 0.028(2) 0.031(3) -0.001(2) -0.002(2) -0.016(2) C2 0.053(3) 0.031(2) 0.032(3) -0.007(3) -0.002(3) -0.020(2) C3 0.047(3) 0.032(2) 0.030(3) -0.003(3) 0.005(3) -0.017(2) C4 0.032(3) 0.019(2) 0.029(3) -0.002(2) 0.002(2) -0.004(2) C5 0.035(3) 0.025(2) 0.041(3) -0.010(3) 0.001(3) -0.008(2) C6 0.034(3) 0.036(3) 0.037(3) -0.005(3) 0.008(3) -0.013(2) C7 0.035(3) 0.033(3) 0.031(3) 0.006(3) -0.004(2) -0.013(2) C8 0.021(2) 0.020(2) 0.023(2) 0.001(2) -0.0015(19) 0.0010(18) C9 0.021(2) 0.027(2) 0.038(3) 0.000(2) -0.008(2) -0.001(2) C10 0.024(2) 0.022(2) 0.046(4) -0.002(2) -0.009(2) -0.006(2) C11 0.031(3) 0.019(2) 0.033(3) -0.003(2) 0.006(2) -0.005(2) C12 0.024(2) 0.0211(18) 0.032(3) 0.001(2) 0.003(2) 0.004(3) C13 0.018(2) 0.025(2) 0.030(3) -0.001(2) -0.004(2) 0.000(2) C14 0.025(2) 0.019(2) 0.020(2) 0.0023(19) 0.001(2) -0.0004(19) N1 0.102(6) 0.048(3) 0.034(3) -0.013(3) 0.025(3) -0.043(4) N2 0.060(4) 0.048(3) 0.036(3) -0.013(2) 0.015(3) -0.028(3) N3 0.026(2) 0.023(2) 0.042(3) -0.006(2) 0.009(2) -0.0056(18) O1 0.172(8) 0.117(6) 0.036(3) -0.034(4) 0.038(4) -0.096(6) O2 0.081(4) 0.073(4) 0.075(4) -0.035(3) 0.047(4) -0.044(3) O3 0.065(3) 0.073(3) 0.044(3) -0.008(3) -0.011(3) -0.038(3) O4 0.083(4) 0.093(4) 0.098(5) -0.070(4) 0.054(4) -0.043(4) O5 0.050(3) 0.033(2) 0.044(3) -0.002(2) 0.014(2) -0.016(2) O6 0.057(3) 0.056(3) 0.035(2) 0.000(2) -0.003(2) -0.036(2) O7 0.036(2) 0.0206(16) 0.0203(18) -0.0001(15) -0.0008(15) 0.0079(15) O8 0.042(2) 0.0245(15) 0.034(3) 0.0027(16) -0.0123(17) -0.0123(16) _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 O5 2.055(4) 4_565 ? Mn1 O6 2.094(4) . ? Mn1 O7 2.141(4) 7_654 ? Mn1 O8 2.166(4) 5 ? Mn1 O7 2.207(4) 6_655 ? C1 C6 1.376(8) . ? C1 C2 1.386(9) . ? C1 C7 1.514(7) . ? C2 C3 1.386(7) . ? C2 H2 0.9500 . ? C3 C4 1.417(8) . ? C3 N1 1.467(9) . ? C4 N3 1.370(7) . ? C4 C5 1.418(8) . ? C5 C6 1.371(8) . ? C5 N2 1.478(8) . ? C6 H6 0.9500 . ? C7 O6 1.243(7) . ? C7 O5 1.254(7) . ? C8 C9 1.392(7) . ? C8 C13 1.407(7) . ? C8 C14 1.456(7) . ? C9 C10 1.386(7) . ? C9 H9 0.9500 . ? C10 C11 1.402(8) . ? C10 H10 0.9500 . ? C11 N3 1.398(7) . ? C11 C12 1.402(8) . ? C12 C13 1.376(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O8 1.260(6) . ? C14 O7 1.283(6) . ? N1 O2 1.204(8) . ? N1 O1 1.232(10) . ? N2 O3 1.208(8) . ? N2 O4 1.219(8) . ? N3 H17 0.902(10) . ? O5 Mn1 2.055(4) 4_564 ? O7 Mn1 2.141(4) 7_644 ? O7 Mn1 2.207(4) 6_654 ? O8 Mn1 2.166(4) 5_444 ? 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 O5 Mn1 O6 104.9(2) 4_565 . ? O5 Mn1 O7 112.72(17) 4_565 7_654 ? O6 Mn1 O7 86.95(17) . 7_654 ? O5 Mn1 O8 94.05(18) 4_565 5 ? O6 Mn1 O8 160.94(19) . 5 ? O7 Mn1 O8 83.74(15) 7_654 5 ? O5 Mn1 O7 95.40(17) 4_565 6_655 ? O6 Mn1 O7 82.73(17) . 6_655 ? O7 Mn1 O7 151.71(13) 7_654 6_655 ? O8 Mn1 O7 97.81(15) 5 6_655 ? C6 C1 C2 119.0(5) . . ? C6 C1 C7 121.2(5) . . ? C2 C1 C7 119.7(5) . . ? C1 C2 C3 120.3(6) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C2 C3 C4 123.0(6) . . ? C2 C3 N1 116.6(6) . . ? C4 C3 N1 120.4(5) . . ? N3 C4 C3 123.1(5) . . ? N3 C4 C5 123.6(5) . . ? C3 C4 C5 113.3(5) . . ? C6 C5 C4 124.1(5) . . ? C6 C5 N2 115.2(6) . . ? C4 C5 N2 120.0(5) . . ? C5 C6 C1 120.2(6) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? O6 C7 O5 127.0(5) . . ? O6 C7 C1 118.1(5) . . ? O5 C7 C1 114.9(5) . . ? C9 C8 C13 119.0(4) . . ? C9 C8 C14 120.8(5) . . ? C13 C8 C14 120.3(4) . . ? C10 C9 C8 120.5(5) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.3(5) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? N3 C11 C12 119.6(5) . . ? N3 C11 C10 121.2(5) . . ? C12 C11 C10 119.2(4) . . ? C13 C12 C11 120.2(5) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 120.8(5) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? O8 C14 O7 119.9(4) . . ? O8 C14 C8 120.9(4) . . ? O7 C14 C8 119.1(4) . . ? O2 N1 O1 124.5(7) . . ? O2 N1 C3 119.4(6) . . ? O1 N1 C3 116.1(7) . . ? O3 N2 O4 125.0(6) . . ? O3 N2 C5 118.0(6) . . ? O4 N2 C5 117.0(6) . . ? C4 N3 C11 126.6(5) . . ? C4 N3 H17 126(5) . . ? C11 N3 H17 106(5) . . ? C7 O5 Mn1 132.6(4) . 4_564 ? C7 O6 Mn1 144.3(4) . . ? C14 O7 Mn1 128.9(3) . 7_644 ? C14 O7 Mn1 101.3(3) . 6_654 ? Mn1 O7 Mn1 125.24(17) 7_644 6_654 ? C14 O8 Mn1 138.7(4) . 5_444 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.867 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.123 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 679475' _database_code_CSD ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 Mn2 N10 O19' _chemical_formula_sum 'C48 H36 Mn2 N10 O19' _chemical_formula_weight 1166.75 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' 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 9.4695(14) _cell_length_b 15.348(2) _cell_length_c 17.220(2) _cell_angle_alpha 93.952(5) _cell_angle_beta 100.876(7) _cell_angle_gamma 102.557(5) _cell_volume 2383.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6376 _cell_measurement_theta_min 2.2528 _cell_measurement_theta_max 27.4835 _exptl_crystal_description sheet _exptl_crystal_colour orange _exptl_crystal_size_max 0.6000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details '(R.H. Blessing, 1995&1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18674 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10746 _reflns_number_gt 6376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku Corp.,2000)' _computing_cell_refinement 'CrystalClear(Rigaku Corp.,2000)' _computing_data_reduction 'CrystalClear(Rigaku Corp.,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+2.0380P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10746 _refine_ls_number_parameters 719 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1296 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2324 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 C1 C 0.4056(5) 0.3057(3) 0.4073(3) 0.0345(10) Uani 1 1 d . . . C2 C 0.3338(6) 0.3747(3) 0.4074(3) 0.0362(10) Uani 1 1 d . . . H2 H 0.2925 0.3931 0.3583 0.043 Uiso 1 1 calc R . . C3 C 0.3215(6) 0.4173(3) 0.4779(3) 0.0361(10) Uani 1 1 d . . . C4 C 0.3845(5) 0.3975(3) 0.5536(3) 0.0345(10) Uani 1 1 d . . . C5 C 0.4568(5) 0.3266(3) 0.5498(2) 0.0340(10) Uani 1 1 d . . . C6 C 0.4638(5) 0.2798(3) 0.4796(3) 0.0343(10) Uani 1 1 d . . . H6 H 0.5084 0.2299 0.4810 0.041 Uiso 1 1 calc R . . C7 C 0.4177(6) 0.2613(3) 0.3280(3) 0.0380(11) Uani 1 1 d . . . C8 C 0.3630(5) 0.4105(3) 0.6967(3) 0.0366(10) Uani 1 1 d . . . C9 C 0.4202(5) 0.4717(3) 0.7640(3) 0.0342(10) Uani 1 1 d . . . H9 H 0.4721 0.5308 0.7592 0.041 Uiso 1 1 calc R . . C10 C 0.4025(5) 0.4479(3) 0.8383(3) 0.0378(11) Uani 1 1 d . . . H10 H 0.4424 0.4907 0.8841 0.045 Uiso 1 1 calc R . . C11 C 0.3266(5) 0.3615(3) 0.8462(3) 0.0367(10) Uani 1 1 d . . . C12 C 0.2713(6) 0.3004(3) 0.7780(3) 0.0407(11) Uani 1 1 d . . . H12 H 0.2204 0.2410 0.7825 0.049 Uiso 1 1 calc R . . C13 C 0.2887(6) 0.3241(3) 0.7035(3) 0.0412(11) Uani 1 1 d . . . H13 H 0.2501 0.2814 0.6576 0.049 Uiso 1 1 calc R . . C14 C 0.2935(6) 0.3384(3) 0.9245(3) 0.0385(11) Uani 1 1 d . . . C15 C 0.0308(5) 0.1913(3) 0.2340(3) 0.0340(10) Uani 1 1 d . . . C16 C -0.0650(5) 0.2477(3) 0.2257(3) 0.0393(11) Uani 1 1 d . . . H16 H -0.0933 0.2676 0.1753 0.047 Uiso 1 1 calc R . . C17 C -0.1207(5) 0.2757(3) 0.2891(3) 0.0381(11) Uani 1 1 d . . . C18 C -0.0821(5) 0.2518(3) 0.3668(3) 0.0360(10) Uani 1 1 d . . . C19 C 0.0143(5) 0.1925(3) 0.3719(3) 0.0335(10) Uani 1 1 d . . . C20 C 0.1022(5) 0.1676(3) 0.1673(3) 0.0377(10) Uani 1 1 d . . . C21 C -0.1567(5) 0.2342(3) 0.4958(3) 0.0384(11) Uani 1 1 d . . . C22 C -0.1109(6) 0.2773(4) 0.5733(3) 0.0465(12) Uani 1 1 d . . . H22 H -0.0690 0.3401 0.5827 0.056 Uiso 1 1 calc R . . C23 C -0.1269(6) 0.2281(4) 0.6359(3) 0.0491(13) Uani 1 1 d . . . H23 H -0.0947 0.2577 0.6886 0.059 Uiso 1 1 calc R . . C24 C -0.1884(6) 0.1368(4) 0.6247(3) 0.0422(12) Uani 1 1 d . . . C25 C -0.2390(6) 0.0948(3) 0.5469(3) 0.0437(12) Uani 1 1 d . . . H25 H -0.2844 0.0323 0.5377 0.052 Uiso 1 1 calc R . . C26 C -0.2234(6) 0.1436(3) 0.4828(3) 0.0425(11) Uani 1 1 d . . . H26 H -0.2587 0.1146 0.4299 0.051 Uiso 1 1 calc R . . C27 C -0.1983(7) 0.0844(4) 0.6935(3) 0.0515(14) Uani 1 1 d . . . C28 C 0.6025(7) -0.0292(4) 0.3296(4) 0.0610(16) Uani 1 1 d . . . H28 H 0.5372 -0.0349 0.3656 0.073 Uiso 1 1 calc R . . C29 C 0.7261(8) -0.0635(4) 0.3469(5) 0.073(2) Uani 1 1 d . . . H29 H 0.7474 -0.0909 0.3942 0.088 Uiso 1 1 calc R . . C30 C 0.8173(8) -0.0569(5) 0.2934(6) 0.088(3) Uani 1 1 d . . . H30 H 0.9030 -0.0804 0.3032 0.106 Uiso 1 1 calc R . . C31 C 0.7849(7) -0.0162(5) 0.2255(5) 0.074(2) Uani 1 1 d . . . H31 H 0.8477 -0.0120 0.1883 0.089 Uiso 1 1 calc R . . C32 C 0.0671(5) 0.1619(3) 0.3086(3) 0.0351(10) Uani 1 1 d . . . H32 H 0.1286 0.1205 0.3157 0.042 Uiso 1 1 calc R . . C33 C 0.6145(6) 0.0633(4) 0.1412(3) 0.0514(14) Uani 1 1 d . . . C34 C 0.6943(8) 0.0749(5) 0.0810(4) 0.0702(19) Uani 1 1 d . . . H34 H 0.7836 0.0552 0.0850 0.084 Uiso 1 1 calc R . . C35 C 0.6430(10) 0.1152(5) 0.0157(5) 0.084(2) Uani 1 1 d . . . H35 H 0.6968 0.1236 -0.0257 0.101 Uiso 1 1 calc R . . C36 C 0.5134(10) 0.1430(5) 0.0110(4) 0.079(2) Uani 1 1 d . . . H36 H 0.4754 0.1710 -0.0332 0.095 Uiso 1 1 calc R . . C37 C 0.4404(8) 0.1286(4) 0.0729(3) 0.0620(17) Uani 1 1 d . . . H37 H 0.3494 0.1461 0.0694 0.074 Uiso 1 1 calc R . . C38 C -0.1004(6) 0.2696(4) -0.1026(3) 0.0509(13) Uani 1 1 d . . . H38 H -0.0508 0.2282 -0.1225 0.061 Uiso 1 1 calc R . . C39 C -0.2291(7) 0.2793(4) -0.1485(3) 0.0562(14) Uani 1 1 d . . . H39 H -0.2682 0.2450 -0.1990 0.067 Uiso 1 1 calc R . . C40 C -0.3009(7) 0.3392(4) -0.1207(4) 0.0618(16) Uani 1 1 d . . . H40 H -0.3903 0.3473 -0.1517 0.074 Uiso 1 1 calc R . . C41 C -0.2416(7) 0.3875(4) -0.0469(3) 0.0566(15) Uani 1 1 d . . . H41 H -0.2896 0.4297 -0.0268 0.068 Uiso 1 1 calc R . . C42 C -0.1120(6) 0.3743(3) -0.0024(3) 0.0412(11) Uani 1 1 d . . . C43 C -0.0395(6) 0.4221(3) 0.0780(3) 0.0433(12) Uani 1 1 d . . . C44 C -0.1056(7) 0.4795(4) 0.1168(3) 0.0548(14) Uani 1 1 d . . . H44 H -0.1970 0.4909 0.0915 0.066 Uiso 1 1 calc R . . C45 C -0.0365(7) 0.5195(4) 0.1924(3) 0.0590(15) Uani 1 1 d . . . H45 H -0.0806 0.5585 0.2200 0.071 Uiso 1 1 calc R . . C46 C 0.0951(7) 0.5033(4) 0.2275(3) 0.0545(14) Uani 1 1 d . . . H46 H 0.1441 0.5302 0.2797 0.065 Uiso 1 1 calc R . . C47 C 0.1557(7) 0.4460(4) 0.1846(3) 0.0534(14) Uani 1 1 d . . . H47 H 0.2477 0.4345 0.2087 0.064 Uiso 1 1 calc R . . C48 C 0.6596(6) 0.0185(4) 0.2119(4) 0.0518(14) Uani 1 1 d . . . H1 H 0.355(6) 0.485(4) 0.613(3) 0.039(16) Uiso 1 1 d . . . H4 H -0.184(8) 0.324(5) 0.420(4) 0.08(2) Uiso 1 1 d . . . N1 N 0.3738(5) 0.4423(3) 0.6227(2) 0.0424(10) Uani 1 1 d . . . N2 N 0.2324(5) 0.4847(3) 0.4710(2) 0.0445(10) Uani 1 1 d . . . N3 N 0.5407(5) 0.3024(3) 0.6228(2) 0.0444(10) Uani 1 1 d . . . N4 N -0.1335(5) 0.2825(3) 0.4303(3) 0.0452(10) Uani 1 1 d . . . N5 N -0.2259(5) 0.3324(3) 0.2712(3) 0.0470(10) Uani 1 1 d . . . N6 N 0.0796(5) 0.1652(3) 0.4487(2) 0.0453(10) Uani 1 1 d . . . N7 N 0.5698(5) 0.0115(3) 0.2650(3) 0.0480(11) Uani 1 1 d . . . N8 N 0.4893(5) 0.0919(3) 0.1365(3) 0.0490(11) Uani 1 1 d . . . N9 N -0.0408(5) 0.3160(3) -0.0305(2) 0.0418(9) Uani 1 1 d . . . N10 N 0.0908(5) 0.4066(3) 0.1115(2) 0.0437(10) Uani 1 1 d . . . O1 O 0.3882(5) 0.3032(2) 0.2702(2) 0.0528(10) Uani 1 1 d . . . O2 O 0.4545(4) 0.1876(2) 0.3271(2) 0.0519(10) Uani 1 1 d . . . O3 O 0.1311(5) 0.4751(3) 0.4137(2) 0.0715(13) Uani 1 1 d . . . O4 O 0.2647(5) 0.5494(3) 0.5229(2) 0.0624(11) Uani 1 1 d . . . O5 O 0.5289(5) 0.2233(3) 0.6309(2) 0.0635(11) Uani 1 1 d . . . O6 O 0.6205(5) 0.3635(3) 0.6706(2) 0.0675(12) Uani 1 1 d . . . O7 O 0.2383(4) 0.2585(2) 0.93423(19) 0.0455(8) Uani 1 1 d . . . O8 O 0.3154(4) 0.4018(2) 0.97932(19) 0.0508(9) Uani 1 1 d . . . O9 O 0.0706(4) 0.1996(3) 0.1030(2) 0.0509(9) Uani 1 1 d . . . O10 O 0.1897(4) 0.1167(3) 0.1791(2) 0.0498(9) Uani 1 1 d . . . O11 O -0.2948(5) 0.3261(3) 0.2032(3) 0.0674(12) Uani 1 1 d . . . O12 O -0.2404(5) 0.3841(3) 0.3254(3) 0.0668(12) Uani 1 1 d . . . O13 O 0.0829(6) 0.0860(3) 0.4508(2) 0.0726(13) Uani 1 1 d . . . O14 O 0.1300(4) 0.2241(3) 0.5050(2) 0.0537(10) Uani 1 1 d . . . O15 O -0.2766(5) 0.0061(3) 0.6804(2) 0.0581(10) Uani 1 1 d . . . O16 O -0.1264(7) 0.1214(4) 0.7599(3) 0.0929(18) Uani 1 1 d . . . O1W O 0.2323(10) -0.0472(5) 0.1386(4) 0.147(3) Uani 1 1 d . . . O2W O 0.3829(4) 0.3180(3) 0.1247(2) 0.0535(9) Uani 1 1 d . . . O3W O 0.9600(12) -0.0803(7) 0.0972(6) 0.081(3) Uiso 0.50 1 d P . . O3'W O 0.9831(13) -0.0278(7) 0.0229(6) 0.092(3) Uiso 0.50 1 d P . . Mn1 Mn 0.37289(9) 0.07335(5) 0.23910(4) 0.0426(2) Uani 1 1 d . . . Mn2 Mn 0.17377(9) 0.30487(5) 0.04516(4) 0.0412(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(3) 0.036(2) 0.030(2) -0.0015(18) 0.0077(19) 0.006(2) C2 0.048(3) 0.036(2) 0.025(2) 0.0017(17) 0.009(2) 0.010(2) C3 0.047(3) 0.029(2) 0.034(2) 0.0005(17) 0.011(2) 0.010(2) C4 0.043(3) 0.028(2) 0.033(2) 0.0022(17) 0.013(2) 0.006(2) C5 0.037(3) 0.041(2) 0.024(2) 0.0058(17) 0.0074(18) 0.007(2) C6 0.037(3) 0.035(2) 0.032(2) -0.0017(18) 0.0110(19) 0.009(2) C7 0.045(3) 0.044(3) 0.027(2) -0.0025(19) 0.011(2) 0.012(2) C8 0.040(3) 0.043(3) 0.032(2) 0.0046(19) 0.010(2) 0.017(2) C9 0.036(3) 0.033(2) 0.033(2) 0.0002(17) 0.0069(19) 0.007(2) C10 0.043(3) 0.044(3) 0.027(2) -0.0034(19) 0.004(2) 0.015(2) C11 0.044(3) 0.042(3) 0.031(2) 0.0043(19) 0.013(2) 0.019(2) C12 0.051(3) 0.037(3) 0.036(2) 0.0016(19) 0.015(2) 0.011(2) C13 0.055(3) 0.035(3) 0.033(2) -0.0014(19) 0.013(2) 0.006(2) C14 0.048(3) 0.046(3) 0.030(2) 0.005(2) 0.010(2) 0.025(2) C15 0.032(2) 0.037(2) 0.033(2) 0.0056(18) 0.0074(19) 0.007(2) C16 0.037(3) 0.040(3) 0.039(3) 0.010(2) 0.004(2) 0.006(2) C17 0.038(3) 0.036(3) 0.044(3) 0.012(2) 0.009(2) 0.016(2) C18 0.036(3) 0.028(2) 0.043(3) 0.0038(18) 0.008(2) 0.006(2) C19 0.037(3) 0.033(2) 0.032(2) 0.0072(17) 0.0084(19) 0.008(2) C20 0.040(3) 0.039(3) 0.030(2) 0.0029(19) 0.006(2) 0.004(2) C21 0.040(3) 0.040(3) 0.042(3) 0.005(2) 0.016(2) 0.016(2) C22 0.048(3) 0.039(3) 0.051(3) -0.006(2) 0.010(2) 0.009(2) C23 0.052(3) 0.055(3) 0.041(3) -0.005(2) 0.013(2) 0.014(3) C24 0.043(3) 0.051(3) 0.038(3) 0.003(2) 0.008(2) 0.023(2) C25 0.049(3) 0.040(3) 0.040(3) 0.000(2) 0.012(2) 0.005(2) C26 0.045(3) 0.042(3) 0.038(3) -0.001(2) 0.011(2) 0.005(2) C27 0.063(4) 0.061(4) 0.037(3) 0.000(2) 0.009(3) 0.033(3) C28 0.072(4) 0.045(3) 0.058(4) 0.003(3) -0.012(3) 0.021(3) C29 0.064(4) 0.047(4) 0.094(5) 0.007(3) -0.023(4) 0.019(3) C30 0.051(4) 0.060(4) 0.146(8) -0.005(5) -0.007(5) 0.025(4) C31 0.041(4) 0.060(4) 0.122(6) -0.003(4) 0.018(4) 0.013(3) C32 0.037(3) 0.034(2) 0.037(2) 0.0061(18) 0.012(2) 0.009(2) C33 0.054(3) 0.043(3) 0.055(3) -0.011(2) 0.021(3) 0.003(3) C34 0.059(4) 0.068(4) 0.083(5) -0.012(4) 0.039(4) 0.001(3) C35 0.106(6) 0.078(5) 0.068(5) -0.007(4) 0.054(4) -0.002(5) C36 0.118(7) 0.069(4) 0.064(4) 0.009(3) 0.046(4) 0.026(4) C37 0.092(5) 0.055(4) 0.051(3) 0.009(3) 0.027(3) 0.031(3) C38 0.057(4) 0.055(3) 0.044(3) 0.006(2) 0.003(3) 0.026(3) C39 0.056(4) 0.064(4) 0.046(3) 0.004(3) 0.001(3) 0.018(3) C40 0.055(4) 0.078(4) 0.053(3) 0.003(3) 0.001(3) 0.027(3) C41 0.055(4) 0.065(4) 0.058(3) 0.008(3) 0.010(3) 0.035(3) C42 0.045(3) 0.038(3) 0.046(3) 0.009(2) 0.012(2) 0.017(2) C43 0.050(3) 0.040(3) 0.044(3) 0.015(2) 0.015(2) 0.013(2) C44 0.056(4) 0.060(4) 0.056(3) 0.005(3) 0.016(3) 0.026(3) C45 0.067(4) 0.061(4) 0.053(3) -0.006(3) 0.018(3) 0.025(3) C46 0.062(4) 0.052(3) 0.048(3) 0.000(2) 0.013(3) 0.010(3) C47 0.056(4) 0.064(4) 0.040(3) 0.006(2) 0.007(3) 0.017(3) C48 0.042(3) 0.039(3) 0.070(4) -0.012(3) 0.009(3) 0.009(2) N1 0.068(3) 0.036(2) 0.030(2) 0.0050(17) 0.020(2) 0.016(2) N2 0.060(3) 0.042(2) 0.039(2) 0.0114(18) 0.015(2) 0.019(2) N3 0.039(2) 0.063(3) 0.034(2) 0.008(2) 0.0110(18) 0.017(2) N4 0.052(3) 0.038(2) 0.053(3) 0.0080(19) 0.020(2) 0.018(2) N5 0.044(3) 0.044(2) 0.058(3) 0.016(2) 0.010(2) 0.018(2) N6 0.042(2) 0.068(3) 0.032(2) 0.014(2) 0.0111(19) 0.020(2) N7 0.049(3) 0.040(2) 0.056(3) -0.0027(19) 0.006(2) 0.018(2) N8 0.062(3) 0.046(2) 0.046(2) -0.0008(19) 0.020(2) 0.021(2) N9 0.044(2) 0.045(2) 0.037(2) 0.0046(17) 0.0059(18) 0.015(2) N10 0.047(3) 0.049(2) 0.038(2) 0.0081(18) 0.0098(19) 0.017(2) O1 0.075(3) 0.055(2) 0.0302(18) 0.0010(15) 0.0150(17) 0.017(2) O2 0.070(3) 0.050(2) 0.0413(19) -0.0045(16) 0.0113(18) 0.029(2) O3 0.089(3) 0.079(3) 0.052(2) 0.001(2) -0.001(2) 0.046(3) O4 0.097(3) 0.048(2) 0.048(2) -0.0044(17) 0.015(2) 0.033(2) O5 0.076(3) 0.064(3) 0.060(3) 0.026(2) 0.010(2) 0.034(2) O6 0.063(3) 0.087(3) 0.044(2) -0.013(2) -0.008(2) 0.021(2) O7 0.058(2) 0.047(2) 0.0373(18) 0.0095(15) 0.0174(17) 0.0170(18) O8 0.071(3) 0.054(2) 0.0301(17) 0.0063(15) 0.0162(17) 0.016(2) O9 0.055(2) 0.064(2) 0.0336(18) 0.0150(16) 0.0070(16) 0.0132(19) O10 0.052(2) 0.065(2) 0.0392(19) 0.0060(16) 0.0109(17) 0.025(2) O11 0.061(3) 0.089(3) 0.061(3) 0.022(2) 0.002(2) 0.042(2) O12 0.084(3) 0.064(3) 0.068(3) 0.010(2) 0.019(2) 0.049(3) O13 0.114(4) 0.072(3) 0.053(2) 0.025(2) 0.019(2) 0.059(3) O14 0.042(2) 0.079(3) 0.0362(19) 0.0026(18) 0.0056(16) 0.008(2) O15 0.070(3) 0.062(3) 0.048(2) 0.0180(19) 0.020(2) 0.019(2) O16 0.136(5) 0.096(4) 0.044(2) -0.004(2) -0.010(3) 0.050(4) O1W 0.193(8) 0.119(6) 0.128(6) -0.007(4) 0.040(5) 0.037(6) O2W 0.049(2) 0.071(3) 0.042(2) 0.0145(18) 0.0063(17) 0.018(2) Mn1 0.0566(5) 0.0446(4) 0.0392(4) 0.0123(3) 0.0207(4) 0.0273(4) Mn2 0.0473(5) 0.0540(5) 0.0301(4) 0.0132(3) 0.0118(3) 0.0230(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 C1 C2 1.378(6) . ? C1 C6 1.384(6) . ? C1 C7 1.520(6) . ? C2 C3 1.376(6) . ? C2 H2 0.9500 . ? C3 C4 1.409(6) . ? C3 N2 1.468(6) . ? C4 N1 1.364(6) . ? C4 C5 1.410(6) . ? C5 C6 1.383(6) . ? C5 N3 1.471(6) . ? C6 H6 0.9500 . ? C7 O1 1.242(6) . ? C7 O2 1.254(6) . ? C8 C9 1.381(6) . ? C8 C13 1.384(7) . ? C8 N1 1.410(6) . ? C9 C10 1.385(6) . ? C9 H9 0.9500 . ? C10 C11 1.393(7) . ? C10 H10 0.9500 . ? C11 C12 1.392(6) . ? C11 C14 1.490(6) . ? C12 C13 1.386(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O7 1.260(6) . ? C14 O8 1.262(6) . ? C14 Mn2 2.578(5) 1_556 ? C15 C16 1.379(7) . ? C15 C32 1.398(6) . ? C15 C20 1.501(6) . ? C16 C17 1.381(7) . ? C16 H16 0.9500 . ? C17 C18 1.415(6) . ? C17 N5 1.463(6) . ? C18 N4 1.372(6) . ? C18 C19 1.418(6) . ? C19 C32 1.376(6) . ? C19 N6 1.480(6) . ? C20 O9 1.254(5) . ? C20 O10 1.255(6) . ? C21 C26 1.380(7) . ? C21 C22 1.394(7) . ? C21 N4 1.417(6) . ? C22 C23 1.370(8) . ? C22 H22 0.9500 . ? C23 C24 1.380(8) . ? C23 H23 0.9500 . ? C24 C25 1.395(7) . ? C24 C27 1.483(8) . ? C25 C26 1.389(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 O16 1.242(7) . ? C27 O15 1.248(7) . ? C28 N7 1.333(7) . ? C28 C29 1.376(9) . ? C28 H28 0.9500 . ? C29 C30 1.371(11) . ? C29 H29 0.9500 . ? C30 C31 1.378(11) . ? C30 H30 0.9500 . ? C31 C48 1.391(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 N8 1.342(7) . ? C33 C34 1.392(8) . ? C33 C48 1.477(8) . ? C34 C35 1.381(10) . ? C34 H34 0.9500 . ? C35 C36 1.375(11) . ? C35 H35 0.9500 . ? C36 C37 1.381(9) . ? C36 H36 0.9500 . ? C37 N8 1.319(7) . ? C37 H37 0.9500 . ? C38 N9 1.344(6) . ? C38 C39 1.365(8) . ? C38 H38 0.9500 . ? C39 C40 1.367(8) . ? C39 H39 0.9500 . ? C40 C41 1.377(8) . ? C40 H40 0.9500 . ? C41 C42 1.382(7) . ? C41 H41 0.9500 . ? C42 N9 1.347(6) . ? C42 C43 1.485(7) . ? C43 N10 1.338(7) . ? C43 C44 1.390(7) . ? C44 C45 1.376(8) . ? C44 H44 0.9500 . ? C45 C46 1.361(8) . ? C45 H45 0.9500 . ? C46 C47 1.392(8) . ? C46 H46 0.9500 . ? C47 N10 1.330(7) . ? C47 H47 0.9500 . ? C48 N7 1.356(7) . ? N1 H1 0.74(5) . ? N2 O3 1.215(6) . ? N2 O4 1.233(5) . ? N3 O5 1.216(6) . ? N3 O6 1.216(6) . ? N4 H4 0.88(7) . ? N5 O11 1.215(6) . ? N5 O12 1.230(6) . ? N6 O13 1.225(6) . ? N6 O14 1.225(6) . ? N7 Mn1 2.256(4) . ? N8 Mn1 2.255(4) . ? N9 Mn2 2.245(4) . ? N10 Mn2 2.233(4) . ? O2 Mn1 2.137(3) . ? O7 Mn2 2.230(3) 1_556 ? O8 Mn2 2.288(4) 1_556 ? O9 Mn2 2.112(4) . ? O10 Mn1 2.107(4) . ? O15 Mn1 2.113(4) 2_556 ? O1W Mn1 2.410(7) . ? O2W Mn2 2.145(4) . ? O3W O3'W 1.583(14) . ? O3'W O3'W 1.23(2) 2_755 ? Mn1 O15 2.113(4) 2_556 ? Mn2 O7 2.230(3) 1_554 ? Mn2 O8 2.288(4) 1_554 ? Mn2 C14 2.578(5) 1_554 ? 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 C2 C1 C6 118.6(4) . . ? C2 C1 C7 118.6(4) . . ? C6 C1 C7 122.8(4) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 123.9(4) . . ? C2 C3 N2 115.9(4) . . ? C4 C3 N2 120.1(4) . . ? N1 C4 C3 122.7(4) . . ? N1 C4 C5 124.3(4) . . ? C3 C4 C5 113.0(4) . . ? C6 C5 C4 124.0(4) . . ? C6 C5 N3 115.4(4) . . ? C4 C5 N3 120.4(4) . . ? C5 C6 C1 119.8(4) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? O1 C7 O2 127.1(4) . . ? O1 C7 C1 114.9(4) . . ? O2 C7 C1 118.0(4) . . ? C9 C8 C13 119.8(4) . . ? C9 C8 N1 117.2(4) . . ? C13 C8 N1 122.8(4) . . ? C8 C9 C10 120.8(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 120.2(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 118.3(4) . . ? C12 C11 C14 121.1(5) . . ? C10 C11 C14 120.4(4) . . ? C13 C12 C11 121.6(5) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C8 C13 C12 119.3(4) . . ? C8 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? O7 C14 O8 121.2(4) . . ? O7 C14 C11 120.8(4) . . ? O8 C14 C11 117.9(4) . . ? O7 C14 Mn2 59.8(2) . 1_556 ? O8 C14 Mn2 62.5(3) . 1_556 ? C11 C14 Mn2 165.9(3) . 1_556 ? C16 C15 C32 117.6(4) . . ? C16 C15 C20 121.4(4) . . ? C32 C15 C20 120.9(4) . . ? C15 C16 C17 121.4(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C18 123.6(4) . . ? C16 C17 N5 115.6(4) . . ? C18 C17 N5 120.8(4) . . ? N4 C18 C17 123.3(4) . . ? N4 C18 C19 123.8(4) . . ? C17 C18 C19 112.8(4) . . ? C32 C19 C18 124.1(4) . . ? C32 C19 N6 113.5(4) . . ? C18 C19 N6 122.1(4) . . ? O9 C20 O10 124.0(4) . . ? O9 C20 C15 117.9(4) . . ? O10 C20 C15 118.1(4) . . ? C26 C21 C22 119.7(5) . . ? C26 C21 N4 119.8(4) . . ? C22 C21 N4 120.5(5) . . ? C23 C22 C21 119.4(5) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 122.1(5) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C23 C24 C25 118.2(5) . . ? C23 C24 C27 121.0(5) . . ? C25 C24 C27 120.8(5) . . ? C26 C25 C24 120.4(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C21 C26 C25 120.1(4) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? O16 C27 O15 124.7(6) . . ? O16 C27 C24 117.5(6) . . ? O15 C27 C24 117.8(5) . . ? N7 C28 C29 123.3(7) . . ? N7 C28 H28 118.3 . . ? C29 C28 H28 118.3 . . ? C30 C29 C28 117.6(7) . . ? C30 C29 H29 121.2 . . ? C28 C29 H29 121.2 . . ? C29 C30 C31 120.2(6) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C48 119.6(7) . . ? C30 C31 H31 120.2 . . ? C48 C31 H31 120.2 . . ? C19 C32 C15 120.4(4) . . ? C19 C32 H32 119.8 . . ? C15 C32 H32 119.8 . . ? N8 C33 C34 120.5(6) . . ? N8 C33 C48 116.5(5) . . ? C34 C33 C48 123.0(6) . . ? C35 C34 C33 119.7(7) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C36 C35 C34 119.3(6) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 117.5(7) . . ? C35 C36 H36 121.2 . . ? C37 C36 H36 121.2 . . ? N8 C37 C36 124.0(7) . . ? N8 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? N9 C38 C39 122.9(5) . . ? N9 C38 H38 118.5 . . ? C39 C38 H38 118.5 . . ? C38 C39 C40 119.1(5) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C39 C40 C41 119.0(6) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C40 C41 C42 119.7(5) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? N9 C42 C41 121.0(5) . . ? N9 C42 C43 114.8(4) . . ? C41 C42 C43 124.1(5) . . ? N10 C43 C44 121.7(5) . . ? N10 C43 C42 117.1(4) . . ? C44 C43 C42 121.2(5) . . ? C45 C44 C43 118.9(5) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? C46 C45 C44 120.0(5) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 118.0(5) . . ? C45 C46 H46 121.0 . . ? C47 C46 H46 121.0 . . ? N10 C47 C46 123.1(5) . . ? N10 C47 H47 118.5 . . ? C46 C47 H47 118.5 . . ? N7 C48 C31 119.9(6) . . ? N7 C48 C33 116.1(5) . . ? C31 C48 C33 124.0(6) . . ? C4 N1 C8 129.5(4) . . ? C4 N1 H1 107(4) . . ? C8 N1 H1 122(4) . . ? O3 N2 O4 122.7(4) . . ? O3 N2 C3 118.6(4) . . ? O4 N2 C3 118.7(4) . . ? O5 N3 O6 124.1(5) . . ? O5 N3 C5 118.5(4) . . ? O6 N3 C5 117.4(4) . . ? C18 N4 C21 124.5(4) . . ? C18 N4 H4 114(4) . . ? C21 N4 H4 118(4) . . ? O11 N5 O12 123.1(4) . . ? O11 N5 C17 118.2(4) . . ? O12 N5 C17 118.7(4) . . ? O13 N6 O14 124.9(4) . . ? O13 N6 C19 117.7(4) . . ? O14 N6 C19 117.4(4) . . ? C28 N7 C48 119.4(5) . . ? C28 N7 Mn1 123.5(4) . . ? C48 N7 Mn1 117.1(4) . . ? C37 N8 C33 119.0(5) . . ? C37 N8 Mn1 123.5(4) . . ? C33 N8 Mn1 117.5(4) . . ? C38 N9 C42 118.3(4) . . ? C38 N9 Mn2 124.0(3) . . ? C42 N9 Mn2 117.7(3) . . ? C47 N10 C43 118.4(5) . . ? C47 N10 Mn2 124.1(4) . . ? C43 N10 Mn2 117.2(3) . . ? C7 O2 Mn1 128.2(3) . . ? C14 O7 Mn2 90.9(3) . 1_556 ? C14 O8 Mn2 88.2(3) . 1_556 ? C20 O9 Mn2 136.2(3) . . ? C20 O10 Mn1 156.1(3) . . ? C27 O15 Mn1 128.7(4) . 2_556 ? O3'W O3'W O3W 166.5(16) 2_755 . ? O10 Mn1 O15 101.19(16) . 2_556 ? O10 Mn1 O2 96.21(14) . . ? O15 Mn1 O2 92.18(16) 2_556 . ? O10 Mn1 N8 92.57(15) . . ? O15 Mn1 N8 152.32(16) 2_556 . ? O2 Mn1 N8 110.23(16) . . ? O10 Mn1 N7 162.48(15) . . ? O15 Mn1 N7 88.81(17) 2_556 . ? O2 Mn1 N7 97.76(15) . . ? N8 Mn1 N7 72.69(17) . . ? O10 Mn1 O1W 73.0(2) . . ? O15 Mn1 O1W 85.1(2) 2_556 . ? O2 Mn1 O1W 168.1(2) . . ? N8 Mn1 O1W 76.0(2) . . ? N7 Mn1 O1W 93.8(2) . . ? O9 Mn2 O2W 91.76(14) . . ? O9 Mn2 O7 114.02(14) . 1_554 ? O2W Mn2 O7 97.43(14) . 1_554 ? O9 Mn2 N10 92.22(15) . . ? O2W Mn2 N10 98.43(15) . . ? O7 Mn2 N10 148.76(14) 1_554 . ? O9 Mn2 N9 93.40(15) . . ? O2W Mn2 N9 170.15(15) . . ? O7 Mn2 N9 88.13(14) 1_554 . ? N10 Mn2 N9 73.00(15) . . ? O9 Mn2 O8 169.12(14) . 1_554 ? O2W Mn2 O8 82.32(14) . 1_554 ? O7 Mn2 O8 58.17(13) 1_554 1_554 ? N10 Mn2 O8 97.66(14) . 1_554 ? N9 Mn2 O8 93.84(15) . 1_554 ? O9 Mn2 C14 143.25(15) . 1_554 ? O2W Mn2 C14 93.14(15) . 1_554 ? O7 Mn2 C14 29.25(13) 1_554 1_554 ? N10 Mn2 C14 122.91(15) . 1_554 ? N9 Mn2 C14 87.74(15) . 1_554 ? O8 Mn2 C14 29.29(14) 1_554 1_554 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.931 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.075 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 679476' _database_code_CSD ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H26 Mn2 N8 O18' _chemical_formula_sum 'C38 H26 Mn2 N8 O18' _chemical_formula_weight 992.55 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.7150(19) _cell_length_b 12.9166(7) _cell_length_c 25.9898(19) _cell_angle_alpha 90.00 _cell_angle_beta 114.048(3) _cell_angle_gamma 90.00 _cell_volume 8189.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8195 _cell_measurement_theta_min 3.0706 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.6000 _exptl_crystal_size_mid 0.3000 _exptl_crystal_size_min 0.1200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details '(R.H. Blessing, 1995&1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31179 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9378 _reflns_number_gt 8195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku Corp.,2000)' _computing_cell_refinement 'CrystalClear(Rigaku Corp.,2000)' _computing_data_reduction 'CrystalClear(Rigaku Corp.,2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1230P)^2^+16.5303P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9378 _refine_ls_number_parameters 597 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1986 _refine_ls_wR_factor_gt 0.1900 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.0000 0.91208(5) 0.2500 0.03150(17) Uani 1 2 d S . . Mn2 Mn 0.060798(18) 0.84875(3) 0.396756(18) 0.03121(14) Uani 1 1 d . . . Mn3 Mn 0.0000 1.0000 0.5000 0.03238(17) Uani 1 2 d S . . C1 C 0.08956(13) 1.1744(3) 0.36240(13) 0.0376(7) Uani 1 1 d . . . C2 C 0.12600(14) 1.2087(3) 0.41496(14) 0.0445(8) Uani 1 1 d . . . H2 H 0.1388 1.1619 0.4459 0.053 Uiso 1 1 calc R . . C3 C 0.14380(14) 1.3104(3) 0.42273(15) 0.0460(8) Uani 1 1 d . . . C4 C 0.12895(13) 1.3835(3) 0.37905(17) 0.0460(8) Uani 1 1 d . . . C5 C 0.08971(15) 1.3469(3) 0.32733(17) 0.0498(9) Uani 1 1 d . . . C6 C 0.07117(14) 1.2459(3) 0.31905(15) 0.0458(8) Uani 1 1 d . . . H6 H 0.0453 1.2251 0.2829 0.055 Uiso 1 1 calc R . . C7 C 0.32183(13) 1.5359(3) 0.46273(14) 0.0386(7) Uani 1 1 d . . . C8 C 0.28400(16) 1.6104(3) 0.4624(2) 0.0622(11) Uani 1 1 d . . . H8 H 0.2969 1.6758 0.4793 0.075 Uiso 1 1 calc R . . C9 C 0.22791(18) 1.5920(3) 0.4380(2) 0.0693(13) Uani 1 1 d . . . H9 H 0.2027 1.6437 0.4383 0.083 Uiso 1 1 calc R . . C10 C 0.20941(14) 1.4960(3) 0.41306(18) 0.0491(9) Uani 1 1 d . . . C11 C 0.24595(15) 1.4230(3) 0.41203(16) 0.0466(8) Uani 1 1 d . . . H11 H 0.2330 1.3582 0.3943 0.056 Uiso 1 1 calc R . . C12 C 0.30184(14) 1.4428(3) 0.43672(15) 0.0420(7) Uani 1 1 d . . . H12 H 0.3267 1.3913 0.4356 0.050 Uiso 1 1 calc R . . C13 C 0.07137(13) 1.0638(3) 0.35201(13) 0.0380(7) Uani 1 1 d . . . C14 C 0.38185(12) 1.5596(2) 0.48752(12) 0.0333(6) Uani 1 1 d . . . C15 C -0.34888(16) 1.2658(4) 0.29940(17) 0.0569(10) Uani 1 1 d . . . C16 C -0.29273(18) 1.2729(4) 0.3317(2) 0.0669(12) Uani 1 1 d . . . H16 H -0.2795 1.2954 0.3698 0.080 Uiso 1 1 calc R . . C17 C -0.25638(17) 1.2474(5) 0.3085(2) 0.0728(14) Uani 1 1 d . . . C18 C -0.27216(18) 1.2074(5) 0.25439(18) 0.0766(17) Uani 1 1 d . . . C19 C -0.3299(2) 1.2097(6) 0.22186(19) 0.088(2) Uani 1 1 d . . . C20 C -0.36655(17) 1.2375(5) 0.24385(19) 0.0725(15) Uani 1 1 d . . . H20 H -0.4047 1.2372 0.2204 0.087 Uiso 1 1 calc R . . C21 C -0.09321(13) 0.9964(3) 0.32655(13) 0.0406(7) Uani 1 1 d . . . C22 C -0.09757(19) 1.0595(5) 0.2822(2) 0.0747(16) Uani 1 1 d . . . H22 H -0.0677 1.0640 0.2713 0.090 Uiso 1 1 calc R . . C23 C -0.1444(2) 1.1164(6) 0.2532(2) 0.094(2) Uani 1 1 d . . . H23 H -0.1462 1.1599 0.2230 0.113 Uiso 1 1 calc R . . C24 C -0.18818(18) 1.1107(5) 0.26759(17) 0.0760(16) Uani 1 1 d . . . C25 C -0.18445(16) 1.0488(5) 0.31255(19) 0.0705(14) Uani 1 1 d . . . H25 H -0.2147 1.0436 0.3227 0.085 Uiso 1 1 calc R . . C26 C -0.13660(15) 0.9946(4) 0.34280(17) 0.0556(10) Uani 1 1 d . . . H26 H -0.1335 0.9558 0.3750 0.067 Uiso 1 1 calc R . . C27 C -0.38893(16) 1.2925(3) 0.32426(19) 0.0539(10) Uani 1 1 d . . . C28 C -0.04166(12) 0.9370(2) 0.35785(12) 0.0330(6) Uani 1 1 d . . . C29 C -0.03212(16) 1.2099(3) 0.42686(15) 0.0479(8) Uani 1 1 d . . . H29 H -0.0634 1.1717 0.4032 0.057 Uiso 1 1 calc R . . C30 C -0.02591(17) 1.3103(3) 0.41116(15) 0.0491(8) Uani 1 1 d . . . H30 H -0.0516 1.3383 0.3767 0.059 Uiso 1 1 calc R . . C31 C 0.01871(14) 1.3698(2) 0.44677(14) 0.0385(7) Uani 1 1 d . . . C32 C 0.05477(15) 1.3224(3) 0.49584(15) 0.0430(7) Uani 1 1 d . . . H32 H 0.0856 1.3595 0.5214 0.052 Uiso 1 1 calc R . . C33 C 0.04597(15) 1.2220(3) 0.50740(15) 0.0442(8) Uani 1 1 d . . . H33 H 0.0712 1.1915 0.5413 0.053 Uiso 1 1 calc R . . C34 C 0.02693(14) 1.4783(2) 0.43397(14) 0.0380(7) Uani 1 1 d . . . C35 C 0.00702(18) 1.5162(3) 0.37959(16) 0.0520(9) Uani 1 1 d . . . H35 H -0.0128 1.4719 0.3488 0.062 Uiso 1 1 calc R . . C36 C 0.01592(18) 1.6188(3) 0.36991(15) 0.0502(9) Uani 1 1 d . . . H36 H 0.0019 1.6431 0.3321 0.060 Uiso 1 1 calc R . . C37 C 0.06271(18) 1.6480(3) 0.46391(15) 0.0478(8) Uani 1 1 d . . . H37 H 0.0825 1.6938 0.4939 0.057 Uiso 1 1 calc R . . C38 C 0.05540(17) 1.5467(3) 0.47667(15) 0.0463(8) Uani 1 1 d . . . H38 H 0.0700 1.5243 0.5148 0.056 Uiso 1 1 calc R . . H1A H 0.1298 1.5347 0.3717 0.056 Uiso 1 1 d R . . H4A H -0.2448 1.1725 0.1975 0.056 Uiso 1 1 d R . . N1 N 0.15184(13) 1.4797(2) 0.38518(18) 0.0611(10) Uani 1 1 d . . . N2 N 0.06991(19) 1.4121(3) 0.27682(19) 0.0816(14) Uani 1 1 d . . . N3 N 0.17666(16) 1.3421(3) 0.48058(15) 0.0613(9) Uani 1 1 d . . . N4 N -0.23680(17) 1.1648(5) 0.23449(16) 0.0947(19) Uani 1 1 d . . . N5 N -0.19828(18) 1.2757(5) 0.3419(3) 0.0952(16) Uani 1 1 d . . . N6 N -0.3533(2) 1.1775(9) 0.1625(2) 0.161(4) Uani 1 1 d . . . N7 N 0.00340(12) 1.1648(2) 0.47315(12) 0.0402(6) Uani 1 1 d . . . N8 N 0.04307(12) 1.6845(2) 0.41103(12) 0.0406(6) Uani 1 1 d . . . O1 O 0.04316(12) 1.0399(2) 0.30182(10) 0.0538(7) Uani 1 1 d . . . O2 O 0.08552(12) 1.00592(19) 0.39354(11) 0.0533(7) Uani 1 1 d . . . O3 O 0.2036(3) 1.2759(3) 0.51270(18) 0.137(2) Uani 1 1 d . . . O4 O 0.17499(17) 1.4308(3) 0.49509(17) 0.0874(11) Uani 1 1 d . . . O5 O 0.0507(3) 1.3682(4) 0.23061(18) 0.125(2) Uani 1 1 d . . . O6 O 0.07236(19) 1.5071(3) 0.2820(2) 0.1032(16) Uani 1 1 d . . . O7 O 0.41290(9) 1.49945(19) 0.47721(10) 0.0420(5) Uani 1 1 d . . . O8 O 0.39689(10) 1.64029(17) 0.51667(9) 0.0404(5) Uani 1 1 d . . . O9 O -0.37158(14) 1.3013(3) 0.37633(14) 0.0713(9) Uani 1 1 d . . . O10 O -0.43878(11) 1.3011(2) 0.29141(14) 0.0610(8) Uani 1 1 d . . . O11 O -0.18077(19) 1.2669(6) 0.3925(2) 0.132(2) Uani 1 1 d . . . O12 O -0.17192(19) 1.3073(5) 0.3164(3) 0.129(2) Uani 1 1 d . . . O13 O -0.3985(3) 1.1673(10) 0.1384(3) 0.217(5) Uani 1 1 d . . . O14 O -0.3257(3) 1.1920(11) 0.1357(2) 0.255(6) Uani 1 1 d . . . O15 O -0.02090(9) 0.93336(19) 0.41037(9) 0.0411(5) Uani 1 1 d . . . O16 O -0.01956(9) 0.89028(18) 0.32966(9) 0.0372(5) Uani 1 1 d . . . O1W O -0.2283(4) 1.1347(14) 0.1274(4) 0.294(8) Uani 1 1 d . . . O2W O -0.2895(5) 1.4796(11) 0.4158(6) 0.259(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0297(3) 0.0281(3) 0.0334(3) 0.000 0.0095(2) 0.000 Mn2 0.0315(2) 0.0245(2) 0.0342(2) 0.00301(16) 0.00988(19) -0.00082(16) Mn3 0.0352(3) 0.0229(3) 0.0393(3) 0.0029(2) 0.0154(3) -0.0021(2) C1 0.0358(15) 0.0339(16) 0.0397(15) 0.0000(12) 0.0119(12) -0.0116(12) C2 0.0429(17) 0.0443(19) 0.0392(16) 0.0055(14) 0.0094(14) -0.0112(14) C3 0.0406(17) 0.048(2) 0.0442(17) -0.0044(15) 0.0121(14) -0.0170(15) C4 0.0303(15) 0.0374(17) 0.063(2) 0.0022(16) 0.0111(15) -0.0067(13) C5 0.0381(17) 0.0415(19) 0.056(2) 0.0153(15) 0.0049(15) -0.0053(14) C6 0.0398(17) 0.0409(18) 0.0450(17) 0.0053(14) 0.0054(14) -0.0090(14) C7 0.0393(16) 0.0329(16) 0.0412(15) -0.0029(13) 0.0138(13) -0.0086(13) C8 0.044(2) 0.044(2) 0.094(3) -0.027(2) 0.024(2) -0.0168(17) C9 0.045(2) 0.046(2) 0.115(4) -0.017(2) 0.030(2) -0.0088(17) C10 0.0364(17) 0.0359(18) 0.066(2) 0.0041(16) 0.0124(16) -0.0087(13) C11 0.0422(18) 0.0369(17) 0.0527(19) -0.0085(15) 0.0110(15) -0.0133(14) C12 0.0384(16) 0.0372(17) 0.0482(18) -0.0057(14) 0.0156(14) -0.0060(13) C13 0.0373(15) 0.0343(16) 0.0401(15) 0.0019(12) 0.0133(13) -0.0096(12) C14 0.0362(15) 0.0295(14) 0.0301(13) 0.0015(11) 0.0093(11) -0.0062(12) C15 0.0441(19) 0.077(3) 0.057(2) 0.025(2) 0.0277(17) 0.0276(19) C16 0.049(2) 0.092(4) 0.061(2) 0.016(2) 0.0248(19) 0.024(2) C17 0.041(2) 0.116(4) 0.066(3) 0.025(3) 0.027(2) 0.027(2) C18 0.051(2) 0.135(5) 0.052(2) 0.039(3) 0.0286(19) 0.049(3) C19 0.054(2) 0.162(6) 0.053(2) 0.029(3) 0.024(2) 0.058(3) C20 0.043(2) 0.120(4) 0.056(2) 0.027(3) 0.0223(18) 0.040(2) C21 0.0316(15) 0.056(2) 0.0346(15) 0.0031(14) 0.0138(12) 0.0096(14) C22 0.058(2) 0.115(4) 0.069(3) 0.043(3) 0.045(2) 0.046(3) C23 0.075(3) 0.159(6) 0.071(3) 0.065(4) 0.052(3) 0.065(4) C24 0.047(2) 0.142(5) 0.045(2) 0.031(3) 0.0254(18) 0.049(3) C25 0.0378(19) 0.117(4) 0.063(2) 0.024(3) 0.0270(18) 0.021(2) C26 0.0388(18) 0.079(3) 0.052(2) 0.0169(19) 0.0221(16) 0.0091(18) C27 0.051(2) 0.053(2) 0.071(2) 0.0221(19) 0.0387(19) 0.0207(17) C28 0.0275(13) 0.0346(15) 0.0376(14) 0.0015(12) 0.0141(11) -0.0014(11) C29 0.053(2) 0.0327(17) 0.0464(18) 0.0011(14) 0.0079(15) -0.0111(14) C30 0.064(2) 0.0313(17) 0.0407(17) 0.0058(13) 0.0094(16) -0.0061(15) C31 0.0485(18) 0.0263(14) 0.0421(16) 0.0001(12) 0.0198(14) -0.0051(13) C32 0.0462(18) 0.0296(16) 0.0460(17) 0.0024(13) 0.0113(14) -0.0084(13) C33 0.0455(18) 0.0312(16) 0.0476(18) 0.0062(13) 0.0104(14) -0.0051(13) C34 0.0491(17) 0.0240(14) 0.0407(16) 0.0010(12) 0.0181(14) -0.0025(13) C35 0.075(3) 0.0286(16) 0.0412(17) -0.0025(13) 0.0120(17) -0.0098(16) C36 0.072(2) 0.0293(16) 0.0394(17) 0.0043(13) 0.0126(16) -0.0073(16) C37 0.070(2) 0.0270(16) 0.0390(17) -0.0011(13) 0.0149(16) -0.0103(15) C38 0.071(2) 0.0271(15) 0.0383(16) 0.0000(13) 0.0197(16) -0.0076(15) N1 0.0367(15) 0.0338(16) 0.096(3) 0.0100(16) 0.0098(16) -0.0081(12) N2 0.072(3) 0.066(3) 0.073(3) 0.028(2) -0.005(2) -0.015(2) N3 0.068(2) 0.056(2) 0.0519(19) -0.0027(16) 0.0158(17) -0.0200(17) N4 0.057(2) 0.184(5) 0.052(2) 0.048(3) 0.0318(18) 0.068(3) N5 0.051(2) 0.131(5) 0.104(4) 0.021(3) 0.033(3) 0.021(3) N6 0.066(3) 0.360(12) 0.055(3) 0.016(5) 0.023(2) 0.092(5) N7 0.0484(15) 0.0244(12) 0.0476(15) 0.0028(11) 0.0193(13) -0.0051(11) N8 0.0537(16) 0.0240(12) 0.0434(14) 0.0020(11) 0.0190(13) -0.0029(11) O1 0.0716(17) 0.0471(15) 0.0384(12) -0.0067(11) 0.0181(12) -0.0248(13) O2 0.0609(16) 0.0358(13) 0.0481(14) 0.0085(10) 0.0067(12) -0.0175(11) O3 0.191(5) 0.072(3) 0.062(2) 0.008(2) -0.035(3) -0.017(3) O4 0.092(3) 0.073(2) 0.089(3) -0.034(2) 0.028(2) -0.016(2) O5 0.173(5) 0.090(3) 0.060(2) 0.024(2) -0.006(3) -0.030(3) O6 0.094(3) 0.058(2) 0.112(3) 0.037(2) -0.005(2) -0.0058(19) O7 0.0347(11) 0.0409(13) 0.0474(13) -0.0045(10) 0.0136(10) -0.0046(9) O8 0.0456(12) 0.0295(11) 0.0372(11) -0.0007(9) 0.0075(10) -0.0102(9) O9 0.0692(19) 0.092(2) 0.0699(19) 0.0125(18) 0.0458(17) 0.0232(18) O10 0.0465(14) 0.0578(17) 0.091(2) 0.0264(15) 0.0403(15) 0.0222(13) O11 0.065(3) 0.225(7) 0.088(3) 0.012(4) 0.012(2) 0.005(3) O12 0.071(3) 0.176(5) 0.164(5) 0.038(4) 0.071(3) 0.011(3) O13 0.093(4) 0.460(16) 0.091(4) -0.060(6) 0.030(3) -0.002(7) O14 0.128(5) 0.585(19) 0.060(3) 0.047(6) 0.047(3) 0.144(8) O15 0.0404(12) 0.0453(13) 0.0332(11) 0.0031(9) 0.0105(9) 0.0034(10) O16 0.0324(10) 0.0394(12) 0.0411(11) 0.0006(9) 0.0164(9) 0.0051(9) O1W 0.166(8) 0.59(3) 0.108(5) 0.062(9) 0.041(5) 0.034(11) O2W 0.196(10) 0.316(15) 0.244(11) -0.072(11) 0.067(9) -0.055(9) _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 O10 2.110(3) 3_545 ? Mn1 O10 2.110(3) 4_445 ? Mn1 O1 2.146(2) . ? Mn1 O1 2.146(2) 2 ? Mn1 O16 2.350(2) 2 ? Mn1 O16 2.350(2) . ? Mn2 O8 2.071(2) 7_576 ? Mn2 O2 2.147(2) . ? Mn2 O9 2.169(3) 3_545 ? Mn2 O16 2.210(2) . ? Mn2 N8 2.238(3) 1_545 ? Mn3 O7 2.154(2) 3_445 ? Mn3 O7 2.154(2) 7_576 ? Mn3 N7 2.253(3) . ? Mn3 N7 2.253(3) 5_576 ? Mn3 O15 2.328(2) . ? Mn3 O15 2.328(2) 5_576 ? C1 C6 1.382(5) . ? C1 C2 1.388(5) . ? C1 C13 1.498(4) . ? C2 C3 1.384(5) . ? C2 H2 0.9500 . ? C3 C4 1.404(5) . ? C3 N3 1.457(5) . ? C4 N1 1.366(5) . ? C4 C5 1.407(5) . ? C5 C6 1.382(5) . ? C5 N2 1.465(5) . ? C6 H6 0.9500 . ? C7 C12 1.375(5) . ? C7 C8 1.393(6) . ? C7 C14 1.496(4) . ? C8 C9 1.389(6) . ? C8 H8 0.9500 . ? C9 C10 1.392(6) . ? C9 H9 0.9500 . ? C10 C11 1.366(5) . ? C10 N1 1.424(5) . ? C11 C12 1.388(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 O2 1.239(4) . ? C13 O1 1.250(4) . ? C14 O7 1.243(4) . ? C14 O8 1.255(4) . ? C15 C20 1.373(6) . ? C15 C16 1.392(6) . ? C15 C27 1.498(5) . ? C16 C17 1.376(6) . ? C16 H16 0.9500 . ? C17 C18 1.393(7) . ? C17 N5 1.483(7) . ? C18 N4 1.364(5) . ? C18 C19 1.426(6) . ? C19 C20 1.367(6) . ? C19 N6 1.469(8) . ? C20 H20 0.9500 . ? C21 C22 1.378(5) . ? C21 C26 1.386(5) . ? C21 C28 1.495(4) . ? C22 C23 1.380(6) . ? C22 H22 0.9500 . ? C23 C24 1.367(6) . ? C23 H23 0.9500 . ? C24 C25 1.386(6) . ? C24 N4 1.416(5) . ? C25 C26 1.387(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 O9 1.244(5) . ? C27 O10 1.260(5) . ? C28 O15 1.248(4) . ? C28 O16 1.266(4) . ? C29 N7 1.326(5) . ? C29 C30 1.389(5) . ? C29 H29 0.9500 . ? C30 C31 1.404(5) . ? C30 H30 0.9500 . ? C31 C32 1.388(5) . ? C31 C34 1.477(4) . ? C32 C33 1.373(5) . ? C32 H32 0.9500 . ? C33 N7 1.345(4) . ? C33 H33 0.9500 . ? C34 C38 1.380(5) . ? C34 C35 1.381(5) . ? C35 C36 1.388(5) . ? C35 H35 0.9500 . ? C36 N8 1.325(4) . ? C36 H36 0.9500 . ? C37 N8 1.341(4) . ? C37 C38 1.383(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? N1 H1A 0.8968 . ? N2 O6 1.233(6) . ? N2 O5 1.235(6) . ? N3 O3 1.207(6) . ? N3 O4 1.212(5) . ? N4 H4A 0.9019 . ? N5 O11 1.207(7) . ? N5 O12 1.218(7) . ? N6 O13 1.119(8) . ? N6 O14 1.216(9) . ? N8 Mn2 2.238(3) 1_565 ? O7 Mn3 2.154(2) 3 ? O8 Mn2 2.071(2) 7_576 ? O9 Mn2 2.169(3) 3_455 ? O10 Mn1 2.110(3) 3_455 ? 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 O10 Mn1 O10 94.45(19) 3_545 4_445 ? O10 Mn1 O1 95.50(13) 3_545 . ? O10 Mn1 O1 161.69(11) 4_445 . ? O10 Mn1 O1 161.69(11) 3_545 2 ? O10 Mn1 O1 95.50(13) 4_445 2 ? O1 Mn1 O1 79.38(16) . 2 ? O10 Mn1 O16 87.92(10) 3_545 2 ? O10 Mn1 O16 82.74(10) 4_445 2 ? O1 Mn1 O16 112.94(9) . 2 ? O1 Mn1 O16 78.16(9) 2 2 ? O10 Mn1 O16 82.74(10) 3_545 . ? O10 Mn1 O16 87.92(10) 4_445 . ? O1 Mn1 O16 78.16(9) . . ? O1 Mn1 O16 112.94(9) 2 . ? O16 Mn1 O16 166.23(12) 2 . ? O8 Mn2 O2 86.41(9) 7_576 . ? O8 Mn2 O9 98.34(12) 7_576 3_545 ? O2 Mn2 O9 87.57(14) . 3_545 ? O8 Mn2 O16 139.93(9) 7_576 . ? O2 Mn2 O16 87.43(10) . . ? O9 Mn2 O16 120.90(11) 3_545 . ? O8 Mn2 N8 86.75(9) 7_576 1_545 ? O2 Mn2 N8 172.89(10) . 1_545 ? O9 Mn2 N8 91.50(13) 3_545 1_545 ? O16 Mn2 N8 99.08(10) . 1_545 ? O7 Mn3 O7 180.00(13) 3_445 7_576 ? O7 Mn3 N7 95.35(10) 3_445 . ? O7 Mn3 N7 84.65(10) 7_576 . ? O7 Mn3 N7 84.65(10) 3_445 5_576 ? O7 Mn3 N7 95.35(10) 7_576 5_576 ? N7 Mn3 N7 180.00(15) . 5_576 ? O7 Mn3 O15 86.10(9) 3_445 . ? O7 Mn3 O15 93.90(9) 7_576 . ? N7 Mn3 O15 93.60(10) . . ? N7 Mn3 O15 86.40(10) 5_576 . ? O7 Mn3 O15 93.90(9) 3_445 5_576 ? O7 Mn3 O15 86.10(9) 7_576 5_576 ? N7 Mn3 O15 86.40(10) . 5_576 ? N7 Mn3 O15 93.60(10) 5_576 5_576 ? O15 Mn3 O15 180.0 . 5_576 ? C6 C1 C2 117.6(3) . . ? C6 C1 C13 120.5(3) . . ? C2 C1 C13 121.8(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 123.6(3) . . ? C2 C3 N3 116.4(3) . . ? C4 C3 N3 119.8(3) . . ? N1 C4 C3 123.5(3) . . ? N1 C4 C5 122.7(4) . . ? C3 C4 C5 113.7(3) . . ? C6 C5 C4 123.1(3) . . ? C6 C5 N2 115.3(4) . . ? C4 C5 N2 121.3(3) . . ? C5 C6 C1 121.2(3) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C12 C7 C8 117.7(3) . . ? C12 C7 C14 121.6(3) . . ? C8 C7 C14 120.6(3) . . ? C9 C8 C7 121.9(4) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 118.5(4) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 N1 121.4(3) . . ? C9 C10 N1 118.2(4) . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 121.2(3) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? O2 C13 O1 126.9(3) . . ? O2 C13 C1 117.2(3) . . ? O1 C13 C1 115.9(3) . . ? O7 C14 O8 124.9(3) . . ? O7 C14 C7 118.2(3) . . ? O8 C14 C7 117.0(3) . . ? C20 C15 C16 118.4(4) . . ? C20 C15 C27 121.0(4) . . ? C16 C15 C27 120.5(4) . . ? C17 C16 C15 120.0(5) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 123.7(4) . . ? C16 C17 N5 116.2(5) . . ? C18 C17 N5 119.8(4) . . ? N4 C18 C17 124.1(4) . . ? N4 C18 C19 122.2(5) . . ? C17 C18 C19 113.6(4) . . ? C20 C19 C18 122.9(5) . . ? C20 C19 N6 116.3(4) . . ? C18 C19 N6 120.7(4) . . ? C19 C20 C15 120.8(4) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? C22 C21 C26 118.0(3) . . ? C22 C21 C28 120.3(3) . . ? C26 C21 C28 121.7(3) . . ? C21 C22 C23 121.3(4) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 120.6(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.0(4) . . ? C23 C24 N4 118.9(4) . . ? C25 C24 N4 122.0(4) . . ? C24 C25 C26 120.2(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 120.7(4) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? O9 C27 O10 123.4(3) . . ? O9 C27 C15 118.4(4) . . ? O10 C27 C15 118.1(4) . . ? O15 C28 O16 120.7(3) . . ? O15 C28 C21 121.0(3) . . ? O16 C28 C21 118.3(3) . . ? N7 C29 C30 123.4(3) . . ? N7 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C29 C30 C31 119.3(3) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 116.7(3) . . ? C32 C31 C34 120.9(3) . . ? C30 C31 C34 122.4(3) . . ? C33 C32 C31 120.1(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? N7 C33 C32 123.3(3) . . ? N7 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? C38 C34 C35 116.9(3) . . ? C38 C34 C31 120.7(3) . . ? C35 C34 C31 122.4(3) . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? N8 C36 C35 122.9(3) . . ? N8 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? N8 C37 C38 122.9(3) . . ? N8 C37 H37 118.5 . . ? C38 C37 H37 118.5 . . ? C34 C38 C37 119.9(3) . . ? C34 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C4 N1 C10 122.2(3) . . ? C4 N1 H1A 118.9 . . ? C10 N1 H1A 118.8 . . ? O6 N2 O5 123.1(4) . . ? O6 N2 C5 119.3(5) . . ? O5 N2 C5 117.5(4) . . ? O3 N3 O4 122.8(4) . . ? O3 N3 C3 116.9(4) . . ? O4 N3 C3 120.3(4) . . ? C18 N4 C24 125.1(3) . . ? C18 N4 H4A 117.4 . . ? C24 N4 H4A 117.6 . . ? O11 N5 O12 124.8(6) . . ? O11 N5 C17 117.5(5) . . ? O12 N5 C17 117.6(5) . . ? O13 N6 O14 117.7(6) . . ? O13 N6 C19 121.4(5) . . ? O14 N6 C19 117.4(8) . . ? C29 N7 C33 117.3(3) . . ? C29 N7 Mn3 126.3(2) . . ? C33 N7 Mn3 116.4(2) . . ? C36 N8 C37 117.3(3) . . ? C36 N8 Mn2 123.8(2) . 1_565 ? C37 N8 Mn2 118.8(2) . 1_565 ? C13 O1 Mn1 141.8(2) . . ? C13 O2 Mn2 128.0(2) . . ? C14 O7 Mn3 132.8(2) . 3 ? C14 O8 Mn2 127.7(2) . 7_576 ? C27 O9 Mn2 108.3(3) . 3_455 ? C27 O10 Mn1 142.3(3) . 3_455 ? C28 O15 Mn3 154.1(2) . . ? C28 O16 Mn2 101.03(18) . . ? C28 O16 Mn1 140.9(2) . . ? Mn2 O16 Mn1 103.36(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.743 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.088