# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/221 data_CC0002 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H61 Cl13 N6 Ti2' _chemical_formula_weight 1254.66 _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' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.101(6) _cell_length_b 14.916(3) _cell_length_c 17.108(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.11(2) _cell_angle_gamma 90.00 _cell_volume 6121.5(24) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10.84 _cell_measurement_theta_max 24.96 _exptl_crystal_description 'hexagonal needles' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method ? _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 7.719 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1342 _exptl_absorpt_correction_T_max 0.6053 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4606 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 60.00 _reflns_number_total 4490 _reflns_number_observed 3653 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 222 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^)+(0.1142P)^2^+18.2158P] 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 4268 _refine_ls_number_parameters 320 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_obs 0.0664 _refine_ls_wR_factor_all 0.1897 _refine_ls_wR_factor_obs 0.1702 _refine_ls_goodness_of_fit_all 1.048 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti1 Ti 0.0000 0.08488(7) 0.2500 0.0217(3) Uani 1 d S . Ti2 Ti 0.0000 0.32415(7) 0.2500 0.0236(3) Uani 1 d S . Cl1 Cl 0.0000 -0.08261(10) 0.2500 0.0375(4) Uani 1 d S . Cl2 Cl -0.09417(5) 0.07776(7) 0.17234(7) 0.0332(3) Uani 1 d . . Cl3 Cl -0.07182(5) 0.34441(8) 0.12793(7) 0.0352(3) Uani 1 d . . N1 N 0.0000 0.2060(3) 0.2500 0.0253(11) Uani 1 d S . N2 N 0.0000 0.4837(4) 0.2500 0.045(2) Uani 1 d S . N3 N 0.0249(2) 0.0821(2) 0.1373(2) 0.0264(8) Uani 1 d . . N4 N 0.0610(2) 0.3306(3) 0.1800(2) 0.0296(9) Uani 1 d . . C1 C -0.0463(3) 0.5292(4) 0.2453(4) 0.0512(15) Uani 1 d . . H1A H -0.0800(3) 0.4974(4) 0.2398(4) 0.061 Uiso 1 calc R . C2 C -0.0467(4) 0.6237(4) 0.2482(4) 0.072(2) Uani 1 d . . C3 C 0.0000 0.6696(6) 0.2500 0.078(4) Uani 1 d S . H3A H 0.0000 0.7333(6) 0.2500 0.093 Uiso 1 calc SR . C4 C -0.1013(5) 0.6695(6) 0.2455(7) 0.120(5) Uani 1 d . . H4A H -0.1171(5) 0.6406(6) 0.2851(7) 0.180 Uiso 1 d R . H4B H -0.1276(5) 0.6642(6) 0.1905(7) 0.180 Uiso 1 d R . H4C H -0.0946(5) 0.7331(6) 0.2595(7) 0.180 Uiso 1 d R . C5 C 0.0654(2) 0.0278(3) 0.1284(3) 0.0290(10) Uani 1 d . . H5A H 0.0828(2) -0.0120(3) 0.1718(3) 0.035 Uiso 1 calc R . C6 C 0.0829(2) 0.0270(4) 0.0588(3) 0.0348(11) Uani 1 d . . C7 C 0.0570(2) 0.0857(4) -0.0039(3) 0.0374(12) Uani 1 d . . H7A H 0.0674(2) 0.0861(4) -0.0530(3) 0.045 Uiso 1 calc R . C8 C 0.0159(2) 0.1435(3) 0.0048(3) 0.0339(11) Uani 1 d . . C9 C 0.0011(2) 0.1390(3) 0.0764(3) 0.0302(10) Uani 1 d . . H9A H -0.0273(2) 0.1781(3) 0.0828(3) 0.036 Uiso 1 calc R . C10 C 0.1287(3) -0.0352(5) 0.0533(4) 0.053(2) Uani 1 d . . H10A H 0.1219(3) -0.0951(5) 0.0720(4) 0.079 Uiso 1 d R . H10B H 0.1646(3) -0.0127(5) 0.0879(4) 0.079 Uiso 1 d R . H10C H 0.1296(3) -0.0386(5) -0.0035(4) 0.079 Uiso 1 d R . C11 C -0.0128(3) 0.2084(4) -0.0613(4) 0.053(2) Uani 1 d . . H11A H -0.0287(3) 0.1756(4) -0.1125(4) 0.079 Uiso 1 d R . H11B H 0.0141(3) 0.2527(4) -0.0690(4) 0.079 Uiso 1 d R . H11C H -0.0426(3) 0.2391(4) -0.0457(4) 0.079 Uiso 1 d R . C12 C 0.1048(2) 0.2733(3) 0.2008(3) 0.0331(11) Uani 1 d . . H12A H 0.1099(2) 0.2362(3) 0.2476(3) 0.040 Uiso 1 calc R . C13 C 0.1424(2) 0.2670(4) 0.1559(3) 0.0395(12) Uani 1 d . . C14 C 0.1355(3) 0.3223(4) 0.0895(4) 0.0495(14) Uani 1 d . . H14A H 0.1615(3) 0.3201(4) 0.0590(4) 0.059 Uiso 1 calc R . C15 C 0.0907(3) 0.3814(4) 0.0665(4) 0.0478(14) Uani 1 d . . C16 C 0.0549(2) 0.3829(4) 0.1138(3) 0.0394(12) Uani 1 d . . H16A H 0.0241(2) 0.4231(4) 0.0990(3) 0.047 Uiso 1 calc R . C17 C 0.1897(3) 0.2012(4) 0.1809(5) 0.056(2) Uani 1 d . . H17A H 0.2246(3) 0.2331(4) 0.2064(5) 0.083 Uiso 1 d R . H17B H 0.1928(3) 0.1690(4) 0.1325(5) 0.083 Uiso 1 d R . H17C H 0.1825(3) 0.1583(4) 0.2200(5) 0.083 Uiso 1 d R . C18 C 0.0807(4) 0.4422(6) -0.0066(5) 0.083(3) Uani 1 d . . H18A H 0.1165(4) 0.4585(6) -0.0147(5) 0.124 Uiso 1 d R . H18B H 0.0614(4) 0.4965(6) 0.0025(5) 0.124 Uiso 1 d R . H18C H 0.0577(4) 0.4109(6) -0.0552(5) 0.124 Uiso 1 d R . C20 C 0.1638(4) 0.8866(5) 0.3657(6) 0.079(2) Uani 1 d . . H20A H 0.1233(4) 0.8774(5) 0.3400(6) 0.095 Uiso 0.60 calc PR 1 H20B H 0.1685(4) 0.9423(5) 0.3985(6) 0.095 Uiso 0.60 calc PR 1 H20C H 0.1796(4) 0.9417(5) 0.3912(6) 0.095 Uiso 0.40 d PR 2 H20D H 0.1240(4) 0.8899(5) 0.3541(6) 0.095 Uiso 0.40 d PR 2 Cl21 Cl 0.18998(14) 0.7974(2) 0.4301(2) 0.1038(9) Uani 1 d . . Cl22 Cl 0.1952(4) 0.8994(6) 0.2913(4) 0.110(3) Uani 0.60 d P 1 Cl23 Cl 0.1886(8) 0.8646(12) 0.2719(15) 0.219(11) Uani 0.40 d P 2 C30 C 0.2938(4) 0.9452(7) 0.1052(8) 0.106(4) Uani 1 d . . H30A H 0.3306(4) 0.9239(7) 0.1023(8) 0.127 Uiso 1 calc R . H30B H 0.2656(4) 0.8994(7) 0.0793(8) 0.127 Uiso 1 calc R . Cl31 Cl 0.27791(11) 1.0427(2) 0.0538(2) 0.1072(8) Uani 1 d . . Cl32 Cl 0.29590(15) 0.9586(3) 0.2090(3) 0.158(2) Uani 1 d . . C40 C 0.3179(9) 0.8145(17) -0.0888(15) 0.140(11) Uani 0.50 d PD 1 H40A H 0.3164(80) 0.7741(91) -0.1345(90) 0.210 Uiso 0.50 calc PR 1 H40B H 0.3563(19) 0.8179(156) -0.0528(41) 0.210 Uiso 0.50 calc PR 1 H40C H 0.3054(62) 0.8744(71) -0.1099(128) 0.210 Uiso 0.50 calc PR 1 C41 C 0.2835(4) 0.7823(7) -0.0451(6) 0.123(5) Uani 1 d D . H41A H 0.3071(4) 0.8049(7) -0.0749(6) 0.147 Uiso 0.50 calc PR 2 C42 C 0.3049(3) 0.7256(6) 0.0210(6) 0.110(4) Uani 1 d D . H42A H 0.3430(3) 0.7081(6) 0.0345(6) 0.133 Uiso 1 calc R . C43 C 0.2724(4) 0.6939(6) 0.0677(6) 0.129(6) Uani 1 d D . H43A H 0.2878(4) 0.6568(6) 0.1139(6) 0.155 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 Ti1 0.0265(6) 0.0189(5) 0.0202(5) 0.000 0.0075(4) 0.000 Ti2 0.0262(6) 0.0187(5) 0.0272(6) 0.000 0.0100(5) 0.000 Cl1 0.0579(11) 0.0194(7) 0.0415(9) 0.000 0.0245(8) 0.000 Cl2 0.0285(6) 0.0371(6) 0.0308(6) -0.0022(4) 0.0037(4) -0.0052(4) Cl3 0.0332(6) 0.0354(6) 0.0346(6) 0.0045(5) 0.0065(5) 0.0046(5) N1 0.029(3) 0.021(2) 0.026(3) 0.000 0.008(2) 0.000 N2 0.060(4) 0.025(3) 0.047(4) 0.000 0.009(3) 0.000 N3 0.031(2) 0.024(2) 0.026(2) -0.0018(15) 0.010(2) -0.002(2) N4 0.031(2) 0.026(2) 0.034(2) 0.002(2) 0.014(2) -0.002(2) C1 0.067(4) 0.031(3) 0.048(3) -0.001(2) 0.005(3) 0.012(3) C2 0.130(8) 0.035(3) 0.037(3) 0.000(3) 0.003(4) 0.030(4) C3 0.143(12) 0.024(4) 0.050(5) 0.000 0.004(6) 0.000 C4 0.156(11) 0.067(5) 0.107(8) -0.014(5) -0.006(7) 0.067(7) C5 0.029(2) 0.032(2) 0.025(2) -0.006(2) 0.008(2) -0.001(2) C6 0.030(3) 0.044(3) 0.033(3) -0.012(2) 0.014(2) -0.006(2) C7 0.041(3) 0.049(3) 0.028(2) -0.009(2) 0.018(2) -0.011(2) C8 0.041(3) 0.034(2) 0.028(2) -0.001(2) 0.012(2) -0.008(2) C9 0.039(3) 0.028(2) 0.024(2) -0.001(2) 0.011(2) -0.001(2) C10 0.042(3) 0.078(4) 0.046(3) -0.012(3) 0.023(3) 0.007(3) C11 0.078(5) 0.048(3) 0.034(3) 0.007(2) 0.021(3) 0.000(3) C12 0.031(3) 0.030(2) 0.041(3) 0.000(2) 0.015(2) -0.003(2) C13 0.034(3) 0.041(3) 0.050(3) -0.004(2) 0.021(2) -0.002(2) C14 0.052(3) 0.056(3) 0.052(3) 0.006(3) 0.034(3) -0.003(3) C15 0.049(3) 0.054(3) 0.051(3) 0.017(3) 0.030(3) 0.002(3) C16 0.039(3) 0.040(3) 0.044(3) 0.012(2) 0.018(2) 0.003(2) C17 0.042(3) 0.057(4) 0.076(4) 0.006(3) 0.030(3) 0.014(3) C18 0.090(6) 0.101(6) 0.074(5) 0.047(5) 0.049(5) 0.017(5) C20 0.086(6) 0.064(4) 0.086(6) 0.012(4) 0.025(5) 0.023(4) Cl21 0.146(2) 0.0719(13) 0.0784(14) 0.0167(11) 0.0096(14) 0.0227(14) Cl22 0.126(5) 0.128(5) 0.108(3) 0.058(3) 0.086(3) 0.069(4) Cl23 0.115(8) 0.191(16) 0.395(27) 0.182(17) 0.145(14) 0.062(10) C30 0.051(5) 0.093(6) 0.171(11) -0.035(7) 0.029(6) 0.010(5) Cl31 0.0746(14) 0.110(2) 0.143(2) 0.017(2) 0.0407(15) -0.0049(13) Cl32 0.102(2) 0.197(4) 0.195(4) 0.105(3) 0.077(2) 0.046(2) C40 0.185(32) 0.112(19) 0.114(20) 0.006(15) 0.031(20) -0.009(20) C41 0.092(8) 0.098(8) 0.148(12) -0.042(8) -0.012(8) -0.001(6) C42 0.062(6) 0.080(6) 0.148(10) -0.044(7) -0.034(6) 0.034(5) C43 0.079(7) 0.100(8) 0.161(12) -0.053(8) -0.039(7) 0.042(6) _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 Ti1 N1 1.806(5) . ? Ti1 N3 2.196(4) . ? Ti1 N3 2.196(4) 2 ? Ti1 Cl2 2.3486(13) 2 ? Ti1 Cl2 2.3486(13) . ? Ti1 Cl1 2.498(2) . ? Ti2 N1 1.763(5) . ? Ti2 N4 2.206(4) . ? Ti2 N4 2.206(4) 2 ? Ti2 Cl3 2.3425(14) 2 ? Ti2 Cl3 2.3425(14) . ? Ti2 N2 2.380(6) . ? N2 C1 1.327(7) 2 ? N2 C1 1.327(7) . ? N3 C9 1.340(6) . ? N3 C5 1.342(6) . ? N4 C16 1.347(7) . ? N4 C12 1.355(7) . ? C1 C2 1.410(9) . ? C2 C3 1.351(10) . ? C2 C4 1.520(14) . ? C3 C2 1.351(10) 2 ? C5 C6 1.386(7) . ? C6 C7 1.390(8) . ? C6 C10 1.502(8) . ? C7 C8 1.385(8) . ? C8 C9 1.384(7) . ? C8 C11 1.503(8) . ? C12 C13 1.384(7) . ? C13 C14 1.372(8) . ? C13 C17 1.503(8) . ? C14 C15 1.391(9) . ? C15 C16 1.376(8) . ? C15 C18 1.504(9) . ? C20 Cl22 1.694(10) . ? C20 Cl21 1.728(8) . ? C20 Cl23 1.91(2) . ? C30 Cl31 1.685(12) . ? C30 Cl32 1.773(13) . ? C40 C41 1.384(10) . ? C41 C43 1.387(8) 7_565 ? C41 C42 1.387(8) . ? C42 C43 1.384(9) . ? C43 C41 1.387(8) 7_565 ? 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 Ti1 N3 91.07(9) . . ? N1 Ti1 N3 91.07(9) . 2 ? N3 Ti1 N3 177.9(2) . 2 ? N1 Ti1 Cl2 92.59(4) . 2 ? N3 Ti1 Cl2 89.80(11) . 2 ? N3 Ti1 Cl2 90.11(11) 2 2 ? N1 Ti1 Cl2 92.59(4) . . ? N3 Ti1 Cl2 90.11(11) . . ? N3 Ti1 Cl2 89.80(11) 2 . ? Cl2 Ti1 Cl2 174.82(7) 2 . ? N1 Ti1 Cl1 180.0 . . ? N3 Ti1 Cl1 88.93(9) . . ? N3 Ti1 Cl1 88.93(9) 2 . ? Cl2 Ti1 Cl1 87.41(4) 2 . ? Cl2 Ti1 Cl1 87.41(4) . . ? N1 Ti2 N4 92.49(10) . . ? N1 Ti2 N4 92.49(10) . 2 ? N4 Ti2 N4 175.0(2) . 2 ? N1 Ti2 Cl3 97.41(4) . 2 ? N4 Ti2 Cl3 90.18(11) . 2 ? N4 Ti2 Cl3 89.18(11) 2 2 ? N1 Ti2 Cl3 97.41(4) . . ? N4 Ti2 Cl3 89.18(11) . . ? N4 Ti2 Cl3 90.18(11) 2 . ? Cl3 Ti2 Cl3 165.18(8) 2 . ? N1 Ti2 N2 180.0 . . ? N4 Ti2 N2 87.51(10) . . ? N4 Ti2 N2 87.51(10) 2 . ? Cl3 Ti2 N2 82.59(4) 2 . ? Cl3 Ti2 N2 82.59(4) . . ? Ti2 N1 Ti1 180.0 . . ? C1 N2 C1 118.5(7) 2 . ? C1 N2 Ti2 120.8(4) 2 . ? C1 N2 Ti2 120.8(4) . . ? C9 N3 C5 118.3(4) . . ? C9 N3 Ti1 119.5(3) . . ? C5 N3 Ti1 122.1(3) . . ? C16 N4 C12 118.0(4) . . ? C16 N4 Ti2 123.7(3) . . ? C12 N4 Ti2 118.0(3) . . ? N2 C1 C2 121.7(7) . . ? C3 C2 C1 119.4(8) . . ? C3 C2 C4 122.8(7) . . ? C1 C2 C4 117.7(9) . . ? C2 C3 C2 119.1(9) 2 . ? N3 C5 C6 123.0(5) . . ? C5 C6 C7 117.5(5) . . ? C5 C6 C10 120.2(5) . . ? C7 C6 C10 122.3(5) . . ? C8 C7 C6 120.3(4) . . ? C9 C8 C7 117.9(5) . . ? C9 C8 C11 120.2(5) . . ? C7 C8 C11 121.9(5) . . ? N3 C9 C8 122.9(5) . . ? N4 C12 C13 122.0(5) . . ? C14 C13 C12 118.5(5) . . ? C14 C13 C17 121.7(5) . . ? C12 C13 C17 119.8(5) . . ? C13 C14 C15 120.7(5) . . ? C16 C15 C14 117.3(5) . . ? C16 C15 C18 120.0(6) . . ? C14 C15 C18 122.8(5) . . ? N4 C16 C15 123.5(5) . . ? Cl22 C20 Cl21 113.0(5) . . ? Cl21 C20 Cl23 104.2(6) . . ? Cl31 C30 Cl32 111.0(6) . . ? C40 C41 C43 120.1(12) . 7_565 ? C40 C41 C42 119.8(11) . . ? C43 C41 C42 120.1(7) 7_565 . ? C43 C42 C41 121.7(6) . . ? C42 C43 C41 118.2(7) . 7_565 ? _refine_diff_density_max 0.709 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.104