# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1928 data_[Mn(L1)2] # 3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Mn N8' _chemical_formula_weight 601.57 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3746(17) _cell_length_b 16.061(6) _cell_length_c 16.726(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.15(2) _cell_angle_gamma 90.00 _cell_volume 2786.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4901 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4901 _reflns_number_gt 3584 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+1.9578P] 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 4901 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 1.422 _refine_ls_shift/su_mean 0.331 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.07291(3) 0.72218(2) 0.11162(2) 0.02653(11) Uani 1 d . . . N7 N -0.05399(17) 0.64457(12) 0.07962(11) 0.0280(4) Uani 1 d . . . N3 N 0.22074(17) 0.78318(12) 0.14183(11) 0.0273(4) Uani 1 d . . . N1 N 0.21333(18) 0.63679(12) 0.10674(11) 0.0296(4) Uani 1 d . . . N5 N 0.06933(18) 0.73421(13) -0.00717(12) 0.0319(5) Uani 1 d . . . N8 N 0.01261(18) 0.68844(12) 0.21709(11) 0.0294(4) Uani 1 d . . . N4 N -0.00546(18) 0.83269(12) 0.11986(12) 0.0295(4) Uani 1 d . . . N6 N -0.07627(19) 0.62451(13) 0.00408(12) 0.0349(5) Uani 1 d . . . N2 N 0.33760(18) 0.74960(13) 0.14950(12) 0.0324(5) Uani 1 d . . . C1 C 0.2056(3) 0.55572(15) 0.08563(16) 0.0380(6) Uani 1 d . . . H1 H 0.1259 0.5344 0.0702 0.046 Uiso 1 calc R . . C2 C 0.3093(3) 0.50395(17) 0.08609(17) 0.0473(7) Uani 1 d . . . H2 H 0.3003 0.4484 0.0715 0.057 Uiso 1 calc R . . C3 C 0.4291(3) 0.53531(18) 0.10878(17) 0.0464(7) Uani 1 d . . . H3 H 0.5012 0.5009 0.1093 0.056 Uiso 1 calc R . . C4 C 0.4399(2) 0.61686(17) 0.13028(16) 0.0390(6) Uani 1 d . . . H4 H 0.5193 0.6384 0.1457 0.047 Uiso 1 calc R . . C5 C 0.3308(2) 0.66784(15) 0.12897(14) 0.0308(5) Uani 1 d . . . C6 C 0.2055(2) 0.86675(15) 0.15867(14) 0.0299(5) Uani 1 d . . . C7 C 0.3017(2) 0.92076(16) 0.18617(15) 0.0362(6) Uani 1 d . . . H7 H 0.3853 0.9018 0.1947 0.043 Uiso 1 calc R . . C8 C 0.2697(3) 1.00214(17) 0.20025(16) 0.0423(7) Uani 1 d . . . H8 H 0.3321 1.0392 0.2185 0.051 Uiso 1 calc R . . C9 C 0.1436(3) 1.02950(16) 0.18725(16) 0.0410(6) Uani 1 d . . . H9 H 0.1236 1.0850 0.1970 0.049 Uiso 1 calc R . . C10 C 0.0488(3) 0.97752(16) 0.16071(16) 0.0373(6) Uani 1 d . . . H10 H -0.0344 0.9976 0.1529 0.045 Uiso 1 calc R . . C11 C 0.0775(2) 0.89303(15) 0.14508(14) 0.0300(5) Uani 1 d . . . C12 C -0.1307(2) 0.85352(15) 0.09306(14) 0.0298(5) Uani 1 d . . . C13 C -0.2371(2) 0.81133(16) 0.12236(15) 0.0347(6) Uani 1 d . . . H13 H -0.2257 0.7686 0.1593 0.042 Uiso 1 calc R . . C14 C -0.3601(2) 0.83217(18) 0.09722(17) 0.0423(7) Uani 1 d . . . H14 H -0.4308 0.8035 0.1174 0.051 Uiso 1 calc R . . C15 C -0.3783(3) 0.89489(19) 0.04269(18) 0.0495(7) Uani 1 d . . . H15 H -0.4612 0.9097 0.0269 0.059 Uiso 1 calc R . . C16 C -0.2735(3) 0.93572(19) 0.01159(17) 0.0494(7) Uani 1 d . . . H16 H -0.2856 0.9777 -0.0260 0.059 Uiso 1 calc R . . C17 C -0.1506(3) 0.91505(17) 0.03567(15) 0.0386(6) Uani 1 d . . . H17 H -0.0803 0.9424 0.0134 0.046 Uiso 1 calc R . . C18 C 0.1290(3) 0.79186(17) -0.05283(16) 0.0429(7) Uani 1 d . . . H18 H 0.1828 0.8306 -0.0283 0.051 Uiso 1 calc R . . C19 C 0.1127(3) 0.7951(2) -0.13407(17) 0.0525(8) Uani 1 d . . . H19 H 0.1521 0.8367 -0.1639 0.063 Uiso 1 calc R . . C20 C 0.0370(3) 0.7357(2) -0.17133(17) 0.0545(8) Uani 1 d . . . H20 H 0.0272 0.7362 -0.2266 0.065 Uiso 1 calc R . . C21 C -0.0229(3) 0.6766(2) -0.12678(16) 0.0486(7) Uani 1 d . . . H21 H -0.0726 0.6357 -0.1514 0.058 Uiso 1 calc R . . C22 C -0.0092(2) 0.67777(16) -0.04355(15) 0.0349(6) Uani 1 d . . . C23 C -0.1079(2) 0.59559(14) 0.13914(14) 0.0293(5) Uani 1 d . . . C24 C -0.1891(3) 0.52725(17) 0.12854(17) 0.0418(6) Uani 1 d . . . H24 H -0.2136 0.5105 0.0775 0.050 Uiso 1 calc R . . C25 C -0.2322(3) 0.48511(17) 0.19438(18) 0.0483(7) Uani 1 d . . . H25 H -0.2866 0.4395 0.1883 0.058 Uiso 1 calc R . . C26 C -0.1946(3) 0.51060(17) 0.27065(17) 0.0430(7) Uani 1 d . . . H26 H -0.2235 0.4809 0.3148 0.052 Uiso 1 calc R . . C27 C -0.1163(2) 0.57807(16) 0.28229(15) 0.0364(6) Uani 1 d . . . H27 H -0.0938 0.5943 0.3338 0.044 Uiso 1 calc R . . C28 C -0.0698(2) 0.62286(14) 0.21577(14) 0.0276(5) Uani 1 d . . . C29 C 0.0328(2) 0.73012(14) 0.29121(14) 0.0306(5) Uani 1 d . . . C30 C -0.0684(3) 0.77168(18) 0.32760(16) 0.0456(7) Uani 1 d . . . H30 H -0.1474 0.7758 0.3015 0.055 Uiso 1 calc R . . C31 C -0.0531(3) 0.80713(19) 0.40248(17) 0.0542(8) Uani 1 d . . . H31 H -0.1218 0.8341 0.4269 0.065 Uiso 1 calc R . . C32 C 0.0632(3) 0.80225(18) 0.44027(17) 0.0513(8) Uani 1 d . . . H32 H 0.0736 0.8251 0.4910 0.062 Uiso 1 calc R . . C33 C 0.1650(3) 0.7636(2) 0.40355(17) 0.0519(8) Uani 1 d . . . H33 H 0.2445 0.7612 0.4292 0.062 Uiso 1 calc R . . C34 C 0.1507(2) 0.72819(17) 0.32887(15) 0.0400(6) Uani 1 d . . . H34 H 0.2207 0.7030 0.3040 0.048 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 Mn 0.02491(19) 0.02551(19) 0.02918(19) -0.00044(16) 0.00132(14) -0.00322(15) N7 0.0262(10) 0.0281(11) 0.0298(11) -0.0001(9) -0.0009(8) -0.0009(8) N3 0.0247(10) 0.0280(10) 0.0294(10) 0.0025(9) 0.0027(8) -0.0038(9) N1 0.0297(10) 0.0289(11) 0.0301(11) -0.0002(9) 0.0012(8) 0.0002(9) N5 0.0291(10) 0.0340(12) 0.0327(11) 0.0021(9) 0.0020(9) 0.0009(9) N8 0.0301(10) 0.0290(11) 0.0289(11) -0.0023(9) 0.0024(8) -0.0057(9) N4 0.0242(10) 0.0269(11) 0.0376(12) -0.0016(9) 0.0026(8) -0.0021(8) N6 0.0378(12) 0.0376(12) 0.0293(11) -0.0019(9) -0.0050(9) -0.0071(10) N2 0.0250(10) 0.0341(11) 0.0381(12) 0.0011(9) 0.0000(8) -0.0015(9) C1 0.0391(15) 0.0300(14) 0.0449(15) -0.0053(12) -0.0037(12) 0.0009(12) C2 0.0506(17) 0.0343(15) 0.0570(18) -0.0073(14) -0.0020(14) 0.0080(13) C3 0.0413(16) 0.0431(17) 0.0549(18) 0.0010(14) -0.0011(13) 0.0153(13) C4 0.0316(14) 0.0425(16) 0.0428(15) 0.0023(13) -0.0019(11) 0.0053(12) C5 0.0294(13) 0.0355(14) 0.0274(12) 0.0031(11) 0.0015(10) 0.0003(11) C6 0.0306(12) 0.0295(13) 0.0297(13) 0.0005(10) 0.0048(10) -0.0044(10) C7 0.0322(14) 0.0403(15) 0.0361(14) -0.0015(12) -0.0037(11) -0.0061(11) C8 0.0472(16) 0.0348(15) 0.0449(16) -0.0067(13) -0.0045(13) -0.0142(13) C9 0.0470(16) 0.0293(14) 0.0467(16) -0.0073(12) 0.0037(13) -0.0041(12) C10 0.0355(14) 0.0334(14) 0.0432(15) -0.0033(12) 0.0060(12) -0.0005(11) C11 0.0313(13) 0.0281(13) 0.0305(13) 0.0001(10) 0.0049(10) -0.0046(10) C12 0.0286(12) 0.0278(13) 0.0331(13) -0.0051(10) 0.0030(10) 0.0012(10) C13 0.0331(13) 0.0318(13) 0.0391(14) -0.0020(11) 0.0037(11) -0.0034(11) C14 0.0291(14) 0.0470(17) 0.0509(17) -0.0080(14) 0.0024(12) -0.0070(12) C15 0.0355(15) 0.0595(19) 0.0535(18) -0.0074(16) -0.0127(13) 0.0092(14) C16 0.0555(19) 0.0520(19) 0.0407(16) 0.0069(14) -0.0056(14) 0.0102(15) C17 0.0378(15) 0.0401(16) 0.0379(15) 0.0041(12) 0.0042(12) -0.0028(12) C18 0.0388(15) 0.0461(17) 0.0438(16) 0.0069(13) 0.0066(12) -0.0039(13) C19 0.0525(18) 0.062(2) 0.0435(17) 0.0168(15) 0.0132(14) -0.0003(15) C20 0.0575(19) 0.076(2) 0.0304(15) 0.0063(15) 0.0027(13) 0.0052(17) C21 0.0511(17) 0.061(2) 0.0332(15) -0.0001(14) -0.0035(13) -0.0022(15) C22 0.0313(13) 0.0406(15) 0.0329(14) -0.0012(12) -0.0010(11) 0.0027(11) C23 0.0265(12) 0.0265(12) 0.0351(13) 0.0031(10) 0.0001(10) -0.0035(10) C24 0.0416(15) 0.0406(15) 0.0430(16) -0.0024(13) -0.0051(12) -0.0120(13) C25 0.0497(17) 0.0372(16) 0.0580(19) 0.0073(14) -0.0002(14) -0.0191(13) C26 0.0418(15) 0.0380(15) 0.0491(16) 0.0141(13) 0.0044(13) -0.0060(13) C27 0.0381(14) 0.0366(15) 0.0344(14) 0.0047(11) 0.0023(11) 0.0001(12) C28 0.0238(11) 0.0256(12) 0.0335(13) 0.0004(10) 0.0006(10) 0.0003(10) C29 0.0370(13) 0.0248(12) 0.0299(13) 0.0014(10) 0.0013(10) -0.0058(10) C30 0.0458(16) 0.0515(17) 0.0396(15) -0.0047(14) -0.0001(12) 0.0095(14) C31 0.072(2) 0.0460(17) 0.0444(18) -0.0070(14) 0.0141(16) 0.0088(16) C32 0.083(2) 0.0410(17) 0.0304(14) -0.0063(12) 0.0032(15) -0.0183(16) C33 0.0544(18) 0.060(2) 0.0409(16) 0.0031(15) -0.0081(14) -0.0212(16) C34 0.0366(14) 0.0447(16) 0.0386(14) -0.0015(13) 0.0005(11) -0.0057(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 Mn N3 1.8877(19) . ? Mn N7 1.8894(19) . ? Mn N8 1.950(2) . ? Mn N4 1.957(2) . ? Mn N5 1.997(2) . ? Mn N1 2.003(2) . ? N7 N6 1.324(3) . ? N7 C23 1.388(3) . ? N3 N2 1.333(3) . ? N3 C6 1.381(3) . ? N1 C1 1.351(3) . ? N1 C5 1.367(3) . ? N5 C18 1.351(3) . ? N5 C22 1.361(3) . ? N8 C28 1.357(3) . ? N8 C29 1.424(3) . ? N4 C11 1.362(3) . ? N4 C12 1.414(3) . ? N6 C22 1.362(3) . ? N2 C5 1.359(3) . ? C1 C2 1.360(4) . ? C2 C3 1.393(4) . ? C3 C4 1.363(4) . ? C4 C5 1.397(3) . ? C6 C7 1.399(3) . ? C6 C11 1.412(3) . ? C7 C8 1.369(4) . ? C8 C9 1.397(4) . ? C9 C10 1.364(4) . ? C10 C11 1.414(3) . ? C12 C13 1.386(3) . ? C12 C17 1.393(3) . ? C13 C14 1.383(4) . ? C14 C15 1.372(4) . ? C15 C16 1.373(4) . ? C16 C17 1.377(4) . ? C18 C19 1.370(4) . ? C19 C20 1.383(4) . ? C20 C21 1.359(4) . ? C21 C22 1.399(4) . ? C23 C24 1.395(3) . ? C23 C28 1.410(3) . ? C24 C25 1.369(4) . ? C25 C26 1.394(4) . ? C26 C27 1.368(4) . ? C27 C28 1.411(3) . ? C29 C34 1.375(3) . ? C29 C30 1.386(3) . ? C30 C31 1.385(4) . ? C31 C32 1.363(4) . ? C32 C33 1.371(4) . ? C33 C34 1.380(4) . ? 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 N3 Mn N7 169.51(8) . . ? N3 Mn N8 99.47(8) . . ? N7 Mn N8 81.26(8) . . ? N3 Mn N4 81.25(8) . . ? N7 Mn N4 109.20(8) . . ? N8 Mn N4 93.10(8) . . ? N3 Mn N5 103.25(8) . . ? N7 Mn N5 76.75(8) . . ? N8 Mn N5 157.22(8) . . ? N4 Mn N5 88.61(8) . . ? N3 Mn N1 77.04(8) . . ? N7 Mn N1 92.47(8) . . ? N8 Mn N1 94.68(8) . . ? N4 Mn N1 157.86(8) . . ? N5 Mn N1 92.13(8) . . ? N6 N7 C23 118.49(19) . . ? N6 N7 Mn 123.43(15) . . ? C23 N7 Mn 116.91(15) . . ? N2 N3 C6 118.57(19) . . ? N2 N3 Mn 123.64(15) . . ? C6 N3 Mn 117.77(15) . . ? C1 N1 C5 118.4(2) . . ? C1 N1 Mn 128.87(17) . . ? C5 N1 Mn 112.77(16) . . ? C18 N5 C22 118.6(2) . . ? C18 N5 Mn 128.41(18) . . ? C22 N5 Mn 112.95(16) . . ? C28 N8 C29 118.06(19) . . ? C28 N8 Mn 113.87(15) . . ? C29 N8 Mn 127.59(15) . . ? C11 N4 C12 120.6(2) . . ? C11 N4 Mn 113.87(15) . . ? C12 N4 Mn 125.03(15) . . ? N7 N6 C22 108.49(19) . . ? N3 N2 C5 108.67(19) . . ? N1 C1 C2 122.7(2) . . ? C1 C2 C3 119.1(3) . . ? C4 C3 C2 119.5(3) . . ? C3 C4 C5 119.6(3) . . ? N2 C5 N1 117.8(2) . . ? N2 C5 C4 121.4(2) . . ? N1 C5 C4 120.8(2) . . ? N3 C6 C7 126.0(2) . . ? N3 C6 C11 111.5(2) . . ? C7 C6 C11 122.5(2) . . ? C8 C7 C6 118.4(2) . . ? C7 C8 C9 120.0(2) . . ? C10 C9 C8 122.2(2) . . ? C9 C10 C11 119.7(2) . . ? N4 C11 C6 115.5(2) . . ? N4 C11 C10 127.4(2) . . ? C6 C11 C10 117.1(2) . . ? C13 C12 C17 118.3(2) . . ? C13 C12 N4 120.3(2) . . ? C17 C12 N4 121.4(2) . . ? C14 C13 C12 120.6(2) . . ? C15 C14 C13 120.3(3) . . ? C14 C15 C16 119.7(3) . . ? C15 C16 C17 120.5(3) . . ? C16 C17 C12 120.5(3) . . ? N5 C18 C19 122.1(3) . . ? C18 C19 C20 119.3(3) . . ? C21 C20 C19 119.7(3) . . ? C20 C21 C22 119.4(3) . . ? N6 C22 N5 117.6(2) . . ? N6 C22 C21 121.5(2) . . ? N5 C22 C21 120.9(2) . . ? N7 C23 C24 126.8(2) . . ? N7 C23 C28 111.3(2) . . ? C24 C23 C28 121.9(2) . . ? C25 C24 C23 119.0(2) . . ? C24 C25 C26 120.0(2) . . ? C27 C26 C25 121.8(2) . . ? C26 C27 C28 119.7(2) . . ? N8 C28 C23 115.5(2) . . ? N8 C28 C27 126.8(2) . . ? C23 C28 C27 117.6(2) . . ? C34 C29 C30 118.9(2) . . ? C34 C29 N8 121.1(2) . . ? C30 C29 N8 119.9(2) . . ? C31 C30 C29 120.6(3) . . ? C32 C31 C30 119.7(3) . . ? C31 C32 C33 120.0(3) . . ? C32 C33 C34 120.7(3) . . ? C29 C34 C33 119.9(3) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.267 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.050