data_global # 1. SUBMISSION DETAILS _publ_contact_letter ; ; _publ_contact_author_name 'Jean-Pierre Tuchagues' _publ_contact_author_address ; Laboratoire de Chimie de Coordination du CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse Cedex 04, France ; _publ_contact_author_phone '?' _publ_contact_author_fax '?' _publ_contact_author_email 'jptuchagues@yahoo.fr' _publ_requested_journal '?' _publ_requested_category CO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name '?' _publ_section_title # Title of paper ; Supramolecular Structures of Dinuclear Manganese(III) Complexes with Penta-anionic Pentadentate Ligands Including Alkoxo, Amido and Phenoxo Donors ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Liliana Stoicescu' # Author 1 ; University of Bucharest, Faculty of Chemistry, Inorganic Chemistry Department, 23 Dumbrava Ro\,sie, 020464 Bucharest, Romania ; ; ? # Footnote for author 1 ; 'Aur\'elie Jeanson' # Author 2 ; Laboratoire de Chimie de Coordination du CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse Cedex 04, France ; ; ? # Footnote 2 ; 'Carine Duhayon' # Author 2 ; Laboratoire de Chimie de Coordination du CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse Cedex 04, France ; ; ? # Footnote 2 ; 'Ana Tesouro-Vallina' # Author 2 ; Laboratoire de Chimie de Coordination du CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse Cedex 04, France ; ; ? # Footnote 2 ; 'Athanassios K. Boudalis' # Author 2 ; Institute of Materials Science, NCSR ?Demokritos?153 10 Aghia Paraskevi Attikis, Greece ; ; ? # Footnote 2 ; 'Jean-Pierre Costes' # Author 2 ; Laboratoire de Chimie de Coordination du CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse Cedex 04, France ; ; ? # Footnote 2 ; 'Jean-Pierre Tuchagues' # Author 2 ; Laboratoire de Chimie de Coordination du CNRS, UPR 8241, 205 route de Narbonne, 31077 Toulouse Cedex 04, France ; ; ? # Footnote 2 ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Gottingen, Germany. MULTI SCAN - c.f. r.h. blessing, acta cryst. (1995), a51, 33-38 WINGX - 1.63 Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-Ray Diffraction Data. Farrugia, L. J. Appl. Crystallogr., 1999, 32, 837. ORTEP3 for Windows, Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565.; ; #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# # data_[Mn2(L2)(pz)(MeOH)4]_complex_2 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H34 Mn2 N4 O9' _chemical_formula_sum 'C25 H34 Mn2 N4 O9' _chemical_formula_weight 644.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4560(5) _cell_length_b 11.0112(5) _cell_length_c 13.8831(6) _cell_angle_alpha 90.821(4) _cell_angle_beta 92.597(4) _cell_angle_gamma 93.403(4) _cell_volume 1441.29(12) _cell_formula_units_Z 2 _cell_measurement_temperature 180 _cell_measurement_reflns_used 5046 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.91 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_unetI/netI 0.0474 _diffrn_reflns_number 12707 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 28.06 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 6965 _reflns_number_gt 5151 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0566P)^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_number_reflns 6965 _refine_ls_number_parameters 381 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.103 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.525 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_number_in_cell C 50 H 68 Mn 4 N 8 O 18 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 0.6880(3) 0.2667(3) 0.07647(18) 0.0340(6) Uani 1 1 d . . . C2 C 0.7645(3) 0.3587(3) 0.0294(2) 0.0484(8) Uani 1 1 d . . . H2 H 0.7545 0.4396 0.0463 0.058 Uiso 1 1 calc R . . C3 C 0.8550(3) 0.3307(4) -0.0421(2) 0.0610(10) Uani 1 1 d . . . H3 H 0.9052 0.3927 -0.0732 0.073 Uiso 1 1 calc R . . C4 C 0.8706(4) 0.2115(4) -0.0672(2) 0.0663(11) Uani 1 1 d . . . H4 H 0.9311 0.1927 -0.1155 0.08 Uiso 1 1 calc R . . C5 C 0.7970(3) 0.1196(3) -0.0210(2) 0.0468(8) Uani 1 1 d . . . H5 H 0.8099 0.0391 -0.0379 0.056 Uiso 1 1 calc R . . C6 C 0.7030(2) 0.1447(3) 0.05093(17) 0.0326(6) Uani 1 1 d . . . C7 C 0.6310(2) 0.0380(2) 0.09728(16) 0.0285(5) Uani 1 1 d . . . C8 C 0.4782(3) -0.0484(3) 0.2140(2) 0.0416(7) Uani 1 1 d . . . H8A H 0.5476 -0.1078 0.2282 0.05 Uiso 1 1 calc R A 1 H8B H 0.4073 -0.0852 0.1681 0.05 Uiso 1 1 calc R A 1 C9A C 0.4071(7) -0.0137(6) 0.3072(4) 0.0325(8) Uani 0.5 1 d P B 1 H9A H 0.4924 0.0016 0.3495 0.039 Uiso 0.5 1 calc PR B 1 C10A C 0.3390(6) -0.0980(5) 0.3594(4) 0.0325(8) Uani 0.5 1 d P B 1 H10A H 0.4135 -0.1355 0.3965 0.039 Uiso 0.5 1 calc PR B 1 H10B H 0.3017 -0.1593 0.3126 0.039 Uiso 0.5 1 calc PR B 1 C9B C 0.3606(7) -0.0189(6) 0.2751(5) 0.0325(8) Uani 0.5 1 d P B 2 H9B H 0.29 -0.0151 0.2215 0.039 Uiso 0.5 1 calc PR B 2 C10B C 0.2796(6) -0.0938(5) 0.3286(4) 0.0325(8) Uani 0.5 1 d P B 2 H10C H 0.3276 -0.1692 0.3279 0.039 Uiso 0.5 1 calc PR B 2 H10D H 0.1937 -0.1096 0.2885 0.039 Uiso 0.5 1 calc PR B 2 C11 C 0.2296(4) -0.0869(3) 0.4241(3) 0.0594(10) Uani 1 1 d . . . H11A H 0.2464 -0.1415 0.4771 0.071 Uiso 1 1 calc R B 1 H11B H 0.1411 -0.1156 0.391 0.071 Uiso 1 1 calc R B 1 C12 C 0.1879(2) 0.0371(2) 0.55939(17) 0.0257(5) Uani 1 1 d . . . C13 C 0.1628(2) 0.1542(2) 0.60832(16) 0.0272(5) Uani 1 1 d . B . C14 C 0.1779(3) 0.1618(3) 0.70932(18) 0.0371(6) Uani 1 1 d . . . H14 H 0.2063 0.0946 0.7433 0.044 Uiso 1 1 calc R B . C15 C 0.1517(3) 0.2668(3) 0.7593(2) 0.0486(8) Uani 1 1 d . B . H15 H 0.1659 0.2709 0.826 0.058 Uiso 1 1 calc R . . C16 C 0.1044(3) 0.3654(3) 0.7103(2) 0.0499(8) Uani 1 1 d . . . H16 H 0.0836 0.4352 0.7441 0.06 Uiso 1 1 calc R B . C17 C 0.0879(3) 0.3606(3) 0.6110(2) 0.0396(6) Uani 1 1 d . B . H17 H 0.0547 0.4272 0.5784 0.048 Uiso 1 1 calc R . . C18 C 0.1202(2) 0.2579(2) 0.55882(17) 0.0282(5) Uani 1 1 d . . . C19 C 0.2067(3) 0.4440(2) 0.32132(19) 0.0352(6) Uani 1 1 d . . . H19 H 0.1252 0.457 0.3542 0.042 Uiso 1 1 calc R . . C20 C 0.2809(3) 0.5306(2) 0.2714(2) 0.0417(7) Uani 1 1 d . . . H20 H 0.2603 0.6114 0.2632 0.05 Uiso 1 1 calc R . . C21 C 0.3924(3) 0.4725(2) 0.23585(19) 0.0363(6) Uani 1 1 d . . . H21 H 0.4624 0.5087 0.1989 0.044 Uiso 1 1 calc R . . C23 C 0.7420(3) 0.3379(3) 0.3584(2) 0.0461(7) Uani 1 1 d . B . H23A H 0.805 0.3343 0.3063 0.069 Uiso 1 1 calc R . . H23B H 0.7959 0.339 0.4187 0.069 Uiso 1 1 calc R . . H23C H 0.6907 0.4104 0.3536 0.069 Uiso 1 1 calc R . . C22 C 0.2628(4) 0.3009(3) 0.0435(2) 0.0655(11) Uani 1 1 d . B . H22A H 0.2204 0.3496 0.0909 0.098 Uiso 1 1 calc R . . H22B H 0.1923 0.2746 -0.0056 0.098 Uiso 1 1 calc R . . H22C H 0.3379 0.3482 0.0149 0.098 Uiso 1 1 calc R . . C25 C 0.4553(3) 0.3420(3) 0.5419(2) 0.0546(9) Uani 1 1 d . B . H25C H 0.4113 0.409 0.5117 0.082 Uiso 1 1 calc R . . H25A H 0.5554 0.3614 0.5514 0.082 Uiso 1 1 calc R . . H25B H 0.4148 0.3268 0.603 0.082 Uiso 1 1 calc R . . C24 C 0.0105(3) 0.1258(3) 0.19480(19) 0.0519(8) Uani 1 1 d . B . H24C H -0.0373 0.1993 0.1842 0.078 Uiso 1 1 calc R . . H24B H -0.0504 0.0571 0.173 0.078 Uiso 1 1 calc R . . H24A H 0.0958 0.1283 0.1597 0.078 Uiso 1 1 calc R . . N1 N 0.5479(2) 0.05826(19) 0.17135(14) 0.0263(4) Uani 1 1 d . B . N2 N 0.2098(2) 0.03376(18) 0.46536(14) 0.0273(4) Uani 1 1 d . B . N3 N 0.3852(2) 0.35519(18) 0.26256(14) 0.0259(4) Uani 1 1 d . . . N4 N 0.2681(2) 0.33793(18) 0.31603(14) 0.0256(4) Uani 1 1 d . . . O1 O 0.60419(19) 0.30305(16) 0.14592(14) 0.0403(5) Uani 1 1 d . . . O2 O 0.6516(2) -0.06732(18) 0.06902(13) 0.0428(5) Uani 1 1 d . . . O3 O 0.36271(15) 0.11073(13) 0.30027(11) 0.0203(3) Uani 1 1 d . . . O4 O 0.18799(17) -0.05728(16) 0.61158(12) 0.0342(4) Uani 1 1 d . B . O5 O 0.10808(17) 0.26029(17) 0.46246(11) 0.0324(4) Uani 1 1 d . B . O7 O 0.64383(17) 0.23326(16) 0.35334(13) 0.0299(4) Uani 1 1 d D . . O6 O 0.3184(2) 0.19765(18) 0.08819(13) 0.0365(4) Uani 1 1 d D . . O9 O 0.43237(18) 0.23667(17) 0.48188(12) 0.0309(4) Uani 1 1 d D . . O8 O 0.04515(18) 0.11516(19) 0.29420(12) 0.0346(4) Uani 1 1 d D . . Mn1 Mn 0.47932(4) 0.20867(3) 0.21508(2) 0.02541(11) Uani 1 1 d . B . Mn2 Mn 0.22946(3) 0.17987(3) 0.38598(2) 0.02240(10) Uani 1 1 d . B . H60 H 0.327(3) 0.143(2) 0.0488(18) 0.052(10) Uiso 1 1 d D . . H80 H -0.022(3) 0.114(3) 0.330(2) 0.075(12) Uiso 1 1 d D . . H70 H 0.686(3) 0.1738(18) 0.369(2) 0.045(9) Uiso 1 1 d D . . H90 H 0.501(2) 0.228(3) 0.4488(19) 0.053(10) Uiso 1 1 d 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 0.0263(12) 0.0483(16) 0.0279(13) 0.0130(12) 0.0032(10) 0.0031(11) C2 0.0446(17) 0.0567(19) 0.0449(17) 0.0202(15) 0.0108(13) 0.0009(14) C3 0.0497(19) 0.084(3) 0.0492(19) 0.0185(19) 0.0212(16) -0.0135(18) C4 0.052(2) 0.102(3) 0.0458(19) -0.003(2) 0.0303(16) -0.014(2) C5 0.0370(15) 0.072(2) 0.0313(15) -0.0064(15) 0.0139(12) -0.0023(15) C6 0.0228(12) 0.0552(17) 0.0199(12) 0.0054(11) 0.0012(9) 0.0025(11) C7 0.0219(11) 0.0436(15) 0.0208(11) 0.0030(11) -0.0003(9) 0.0105(11) C8 0.0482(16) 0.0356(15) 0.0425(16) 0.0065(13) 0.0161(13) 0.0042(13) C9A 0.042(3) 0.0256(11) 0.031(3) 0.0013(17) 0.0049(15) 0.0090(19) C10A 0.042(3) 0.0256(11) 0.031(3) 0.0013(17) 0.0049(15) 0.0090(19) C9B 0.042(3) 0.0256(11) 0.031(3) 0.0013(17) 0.0049(15) 0.0090(19) C10B 0.042(3) 0.0256(11) 0.031(3) 0.0013(17) 0.0049(15) 0.0090(19) C11 0.086(2) 0.0346(17) 0.062(2) 0.0009(15) 0.0443(19) 0.0052(16) C12 0.0144(10) 0.0379(14) 0.0255(12) 0.0096(10) 0.0028(9) 0.0031(9) C13 0.0189(11) 0.0409(14) 0.0220(11) 0.0031(10) 0.0049(9) -0.0015(10) C14 0.0328(14) 0.0535(18) 0.0238(13) 0.0057(12) 0.0018(10) -0.0083(12) C15 0.0507(18) 0.071(2) 0.0227(13) -0.0085(14) 0.0094(12) -0.0133(16) C16 0.0550(18) 0.056(2) 0.0388(16) -0.0137(15) 0.0206(14) -0.0059(16) C17 0.0409(15) 0.0418(16) 0.0376(15) -0.0006(13) 0.0142(12) 0.0070(12) C18 0.0213(11) 0.0387(14) 0.0255(12) 0.0008(11) 0.0086(9) 0.0037(10) C19 0.0403(14) 0.0307(14) 0.0362(14) -0.0012(11) -0.0003(12) 0.0166(12) C20 0.0574(18) 0.0242(13) 0.0440(16) -0.0002(12) -0.0069(14) 0.0130(13) C21 0.0452(15) 0.0259(13) 0.0372(15) 0.0061(11) -0.0013(12) -0.0012(11) C23 0.0363(15) 0.0369(16) 0.064(2) -0.0005(14) -0.0012(14) -0.0065(12) C22 0.100(3) 0.059(2) 0.0390(17) -0.0022(16) -0.0203(18) 0.041(2) C25 0.0452(17) 0.060(2) 0.057(2) -0.0235(17) 0.0098(15) -0.0127(15) C24 0.0407(16) 0.089(3) 0.0249(14) 0.0089(15) -0.0026(12) -0.0052(16) N1 0.0260(10) 0.0324(11) 0.0216(10) 0.0026(8) 0.0058(8) 0.0064(8) N2 0.0287(10) 0.0314(11) 0.0226(10) 0.0011(9) 0.0057(8) 0.0051(9) N3 0.0297(10) 0.0233(10) 0.0254(10) 0.0053(8) 0.0022(8) 0.0043(8) N4 0.0266(10) 0.0270(11) 0.0242(10) 0.0001(8) 0.0030(8) 0.0090(8) O1 0.0410(10) 0.0351(10) 0.0475(11) 0.0116(9) 0.0226(9) 0.0073(8) O2 0.0515(12) 0.0486(12) 0.0310(10) -0.0047(9) 0.0132(9) 0.0179(10) O3 0.0228(8) 0.0168(7) 0.0220(8) 0.0004(6) 0.0029(6) 0.0042(6) O4 0.0292(9) 0.0424(11) 0.0336(9) 0.0167(8) 0.0118(7) 0.0130(8) O5 0.0336(9) 0.0445(11) 0.0219(8) 0.0062(8) 0.0072(7) 0.0194(8) O7 0.0238(8) 0.0257(9) 0.0407(10) 0.0026(8) 0.0026(7) 0.0041(7) O6 0.0455(11) 0.0414(11) 0.0242(9) -0.0023(8) -0.0019(8) 0.0186(9) O9 0.0265(9) 0.0388(10) 0.0271(9) -0.0050(8) 0.0006(7) 0.0025(8) O8 0.0219(9) 0.0607(13) 0.0210(9) 0.0073(8) 0.0009(7) 0.0000(8) Mn1 0.02549(19) 0.0283(2) 0.02382(19) 0.00463(15) 0.00812(14) 0.00707(15) Mn2 0.02158(18) 0.0288(2) 0.01779(18) 0.00324(14) 0.00370(13) 0.00663(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 1.347(3) . ? C1 C2 1.397(4) . ? C1 C6 1.402(4) . ? C2 C3 1.383(4) . ? C2 H2 0.93 . ? C3 C4 1.371(5) . ? C3 H3 0.93 . ? C4 C5 1.377(4) . ? C4 H4 0.93 . ? C5 C6 1.402(3) . ? C5 H5 0.93 . ? C6 C7 1.492(4) . ? C7 O2 1.248(3) . ? C7 N1 1.346(3) . ? C8 N1 1.458(3) . ? C8 C9B 1.477(7) . ? C8 C9A 1.540(7) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9A C10A 1.338(8) . ? C9A O3 1.460(7) . ? C9A H9A 0.98 . ? C10A C11 1.411(7) . ? C10A H10A 0.97 . ? C10A H10B 0.97 . ? C9B C10B 1.347(7) . ? C9B O3 1.464(7) . ? C9B H9B 0.98 . ? C10B C11 1.430(6) . ? C10B H10C 0.97 . ? C10B H10D 0.97 . ? C11 N2 1.465(3) . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 O4 1.276(3) . ? C12 N2 1.331(3) . ? C12 C13 1.486(3) . ? C13 C14 1.404(3) . ? C13 C18 1.410(3) . ? C14 C15 1.381(4) . ? C14 H14 0.93 . ? C15 C16 1.376(4) . ? C15 H15 0.93 . ? C16 C17 1.381(4) . ? C16 H16 0.93 . ? C17 C18 1.391(4) . ? C17 H17 0.93 . ? C18 O5 1.338(3) . ? C19 N4 1.338(3) . ? C19 C20 1.365(4) . ? C19 H19 0.93 . ? C20 C21 1.372(4) . ? C20 H20 0.93 . ? C21 N3 1.348(3) . ? C21 H21 0.93 . ? C23 O7 1.435(3) . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C22 O6 1.420(3) . ? C22 H22A 0.96 . ? C22 H22B 0.96 . ? C22 H22C 0.96 . ? C25 O9 1.418(3) . ? C25 H25C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C24 O8 1.412(3) . ? C24 H24C 0.96 . ? C24 H24B 0.96 . ? C24 H24A 0.96 . ? N1 Mn1 1.915(2) . ? N2 Mn2 1.968(2) . ? N3 N4 1.366(3) . ? N3 Mn1 2.006(2) . ? N4 Mn2 2.028(2) . ? O1 Mn1 1.8390(17) . ? O3 Mn1 1.9472(15) . ? O3 Mn2 1.9511(15) . ? O5 Mn2 1.8530(16) . ? O7 Mn1 2.4171(18) . ? O7 H70 0.811(10) . ? O6 Mn1 2.2719(18) . ? O6 H60 0.821(10) . ? O9 Mn2 2.3339(17) . ? O9 H90 0.819(10) . ? O8 Mn2 2.1895(17) . ? O8 H80 0.821(20) . ? 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 O1 C1 C2 116.3(3) . . ? O1 C1 C6 124.0(2) . . ? C2 C1 C6 119.7(3) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 118.1(3) . . ? C1 C6 C7 125.1(2) . . ? C5 C6 C7 116.8(3) . . ? O2 C7 N1 121.5(2) . . ? O2 C7 C6 120.0(2) . . ? N1 C7 C6 118.5(2) . . ? N1 C8 C9B 113.4(3) . . ? N1 C8 C9A 111.0(3) . . ? N1 C8 H8A 109.4 . . ? C9B C8 H8A 125.8 . . ? C9A C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C9B C8 H8B 87.5 . . ? C9A C8 H8B 109.4 . . ? H8A C8 H8B 108 . . ? C10A C9A O3 122.4(5) . . ? C10A C9A C8 121.2(5) . . ? O3 C9A C8 109.3(4) . . ? C10A C9A H9A 98.9 . . ? O3 C9A H9A 98.9 . . ? C8 C9A H9A 98.9 . . ? C9A C10A C11 130.4(5) . . ? C9A C10A H10A 104.7 . . ? C11 C10A H10A 104.7 . . ? C9A C10A H10B 104.7 . . ? C11 C10A H10B 104.7 . . ? H10A C10A H10B 105.7 . . ? C10B C9B O3 116.0(5) . . ? C10B C9B C8 128.9(5) . . ? O3 C9B C8 112.6(5) . . ? C10B C9B H9B 95.2 . . ? O3 C9B H9B 95.2 . . ? C8 C9B H9B 95.2 . . ? C9B C10B C11 134.2(5) . . ? C9B C10B H10C 103.6 . . ? C11 C10B H10C 103.6 . . ? C9B C10B H10D 103.6 . . ? C11 C10B H10D 103.6 . . ? H10C C10B H10D 105.3 . . ? C10A C11 N2 118.0(3) . . ? C10B C11 N2 118.0(3) . . ? C10A C11 H11A 107.8 . . ? C10B C11 H11A 127.9 . . ? N2 C11 H11A 107.8 . . ? C10A C11 H11B 107.8 . . ? C10B C11 H11B 81.9 . . ? N2 C11 H11B 107.8 . . ? H11A C11 H11B 107.1 . . ? O4 C12 N2 122.8(2) . . ? O4 C12 C13 116.9(2) . . ? N2 C12 C13 120.2(2) . . ? C14 C13 C18 117.9(2) . . ? C14 C13 C12 118.6(2) . . ? C18 C13 C12 123.4(2) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C15 C16 C17 119.9(3) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C18 121.1(3) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? O5 C18 C17 118.5(2) . . ? O5 C18 C13 122.0(2) . . ? C17 C18 C13 119.6(2) . . ? N4 C19 C20 110.1(2) . . ? N4 C19 H19 124.9 . . ? C20 C19 H19 124.9 . . ? C19 C20 C21 105.1(2) . . ? C19 C20 H20 127.4 . . ? C21 C20 H20 127.4 . . ? N3 C21 C20 109.7(2) . . ? N3 C21 H21 125.1 . . ? C20 C21 H21 125.1 . . ? O7 C23 H23A 109.5 . . ? O7 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O7 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C22 H22A 109.5 . . ? O6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O9 C25 H25C 109.5 . . ? O9 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? O9 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O8 C24 H24C 109.5 . . ? O8 C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? O8 C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? C7 N1 C8 116.8(2) . . ? C7 N1 Mn1 128.81(18) . . ? C8 N1 Mn1 113.36(15) . . ? C12 N2 C11 115.6(2) . . ? C12 N2 Mn2 123.58(17) . . ? C11 N2 Mn2 120.63(17) . . ? C21 N3 N4 107.3(2) . . ? C21 N3 Mn1 132.33(18) . . ? N4 N3 Mn1 118.60(15) . . ? C19 N4 N3 107.7(2) . . ? C19 N4 Mn2 130.78(17) . . ? N3 N4 Mn2 120.86(14) . . ? C1 O1 Mn1 127.87(17) . . ? C9A O3 Mn1 112.2(3) . . ? C9B O3 Mn1 111.7(3) . . ? C9A O3 Mn2 123.5(3) . . ? C9B O3 Mn2 123.5(3) . . ? Mn1 O3 Mn2 123.15(8) . . ? C18 O5 Mn2 121.75(14) . . ? C23 O7 Mn1 118.44(16) . . ? C23 O7 H70 109(2) . . ? Mn1 O7 H70 116(2) . . ? C22 O6 Mn1 123.88(18) . . ? C22 O6 H60 111(2) . . ? Mn1 O6 H60 116(2) . . ? C25 O9 Mn2 127.08(17) . . ? C25 O9 H90 111(2) . . ? Mn2 O9 H90 107(2) . . ? C24 O8 Mn2 132.88(17) . . ? C24 O8 H80 116(3) . . ? Mn2 O8 H80 105(3) . . ? O1 Mn1 N1 94.06(8) . . ? O1 Mn1 O3 173.61(8) . . ? N1 Mn1 O3 86.31(7) . . ? O1 Mn1 N3 91.98(8) . . ? N1 Mn1 N3 173.16(8) . . ? O3 Mn1 N3 88.04(7) . . ? O1 Mn1 O6 91.05(8) . . ? N1 Mn1 O6 88.61(8) . . ? O3 Mn1 O6 95.34(7) . . ? N3 Mn1 O6 88.08(7) . . ? O1 Mn1 O7 88.71(8) . . ? N1 Mn1 O7 95.30(7) . . ? O3 Mn1 O7 84.90(6) . . ? N3 Mn1 O7 88.03(7) . . ? O6 Mn1 O7 176.09(6) . . ? O5 Mn2 O3 174.37(7) . . ? O5 Mn2 N2 91.01(8) . . ? O3 Mn2 N2 94.45(7) . . ? O5 Mn2 N4 88.36(8) . . ? O3 Mn2 N4 86.06(7) . . ? N2 Mn2 N4 173.10(8) . . ? O5 Mn2 O8 88.53(7) . . ? O3 Mn2 O8 92.82(7) . . ? N2 Mn2 O8 90.66(8) . . ? N4 Mn2 O8 96.19(7) . . ? O5 Mn2 O9 94.54(7) . . ? O3 Mn2 O9 84.33(6) . . ? N2 Mn2 O9 87.13(7) . . ? N4 Mn2 O9 86.08(7) . . ? O8 Mn2 O9 176.25(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H60 O2 0.821(10) 1.848(15) 2.630(3) 159(3) 2_655 O8 H80 O4 0.821(10) 1.878(16) 2.664(2) 160(4) 2_556 O7 H70 O4 0.811(10) 1.819(12) 2.616(2) 167(3) 2_656 O9 H90 O7 0.819(10) 1.936(12) 2.741(2) 168(3) .