Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Dominic S. Wright' 'Carmen Soria Alvarez' 'Alan Bashall' 'Andrew Bond' 'Dale Cave' 'Eilis A. Harron' 'Richard A. Layfield' 'M. McPartlin' 'Marta E. G. Mosquera' 'Jeremy M. Rawson' 'Paul T. Wood' _publ_contact_author_name 'Dr Dominic S. Wright' _publ_contact_author_address ; Department of Chemistry Cambridge University Lensfield Road Cambridge CB4 1DF UNITED KINGDOM ; _publ_contact_author_email DSW1000@CUS.CAM.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Applications of Manganocene in the Synthesis of Mn(II) Amide and Imide Cages ; data_my491 _database_code_CSD 207480 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H40 Mn2 N4' _chemical_formula_weight 710.66 _chemical_melting_point ? _chemical_compound_source ? 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.237(3) _cell_length_b 10.815(3) _cell_length_c 11.813(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.639(14) _cell_angle_gamma 90.00 _cell_volume 1815.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark res' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method ? _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker P4' _diffrn_measurement_method theta/2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3301 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 23.00 _reflns_number_total 2522 _reflns_number_observed 2043 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. H-atoms on the Cp ring were directly located all other were in calculated potions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+1.3501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2522 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_obs 0.0404 _refine_ls_wR_factor_all 0.0999 _refine_ls_wR_factor_obs 0.0921 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.069 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max 0.323 _refine_ls_shift/esd_mean 0.049 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.57523(3) 1.08185(4) -0.03579(4) 0.0345(2) Uani 1 d . . N1 N 0.6616(2) 0.9975(2) 0.1068(2) 0.0309(6) Uani 1 d . . N2 N 0.5514(2) 0.8873(3) -0.0574(2) 0.0346(7) Uani 1 d . . H2N H 0.5322(24) 0.8535(32) -0.1125(29) 0.042 Uiso 1 d . . C2 C 0.7094(2) 1.0529(3) 0.1924(3) 0.0379(8) Uani 1 d . . H2 H 0.7011(2) 1.1384(3) 0.2023(3) 0.046 Uiso 1 calc R . C3 C 0.7717(2) 0.9900(3) 0.2688(3) 0.0450(9) Uani 1 d . . H3 H 0.8034(2) 1.0325(3) 0.3292(3) 0.054 Uiso 1 calc R . C4 C 0.7857(2) 0.8669(3) 0.2547(3) 0.0440(9) Uani 1 d . . H4 H 0.8280(2) 0.8242(3) 0.3049(3) 0.053 Uiso 1 calc R . C4T C 0.9615(5) 0.3411(6) 0.0182(5) 0.104(2) Uani 1 d . . H4T H 0.9525(5) 0.4032(6) -0.0371(5) 0.124 Uiso 1 calc R . C5 C 0.7371(2) 0.8027(3) 0.1647(3) 0.0355(8) Uani 1 d . . C6 C 0.6738(2) 0.8718(3) 0.0930(3) 0.0285(7) Uani 1 d . . C7 C 0.6191(2) 0.8147(3) 0.0010(3) 0.0317(7) Uani 1 d . . C8 C 0.6372(2) 0.6909(3) -0.0197(3) 0.0442(9) Uani 1 d . . H8 H 0.6058(2) 0.6515(3) -0.0821(3) 0.053 Uiso 1 calc R . C9 C 0.7012(3) 0.6236(3) 0.0506(3) 0.0521(10) Uani 1 d . . H9 H 0.7114(3) 0.5398(3) 0.0342(3) 0.063 Uiso 1 calc R . C10 C 0.7494(3) 0.6754(3) 0.1419(3) 0.0514(10) Uani 1 d . . H10 H 0.7903(3) 0.6272(3) 0.1893(3) 0.062 Uiso 1 calc R . C11 C 0.6795(3) 1.1383(4) -0.1900(4) 0.0592(11) Uani 1 d . . C12 C 0.5886(3) 1.1607(4) -0.2344(3) 0.0544(10) Uani 1 d . . C13 C 0.5500(3) 1.2534(4) -0.1739(4) 0.0601(11) Uani 1 d . . C14 C 0.6169(4) 1.2906(4) -0.0898(4) 0.076(2) Uani 1 d . . C15 C 0.6984(3) 1.2177(5) -0.1006(4) 0.0737(15) Uani 1 d . . H11 H 0.7207 1.0664 -0.2299 0.100(16) Uiso 1 d . . H12 H 0.5608 1.1013 -0.3034 0.101(16) Uiso 1 d . . H13 H 0.4811 1.2951 -0.1795 0.091(14) Uiso 1 d . . H14 H 0.6010 1.3650 -0.0445 0.091(15) Uiso 1 d . . H15 H 0.7616 1.2213 -0.0450 0.109(16) Uiso 1 d . . C1T C 0.9896(3) 0.1576(5) 0.1772(3) 0.0651(12) Uani 1 d . . H1T H 0.9983(3) 0.0947(5) 0.2318(3) 0.078 Uiso 1 calc R . C2T C 0.9253(4) 0.2484(6) 0.1912(5) 0.0862(15) Uani 1 d . . H2T H 0.8907(4) 0.2472(6) 0.2564(5) 0.103 Uiso 1 calc R . C3T C 0.9088(4) 0.3430(5) 0.1124(5) 0.089(2) Uani 1 d . . H3T H 0.8640(4) 0.4051(5) 0.1229(5) 0.107 Uiso 1 calc R . C5T C 1.0273(3) 0.2492(5) 0.0039(4) 0.0747(14) Uani 1 d . . H5T H 1.0619(3) 0.2503(5) -0.0612(4) 0.090 Uiso 1 calc R . C6T C 1.0433(3) 0.1575(4) 0.0812(4) 0.0658(12) Uani 1 d . . C7T C 1.1125(3) 0.0616(5) 0.0656(5) 0.090(2) Uani 1 d . . H7T1 H 1.1017(16) -0.0070(15) 0.1161(22) 0.136 Uiso 1 calc R . H7T2 H 1.1751(3) 0.0947(10) 0.0827(30) 0.136 Uiso 1 calc R . H7T3 H 1.1070(17) 0.0330(23) -0.0124(9) 0.136 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0366(3) 0.0305(3) 0.0360(3) 0.0111(2) -0.0004(2) -0.0013(2) N1 0.0342(15) 0.0281(15) 0.0305(15) 0.0014(12) 0.0030(12) 0.0011(12) N2 0.042(2) 0.034(2) 0.0268(15) -0.0020(12) -0.0066(13) -0.0019(13) C2 0.045(2) 0.032(2) 0.037(2) -0.003(2) 0.002(2) 0.001(2) C3 0.048(2) 0.047(2) 0.038(2) -0.007(2) -0.009(2) 0.003(2) C4 0.042(2) 0.052(2) 0.037(2) 0.008(2) -0.007(2) 0.007(2) C4T 0.110(5) 0.107(5) 0.090(4) 0.025(4) -0.031(4) -0.017(4) C5 0.036(2) 0.033(2) 0.037(2) 0.003(2) 0.003(2) 0.006(2) C6 0.031(2) 0.025(2) 0.030(2) 0.0036(14) 0.0065(14) 0.0010(14) C7 0.036(2) 0.029(2) 0.030(2) -0.0005(14) 0.0055(14) -0.0005(15) C8 0.048(2) 0.036(2) 0.049(2) -0.012(2) 0.002(2) 0.003(2) C9 0.057(2) 0.030(2) 0.069(3) -0.004(2) 0.005(2) 0.009(2) C10 0.052(2) 0.036(2) 0.065(3) 0.008(2) -0.004(2) 0.013(2) C11 0.065(3) 0.053(2) 0.062(3) 0.023(2) 0.019(2) 0.005(2) C12 0.068(3) 0.056(3) 0.038(2) 0.015(2) 0.002(2) -0.012(2) C13 0.062(3) 0.061(3) 0.059(3) 0.033(2) 0.017(2) 0.011(2) C14 0.144(5) 0.035(2) 0.053(3) 0.003(2) 0.041(3) -0.026(3) C15 0.063(3) 0.091(4) 0.065(3) 0.046(3) -0.015(2) -0.040(3) C1T 0.061(3) 0.085(3) 0.050(3) -0.006(2) 0.010(2) -0.019(3) C2T 0.077(3) 0.105(4) 0.077(3) -0.005(3) 0.011(3) -0.009(3) C3T 0.085(4) 0.090(4) 0.090(4) -0.017(4) -0.014(3) 0.003(3) C5T 0.072(3) 0.095(4) 0.056(3) 0.017(3) -0.009(2) -0.020(3) C6T 0.049(2) 0.080(3) 0.066(3) -0.017(3) -0.014(2) -0.017(2) C7T 0.065(3) 0.105(4) 0.101(4) -0.038(3) -0.003(3) -0.009(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 N2 2.143(3) . ? Mn1 N2 2.197(3) 3_675 ? Mn1 N1 2.219(2) . ? Mn1 C14 2.429(4) . ? Mn1 C15 2.448(4) . ? Mn1 C13 2.482(4) . ? Mn1 C11 2.497(4) . ? Mn1 C12 2.515(4) . ? Mn1 Mn1 2.9440(10) 3_675 ? N1 C2 1.325(4) . ? N1 C6 1.381(4) . ? N2 C7 1.392(4) . ? N2 Mn1 2.197(3) 3_675 ? C2 C3 1.401(5) . ? C3 C4 1.358(5) . ? C4 C5 1.413(5) . ? C4T C3T 1.382(7) . ? C4T C5T 1.383(7) . ? C5 C10 1.416(5) . ? C5 C6 1.411(4) . ? C6 C7 1.436(4) . ? C7 C8 1.388(4) . ? C8 C9 1.397(5) . ? C9 C10 1.362(5) . ? C11 C15 1.374(6) . ? C11 C12 1.385(5) . ? C12 C13 1.367(6) . ? C13 C14 1.391(6) . ? C14 C15 1.416(7) . ? C1T C2T 1.360(7) . ? C1T C6T 1.407(6) . ? C2T C3T 1.393(7) . ? C5T C6T 1.358(6) . ? C6T C7T 1.450(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 N2 Mn1 N2 94.58(10) . 3_675 ? N2 Mn1 N1 76.28(9) . . ? N2 Mn1 N1 96.60(9) 3_675 . ? N2 Mn1 C14 156.94(13) . . ? N2 Mn1 C14 102.26(15) 3_675 . ? N1 Mn1 C14 116.7(2) . . ? N2 Mn1 C15 131.5(2) . . ? N2 Mn1 C15 133.8(2) 3_675 . ? N1 Mn1 C15 96.34(12) . . ? C14 Mn1 C15 33.7(2) . . ? N2 Mn1 C13 129.81(14) . . ? N2 Mn1 C13 97.30(12) 3_675 . ? N1 Mn1 C13 148.96(13) . . ? C14 Mn1 C13 32.9(2) . . ? C15 Mn1 C13 54.71(14) . . ? N2 Mn1 C11 104.49(13) . . ? N2 Mn1 C11 150.82(12) 3_675 . ? N1 Mn1 C11 109.14(12) . . ? C14 Mn1 C11 54.20(15) . . ? C15 Mn1 C11 32.25(15) . . ? C13 Mn1 C11 53.52(13) . . ? N2 Mn1 C12 104.04(12) . . ? N2 Mn1 C12 121.97(12) 3_675 . ? N1 Mn1 C12 140.95(12) . . ? C14 Mn1 C12 53.54(14) . . ? C15 Mn1 C12 53.59(13) . . ? C13 Mn1 C12 31.74(13) . . ? C11 Mn1 C12 32.09(13) . . ? N2 Mn1 Mn1 48.05(8) . 3_675 ? N2 Mn1 Mn1 46.53(7) 3_675 3_675 ? N1 Mn1 Mn1 85.02(7) . 3_675 ? C14 Mn1 Mn1 145.92(15) . 3_675 ? C15 Mn1 Mn1 178.45(11) . 3_675 ? C13 Mn1 Mn1 124.12(10) . 3_675 ? C11 Mn1 Mn1 146.46(12) . 3_675 ? C12 Mn1 Mn1 124.86(9) . 3_675 ? C2 N1 C6 118.3(3) . . ? C2 N1 Mn1 128.8(2) . . ? C6 N1 Mn1 112.5(2) . . ? C7 N2 Mn1 113.3(2) . . ? C7 N2 Mn1 113.7(2) . 3_675 ? Mn1 N2 Mn1 85.42(10) . 3_675 ? N1 C2 C3 123.0(3) . . ? C4 C3 C2 119.3(3) . . ? C3 C4 C5 120.4(3) . . ? C3T C4T C5T 121.0(5) . . ? C4 C5 C10 124.1(3) . . ? C4 C5 C6 117.1(3) . . ? C10 C5 C6 118.9(3) . . ? N1 C6 C7 116.5(3) . . ? N1 C6 C5 122.0(3) . . ? C7 C6 C5 121.5(3) . . ? C8 C7 C6 116.7(3) . . ? C8 C7 N2 126.0(3) . . ? C6 C7 N2 117.2(3) . . ? C9 C8 C7 121.3(3) . . ? C8 C9 C10 122.2(3) . . ? C9 C10 C5 119.2(3) . . ? C15 C11 C12 108.4(4) . . ? C15 C11 Mn1 71.9(2) . . ? C12 C11 Mn1 74.6(2) . . ? C11 C12 C13 109.1(4) . . ? C11 C12 Mn1 73.3(2) . . ? C13 C12 Mn1 72.8(2) . . ? C14 C13 C12 107.8(4) . . ? C14 C13 Mn1 71.5(2) . . ? C12 C13 Mn1 75.5(2) . . ? C13 C14 C15 107.6(4) . . ? C13 C14 Mn1 75.6(2) . . ? C15 C14 Mn1 73.8(2) . . ? C11 C15 C14 107.1(4) . . ? C11 C15 Mn1 75.9(2) . . ? C14 C15 Mn1 72.4(2) . . ? C2T C1T C6T 120.2(5) . . ? C1T C2T C3T 122.4(5) . . ? C4T C3T C2T 116.7(5) . . ? C6T C5T C4T 122.0(5) . . ? C5T C6T C7T 121.6(5) . . ? C5T C6T C1T 117.7(5) . . ? C7T C6T C1T 120.7(5) . . ? _refine_diff_density_max 0.508 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.050 data_dw0122 _database_code_CSD 207481 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H128 Mn8 N24 O16' _chemical_formula_weight 2481.88 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 24.3007(12) _cell_length_b 24.3007(12) _cell_length_c 20.5467(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12133.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8109 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 22.46 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5136 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multiscan #_exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 13230 _diffrn_reflns_av_R_equivalents 0.1047 _diffrn_reflns_av_sigmaI/netI 0.0946 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 22.45 _reflns_number_total 3934 _reflns_number_gt 2725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+40.6535P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3934 _refine_ls_number_parameters 336 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_obs 0.0592 _refine_ls_wR_factor_all 0.2008 _refine_ls_wR_factor_obs 0.1402 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.336 _refine_ls_restrained_S_obs 1.181 _refine_ls_shift/esd_max -0.537 _refine_ls_shift/esd_mean 0.063 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.07655(3) -0.25338(4) -0.07976(4) 0.0293(3) Uani 1 d . . Mn2 Mn 0.10483(4) -0.12243(4) -0.05343(5) 0.0406(3) Uani 1 d . . N1 N 0.0376(2) -0.1768(2) -0.0764(2) 0.0301(11) Uani 1 d . . N2 N 0.1596(2) -0.2305(2) -0.0753(2) 0.0406(13) Uani 1 d . . H2 H 0.1791(2) -0.2348(2) -0.1110(2) 0.049 Uiso 1 calc R . N3 N 0.1571(2) -0.1713(2) 0.0114(3) 0.0441(14) Uani 1 d . . N4 N 0.2375(2) -0.2265(3) -0.0105(3) 0.059(2) Uani 1 d . . N5 N 0.0226(2) -0.1145(2) 0.0058(2) 0.0387(13) Uani 1 d . . N6 N -0.0452(2) -0.1840(2) -0.0164(2) 0.0331(12) Uani 1 d . . O3 O 0.1485(3) -0.1174(2) 0.0982(3) 0.085(2) Uani 1 d . . O4 O 0.3104(3) -0.2207(4) 0.0594(4) 0.122(3) Uani 1 d . . O5 O 0.0060(2) -0.0527(2) 0.0885(3) 0.070(2) Uani 1 d . . O6 O -0.1224(2) -0.1915(2) 0.0404(2) 0.0608(14) Uani 1 d . . C1 C 0.1113(3) -0.0301(3) -0.1038(5) 0.072(3) Uani 1 d . . H1 H 0.0806(3) -0.0061(3) -0.0991(5) 0.087 Uiso 1 calc R . C2 C 0.1203(4) -0.0661(4) -0.1536(4) 0.069(2) Uani 1 d . . H2A H 0.0963(4) -0.0714(4) -0.1896(4) 0.083 Uiso 1 calc R . C3 C 0.1671(5) -0.0925(4) -0.1445(6) 0.087(3) Uani 1 d . . H3 H 0.1815(5) -0.1196(4) -0.1731(6) 0.105 Uiso 1 calc R . C4 C 0.1914(4) -0.0757(5) -0.0898(8) 0.103(4) Uani 1 d . . H4 H 0.2257(4) -0.0884(5) -0.0734(8) 0.124 Uiso 1 calc R . C5 C 0.1565(5) -0.0354(4) -0.0602(5) 0.093(3) Uani 1 d . . H5 H 0.1623(5) -0.0164(4) -0.0203(5) 0.111 Uiso 1 calc R . C11 C 0.1853(3) -0.2102(3) -0.0240(3) 0.044(2) Uani 1 d . . C13 C 0.2592(3) -0.2068(4) 0.0425(5) 0.082(3) Uani 1 d . . C14 C 0.2327(4) -0.1711(4) 0.0853(5) 0.082(3) Uani 1 d . . H14 H 0.2490(4) -0.1592(4) 0.1248(5) 0.099 Uiso 1 calc R . C15 C 0.1809(4) -0.1542(3) 0.0660(4) 0.064(2) Uani 1 d . . C17 C 0.1685(5) -0.0958(5) 0.1595(5) 0.126(5) Uani 1 d . . H17A H 0.1402(15) -0.0725(30) 0.1792(22) 0.189 Uiso 1 calc R . H17B H 0.2018(22) -0.0740(31) 0.1518(7) 0.189 Uiso 1 calc R . H17C H 0.1771(35) -0.1264(5) 0.1889(16) 0.189 Uiso 1 calc R . C18 C 0.3375(5) -0.2573(7) 0.0155(8) 0.162(6) Uani 1 d . . H18A H 0.3181(30) -0.2926(17) 0.0148(44) 0.243 Uiso 1 calc R . H18B H 0.3755(16) -0.2630(40) 0.0299(34) 0.243 Uiso 1 calc R . H18C H 0.3375(43) -0.2413(23) -0.0283(15) 0.243 Uiso 1 calc R . C21 C 0.0043(2) -0.1595(2) -0.0290(3) 0.0309(14) Uani 1 d . . C23 C -0.0093(3) -0.0967(3) 0.0530(3) 0.047(2) Uani 1 d . . C24 C -0.0599(3) -0.1193(3) 0.0696(3) 0.052(2) Uani 1 d . . H24 H -0.0820(3) -0.1052(3) 0.1039(3) 0.062 Uiso 1 calc R . C25 C -0.0752(3) -0.1632(3) 0.0329(3) 0.041(2) Uani 1 d . . C27 C 0.0544(3) -0.0227(3) 0.0683(5) 0.081(3) Uani 1 d . . H27A H 0.0612(15) 0.0077(16) 0.0986(18) 0.121 Uiso 1 calc R . H27B H 0.0487(10) -0.0079(21) 0.0244(13) 0.121 Uiso 1 calc R . H27C H 0.0863(6) -0.0475(7) 0.0680(29) 0.121 Uiso 1 calc R . C28 C -0.1597(4) -0.1722(4) 0.0902(5) 0.102(4) Uani 1 d . . H28A H -0.1910(16) -0.1974(18) 0.0936(26) 0.153 Uiso 1 calc R . H28B H -0.1729(24) -0.1353(14) 0.0788(18) 0.153 Uiso 1 calc R . H28C H -0.1403(10) -0.1706(29) 0.1321(8) 0.153 Uiso 1 calc R . C1S C 0.0000 -0.2500 -0.3951(13) 0.186(9) Uani 1 d SU . C2S C -0.0272(8) -0.1894(10) -0.4187(13) 0.229(9) Uani 1 d U . C3S C -0.0153(13) -0.1926(14) -0.4950(20) 0.321(15) Uani 1 d U . C4S C 0.0000 -0.2500 -0.5032(14) 0.185(10) Uani 1 d SU . C1T C 0.2732(6) 0.1333(8) -0.1883(7) 0.258(11) Uani 1 d GU . H1T H 0.3046(6) 0.1517(8) -0.1713(7) 0.310 Uiso 0.83 calc PR . C2T C 0.2345(9) 0.1624(5) -0.2244(8) 0.220(9) Uani 1 d GU . H2T H 0.2394(13) 0.2006(5) -0.2320(12) 0.264 Uiso 0.83 calc PR . C3T C 0.1886(7) 0.1355(9) -0.2492(6) 0.230(10) Uani 1 d GU . H3T H 0.1622(10) 0.1553(13) -0.2739(8) 0.276 Uiso 0.83 calc PR . C4T C 0.1814(6) 0.0795(9) -0.2380(7) 0.243(10) Uani 1 d GU . H4T H 0.1501(7) 0.0611(14) -0.2550(10) 0.291 Uiso 0.83 calc PR . C5T C 0.2202(9) 0.0505(5) -0.2019(8) 0.241(10) Uani 1 d GU . H5T H 0.2152(13) 0.0122(5) -0.1943(12) 0.289 Uiso 0.83 calc PR . C6T C 0.2660(7) 0.0774(8) -0.1771(6) 0.203(8) Uani 1 d GU . H6T H 0.2925(9) 0.0575(12) -0.1524(8) 0.244 Uiso 0.83 calc PR . 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 0.0307(5) 0.0291(5) 0.0283(5) 0.0000(4) 0.0001(4) 0.0001(4) Mn2 0.0311(6) 0.0369(6) 0.0539(7) -0.0016(5) -0.0048(5) -0.0024(4) N1 0.030(3) 0.031(3) 0.029(3) -0.002(2) -0.001(2) 0.000(2) N2 0.033(3) 0.050(3) 0.039(3) -0.003(3) 0.006(3) -0.004(3) N3 0.049(3) 0.042(3) 0.041(3) -0.008(3) -0.013(3) 0.002(3) N4 0.033(4) 0.070(4) 0.074(4) 0.005(4) -0.019(3) -0.003(3) N5 0.034(3) 0.039(3) 0.043(3) -0.021(3) 0.000(3) 0.001(2) N6 0.027(3) 0.040(3) 0.032(3) -0.006(2) 0.005(2) -0.003(2) O3 0.115(5) 0.072(4) 0.067(4) -0.028(3) -0.035(4) 0.015(4) O4 0.068(5) 0.149(7) 0.148(7) -0.011(6) -0.059(5) 0.016(5) O5 0.052(3) 0.071(4) 0.086(4) -0.052(3) 0.007(3) -0.004(3) O6 0.053(3) 0.074(4) 0.055(3) -0.027(3) 0.026(3) -0.019(3) C1 0.055(5) 0.042(5) 0.119(8) 0.004(5) 0.017(6) 0.002(4) C2 0.066(6) 0.060(5) 0.083(6) 0.004(5) 0.009(5) -0.028(5) C3 0.061(7) 0.068(6) 0.133(10) 0.016(6) 0.034(7) 0.008(6) C4 0.029(5) 0.104(9) 0.177(12) 0.066(9) 0.010(7) -0.003(5) C5 0.107(9) 0.083(7) 0.087(7) 0.003(6) 0.000(7) -0.066(7) C11 0.038(4) 0.045(4) 0.050(4) 0.004(4) -0.011(4) -0.003(3) C13 0.049(6) 0.082(7) 0.114(8) 0.018(6) -0.039(6) 0.002(5) C14 0.078(7) 0.075(6) 0.093(7) -0.005(5) -0.053(6) -0.003(5) C15 0.081(6) 0.054(5) 0.056(5) -0.008(4) -0.019(5) -0.003(5) C17 0.185(12) 0.118(9) 0.074(7) -0.048(7) -0.059(7) 0.020(8) C18 0.064(8) 0.235(17) 0.187(14) 0.001(13) -0.045(9) 0.060(10) C21 0.034(4) 0.033(4) 0.026(3) -0.001(3) -0.006(3) 0.005(3) C23 0.046(4) 0.046(4) 0.050(4) -0.027(4) -0.008(4) 0.006(4) C24 0.042(4) 0.060(5) 0.053(4) -0.026(4) 0.011(4) 0.001(4) C25 0.038(4) 0.045(4) 0.040(4) -0.009(3) 0.002(3) -0.003(3) C27 0.050(5) 0.066(5) 0.126(8) -0.060(5) 0.010(5) -0.016(4) C28 0.069(6) 0.137(9) 0.100(7) -0.056(7) 0.060(6) -0.035(6) C1S 0.113(13) 0.214(17) 0.230(18) 0.000 0.000 -0.096(14) C2S 0.148(13) 0.266(17) 0.271(18) -0.063(15) 0.022(13) -0.074(13) C3S 0.241(20) 0.349(23) 0.373(23) 0.020(19) -0.045(18) -0.036(18) C4S 0.153(16) 0.196(18) 0.207(18) 0.000 0.000 -0.023(15) C1T 0.302(19) 0.318(20) 0.155(14) -0.021(14) 0.145(14) 0.038(16) C2T 0.225(16) 0.279(17) 0.156(13) 0.006(12) 0.152(13) 0.035(14) C3T 0.285(18) 0.252(18) 0.153(13) -0.010(13) 0.136(13) 0.008(15) C4T 0.281(18) 0.261(18) 0.187(15) -0.039(15) 0.082(14) 0.013(16) C5T 0.258(18) 0.255(18) 0.208(16) -0.006(14) 0.088(15) 0.008(16) C6T 0.255(17) 0.188(14) 0.166(13) -0.010(12) 0.084(13) -0.044(14) _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 N1 2.088(5) . ? Mn1 N2 2.095(5) . ? Mn1 N1 2.101(5) 11_655 ? Mn1 N6 2.144(5) 2_545 ? Mn1 Mn1 3.2234(14) 12 ? Mn1 Mn1 3.2234(14) 11_655 ? Mn2 N1 2.154(5) . ? Mn2 N3 2.190(5) . ? Mn2 N5 2.347(5) . ? Mn2 C5 2.464(8) . ? Mn2 C4 2.504(8) . ? Mn2 C1 2.475(8) . ? Mn2 C3 2.515(9) . ? Mn2 C2 2.500(8) . ? N1 C21 1.335(7) . ? N1 Mn1 2.101(5) 12 ? N2 C11 1.322(8) . ? N3 C15 1.327(9) . ? N3 C11 1.376(8) . ? N4 C13 1.301(11) . ? N4 C11 1.357(8) . ? N5 C23 1.317(8) . ? N5 C21 1.379(7) . ? N6 C21 1.366(7) . ? N6 C25 1.346(7) . ? N6 Mn1 2.144(5) 2_545 ? O3 C15 1.362(9) . ? O3 C17 1.448(9) . ? O4 C13 1.333(10) . ? O4 C18 1.43(2) . ? O5 C23 1.347(8) . ? O5 C27 1.445(9) . ? O6 C25 1.346(7) . ? O6 C28 1.445(8) . ? C1 C2 1.363(11) . ? C1 C5 1.425(13) . ? C2 C3 1.319(12) . ? C3 C4 1.334(14) . ? C4 C5 1.432(14) . ? C13 C14 1.393(13) . ? C14 C15 1.382(11) . ? C23 C24 1.387(9) . ? C24 C25 1.358(9) . ? C1S C2S 1.69(3) . ? C1S C2S 1.69(3) 2_545 ? C2S C3S 1.60(4) . ? C3S C4S 1.45(3) . ? C4S C3S 1.45(3) 2_545 ? C1T C2T 1.39 . ? C1T C6T 1.39 . ? C2T C3T 1.39 . ? C3T C4T 1.39 . ? C4T C5T 1.39 . ? C5T C6T 1.39 . ? 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 N1 Mn1 N2 101.4(2) . . ? N1 Mn1 N1 111.4(2) . 11_655 ? N2 Mn1 N1 100.5(2) . 11_655 ? N1 Mn1 N6 116.8(2) . 2_545 ? N2 Mn1 N6 120.3(2) . 2_545 ? N1 Mn1 N6 105.2(2) 11_655 2_545 ? N1 Mn1 Mn1 39.85(13) . 12 ? N2 Mn1 Mn1 113.33(15) . 12 ? N1 Mn1 Mn1 71.81(13) 11_655 12 ? N6 Mn1 Mn1 125.59(13) 2_545 12 ? N1 Mn1 Mn1 103.73(13) . 11_655 ? N2 Mn1 Mn1 138.76(15) . 11_655 ? N1 Mn1 Mn1 39.54(13) 11_655 11_655 ? N6 Mn1 Mn1 75.18(13) 2_545 11_655 ? Mn1 Mn1 Mn1 70.57(3) 12 11_655 ? N1 Mn2 N3 103.9(2) . . ? N1 Mn2 N5 61.2(2) . . ? N3 Mn2 N5 102.9(2) . . ? N1 Mn2 C5 154.3(3) . . ? N3 Mn2 C5 101.7(3) . . ? N5 Mn2 C5 113.1(3) . . ? N1 Mn2 C4 148.2(4) . . ? N3 Mn2 C4 86.5(3) . . ? N5 Mn2 C4 146.4(4) . . ? C5 Mn2 C4 33.5(3) . . ? N1 Mn2 C1 120.8(3) . . ? N3 Mn2 C1 135.1(3) . . ? N5 Mn2 C1 101.3(2) . . ? C5 Mn2 C1 33.5(3) . . ? C4 Mn2 C1 54.0(3) . . ? N1 Mn2 C3 118.1(3) . . ? N3 Mn2 C3 105.1(3) . . ? N5 Mn2 C3 151.0(3) . . ? C5 Mn2 C3 53.3(3) . . ? C4 Mn2 C3 30.8(3) . . ? C1 Mn2 C3 52.3(3) . . ? N1 Mn2 C2 105.6(2) . . ? N3 Mn2 C2 135.3(3) . . ? N5 Mn2 C2 120.6(3) . . ? C5 Mn2 C2 53.7(3) . . ? C4 Mn2 C2 51.7(3) . . ? C1 Mn2 C2 31.8(3) . . ? C3 Mn2 C2 30.5(3) . . ? C21 N1 Mn1 125.4(4) . . ? C21 N1 Mn1 114.7(4) . 12 ? Mn1 N1 Mn1 100.6(2) . 12 ? C21 N1 Mn2 96.1(3) . . ? Mn1 N1 Mn2 102.1(2) . . ? Mn1 N1 Mn2 118.5(2) 12 . ? C11 N2 Mn1 126.1(4) . . ? C15 N3 C11 116.3(6) . . ? C15 N3 Mn2 126.7(5) . . ? C11 N3 Mn2 109.9(4) . . ? C13 N4 C11 116.3(7) . . ? C23 N5 C21 116.9(5) . . ? C23 N5 Mn2 155.7(4) . . ? C21 N5 Mn2 86.6(3) . . ? C21 N6 C25 117.2(5) . . ? C21 N6 Mn1 120.5(4) . 2_545 ? C25 N6 Mn1 122.0(4) . 2_545 ? C15 O3 C17 117.8(7) . . ? C13 O4 C18 115.1(9) . . ? C23 O5 C27 118.0(5) . . ? C25 O6 C28 116.7(6) . . ? C2 C1 C5 106.9(8) . . ? C2 C1 Mn2 75.1(5) . . ? C5 C1 Mn2 72.8(5) . . ? C1 C2 C3 110.1(9) . . ? C1 C2 Mn2 73.1(5) . . ? C3 C2 Mn2 75.4(6) . . ? C4 C3 C2 110.7(10) . . ? C4 C3 Mn2 74.2(6) . . ? C2 C3 Mn2 74.1(5) . . ? C3 C4 C5 107.8(9) . . ? C3 C4 Mn2 75.0(6) . . ? C5 C4 Mn2 71.7(4) . . ? C4 C5 C1 104.5(9) . . ? C4 C5 Mn2 74.8(5) . . ? C1 C5 Mn2 73.6(4) . . ? N4 C11 N2 119.8(6) . . ? N4 C11 N3 124.0(6) . . ? N2 C11 N3 116.2(6) . . ? N4 C13 C14 124.6(7) . . ? N4 C13 O4 120.1(10) . . ? C14 C13 O4 115.2(9) . . ? C13 C14 C15 115.2(8) . . ? O3 C15 N3 111.4(7) . . ? O3 C15 C14 125.5(8) . . ? N3 C15 C14 123.1(8) . . ? N1 C21 N6 122.3(5) . . ? N1 C21 N5 115.6(5) . . ? N6 C21 N5 122.0(5) . . ? N5 C23 O5 119.8(6) . . ? N5 C23 C24 124.9(6) . . ? O5 C23 C24 115.3(6) . . ? C25 C24 C23 114.7(6) . . ? C24 C25 N6 124.2(6) . . ? C24 C25 O6 124.8(6) . . ? N6 C25 O6 110.9(5) . . ? C2S C1S C2S 146.6(27) . 2_545 ? C3S C2S C1S 99.7(21) . . ? C4S C3S C2S 102.0(28) . . ? C3S C4S C3S 166.8(44) . 2_545 ? C2T C1T C6T 120.0 . . ? C3T C2T C1T 120.0 . . ? C2T C3T C4T 120.0 . . ? C5T C4T C3T 120.0 . . ? C4T C5T C6T 120.0 . . ? C5T C6T C1T 120.0 . . ? _refine_diff_density_max 0.489 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.079 data_dw0130 _database_code_CSD 207482 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C110 H128 Mn8 N24 O8' _chemical_formula_weight 2353.88 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 23.6528(8) _cell_length_b 23.6528(8) _cell_length_c 20.7070(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11584.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 15669 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method ? _exptl_crystal_F_000 4880 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type multiscan #_exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 #_diffrn_radiation_type MoK\a #_diffrn_radiation_source 'fine-focus sealed tube' #_diffrn_radiation_monochromator graphite #_diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 #_diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 22318 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5674 _reflns_number_observed 4000 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 18 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+17.8397P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5656 _refine_ls_number_parameters 318 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_obs 0.0571 _refine_ls_wR_factor_all 0.1993 _refine_ls_wR_factor_obs 0.1490 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.122 _refine_ls_restrained_S_all 1.290 _refine_ls_restrained_S_obs 1.189 _refine_ls_shift/esd_max 1.463 _refine_ls_shift/esd_mean 0.142 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.07741(2) -0.25947(2) -0.07947(3) 0.0377(2) Uani 1 d . . Mn2 Mn 0.11562(3) -0.12920(3) -0.05207(3) 0.0482(2) Uani 1 d . . N2 N 0.16314(14) -0.2380(2) -0.0727(2) 0.0528(9) Uani 1 d . . H2A H 0.18303(14) -0.2409(2) -0.1085(2) 0.063 Uiso 1 calc R . N1 N 0.04128(13) -0.17958(12) -0.07631(14) 0.0385(7) Uani 1 d . . N4 N 0.2430(2) -0.2422(2) -0.0073(2) 0.0667(11) Uani 1 d . . N3 N 0.1655(2) -0.1803(2) 0.0156(2) 0.0547(9) Uani 1 d . . N5 N 0.03311(15) -0.11310(15) 0.0038(2) 0.0528(9) Uani 1 d . . N6 N -0.04405(13) -0.17629(13) -0.01664(14) 0.0396(7) Uani 1 d . . O4 O 0.3187(2) -0.2445(3) 0.0619(3) 0.131(2) Uani 1 d . . O6 O -0.12381(13) -0.17336(14) 0.03878(15) 0.0649(9) Uani 1 d . . C1 C 0.1253(3) -0.0335(2) -0.0980(5) 0.101(2) Uani 1 d . . H1 H 0.0941(3) -0.0085(2) -0.0945(5) 0.121 Uiso 1 calc R . C2 C 0.1352(3) -0.0704(3) -0.1469(3) 0.086(2) Uani 1 d . . H2 H 0.1116(3) -0.0762(3) -0.1834(3) 0.103 Uiso 1 calc R . C3 C 0.1831(3) -0.0968(3) -0.1352(4) 0.094(2) Uani 1 d . . H3 H 0.1993(3) -0.1247(3) -0.1626(4) 0.113 Uiso 1 calc R . C4 C 0.2060(3) -0.0793(4) -0.0801(5) 0.113(3) Uani 1 d . . H4 H 0.2406(3) -0.0921(4) -0.0622(5) 0.136 Uiso 1 calc R . C5 C 0.1700(4) -0.0391(3) -0.0534(3) 0.114(3) Uani 1 d . . H5 H 0.1746(4) -0.0195(3) -0.0136(3) 0.137 Uiso 1 calc R . C11 C 0.1910(2) -0.2206(2) -0.0206(2) 0.0505(10) Uani 1 d . . C13 C 0.2663(3) -0.2257(3) 0.0464(3) 0.087(2) Uani 1 d . . C14 C 0.2413(3) -0.1880(3) 0.0892(3) 0.100(2) Uani 1 d . . H14 H 0.2587(3) -0.1786(3) 0.1290(3) 0.120 Uiso 1 calc R . C15 C 0.1910(3) -0.1653(2) 0.0718(2) 0.0763(15) Uani 1 d . . C17 C 0.1616(3) -0.1205(3) 0.1111(3) 0.102(2) Uani 1 d . . H17A H 0.1778(15) -0.1195(15) 0.1547(8) 0.153 Uiso 1 calc R . H17B H 0.1212(5) -0.1292(12) 0.1139(21) 0.153 Uiso 1 calc R . H17C H 0.1667(19) -0.0836(4) 0.0904(14) 0.153 Uiso 1 calc R . C18 C 0.3465(4) -0.2805(6) 0.0150(6) 0.183(5) Uani 1 d . . H18A H 0.3246(22) -0.3153(18) 0.0093(35) 0.275 Uiso 1 calc R . H18B H 0.3845(16) -0.2900(35) 0.0305(23) 0.275 Uiso 1 calc R . H18C H 0.3493(37) -0.2606(15) -0.0263(15) 0.275 Uiso 1 calc R . C21 C 0.0092(2) -0.1575(2) -0.0300(2) 0.0406(9) Uani 1 d . . C23 C 0.0024(2) -0.0879(2) 0.0493(2) 0.0596(12) Uani 1 d . . C24 C -0.0511(2) -0.1058(2) 0.0652(2) 0.0576(11) Uani 1 d . . H24 H -0.0723(2) -0.0883(2) 0.0986(2) 0.069 Uiso 1 calc R . C25 C -0.0722(2) -0.1505(2) 0.0302(2) 0.0480(10) Uani 1 d . . C27 C 0.0290(3) -0.0372(2) 0.0809(3) 0.089(2) Uani 1 d . . H27A H -0.0006(3) -0.0131(10) 0.0993(19) 0.134 Uiso 1 calc R . H27B H 0.0504(16) -0.0157(11) 0.0486(5) 0.134 Uiso 1 calc R . H27C H 0.0546(15) -0.0497(3) 0.1153(14) 0.134 Uiso 1 calc R . C28 C -0.1599(3) -0.1477(3) 0.0859(3) 0.104(2) Uani 1 d . . H28A H -0.1428(11) -0.1515(19) 0.1288(4) 0.156 Uiso 1 calc R . H28B H -0.1968(8) -0.1666(15) 0.0855(18) 0.156 Uiso 1 calc R . H28C H -0.1649(18) -0.1076(6) 0.0757(14) 0.156 Uiso 1 calc R . C1S C 0.0000 -0.2500 -0.3773(5) 0.163(6) Uani 1 d SU . C2S C -0.0121(6) -0.1965(8) -0.4144(10) 0.223(7) Uani 1 d U . C3S C -0.0069(10) -0.1983(10) -0.4762(15) 0.299(11) Uani 1 d U . C4S C 0.0000 -0.2500 -0.4991(8) 0.175(7) Uani 1 d SU . C1T C 0.2982(5) 0.1266(7) -0.1860(6) 0.268(8) Uani 1 d GU . H1T H 0.3322(5) 0.1446(7) -0.1727(6) 0.321 Uiso 0.83 calc PR . C2T C 0.2581(8) 0.1566(4) -0.2210(5) 0.230(7) Uani 1 d GU . H2T H 0.2647(11) 0.1951(4) -0.2316(8) 0.276 Uiso 0.83 calc PR . C3T C 0.2084(6) 0.1303(7) -0.2404(4) 0.278(9) Uani 1 d GU . H3T H 0.1810(8) 0.1509(10) -0.2644(5) 0.334 Uiso 0.83 calc PR . C4T C 0.1988(5) 0.0740(7) -0.2249(5) 0.246(8) Uani 1 d GU . H4T H 0.1648(6) 0.0560(10) -0.2382(7) 0.295 Uiso 0.83 calc PR . C5T C 0.2389(7) 0.0439(4) -0.1899(5) 0.212(6) Uani 1 d GU . H5T H 0.2324(10) 0.0054(4) -0.1792(8) 0.254 Uiso 0.83 calc PR . C6T C 0.2887(6) 0.0702(6) -0.1704(5) 0.263(8) Uani 1 d GU . H6T H 0.3161(7) 0.0497(9) -0.1465(7) 0.316 Uiso 0.83 calc PR . 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 0.0398(3) 0.0375(3) 0.0357(3) 0.0003(2) -0.0012(2) -0.0002(2) Mn2 0.0421(4) 0.0465(4) 0.0560(4) -0.0034(3) -0.0008(3) -0.0032(3) N2 0.046(2) 0.069(2) 0.044(2) -0.004(2) 0.003(2) -0.008(2) N1 0.042(2) 0.037(2) 0.036(2) -0.0016(13) -0.0020(13) 0.0011(13) N4 0.054(2) 0.073(3) 0.074(3) 0.003(2) -0.017(2) 0.002(2) N3 0.056(2) 0.057(2) 0.051(2) -0.005(2) -0.013(2) -0.003(2) N5 0.053(2) 0.049(2) 0.057(2) -0.017(2) 0.004(2) -0.005(2) N6 0.042(2) 0.038(2) 0.039(2) -0.0058(13) 0.0022(14) 0.0004(14) O4 0.086(3) 0.177(5) 0.131(4) -0.003(4) -0.062(3) 0.027(3) O6 0.058(2) 0.071(2) 0.066(2) -0.019(2) 0.017(2) -0.006(2) C1 0.062(4) 0.046(3) 0.196(8) 0.017(4) 0.037(5) 0.003(3) C2 0.103(5) 0.075(4) 0.080(4) 0.009(3) -0.008(3) -0.035(4) C3 0.100(5) 0.068(4) 0.116(5) 0.011(4) 0.051(5) 0.009(4) C4 0.045(3) 0.151(7) 0.143(7) 0.078(6) -0.008(4) -0.019(4) C5 0.146(7) 0.120(6) 0.077(4) -0.032(4) 0.032(4) -0.091(6) C11 0.046(2) 0.051(2) 0.054(2) 0.003(2) -0.007(2) -0.005(2) C13 0.075(4) 0.099(5) 0.088(4) 0.009(4) -0.031(3) 0.006(3) C14 0.098(5) 0.126(6) 0.077(4) -0.008(4) -0.048(4) 0.005(4) C15 0.090(4) 0.077(4) 0.063(3) -0.004(3) -0.019(3) -0.006(3) C17 0.129(6) 0.103(5) 0.073(4) -0.033(3) -0.025(4) 0.011(4) C18 0.091(6) 0.257(13) 0.202(10) -0.060(10) -0.052(6) 0.087(7) C21 0.048(2) 0.038(2) 0.036(2) -0.002(2) -0.003(2) 0.002(2) C23 0.064(3) 0.052(3) 0.063(3) -0.023(2) 0.002(2) 0.002(2) C24 0.057(3) 0.056(3) 0.060(3) -0.021(2) 0.006(2) 0.004(2) C25 0.047(2) 0.050(2) 0.047(2) -0.005(2) 0.005(2) 0.002(2) C27 0.095(4) 0.077(4) 0.096(4) -0.054(3) 0.000(3) -0.004(3) C28 0.077(4) 0.126(5) 0.108(5) -0.045(4) 0.053(4) -0.019(4) C1S 0.097(8) 0.309(17) 0.083(6) 0.000 0.000 -0.087(11) C2S 0.106(8) 0.268(14) 0.296(16) -0.059(13) 0.037(10) -0.035(9) C3S 0.192(15) 0.313(19) 0.392(21) 0.028(18) -0.061(16) 0.003(15) C4S 0.165(13) 0.251(17) 0.109(9) 0.000 0.000 -0.031(14) C1T 0.378(18) 0.269(16) 0.157(11) 0.000(11) 0.060(12) -0.039(14) C2T 0.273(14) 0.282(14) 0.135(9) 0.029(10) 0.105(10) -0.016(13) C3T 0.330(17) 0.353(18) 0.153(9) 0.024(11) 0.150(11) -0.009(14) C4T 0.295(16) 0.259(16) 0.184(11) 0.037(11) 0.090(12) 0.046(13) C5T 0.242(13) 0.188(11) 0.206(11) -0.086(9) 0.105(10) -0.005(11) C6T 0.290(16) 0.193(13) 0.307(16) -0.084(13) 0.046(13) -0.032(12) _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 N1 2.075(3) . ? Mn1 N2 2.095(3) . ? Mn1 N1 2.097(3) 11_655 ? Mn1 N6 2.150(3) 2_545 ? Mn1 Mn1 3.2187(9) 12 ? Mn1 Mn1 3.2187(9) 11_655 ? Mn1 Mn2 3.2609(8) . ? Mn2 N1 2.183(3) . ? Mn2 N3 2.195(4) . ? Mn2 N5 2.300(3) . ? Mn2 C5 2.490(6) . ? Mn2 C4 2.508(6) . ? Mn2 C1 2.466(5) . ? Mn2 C3 2.470(6) . ? Mn2 C2 2.450(6) . ? Mn2 C21 2.644(4) . ? N2 C11 1.329(5) . ? N1 C21 1.329(5) . ? N1 Mn1 2.097(3) 12 ? N4 C11 1.360(6) . ? N4 C13 1.301(7) . ? N3 C15 1.358(6) . ? N3 C11 1.354(6) . ? N5 C23 1.331(5) . ? N5 C21 1.383(5) . ? N6 C21 1.364(5) . ? N6 C25 1.325(5) . ? N6 Mn1 2.150(3) 2_545 ? O4 C13 1.355(7) . ? O4 C18 1.448(10) . ? O6 C25 1.347(5) . ? O6 C28 1.432(6) . ? C1 C2 1.357(9) . ? C1 C5 1.410(10) . ? C2 C3 1.317(9) . ? C3 C4 1.327(10) . ? C4 C5 1.392(11) . ? C13 C14 1.389(9) . ? C14 C15 1.354(8) . ? C15 C17 1.507(8) . ? C23 C27 1.504(6) . ? C23 C24 1.373(6) . ? C24 C25 1.375(6) . ? C1S C2S 1.51(2) . ? C1S C2S 1.51(2) 2_545 ? C2S C3S 1.29(3) . ? C3S C4S 1.32(3) . ? C4S C3S 1.32(3) 2_545 ? C1T C2T 1.39 . ? C1T C6T 1.39 . ? C2T C3T 1.39 . ? C3T C4T 1.39 . ? C4T C5T 1.39 . ? C5T C6T 1.39 . ? 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 N1 Mn1 N2 100.14(13) . . ? N1 Mn1 N1 108.88(11) . 11_655 ? N2 Mn1 N1 103.00(12) . 11_655 ? N1 Mn1 N6 118.25(12) . 2_545 ? N2 Mn1 N6 119.07(13) . 2_545 ? N1 Mn1 N6 106.29(12) 11_655 2_545 ? N1 Mn1 Mn1 39.77(8) . 12 ? N2 Mn1 Mn1 111.58(10) . 12 ? N1 Mn1 Mn1 69.20(9) 11_655 12 ? N6 Mn1 Mn1 128.49(8) 2_545 12 ? N1 Mn1 Mn1 102.14(8) . 11_655 ? N2 Mn1 Mn1 141.07(10) . 11_655 ? N1 Mn1 Mn1 39.27(8) 11_655 11_655 ? N6 Mn1 Mn1 76.55(8) 2_545 11_655 ? Mn1 Mn1 Mn1 69.93(2) 12 11_655 ? N1 Mn1 Mn2 41.24(8) . . ? N2 Mn1 Mn2 59.43(11) . . ? N1 Mn1 Mn2 121.51(9) 11_655 . ? N6 Mn1 Mn2 131.61(8) 2_545 . ? Mn1 Mn1 Mn2 68.72(2) 12 . ? Mn1 Mn1 Mn2 138.65(2) 11_655 . ? N1 Mn2 N3 106.20(12) . . ? N1 Mn2 N5 61.47(11) . . ? N3 Mn2 N5 103.07(14) . . ? N1 Mn2 C5 151.8(3) . . ? N3 Mn2 C5 101.6(3) . . ? N5 Mn2 C5 107.6(2) . . ? N1 Mn2 C4 152.8(3) . . ? N3 Mn2 C4 87.1(2) . . ? N5 Mn2 C4 139.6(3) . . ? C5 Mn2 C4 32.3(3) . . ? N1 Mn2 C1 119.2(2) . . ? N3 Mn2 C1 134.6(2) . . ? N5 Mn2 C1 96.9(2) . . ? C5 Mn2 C1 33.1(3) . . ? C4 Mn2 C1 53.1(2) . . ? N1 Mn2 C3 122.0(2) . . ? N3 Mn2 C3 105.6(2) . . ? N5 Mn2 C3 148.0(2) . . ? C5 Mn2 C3 52.6(2) . . ? C4 Mn2 C3 30.9(2) . . ? C1 Mn2 C3 52.1(2) . . ? N1 Mn2 C2 106.1(2) . . ? N3 Mn2 C2 136.3(2) . . ? N5 Mn2 C2 118.0(2) . . ? C5 Mn2 C2 53.7(2) . . ? C4 Mn2 C2 52.2(2) . . ? C1 Mn2 C2 32.1(2) . . ? C3 Mn2 C2 31.1(2) . . ? N1 Mn2 C21 30.08(11) . . ? N3 Mn2 C21 105.16(13) . . ? N5 Mn2 C21 31.51(11) . . ? C5 Mn2 C21 135.3(3) . . ? C4 Mn2 C21 165.9(2) . . ? C1 Mn2 C21 112.8(2) . . ? C3 Mn2 C21 144.5(2) . . ? C2 Mn2 C21 117.5(2) . . ? N1 Mn2 Mn1 38.81(8) . . ? N3 Mn2 Mn1 74.90(9) . . ? N5 Mn2 Mn1 90.50(9) . . ? C5 Mn2 Mn1 161.9(2) . . ? C4 Mn2 Mn1 129.8(3) . . ? C1 Mn2 Mn1 145.7(2) . . ? C3 Mn2 Mn1 110.5(2) . . ? C2 Mn2 Mn1 116.69(15) . . ? C21 Mn2 Mn1 61.76(8) . . ? C11 N2 Mn1 127.5(3) . . ? C21 N1 Mn1 128.0(2) . . ? C21 N1 Mn2 94.6(2) . . ? Mn1 N1 Mn2 99.94(13) . . ? C21 N1 Mn1 115.8(2) . 12 ? Mn1 N1 Mn1 100.96(12) . 12 ? Mn2 N1 Mn1 117.38(14) . 12 ? C11 N4 C13 116.4(5) . . ? C15 N3 C11 117.5(4) . . ? C15 N3 Mn2 129.9(3) . . ? C11 N3 Mn2 105.8(3) . . ? C23 N5 C21 118.4(4) . . ? C23 N5 Mn2 153.3(3) . . ? C21 N5 Mn2 88.1(2) . . ? C21 N6 C25 117.5(3) . . ? C21 N6 Mn1 116.5(2) . 2_545 ? C25 N6 Mn1 125.7(3) . 2_545 ? C13 O4 C18 116.8(5) . . ? C25 O6 C28 117.4(4) . . ? C2 C1 C5 107.4(6) . . ? C2 C1 Mn2 73.3(3) . . ? C5 C1 Mn2 74.4(4) . . ? C1 C2 C3 108.4(6) . . ? C1 C2 Mn2 74.6(4) . . ? C3 C2 Mn2 75.3(4) . . ? C4 C3 C2 111.1(7) . . ? C4 C3 Mn2 76.2(4) . . ? C2 C3 Mn2 73.7(4) . . ? C3 C4 C5 107.9(6) . . ? C3 C4 Mn2 72.9(4) . . ? C5 C4 Mn2 73.1(3) . . ? C4 C5 C1 105.1(6) . . ? C4 C5 Mn2 74.6(4) . . ? C1 C5 Mn2 72.5(3) . . ? N4 C11 N3 123.6(4) . . ? N4 C11 N2 119.7(4) . . ? N3 C11 N2 116.6(4) . . ? N4 C13 C14 123.8(5) . . ? N4 C13 O4 119.4(6) . . ? C14 C13 O4 116.7(6) . . ? C13 C14 C15 117.4(5) . . ? C17 C15 N3 116.3(5) . . ? C17 C15 C14 122.8(5) . . ? N3 C15 C14 120.9(5) . . ? N6 C21 N1 123.1(3) . . ? N6 C21 N5 121.5(3) . . ? N1 C21 N5 115.5(3) . . ? N6 C21 Mn2 175.2(3) . . ? N1 C21 Mn2 55.4(2) . . ? N5 C21 Mn2 60.4(2) . . ? N5 C23 C27 115.9(4) . . ? N5 C23 C24 122.3(4) . . ? C27 C23 C24 121.8(4) . . ? C25 C24 C23 116.5(4) . . ? O6 C25 C24 124.7(4) . . ? O6 C25 N6 111.5(3) . . ? C24 C25 N6 123.8(4) . . ? C2S C1S C2S 118.8(16) . 2_545 ? C3S C2S C1S 117.4(20) . . ? C4S C3S C2S 113.6(27) . . ? C3S C4S C3S 137.9(33) . 2_545 ? C2T C1T C6T 120.0 . . ? C3T C2T C1T 120.0 . . ? C4T C3T C2T 120.0 . . ? C3T C4T C5T 120.0 . . ? C6T C5T C4T 120.0 . . ? C5T C6T C1T 120.0 . . ? _refine_diff_density_max 0.577 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.071 data_dw0134 _database_code_CSD 207483 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H30 Mn N2' _chemical_formula_weight 425.46 _chemical_melting_point ? _chemical_compound_source ? 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2142(4) _cell_length_b 14.7038(5) _cell_length_c 18.9720(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.466(2) _cell_angle_gamma 90.00 _cell_volume 2253.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8861 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method ? _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type multiscan #_exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' #_diffrn_radiation_monochromator graphite #_diffrn_radiation_type MoK\a #_diffrn_radiation_source 'fine-focus sealed tube' #_diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 12131 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3970 _reflns_number_observed 2939 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 285 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0650P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3685 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_obs 0.0457 _refine_ls_wR_factor_all 0.1560 _refine_ls_wR_factor_obs 0.1011 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.423 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.866 _refine_ls_shift/esd_mean 0.051 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn -0.15884(4) 0.17578(2) 0.73355(2) 0.02618(15) Uani 1 d . . N1 N 0.0388(2) 0.13563(13) 0.82472(10) 0.0261(5) Uani 1 d . . H1N H 0.0908(31) 0.1859(16) 0.8295(13) 0.028(7) Uiso 1 d . . N2 N 0.0114(2) 0.09593(14) 0.67537(11) 0.0279(5) Uani 1 d . . H2N H -0.0272(29) 0.0439(17) 0.6737(13) 0.026(7) Uiso 1 d . . C1 C 0.1425(3) 0.0650(2) 0.79951(13) 0.0310(6) Uani 1 d . . H1A H 0.0864(3) 0.0053(2) 0.79829(13) 0.037 Uiso 1 calc R . H1B H 0.2498(3) 0.0605(2) 0.83294(13) 0.037 Uiso 1 calc R . C2 C 0.1718(3) 0.0889(2) 0.72562(12) 0.0309(6) Uani 1 d . . H2A H 0.2315(3) 0.1476(2) 0.72723(12) 0.037 Uiso 1 calc R . H2B H 0.2412(3) 0.0416(2) 0.70866(12) 0.037 Uiso 1 calc R . C10 C -0.0104(3) 0.1122(2) 0.89368(13) 0.0359(6) Uani 1 d . . H10A H -0.0714(3) 0.0538(2) 0.88802(13) 0.043 Uiso 1 calc R . H10B H -0.0873(3) 0.1595(2) 0.90522(13) 0.043 Uiso 1 calc R . C11 C 0.1322(3) 0.1039(2) 0.95576(13) 0.0322(6) Uani 1 d . . C12 C 0.1996(3) 0.0207(2) 0.97984(14) 0.0410(7) Uani 1 d . . H12 H 0.1554(3) -0.0334(2) 0.95651(14) 0.049 Uiso 1 calc R . C13 C 0.3296(4) 0.0149(2) 1.0370(2) 0.0490(8) Uani 1 d . . H13 H 0.3746(4) -0.0429(2) 1.0523(2) 0.059 Uiso 1 calc R . C14 C 0.3941(4) 0.0921(2) 1.0720(2) 0.0513(8) Uani 1 d . . H14 H 0.4826(4) 0.0879(2) 1.1118(2) 0.062 Uiso 1 calc R . C15 C 0.3303(4) 0.1749(2) 1.0492(2) 0.0547(8) Uani 1 d . . H15 H 0.3751(4) 0.2287(2) 1.0729(2) 0.066 Uiso 1 calc R . C16 C 0.2004(4) 0.1808(2) 0.9915(2) 0.0445(7) Uani 1 d . . H16 H 0.1572(4) 0.2389(2) 0.9761(2) 0.053 Uiso 1 calc R . C20 C 0.0414(3) 0.1246(2) 0.60395(13) 0.0397(7) Uani 1 d . . H20A H 0.1158(3) 0.0800(2) 0.58686(13) 0.048 Uiso 1 calc R . H20B H 0.0982(3) 0.1843(2) 0.60850(13) 0.048 Uiso 1 calc R . C21 C -0.1158(3) 0.1321(2) 0.54932(13) 0.0348(6) Uani 1 d . . C22 C -0.1959(3) 0.0553(2) 0.51820(14) 0.0419(7) Uani 1 d . . H22 H -0.1513(3) -0.0030(2) 0.53194(14) 0.050 Uiso 1 calc R . C23 C -0.3397(4) 0.0616(2) 0.4675(2) 0.0543(8) Uani 1 d . . H23 H -0.3927(4) 0.0082(2) 0.4465(2) 0.065 Uiso 1 calc R . C24 C -0.4055(4) 0.1462(3) 0.4477(2) 0.0596(9) Uani 1 d . . H24 H -0.5042(4) 0.1511(3) 0.4130(2) 0.071 Uiso 1 calc R . C25 C -0.3281(4) 0.2231(2) 0.4781(2) 0.0584(9) Uani 1 d . . H25 H -0.3737(4) 0.2812(2) 0.4644(2) 0.070 Uiso 1 calc R . C26 C -0.1841(4) 0.2167(2) 0.52870(15) 0.0461(7) Uani 1 d . . H26 H -0.1317(4) 0.2704(2) 0.54947(15) 0.055 Uiso 1 calc R . C31 C -0.1126(4) 0.3295(2) 0.7144(2) 0.0425(7) Uani 1 d . . C32 C -0.1430(5) 0.3449(2) 0.7834(2) 0.0498(8) Uani 1 d . . C33 C 0.0099(7) 0.3550(2) 0.8273(2) 0.0744(14) Uani 1 d . . C34 C 0.1329(6) 0.3470(2) 0.7856(3) 0.0738(13) Uani 1 d . . C35 C 0.0580(4) 0.3322(2) 0.7166(2) 0.0534(9) Uani 1 d . . H31 H -0.1912(42) 0.3291(19) 0.6737(19) 0.062(10) Uiso 1 d . . H32 H -0.2579(44) 0.3532(20) 0.7980(17) 0.068(10) Uiso 1 d . . H33 H 0.0148(48) 0.3611(24) 0.8692(21) 0.076(14) Uiso 1 d . . H34 H 0.2381(58) 0.3493(25) 0.7991(22) 0.092(15) Uiso 1 d . . H35 H 0.1064(42) 0.3221(19) 0.6752(18) 0.065(11) Uiso 1 d . . C41 C -0.3778(3) 0.0550(2) 0.6903(2) 0.0366(6) Uani 1 d . . C42 C -0.4348(3) 0.1383(2) 0.66049(15) 0.0331(6) Uani 1 d . . C43 C -0.4595(3) 0.1961(2) 0.7164(2) 0.0387(7) Uani 1 d . . C44 C -0.4161(3) 0.1473(2) 0.7805(2) 0.0420(7) Uani 1 d . . C45 C -0.3667(3) 0.0599(2) 0.7642(2) 0.0403(7) Uani 1 d . . H41 H -0.3503(34) 0.0040(19) 0.6644(16) 0.056(9) Uiso 1 d . . H42 H -0.4531(33) 0.1527(17) 0.6112(15) 0.042(8) Uiso 1 d . . H43 H -0.4959(32) 0.2548(18) 0.7111(13) 0.040(8) Uiso 1 d . . H44 H -0.4152(36) 0.1670(18) 0.8240(17) 0.050(9) Uiso 1 d . . H45 H -0.3346(30) 0.0085(17) 0.7954(14) 0.037(7) Uiso 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 0.0226(2) 0.0265(2) 0.0292(2) 0.0003(2) 0.0042(2) -0.00162(14) N1 0.0279(12) 0.0231(11) 0.0281(12) -0.0031(9) 0.0075(9) -0.0046(9) N2 0.0278(12) 0.0270(12) 0.0300(12) -0.0034(9) 0.0083(9) -0.0062(9) C1 0.0260(14) 0.0304(13) 0.036(2) 0.0013(11) 0.0043(11) 0.0040(10) C2 0.0230(14) 0.0387(14) 0.0314(15) -0.0068(11) 0.0061(11) 0.0006(10) C10 0.031(2) 0.048(2) 0.0283(15) -0.0021(12) 0.0053(12) -0.0026(11) C11 0.0292(15) 0.043(2) 0.0257(14) -0.0002(12) 0.0084(11) -0.0038(11) C12 0.044(2) 0.043(2) 0.036(2) 0.0019(13) 0.0067(13) -0.0101(12) C13 0.046(2) 0.058(2) 0.043(2) 0.0181(15) 0.0070(15) 0.0048(14) C14 0.032(2) 0.088(2) 0.032(2) 0.004(2) 0.0009(13) -0.008(2) C15 0.057(2) 0.069(2) 0.036(2) -0.014(2) 0.002(2) -0.019(2) C16 0.048(2) 0.046(2) 0.039(2) -0.0068(13) 0.0063(15) -0.0015(13) C20 0.036(2) 0.056(2) 0.029(2) -0.0055(12) 0.0120(13) -0.0068(12) C21 0.038(2) 0.048(2) 0.0215(14) -0.0018(12) 0.0133(12) -0.0031(12) C22 0.047(2) 0.046(2) 0.033(2) -0.0055(13) 0.0077(14) -0.0019(13) C23 0.049(2) 0.073(2) 0.038(2) -0.009(2) 0.001(2) -0.011(2) C24 0.047(2) 0.093(3) 0.036(2) 0.013(2) 0.002(2) 0.004(2) C25 0.066(2) 0.066(2) 0.047(2) 0.022(2) 0.019(2) 0.015(2) C26 0.058(2) 0.046(2) 0.038(2) 0.0047(14) 0.020(2) -0.0050(14) C31 0.051(2) 0.0220(14) 0.055(2) 0.0011(13) 0.011(2) -0.0042(12) C32 0.069(2) 0.0252(14) 0.061(2) -0.0036(14) 0.026(2) -0.0011(13) C33 0.143(5) 0.024(2) 0.049(3) -0.009(2) -0.002(3) -0.012(2) C34 0.058(3) 0.028(2) 0.125(4) -0.002(2) -0.013(3) -0.012(2) C35 0.057(2) 0.028(2) 0.082(3) -0.002(2) 0.028(2) -0.0084(13) C41 0.0237(15) 0.040(2) 0.044(2) 0.0016(14) -0.0011(12) -0.0031(11) C42 0.0253(15) 0.044(2) 0.029(2) 0.0079(13) 0.0024(12) -0.0013(11) C43 0.0221(15) 0.039(2) 0.053(2) 0.0020(14) 0.0034(13) -0.0002(11) C44 0.030(2) 0.069(2) 0.028(2) -0.008(2) 0.0067(13) -0.0066(13) C45 0.027(2) 0.052(2) 0.038(2) 0.0180(14) -0.0045(13) -0.0104(12) _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 N1 2.226(2) . ? Mn1 N2 2.261(2) . ? Mn1 C31 2.332(2) . ? Mn1 C43 2.450(3) . ? Mn1 C44 2.474(3) . ? Mn1 C42 2.494(3) . ? Mn1 C45 2.553(3) . ? Mn1 C41 2.554(3) . ? N1 C10 1.479(3) . ? N1 C1 1.477(3) . ? N1 H1N 0.85(2) . ? N2 C2 1.483(3) . ? N2 C20 1.482(3) . ? N2 H2N 0.83(2) . ? C1 C2 1.506(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C10 C11 1.508(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C16 1.383(4) . ? C11 C12 1.385(3) . ? C12 C13 1.380(4) . ? C12 H12 0.95 . ? C13 C14 1.372(4) . ? C13 H13 0.95 . ? C14 C15 1.365(4) . ? C14 H14 0.95 . ? C15 C16 1.386(4) . ? C15 H15 0.95 . ? C16 H16 0.95 . ? C20 C21 1.506(4) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.384(4) . ? C21 C26 1.391(4) . ? C22 C23 1.385(4) . ? C22 H22 0.95 . ? C23 C24 1.380(4) . ? C23 H23 0.95 . ? C24 C25 1.373(5) . ? C24 H24 0.95 . ? C25 C26 1.384(4) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C31 C32 1.394(4) . ? C31 C35 1.395(4) . ? C31 H31 0.91(3) . ? C32 C33 1.383(5) . ? C32 H32 1.04(3) . ? C33 C34 1.396(6) . ? C33 H33 0.79(4) . ? C34 C35 1.359(6) . ? C34 H34 0.86(5) . ? C35 H35 0.95(3) . ? C41 C42 1.394(4) . ? C41 C45 1.390(4) . ? C41 H41 0.95(3) . ? C42 C43 1.402(4) . ? C42 H42 0.94(3) . ? C43 C44 1.402(4) . ? C43 H43 0.91(3) . ? C44 C45 1.399(4) . ? C44 H44 0.87(3) . ? C45 H45 0.97(3) . ? 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 N1 Mn1 N2 79.22(7) . . ? N1 Mn1 C31 105.17(10) . . ? N2 Mn1 C31 107.14(10) . . ? N1 Mn1 C43 135.30(9) . . ? N2 Mn1 C43 134.13(9) . . ? C31 Mn1 C43 92.87(10) . . ? N1 Mn1 C44 103.03(9) . . ? N2 Mn1 C44 137.08(9) . . ? C31 Mn1 C44 113.23(11) . . ? C43 Mn1 C44 33.07(9) . . ? N1 Mn1 C42 146.52(8) . . ? N2 Mn1 C42 101.20(8) . . ? C31 Mn1 C42 106.55(11) . . ? C43 Mn1 C42 32.93(9) . . ? C44 Mn1 C42 54.07(9) . . ? N1 Mn1 C45 93.98(8) . . ? N2 Mn1 C45 105.26(9) . . ? C31 Mn1 C45 144.80(11) . . ? C43 Mn1 C45 53.97(9) . . ? C44 Mn1 C45 32.25(9) . . ? C42 Mn1 C45 53.24(9) . . ? N1 Mn1 C41 115.90(8) . . ? N2 Mn1 C41 86.80(8) . . ? C31 Mn1 C41 138.51(11) . . ? C43 Mn1 C41 53.70(9) . . ? C44 Mn1 C41 53.13(10) . . ? C42 Mn1 C41 32.03(8) . . ? C45 Mn1 C41 31.60(9) . . ? C10 N1 C1 112.9(2) . . ? C10 N1 Mn1 118.09(15) . . ? C1 N1 Mn1 108.48(14) . . ? C10 N1 H1N 108.8(17) . . ? C1 N1 H1N 109.7(17) . . ? Mn1 N1 H1N 97.6(17) . . ? C2 N2 C20 109.4(2) . . ? C2 N2 Mn1 106.15(13) . . ? C20 N2 Mn1 121.3(2) . . ? C2 N2 H2N 104.5(17) . . ? C20 N2 H2N 110.7(17) . . ? Mn1 N2 H2N 103.5(17) . . ? N1 C1 C2 109.6(2) . . ? N1 C1 H1A 109.75(12) . . ? C2 C1 H1A 109.74(12) . . ? N1 C1 H1B 109.74(12) . . ? C2 C1 H1B 109.74(13) . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 109.9(2) . . ? N2 C2 H2A 109.67(12) . . ? C1 C2 H2A 109.67(12) . . ? N2 C2 H2B 109.68(12) . . ? C1 C2 H2B 109.68(12) . . ? H2A C2 H2B 108.2 . . ? N1 C10 C11 114.3(2) . . ? N1 C10 H10A 108.69(12) . . ? C11 C10 H10A 108.68(14) . . ? N1 C10 H10B 108.68(13) . . ? C11 C10 H10B 108.69(13) . . ? H10A C10 H10B 107.6 . . ? C16 C11 C12 117.3(2) . . ? C16 C11 C10 120.3(2) . . ? C12 C11 C10 122.4(2) . . ? C13 C12 C11 121.3(3) . . ? C13 C12 H12 119.3(2) . . ? C11 C12 H12 119.3(2) . . ? C14 C13 C12 120.3(3) . . ? C14 C13 H13 119.8(2) . . ? C12 C13 H13 119.9(2) . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14 120.3(2) . . ? C13 C14 H14 120.2(2) . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 119.9(2) . . ? C16 C15 H15 119.9(2) . . ? C15 C16 C11 121.4(3) . . ? C15 C16 H16 119.3(2) . . ? C11 C16 H16 119.3(2) . . ? N2 C20 C21 112.7(2) . . ? N2 C20 H20A 109.05(13) . . ? C21 C20 H20A 109.06(14) . . ? N2 C20 H20B 109.05(13) . . ? C21 C20 H20B 109.04(14) . . ? H20A C20 H20B 107.8 . . ? C22 C21 C26 118.2(3) . . ? C22 C21 C20 121.0(2) . . ? C26 C21 C20 120.7(2) . . ? C23 C22 C21 121.4(3) . . ? C23 C22 H22 119.3(2) . . ? C21 C22 H22 119.3(2) . . ? C22 C23 C24 119.5(3) . . ? C22 C23 H23 120.3(2) . . ? C24 C23 H23 120.3(2) . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0(2) . . ? C23 C24 H24 120.0(2) . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25 119.8(2) . . ? C24 C25 H25 119.8(2) . . ? C25 C26 C21 120.4(3) . . ? C25 C26 H26 119.8(2) . . ? C21 C26 H26 119.8(2) . . ? C32 C31 C35 108.5(3) . . ? C32 C31 Mn1 87.1(2) . . ? C35 C31 Mn1 102.4(2) . . ? C32 C31 H31 125.2(21) . . ? C35 C31 H31 125.3(22) . . ? Mn1 C31 H31 90.8(18) . . ? C33 C32 C31 106.5(4) . . ? C33 C32 H32 126.6(19) . . ? C31 C32 H32 126.6(19) . . ? C34 C33 C32 108.7(4) . . ? C34 C33 H33 131.8(30) . . ? C32 C33 H33 119.3(30) . . ? C35 C34 C33 108.1(4) . . ? C35 C34 H34 123.4(28) . . ? C33 C34 H34 128.5(28) . . ? C34 C35 C31 108.0(4) . . ? C34 C35 H35 129.4(21) . . ? C31 C35 H35 122.5(21) . . ? C42 C41 C45 108.7(3) . . ? C42 C41 Mn1 71.62(15) . . ? C45 C41 Mn1 74.2(2) . . ? C42 C41 H41 125.4(18) . . ? C45 C41 H41 125.9(18) . . ? Mn1 C41 H41 119.9(17) . . ? C41 C42 C43 108.0(3) . . ? C41 C42 Mn1 76.35(15) . . ? C43 C42 Mn1 71.79(15) . . ? C41 C42 H42 125.5(16) . . ? C43 C42 H42 126.5(16) . . ? Mn1 C42 H42 117.8(16) . . ? C44 C43 C42 107.3(2) . . ? C44 C43 Mn1 74.4(2) . . ? C42 C43 Mn1 75.3(2) . . ? C44 C43 H43 127.3(16) . . ? C42 C43 H43 125.3(16) . . ? Mn1 C43 H43 115.6(17) . . ? C43 C44 C45 108.5(3) . . ? C43 C44 Mn1 72.5(2) . . ? C45 C44 Mn1 77.0(2) . . ? C43 C44 H44 127.3(18) . . ? C45 C44 H44 124.2(18) . . ? Mn1 C44 H44 115.0(19) . . ? C41 C45 C44 107.5(3) . . ? C41 C45 Mn1 74.22(15) . . ? C44 C45 Mn1 70.7(2) . . ? C41 C45 H45 122.5(15) . . ? C44 C45 H45 129.9(15) . . ? Mn1 C45 H45 122.8(15) . . ? _refine_diff_density_max 0.267 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.069