# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 872196' #TrackingRef 'compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 N14 O24 P4 Zn3' _chemical_formula_weight 1368.78 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 29.620(6) _cell_length_b 61.500(12) _cell_length_c 5.3200(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9691(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4450 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 25.68 _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.876 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5536 _exptl_absorpt_coefficient_mu 1.710 _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 298(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 19177 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -74 _diffrn_reflns_limit_k_max 74 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4450 _reflns_number_gt 4255 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1068P)^2^+31.4027P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(16) _refine_ls_number_reflns 4450 _refine_ls_number_parameters 368 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_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 Zn1 Zn 0.942294(16) 0.241575(7) -0.11560(10) 0.01775(16) Uani 1 1 d . . . Zn2 Zn 0.7500 0.2500 -0.1341(3) 0.0549(3) Uani 1 2 d SU . . P1 P 0.84747(4) 0.23280(2) -0.3272(3) 0.0277(3) Uani 1 1 d . . . P2 P 0.97861(3) 0.221146(16) -0.6178(2) 0.0161(2) Uani 1 1 d . . . N1 N 0.54933(16) 0.18880(8) 1.4817(10) 0.0338(10) Uani 1 1 d . . . H1 H 0.5291 0.1923 1.5874 0.051 Uiso 1 1 d R . . N2 N 0.69111(18) 0.07427(7) 0.5393(10) 0.0345(11) Uani 1 1 d . . . H2 H 0.6913 0.0605 0.5313 0.052 Uiso 1 1 d R . . N3 N 0.7398(3) 0.22234(13) 0.0850(12) 0.0715(19) Uani 1 1 d . . . N4 N 0.65817(15) 0.18277(6) 0.7616(9) 0.0272(9) Uani 1 1 d . . . N5 N 0.64494(14) 0.14627(6) 0.8743(10) 0.0276(9) Uani 1 1 d . . . N6 N 0.69325(14) 0.15454(7) 0.5346(10) 0.0270(9) Uani 1 1 d . . . N7 N 0.5750(2) 0.08923(9) 0.3129(12) 0.0488(14) Uani 1 1 d . . . C1 C 0.7552(3) 0.20173(16) 0.0880(15) 0.0715(19) Uani 1 1 d . . . H1A H 0.7780 0.1980 -0.0245 0.086 Uiso 1 1 calc R . . C2 C 0.7396(2) 0.18591(13) 0.2452(15) 0.0493(17) Uani 1 1 d . . . H2A H 0.7509 0.1718 0.2396 0.059 Uiso 1 1 calc R . . C3 C 0.7098(3) 0.22747(12) 0.251(2) 0.065(2) Uani 1 1 d . . . H3A H 0.7004 0.2419 0.2594 0.078 Uiso 1 1 calc R . . C4 C 0.6910(2) 0.21296(10) 0.4148(17) 0.0514(18) Uani 1 1 d . . . H4A H 0.6684 0.2174 0.5248 0.062 Uiso 1 1 calc R . . C5 C 0.70561(18) 0.19194(8) 0.4164(11) 0.0298(11) Uani 1 1 d . . . C6 C 0.68533(17) 0.17579(8) 0.5810(10) 0.0256(11) Uani 1 1 d . . . C7 C 0.63858(16) 0.16781(7) 0.9004(11) 0.0248(9) Uani 1 1 d . . . C8 C 0.67201(17) 0.14090(8) 0.6892(10) 0.0255(11) Uani 1 1 d . . . C9 C 0.67866(16) 0.11699(7) 0.6373(12) 0.0258(10) Uani 1 1 d . . . C10 C 0.7062(2) 0.11094(9) 0.4378(12) 0.0387(14) Uani 1 1 d . . . H10A H 0.7199 0.1212 0.3350 0.046 Uiso 1 1 calc R . . C11 C 0.7123(2) 0.08883(9) 0.3995(14) 0.0396(13) Uani 1 1 d . . . H11A H 0.7317 0.0841 0.2731 0.048 Uiso 1 1 calc R . . C12 C 0.6646(2) 0.07962(9) 0.7320(12) 0.0339(12) Uani 1 1 d . . . H12A H 0.6507 0.0690 0.8290 0.041 Uiso 1 1 calc R . . C13 C 0.6583(2) 0.10158(8) 0.7839(12) 0.0314(12) Uani 1 1 d . . . H13A H 0.6403 0.1058 0.9184 0.038 Uiso 1 1 calc R . . C14 C 0.60770(16) 0.17509(7) 1.1030(11) 0.0252(10) Uani 1 1 d . . . C15 C 0.58769(19) 0.15999(8) 1.2675(12) 0.0307(11) Uani 1 1 d . . . H15A H 0.5935 0.1452 1.2509 0.037 Uiso 1 1 calc R . . C16 C 0.5599(2) 0.16735(10) 1.4502(12) 0.0369(14) Uani 1 1 d . . . H16A H 0.5472 0.1573 1.5601 0.044 Uiso 1 1 calc R . . C17 C 0.59686(18) 0.19703(8) 1.1323(13) 0.0315(11) Uani 1 1 d . . . H17A H 0.6093 0.2075 1.0265 0.038 Uiso 1 1 calc R . . C18 C 0.56740(19) 0.20289(9) 1.3213(11) 0.0327(12) Uani 1 1 d . . . H18A H 0.5598 0.2175 1.3372 0.039 Uiso 1 1 calc R . . O1 O 0.85513(15) 0.23158(9) -0.6197(10) 0.0483(11) Uani 1 1 d . . . O2 O 0.85828(17) 0.20945(7) -0.2209(11) 0.0454(11) Uani 1 1 d . . . H5 H 0.8680 0.2026 -0.3483 0.068 Uiso 1 1 d R . . O3 O 0.79868(15) 0.23862(8) -0.2934(13) 0.0566(14) Uani 1 1 d U . . O4 O 0.88001(12) 0.24815(6) -0.2010(8) 0.0312(9) Uani 1 1 d . . . O5 O 0.96379(11) 0.21881(5) -0.3434(7) 0.0199(6) Uani 1 1 d . . . O6 O 0.94054(12) 0.23168(8) -0.7680(7) 0.0335(9) Uani 1 1 d . . . O7 O 0.98466(14) 0.19755(6) -0.7138(8) 0.0315(9) Uani 1 1 d . . . H6 H 0.9615 0.1984 -0.8037 0.047 Uiso 1 1 d R . . O8 O 1.02242(13) 0.23271(6) -0.6517(9) 0.0325(9) Uani 1 1 d . . . O9 O 0.5710(3) 0.10756(9) 0.2280(16) 0.088(2) Uani 1 1 d . . . O10 O 0.5521(3) 0.08435(14) 0.5026(19) 0.096(3) Uani 1 1 d . . . O11 O 0.5988(2) 0.07493(10) 0.2161(13) 0.0728(18) Uani 1 1 d . . . O12 O 0.5268(3) 0.12363(14) 0.7679(18) 0.088(2) Uani 1 1 d D . . H4 H 0.532(4) 0.1136(14) 0.875(17) 0.08(3) Uiso 1 1 d D . . H3 H 0.526(5) 0.122(2) 0.609(6) 0.11(5) Uiso 1 1 d 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 Zn1 0.0192(2) 0.0171(2) 0.0169(3) -0.0009(2) 0.0009(2) -0.00136(18) Zn2 0.0545(7) 0.0516(6) 0.0587(8) 0.000 0.000 0.0011(5) P1 0.0183(6) 0.0319(6) 0.0329(8) -0.0024(6) 0.0002(5) -0.0003(5) P2 0.0184(5) 0.0154(4) 0.0146(5) 0.0013(5) 0.0040(5) -0.0008(4) N1 0.030(2) 0.039(3) 0.033(3) -0.003(2) 0.0082(19) 0.0100(19) N2 0.046(3) 0.020(2) 0.037(3) -0.005(2) -0.002(2) 0.0088(18) N3 0.103(4) 0.081(3) 0.031(2) 0.015(3) 0.003(2) -0.063(4) N4 0.033(2) 0.0173(18) 0.031(2) -0.0019(17) 0.0068(19) 0.0049(16) N5 0.036(2) 0.0190(17) 0.028(2) 0.0021(19) 0.012(2) 0.0043(15) N6 0.032(2) 0.0174(19) 0.032(2) 0.0022(18) 0.0071(18) 0.0020(16) N7 0.058(3) 0.041(3) 0.047(4) 0.008(3) 0.001(3) 0.000(3) C1 0.103(4) 0.081(3) 0.031(2) 0.015(3) 0.003(2) -0.063(4) C2 0.046(4) 0.060(4) 0.042(4) -0.013(3) 0.025(3) -0.019(3) C3 0.090(6) 0.029(3) 0.077(6) 0.024(4) -0.005(5) -0.021(3) C4 0.056(4) 0.033(3) 0.065(5) 0.001(4) 0.014(4) -0.004(3) C5 0.032(2) 0.027(2) 0.031(3) 0.000(2) 0.003(2) -0.008(2) C6 0.028(2) 0.024(2) 0.025(3) 0.0011(19) 0.005(2) -0.0013(18) C7 0.026(2) 0.023(2) 0.025(2) -0.006(2) 0.001(2) -0.0021(17) C8 0.031(2) 0.017(2) 0.029(3) -0.0015(19) 0.005(2) 0.0056(17) C9 0.030(2) 0.015(2) 0.032(3) -0.006(2) 0.005(2) 0.0034(17) C10 0.053(3) 0.023(2) 0.040(4) -0.004(2) 0.018(3) 0.005(2) C11 0.054(3) 0.028(2) 0.037(3) -0.010(3) 0.012(3) 0.006(2) C12 0.042(3) 0.022(2) 0.037(3) 0.003(2) -0.004(3) 0.000(2) C13 0.038(3) 0.023(2) 0.033(3) -0.004(2) 0.008(2) 0.007(2) C14 0.025(2) 0.022(2) 0.028(3) -0.002(2) 0.007(2) 0.0043(17) C15 0.034(3) 0.024(2) 0.034(3) -0.002(2) 0.009(2) 0.003(2) C16 0.040(3) 0.038(3) 0.032(3) 0.003(2) 0.013(2) 0.006(2) C17 0.038(3) 0.022(2) 0.034(3) 0.001(2) 0.011(3) 0.0058(19) C18 0.035(3) 0.028(2) 0.035(3) -0.005(2) 0.004(2) 0.006(2) O1 0.034(2) 0.078(3) 0.033(2) -0.005(3) -0.006(2) 0.0013(19) O2 0.049(3) 0.035(2) 0.051(3) 0.001(2) 0.004(2) 0.0004(19) O3 0.027(2) 0.050(3) 0.093(5) 0.003(3) -0.0047(19) -0.0032(16) O4 0.0237(17) 0.0240(16) 0.046(2) -0.0040(16) 0.0020(16) 0.0017(14) O5 0.0296(16) 0.0163(13) 0.0139(16) 0.0005(13) 0.0025(14) 0.0008(12) O6 0.0207(18) 0.063(3) 0.0164(19) 0.0124(18) 0.0009(13) 0.0047(16) O7 0.037(2) 0.0245(17) 0.033(2) -0.0096(15) 0.0163(17) -0.0114(15) O8 0.0298(18) 0.0233(16) 0.044(2) -0.0004(17) 0.0054(18) -0.0106(13) O9 0.143(6) 0.036(3) 0.086(5) 0.018(3) -0.001(5) 0.001(3) O10 0.116(6) 0.087(5) 0.086(5) 0.021(4) 0.043(5) 0.001(4) O11 0.086(4) 0.059(3) 0.073(4) 0.007(3) 0.025(4) 0.008(3) O12 0.112(6) 0.083(5) 0.070(5) 0.004(4) 0.025(5) 0.035(4) _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 Zn1 O8 1.905(3) 6_755 ? Zn1 O4 1.943(4) . ? Zn1 O6 1.948(4) 1_556 ? Zn1 O5 1.958(3) . ? Zn2 O3 1.813(5) 14_655 ? Zn2 O3 1.813(5) . ? Zn2 N3 2.084(7) 14_655 ? Zn2 N3 2.084(7) . ? P1 O4 1.507(4) . ? P1 O3 1.500(5) . ? P1 O1 1.574(5) . ? P1 O2 1.576(5) . ? P2 O8 1.491(4) . ? P2 O6 1.526(4) . ? P2 O5 1.531(4) . ? P2 O7 1.549(4) . ? N1 C18 1.329(8) . ? N1 C16 1.366(8) . ? N2 C11 1.323(9) . ? N2 C12 1.333(9) . ? N3 C3 1.293(14) . ? N3 C1 1.347(15) . ? N4 C7 1.315(7) . ? N4 C6 1.324(7) . ? N5 C8 1.312(7) . ? N5 C7 1.345(6) . ? N6 C8 1.333(7) . ? N6 C6 1.350(7) . ? N7 O9 1.220(8) . ? N7 O11 1.239(8) . ? N7 O10 1.251(10) . ? C1 C2 1.364(11) . ? C2 C5 1.408(9) . ? C3 C4 1.365(11) . ? C4 C5 1.363(9) . ? C5 C6 1.454(7) . ? C7 C14 1.483(7) . ? C8 C9 1.510(6) . ? C9 C13 1.367(8) . ? C9 C10 1.389(8) . ? C10 C11 1.387(7) . ? C12 C13 1.391(8) . ? C14 C17 1.396(6) . ? C14 C15 1.407(8) . ? C15 C16 1.353(8) . ? C17 C18 1.379(8) . ? O6 Zn1 1.948(4) 1_554 ? O8 Zn1 1.905(3) 6_754 ? 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 O8 Zn1 O4 108.94(16) 6_755 . ? O8 Zn1 O6 111.69(19) 6_755 1_556 ? O4 Zn1 O6 105.18(17) . 1_556 ? O8 Zn1 O5 110.64(16) 6_755 . ? O4 Zn1 O5 108.23(15) . . ? O6 Zn1 O5 111.91(16) 1_556 . ? O3 Zn2 O3 124.3(4) 14_655 . ? O3 Zn2 N3 93.5(3) 14_655 14_655 ? O3 Zn2 N3 117.5(3) . 14_655 ? O3 Zn2 N3 117.5(3) 14_655 . ? O3 Zn2 N3 93.5(3) . . ? N3 Zn2 N3 112.0(4) 14_655 . ? O4 P1 O3 114.4(3) . . ? O4 P1 O1 112.2(3) . . ? O3 P1 O1 105.6(3) . . ? O4 P1 O2 106.3(3) . . ? O3 P1 O2 111.7(3) . . ? O1 P1 O2 106.4(3) . . ? O8 P2 O6 112.2(2) . . ? O8 P2 O5 114.2(2) . . ? O6 P2 O5 109.09(19) . . ? O8 P2 O7 107.8(2) . . ? O6 P2 O7 108.1(3) . . ? O5 P2 O7 105.05(19) . . ? C18 N1 C16 117.3(5) . . ? C11 N2 C12 123.0(5) . . ? C3 N3 C1 117.0(6) . . ? C3 N3 Zn2 106.4(6) . . ? C1 N3 Zn2 136.5(6) . . ? C7 N4 C6 116.7(4) . . ? C8 N5 C7 114.3(4) . . ? C8 N6 C6 114.5(5) . . ? O9 N7 O11 123.8(7) . . ? O9 N7 O10 117.9(8) . . ? O11 N7 O10 118.2(7) . . ? C2 C1 N3 124.3(9) . . ? C1 C2 C5 116.8(8) . . ? N3 C3 C4 123.8(8) . . ? C3 C4 C5 119.6(8) . . ? C4 C5 C2 118.2(6) . . ? C4 C5 C6 121.4(5) . . ? C2 C5 C6 120.3(5) . . ? N4 C6 N6 123.5(5) . . ? N4 C6 C5 117.8(4) . . ? N6 C6 C5 118.6(5) . . ? N4 C7 N5 124.7(5) . . ? N4 C7 C14 118.0(4) . . ? N5 C7 C14 117.3(4) . . ? N5 C8 N6 126.4(4) . . ? N5 C8 C9 117.5(4) . . ? N6 C8 C9 116.0(4) . . ? C13 C9 C10 120.6(5) . . ? C13 C9 C8 120.9(5) . . ? C10 C9 C8 118.5(5) . . ? C9 C10 C11 116.8(5) . . ? N2 C11 C10 121.3(6) . . ? N2 C12 C13 118.1(5) . . ? C9 C13 C12 120.1(5) . . ? C17 C14 C15 118.1(5) . . ? C17 C14 C7 121.0(5) . . ? C15 C14 C7 120.8(4) . . ? C16 C15 C14 118.8(5) . . ? C15 C16 N1 123.4(5) . . ? C18 C17 C14 118.7(5) . . ? N1 C18 C17 123.5(5) . . ? P1 O3 Zn2 156.1(4) . . ? P1 O4 Zn1 125.5(2) . . ? P2 O5 Zn1 128.05(18) . . ? P2 O6 Zn1 127.6(2) . 1_554 ? P2 O8 Zn1 149.5(3) . 6_754 ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.729 _refine_diff_density_min -1.700 _refine_diff_density_rms 0.137