Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ANTONIO.OTERO@UCLM.ES _publ_contact_author_name 'Prof Antonio Otero' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name A.Otero J.Fernandez-Baeza A.Antinolo J.Tejeda A.Lara-Sanchez ; L.Sanchez-Barba ; M.T.Exposito A.M.Rodriguez data_7 _database_code_CSD 188238 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H38 Cl4 N8 Nb2 O4' _chemical_formula_weight 1058.44 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' Cl Cl 0.1484 0.1585 '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' Nb Nb -2.0727 0.6215 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 36.442(5) _cell_length_b 36.442(8) _cell_length_c 19.618(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 22563(7) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9612 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'four circle diffractometer Nonius-Mach3' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 17979 _diffrn_reflns_av_R_equivalents 0.1485 _diffrn_reflns_av_sigmaI/netI 0.1305 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.99 _reflns_number_total 5954 _reflns_number_gt 1184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XCAD4 (Harms, Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0452P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5954 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3362 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.831 _refine_ls_shift/su_max 0.159 _refine_ls_shift/su_mean 0.022 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 Nb1 Nb 0.31443(3) 0.41682(3) 0.14690(4) 0.0811(3) Uani 1 1 d . . . Cl1 Cl 0.33156(8) 0.46808(8) 0.06312(13) 0.1121(10) Uani 1 1 d . . . Cl2 Cl 0.32089(8) 0.46147(8) 0.23815(13) 0.1104(10) Uani 1 1 d . . . O1 O 0.28562(17) 0.36982(17) 0.0867(2) 0.0698(16) Uani 1 1 d . . . O2 O 0.36202(17) 0.41836(18) 0.1531(3) 0.0936(18) Uani 1 1 d . . . N1 N 0.2829(3) 0.3638(3) 0.2224(4) 0.077(2) Uani 1 1 d . . . N2 N 0.2439(3) 0.3294(3) 0.2073(4) 0.074(2) Uani 1 1 d . . . N3 N 0.2378(2) 0.4023(3) 0.1486(4) 0.084(2) Uani 1 1 d . A . N4 N 0.2083(3) 0.3610(3) 0.1561(4) 0.077(2) Uani 1 1 d . . . C1 C 0.2197(3) 0.3287(3) 0.1485(4) 0.065(2) Uani 1 1 d . . . H1 H 0.1937 0.3010 0.1469 0.078 Uiso 1 1 calc . . . C2 C 0.2462(4) 0.3333 0.0833 0.073(4) Uani 1 2 d S . . C3 C 0.2325(4) 0.2982(3) 0.2546(5) 0.073(3) Uani 1 1 d . . . C4 C 0.2655(4) 0.3143(5) 0.2991(5) 0.095(3) Uani 1 1 d . . . H4 H 0.2671 0.3000 0.3372 0.114 Uiso 1 1 calc . . . C5 C 0.2959(4) 0.3539(4) 0.2806(5) 0.091(3) Uani 1 1 d . . . C6 C 0.1920(4) 0.2579(3) 0.2521(5) 0.106(4) Uani 1 1 d . . . H6A H 0.1767 0.2572 0.2119 0.159 Uiso 1 1 calc . . . H6B H 0.1755 0.2555 0.2918 0.159 Uiso 1 1 calc . . . H6C H 0.1975 0.2347 0.2510 0.159 Uiso 1 1 calc . . . C7 C 0.3370(3) 0.3835(4) 0.3121(5) 0.122(4) Uani 1 1 d . . . H7A H 0.3509 0.4090 0.2856 0.183 Uiso 1 1 calc . . . H7B H 0.3544 0.3706 0.3137 0.183 Uiso 1 1 calc . . . H7C H 0.3324 0.3901 0.3576 0.183 Uiso 1 1 calc . . . C8 C 0.1737(4) 0.3587(5) 0.1876(5) 0.084(3) Uani 1 1 d . . . C9 C 0.1797(4) 0.3965(5) 0.1985(6) 0.104(4) Uani 1 1 d . A . H9 H 0.1612 0.4037 0.2191 0.124 Uiso 1 1 calc . . . C10 C 0.2187(4) 0.4231(4) 0.1733(6) 0.103(4) Uani 1 1 d . . . C11 C 0.1372(4) 0.3165(4) 0.2056(7) 0.093(3) Uani 1 1 d . . . C12 C 0.1154(4) 0.2851(5) 0.1615(6) 0.111(4) Uani 1 1 d . . . H12 H 0.1232 0.2897 0.1158 0.133 Uiso 1 1 calc . . . C13 C 0.0815(5) 0.2457(5) 0.1805(9) 0.138(5) Uani 1 1 d . . . H13 H 0.0671 0.2242 0.1487 0.165 Uiso 1 1 calc . . . C14 C 0.0699(4) 0.2400(5) 0.2498(10) 0.137(5) Uani 1 1 d . . . H14 H 0.0483 0.2137 0.2642 0.164 Uiso 1 1 calc . . . C15 C 0.0887(6) 0.2704(6) 0.2947(8) 0.148(6) Uani 1 1 d . . . H15 H 0.0798 0.2665 0.3399 0.178 Uiso 1 1 calc . . . C16 C 0.1225(4) 0.3091(4) 0.2723(8) 0.116(4) Uani 1 1 d . . . H16 H 0.1357 0.3310 0.3037 0.140 Uiso 1 1 calc . . . C17 C 0.2350(4) 0.4666(4) 0.1549(12) 0.104(7) Uani 0.60 1 d PG A 1 C18 C 0.2335(4) 0.4909(7) 0.2082(7) 0.115(7) Uani 0.60 1 d PG A 1 H18 H 0.2228 0.4785 0.2504 0.138 Uiso 0.60 1 calc P B 1 C19 C 0.2479(5) 0.5338(7) 0.1985(9) 0.228(15) Uani 0.60 1 d PG A 1 H19 H 0.2469 0.5501 0.2341 0.274 Uiso 0.60 1 calc P C 1 C20 C 0.2639(5) 0.5523(5) 0.1354(12) 0.166(10) Uani 0.60 1 d PG A 1 H20 H 0.2736 0.5810 0.1289 0.199 Uiso 0.60 1 calc P D 1 C21 C 0.2655(5) 0.5280(8) 0.0821(7) 0.184(10) Uani 0.60 1 d PG A 1 H21 H 0.2762 0.5404 0.0400 0.221 Uiso 0.60 1 calc P E 1 C22 C 0.2510(5) 0.4851(8) 0.0919(9) 0.146(9) Uani 0.60 1 d PG A 1 H22 H 0.2521 0.4689 0.0562 0.175 Uiso 0.60 1 calc P F 1 C17A C 0.2454 0.4713 0.1875 0.121 Uani 0.40 1 d P A 2 C18A C 0.2454 0.4922 0.2466 0.181 Uani 0.40 1 d P A 2 H18A H 0.2345 0.4771 0.2869 0.217 Uiso 0.40 1 calc P G 2 C19A C 0.2616 0.5358 0.2457 0.346 Uani 0.40 1 d P A 2 H19A H 0.2616 0.5498 0.2853 0.415 Uiso 0.40 1 calc P H 2 C20A C 0.2778 0.5584 0.1856 0.222 Uani 0.40 1 d P A 2 H20A H 0.2887 0.5875 0.1850 0.267 Uiso 0.40 1 calc P I 2 C21A C 0.2779 0.5374 0.1264 0.242 Uani 0.40 1 d P A 2 H21A H 0.2887 0.5526 0.0862 0.290 Uiso 0.40 1 calc P J 2 C22A C 0.2616 0.4939 0.1274 0.170 Uani 0.40 1 d P A 2 H22A H 0.2617 0.4798 0.0878 0.204 Uiso 0.40 1 calc P K 2 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 Nb1 0.0730(7) 0.0863(7) 0.0814(6) -0.0003(5) 0.0078(5) 0.0377(6) Cl1 0.113(2) 0.096(2) 0.111(2) 0.0147(17) 0.0156(17) 0.0399(18) Cl2 0.108(2) 0.108(2) 0.104(2) -0.0164(16) 0.0050(16) 0.0456(18) O1 0.063(4) 0.073(4) 0.063(4) 0.002(3) 0.005(3) 0.025(3) O2 0.063(4) 0.106(5) 0.109(5) 0.005(4) 0.006(3) 0.040(4) N1 0.074(6) 0.084(6) 0.071(6) 0.005(5) 0.002(5) 0.039(6) N2 0.082(6) 0.074(6) 0.061(6) 0.017(5) 0.020(5) 0.035(5) N3 0.075(6) 0.066(6) 0.110(6) 0.008(5) 0.011(5) 0.035(6) N4 0.069(6) 0.088(7) 0.081(6) 0.003(5) 0.004(5) 0.044(6) C1 0.071(7) 0.067(7) 0.050(6) 0.009(5) 0.002(5) 0.030(6) C2 0.085(8) 0.096(12) 0.043(8) 0.005(8) 0.003(4) 0.048(6) C3 0.096(9) 0.062(8) 0.063(7) 0.003(6) 0.009(7) 0.040(7) C4 0.111(11) 0.128(11) 0.063(7) -0.002(7) -0.006(7) 0.074(10) C5 0.103(10) 0.106(10) 0.059(7) -0.005(7) -0.002(7) 0.049(9) C6 0.144(10) 0.092(9) 0.076(7) 0.031(6) 0.014(7) 0.054(8) C7 0.088(8) 0.149(11) 0.111(8) -0.020(8) -0.038(7) 0.046(8) C8 0.072(9) 0.106(11) 0.081(7) -0.012(7) 0.009(6) 0.050(9) C9 0.101(10) 0.110(11) 0.127(9) 0.004(8) 0.034(8) 0.073(9) C10 0.107(11) 0.073(9) 0.155(11) 0.005(8) 0.021(8) 0.064(9) C11 0.080(9) 0.118(12) 0.086(9) -0.015(8) 0.006(8) 0.053(9) C12 0.068(9) 0.139(12) 0.103(10) 0.015(9) 0.001(8) 0.035(9) C13 0.092(10) 0.152(14) 0.133(13) -0.028(11) -0.026(9) 0.033(10) C14 0.101(12) 0.137(14) 0.152(16) 0.019(11) 0.037(11) 0.044(10) C15 0.123(14) 0.151(16) 0.146(14) 0.000(12) 0.028(11) 0.050(12) C16 0.108(10) 0.112(11) 0.144(12) -0.021(9) 0.019(9) 0.065(9) C17 0.079(14) 0.12(2) 0.096(16) -0.024(14) -0.014(13) 0.037(14) C18 0.111(16) 0.094(16) 0.137(19) 0.020(15) 0.008(13) 0.051(14) C19 0.22(3) 0.19(3) 0.31(4) 0.03(3) 0.15(3) 0.12(3) C20 0.16(2) 0.092(17) 0.23(3) -0.014(19) 0.06(2) 0.054(16) C21 0.13(2) 0.18(3) 0.23(3) -0.06(2) -0.033(19) 0.08(2) C22 0.112(19) 0.099(18) 0.22(3) -0.002(19) -0.029(18) 0.045(16) C17A 0.150 0.178 0.114 -0.067 -0.027 0.140 C18A 0.228 0.168 0.245 -0.072 -0.079 0.172 C19A 0.330 0.072 0.550 0.061 0.174 0.036 C20A 0.308 0.078 0.298 0.013 0.086 0.110 C21A 0.237 0.083 0.431 -0.031 0.039 0.100 C22A 0.237 0.066 0.248 -0.021 -0.076 0.106 _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 Nb1 O2 1.711(5) . ? Nb1 O1 1.906(5) . ? Nb1 N1 2.243(7) . ? Nb1 Cl1 2.327(3) . ? Nb1 Cl2 2.350(3) . ? Nb1 N3 2.568(8) . ? O1 C2 1.387(8) . ? N1 C5 1.353(11) . ? N1 N2 1.376(9) . ? N2 C3 1.362(10) . ? N2 C1 1.442(10) . ? N3 N4 1.352(9) . ? N3 C10 1.352(10) . ? N4 C8 1.371(11) . ? N4 C1 1.441(10) . ? C1 C2 1.560(10) . ? C2 O1 1.387(8) 18_554 ? C2 C1 1.560(10) 18_554 ? C3 C4 1.359(11) . ? C3 C6 1.473(12) . ? C4 C5 1.357(12) . ? C5 C7 1.473(13) . ? C8 C9 1.297(12) . ? C8 C11 1.487(14) . ? C9 C10 1.350(13) . ? C10 C17 1.433(15) . ? C10 C17A 1.548(12) . ? C11 C12 1.335(13) . ? C11 C16 1.388(14) . ? C12 C13 1.399(15) . ? C13 C14 1.407(17) . ? C14 C15 1.309(16) . ? C15 C16 1.401(16) . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C17A C18A 1.3900 . ? C17A C22A 1.3900 . ? C18A C19A 1.3900 . ? C19A C20A 1.3900 . ? C20A C21A 1.3900 . ? C21A C22A 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nb1 O1 99.6(3) . . ? O2 Nb1 N1 93.2(3) . . ? O1 Nb1 N1 79.7(3) . . ? O2 Nb1 Cl1 99.4(2) . . ? O1 Nb1 Cl1 95.14(17) . . ? N1 Nb1 Cl1 167.0(2) . . ? O2 Nb1 Cl2 100.1(2) . . ? O1 Nb1 Cl2 156.01(18) . . ? N1 Nb1 Cl2 85.6(2) . . ? Cl1 Nb1 Cl2 95.08(10) . . ? O2 Nb1 N3 170.1(3) . . ? O1 Nb1 N3 76.7(3) . . ? N1 Nb1 N3 77.2(3) . . ? Cl1 Nb1 N3 90.13(19) . . ? Cl2 Nb1 N3 81.7(2) . . ? C2 O1 Nb1 137.0(4) . . ? C5 N1 N2 106.2(8) . . ? C5 N1 Nb1 133.6(9) . . ? N2 N1 Nb1 119.5(6) . . ? N1 N2 C3 110.9(8) . . ? N1 N2 C1 122.2(8) . . ? C3 N2 C1 126.9(9) . . ? N4 N3 C10 103.8(9) . . ? N4 N3 Nb1 114.2(6) . . ? C10 N3 Nb1 134.6(8) . . ? N3 N4 C8 108.2(9) . . ? N3 N4 C1 120.3(8) . . ? C8 N4 C1 129.2(10) . . ? N4 C1 N2 109.1(7) . . ? N4 C1 C2 114.3(7) . . ? N2 C1 C2 108.3(7) . . ? O1 C2 O1 112.5(11) . 18_554 ? O1 C2 C1 105.9(4) . 18_554 ? O1 C2 C1 110.7(4) 18_554 18_554 ? O1 C2 C1 110.7(4) . . ? O1 C2 C1 105.9(4) 18_554 . ? C1 C2 C1 111.3(11) 18_554 . ? N2 C3 C4 104.1(9) . . ? N2 C3 C6 123.0(10) . . ? C4 C3 C6 132.9(11) . . ? C5 C4 C3 111.2(10) . . ? N1 C5 C4 107.5(10) . . ? N1 C5 C7 121.5(12) . . ? C4 C5 C7 131.0(12) . . ? C9 C8 N4 110.3(11) . . ? C9 C8 C11 130.5(12) . . ? N4 C8 C11 119.2(12) . . ? C8 C9 C10 105.2(10) . . ? N3 C10 C9 112.4(10) . . ? N3 C10 C17 118.9(14) . . ? C9 C10 C17 126.4(13) . . ? N3 C10 C17A 119.4(11) . . ? C9 C10 C17A 126.0(12) . . ? C17 C10 C17A 27.5(8) . . ? C12 C11 C16 116.0(12) . . ? C12 C11 C8 125.0(12) . . ? C16 C11 C8 118.9(12) . . ? C11 C12 C13 123.3(12) . . ? C12 C13 C14 117.0(12) . . ? C15 C14 C13 122.3(16) . . ? C14 C15 C16 117.7(15) . . ? C15 C16 C11 123.5(12) . . ? C18 C17 C22 120.0 . . ? C18 C17 C10 112.9(18) . . ? C22 C17 C10 127.1(18) . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C21 C22 C17 120.0 . . ? C18A C17A C22A 120.0 . . ? C18A C17A C10 126.9(5) . . ? C22A C17A C10 111.1(5) . . ? C19A C18A C17A 120.0 . . ? C18A C19A C20A 120.0 . . ? C19A C20A C21A 120.0 . . ? C22A C21A C20A 120.0 . . ? C21A C22A C17A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.294 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.062