# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1581 data_mx401 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H54 As2 Mn2 N4' _chemical_formula_weight 778.53 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' 'As' 'As' 0.0499 2.0058 '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 10.336(2) _cell_length_b 17.095(6) _cell_length_c 20.506(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.99(2) _cell_angle_gamma 90.00 _cell_volume 3515.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 2.615 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.2738 _exptl_absorpt_correction_T_max 0.3445 _exptl_absorpt_process_details ? _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_type 'Bruker P$' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6294 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 23.01 _reflns_number_total 4893 _reflns_number_gt 3271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS ' _computing_cell_refinement 'Bruker XSCANS ' _computing_data_reduction 'Bruker XSCANS ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+35.6456P] 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 4893 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.759 _refine_ls_shift/su_mean 0.094 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 As1 As 0.95176(9) 0.91505(6) 0.22540(5) 0.0328(3) Uani 1 1 d . . . As2 As 0.97658(9) 0.76168(6) 0.28610(5) 0.0342(3) Uani 1 1 d . . . Mn1 Mn 0.74502(14) 0.86900(9) 0.30329(7) 0.0368(4) Uani 1 1 d . . . Mn2 Mn 0.72497(14) 0.79383(9) 0.17261(7) 0.0374(4) Uani 1 1 d . . . N1A N 0.9511(7) 0.8064(4) 0.1979(4) 0.0318(19) Uani 1 1 d . . . C1A C 1.0467(9) 0.7841(6) 0.1572(5) 0.038(3) Uani 1 1 d . . . H1A H 1.1383 0.7967 0.1829 0.046 Uiso 1 1 calc R . . C2A C 1.0389(10) 0.6990(6) 0.1411(5) 0.044(3) Uani 1 1 d . . . H2A1 H 0.9473 0.6855 0.1177 0.053 Uiso 1 1 calc R . . H2A2 H 1.0625 0.6688 0.1829 0.053 Uiso 1 1 calc R . . C3A C 1.1342(11) 0.6775(7) 0.0964(6) 0.059(3) Uani 1 1 d . . . H3A1 H 1.2266 0.6862 0.1214 0.071 Uiso 1 1 calc R . . H3A2 H 1.1241 0.6219 0.0846 0.071 Uiso 1 1 calc R . . C4A C 1.1050(11) 0.7269(7) 0.0317(6) 0.061(3) Uani 1 1 d . . . H4A1 H 1.1712 0.7150 0.0060 0.073 Uiso 1 1 calc R . . H4A2 H 1.0168 0.7131 0.0038 0.073 Uiso 1 1 calc R . . C5A C 1.1088(11) 0.8136(7) 0.0475(5) 0.055(3) Uani 1 1 d . . . H5A1 H 1.1999 0.8289 0.0704 0.066 Uiso 1 1 calc R . . H5A2 H 1.0824 0.8436 0.0057 0.066 Uiso 1 1 calc R . . C6A C 1.0148(10) 0.8319(6) 0.0922(5) 0.039(3) Uani 1 1 d . . . H6A1 H 0.9230 0.8209 0.0674 0.047 Uiso 1 1 calc R . . H6A2 H 1.0208 0.8877 0.1034 0.047 Uiso 1 1 calc R . . N1B N 0.7977(7) 0.7507(4) 0.2760(4) 0.0287(18) Uani 1 1 d . . . C1B C 0.7558(9) 0.6779(5) 0.3078(4) 0.031(2) Uani 1 1 d . . . H1B H 0.6576 0.6800 0.3003 0.038 Uiso 1 1 calc R . . C2B C 0.7893(10) 0.6001(6) 0.2783(5) 0.045(3) Uani 1 1 d . . . H2B1 H 0.7473 0.5987 0.2300 0.053 Uiso 1 1 calc R . . H2B2 H 0.8860 0.5962 0.2840 0.053 Uiso 1 1 calc R . . C3B C 0.7410(11) 0.5309(7) 0.3124(6) 0.055(3) Uani 1 1 d . . . H3B1 H 0.6434 0.5321 0.3024 0.066 Uiso 1 1 calc R . . H3B2 H 0.7674 0.4824 0.2937 0.066 Uiso 1 1 calc R . . C4B C 0.7954(12) 0.5302(7) 0.3879(6) 0.062(3) Uani 1 1 d . . . H4B1 H 0.8923 0.5227 0.3987 0.074 Uiso 1 1 calc R . . H4B2 H 0.7558 0.4869 0.4076 0.074 Uiso 1 1 calc R . . C5B C 0.7621(11) 0.6081(7) 0.4172(5) 0.056(3) Uani 1 1 d . . . H5B1 H 0.6653 0.6128 0.4104 0.067 Uiso 1 1 calc R . . H5B2 H 0.8022 0.6092 0.4656 0.067 Uiso 1 1 calc R . . C6B C 0.8135(11) 0.6763(7) 0.3842(5) 0.046(3) Uani 1 1 d . . . H6B1 H 0.9110 0.6732 0.3935 0.055 Uiso 1 1 calc R . . H6B2 H 0.7904 0.7251 0.4037 0.055 Uiso 1 1 calc R . . N1C N 0.7711(7) 0.9173(4) 0.2094(4) 0.0281(17) Uani 1 1 d . . . C1C C 0.7051(10) 0.9892(6) 0.1740(5) 0.039(2) Uani 1 1 d . . . H1C H 0.6082 0.9834 0.1698 0.047 Uiso 1 1 calc R . . C2C C 0.7244(11) 0.9982(7) 0.1029(5) 0.048(3) Uani 1 1 d . . . H2C1 H 0.6930 0.9508 0.0771 0.058 Uiso 1 1 calc R . . H2C2 H 0.8197 1.0042 0.1050 0.058 Uiso 1 1 calc R . . C3C C 0.6477(11) 1.0700(7) 0.0662(5) 0.054(3) Uani 1 1 d . . . H3C1 H 0.6670 1.0759 0.0220 0.065 Uiso 1 1 calc R . . H3C2 H 0.5516 1.0616 0.0595 0.065 Uiso 1 1 calc R . . C4C C 0.6874(12) 1.1434(7) 0.1065(5) 0.062(3) Uani 1 1 d . . . H4C1 H 0.6333 1.1870 0.0837 0.074 Uiso 1 1 calc R . . H4C2 H 0.7809 1.1551 0.1080 0.074 Uiso 1 1 calc R . . C5C C 0.6709(11) 1.1377(6) 0.1773(6) 0.051(3) Uani 1 1 d . . . H5C1 H 0.5760 1.1331 0.1766 0.061 Uiso 1 1 calc R . . H5C2 H 0.7054 1.1852 0.2022 0.061 Uiso 1 1 calc R . . C6C C 0.7481(10) 1.0646(6) 0.2132(5) 0.046(3) Uani 1 1 d . . . H6C1 H 0.8440 1.0723 0.2184 0.055 Uiso 1 1 calc R . . H6C2 H 0.7320 1.0596 0.2582 0.055 Uiso 1 1 calc R . . N1D N 0.9677(7) 0.8699(4) 0.3123(3) 0.0276(17) Uani 1 1 d . . . C1D C 1.0736(8) 0.8993(5) 0.3713(4) 0.029(2) Uani 1 1 d . . . H1D H 1.0618 0.8703 0.4112 0.035 Uiso 1 1 calc R . . C2D C 1.2164(9) 0.8848(6) 0.3666(5) 0.042(3) Uani 1 1 d . . . H2D1 H 1.2310 0.8284 0.3634 0.050 Uiso 1 1 calc R . . H2D2 H 1.2308 0.9096 0.3259 0.050 Uiso 1 1 calc R . . C3D C 1.3164(9) 0.9176(6) 0.4280(5) 0.045(3) Uani 1 1 d . . . H3D1 H 1.3099 0.8881 0.4680 0.054 Uiso 1 1 calc R . . H3D2 H 1.4070 0.9112 0.4220 0.054 Uiso 1 1 calc R . . C4D C 1.2912(10) 1.0024(7) 0.4384(5) 0.051(3) Uani 1 1 d . . . H4D1 H 1.3062 1.0327 0.4003 0.061 Uiso 1 1 calc R . . H4D2 H 1.3542 1.0209 0.4791 0.061 Uiso 1 1 calc R . . C5D C 1.1490(10) 1.0159(7) 0.4449(5) 0.054(3) Uani 1 1 d . . . H5D1 H 1.1340 1.0721 0.4494 0.065 Uiso 1 1 calc R . . H5D2 H 1.1364 0.9898 0.4855 0.065 Uiso 1 1 calc R . . C6D C 1.0481(10) 0.9841(6) 0.3833(5) 0.046(3) Uani 1 1 d . . . H6D1 H 0.9578 0.9899 0.3899 0.055 Uiso 1 1 calc R . . H6D2 H 1.0535 1.0147 0.3436 0.055 Uiso 1 1 calc R . . C1E C 0.5690(13) 0.8338(9) 0.3574(7) 0.070(4) Uani 1 1 d . . . H1E H 0.5509 0.7803 0.3614 0.085 Uiso 1 1 calc R . . C2E C 0.6639(11) 0.8790(7) 0.4026(5) 0.047(3) Uani 1 1 d . . . H2E H 0.7226 0.8615 0.4424 0.056 Uiso 1 1 calc R . . C3E C 0.6541(11) 0.9542(6) 0.3772(5) 0.046(3) Uani 1 1 d . . . H3E H 0.7057 0.9970 0.3974 0.055 Uiso 1 1 calc R . . C4E C 0.5574(11) 0.9571(7) 0.3181(5) 0.050(3) Uani 1 1 d . . . H4E H 0.5311 1.0017 0.2913 0.060 Uiso 1 1 calc R . . C5E C 0.5066(12) 0.8839(9) 0.3051(7) 0.072(4) Uani 1 1 d . . . H5E H 0.4401 0.8692 0.2671 0.086 Uiso 1 1 calc R . . C1F C 0.5012(13) 0.8209(7) 0.1030(8) 0.077(5) Uani 1 1 d . . . H1F H 0.4658 0.8716 0.1022 0.093 Uiso 1 1 calc R . . C2F C 0.5797(14) 0.7927(8) 0.0622(6) 0.069(4) Uani 1 1 d . . . H2F H 0.6102 0.8215 0.0299 0.082 Uiso 1 1 calc R . . C3F C 0.6051(12) 0.7141(8) 0.0774(6) 0.062(3) Uani 1 1 d . . . H3F H 0.6541 0.6808 0.0558 0.075 Uiso 1 1 calc R . . C4F C 0.5477(11) 0.6922(8) 0.1290(6) 0.060(3) Uani 1 1 d . . . H4F H 0.5501 0.6426 0.1490 0.073 Uiso 1 1 calc R . . C5F C 0.4848(11) 0.7603(9) 0.1454(7) 0.067(4) Uani 1 1 d . . . H5F H 0.4389 0.7640 0.1796 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0287(6) 0.0406(6) 0.0296(5) 0.0004(5) 0.0081(4) 0.0015(5) As2 0.0275(5) 0.0406(6) 0.0338(5) 0.0016(5) 0.0061(4) 0.0014(5) Mn1 0.0298(8) 0.0486(10) 0.0341(8) -0.0008(7) 0.0116(6) 0.0031(7) Mn2 0.0304(8) 0.0471(10) 0.0327(8) -0.0012(7) 0.0038(6) 0.0019(7) N1A 0.030(4) 0.036(5) 0.031(4) 0.004(4) 0.012(4) 0.003(4) C1A 0.022(5) 0.058(7) 0.034(5) -0.009(5) 0.005(4) -0.010(5) C2A 0.046(7) 0.036(6) 0.049(6) -0.020(5) 0.012(5) -0.007(5) C3A 0.050(7) 0.046(7) 0.090(9) -0.018(7) 0.035(7) 0.003(6) C4A 0.051(7) 0.079(9) 0.060(7) -0.031(7) 0.029(6) -0.013(7) C5A 0.056(7) 0.077(9) 0.035(6) -0.009(6) 0.017(5) -0.005(6) C6A 0.040(6) 0.043(6) 0.038(6) -0.001(5) 0.012(5) 0.014(5) N1B 0.027(4) 0.018(4) 0.040(4) 0.012(3) 0.006(3) 0.008(3) C1B 0.030(5) 0.030(5) 0.031(5) 0.006(4) 0.003(4) 0.008(4) C2B 0.034(6) 0.060(8) 0.040(6) -0.008(6) 0.011(5) -0.001(5) C3B 0.050(7) 0.049(7) 0.069(8) 0.002(6) 0.019(6) 0.012(6) C4B 0.060(8) 0.050(8) 0.077(9) 0.014(7) 0.018(7) -0.008(6) C5B 0.056(7) 0.074(9) 0.038(6) 0.011(6) 0.012(5) -0.006(6) C6B 0.047(7) 0.055(7) 0.038(6) 0.000(5) 0.012(5) -0.007(6) N1C 0.029(4) 0.015(4) 0.041(4) 0.004(4) 0.011(4) 0.006(3) C1C 0.032(6) 0.047(7) 0.035(6) -0.001(5) 0.003(4) 0.006(5) C2C 0.048(7) 0.062(8) 0.037(6) 0.005(6) 0.014(5) 0.005(6) C3C 0.058(7) 0.060(8) 0.040(6) 0.015(6) 0.001(5) 0.007(6) C4C 0.057(8) 0.071(9) 0.049(7) 0.015(7) -0.002(6) 0.000(7) C5C 0.044(7) 0.038(7) 0.065(8) 0.009(6) 0.000(6) 0.008(5) C6C 0.032(6) 0.072(8) 0.034(6) 0.005(6) 0.007(5) 0.003(6) N1D 0.031(4) 0.021(4) 0.029(4) -0.001(3) 0.003(3) -0.007(3) C1D 0.028(5) 0.032(6) 0.026(5) 0.000(4) 0.006(4) -0.001(4) C2D 0.029(6) 0.042(6) 0.053(6) -0.003(5) 0.006(5) 0.007(5) C3D 0.026(6) 0.061(7) 0.047(6) -0.018(6) 0.009(5) -0.003(5) C4D 0.045(7) 0.070(9) 0.035(6) -0.004(6) 0.006(5) -0.017(6) C5D 0.052(7) 0.057(8) 0.049(7) -0.018(6) 0.001(6) 0.011(6) C6D 0.038(6) 0.054(7) 0.042(6) -0.007(5) 0.000(5) 0.010(5) C1E 0.054(8) 0.095(11) 0.080(9) 0.000(9) 0.050(8) -0.005(8) C2E 0.045(7) 0.052(8) 0.046(6) -0.005(6) 0.017(5) 0.004(6) C3E 0.052(7) 0.036(7) 0.054(7) -0.014(6) 0.022(6) -0.004(5) C4E 0.051(7) 0.061(8) 0.038(6) 0.007(6) 0.012(5) 0.024(6) C5E 0.040(7) 0.108(12) 0.077(10) -0.055(9) 0.031(7) -0.022(8) C1F 0.053(8) 0.030(7) 0.120(13) -0.019(8) -0.035(8) 0.001(6) C2F 0.072(9) 0.066(10) 0.048(7) 0.006(7) -0.023(7) -0.022(8) C3F 0.064(8) 0.064(9) 0.054(7) -0.025(7) 0.003(6) -0.010(7) C4F 0.043(7) 0.060(9) 0.065(8) 0.008(7) -0.012(6) -0.016(6) C5F 0.030(7) 0.088(11) 0.081(9) -0.019(9) 0.009(6) -0.008(7) _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 As1 N1C 1.816(7) . ? As1 N1D 1.912(7) . ? As1 N1A 1.940(8) . ? As1 As2 2.8872(16) . ? As1 Mn1 3.0639(18) . ? As2 N1B 1.820(7) . ? As2 N1A 1.923(7) . ? As2 N1D 1.935(7) . ? Mn1 N1C 2.170(7) . ? Mn1 N1B 2.202(7) . ? Mn1 N1D 2.264(7) . ? Mn1 C2E 2.389(10) . ? Mn1 C1E 2.425(11) . ? Mn1 C3E 2.449(10) . ? Mn1 C5E 2.487(11) . ? Mn1 C4E 2.530(10) . ? Mn1 Mn2 2.934(2) . ? Mn2 N1B 2.198(7) . ? Mn2 N1C 2.253(7) . ? Mn2 N1A 2.278(7) . ? Mn2 C2F 2.395(11) . ? Mn2 C1F 2.450(12) . ? Mn2 C3F 2.456(11) . ? Mn2 C5F 2.476(11) . ? Mn2 C4F 2.526(11) . ? N1A C1A 1.489(11) . ? C1A C2A 1.489(14) . ? C1A C6A 1.529(13) . ? C1A H1A 0.9900 . ? C2A C3A 1.545(13) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C3A C4A 1.540(16) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C4A C5A 1.516(16) . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C5A C6A 1.520(13) . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? N1B C1B 1.516(11) . ? C1B C2B 1.535(13) . ? C1B C6B 1.535(12) . ? C1B H1B 0.9900 . ? C2B C3B 1.518(14) . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C3B C4B 1.513(15) . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C4B C5B 1.534(16) . ? C4B H4B1 0.9800 . ? C4B H4B2 0.9800 . ? C5B C6B 1.506(14) . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? N1C C1C 1.506(12) . ? C1C C6C 1.527(14) . ? C1C C2C 1.526(13) . ? C1C H1C 0.9900 . ? C2C C3C 1.554(14) . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C3C C4C 1.503(16) . ? C3C H3C1 0.9800 . ? C3C H3C2 0.9800 . ? C4C C5C 1.506(15) . ? C4C H4C1 0.9800 . ? C4C H4C2 0.9800 . ? C5C C6C 1.568(14) . ? C5C H5C1 0.9800 . ? C5C H5C2 0.9800 . ? C6C H6C1 0.9800 . ? C6C H6C2 0.9800 . ? N1D C1D 1.508(11) . ? C1D C6D 1.505(13) . ? C1D C2D 1.522(12) . ? C1D H1D 0.9900 . ? C2D C3D 1.529(13) . ? C2D H2D1 0.9800 . ? C2D H2D2 0.9800 . ? C3D C4D 1.497(15) . ? C3D H3D1 0.9800 . ? C3D H3D2 0.9800 . ? C4D C5D 1.525(14) . ? C4D H4D1 0.9800 . ? C4D H4D2 0.9800 . ? C5D C6D 1.531(13) . ? C5D H5D1 0.9800 . ? C5D H5D2 0.9800 . ? C6D H6D1 0.9800 . ? C6D H6D2 0.9800 . ? C1E C5E 1.402(18) . ? C1E C2E 1.408(16) . ? C1E H1E 0.9400 . ? C2E C3E 1.382(15) . ? C2E H2E 0.9400 . ? C3E C4E 1.374(14) . ? C3E H3E 0.9400 . ? C4E C5E 1.358(17) . ? C4E H4E 0.9400 . ? C5E H5E 0.9400 . ? C1F C5F 1.388(18) . ? C1F C2F 1.385(18) . ? C1F H1F 0.9400 . ? C2F C3F 1.389(17) . ? C2F H2F 0.9400 . ? C3F C4F 1.385(16) . ? C3F H3F 0.9400 . ? C4F C5F 1.412(17) . ? C4F H4F 0.9400 . ? C5F H5F 0.9400 . ? 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 N1C As1 N1D 91.7(3) . . ? N1C As1 N1A 92.1(3) . . ? N1D As1 N1A 83.0(3) . . ? N1C As1 As2 94.4(2) . . ? N1D As1 As2 41.7(2) . . ? N1A As1 As2 41.4(2) . . ? N1C As1 Mn1 44.2(2) . . ? N1D As1 Mn1 47.5(2) . . ? N1A As1 Mn1 87.2(2) . . ? As2 As1 Mn1 62.77(4) . . ? N1B As2 N1A 91.7(3) . . ? N1B As2 N1D 90.9(3) . . ? N1A As2 N1D 82.9(3) . . ? N1B As2 As1 93.6(2) . . ? N1A As2 As1 41.9(2) . . ? N1D As2 As1 41.1(2) . . ? N1C Mn1 N1B 91.9(3) . . ? N1C Mn1 N1D 74.2(3) . . ? N1B Mn1 N1D 73.6(3) . . ? N1C Mn1 C2E 150.9(3) . . ? N1B Mn1 C2E 116.2(3) . . ? N1D Mn1 C2E 119.3(3) . . ? N1C Mn1 C1E 140.2(4) . . ? N1B Mn1 C1E 98.5(4) . . ? N1D Mn1 C1E 145.6(4) . . ? C2E Mn1 C1E 34.0(4) . . ? N1C Mn1 C3E 118.1(3) . . ? N1B Mn1 C3E 149.3(3) . . ? N1D Mn1 C3E 118.7(3) . . ? C2E Mn1 C3E 33.2(3) . . ? C1E Mn1 C3E 54.7(4) . . ? N1C Mn1 C5E 108.1(4) . . ? N1B Mn1 C5E 113.9(4) . . ? N1D Mn1 C5E 171.7(3) . . ? C2E Mn1 C5E 55.0(4) . . ? C1E Mn1 C5E 33.1(4) . . ? C3E Mn1 C5E 53.1(4) . . ? N1C Mn1 C4E 98.2(3) . . ? N1B Mn1 C4E 145.2(4) . . ? N1D Mn1 C4E 141.2(4) . . ? C2E Mn1 C4E 54.4(4) . . ? C1E Mn1 C4E 54.0(4) . . ? C3E Mn1 C4E 32.0(3) . . ? C5E Mn1 C4E 31.4(4) . . ? N1C Mn1 Mn2 49.67(19) . . ? N1B Mn1 Mn2 48.14(19) . . ? N1D Mn1 Mn2 85.62(18) . . ? C2E Mn1 Mn2 148.0(3) . . ? C1E Mn1 Mn2 114.4(4) . . ? C3E Mn1 Mn2 150.9(3) . . ? C5E Mn1 Mn2 102.0(3) . . ? C4E Mn1 Mn2 118.9(3) . . ? N1C Mn1 As1 35.70(19) . . ? N1B Mn1 As1 81.78(19) . . ? N1D Mn1 As1 38.50(18) . . ? C2E Mn1 As1 149.2(3) . . ? C1E Mn1 As1 175.8(4) . . ? C3E Mn1 As1 126.2(3) . . ? C5E Mn1 As1 143.1(4) . . ? C4E Mn1 As1 124.1(3) . . ? Mn2 Mn1 As1 62.65(5) . . ? N1B Mn2 N1C 89.8(3) . . ? N1B Mn2 N1A 73.7(3) . . ? N1C Mn2 N1A 73.3(3) . . ? N1B Mn2 C2F 154.0(4) . . ? N1C Mn2 C2F 111.0(4) . . ? N1A Mn2 C2F 126.2(4) . . ? N1B Mn2 C1F 132.8(5) . . ? N1C Mn2 C1F 96.4(3) . . ? N1A Mn2 C1F 152.4(5) . . ? C2F Mn2 C1F 33.2(4) . . ? N1B Mn2 C3F 124.7(4) . . ? N1C Mn2 C3F 144.2(4) . . ? N1A Mn2 C3F 121.7(4) . . ? C2F Mn2 C3F 33.2(4) . . ? C1F Mn2 C3F 54.4(4) . . ? N1B Mn2 C5F 103.3(4) . . ? N1C Mn2 C5F 114.3(4) . . ? N1A Mn2 C5F 172.0(4) . . ? C2F Mn2 C5F 54.5(5) . . ? C1F Mn2 C5F 32.7(4) . . ? C3F Mn2 C5F 53.6(4) . . ? N1B Mn2 C4F 99.2(3) . . ? N1C Mn2 C4F 147.1(4) . . ? N1A Mn2 C4F 139.6(4) . . ? C2F Mn2 C4F 54.9(4) . . ? C1F Mn2 C4F 54.7(4) . . ? C3F Mn2 C4F 32.2(4) . . ? C5F Mn2 C4F 32.8(4) . . ? N1B Mn2 Mn1 48.24(19) . . ? N1C Mn2 Mn1 47.25(18) . . ? N1A Mn2 Mn1 84.76(19) . . ? C2F Mn2 Mn1 139.2(4) . . ? C1F Mn2 Mn1 107.3(4) . . ? C3F Mn2 Mn1 151.6(3) . . ? C5F Mn2 Mn1 98.8(3) . . ? C4F Mn2 Mn1 120.6(3) . . ? C1A N1A As2 117.8(6) . . ? C1A N1A As1 116.9(6) . . ? As2 N1A As1 96.7(3) . . ? C1A N1A Mn2 129.1(6) . . ? As2 N1A Mn2 94.4(3) . . ? As1 N1A Mn2 95.1(3) . . ? C2A C1A N1A 111.5(8) . . ? C2A C1A C6A 109.9(8) . . ? N1A C1A C6A 108.6(8) . . ? C2A C1A H1A 108.9 . . ? N1A C1A H1A 109.0 . . ? C6A C1A H1A 108.9 . . ? C1A C2A C3A 110.9(9) . . ? C1A C2A H2A1 109.4 . . ? C3A C2A H2A1 109.4 . . ? C1A C2A H2A2 109.5 . . ? C3A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 108.1 . . ? C4A C3A C2A 111.1(9) . . ? C4A C3A H3A1 109.4 . . ? C2A C3A H3A1 109.4 . . ? C4A C3A H3A2 109.5 . . ? C2A C3A H3A2 109.4 . . ? H3A1 C3A H3A2 108.0 . . ? C5A C4A C3A 111.2(9) . . ? C5A C4A H4A1 109.3 . . ? C3A C4A H4A1 109.4 . . ? C5A C4A H4A2 109.5 . . ? C3A C4A H4A2 109.3 . . ? H4A1 C4A H4A2 108.0 . . ? C6A C5A C4A 110.0(9) . . ? C6A C5A H5A1 109.6 . . ? C4A C5A H5A1 109.7 . . ? C6A C5A H5A2 109.7 . . ? C4A C5A H5A2 109.6 . . ? H5A1 C5A H5A2 108.2 . . ? C5A C6A C1A 112.4(8) . . ? C5A C6A H6A1 109.1 . . ? C1A C6A H6A1 109.1 . . ? C5A C6A H6A2 109.1 . . ? C1A C6A H6A2 109.2 . . ? H6A1 C6A H6A2 107.9 . . ? C1B N1B As2 115.1(5) . . ? C1B N1B Mn2 128.6(5) . . ? As2 N1B Mn2 100.2(3) . . ? C1B N1B Mn1 122.0(5) . . ? As2 N1B Mn1 100.5(3) . . ? Mn2 N1B Mn1 83.6(2) . . ? N1B C1B C2B 115.2(7) . . ? N1B C1B C6B 111.9(8) . . ? C2B C1B C6B 108.5(8) . . ? N1B C1B H1B 106.9 . . ? C2B C1B H1B 106.9 . . ? C6B C1B H1B 106.9 . . ? C3B C2B C1B 111.2(8) . . ? C3B C2B H2B1 109.4 . . ? C1B C2B H2B1 109.5 . . ? C3B C2B H2B2 109.5 . . ? C1B C2B H2B2 109.2 . . ? H2B1 C2B H2B2 108.0 . . ? C4B C3B C2B 113.3(10) . . ? C4B C3B H3B1 109.0 . . ? C2B C3B H3B1 109.0 . . ? C4B C3B H3B2 108.9 . . ? C2B C3B H3B2 108.8 . . ? H3B1 C3B H3B2 107.7 . . ? C3B C4B C5B 109.3(10) . . ? C3B C4B H4B1 109.8 . . ? C5B C4B H4B1 109.8 . . ? C3B C4B H4B2 109.8 . . ? C5B C4B H4B2 109.9 . . ? H4B1 C4B H4B2 108.2 . . ? C6B C5B C4B 111.0(9) . . ? C6B C5B H5B1 109.4 . . ? C4B C5B H5B1 109.4 . . ? C6B C5B H5B2 109.5 . . ? C4B C5B H5B2 109.4 . . ? H5B1 C5B H5B2 108.0 . . ? C5B C6B C1B 112.3(9) . . ? C5B C6B H6B1 109.2 . . ? C1B C6B H6B1 108.9 . . ? C5B C6B H6B2 109.1 . . ? C1B C6B H6B2 109.3 . . ? H6B1 C6B H6B2 107.9 . . ? C1C N1C As1 115.5(6) . . ? C1C N1C Mn1 126.9(5) . . ? As1 N1C Mn1 100.1(3) . . ? C1C N1C Mn2 124.7(6) . . ? As1 N1C Mn2 99.6(3) . . ? Mn1 N1C Mn2 83.1(2) . . ? N1C C1C C6C 113.2(7) . . ? N1C C1C C2C 113.3(8) . . ? C6C C1C C2C 109.3(9) . . ? N1C C1C H1C 106.9 . . ? C6C C1C H1C 106.9 . . ? C2C C1C H1C 106.9 . . ? C1C C2C C3C 111.9(9) . . ? C1C C2C H2C1 109.3 . . ? C3C C2C H2C1 109.2 . . ? C1C C2C H2C2 109.1 . . ? C3C C2C H2C2 109.4 . . ? H2C1 C2C H2C2 108.0 . . ? C4C C3C C2C 110.7(9) . . ? C4C C3C H3C1 109.5 . . ? C2C C3C H3C1 109.5 . . ? C4C C3C H3C2 109.4 . . ? C2C C3C H3C2 109.6 . . ? H3C1 C3C H3C2 108.1 . . ? C3C C4C C5C 113.4(10) . . ? C3C C4C H4C1 109.0 . . ? C5C C4C H4C1 109.0 . . ? C3C C4C H4C2 108.8 . . ? C5C C4C H4C2 108.8 . . ? H4C1 C4C H4C2 107.7 . . ? C4C C5C C6C 109.9(9) . . ? C4C C5C H5C1 109.6 . . ? C6C C5C H5C1 109.7 . . ? C4C C5C H5C2 109.7 . . ? C6C C5C H5C2 109.7 . . ? H5C1 C5C H5C2 108.2 . . ? C1C C6C C5C 112.0(8) . . ? C1C C6C H6C1 109.0 . . ? C5C C6C H6C1 109.3 . . ? C1C C6C H6C2 109.2 . . ? C5C C6C H6C2 109.3 . . ? H6C1 C6C H6C2 107.9 . . ? C1D N1D As1 119.7(5) . . ? C1D N1D As2 117.9(5) . . ? As1 N1D As2 97.3(3) . . ? C1D N1D Mn1 126.5(5) . . ? As1 N1D Mn1 94.0(3) . . ? As2 N1D Mn1 94.9(3) . . ? C6D C1D N1D 109.3(7) . . ? C6D C1D C2D 112.3(8) . . ? N1D C1D C2D 115.0(7) . . ? C6D C1D H1D 106.6 . . ? N1D C1D H1D 106.6 . . ? C2D C1D H1D 106.6 . . ? C3D C2D C1D 111.2(8) . . ? C3D C2D H2D1 109.4 . . ? C1D C2D H2D1 109.5 . . ? C3D C2D H2D2 109.4 . . ? C1D C2D H2D2 109.3 . . ? H2D1 C2D H2D2 108.0 . . ? C4D C3D C2D 111.5(9) . . ? C4D C3D H3D1 109.3 . . ? C2D C3D H3D1 109.3 . . ? C4D C3D H3D2 109.4 . . ? C2D C3D H3D2 109.3 . . ? H3D1 C3D H3D2 108.0 . . ? C3D C4D C5D 111.3(9) . . ? C3D C4D H4D1 109.3 . . ? C5D C4D H4D1 109.3 . . ? C3D C4D H4D2 109.4 . . ? C5D C4D H4D2 109.4 . . ? H4D1 C4D H4D2 108.0 . . ? C4D C5D C6D 110.6(8) . . ? C4D C5D H5D1 109.6 . . ? C6D C5D H5D1 109.6 . . ? C4D C5D H5D2 109.4 . . ? C6D C5D H5D2 109.5 . . ? H5D1 C5D H5D2 108.1 . . ? C1D C6D C5D 111.4(8) . . ? C1D C6D H6D1 109.5 . . ? C5D C6D H6D1 109.3 . . ? C1D C6D H6D2 109.2 . . ? C5D C6D H6D2 109.3 . . ? H6D1 C6D H6D2 108.0 . . ? C5E C1E C2E 106.6(12) . . ? C5E C1E Mn1 75.9(7) . . ? C2E C1E Mn1 71.6(6) . . ? C5E C1E H1E 126.6 . . ? C2E C1E H1E 126.7 . . ? Mn1 C1E H1E 117.8 . . ? C3E C2E C1E 106.7(11) . . ? C3E C2E Mn1 75.8(6) . . ? C1E C2E Mn1 74.4(6) . . ? C3E C2E H2E 126.6 . . ? C1E C2E H2E 126.7 . . ? Mn1 C2E H2E 115.6 . . ? C4E C3E C2E 109.7(10) . . ? C4E C3E Mn1 77.3(6) . . ? C2E C3E Mn1 71.0(6) . . ? C4E C3E H3E 125.0 . . ? C2E C3E H3E 125.3 . . ? Mn1 C3E H3E 118.3 . . ? C5E C4E C3E 107.7(11) . . ? C5E C4E Mn1 72.5(7) . . ? C3E C4E Mn1 70.7(6) . . ? C5E C4E H4E 126.1 . . ? C3E C4E H4E 126.2 . . ? Mn1 C4E H4E 122.1 . . ? C4E C5E C1E 109.2(12) . . ? C4E C5E Mn1 76.1(7) . . ? C1E C5E Mn1 71.0(7) . . ? C4E C5E H5E 125.3 . . ? C1E C5E H5E 125.5 . . ? Mn1 C5E H5E 119.5 . . ? C5F C1F C2F 107.2(11) . . ? C5F C1F Mn2 74.7(7) . . ? C2F C1F Mn2 71.2(7) . . ? C5F C1F H1F 126.4 . . ? C2F C1F H1F 126.4 . . ? Mn2 C1F H1F 119.6 . . ? C3F C2F C1F 108.0(12) . . ? C3F C2F Mn2 75.8(7) . . ? C1F C2F Mn2 75.6(7) . . ? C3F C2F H2F 126.0 . . ? C1F C2F H2F 126.1 . . ? Mn2 C2F H2F 114.9 . . ? C2F C3F C4F 109.9(12) . . ? C2F C3F Mn2 71.0(6) . . ? C4F C3F Mn2 76.7(7) . . ? C2F C3F H3F 125.1 . . ? C4F C3F H3F 125.0 . . ? Mn2 C3F H3F 119.1 . . ? C3F C4F C5F 105.4(12) . . ? C3F C4F Mn2 71.1(6) . . ? C5F C4F Mn2 71.7(7) . . ? C3F C4F H4F 127.4 . . ? C5F C4F H4F 127.3 . . ? Mn2 C4F H4F 121.7 . . ? C1F C5F C4F 109.5(12) . . ? C1F C5F Mn2 72.6(7) . . ? C4F C5F Mn2 75.5(6) . . ? C1F C5F H5F 125.3 . . ? C4F C5F H5F 125.2 . . ? Mn2 C5F H5F 118.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.868 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.153 data_dw9916 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H54 Mn2 N4 Sb2' _chemical_formula_weight 872.19 _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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 11.775(2) _cell_length_b 11.775(2) _cell_length_c 26.095(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3618.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method ? _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 2.187 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 KappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5231 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.06 _reflns_number_total 3156 _reflns_number_observed 2983 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0713P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(5) _refine_ls_number_reflns 3155 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_obs 0.0277 _refine_ls_wR_factor_all 0.1256 _refine_ls_wR_factor_obs 0.0786 _refine_ls_goodness_of_fit_all 1.185 _refine_ls_goodness_of_fit_obs 0.804 _refine_ls_restrained_S_all 1.247 _refine_ls_restrained_S_obs 0.804 _refine_ls_shift/esd_max -0.009 _refine_ls_shift/esd_mean 0.001 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 Sb1 Sb 0.33514(3) 0.52380(3) 0.015389(15) 0.0179(2) Uani 1 d . . Mn1 Mn 0.31208(8) 0.27229(8) 0.05686(3) 0.0182(2) Uani 1 d . . N1 N 0.4477(4) 0.4086(4) 0.0507(2) 0.0176(11) Uani 1 d . . N2 N 0.2152(4) 0.3993(4) 0.0121(2) 0.0186(11) Uani 1 d . . C1 C 0.3508(7) 0.2159(7) 0.1518(3) 0.039(2) Uani 1 d . . H1A H 0.4255(7) 0.2226(7) 0.1698(3) 0.046 Uiso 1 calc R . C2 C 0.3145(7) 0.1223(7) 0.1237(3) 0.036(2) Uani 1 d . . H2A H 0.3556(7) 0.0482(7) 0.1211(3) 0.043 Uiso 1 calc R . C3 C 0.2014(7) 0.1417(6) 0.1085(3) 0.032(2) Uani 1 d . . H3A H 0.1481(7) 0.0828(6) 0.0949(3) 0.038 Uiso 1 calc R . C4 C 0.1701(6) 0.2484(7) 0.1272(2) 0.031(2) Uani 1 d . . H4A H 0.0912(6) 0.2799(7) 0.1271(2) 0.037 Uiso 1 calc R . C5 C 0.2629(8) 0.2949(7) 0.1540(3) 0.041(2) Uani 1 d . . H5A H 0.2630(8) 0.3674(7) 0.1740(3) 0.050 Uiso 1 calc R . C6 C 0.5163(5) 0.4448(6) 0.0950(2) 0.0234(14) Uani 1 d . . H6A H 0.4637(5) 0.4504(6) 0.1250(2) 0.028 Uiso 1 calc R . C7 C 0.5712(6) 0.5589(6) 0.0887(3) 0.028(2) Uani 1 d . . H7A H 0.5121(6) 0.6160(6) 0.0805(3) 0.033 Uiso 1 calc R . H7B H 0.6249(6) 0.5560(6) 0.0595(3) 0.033 Uiso 1 calc R . C8 C 0.6356(7) 0.5963(8) 0.1374(3) 0.045(2) Uani 1 d . . H8A H 0.6743(7) 0.6695(8) 0.1309(3) 0.054 Uiso 1 calc R . H8B H 0.5809(7) 0.6076(8) 0.1657(3) 0.054 Uiso 1 calc R . C9 C 0.7235(7) 0.5067(8) 0.1530(4) 0.057(3) Uani 1 d . . H9A H 0.7845(7) 0.5037(8) 0.1269(4) 0.068 Uiso 1 calc R . H9B H 0.7581(7) 0.5283(8) 0.1861(4) 0.068 Uiso 1 calc R . C10 C 0.6691(7) 0.3904(8) 0.1579(3) 0.046(2) Uani 1 d . . H10A H 0.6142(7) 0.3913(8) 0.1866(3) 0.055 Uiso 1 calc R . H10B H 0.7284(7) 0.3335(8) 0.1659(3) 0.055 Uiso 1 calc R . C11 C 0.6076(6) 0.3554(7) 0.1087(3) 0.029(2) Uani 1 d . . H11A H 0.5712(6) 0.2804(7) 0.1135(3) 0.035 Uiso 1 calc R . H11B H 0.6629(6) 0.3490(7) 0.0803(3) 0.035 Uiso 1 calc R . C12 C 0.0951(5) 0.4288(5) 0.0250(2) 0.0196(13) Uani 1 d . . H12A H 0.0910(5) 0.4448(5) 0.0625(2) 0.023 Uiso 1 calc R . C13 C 0.0535(5) 0.5338(6) -0.0036(3) 0.0237(14) Uani 1 d . . H13A H 0.0583(5) 0.5203(6) -0.0409(3) 0.028 Uiso 1 calc R . H13B H 0.1031(5) 0.5991(6) 0.0049(3) 0.028 Uiso 1 calc R . C14 C -0.0696(6) 0.5621(6) 0.0110(3) 0.035(2) Uani 1 d . . H14A H -0.0732(6) 0.5830(6) 0.0477(3) 0.042 Uiso 1 calc R . H14B H -0.0960(6) 0.6281(6) -0.0093(3) 0.042 Uiso 1 calc R . C15 C -0.1474(6) 0.4610(7) 0.0011(3) 0.036(2) Uani 1 d . . H15A H -0.2251(6) 0.4791(7) 0.0131(3) 0.044 Uiso 1 calc R . H15B H -0.1511(6) 0.4461(7) -0.0362(3) 0.044 Uiso 1 calc R . C16 C -0.1052(6) 0.3558(6) 0.0283(3) 0.029(2) Uani 1 d . . H16A H -0.1541(6) 0.2904(6) 0.0192(3) 0.034 Uiso 1 calc R . H16B H -0.1101(6) 0.3673(6) 0.0658(3) 0.034 Uiso 1 calc R . C17 C 0.0170(5) 0.3298(6) 0.0135(3) 0.0248(14) Uani 1 d . . H17A H 0.0433(5) 0.2621(6) 0.0326(3) 0.030 Uiso 1 calc R . H17B H 0.0205(5) 0.3119(6) -0.0235(3) 0.030 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 Sb1 0.0174(2) 0.0153(2) 0.0212(2) -0.0010(2) 0.0014(2) -0.0007(2) Mn1 0.0184(5) 0.0177(5) 0.0186(4) 0.0020(4) 0.0015(4) -0.0002(4) N1 0.015(3) 0.017(3) 0.020(2) -0.003(2) 0.000(2) 0.003(2) N2 0.015(2) 0.019(3) 0.023(3) 0.003(2) -0.002(2) 0.003(2) C1 0.035(4) 0.053(5) 0.028(4) 0.009(4) 0.001(3) -0.005(4) C2 0.047(5) 0.032(4) 0.028(3) 0.009(3) 0.015(3) 0.014(3) C3 0.042(4) 0.027(4) 0.026(3) 0.004(3) 0.008(3) -0.007(3) C4 0.027(4) 0.041(4) 0.026(3) 0.012(3) 0.008(3) 0.004(3) C5 0.061(6) 0.033(4) 0.030(4) 0.001(3) 0.012(4) -0.010(4) C6 0.016(3) 0.031(4) 0.024(3) -0.008(3) -0.002(3) -0.001(3) C7 0.023(4) 0.024(4) 0.036(3) -0.014(3) -0.007(3) -0.005(3) C8 0.037(5) 0.046(5) 0.052(5) -0.021(4) -0.011(4) -0.008(4) C9 0.036(5) 0.076(7) 0.058(5) -0.023(5) -0.028(4) 0.005(5) C10 0.043(5) 0.053(5) 0.043(4) -0.010(4) -0.029(4) 0.018(4) C11 0.023(4) 0.034(4) 0.030(3) -0.006(3) -0.006(3) 0.003(3) C12 0.014(3) 0.023(3) 0.022(3) 0.000(3) -0.002(2) 0.001(3) C13 0.022(3) 0.020(3) 0.028(3) 0.003(3) 0.000(3) 0.002(3) C14 0.031(4) 0.033(4) 0.041(4) 0.003(4) 0.003(4) 0.010(3) C15 0.021(3) 0.043(5) 0.045(4) -0.005(4) 0.004(3) 0.004(4) C16 0.016(3) 0.032(4) 0.037(4) -0.001(3) 0.007(3) -0.006(3) C17 0.019(3) 0.029(3) 0.027(3) -0.002(3) 0.003(3) 0.000(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 Sb1 N2 2.037(5) . ? Sb1 N1 2.109(5) . ? Sb1 N1 2.128(5) 7 ? Sb1 Mn1 3.1648(11) . ? Sb1 Mn1 3.2122(11) 7 ? Sb1 Sb1 3.2426(9) 7 ? Mn1 N2 2.178(5) 7 ? Mn1 N2 2.214(5) . ? Mn1 N1 2.270(5) . ? Mn1 C3 2.424(7) . ? Mn1 C2 2.482(7) . ? Mn1 C4 2.499(7) . ? Mn1 C1 2.605(7) . ? Mn1 C5 2.615(7) . ? Mn1 Mn1 3.041(2) 7 ? Mn1 Sb1 3.2122(11) 7 ? N1 C6 1.473(8) . ? N1 Sb1 2.128(5) 7 ? N2 C12 1.494(8) . ? N2 Mn1 2.178(5) 7 ? C1 C2 1.390(11) . ? C1 C5 1.393(12) . ? C2 C3 1.408(11) . ? C3 C4 1.398(11) . ? C4 C5 1.409(11) . ? C6 C7 1.500(9) . ? C6 C11 1.546(10) . ? C7 C8 1.544(10) . ? C8 C9 1.533(13) . ? C9 C10 1.517(13) . ? C10 C11 1.530(9) . ? C12 C17 1.515(9) . ? C12 C13 1.524(9) . ? C13 C14 1.536(9) . ? C14 C15 1.525(11) . ? C15 C16 1.511(10) . ? C16 C17 1.521(9) . ? 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 Sb1 N1 89.5(2) . . ? N2 Sb1 N1 86.8(2) . 7 ? N1 Sb1 N1 80.1(2) . 7 ? N2 Sb1 Mn1 44.08(14) . . ? N1 Sb1 Mn1 45.78(14) . . ? N1 Sb1 Mn1 85.31(13) 7 . ? N2 Sb1 Mn1 42.03(14) . 7 ? N1 Sb1 Mn1 84.39(13) . 7 ? N1 Sb1 Mn1 44.84(14) 7 7 ? Mn1 Sb1 Mn1 56.95(3) . 7 ? N2 Sb1 Sb1 88.37(14) . 7 ? N1 Sb1 Sb1 40.27(12) . 7 ? N1 Sb1 Sb1 39.84(13) 7 7 ? Mn1 Sb1 Sb1 60.16(2) . 7 ? Mn1 Sb1 Sb1 58.72(2) 7 7 ? N2 Mn1 N2 90.9(2) 7 . ? N2 Mn1 N1 80.1(2) 7 . ? N2 Mn1 N1 81.2(2) . . ? N2 Mn1 C3 121.1(2) 7 . ? N2 Mn1 C3 116.4(2) . . ? N1 Mn1 C3 150.0(2) . . ? N2 Mn1 C2 110.8(2) 7 . ? N2 Mn1 C2 149.0(2) . . ? N1 Mn1 C2 123.0(2) . . ? C3 Mn1 C2 33.3(3) . . ? N2 Mn1 C4 152.6(2) 7 . ? N2 Mn1 C4 96.8(2) . . ? N1 Mn1 C4 127.0(2) . . ? C3 Mn1 C4 33.0(3) . . ? C2 Mn1 C4 54.0(2) . . ? N2 Mn1 C1 128.6(2) 7 . ? N2 Mn1 C1 139.8(2) . . ? N1 Mn1 C1 97.1(2) . . ? C3 Mn1 C1 53.4(2) . . ? C2 Mn1 C1 31.6(3) . . ? C4 Mn1 C1 52.4(2) . . ? N2 Mn1 C5 159.6(2) 7 . ? N2 Mn1 C5 109.2(2) . . ? N1 Mn1 C5 98.8(2) . . ? C3 Mn1 C5 53.6(2) . . ? C2 Mn1 C5 52.7(3) . . ? C4 Mn1 C5 31.9(2) . . ? C1 Mn1 C5 31.0(3) . . ? N2 Mn1 Mn1 46.68(13) 7 7 ? N2 Mn1 Mn1 45.71(13) . 7 ? N1 Mn1 Mn1 86.01(12) . 7 ? C3 Mn1 Mn1 123.9(2) . 7 ? C2 Mn1 Mn1 142.9(2) . 7 ? C4 Mn1 Mn1 129.1(2) . 7 ? C1 Mn1 Mn1 173.9(2) . 7 ? C5 Mn1 Mn1 153.7(2) . 7 ? N2 Mn1 Sb1 88.04(13) 7 . ? N2 Mn1 Sb1 39.80(13) . . ? N1 Mn1 Sb1 41.74(12) . . ? C3 Mn1 Sb1 146.1(2) . . ? C2 Mn1 Sb1 154.8(2) . . ? C4 Mn1 Sb1 114.5(2) . . ? C1 Mn1 Sb1 123.3(2) . . ? C5 Mn1 Sb1 104.8(2) . . ? Mn1 Mn1 Sb1 62.31(2) 7 . ? N2 Mn1 Sb1 38.76(14) 7 7 ? N2 Mn1 Sb1 86.25(13) . 7 ? N1 Mn1 Sb1 41.37(12) . 7 ? C3 Mn1 Sb1 152.8(2) . 7 ? C2 Mn1 Sb1 124.6(2) . 7 ? C4 Mn1 Sb1 167.5(2) . 7 ? C1 Mn1 Sb1 118.8(2) . 7 ? C5 Mn1 Sb1 135.9(2) . 7 ? Mn1 Mn1 Sb1 60.74(2) 7 7 ? Sb1 Mn1 Sb1 61.12(2) . 7 ? C6 N1 Sb1 120.1(4) . . ? C6 N1 Sb1 121.5(4) . 7 ? Sb1 N1 Sb1 99.9(2) . 7 ? C6 N1 Mn1 122.4(4) . . ? Sb1 N1 Mn1 92.5(2) . . ? Sb1 N1 Mn1 93.8(2) 7 . ? C12 N2 Sb1 118.7(4) . . ? C12 N2 Mn1 125.9(4) . 7 ? Sb1 N2 Mn1 99.2(2) . 7 ? C12 N2 Mn1 121.7(4) . . ? Sb1 N2 Mn1 96.1(2) . . ? Mn1 N2 Mn1 87.6(2) 7 . ? C2 C1 C5 108.8(7) . . ? C2 C1 Mn1 69.3(4) . . ? C5 C1 Mn1 74.9(4) . . ? C1 C2 C3 108.1(7) . . ? C1 C2 Mn1 79.1(4) . . ? C3 C2 Mn1 71.1(4) . . ? C4 C3 C2 107.2(7) . . ? C4 C3 Mn1 76.5(4) . . ? C2 C3 Mn1 75.6(4) . . ? C3 C4 C5 108.6(7) . . ? C3 C4 Mn1 70.6(4) . . ? C5 C4 Mn1 78.6(4) . . ? C1 C5 C4 107.2(7) . . ? C1 C5 Mn1 74.2(4) . . ? C4 C5 Mn1 69.5(4) . . ? N1 C6 C7 114.2(5) . . ? N1 C6 C11 111.4(5) . . ? C7 C6 C11 109.6(6) . . ? C6 C7 C8 112.1(6) . . ? C9 C8 C7 110.7(7) . . ? C10 C9 C8 111.0(7) . . ? C9 C10 C11 111.8(7) . . ? C10 C11 C6 109.8(6) . . ? N2 C12 C17 110.6(5) . . ? N2 C12 C13 112.5(5) . . ? C17 C12 C13 109.5(5) . . ? C12 C13 C14 111.0(5) . . ? C15 C14 C13 110.8(6) . . ? C16 C15 C14 111.3(6) . . ? C15 C16 C17 110.9(6) . . ? C12 C17 C16 111.7(6) . . ? _refine_diff_density_max 0.939 _refine_diff_density_min -1.598 _refine_diff_density_rms 0.424