Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 2007-06-13 _audit_creation_method 'by CrystalStructure 3.8' _audit_update_record ? _publ_contact_author_name 'Yuji Mikata' _publ_contact_author_address ; KYOUSEI Science Center Nara Women's University Nara 630-8506 JAPAN ; _publ_contact_author_email MIKATA@CC.NARA-WU.AC.JP _publ_section_title ; Quinoline-based tetradendate nitrogen ligands stabilize the bis(u-oxo) dinuclear manganese(III,III) core ; _publ_section_references ; Rigaku/MSC and Rigaku Corporation. (2006). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Sheldrick, G.M. (1997). SHELXL97. University of Gottingen, Germany. ; loop_ _publ_author_name 'Yuji Mikata' 'Koichi Fukui' 'Akio Ichimura' 'Ayano Kawamura' 'Masahiro Mikuriya' 'Haruko So' ; A.Yamashita ; 'Shigenobu Yano' # Attachment 'B705080A-cif-bqdpen.txt' #============================================================================== data___i-Pr2enQ2-55-1 _database_code_depnum_ccdc_archive 'CCDC 297397' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H34 N4 ' _chemical_formula_moiety 'C28 H34 N4 ' _chemical_formula_weight 426.60 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _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_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.2432(2) _cell_length_b 8.8278(2) _cell_length_c 9.6628(2) _cell_angle_alpha 81.368(6) _cell_angle_beta 84.698(6) _cell_angle_gamma 74.897(6) _cell_volume 588.84(2) _cell_formula_units_Z 1 _cell_measurement_reflns_used 1435 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.7 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 230.00 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.994 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 6342 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 28.69 _diffrn_measured_fraction_theta_max 0.9762 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.9762 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2952 _reflns_number_gt 2257 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1110 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2952 _refine_ls_number_parameters 214 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0624P)^2^+0.0154P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.31 _refine_diff_density_min -0.16 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 N(1) N 0.33998(10) 0.70402(8) 0.95849(8) 0.0232(2) Uani 1.00 1 d . . . N(2) N 0.38827(11) 1.06241(9) 0.75310(8) 0.0249(2) Uani 1.00 1 d . . . C(1) C 0.4460(1) 0.56319(10) 1.04488(10) 0.0265(2) Uani 1.00 1 d . . . C(2) C 0.46121(13) 0.80946(10) 0.89923(10) 0.0254(2) Uani 1.00 1 d . . . C(3) C 0.38281(12) 0.91252(10) 0.76813(9) 0.0230(2) Uani 1.00 1 d . . . C(4) C 0.3118(1) 0.84560(11) 0.66597(10) 0.0269(2) Uani 1.00 1 d . . . C(5) C 0.2468(1) 0.93763(12) 0.54590(10) 0.0284(2) Uani 1.00 1 d . . . C(6) C 0.1797(1) 1.20492(13) 0.40497(11) 0.0322(2) Uani 1.00 1 d . . . C(7) C 0.1843(2) 1.36002(13) 0.39221(12) 0.0377(3) Uani 1.00 1 d . . . C(8) C 0.2598(2) 1.41631(13) 0.49777(12) 0.0390(3) Uani 1.00 1 d . . . C(9) C 0.3267(2) 1.31750(12) 0.61490(12) 0.0343(3) Uani 1.00 1 d . . . C(10) C 0.32174(13) 1.15657(10) 0.63223(10) 0.0251(2) Uani 1.00 1 d . . . C(11) C 0.24828(13) 1.09942(11) 0.52547(10) 0.0257(2) Uani 1.00 1 d . . . C(12) C 0.1802(2) 0.82548(12) 1.17442(11) 0.0315(2) Uani 1.00 1 d . . . C(13) C 0.16076(13) 0.79132(10) 1.02664(9) 0.0244(2) Uani 1.00 1 d . . . C(14) C 0.0013(2) 0.70955(13) 1.02350(12) 0.0345(3) Uani 1.00 1 d . . . H(1) H 0.541(2) 0.5884(12) 1.1038(11) 0.030(3) Uiso 1.00 1 . . . . H(2) H 0.352(2) 0.5177(13) 1.1123(12) 0.034(3) Uiso 1.00 1 . . . . H(3) H 0.592(2) 0.7414(12) 0.8722(11) 0.029(3) Uiso 1.00 1 . . . . H(4) H 0.483(2) 0.8794(13) 0.9673(12) 0.034(3) Uiso 1.00 1 . . . . H(5) H 0.313(2) 0.7339(13) 0.6856(11) 0.032(3) Uiso 1.00 1 . . . . H(6) H 0.196(2) 0.8917(13) 0.4740(12) 0.038(3) Uiso 1.00 1 . . . . H(7) H 0.128(2) 1.163(1) 0.3309(13) 0.046(3) Uiso 1.00 1 . . . . H(8) H 0.133(2) 1.434(1) 0.3077(13) 0.042(3) Uiso 1.00 1 . . . . H(9) H 0.263(2) 1.528(2) 0.486(1) 0.054(4) Uiso 1.00 1 . . . . H(10) H 0.379(2) 1.356(1) 0.6890(13) 0.045(3) Uiso 1.00 1 . . . . H(11) H 0.199(2) 0.723(2) 1.2438(13) 0.045(3) Uiso 1.00 1 . . . . H(12) H 0.285(2) 0.8763(13) 1.1757(12) 0.040(3) Uiso 1.00 1 . . . . H(13) H 0.061(2) 0.898(2) 1.2080(13) 0.050(4) Uiso 1.00 1 . . . . H(14) H 0.127(1) 0.8954(12) 0.9648(11) 0.024(3) Uiso 1.00 1 . . . . H(15) H 0.030(2) 0.604(2) 1.081(1) 0.049(4) Uiso 1.00 1 . . . . H(16) H -0.012(2) 0.696(1) 0.9248(13) 0.044(3) Uiso 1.00 1 . . . . H(17) H -0.122(2) 0.775(2) 1.0600(13) 0.050(4) Uiso 1.00 1 . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N(1) 0.0249(4) 0.0179(4) 0.0226(4) -0.0001(3) -0.0002(3) 0.0006(3) N(2) 0.0264(4) 0.0233(4) 0.0239(4) -0.0050(3) -0.0013(3) -0.0013(3) C(1) 0.0336(5) 0.0188(4) 0.0218(5) 0.0021(4) -0.0030(4) -0.0007(4) C(2) 0.0254(5) 0.0231(4) 0.0259(5) -0.0039(4) -0.0032(4) -0.0007(4) C(3) 0.0202(4) 0.0240(4) 0.0230(5) -0.0036(3) 0.0011(3) -0.0020(4) C(4) 0.0297(5) 0.0250(5) 0.0270(5) -0.0090(4) -0.0005(4) -0.0034(4) C(5) 0.0280(5) 0.0347(5) 0.0241(5) -0.0106(4) -0.0015(4) -0.0039(4) C(6) 0.0284(5) 0.0417(6) 0.0235(5) -0.0074(4) -0.0018(4) 0.0027(4) C(7) 0.0350(6) 0.0391(6) 0.0295(6) -0.0008(5) 0.0004(4) 0.0093(5) C(8) 0.0478(6) 0.0257(5) 0.0372(6) -0.0040(4) 0.0023(5) 0.0039(4) C(9) 0.0421(6) 0.0268(5) 0.0324(6) -0.0070(4) -0.0017(5) -0.0018(4) C(10) 0.0238(4) 0.0255(4) 0.0233(5) -0.0037(4) 0.0015(4) -0.0007(4) C(11) 0.0207(4) 0.0313(5) 0.0228(5) -0.0051(4) 0.0014(4) 0.0001(4) C(12) 0.0320(5) 0.0313(5) 0.0297(6) -0.0029(4) 0.0004(4) -0.0101(4) C(13) 0.0243(4) 0.0200(4) 0.0256(5) -0.0004(3) -0.0009(4) -0.0015(4) C(14) 0.0308(5) 0.0377(6) 0.0365(6) -0.0102(4) -0.0019(4) -0.0067(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N(1) C(1) 1.463(1) ? . . N(1) C(2) 1.462(1) ? . . N(1) C(13) 1.478(1) ? . . N(2) C(3) 1.320(1) ? . . N(2) C(10) 1.375(1) ? . . C(2) C(3) 1.508(1) ? . . C(3) C(4) 1.420(1) ? . . C(4) C(5) 1.359(1) ? . . C(5) C(11) 1.415(1) ? . . C(6) C(7) 1.365(2) ? . . C(6) C(11) 1.418(1) ? . . C(7) C(8) 1.409(2) ? . . C(8) C(9) 1.364(1) ? . . C(9) C(10) 1.415(1) ? . . C(10) C(11) 1.414(2) ? . . C(12) C(13) 1.529(1) ? . . C(13) C(14) 1.518(2) ? . . C(1) H(1) 1.02(1) ? . . C(1) H(2) 1.02(1) ? . . C(2) H(3) 1.01(1) ? . . C(2) H(4) 1.01(1) ? . . C(4) H(5) 0.97(1) ? . . C(5) H(6) 0.99(1) ? . . C(6) H(7) 0.99(1) ? . . C(7) H(8) 1.00(1) ? . . C(8) H(9) 0.98(1) ? . . C(9) H(10) 0.98(1) ? . . C(12) H(11) 1.03(1) ? . . C(12) H(12) 0.98(1) ? . . C(12) H(13) 0.99(1) ? . . C(13) H(14) 1.004(9) ? . . C(14) H(15) 1.00(1) ? . . C(14) H(16) 0.99(1) ? . . C(14) H(17) 1.00(1) ? . . H(8) C(7) 1.00(1) ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(2) N(1) C(1) 112.20(7) ? . . . C(13) N(1) C(1) 114.88(7) ? . . . N(1) C(2) C(3) 111.73(8) ? . . . C(13) N(1) C(2) 111.44(7) ? . . . N(1) C(13) C(12) 114.82(8) ? . . . N(1) C(13) C(14) 110.72(8) ? . . . N(2) C(3) C(2) 117.23(9) ? . . . N(2) C(3) C(4) 123.05(8) ? . . . C(10) N(2) C(3) 117.75(9) ? . . . N(2) C(10) C(9) 118.3(1) ? . . . N(2) C(10) C(11) 122.79(8) ? . . . C(2) C(3) C(4) 119.69(8) ? . . . C(3) C(4) C(5) 119.56(9) ? . . . C(4) C(5) C(11) 119.5(1) ? . . . C(5) C(11) C(10) 117.36(8) ? . . . C(5) C(11) C(6) 123.4(1) ? . . . C(11) C(6) C(7) 120.4(1) ? . . . C(6) C(7) C(8) 120.3(1) ? . . . C(6) C(11) C(10) 119.27(9) ? . . . C(7) C(8) C(9) 120.6(1) ? . . . C(8) C(9) C(10) 120.5(1) ? . . . C(9) C(10) C(11) 118.92(9) ? . . . C(12) C(13) C(14) 111.46(8) ? . . . N(1) C(1) H(1) 112.2(5) ? . . . N(1) C(1) H(2) 108.9(6) ? . . . N(1) C(2) H(3) 107.9(7) ? . . . N(1) C(2) H(4) 113.8(6) ? . . . N(1) C(13) H(14) 103.8(6) ? . . . H(2) C(1) H(1) 107.2(9) ? . . . H(3) C(2) C(3) 107.4(6) ? . . . H(4) C(2) C(3) 108.9(6) ? . . . H(4) C(2) H(3) 106.8(9) ? . . . C(3) C(4) H(5) 117.6(7) ? . . . H(5) C(4) C(5) 122.8(7) ? . . . C(4) C(5) H(6) 120.0(6) ? . . . H(6) C(5) C(11) 120.5(6) ? . . . H(7) C(6) C(7) 121.2(7) ? . . . C(6) C(7) H(8) 119.7(8) ? . . . H(7) C(6) C(11) 118.4(7) ? . . . H(8) C(7) C(8) 120.1(8) ? . . . C(7) C(8) H(9) 118.8(8) ? . . . C(8) C(9) H(10) 121.0(7) ? . . . H(9) C(8) C(9) 120.6(8) ? . . . H(10) C(9) C(10) 118.5(7) ? . . . H(11) C(12) C(13) 110.2(8) ? . . . H(12) C(12) C(13) 110.8(7) ? . . . H(13) C(12) C(13) 110.6(8) ? . . . C(12) C(13) H(14) 107.7(7) ? . . . H(12) C(12) H(11) 111(1) ? . . . H(13) C(12) H(11) 106(1) ? . . . H(13) C(12) H(12) 107(1) ? . . . H(14) C(13) C(14) 107.7(7) ? . . . C(13) C(14) H(15) 111.0(8) ? . . . C(13) C(14) H(16) 108.8(8) ? . . . C(13) C(14) H(17) 110.5(9) ? . . . H(16) C(14) H(15) 109(1) ? . . . H(17) C(14) H(15) 108(1) ? . . . H(17) C(14) H(16) 108(1) ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(1) N(1) C(2) C(3) 155.99(7) ? . . . . C(13) N(1) C(2) C(3) -73.58(9) ? . . . . C(1) N(1) C(13) C(12) 48.6(1) ? . . . . C(1) N(1) C(13) C(14) -78.7(1) ? . . . . C(2) N(1) C(13) C(12) -80.42(9) ? . . . . C(2) N(1) C(13) C(14) 152.29(7) ? . . . . C(10) N(2) C(3) C(2) 178.34(7) ? . . . . C(10) N(2) C(3) C(4) -0.1(1) ? . . . . C(3) N(2) C(10) C(9) 179.96(8) ? . . . . C(3) N(2) C(10) C(11) 0.2(1) ? . . . . N(1) C(2) C(3) N(2) 138.12(8) ? . . . . N(1) C(2) C(3) C(4) -43.4(1) ? . . . . N(2) C(3) C(4) C(5) 0.4(1) ? . . . . C(2) C(3) C(4) C(5) -177.93(8) ? . . . . C(3) C(4) C(5) C(11) -0.9(1) ? . . . . C(4) C(5) C(11) C(6) -178.66(9) ? . . . . C(4) C(5) C(11) C(10) 1.1(1) ? . . . . C(11) C(6) C(7) C(8) 1.0(2) ? . . . . C(7) C(6) C(11) C(5) 179.61(9) ? . . . . C(7) C(6) C(11) C(10) -0.1(1) ? . . . . C(6) C(7) C(8) C(9) -1.0(2) ? . . . . C(7) C(8) C(9) C(10) 0.2(2) ? . . . . C(8) C(9) C(10) N(2) -179.06(9) ? . . . . C(8) C(9) C(10) C(11) 0.7(1) ? . . . . N(2) C(10) C(11) C(5) -0.7(1) ? . . . . N(2) C(10) C(11) C(6) 179.03(9) ? . . . . C(9) C(10) C(11) C(5) 179.55(8) ? . . . . C(9) C(10) C(11) C(6) -0.7(1) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N(1) N(2) 3.554(1) ? . . N(1) C(3) 2.458(1) ? . . N(1) C(4) 2.917(1) ? . . N(1) C(12) 2.534(1) ? . . N(1) C(14) 2.465(1) ? . . N(2) C(2) 2.416(1) ? . . N(2) C(4) 2.409(1) ? . . N(2) C(5) 2.811(1) ? . . N(2) C(9) 2.395(1) ? . . N(2) C(11) 2.449(1) ? . . C(1) C(2) 2.428(1) ? . . C(1) C(12) 2.956(1) ? . . C(1) C(13) 2.480(1) ? . . C(1) C(14) 3.156(1) ? . . C(2) C(4) 2.532(1) ? . . C(2) C(12) 3.193(1) ? . . C(2) C(13) 2.430(1) ? . . C(3) C(5) 2.401(1) ? . . C(3) C(9) 3.592(1) ? . . C(3) C(10) 2.307(1) ? . . C(3) C(11) 2.756(1) ? . . C(3) C(13) 3.053(1) ? . . C(4) C(10) 2.735(1) ? . . C(4) C(11) 2.396(1) ? . . C(4) C(13) 3.555(1) ? . . C(5) C(6) 2.494(1) ? . . C(5) C(10) 2.417(2) ? . . C(6) C(8) 2.405(2) ? . . C(6) C(9) 2.791(2) ? . . C(6) C(10) 2.443(1) ? . . C(7) C(9) 2.409(2) ? . . C(7) C(10) 2.800(1) ? . . C(7) C(11) 2.415(1) ? . . C(8) C(10) 2.413(1) ? . . C(8) C(11) 2.792(2) ? . . C(9) C(11) 2.436(2) ? . . C(12) C(14) 2.518(2) ? . . N(1) H(1) 2.08(1) ? . . N(1) H(2) 2.03(1) ? . . N(1) H(3) 2.02(1) ? . . N(1) H(4) 2.09(1) ? . . N(1) H(5) 2.63(1) ? . . N(1) H(11) 2.86(1) ? . . N(1) H(12) 2.71(1) ? . . N(1) H(13) 3.37(1) ? . . N(1) H(14) 1.975(9) ? . . N(1) H(15) 2.73(1) ? . . N(1) H(16) 2.62(1) ? . . N(1) H(17) 3.32(1) ? . . N(2) H(3) 2.947(9) ? . . N(2) H(4) 2.46(1) ? . . N(2) H(5) 3.25(1) ? . . N(2) H(10) 2.56(1) ? . . N(2) H(14) 3.13(1) ? . . C(1) H(3) 2.48(1) ? . . C(1) H(4) 2.85(1) ? . . C(1) H(8) 3.51(1) ? . 54601 C(1) H(11) 2.78(1) ? . . C(1) H(12) 3.11(1) ? . . C(1) H(14) 3.266(9) ? . . C(1) H(15) 2.93(1) ? . . C(1) H(16) 3.47(1) ? . . C(2) H(1) 2.55(1) ? . . C(2) H(2) 3.27(1) ? . . C(2) H(5) 2.66(1) ? . . C(2) H(12) 2.93(1) ? . . C(2) H(14) 2.40(1) ? . . C(2) H(17) 3.44(1) ? . 65501 C(3) H(3) 2.05(1) ? . . C(3) H(4) 2.07(1) ? . . C(3) H(5) 2.06(1) ? . . C(3) H(6) 3.31(1) ? . . C(3) H(14) 2.55(1) ? . . C(4) H(3) 2.85(1) ? . . C(4) H(4) 3.35(1) ? . . C(4) H(6) 2.05(1) ? . . C(4) H(14) 3.11(1) ? . . C(5) H(5) 2.06(1) ? . . C(5) H(7) 2.69(1) ? . . C(6) H(6) 2.72(1) ? . . C(6) H(8) 2.05(1) ? . . C(6) H(9) 3.28(2) ? . . C(7) H(2) 3.14(1) ? . 56401 C(7) H(7) 2.06(1) ? . . C(7) H(9) 2.07(2) ? . . C(7) H(10) 3.30(1) ? . . C(7) H(11) 3.33(1) ? . 56401 C(7) H(15) 3.51(1) ? . 56401 C(8) H(7) 3.31(1) ? . . C(8) H(8) 2.10(1) ? . . C(8) H(10) 2.05(1) ? . . C(8) H(11) 3.34(1) ? . 56401 C(9) H(8) 3.31(1) ? . . C(9) H(9) 2.05(1) ? . . C(10) H(6) 3.33(1) ? . . C(10) H(7) 3.33(1) ? . . C(10) H(9) 3.31(1) ? . . C(10) H(10) 2.07(1) ? . . C(11) H(5) 3.30(1) ? . . C(11) H(6) 2.10(1) ? . . C(11) H(7) 2.08(1) ? . . C(11) H(8) 3.32(1) ? . . C(11) H(10) 3.32(1) ? . . C(12) H(1) 2.99(1) ? . . C(12) H(2) 2.81(1) ? . . C(12) H(4) 2.91(1) ? . . C(12) H(6) 3.06(1) ? . 55601 C(12) H(7) 3.46(1) ? . 55601 C(12) H(8) 3.60(1) ? . 54601 C(12) H(14) 2.07(1) ? . . C(12) H(15) 2.77(2) ? . . C(12) H(16) 3.37(1) ? . . C(12) H(17) 2.71(2) ? . . C(13) H(1) 2.96(1) ? . . C(13) H(2) 2.51(1) ? . . C(13) H(3) 3.28(1) ? . . C(13) H(4) 2.63(1) ? . . C(13) H(5) 3.45(1) ? . . C(13) H(11) 2.12(1) ? . . C(13) H(12) 2.09(1) ? . . C(13) H(13) 2.09(1) ? . . C(13) H(15) 2.09(1) ? . . C(13) H(16) 2.07(1) ? . . C(13) H(17) 2.09(1) ? . . C(14) H(2) 2.79(1) ? . . C(14) H(3) 3.36(1) ? . 45501 C(14) H(8) 3.41(1) ? . 54601 C(14) H(11) 2.71(1) ? . . C(14) H(12) 3.37(1) ? . . C(14) H(13) 2.75(1) ? . . C(14) H(14) 2.06(1) ? . . H(2) C(7) 3.14(1) ? . 54601 H(3) C(14) 3.36(1) ? . 65501 H(6) C(12) 3.06(1) ? . 55401 H(7) C(12) 3.46(1) ? . 55401 H(8) C(1) 3.51(1) ? . 56401 H(8) C(6) 2.05(1) ? . . H(8) C(8) 2.10(1) ? . . H(8) C(9) 3.31(1) ? . . H(8) C(11) 3.32(1) ? . . H(8) C(12) 3.60(1) ? . 56401 H(8) C(14) 3.41(1) ? . 56401 H(11) C(7) 3.33(1) ? . 54601 H(11) C(8) 3.34(1) ? . 54601 H(15) C(7) 3.51(1) ? . 54601 H(17) C(2) 3.44(1) ? . 45501 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data___BQDMEN-Mn2-070127-55 _database_code_depnum_ccdc_archive 'CCDC 297398' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C54 H66 Cl2 Mn2 N10 O12 ' _chemical_formula_moiety 'C54 H66 Cl2 Mn2 N10 O12 ' _chemical_formula_weight 1227.96 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' _symmetry_space_group_name_Hall 'P 4abw 2nw' _symmetry_Int_Tables_number 92 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-Y,1/2+X,1/4+Z 3 -X,-Y,1/2+Z 4 1/2+Y,1/2-X,3/4+Z 5 1/2-X,1/2+Y,1/4-Z 6 +Y,+X,-Z 7 1/2+X,1/2-Y,3/4-Z 8 -Y,-X,1/2-Z #------------------------------------------------------------------------------ _cell_length_a 12.9335(4) _cell_length_b 12.9335(4) _cell_length_c 32.6230(13) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 5457.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13061 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description unknown _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560.00 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 0.881 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 53797 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6257 _reflns_number_gt 6083 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1360 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 6257 _refine_ls_number_parameters 362 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0718P)^2^+3.7164P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.64 _refine_diff_density_min -0.51 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 2623 Friedel Pairs' _refine_ls_abs_structure_Flack 0.03(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mn Mn 0.337 0.728 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn(1) Mn 0.18272(3) 0.78515(3) 0.210161(13) 0.02703(12) Uani 1.00 1 d . . . Cl(1) Cl 0.42799(6) 1.00577(7) 0.46287(3) 0.0439(2) Uani 1.00 1 d . . . O(1) O 0.26644(15) 0.86643(15) 0.24155(6) 0.0288(4) Uani 1.00 1 d . . . O(2) O 0.3886(4) 0.9105(3) 0.4696(3) 0.191(3) Uani 1.00 1 d . . . O(3) O 0.3488(3) 1.0747(3) 0.45042(14) 0.0982(14) Uani 1.00 1 d . . . O(4) O 0.4821(6) 1.0405(4) 0.4947(2) 0.189(3) Uani 1.00 1 d . . . O(5) O 0.4938(7) 0.9880(7) 0.4325(2) 0.221(4) Uani 1.00 1 d . . . O(6) O -0.2863(3) 0.7316(4) 0.14169(13) 0.1024(14) Uani 1.00 1 d . . . N(1) N 0.2533(2) 0.8164(2) 0.15113(7) 0.0327(5) Uani 1.00 1 d . . . N(2) N 0.06390(19) 0.7178(2) 0.17292(8) 0.0314(5) Uani 1.00 1 d . . . N(3) N 0.3068(2) 0.6453(2) 0.19588(7) 0.0334(5) Uani 1.00 1 d . . . N(4) N 0.0516(2) 0.9174(2) 0.19845(7) 0.0318(5) Uani 1.00 1 d . . . N(5) N -0.2767(3) 0.8564(3) 0.09322(16) 0.0774(12) Uani 1.00 1 d . . . C(1) C 0.1960(2) 0.7514(2) 0.12069(9) 0.0404(7) Uani 1.00 1 d . . . C(2) C 0.0818(2) 0.7540(2) 0.12991(9) 0.0387(7) Uani 1.00 1 d . . . C(3) C 0.3627(2) 0.7837(2) 0.15225(10) 0.0385(6) Uani 1.00 1 d . . . C(4) C 0.3766(2) 0.6771(2) 0.16946(9) 0.0360(6) Uani 1.00 1 d . . . C(5) C 0.4628(2) 0.6180(3) 0.15774(12) 0.0438(7) Uani 1.00 1 d . . . C(6) C 0.4773(2) 0.5240(3) 0.17437(12) 0.0480(8) Uani 1.00 1 d . . . C(7) C 0.4164(3) 0.3892(2) 0.22306(13) 0.0526(10) Uani 1.00 1 d . . . C(8) C 0.3459(3) 0.3574(2) 0.25131(14) 0.0563(10) Uani 1.00 1 d . . . C(9) C 0.2607(3) 0.4197(2) 0.26109(12) 0.0508(9) Uani 1.00 1 d . . . C(10) C 0.2476(3) 0.5144(2) 0.24266(10) 0.0435(7) Uani 1.00 1 d . . . C(11) C 0.3201(2) 0.5492(2) 0.21367(10) 0.0367(6) Uani 1.00 1 d . . . C(12) C 0.4065(2) 0.4863(2) 0.20344(12) 0.0432(8) Uani 1.00 1 d . . . C(13) C 0.2516(3) 0.9257(2) 0.13770(11) 0.0438(7) Uani 1.00 1 d . . . C(14) C -0.0365(2) 0.7557(2) 0.18804(10) 0.0363(6) Uani 1.00 1 d . . . C(15) C -0.0382(2) 0.8720(2) 0.19174(9) 0.0330(6) Uani 1.00 1 d . . . C(16) C -0.1326(2) 0.9264(3) 0.18835(11) 0.0414(7) Uani 1.00 1 d . . . C(17) C -0.1321(2) 1.0309(3) 0.19267(11) 0.0454(8) Uani 1.00 1 d . . . C(18) C -0.0318(3) 1.1919(3) 0.20464(11) 0.0522(9) Uani 1.00 1 d . . . C(19) C 0.0620(3) 1.2382(2) 0.21182(12) 0.0535(9) Uani 1.00 1 d . . . C(20) C 0.1512(3) 1.1783(2) 0.21457(10) 0.0463(7) Uani 1.00 1 d . . . C(21) C 0.1477(2) 1.0730(2) 0.21039(10) 0.0374(6) Uani 1.00 1 d . . . C(22) C 0.0528(2) 1.0239(2) 0.20266(9) 0.0345(6) Uani 1.00 1 d . . . C(23) C -0.0382(2) 1.0833(2) 0.19963(10) 0.0404(7) Uani 1.00 1 d . . . C(24) C 0.0611(3) 0.6036(2) 0.17418(12) 0.0435(7) Uani 1.00 1 d . . . C(25) C -0.2506(3) 0.7657(4) 0.10962(16) 0.0678(12) Uani 1.00 1 d . . . C(26) C -0.3490(7) 0.9201(7) 0.1115(3) 0.186(6) Uani 1.00 1 d . . . C(27) C -0.2334(6) 0.8791(7) 0.0533(2) 0.139(3) Uani 1.00 1 d . . . H(1) H 0.2213 0.6793 0.1220 0.048 Uiso 1.00 1 c R . . H(2) H 0.2085 0.7780 0.0927 0.048 Uiso 1.00 1 c R . . H(3) H 0.0553 0.8253 0.1266 0.046 Uiso 1.00 1 c R . . H(4) H 0.0444 0.7087 0.1105 0.046 Uiso 1.00 1 c R . . H(5) H 0.4025 0.8334 0.1691 0.046 Uiso 1.00 1 c R . . H(6) H 0.3912 0.7857 0.1241 0.046 Uiso 1.00 1 c R . . H(7) H 0.5106 0.6442 0.1382 0.053 Uiso 1.00 1 c R . . H(8) H 0.5351 0.4833 0.1665 0.058 Uiso 1.00 1 c R . . H(9) H 0.4731 0.3457 0.2164 0.063 Uiso 1.00 1 c R . . H(10) H 0.3545 0.2925 0.2645 0.068 Uiso 1.00 1 c R . . H(11) H 0.2115 0.3962 0.2806 0.061 Uiso 1.00 1 c R . . H(12) H 0.1898 0.5563 0.2495 0.052 Uiso 1.00 1 c R . . H(13) H 0.1885 0.9388 0.1219 0.053 Uiso 1.00 1 c R . . H(14) H 0.3122 0.9397 0.1206 0.053 Uiso 1.00 1 c R . . H(15) H 0.2529 0.9710 0.1618 0.053 Uiso 1.00 1 c R . . H(16) H -0.0509 0.7246 0.2152 0.044 Uiso 1.00 1 c R . . H(17) H -0.0918 0.7334 0.1690 0.044 Uiso 1.00 1 c R . . H(18) H -0.1953 0.8905 0.1832 0.050 Uiso 1.00 1 c R . . H(19) H -0.1951 1.0685 0.1910 0.054 Uiso 1.00 1 c R . . H(20) H -0.0926 1.2329 0.2030 0.063 Uiso 1.00 1 c R . . H(21) H 0.0661 1.3111 0.2149 0.064 Uiso 1.00 1 c R . . H(22) H 0.2158 1.2111 0.2195 0.056 Uiso 1.00 1 c R . . H(23) H 0.2092 1.0333 0.2127 0.045 Uiso 1.00 1 c R . . H(24) H 0.1056 0.5757 0.1525 0.052 Uiso 1.00 1 c R . . H(25) H -0.0101 0.5798 0.1699 0.052 Uiso 1.00 1 c R . . H(26) H 0.0858 0.5796 0.2009 0.052 Uiso 1.00 1 c R . . H(27) H -0.2010 0.7248 0.0955 0.081 Uiso 1.00 1 c R . . H(28) H -0.4180 0.9031 0.1010 0.223 Uiso 1.00 1 c R . . H(29) H -0.3329 0.9924 0.1051 0.223 Uiso 1.00 1 c R . . H(30) H -0.3474 0.9100 0.1412 0.223 Uiso 1.00 1 c R . . H(31) H -0.1669 0.9143 0.0567 0.167 Uiso 1.00 1 c R . . H(32) H -0.2810 0.9240 0.0381 0.167 Uiso 1.00 1 c R . . H(33) H -0.2232 0.8145 0.0382 0.167 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mn(1) 0.0293(2) 0.0277(2) 0.02416(19) -0.00126(16) -0.00137(16) -0.00126(16) Cl(1) 0.0391(4) 0.0488(4) 0.0436(4) 0.0010(3) -0.0066(3) -0.0034(3) O(1) 0.0294(10) 0.0297(9) 0.0273(9) -0.0023(7) -0.0022(7) 0.0008(7) O(2) 0.073(2) 0.075(3) 0.424(12) -0.015(2) -0.036(5) 0.080(5) O(3) 0.098(3) 0.081(2) 0.116(3) 0.043(2) -0.043(2) -0.008(2) O(4) 0.268(8) 0.108(4) 0.190(6) 0.032(4) -0.174(6) -0.045(4) O(5) 0.213(7) 0.297(9) 0.154(5) 0.155(7) 0.121(5) 0.083(6) O(6) 0.095(3) 0.141(4) 0.071(2) -0.029(2) -0.008(2) 0.013(2) N(1) 0.0383(12) 0.0339(12) 0.0260(11) 0.0011(10) 0.0015(9) 0.0003(9) N(2) 0.0335(12) 0.0322(12) 0.0285(11) -0.0033(10) -0.0045(9) -0.0041(9) N(3) 0.0385(14) 0.0320(12) 0.0297(11) 0.0047(10) -0.0040(10) -0.0053(9) N(4) 0.0349(12) 0.0343(12) 0.0262(10) 0.0009(10) -0.0017(9) 0.0009(9) N(5) 0.060(2) 0.077(2) 0.095(3) -0.001(2) -0.033(2) 0.013(2) C(1) 0.0477(19) 0.0475(17) 0.0260(13) 0.0044(14) -0.0015(12) -0.0078(12) C(2) 0.0423(17) 0.0480(17) 0.0258(13) 0.0000(14) -0.0067(12) -0.0049(12) C(3) 0.0348(15) 0.0442(17) 0.0364(15) 0.0000(13) 0.0045(12) -0.0016(13) C(4) 0.0326(14) 0.0443(16) 0.0312(13) 0.0002(13) -0.0033(11) -0.0094(13) C(5) 0.0326(15) 0.052(2) 0.0469(18) 0.0069(14) -0.0009(13) -0.0132(15) C(6) 0.0378(17) 0.051(2) 0.056(2) 0.0119(15) -0.0088(15) -0.0217(16) C(7) 0.055(2) 0.0369(17) 0.066(2) 0.0118(16) -0.0278(19) -0.0116(17) C(8) 0.072(2) 0.0311(16) 0.066(2) 0.0044(16) -0.030(2) -0.0029(16) C(9) 0.072(2) 0.0348(17) 0.0452(19) -0.0068(16) -0.0126(18) 0.0001(14) C(10) 0.058(2) 0.0342(16) 0.0377(17) 0.0015(14) -0.0059(15) -0.0046(13) C(11) 0.0424(16) 0.0296(13) 0.0382(15) -0.0015(12) -0.0131(13) -0.0072(12) C(12) 0.0434(17) 0.0369(16) 0.0492(19) 0.0067(13) -0.0169(15) -0.0146(14) C(13) 0.0495(18) 0.0451(18) 0.0368(16) 0.0016(15) 0.0067(14) 0.0084(14) C(14) 0.0299(14) 0.0396(16) 0.0395(15) -0.0045(12) -0.0032(12) -0.0036(13) C(15) 0.0332(14) 0.0383(15) 0.0274(13) 0.0037(12) -0.0018(11) -0.0006(11) C(16) 0.0322(15) 0.054(2) 0.0376(16) 0.0042(14) -0.0032(13) 0.0018(14) C(17) 0.0443(18) 0.052(2) 0.0396(16) 0.0166(16) -0.0046(14) 0.0041(15) C(18) 0.074(2) 0.0396(18) 0.0434(18) 0.0153(18) -0.0030(17) 0.0016(15) C(19) 0.086(3) 0.0356(17) 0.0390(17) 0.0052(18) 0.0031(18) 0.0050(14) C(20) 0.065(2) 0.0373(16) 0.0362(16) -0.0069(15) 0.0026(15) 0.0029(14) C(21) 0.0462(17) 0.0364(15) 0.0298(14) -0.0036(13) 0.0012(12) -0.0009(12) C(22) 0.0419(16) 0.0346(14) 0.0271(13) 0.0014(12) 0.0003(11) 0.0003(11) C(23) 0.0476(18) 0.0391(16) 0.0345(15) 0.0124(14) 0.0008(13) 0.0054(12) C(24) 0.0505(19) 0.0338(16) 0.0460(18) -0.0061(14) -0.0104(15) -0.0062(14) C(25) 0.051(2) 0.083(3) 0.070(2) -0.002(2) -0.012(2) -0.020(2) C(26) 0.140(7) 0.171(9) 0.247(11) 0.101(7) -0.116(8) -0.110(8) C(27) 0.099(5) 0.167(7) 0.151(7) -0.068(5) -0.056(5) 0.077(6) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR92 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mn(1) Mn(1) 2.6649(5) yes . 8_665 Mn(1) O(1) 1.8238(19) yes . . Mn(1) O(1) 1.8251(19) yes . 8_665 Mn(1) N(1) 2.169(2) yes . . Mn(1) N(2) 2.144(2) yes . . Cl(1) O(2) 1.352(5) yes . . Cl(1) O(3) 1.417(4) yes . . Cl(1) O(4) 1.329(7) yes . . Cl(1) O(5) 1.326(8) yes . . O(6) C(25) 1.226(6) yes . . N(1) C(1) 1.497(4) yes . . N(1) C(3) 1.477(4) yes . . N(1) C(13) 1.481(4) yes . . N(2) C(2) 1.497(4) yes . . N(2) C(14) 1.473(4) yes . . N(2) C(24) 1.478(4) yes . . N(3) C(4) 1.314(3) yes . . N(3) C(11) 1.382(3) yes . . N(4) C(15) 1.319(4) yes . . N(4) C(22) 1.384(4) yes . . N(5) C(25) 1.333(7) yes . . N(5) C(26) 1.382(11) yes . . N(5) C(27) 1.446(10) yes . . C(1) C(2) 1.507(4) yes . . C(3) C(4) 1.501(4) yes . . C(4) C(5) 1.405(4) yes . . C(5) C(6) 1.344(5) yes . . C(6) C(12) 1.406(5) yes . . C(7) C(8) 1.360(6) yes . . C(7) C(12) 1.415(5) yes . . C(8) C(9) 1.402(6) yes . . C(9) C(10) 1.376(5) yes . . C(10) C(11) 1.405(4) yes . . C(11) C(12) 1.423(4) yes . . C(14) C(15) 1.509(4) yes . . C(15) C(16) 1.414(4) yes . . C(16) C(17) 1.359(5) yes . . C(17) C(23) 1.410(5) yes . . C(18) C(19) 1.373(6) yes . . C(18) C(23) 1.416(5) yes . . C(19) C(20) 1.393(6) yes . . C(20) C(21) 1.369(4) yes . . C(21) C(22) 1.405(4) yes . . C(22) C(23) 1.409(4) yes . . C(1) H(1) 0.990 no . . C(1) H(2) 0.990 no . . C(2) H(3) 0.990 no . . C(2) H(4) 0.990 no . . C(3) H(5) 0.990 no . . C(3) H(6) 0.990 no . . C(5) H(7) 0.950 no . . C(6) H(8) 0.950 no . . C(7) H(9) 0.950 no . . C(8) H(10) 0.950 no . . C(9) H(11) 0.950 no . . C(10) H(12) 0.950 no . . C(13) H(13) 0.980 no . . C(13) H(14) 0.980 no . . C(13) H(15) 0.980 no . . C(14) H(16) 0.990 no . . C(14) H(17) 0.990 no . . C(16) H(18) 0.950 no . . C(17) H(19) 0.950 no . . C(18) H(20) 0.950 no . . C(19) H(21) 0.950 no . . C(20) H(22) 0.950 no . . C(21) H(23) 0.950 no . . C(24) H(24) 0.980 no . . C(24) H(25) 0.980 no . . C(24) H(26) 0.980 no . . C(25) H(27) 0.950 no . . C(26) H(28) 0.980 no . . C(26) H(29) 0.980 no . . C(26) H(30) 0.980 no . . C(27) H(31) 0.980 no . . C(27) H(32) 0.980 no . . C(27) H(33) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Mn(1) Mn(1) O(1) 43.10(6) yes 8_665 . . Mn(1) Mn(1) O(1) 43.06(6) yes 8_665 . 8_665 Mn(1) Mn(1) N(1) 140.47(7) yes 8_665 . . Mn(1) Mn(1) N(2) 136.71(7) yes 8_665 . . O(1) Mn(1) O(1) 86.15(8) yes . . 8_665 O(1) Mn(1) N(1) 98.12(9) yes . . . O(1) Mn(1) N(2) 167.95(9) yes . . . O(1) Mn(1) N(1) 168.80(9) yes 8_665 . . O(1) Mn(1) N(2) 95.21(9) yes 8_665 . . N(1) Mn(1) N(2) 82.78(9) yes . . . O(2) Cl(1) O(3) 110.3(3) yes . . . O(2) Cl(1) O(4) 112.4(5) yes . . . O(2) Cl(1) O(5) 101.8(5) yes . . . O(3) Cl(1) O(4) 113.0(3) yes . . . O(3) Cl(1) O(5) 111.0(4) yes . . . O(4) Cl(1) O(5) 107.7(5) yes . . . Mn(1) O(1) Mn(1) 93.83(9) yes . . 8_665 Mn(1) N(1) C(1) 106.01(18) yes . . . Mn(1) N(1) C(3) 109.15(18) yes . . . Mn(1) N(1) C(13) 115.73(19) yes . . . C(1) N(1) C(3) 109.3(2) yes . . . C(1) N(1) C(13) 109.4(2) yes . . . C(3) N(1) C(13) 107.1(2) yes . . . Mn(1) N(2) C(2) 107.03(18) yes . . . Mn(1) N(2) C(14) 107.89(18) yes . . . Mn(1) N(2) C(24) 114.1(2) yes . . . C(2) N(2) C(14) 110.3(2) yes . . . C(2) N(2) C(24) 110.0(2) yes . . . C(14) N(2) C(24) 107.5(2) yes . . . C(4) N(3) C(11) 118.1(2) yes . . . C(15) N(4) C(22) 118.0(2) yes . . . C(25) N(5) C(26) 121.6(6) yes . . . C(25) N(5) C(27) 116.2(5) yes . . . C(26) N(5) C(27) 121.9(6) yes . . . N(1) C(1) C(2) 109.9(2) yes . . . N(2) C(2) C(1) 109.4(2) yes . . . N(1) C(3) C(4) 112.8(2) yes . . . N(3) C(4) C(3) 116.8(2) yes . . . N(3) C(4) C(5) 123.6(3) yes . . . C(3) C(4) C(5) 119.6(2) yes . . . C(4) C(5) C(6) 119.5(3) yes . . . C(5) C(6) C(12) 119.7(3) yes . . . C(8) C(7) C(12) 121.0(3) yes . . . C(7) C(8) C(9) 120.5(3) yes . . . C(8) C(9) C(10) 120.6(3) yes . . . C(9) C(10) C(11) 119.8(3) yes . . . N(3) C(11) C(10) 119.2(2) yes . . . N(3) C(11) C(12) 120.9(2) yes . . . C(10) C(11) C(12) 119.9(2) yes . . . C(6) C(12) C(7) 123.7(3) yes . . . C(6) C(12) C(11) 118.1(3) yes . . . C(7) C(12) C(11) 118.2(3) yes . . . N(2) C(14) C(15) 111.7(2) yes . . . N(4) C(15) C(14) 116.5(2) yes . . . N(4) C(15) C(16) 123.4(3) yes . . . C(14) C(15) C(16) 120.1(2) yes . . . C(15) C(16) C(17) 118.9(3) yes . . . C(16) C(17) C(23) 120.0(3) yes . . . C(19) C(18) C(23) 120.3(3) yes . . . C(18) C(19) C(20) 120.0(3) yes . . . C(19) C(20) C(21) 121.3(3) yes . . . C(20) C(21) C(22) 119.8(3) yes . . . N(4) C(22) C(21) 118.6(2) yes . . . N(4) C(22) C(23) 121.8(3) yes . . . C(21) C(22) C(23) 119.7(3) yes . . . C(17) C(23) C(18) 123.1(3) yes . . . C(17) C(23) C(22) 117.9(3) yes . . . C(18) C(23) C(22) 118.9(3) yes . . . O(6) C(25) N(5) 124.3(5) yes . . . N(1) C(1) H(1) 109.7 no . . . N(1) C(1) H(2) 109.7 no . . . C(2) C(1) H(1) 109.7 no . . . C(2) C(1) H(2) 109.7 no . . . H(1) C(1) H(2) 108.2 no . . . N(2) C(2) H(3) 109.8 no . . . N(2) C(2) H(4) 109.8 no . . . C(1) C(2) H(3) 109.8 no . . . C(1) C(2) H(4) 109.8 no . . . H(3) C(2) H(4) 108.3 no . . . N(1) C(3) H(5) 109.0 no . . . N(1) C(3) H(6) 109.0 no . . . C(4) C(3) H(5) 109.0 no . . . C(4) C(3) H(6) 109.0 no . . . H(5) C(3) H(6) 107.8 no . . . C(4) C(5) H(7) 120.2 no . . . C(6) C(5) H(7) 120.2 no . . . C(5) C(6) H(8) 120.1 no . . . C(12) C(6) H(8) 120.2 no . . . C(8) C(7) H(9) 119.5 no . . . C(12) C(7) H(9) 119.5 no . . . C(7) C(8) H(10) 119.8 no . . . C(9) C(8) H(10) 119.8 no . . . C(8) C(9) H(11) 119.7 no . . . C(10) C(9) H(11) 119.7 no . . . C(9) C(10) H(12) 120.1 no . . . C(11) C(10) H(12) 120.1 no . . . N(1) C(13) H(13) 109.5 no . . . N(1) C(13) H(14) 109.5 no . . . N(1) C(13) H(15) 109.5 no . . . H(13) C(13) H(14) 109.5 no . . . H(13) C(13) H(15) 109.5 no . . . H(14) C(13) H(15) 109.5 no . . . N(2) C(14) H(16) 109.3 no . . . N(2) C(14) H(17) 109.3 no . . . C(15) C(14) H(16) 109.3 no . . . C(15) C(14) H(17) 109.3 no . . . H(16) C(14) H(17) 107.9 no . . . C(15) C(16) H(18) 120.6 no . . . C(17) C(16) H(18) 120.6 no . . . C(16) C(17) H(19) 120.0 no . . . C(23) C(17) H(19) 120.0 no . . . C(19) C(18) H(20) 119.9 no . . . C(23) C(18) H(20) 119.9 no . . . C(18) C(19) H(21) 120.0 no . . . C(20) C(19) H(21) 120.0 no . . . C(19) C(20) H(22) 119.4 no . . . C(21) C(20) H(22) 119.4 no . . . C(20) C(21) H(23) 120.1 no . . . C(22) C(21) H(23) 120.1 no . . . N(2) C(24) H(24) 109.5 no . . . N(2) C(24) H(25) 109.5 no . . . N(2) C(24) H(26) 109.5 no . . . H(24) C(24) H(25) 109.5 no . . . H(24) C(24) H(26) 109.5 no . . . H(25) C(24) H(26) 109.5 no . . . O(6) C(25) H(27) 117.9 no . . . N(5) C(25) H(27) 117.8 no . . . N(5) C(26) H(28) 109.5 no . . . N(5) C(26) H(29) 109.5 no . . . N(5) C(26) H(30) 109.5 no . . . H(28) C(26) H(29) 109.5 no . . . H(28) C(26) H(30) 109.5 no . . . H(29) C(26) H(30) 109.5 no . . . N(5) C(27) H(31) 109.5 no . . . N(5) C(27) H(32) 109.5 no . . . N(5) C(27) H(33) 109.5 no . . . H(31) C(27) H(32) 109.5 no . . . H(31) C(27) H(33) 109.5 no . . . H(32) C(27) H(33) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Mn(1) Mn(1) O(1) -177.95(12) ? . . 8_665 8_665 O(1) Mn(1) Mn(1) N(1) -163.86(14) ? . . 8_665 8_665 O(1) Mn(1) Mn(1) N(2) 19.69(13) ? . . 8_665 8_665 O(1) Mn(1) Mn(1) N(1) 14.09(14) ? 8_665 . 8_665 8_665 O(1) Mn(1) Mn(1) N(2) -162.36(13) ? 8_665 . 8_665 8_665 O(1) Mn(1) Mn(1) O(1) 177.95(12) ? 8_665 . 8_665 . Mn(1) Mn(1) N(1) C(1) 168.18(15) ? 8_665 . . . Mn(1) Mn(1) N(1) C(3) 50.6(2) ? 8_665 . . . Mn(1) Mn(1) N(1) C(13) -70.4(2) ? 8_665 . . . N(1) Mn(1) Mn(1) O(1) -163.86(14) ? . . 8_665 8_665 N(1) Mn(1) Mn(1) N(1) -149.77(15) ? . . 8_665 8_665 N(1) Mn(1) Mn(1) N(2) 33.78(15) ? . . 8_665 8_665 N(1) Mn(1) Mn(1) O(1) 14.09(14) ? . . 8_665 . Mn(1) Mn(1) N(2) C(2) 163.27(15) ? 8_665 . . . Mn(1) Mn(1) N(2) C(14) 44.6(2) ? 8_665 . . . Mn(1) Mn(1) N(2) C(24) -74.8(2) ? 8_665 . . . N(2) Mn(1) Mn(1) O(1) 19.69(13) ? . . 8_665 8_665 N(2) Mn(1) Mn(1) N(1) 33.78(15) ? . . 8_665 8_665 N(2) Mn(1) Mn(1) N(2) -142.67(14) ? . . 8_665 8_665 N(2) Mn(1) Mn(1) O(1) -162.36(13) ? . . 8_665 . O(1) Mn(1) O(1) Mn(1) 1.41(8) ? . . 8_665 8_665 O(1) Mn(1) O(1) Mn(1) -1.40(8) ? 8_665 . . 8_665 O(1) Mn(1) N(1) C(1) 177.86(19) ? . . . . O(1) Mn(1) N(1) C(3) 60.2(2) ? . . . . O(1) Mn(1) N(1) C(13) -60.7(2) ? . . . . N(1) Mn(1) O(1) Mn(1) -170.99(9) ? . . . 8_665 O(1) Mn(1) N(2) C(2) 80.6(5) ? . . . . O(1) Mn(1) N(2) C(14) -38.0(5) ? . . . . O(1) Mn(1) N(2) C(24) -157.4(4) ? . . . . N(2) Mn(1) O(1) Mn(1) 95.6(4) ? . . . 8_665 O(1) Mn(1) N(1) C(1) 66.0(5) ? 8_665 . . . O(1) Mn(1) N(1) C(3) -51.6(5) ? 8_665 . . . O(1) Mn(1) N(1) C(13) -172.5(4) ? 8_665 . . . N(1) Mn(1) O(1) Mn(1) 114.3(4) ? . . 8_665 8_665 O(1) Mn(1) N(2) C(2) 176.63(19) ? 8_665 . . . O(1) Mn(1) N(2) C(14) 57.98(19) ? 8_665 . . . O(1) Mn(1) N(2) C(24) -61.4(2) ? 8_665 . . . N(2) Mn(1) O(1) Mn(1) -166.58(9) ? . . 8_665 8_665 N(1) Mn(1) N(2) C(2) -14.45(19) ? . . . . N(1) Mn(1) N(2) C(14) -133.1(2) ? . . . . N(1) Mn(1) N(2) C(24) 107.5(2) ? . . . . N(2) Mn(1) N(1) C(1) -14.27(19) ? . . . . N(2) Mn(1) N(1) C(3) -131.9(2) ? . . . . N(2) Mn(1) N(1) C(13) 107.2(2) ? . . . . Mn(1) N(1) C(1) C(2) 41.3(2) ? . . . . Mn(1) N(1) C(3) C(4) 48.3(2) ? . . . . C(1) N(1) C(3) C(4) -67.3(3) ? . . . . C(3) N(1) C(1) C(2) 158.8(2) ? . . . . C(13) N(1) C(1) C(2) -84.2(3) ? . . . . C(13) N(1) C(3) C(4) 174.3(2) ? . . . . Mn(1) N(2) C(2) C(1) 41.3(3) ? . . . . Mn(1) N(2) C(14) C(15) 51.2(2) ? . . . . C(2) N(2) C(14) C(15) -65.4(3) ? . . . . C(14) N(2) C(2) C(1) 158.4(2) ? . . . . C(24) N(2) C(2) C(1) -83.2(3) ? . . . . C(24) N(2) C(14) C(15) 174.7(2) ? . . . . C(4) N(3) C(11) C(10) 178.7(2) ? . . . . C(4) N(3) C(11) C(12) -0.4(4) ? . . . . C(11) N(3) C(4) C(3) -177.1(2) ? . . . . C(11) N(3) C(4) C(5) 1.3(4) ? . . . . C(15) N(4) C(22) C(21) 179.1(2) ? . . . . C(15) N(4) C(22) C(23) -0.5(4) ? . . . . C(22) N(4) C(15) C(14) -179.0(2) ? . . . . C(22) N(4) C(15) C(16) 0.5(4) ? . . . . C(26) N(5) C(25) O(6) -0.8(9) ? . . . . C(27) N(5) C(25) O(6) -174.5(5) ? . . . . N(1) C(1) C(2) N(2) -57.1(3) ? . . . . N(1) C(3) C(4) N(3) -28.0(3) ? . . . . N(1) C(3) C(4) C(5) 153.6(2) ? . . . . N(3) C(4) C(5) C(6) -0.9(5) ? . . . . C(3) C(4) C(5) C(6) 177.5(3) ? . . . . C(4) C(5) C(6) C(12) -0.4(5) ? . . . . C(5) C(6) C(12) C(7) -178.9(3) ? . . . . C(5) C(6) C(12) C(11) 1.2(5) ? . . . . C(8) C(7) C(12) C(6) 179.3(3) ? . . . . C(8) C(7) C(12) C(11) -0.8(5) ? . . . . C(12) C(7) C(8) C(9) 1.1(6) ? . . . . C(7) C(8) C(9) C(10) -0.8(6) ? . . . . C(8) C(9) C(10) C(11) 0.2(4) ? . . . . C(9) C(10) C(11) N(3) -179.0(3) ? . . . . C(9) C(10) C(11) C(12) 0.1(3) ? . . . . N(3) C(11) C(12) C(6) -0.8(5) ? . . . . N(3) C(11) C(12) C(7) 179.3(3) ? . . . . C(10) C(11) C(12) C(6) -179.9(3) ? . . . . C(10) C(11) C(12) C(7) 0.2(4) ? . . . . N(2) C(14) C(15) N(4) -27.6(3) ? . . . . N(2) C(14) C(15) C(16) 152.9(2) ? . . . . N(4) C(15) C(16) C(17) -0.8(5) ? . . . . C(14) C(15) C(16) C(17) 178.6(3) ? . . . . C(15) C(16) C(17) C(23) 1.2(5) ? . . . . C(16) C(17) C(23) C(18) -179.7(3) ? . . . . C(16) C(17) C(23) C(22) -1.2(5) ? . . . . C(19) C(18) C(23) C(17) 179.2(3) ? . . . . C(19) C(18) C(23) C(22) 0.8(5) ? . . . . C(23) C(18) C(19) C(20) -0.6(5) ? . . . . C(18) C(19) C(20) C(21) -0.2(4) ? . . . . C(19) C(20) C(21) C(22) 0.8(5) ? . . . . C(20) C(21) C(22) N(4) 179.8(2) ? . . . . C(20) C(21) C(22) C(23) -0.6(4) ? . . . . N(4) C(22) C(23) C(17) 0.9(4) ? . . . . N(4) C(22) C(23) C(18) 179.4(2) ? . . . . C(21) C(22) C(23) C(17) -178.7(3) ? . . . . C(21) C(22) C(23) C(18) -0.2(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(2) C(7) 3.596(6) ? . 2_555 O(2) C(8) 3.448(7) ? . 2_555 O(2) C(20) 3.466(6) ? . 2_655 O(2) C(21) 3.448(6) ? . 2_655 O(3) C(2) 3.569(5) ? . 8_665 O(3) C(25) 3.347(6) ? . 8_665 O(3) C(27) 3.595(9) ? . 8_665 O(4) C(10) 3.532(9) ? . 7_565 O(4) C(19) 3.358(7) ? . 7_575 O(4) C(24) 3.395(8) ? . 7_565 O(5) C(3) 3.447(9) ? . 2_655 O(5) C(13) 3.546(10) ? . 2_655 O(5) C(26) 3.325(13) ? . 2_665 O(6) C(14) 3.580(5) ? . . O(6) C(16) 3.551(6) ? . . C(1) C(20) 3.541(4) ? . 5_545 C(2) O(3) 3.569(5) ? . 8_665 C(3) O(5) 3.447(10) ? . 4_464 C(7) O(2) 3.596(6) ? . 4_454 C(8) O(2) 3.448(6) ? . 4_454 C(10) O(4) 3.532(9) ? . 7_465 C(13) O(5) 3.546(9) ? . 4_464 C(14) O(6) 3.580(5) ? . . C(16) O(6) 3.551(6) ? . . C(19) O(4) 3.358(7) ? . 7_475 C(20) O(2) 3.466(6) ? . 4_464 C(20) C(1) 3.541(4) ? . 5_555 C(21) O(2) 3.448(6) ? . 4_464 C(24) O(4) 3.395(8) ? . 7_465 C(25) O(3) 3.347(6) ? . 8_665 C(26) O(5) 3.325(13) ? . 4_364 C(27) O(3) 3.595(10) ? . 8_665 Cl(1) H(4) 3.045 ? . 8_665 Cl(1) H(9) 3.567 ? . 2_555 Cl(1) H(32) 3.236 ? . 3_575 O(2) H(1) 3.548 ? . 8_665 O(2) H(2) 3.336 ? . 8_665 O(2) H(4) 2.957 ? . 8_665 O(2) H(9) 3.138 ? . 2_555 O(2) H(10) 2.856 ? . 2_555 O(2) H(15) 3.318 ? . 2_655 O(2) H(16) 2.863 ? . 7_565 O(2) H(22) 2.829 ? . 2_655 O(2) H(23) 2.801 ? . 2_655 O(2) H(32) 3.395 ? . 3_575 O(3) H(4) 2.622 ? . 8_665 O(3) H(9) 2.886 ? . 2_555 O(3) H(19) 3.179 ? . 2_665 O(3) H(27) 2.413 ? . 8_665 O(3) H(32) 2.993 ? . 3_575 O(3) H(33) 3.590 ? . 3_575 O(3) H(33) 2.880 ? . 8_665 O(4) H(11) 3.187 ? . 7_565 O(4) H(12) 2.970 ? . 7_565 O(4) H(20) 3.526 ? . 7_575 O(4) H(21) 2.569 ? . 7_575 O(4) H(25) 3.193 ? . 7_565 O(4) H(26) 2.713 ? . 7_565 O(4) H(32) 2.997 ? . 3_575 O(5) H(4) 3.000 ? . 8_665 O(5) H(5) 2.532 ? . 2_655 O(5) H(11) 3.409 ? . 7_565 O(5) H(12) 3.416 ? . 7_565 O(5) H(14) 3.162 ? . 2_655 O(5) H(15) 3.149 ? . 2_655 O(5) H(24) 3.157 ? . 8_665 O(5) H(25) 3.486 ? . 8_665 O(5) H(28) 3.213 ? . 2_665 O(5) H(29) 3.432 ? . 2_665 O(5) H(30) 2.809 ? . 2_665 O(6) H(7) 2.863 ? . 1_455 O(6) H(10) 3.257 ? . 8_565 O(6) H(11) 2.997 ? . 8_565 O(6) H(17) 2.668 ? . . O(6) H(18) 2.727 ? . . O(6) H(19) 3.433 ? . 5_445 O(6) H(20) 3.464 ? . 5_445 O(6) H(29) 3.459 ? . 5_445 N(3) H(13) 3.467 ? . 5_545 N(5) H(8) 3.543 ? . 5_555 N(5) H(18) 3.148 ? . . N(5) H(20) 2.773 ? . 5_445 C(1) H(22) 3.197 ? . 5_545 C(2) H(9) 3.433 ? . 5_555 C(4) H(13) 3.467 ? . 5_545 C(5) H(13) 3.183 ? . 5_545 C(6) H(3) 3.091 ? . 5_545 C(6) H(13) 2.844 ? . 5_545 C(6) H(31) 2.899 ? . 5_545 C(7) H(2) 3.046 ? . 5_545 C(7) H(3) 3.376 ? . 5_545 C(7) H(13) 3.441 ? . 5_545 C(7) H(22) 3.472 ? . 1_545 C(7) H(31) 3.573 ? . 2_655 C(7) H(31) 3.397 ? . 5_545 C(8) H(2) 3.309 ? . 5_545 C(8) H(22) 2.737 ? . 1_545 C(9) H(21) 3.252 ? . 1_545 C(9) H(22) 3.075 ? . 1_545 C(11) H(13) 3.137 ? . 5_545 C(11) H(14) 3.533 ? . 5_545 C(12) H(2) 3.425 ? . 5_545 C(12) H(3) 3.377 ? . 5_545 C(12) H(13) 2.815 ? . 5_545 C(12) H(31) 3.509 ? . 5_545 C(13) H(1) 3.313 ? . 5_555 C(13) H(24) 2.983 ? . 5_555 C(16) H(30) 3.183 ? . . C(17) H(7) 3.403 ? . 5_555 C(17) H(27) 3.536 ? . 5_455 C(18) H(6) 3.372 ? . 5_555 C(18) H(7) 3.103 ? . 5_555 C(18) H(28) 3.344 ? . 5_455 C(18) H(33) 3.552 ? . 5_455 C(19) H(2) 3.498 ? . 5_555 C(19) H(6) 2.932 ? . 5_555 C(19) H(11) 3.599 ? . 1_565 C(19) H(28) 3.496 ? . 5_455 C(20) H(1) 3.269 ? . 5_555 C(20) H(2) 2.905 ? . 5_555 C(20) H(6) 3.255 ? . 5_555 C(20) H(10) 3.427 ? . 1_565 C(21) H(1) 3.461 ? . 5_555 C(22) H(7) 3.447 ? . 5_555 C(23) H(7) 2.993 ? . 5_555 C(24) H(14) 3.051 ? . 5_545 C(24) H(28) 3.289 ? . 5_445 C(24) H(29) 3.419 ? . 5_445 C(25) H(7) 3.589 ? . 1_455 C(25) H(17) 2.853 ? . . C(25) H(18) 2.978 ? . . C(25) H(19) 3.119 ? . 5_445 C(25) H(20) 2.911 ? . 5_445 C(26) H(18) 3.093 ? . . C(26) H(20) 3.295 ? . 5_445 C(26) H(25) 2.939 ? . 5_455 C(27) H(8) 3.060 ? . 5_555 C(27) H(9) 3.570 ? . 4_464 C(27) H(9) 3.456 ? . 5_555 C(27) H(20) 2.947 ? . 5_445 C(27) H(33) 3.324 ? . 6_465 H(1) O(2) 3.548 ? . 8_665 H(1) C(13) 3.313 ? . 5_545 H(1) C(20) 3.269 ? . 5_545 H(1) C(21) 3.461 ? . 5_545 H(1) H(13) 3.327 ? . 5_545 H(1) H(14) 3.138 ? . 5_545 H(1) H(15) 2.929 ? . 5_545 H(1) H(22) 3.119 ? . 5_545 H(1) H(23) 3.465 ? . 5_545 H(2) O(2) 3.336 ? . 8_665 H(2) C(7) 3.046 ? . 5_555 H(2) C(8) 3.309 ? . 5_555 H(2) C(12) 3.425 ? . 5_555 H(2) C(19) 3.498 ? . 5_545 H(2) C(20) 2.905 ? . 5_545 H(2) H(9) 3.161 ? . 5_555 H(2) H(10) 3.595 ? . 5_555 H(2) H(21) 3.495 ? . 5_545 H(2) H(22) 2.411 ? . 5_545 H(3) C(6) 3.091 ? . 5_555 H(3) C(7) 3.376 ? . 5_555 H(3) C(12) 3.377 ? . 5_555 H(3) H(8) 2.743 ? . 5_555 H(3) H(9) 3.069 ? . 5_555 H(4) Cl(1) 3.045 ? . 8_665 H(4) O(2) 2.957 ? . 8_665 H(4) O(3) 2.622 ? . 8_665 H(4) O(5) 3.000 ? . 8_665 H(4) H(9) 3.080 ? . 5_555 H(4) H(27) 3.217 ? . . H(5) O(5) 2.532 ? . 4_464 H(5) H(28) 3.338 ? . 1_655 H(5) H(30) 3.503 ? . 1_655 H(6) C(18) 3.372 ? . 5_545 H(6) C(19) 2.932 ? . 5_545 H(6) C(20) 3.255 ? . 5_545 H(6) H(21) 2.974 ? . 5_545 H(6) H(22) 3.487 ? . 5_545 H(6) H(28) 2.994 ? . 1_655 H(7) O(6) 2.863 ? . 1_655 H(7) C(17) 3.403 ? . 5_545 H(7) C(18) 3.103 ? . 5_545 H(7) C(22) 3.447 ? . 5_545 H(7) C(23) 2.993 ? . 5_545 H(7) C(25) 3.589 ? . 1_655 H(7) H(20) 3.361 ? . 5_545 H(8) N(5) 3.543 ? . 5_545 H(8) C(27) 3.060 ? . 5_545 H(8) H(3) 2.743 ? . 5_545 H(8) H(13) 3.204 ? . 5_545 H(8) H(31) 2.113 ? . 5_545 H(8) H(32) 3.590 ? . 5_545 H(8) H(33) 3.587 ? . 5_545 H(9) Cl(1) 3.567 ? . 4_454 H(9) O(2) 3.138 ? . 4_454 H(9) O(3) 2.886 ? . 4_454 H(9) C(2) 3.433 ? . 5_545 H(9) C(27) 3.570 ? . 2_655 H(9) C(27) 3.456 ? . 5_545 H(9) H(2) 3.161 ? . 5_545 H(9) H(3) 3.069 ? . 5_545 H(9) H(4) 3.080 ? . 5_545 H(9) H(31) 3.290 ? . 2_655 H(9) H(31) 2.763 ? . 5_545 H(9) H(32) 3.152 ? . 2_655 H(9) H(33) 3.263 ? . 5_545 H(10) O(2) 2.856 ? . 4_454 H(10) O(6) 3.257 ? . 8_655 H(10) C(20) 3.427 ? . 1_545 H(10) H(2) 3.595 ? . 5_545 H(10) H(16) 3.353 ? . 8_655 H(10) H(17) 3.568 ? . 8_655 H(10) H(22) 2.547 ? . 1_545 H(10) H(31) 3.334 ? . 2_655 H(10) H(32) 3.116 ? . 2_655 H(11) O(4) 3.187 ? . 7_465 H(11) O(5) 3.409 ? . 7_465 H(11) O(6) 2.997 ? . 8_655 H(11) C(19) 3.599 ? . 1_545 H(11) H(18) 3.144 ? . 8_655 H(11) H(21) 3.057 ? . 1_545 H(11) H(22) 3.117 ? . 1_545 H(11) H(30) 3.060 ? . 8_655 H(12) O(4) 2.970 ? . 7_465 H(12) O(5) 3.416 ? . 7_465 H(13) N(3) 3.467 ? . 5_555 H(13) C(4) 3.467 ? . 5_555 H(13) C(5) 3.183 ? . 5_555 H(13) C(6) 2.844 ? . 5_555 H(13) C(7) 3.441 ? . 5_555 H(13) C(11) 3.137 ? . 5_555 H(13) C(12) 2.815 ? . 5_555 H(13) H(1) 3.327 ? . 5_555 H(13) H(8) 3.204 ? . 5_555 H(13) H(24) 3.296 ? . 5_555 H(14) O(5) 3.162 ? . 4_464 H(14) C(11) 3.533 ? . 5_555 H(14) C(24) 3.051 ? . 5_555 H(14) H(1) 3.138 ? . 5_555 H(14) H(24) 2.188 ? . 5_555 H(14) H(25) 3.402 ? . 5_555 H(14) H(26) 3.232 ? . 5_555 H(14) H(28) 3.579 ? . 1_655 H(15) O(2) 3.318 ? . 4_464 H(15) O(5) 3.149 ? . 4_464 H(15) H(1) 2.929 ? . 5_555 H(15) H(24) 3.096 ? . 5_555 H(16) O(2) 2.863 ? . 7_465 H(16) H(10) 3.353 ? . 8_565 H(17) O(6) 2.668 ? . . H(17) C(25) 2.853 ? . . H(17) H(10) 3.568 ? . 8_565 H(17) H(27) 2.784 ? . . H(17) H(29) 3.359 ? . 5_445 H(18) O(6) 2.727 ? . . H(18) N(5) 3.148 ? . . H(18) C(25) 2.978 ? . . H(18) C(26) 3.093 ? . . H(18) H(11) 3.144 ? . 8_565 H(18) H(27) 3.574 ? . . H(18) H(29) 3.374 ? . . H(18) H(30) 2.409 ? . . H(19) O(3) 3.179 ? . 4_364 H(19) O(6) 3.433 ? . 5_455 H(19) C(25) 3.119 ? . 5_455 H(19) H(27) 2.704 ? . 5_455 H(19) H(29) 3.465 ? . . H(19) H(30) 3.276 ? . . H(19) H(33) 3.421 ? . 5_455 H(20) O(4) 3.526 ? . 7_475 H(20) O(6) 3.464 ? . 5_455 H(20) N(5) 2.773 ? . 5_455 H(20) C(25) 2.911 ? . 5_455 H(20) C(26) 3.295 ? . 5_455 H(20) C(27) 2.947 ? . 5_455 H(20) H(7) 3.361 ? . 5_555 H(20) H(27) 3.106 ? . 5_455 H(20) H(28) 2.824 ? . 5_455 H(20) H(32) 2.977 ? . 5_455 H(20) H(33) 2.622 ? . 5_455 H(21) O(4) 2.569 ? . 7_475 H(21) C(9) 3.252 ? . 1_565 H(21) H(2) 3.495 ? . 5_555 H(21) H(6) 2.974 ? . 5_555 H(21) H(11) 3.057 ? . 1_565 H(21) H(26) 3.511 ? . 1_565 H(21) H(28) 3.116 ? . 5_455 H(22) O(2) 2.829 ? . 4_464 H(22) C(1) 3.197 ? . 5_555 H(22) C(7) 3.472 ? . 1_565 H(22) C(8) 2.737 ? . 1_565 H(22) C(9) 3.075 ? . 1_565 H(22) H(1) 3.119 ? . 5_555 H(22) H(2) 2.411 ? . 5_555 H(22) H(6) 3.487 ? . 5_555 H(22) H(10) 2.547 ? . 1_565 H(22) H(11) 3.117 ? . 1_565 H(23) O(2) 2.801 ? . 4_464 H(23) H(1) 3.465 ? . 5_555 H(24) O(5) 3.157 ? . 8_665 H(24) C(13) 2.983 ? . 5_545 H(24) H(13) 3.296 ? . 5_545 H(24) H(14) 2.188 ? . 5_545 H(24) H(15) 3.096 ? . 5_545 H(24) H(28) 3.298 ? . 5_445 H(25) O(4) 3.193 ? . 7_465 H(25) O(5) 3.486 ? . 8_665 H(25) C(26) 2.939 ? . 5_445 H(25) H(14) 3.402 ? . 5_545 H(25) H(28) 2.559 ? . 5_445 H(25) H(29) 2.464 ? . 5_445 H(25) H(30) 3.492 ? . 5_445 H(26) O(4) 2.713 ? . 7_465 H(26) H(14) 3.232 ? . 5_545 H(26) H(21) 3.511 ? . 1_545 H(26) H(28) 3.576 ? . 5_445 H(27) O(3) 2.413 ? . 8_665 H(27) C(17) 3.536 ? . 5_445 H(27) H(4) 3.217 ? . . H(27) H(17) 2.784 ? . . H(27) H(18) 3.574 ? . . H(27) H(19) 2.704 ? . 5_445 H(27) H(20) 3.106 ? . 5_445 H(27) H(29) 3.439 ? . 5_445 H(28) O(5) 3.213 ? . 4_364 H(28) C(18) 3.344 ? . 5_445 H(28) C(19) 3.496 ? . 5_445 H(28) C(24) 3.289 ? . 5_455 H(28) H(5) 3.338 ? . 1_455 H(28) H(6) 2.994 ? . 1_455 H(28) H(14) 3.579 ? . 1_455 H(28) H(20) 2.824 ? . 5_445 H(28) H(21) 3.116 ? . 5_445 H(28) H(24) 3.298 ? . 5_455 H(28) H(25) 2.559 ? . 5_455 H(28) H(26) 3.576 ? . 5_455 H(29) O(5) 3.432 ? . 4_364 H(29) O(6) 3.459 ? . 5_455 H(29) C(24) 3.419 ? . 5_455 H(29) H(17) 3.359 ? . 5_455 H(29) H(18) 3.374 ? . . H(29) H(19) 3.465 ? . . H(29) H(25) 2.464 ? . 5_455 H(29) H(27) 3.439 ? . 5_455 H(30) O(5) 2.809 ? . 4_364 H(30) C(16) 3.183 ? . . H(30) H(5) 3.503 ? . 1_455 H(30) H(11) 3.060 ? . 8_565 H(30) H(18) 2.409 ? . . H(30) H(19) 3.276 ? . . H(30) H(25) 3.492 ? . 5_455 H(31) C(6) 2.899 ? . 5_555 H(31) C(7) 3.573 ? . 4_464 H(31) C(7) 3.397 ? . 5_555 H(31) C(12) 3.509 ? . 5_555 H(31) H(8) 2.113 ? . 5_555 H(31) H(9) 3.290 ? . 4_464 H(31) H(9) 2.763 ? . 5_555 H(31) H(10) 3.334 ? . 4_464 H(31) H(33) 3.578 ? . 6_465 H(32) Cl(1) 3.236 ? . 3_574 H(32) O(2) 3.395 ? . 3_574 H(32) O(3) 2.993 ? . 3_574 H(32) O(4) 2.997 ? . 3_574 H(32) H(8) 3.590 ? . 5_555 H(32) H(9) 3.152 ? . 4_464 H(32) H(10) 3.116 ? . 4_464 H(32) H(20) 2.977 ? . 5_445 H(32) H(33) 3.368 ? . 6_465 H(33) O(3) 3.590 ? . 3_574 H(33) O(3) 2.880 ? . 8_665 H(33) C(18) 3.552 ? . 5_445 H(33) C(27) 3.324 ? . 6_465 H(33) H(8) 3.587 ? . 5_555 H(33) H(9) 3.263 ? . 5_555 H(33) H(19) 3.421 ? . 5_445 H(33) H(20) 2.622 ? . 5_445 H(33) H(31) 3.578 ? . 6_465 H(33) H(32) 3.368 ? . 6_465 H(33) H(33) 2.584 ? . 6_465 Mn(1) O(1) 1.8251(19) ? . 8_665 Mn(1) Mn(1) 2.6649(5) ? . 8_665 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== # Attachment 'B705080A-cif-2.txt' data_etmn10 _database_code_depnum_ccdc_archive 'CCDC 297399' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H62 Cl2 Mn2 N8 O11' _chemical_formula_weight 1155.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 16.018(6) _cell_length_b 21.574(7) _cell_length_c 17.179(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.4191(11) _cell_angle_gamma 90.00 _cell_volume 5488(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8351 _exptl_absorpt_correction_T_max 0.8855 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40797 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9395 _reflns_number_gt 8327 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1142P)^2^+10.4545P] 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 9395 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.2285 _refine_ls_wR_factor_gt 0.2164 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _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 0.20540(4) 0.05512(3) 0.24091(4) 0.0303(2) Uani 1 1 d . . . Mn2 Mn 0.29940(4) -0.04961(3) 0.25862(4) 0.0288(2) Uani 1 1 d . . . Cl1 Cl 0.50889(10) -0.20572(6) 0.09341(9) 0.0553(4) Uani 1 1 d . . . Cl2 Cl 0.41039(11) -0.27141(7) 0.48087(11) 0.0648(4) Uani 1 1 d . . . O1 O 0.19644(19) -0.01602(13) 0.18087(17) 0.0309(6) Uani 1 1 d . . . O2 O 0.30808(19) 0.02192(13) 0.31828(17) 0.0311(6) Uani 1 1 d . . . O3 O 0.4554(3) -0.1525(2) 0.0622(4) 0.101(2) Uani 1 1 d . . . O4 O 0.6006(3) -0.1864(2) 0.1376(4) 0.0828(14) Uani 1 1 d . . . O5 O 0.5078(4) -0.2459(3) 0.0292(4) 0.114(2) Uani 1 1 d . . . O6 O 0.4766(4) -0.2367(2) 0.1487(3) 0.0774(13) Uani 1 1 d . . . O7 O 0.4572(6) -0.2903(3) 0.5664(4) 0.146(3) Uani 1 1 d . . . O8 O 0.3556(6) -0.3182(4) 0.4388(4) 0.144(3) Uani 1 1 d . . . O9 O 0.4713(4) -0.2498(3) 0.4464(5) 0.123(3) Uani 1 1 d . . . O10 O 0.3570(4) -0.2192(3) 0.4830(5) 0.112(2) Uani 1 1 d . . . N1 N 0.1077(3) 0.10790(16) 0.1408(2) 0.0372(9) Uani 1 1 d . . . N2 N 0.1874(3) 0.12976(16) 0.3169(2) 0.0362(8) Uani 1 1 d . . . N3 N 0.2900(3) 0.11984(16) 0.1807(2) 0.0354(8) Uani 1 1 d . . . N4 N 0.0943(2) 0.01995(16) 0.2970(2) 0.0343(8) Uani 1 1 d . . . N5 N 0.4348(3) -0.08093(16) 0.3274(2) 0.0346(8) Uani 1 1 d . . . N6 N 0.2805(2) -0.14335(16) 0.2126(2) 0.0325(8) Uani 1 1 d . . . N7 N 0.3878(3) -0.01965(16) 0.1763(2) 0.0348(8) Uani 1 1 d . . . N8 N 0.2336(2) -0.10677(16) 0.3433(2) 0.0330(8) Uani 1 1 d . . . C1 C 0.1011(3) 0.1704(2) 0.1764(3) 0.0416(11) Uani 1 1 d . . . H1 H 0.1516 0.1970 0.1766 0.050 Uiso 1 1 calc R . . H2 H 0.0438 0.1906 0.1408 0.050 Uiso 1 1 calc R . . C2 C 0.1046(3) 0.1638(2) 0.2638(3) 0.0420(11) Uani 1 1 d . . . H3 H 0.1043 0.2053 0.2882 0.050 Uiso 1 1 calc R . . H4 H 0.0506 0.1410 0.2629 0.050 Uiso 1 1 calc R . . C3 C 0.1404(4) 0.1149(2) 0.0719(3) 0.0451(12) Uani 1 1 d . . . H5 H 0.1036 0.1468 0.0322 0.054 Uiso 1 1 calc R . . H6 H 0.1318 0.0753 0.0408 0.054 Uiso 1 1 calc R . . C4 C 0.2381(4) 0.1331(2) 0.1019(3) 0.0414(11) Uani 1 1 d . . . C5 C 0.2692(4) 0.1619(2) 0.0451(3) 0.0506(13) Uani 1 1 d . . . H7 H 0.2287 0.1705 -0.0108 0.061 Uiso 1 1 calc R . . C6 C 0.3576(4) 0.1772(2) 0.0704(4) 0.0572(14) Uani 1 1 d . . . H8 H 0.3798 0.1965 0.0324 0.069 Uiso 1 1 calc R . . C7 C 0.5099(4) 0.1782(2) 0.1844(4) 0.0617(16) Uani 1 1 d . . . H9 H 0.5352 0.1964 0.1479 0.074 Uiso 1 1 calc R . . C8 C 0.5636(4) 0.1657(2) 0.2656(4) 0.0610(16) Uani 1 1 d . . . H10 H 0.6259 0.1761 0.2861 0.073 Uiso 1 1 calc R . . C9 C 0.5275(4) 0.1376(2) 0.3191(4) 0.0529(13) Uani 1 1 d . . . H11 H 0.5656 0.1296 0.3760 0.063 Uiso 1 1 calc R . . C10 C 0.4383(3) 0.1215(2) 0.2909(3) 0.0435(11) Uani 1 1 d . . . H12 H 0.4154 0.1012 0.3277 0.052 Uiso 1 1 calc R . . C11 C 0.3801(3) 0.13488(19) 0.2070(3) 0.0392(10) Uani 1 1 d . . . C12 C 0.4160(4) 0.1642(2) 0.1536(4) 0.0481(12) Uani 1 1 d . . . C13 C 0.0185(3) 0.0761(2) 0.1083(3) 0.0481(12) Uani 1 1 d . . . H13 H -0.0046 0.0750 0.1541 0.058 Uiso 1 1 calc R . . H14 H 0.0281 0.0327 0.0950 0.058 Uiso 1 1 calc R . . C14 C -0.0534(4) 0.1039(3) 0.0319(4) 0.0676(18) Uani 1 1 d . . . H15 H -0.0646 0.1468 0.0440 0.101 Uiso 1 1 calc R . . H16 H -0.1091 0.0798 0.0172 0.101 Uiso 1 1 calc R . . H17 H -0.0333 0.1032 -0.0153 0.101 Uiso 1 1 calc R . . C15 C 0.1741(3) 0.1020(2) 0.3899(3) 0.0394(10) Uani 1 1 d . . . H18 H 0.1564 0.1349 0.4208 0.047 Uiso 1 1 calc R . . H19 H 0.2319 0.0840 0.4286 0.047 Uiso 1 1 calc R . . C16 C 0.1035(3) 0.0528(2) 0.3640(3) 0.0394(11) Uani 1 1 d . . . C17 C 0.0504(4) 0.0436(2) 0.4117(3) 0.0492(12) Uani 1 1 d . . . H20 H 0.0589 0.0690 0.4593 0.059 Uiso 1 1 calc R . . C18 C -0.0133(4) -0.0018(3) 0.3895(4) 0.0540(13) Uani 1 1 d . . . H21 H -0.0491 -0.0085 0.4218 0.065 Uiso 1 1 calc R . . C19 C -0.0902(4) -0.0868(3) 0.2910(4) 0.0562(14) Uani 1 1 d . . . H22 H -0.1281 -0.0949 0.3210 0.067 Uiso 1 1 calc R . . C20 C -0.0984(4) -0.1211(3) 0.2232(4) 0.0556(14) Uani 1 1 d . . . H23 H -0.1424 -0.1531 0.2053 0.067 Uiso 1 1 calc R . . C21 C -0.0421(4) -0.1101(2) 0.1785(3) 0.0480(12) Uani 1 1 d . . . H24 H -0.0487 -0.1349 0.1308 0.058 Uiso 1 1 calc R . . C22 C 0.0219(3) -0.0641(2) 0.2025(3) 0.0406(11) Uani 1 1 d . . . H25 H 0.0598 -0.0573 0.1722 0.049 Uiso 1 1 calc R . . C23 C 0.0307(3) -0.0268(2) 0.2735(3) 0.0374(10) Uani 1 1 d . . . C24 C -0.0260(3) -0.0391(2) 0.3178(3) 0.0457(12) Uani 1 1 d . . . C25 C 0.2675(3) 0.1713(2) 0.3475(3) 0.0414(11) Uani 1 1 d . . . H26 H 0.2717 0.1924 0.2980 0.050 Uiso 1 1 calc R . . H27 H 0.3219 0.1450 0.3723 0.050 Uiso 1 1 calc R . . C26 C 0.2710(4) 0.2208(2) 0.4119(4) 0.0555(14) Uani 1 1 d . . . H28 H 0.2166 0.2465 0.3896 0.083 Uiso 1 1 calc R . . H29 H 0.3246 0.2467 0.4232 0.083 Uiso 1 1 calc R . . H30 H 0.2741 0.2009 0.4642 0.083 Uiso 1 1 calc R . . C27 C 0.4445(3) -0.1418(2) 0.2899(3) 0.0388(10) Uani 1 1 d . . . H31 H 0.4557 -0.1347 0.2378 0.047 Uiso 1 1 calc R . . H32 H 0.4966 -0.1648 0.3301 0.047 Uiso 1 1 calc R . . C28 C 0.3602(3) -0.17894(19) 0.2702(3) 0.0380(10) Uani 1 1 d . . . H33 H 0.3655 -0.2185 0.2432 0.046 Uiso 1 1 calc R . . H34 H 0.3516 -0.1888 0.3230 0.046 Uiso 1 1 calc R . . C29 C 0.4994(3) -0.0363(2) 0.3160(3) 0.0394(10) Uani 1 1 d . . . H35 H 0.5598 -0.0559 0.3345 0.047 Uiso 1 1 calc R . . H36 H 0.5042 0.0003 0.3523 0.047 Uiso 1 1 calc R . . C30 C 0.4722(3) -0.0152(2) 0.2267(3) 0.0384(10) Uani 1 1 d . . . C31 C 0.5401(3) 0.0112(2) 0.2023(4) 0.0453(12) Uani 1 1 d . . . H37 H 0.6011 0.0130 0.2409 0.054 Uiso 1 1 calc R . . C32 C 0.5163(4) 0.0337(2) 0.1228(4) 0.0477(12) Uani 1 1 d . . . H38 H 0.5602 0.0527 0.1059 0.057 Uiso 1 1 calc R . . C33 C 0.3968(4) 0.0500(2) -0.0183(4) 0.0534(14) Uani 1 1 d . . . H39 H 0.4388 0.0692 -0.0374 0.064 Uiso 1 1 calc R . . C34 C 0.3092(5) 0.0434(3) -0.0720(4) 0.0568(15) Uani 1 1 d . . . H40 H 0.2906 0.0570 -0.1287 0.068 Uiso 1 1 calc R . . C35 C 0.2470(4) 0.0166(2) -0.0436(3) 0.0482(12) Uani 1 1 d . . . H41 H 0.1861 0.0119 -0.0816 0.058 Uiso 1 1 calc R . . C36 C 0.2719(3) -0.0033(2) 0.0386(3) 0.0405(11) Uani 1 1 d . . . H42 H 0.2279 -0.0202 0.0572 0.049 Uiso 1 1 calc R . . C37 C 0.3622(3) 0.00141(19) 0.0945(3) 0.0372(10) Uani 1 1 d . . . C38 C 0.4259(4) 0.0286(2) 0.0659(3) 0.0430(11) Uani 1 1 d . . . C39 C 0.4528(3) -0.0865(2) 0.4185(3) 0.0421(11) Uani 1 1 d . . . H43 H 0.4122 -0.1187 0.4255 0.051 Uiso 1 1 calc R . . H44 H 0.4363 -0.0467 0.4377 0.051 Uiso 1 1 calc R . . C40 C 0.5489(4) -0.1024(3) 0.4762(3) 0.0570(14) Uani 1 1 d . . . H45 H 0.5657 -0.1426 0.4599 0.085 Uiso 1 1 calc R . . H46 H 0.5530 -0.1046 0.5346 0.085 Uiso 1 1 calc R . . H47 H 0.5901 -0.0704 0.4716 0.085 Uiso 1 1 calc R . . C41 C 0.1979(3) -0.1680(2) 0.2184(3) 0.0377(10) Uani 1 1 d . . . H48 H 0.1966 -0.2135 0.2105 0.045 Uiso 1 1 calc R . . H49 H 0.1451 -0.1504 0.1720 0.045 Uiso 1 1 calc R . . C42 C 0.1890(3) -0.1543(2) 0.2998(3) 0.0358(10) Uani 1 1 d . . . C43 C 0.1319(3) -0.1919(2) 0.3254(3) 0.0442(11) Uani 1 1 d . . . H50 H 0.1003 -0.2258 0.2915 0.053 Uiso 1 1 calc R . . C44 C 0.1227(4) -0.1793(2) 0.3987(3) 0.0475(12) Uani 1 1 d . . . H51 H 0.0843 -0.2040 0.4164 0.057 Uiso 1 1 calc R . . C45 C 0.1651(4) -0.1144(3) 0.5268(3) 0.0509(13) Uani 1 1 d . . . H52 H 0.1285 -0.1387 0.5475 0.061 Uiso 1 1 calc R . . C46 C 0.2114(4) -0.0662(3) 0.5724(3) 0.0522(13) Uani 1 1 d . . . H53 H 0.2084 -0.0572 0.6254 0.063 Uiso 1 1 calc R . . C47 C 0.2646(3) -0.0290(2) 0.5419(3) 0.0447(11) Uani 1 1 d . . . H54 H 0.2958 0.0057 0.5739 0.054 Uiso 1 1 calc R . . C48 C 0.2720(3) -0.0423(2) 0.4665(3) 0.0403(11) Uani 1 1 d . . . H55 H 0.3083 -0.0170 0.4466 0.048 Uiso 1 1 calc R . . C49 C 0.2256(3) -0.0933(2) 0.4189(3) 0.0355(10) Uani 1 1 d . . . C50 C 0.1698(3) -0.1296(2) 0.4484(3) 0.0413(11) Uani 1 1 d . . . C51 C 0.2737(3) -0.1466(2) 0.1236(3) 0.0375(10) Uani 1 1 d . . . H56 H 0.3318 -0.1324 0.1220 0.045 Uiso 1 1 calc R . . H57 H 0.2267 -0.1169 0.0898 0.045 Uiso 1 1 calc R . . C52 C 0.2518(4) -0.2092(2) 0.0817(3) 0.0494(12) Uani 1 1 d . . . H58 H 0.3001 -0.2385 0.1116 0.074 Uiso 1 1 calc R . . H59 H 0.2463 -0.2056 0.0231 0.074 Uiso 1 1 calc R . . H60 H 0.1946 -0.2242 0.0831 0.074 Uiso 1 1 calc R . . O11 O 0.6836(4) -0.1246(3) 0.3164(5) 0.120(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 Mn1 0.0346(4) 0.0234(3) 0.0249(4) 0.0000(2) 0.0023(3) 0.0037(2) Mn2 0.0302(4) 0.0237(3) 0.0257(4) -0.0013(2) 0.0030(3) 0.0015(2) Cl1 0.0543(8) 0.0514(7) 0.0685(9) 0.0158(6) 0.0327(7) 0.0131(6) Cl2 0.0599(9) 0.0600(9) 0.0788(10) 0.0276(8) 0.0313(8) 0.0098(7) O1 0.0305(15) 0.0310(15) 0.0247(14) -0.0013(11) 0.0033(12) 0.0021(12) O2 0.0312(15) 0.0284(14) 0.0255(14) -0.0021(11) 0.0017(12) 0.0015(12) O3 0.071(3) 0.087(3) 0.155(5) 0.069(4) 0.053(3) 0.031(3) O4 0.057(3) 0.067(3) 0.118(4) 0.011(3) 0.025(3) 0.005(2) O5 0.108(5) 0.154(6) 0.098(4) -0.050(4) 0.058(4) -0.010(4) O6 0.093(3) 0.069(3) 0.090(3) 0.025(2) 0.057(3) 0.007(2) O7 0.152(7) 0.132(6) 0.105(5) 0.064(4) -0.006(4) -0.036(5) O8 0.184(8) 0.143(6) 0.104(5) -0.056(5) 0.053(5) -0.059(6) O9 0.100(4) 0.117(5) 0.200(7) 0.080(5) 0.109(5) 0.044(4) O10 0.109(5) 0.094(4) 0.160(6) 0.020(4) 0.082(5) 0.029(3) N1 0.039(2) 0.0276(18) 0.034(2) 0.0022(15) 0.0021(17) 0.0034(15) N2 0.040(2) 0.0277(18) 0.034(2) -0.0008(15) 0.0063(17) 0.0083(15) N3 0.040(2) 0.0259(17) 0.035(2) 0.0027(15) 0.0081(17) -0.0005(15) N4 0.034(2) 0.0315(18) 0.0332(19) -0.0013(15) 0.0079(16) 0.0055(15) N5 0.038(2) 0.0291(18) 0.0305(19) -0.0018(14) 0.0057(16) 0.0002(15) N6 0.0306(19) 0.0278(17) 0.0346(19) -0.0019(14) 0.0074(16) -0.0002(14) N7 0.040(2) 0.0257(17) 0.037(2) -0.0030(15) 0.0127(17) -0.0023(15) N8 0.038(2) 0.0265(17) 0.0329(19) 0.0060(15) 0.0123(16) 0.0026(15) C1 0.041(3) 0.029(2) 0.043(3) 0.0013(19) 0.003(2) 0.0062(19) C2 0.042(3) 0.030(2) 0.045(3) 0.0016(19) 0.007(2) 0.0078(19) C3 0.057(3) 0.037(2) 0.030(2) 0.0042(19) 0.004(2) 0.003(2) C4 0.054(3) 0.027(2) 0.038(3) 0.0047(19) 0.011(2) 0.004(2) C5 0.068(4) 0.037(3) 0.043(3) 0.013(2) 0.017(3) 0.006(2) C6 0.075(4) 0.034(3) 0.064(4) 0.017(2) 0.029(3) 0.004(3) C7 0.073(4) 0.030(3) 0.084(4) 0.001(3) 0.032(4) -0.009(2) C8 0.059(3) 0.037(3) 0.086(5) -0.014(3) 0.027(3) -0.017(2) C9 0.046(3) 0.044(3) 0.058(3) -0.016(2) 0.008(3) -0.004(2) C10 0.045(3) 0.035(2) 0.042(3) -0.007(2) 0.007(2) -0.001(2) C11 0.048(3) 0.021(2) 0.046(3) -0.0029(18) 0.015(2) -0.0030(18) C12 0.061(3) 0.025(2) 0.062(3) 0.002(2) 0.028(3) -0.003(2) C13 0.042(3) 0.042(3) 0.043(3) 0.007(2) -0.004(2) 0.000(2) C14 0.053(4) 0.063(4) 0.059(4) 0.015(3) -0.011(3) -0.004(3) C15 0.050(3) 0.031(2) 0.034(2) -0.0032(18) 0.013(2) 0.005(2) C16 0.046(3) 0.034(2) 0.034(2) 0.0043(18) 0.011(2) 0.0067(19) C17 0.056(3) 0.053(3) 0.038(3) 0.001(2) 0.017(2) 0.001(2) C18 0.055(3) 0.061(3) 0.050(3) 0.008(3) 0.024(3) 0.002(3) C19 0.050(3) 0.057(3) 0.059(3) 0.011(3) 0.018(3) -0.004(3) C20 0.055(3) 0.046(3) 0.056(3) 0.007(3) 0.010(3) -0.007(2) C21 0.051(3) 0.039(3) 0.044(3) 0.002(2) 0.006(2) -0.005(2) C22 0.040(3) 0.035(2) 0.037(3) 0.0046(19) 0.004(2) 0.0051(19) C23 0.034(2) 0.033(2) 0.037(2) 0.0061(19) 0.0049(19) 0.0048(18) C24 0.043(3) 0.048(3) 0.047(3) 0.009(2) 0.019(2) 0.004(2) C25 0.044(3) 0.034(2) 0.038(3) -0.0064(19) 0.006(2) -0.002(2) C26 0.058(3) 0.044(3) 0.051(3) -0.015(2) 0.006(3) 0.001(2) C27 0.036(2) 0.032(2) 0.040(2) -0.0017(19) 0.005(2) 0.0058(18) C28 0.041(3) 0.025(2) 0.041(3) 0.0000(18) 0.008(2) 0.0056(18) C29 0.032(2) 0.039(2) 0.041(3) -0.008(2) 0.006(2) -0.0029(19) C30 0.038(3) 0.031(2) 0.041(3) -0.0061(19) 0.009(2) -0.0032(18) C31 0.038(3) 0.039(3) 0.059(3) -0.008(2) 0.019(2) -0.005(2) C32 0.050(3) 0.039(3) 0.065(3) -0.007(2) 0.035(3) -0.008(2) C33 0.071(4) 0.047(3) 0.056(3) 0.006(2) 0.040(3) 0.000(3) C34 0.084(4) 0.052(3) 0.041(3) 0.007(2) 0.031(3) 0.008(3) C35 0.058(3) 0.045(3) 0.037(3) 0.004(2) 0.014(2) 0.004(2) C36 0.050(3) 0.035(2) 0.035(2) 0.0005(19) 0.013(2) 0.000(2) C37 0.049(3) 0.027(2) 0.039(2) -0.0016(18) 0.020(2) -0.0028(19) C38 0.051(3) 0.033(2) 0.049(3) -0.001(2) 0.023(2) -0.004(2) C39 0.040(3) 0.048(3) 0.028(2) 0.0003(19) 0.002(2) 0.004(2) C40 0.051(3) 0.069(4) 0.039(3) 0.005(3) 0.003(2) 0.014(3) C41 0.038(2) 0.026(2) 0.046(3) -0.0008(19) 0.013(2) -0.0045(18) C42 0.035(2) 0.030(2) 0.039(2) 0.0065(18) 0.010(2) 0.0044(18) C43 0.045(3) 0.037(2) 0.050(3) 0.006(2) 0.017(2) -0.004(2) C44 0.047(3) 0.045(3) 0.055(3) 0.017(2) 0.024(3) 0.003(2) C45 0.052(3) 0.062(3) 0.046(3) 0.016(3) 0.027(3) 0.008(3) C46 0.057(3) 0.065(3) 0.036(3) 0.007(2) 0.018(2) 0.020(3) C47 0.047(3) 0.051(3) 0.031(2) -0.001(2) 0.009(2) 0.009(2) C48 0.039(3) 0.037(2) 0.037(3) 0.0047(19) 0.006(2) 0.0081(19) C49 0.039(2) 0.034(2) 0.031(2) 0.0071(18) 0.0097(19) 0.0087(18) C50 0.041(3) 0.039(2) 0.044(3) 0.012(2) 0.017(2) 0.009(2) C51 0.042(3) 0.034(2) 0.032(2) -0.0063(18) 0.010(2) -0.0018(19) C52 0.057(3) 0.042(3) 0.048(3) -0.015(2) 0.019(3) -0.006(2) O11 0.082(4) 0.097(4) 0.172(7) -0.022(4) 0.040(4) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 1.821(3) . ? Mn1 O1 1.824(3) . ? Mn1 N1 2.157(4) . ? Mn1 N2 2.161(4) . ? Mn1 N3 2.434(4) . ? Mn1 N4 2.446(4) . ? Mn1 Mn2 2.6675(11) . ? Mn2 O2 1.828(3) . ? Mn2 O1 1.830(3) . ? Mn2 N5 2.145(4) . ? Mn2 N6 2.150(4) . ? Mn2 N8 2.433(4) . ? Mn2 N7 2.440(4) . ? Cl1 O5 1.397(5) . ? Cl1 O3 1.410(5) . ? Cl1 O6 1.411(4) . ? Cl1 O4 1.435(5) . ? Cl2 O8 1.353(7) . ? Cl2 O9 1.400(5) . ? Cl2 O10 1.423(6) . ? Cl2 O7 1.430(6) . ? N1 C3 1.473(6) . ? N1 C13 1.489(6) . ? N1 C1 1.502(6) . ? N2 C15 1.476(6) . ? N2 C2 1.485(6) . ? N2 C25 1.486(6) . ? N3 C4 1.321(6) . ? N3 C11 1.376(6) . ? N4 C16 1.311(6) . ? N4 C23 1.380(6) . ? N5 C29 1.480(6) . ? N5 C39 1.485(6) . ? N5 C27 1.496(6) . ? N6 C41 1.465(6) . ? N6 C51 1.492(6) . ? N6 C28 1.494(6) . ? N7 C30 1.301(6) . ? N7 C37 1.381(6) . ? N8 C42 1.308(6) . ? N8 C49 1.384(6) . ? C1 C2 1.488(7) . ? C3 C4 1.500(7) . ? C4 C5 1.400(7) . ? C5 C6 1.354(8) . ? C6 C12 1.406(8) . ? C7 C8 1.358(9) . ? C7 C12 1.424(8) . ? C8 C9 1.397(9) . ? C9 C10 1.368(7) . ? C10 C11 1.416(7) . ? C11 C12 1.407(7) . ? C13 C14 1.500(7) . ? C15 C16 1.490(7) . ? C16 C17 1.402(7) . ? C17 C18 1.360(8) . ? C18 C24 1.420(8) . ? C19 C20 1.344(8) . ? C19 C24 1.402(8) . ? C20 C21 1.409(8) . ? C21 C22 1.373(7) . ? C22 C23 1.422(7) . ? C23 C24 1.415(7) . ? C25 C26 1.522(7) . ? C27 C28 1.495(7) . ? C29 C30 1.496(7) . ? C30 C31 1.425(7) . ? C31 C32 1.359(8) . ? C32 C38 1.409(8) . ? C33 C34 1.362(9) . ? C33 C38 1.416(8) . ? C34 C35 1.392(8) . ? C35 C36 1.381(7) . ? C36 C37 1.402(7) . ? C37 C38 1.418(7) . ? C39 C40 1.519(7) . ? C41 C42 1.488(7) . ? C42 C43 1.414(7) . ? C43 C44 1.350(7) . ? C44 C50 1.398(7) . ? C45 C46 1.342(8) . ? C45 C50 1.416(7) . ? C46 C47 1.409(8) . ? C47 C48 1.376(7) . ? C48 C49 1.403(7) . ? C49 C50 1.418(7) . ? C51 C52 1.509(6) . ? 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 O2 Mn1 O1 86.34(12) . . ? O2 Mn1 N1 165.52(15) . . ? O1 Mn1 N1 96.68(13) . . ? O2 Mn1 N2 98.24(13) . . ? O1 Mn1 N2 165.70(15) . . ? N1 Mn1 N2 82.27(14) . . ? O2 Mn1 N3 92.39(13) . . ? O1 Mn1 N3 100.30(13) . . ? N1 Mn1 N3 73.14(14) . . ? N2 Mn1 N3 93.07(14) . . ? O2 Mn1 N4 100.41(13) . . ? O1 Mn1 N4 92.85(13) . . ? N1 Mn1 N4 93.60(14) . . ? N2 Mn1 N4 73.03(14) . . ? N3 Mn1 N4 162.22(12) . . ? O2 Mn1 Mn2 43.14(9) . . ? O1 Mn1 Mn2 43.20(9) . . ? N1 Mn1 Mn2 138.10(10) . . ? N2 Mn1 Mn2 139.63(10) . . ? N3 Mn1 Mn2 98.79(9) . . ? N4 Mn1 Mn2 98.99(9) . . ? O2 Mn2 O1 85.96(12) . . ? O2 Mn2 N5 96.45(13) . . ? O1 Mn2 N5 165.27(14) . . ? O2 Mn2 N6 165.92(14) . . ? O1 Mn2 N6 98.22(13) . . ? N5 Mn2 N6 82.93(13) . . ? O2 Mn2 N8 92.87(13) . . ? O1 Mn2 N8 99.32(13) . . ? N5 Mn2 N8 95.08(13) . . ? N6 Mn2 N8 73.22(13) . . ? O2 Mn2 N7 99.47(13) . . ? O1 Mn2 N7 91.89(13) . . ? N5 Mn2 N7 73.38(14) . . ? N6 Mn2 N7 93.85(13) . . ? N8 Mn2 N7 163.89(12) . . ? O2 Mn2 Mn1 42.94(9) . . ? O1 Mn2 Mn1 43.02(9) . . ? N5 Mn2 Mn1 137.54(10) . . ? N6 Mn2 Mn1 139.52(10) . . ? N8 Mn2 Mn1 98.23(9) . . ? N7 Mn2 Mn1 97.86(9) . . ? O5 Cl1 O3 112.5(4) . . ? O5 Cl1 O6 109.9(4) . . ? O3 Cl1 O6 108.4(3) . . ? O5 Cl1 O4 107.5(4) . . ? O3 Cl1 O4 108.4(3) . . ? O6 Cl1 O4 110.3(3) . . ? O8 Cl2 O9 116.0(5) . . ? O8 Cl2 O10 109.3(5) . . ? O9 Cl2 O10 105.6(4) . . ? O8 Cl2 O7 108.4(5) . . ? O9 Cl2 O7 110.6(5) . . ? O10 Cl2 O7 106.5(5) . . ? Mn1 O1 Mn2 93.78(13) . . ? Mn1 O2 Mn2 93.92(13) . . ? C3 N1 C13 109.4(4) . . ? C3 N1 C1 109.7(4) . . ? C13 N1 C1 111.0(4) . . ? C3 N1 Mn1 108.9(3) . . ? C13 N1 Mn1 110.9(3) . . ? C1 N1 Mn1 106.9(3) . . ? C15 N2 C2 109.7(4) . . ? C15 N2 C25 109.2(4) . . ? C2 N2 C25 111.5(4) . . ? C15 N2 Mn1 107.9(3) . . ? C2 N2 Mn1 106.9(3) . . ? C25 N2 Mn1 111.5(3) . . ? C4 N3 C11 117.2(4) . . ? C4 N3 Mn1 108.9(3) . . ? C11 N3 Mn1 132.8(3) . . ? C16 N4 C23 118.5(4) . . ? C16 N4 Mn1 108.8(3) . . ? C23 N4 Mn1 132.7(3) . . ? C29 N5 C39 109.1(3) . . ? C29 N5 C27 108.8(4) . . ? C39 N5 C27 111.9(4) . . ? C29 N5 Mn2 109.5(3) . . ? C39 N5 Mn2 110.8(3) . . ? C27 N5 Mn2 106.8(3) . . ? C41 N6 C51 109.8(3) . . ? C41 N6 C28 109.5(3) . . ? C51 N6 C28 111.5(3) . . ? C41 N6 Mn2 108.7(3) . . ? C51 N6 Mn2 111.4(3) . . ? C28 N6 Mn2 106.0(2) . . ? C30 N7 C37 118.9(4) . . ? C30 N7 Mn2 108.6(3) . . ? C37 N7 Mn2 131.6(3) . . ? C42 N8 C49 118.3(4) . . ? C42 N8 Mn2 108.8(3) . . ? C49 N8 Mn2 132.2(3) . . ? C2 C1 N1 110.1(4) . . ? N2 C2 C1 110.4(4) . . ? N1 C3 C4 113.2(4) . . ? N3 C4 C5 123.9(5) . . ? N3 C4 C3 117.5(4) . . ? C5 C4 C3 118.6(4) . . ? C6 C5 C4 119.4(5) . . ? C5 C6 C12 119.2(5) . . ? C8 C7 C12 120.3(6) . . ? C7 C8 C9 120.2(6) . . ? C10 C9 C8 121.1(6) . . ? C9 C10 C11 120.1(5) . . ? N3 C11 C12 122.0(4) . . ? N3 C11 C10 119.2(4) . . ? C12 C11 C10 118.8(5) . . ? C6 C12 C11 118.3(5) . . ? C6 C12 C7 122.4(5) . . ? C11 C12 C7 119.4(5) . . ? N1 C13 C14 116.8(4) . . ? N2 C15 C16 112.0(4) . . ? N4 C16 C17 123.0(5) . . ? N4 C16 C15 117.8(4) . . ? C17 C16 C15 119.2(4) . . ? C18 C17 C16 119.8(5) . . ? C17 C18 C24 119.7(5) . . ? C20 C19 C24 120.4(6) . . ? C19 C20 C21 120.5(5) . . ? C22 C21 C20 121.2(5) . . ? C21 C22 C23 119.0(5) . . ? N4 C23 C24 122.2(4) . . ? N4 C23 C22 119.1(4) . . ? C24 C23 C22 118.7(4) . . ? C19 C24 C23 120.1(5) . . ? C19 C24 C18 123.0(5) . . ? C23 C24 C18 116.8(5) . . ? N2 C25 C26 117.9(4) . . ? C28 C27 N5 109.6(4) . . ? N6 C28 C27 110.1(4) . . ? N5 C29 C30 112.8(4) . . ? N7 C30 C31 123.2(5) . . ? N7 C30 C29 118.9(4) . . ? C31 C30 C29 117.8(4) . . ? C32 C31 C30 119.1(5) . . ? C31 C32 C38 119.3(5) . . ? C34 C33 C38 120.8(5) . . ? C33 C34 C35 119.7(5) . . ? C36 C35 C34 121.4(5) . . ? C35 C36 C37 119.9(5) . . ? N7 C37 C36 120.1(4) . . ? N7 C37 C38 121.0(4) . . ? C36 C37 C38 118.9(4) . . ? C32 C38 C33 122.3(5) . . ? C32 C38 C37 118.4(5) . . ? C33 C38 C37 119.2(5) . . ? N5 C39 C40 116.6(4) . . ? N6 C41 C42 113.9(4) . . ? N8 C42 C43 123.3(4) . . ? N8 C42 C41 117.8(4) . . ? C43 C42 C41 118.9(4) . . ? C44 C43 C42 119.1(5) . . ? C43 C44 C50 120.0(5) . . ? C46 C45 C50 121.1(5) . . ? C45 C46 C47 120.2(5) . . ? C48 C47 C46 120.9(5) . . ? C47 C48 C49 119.6(5) . . ? N8 C49 C48 119.5(4) . . ? N8 C49 C50 121.1(4) . . ? C48 C49 C50 119.4(4) . . ? C44 C50 C45 123.1(5) . . ? C44 C50 C49 118.1(4) . . ? C45 C50 C49 118.8(5) . . ? N6 C51 C52 116.3(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.460 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.219