Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2002 data_001018c _database_code_CSD 172823 _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Chen, Langxing' 'He, Xiwen' 'Leng, Xuebing' 'Li, Qingshan' 'Sun, Hao' 'Xu, Fengbo' 'Zeng, Xianshun' 'Zhang, Zheng-Zhi' _publ_contact_author_name 'Dr Xianshun Zeng' _publ_contact_author_address ; Dr Xianshun Zeng Nankai University a. State Key Laboratory of Elemento Tianjin 300071 CHINA ; _publ_contact_author_email 'XSHZENG@EYOU.COM' _publ_section_title ; The first synthesis of novel tweezer-like receptor molecules bis(phenylselenoalkoxy)calix[4]arene derivatives as sensors for ion-selective electrodes ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H78 Cl2 O4 Se2' _chemical_formula_weight 1128.07 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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' _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 21.4021(18) _cell_length_b 12.7375(11) _cell_length_c 21.3752(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.207(2) _cell_angle_gamma 90.00 _cell_volume 5827.0(9) _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 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 1.406 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6778 _exptl_absorpt_correction_T_max 0.8168 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11775 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5140 _reflns_number_gt 3565 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1002P)^2^+4.8651P] 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 5140 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1747 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _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 Se1 Se 0.15653(2) 0.02317(5) 0.75218(3) 0.0775(2) Uani 0.90 1 d P . . Se2 Se 0.1106(4) -0.0635(4) 0.7640(2) 0.100(2) Uani 0.10 1 d P . . O1 O -0.05349(10) 0.28893(18) 0.69712(10) 0.0460(6) Uani 1 1 d . . . H1C H -0.0174 0.2864 0.6845 0.069 Uiso 1 1 calc R . . O2 O 0.06894(9) 0.25855(16) 0.66774(9) 0.0365(5) Uani 1 1 d . . . C1 C -0.16533(14) 0.3486(3) 0.75189(14) 0.0390(7) Uani 1 1 d . . . H1A H -0.2104 0.3544 0.7546 0.047 Uiso 1 1 calc R . . H1B H -0.1545 0.2748 0.7540 0.047 Uiso 1 1 calc R . . C2 C -0.14339(13) 0.3940(2) 0.68975(14) 0.0365(7) Uani 1 1 d . . . C3 C -0.17860(14) 0.4680(3) 0.65828(15) 0.0421(8) Uani 1 1 d . . . H3A H -0.2172 0.4870 0.6746 0.051 Uiso 1 1 calc R . . C4 C -0.15868(15) 0.5153(3) 0.60319(15) 0.0435(8) Uani 1 1 d . . . C5 C -0.10137(14) 0.4828(3) 0.57940(14) 0.0400(7) Uani 1 1 d . . . H5A H -0.0873 0.5129 0.5424 0.048 Uiso 1 1 calc R . . C6 C -0.06428(13) 0.4076(2) 0.60842(13) 0.0354(7) Uani 1 1 d . . . C7 C -0.00218(13) 0.3760(3) 0.57956(14) 0.0381(7) Uani 1 1 d . . . H7A H -0.0015 0.3992 0.5363 0.046 Uiso 1 1 calc R . . H7B H 0.0009 0.3000 0.5796 0.046 Uiso 1 1 calc R . . C8 C 0.05477(13) 0.4212(3) 0.61346(13) 0.0352(7) Uani 1 1 d . . . C9 C 0.07408(15) 0.5244(3) 0.60270(15) 0.0398(7) Uani 1 1 d . . . H9A H 0.0525 0.5644 0.5733 0.048 Uiso 1 1 calc R . . C10 C 0.12401(15) 0.5695(3) 0.63403(15) 0.0415(7) Uani 1 1 d . . . C11 C 0.15323(15) 0.5085(3) 0.67980(15) 0.0423(7) Uani 1 1 d . . . H11A H 0.1863 0.5376 0.7022 0.051 Uiso 1 1 calc R . . C12 C 0.13535(13) 0.4064(2) 0.69342(13) 0.0351(7) Uani 1 1 d . . . C13 C -0.08560(13) 0.3633(2) 0.66442(14) 0.0357(7) Uani 1 1 d . . . C14 C 0.08738(13) 0.3623(2) 0.65752(13) 0.0339(7) Uani 1 1 d . . . C15 C -0.19971(17) 0.5995(3) 0.57208(17) 0.0552(10) Uani 1 1 d . . . C16 C -0.26279(19) 0.5512(4) 0.5540(2) 0.0729(13) Uani 1 1 d . . . H16A H -0.2562 0.4945 0.5252 0.109 Uiso 1 1 calc R . . H16B H -0.2886 0.6037 0.5346 0.109 Uiso 1 1 calc R . . H16C H -0.2831 0.5251 0.5908 0.109 Uiso 1 1 calc R . . C17 C -0.2107(2) 0.6898(3) 0.6188(2) 0.0698(11) Uani 1 1 d . . . H17A H -0.2296 0.6625 0.6561 0.105 Uiso 1 1 calc R . . H17B H -0.2380 0.7411 0.6002 0.105 Uiso 1 1 calc R . . H17C H -0.1715 0.7221 0.6292 0.105 Uiso 1 1 calc R . . C18 C -0.1693(2) 0.6444(5) 0.5130(2) 0.0966(19) Uani 1 1 d . . . H18A H -0.1620 0.5887 0.4836 0.145 Uiso 1 1 calc R . . H18B H -0.1302 0.6768 0.5238 0.145 Uiso 1 1 calc R . . H18C H -0.1965 0.6957 0.4945 0.145 Uiso 1 1 calc R . . C19 C 0.14755(18) 0.6806(3) 0.61763(18) 0.0558(9) Uani 1 1 d . . . C20 C 0.0929(3) 0.7544(4) 0.6055(3) 0.107(2) Uani 1 1 d . . . H20A H 0.0669 0.7261 0.5729 0.160 Uiso 1 1 calc R . . H20B H 0.1085 0.8218 0.5929 0.160 Uiso 1 1 calc R . . H20C H 0.0688 0.7619 0.6431 0.160 Uiso 1 1 calc R . . C21 C 0.1874(3) 0.6730(4) 0.5593(3) 0.0975(18) Uani 1 1 d . . . H21A H 0.2215 0.6255 0.5667 0.146 Uiso 1 1 calc R . . H21B H 0.2035 0.7412 0.5490 0.146 Uiso 1 1 calc R . . H21C H 0.1624 0.6475 0.5251 0.146 Uiso 1 1 calc R . . C22 C 0.1875(3) 0.7284(4) 0.6697(3) 0.1001(18) Uani 1 1 d . . . H22A H 0.2232 0.6844 0.6774 0.150 Uiso 1 1 calc R . . H22B H 0.1632 0.7339 0.7072 0.150 Uiso 1 1 calc R . . H22C H 0.2013 0.7970 0.6573 0.150 Uiso 1 1 calc R . . C23 C 0.10451(16) 0.1824(3) 0.63316(16) 0.0471(8) Uani 1 1 d . . . H23A H 0.1481 0.1849 0.6458 0.057 Uiso 1 1 calc R . . H23B H 0.1019 0.1971 0.5887 0.057 Uiso 1 1 calc R . . C24 C 0.07743(19) 0.0755(3) 0.64698(19) 0.0599(10) Uani 1 1 d . . . H24A H 0.0357 0.0724 0.6291 0.072 Uiso 1 1 calc R . . H24B H 0.1026 0.0233 0.6256 0.072 Uiso 1 1 calc R . . C25 C 0.0733(2) 0.0450(3) 0.7146(2) 0.0700(11) Uani 1 1 d . . . C26 C 0.1265(2) 0.0162(4) 0.8373(2) 0.0800(14) Uani 1 1 d . . . C27 C 0.0954(3) -0.0723(6) 0.8571(4) 0.114(2) Uani 1 1 d . . . C28 C 0.0726(4) -0.0783(7) 0.9174(6) 0.150(4) Uani 1 1 d . . . H28A H 0.0514 -0.1375 0.9313 0.180 Uiso 1 1 calc R . . C29 C 0.0829(4) 0.0109(11) 0.9580(4) 0.158(4) Uani 1 1 d . . . H29A H 0.0697 0.0087 0.9994 0.190 Uiso 1 1 calc R . . C30 C 0.1116(4) 0.0974(7) 0.9355(3) 0.122(2) Uani 1 1 d . . . H30A H 0.1169 0.1561 0.9608 0.146 Uiso 1 1 calc R . . C31 C 0.1326(3) 0.0984(5) 0.8760(3) 0.0921(15) Uani 1 1 d . . . H31A H 0.1521 0.1587 0.8613 0.110 Uiso 1 1 calc R . . C32 C 1.0000 0.5816(5) 0.7500 0.0728(17) Uani 1 2 d S . . Cl1 Cl 0.95009(7) 0.65497(14) 0.70467(7) 0.1067(5) Uani 1 1 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 Se1 0.0632(3) 0.0885(4) 0.0808(4) 0.0009(3) 0.0083(3) 0.0210(3) Se2 0.184(6) 0.050(3) 0.065(3) -0.002(2) 0.029(3) 0.042(3) O1 0.0346(11) 0.0558(15) 0.0477(13) 0.0157(11) 0.0040(9) 0.0078(10) O2 0.0330(10) 0.0353(12) 0.0414(11) -0.0043(9) 0.0042(8) 0.0032(9) C1 0.0302(15) 0.0453(19) 0.0415(17) 0.0026(14) 0.0004(13) -0.0036(13) C2 0.0304(15) 0.0429(18) 0.0361(16) -0.0028(13) -0.0024(12) -0.0042(13) C3 0.0294(15) 0.052(2) 0.0447(18) 0.0021(15) 0.0010(13) 0.0039(14) C4 0.0359(16) 0.054(2) 0.0400(17) 0.0036(15) -0.0028(13) 0.0067(15) C5 0.0369(16) 0.0483(19) 0.0347(16) 0.0056(14) 0.0002(13) 0.0003(14) C6 0.0311(14) 0.0419(18) 0.0332(15) -0.0037(13) -0.0016(12) -0.0008(13) C7 0.0360(16) 0.0475(19) 0.0308(15) -0.0019(13) -0.0007(12) 0.0030(14) C8 0.0290(14) 0.0453(19) 0.0313(15) -0.0045(13) 0.0041(11) 0.0042(13) C9 0.0403(17) 0.0428(18) 0.0363(16) 0.0031(14) 0.0028(13) 0.0049(14) C10 0.0429(17) 0.0426(18) 0.0392(17) -0.0022(14) 0.0064(14) -0.0017(14) C11 0.0362(16) 0.0479(19) 0.0429(18) -0.0046(15) 0.0018(13) -0.0039(14) C12 0.0286(14) 0.0432(18) 0.0335(15) -0.0039(13) 0.0024(12) 0.0051(13) C13 0.0309(15) 0.0385(17) 0.0377(16) 0.0012(13) -0.0028(12) -0.0015(13) C14 0.0309(15) 0.0379(17) 0.0330(15) -0.0042(13) 0.0072(12) 0.0041(13) C15 0.049(2) 0.066(2) 0.050(2) 0.0152(17) 0.0057(16) 0.0221(18) C16 0.054(2) 0.095(3) 0.070(3) -0.004(2) -0.018(2) 0.030(2) C17 0.066(3) 0.061(3) 0.083(3) 0.010(2) -0.005(2) 0.019(2) C18 0.085(3) 0.120(4) 0.085(3) 0.062(3) 0.027(3) 0.055(3) C19 0.061(2) 0.048(2) 0.058(2) 0.0019(17) 0.0072(17) -0.0087(18) C20 0.087(4) 0.053(3) 0.180(6) 0.032(3) 0.002(4) 0.000(3) C21 0.119(4) 0.078(3) 0.096(4) 0.001(3) 0.042(3) -0.033(3) C22 0.141(5) 0.066(3) 0.093(4) 0.001(3) -0.022(3) -0.044(3) C23 0.0467(19) 0.047(2) 0.0475(19) -0.0124(15) 0.0062(15) 0.0075(16) C24 0.061(2) 0.047(2) 0.072(3) -0.0153(19) 0.0075(19) 0.0025(18) C25 0.067(3) 0.060(3) 0.083(3) 0.005(2) 0.008(2) 0.005(2) C26 0.082(3) 0.079(3) 0.079(3) 0.006(3) -0.004(2) 0.028(3) C27 0.124(5) 0.101(5) 0.118(5) 0.031(4) 0.009(4) -0.003(4) C28 0.114(6) 0.133(7) 0.202(10) 0.084(7) -0.004(6) 0.002(5) C29 0.118(6) 0.268(14) 0.088(5) 0.062(7) -0.004(4) 0.045(8) C30 0.127(5) 0.166(7) 0.072(4) -0.025(4) -0.019(4) 0.024(5) C31 0.094(4) 0.100(4) 0.082(4) -0.006(3) -0.014(3) 0.014(3) C32 0.077(4) 0.072(4) 0.070(4) 0.000 0.018(3) 0.000 Cl1 0.0886(9) 0.1339(13) 0.0974(10) 0.0096(9) -0.0177(7) 0.0078(9) _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 Se1 Se2 1.501(7) . ? Se1 C26 1.933(5) . ? Se1 C25 1.972(5) . ? Se2 C26 1.895(8) . ? Se2 C25 1.913(7) . ? Se2 C27 2.019(9) . ? O1 C13 1.362(4) . ? O2 C14 1.396(4) . ? O2 C23 1.439(4) . ? C1 C12 1.521(4) 2_556 ? C1 C2 1.524(4) . ? C2 C3 1.380(4) . ? C2 C13 1.407(4) . ? C3 C4 1.391(5) . ? C4 C5 1.392(5) . ? C4 C15 1.536(5) . ? C5 C6 1.389(4) . ? C6 C13 1.401(4) . ? C6 C7 1.521(4) . ? C7 C8 1.528(4) . ? C8 C14 1.391(4) . ? C8 C9 1.397(5) . ? C9 C10 1.384(5) . ? C10 C11 1.396(5) . ? C10 C19 1.542(5) . ? C11 C12 1.386(5) . ? C12 C14 1.398(4) . ? C12 C1 1.521(4) 2_556 ? C15 C16 1.532(6) . ? C15 C18 1.534(5) . ? C15 C17 1.542(6) . ? C19 C21 1.517(6) . ? C19 C20 1.523(6) . ? C19 C22 1.529(6) . ? C23 C24 1.510(5) . ? C24 C25 1.499(6) . ? C26 C31 1.341(7) . ? C26 C27 1.376(8) . ? C27 C28 1.382(12) . ? C28 C29 1.446(13) . ? C29 C30 1.352(12) . ? C30 C31 1.349(9) . ? C32 Cl1 1.717(4) 2_756 ? C32 Cl1 1.717(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 Se2 Se1 C26 65.6(3) . . ? Se2 Se1 C25 65.2(3) . . ? C26 Se1 C25 95.0(2) . . ? Se1 Se2 C26 68.3(3) . . ? Se1 Se2 C25 69.4(2) . . ? C26 Se2 C25 98.2(3) . . ? Se1 Se2 C27 108.4(4) . . ? C26 Se2 C27 41.0(3) . . ? C25 Se2 C27 121.1(3) . . ? C14 O2 C23 114.0(2) . . ? C12 C1 C2 110.8(2) 2_556 . ? C3 C2 C13 118.7(3) . . ? C3 C2 C1 121.0(3) . . ? C13 C2 C1 120.3(3) . . ? C2 C3 C4 122.7(3) . . ? C3 C4 C5 117.0(3) . . ? C3 C4 C15 119.5(3) . . ? C5 C4 C15 123.5(3) . . ? C6 C5 C4 123.0(3) . . ? C5 C6 C13 118.1(3) . . ? C5 C6 C7 120.0(3) . . ? C13 C6 C7 121.9(3) . . ? C6 C7 C8 113.9(2) . . ? C14 C8 C9 118.1(3) . . ? C14 C8 C7 121.0(3) . . ? C9 C8 C7 120.8(3) . . ? C10 C9 C8 122.6(3) . . ? C9 C10 C11 116.8(3) . . ? C9 C10 C19 121.5(3) . . ? C11 C10 C19 121.6(3) . . ? C12 C11 C10 123.1(3) . . ? C11 C12 C14 117.7(3) . . ? C11 C12 C1 119.9(3) . 2_556 ? C14 C12 C1 122.3(3) . 2_556 ? O1 C13 C6 123.6(3) . . ? O1 C13 C2 116.0(3) . . ? C6 C13 C2 120.4(3) . . ? C8 C14 O2 118.4(3) . . ? C8 C14 C12 121.4(3) . . ? O2 C14 C12 120.2(3) . . ? C16 C15 C18 108.6(4) . . ? C16 C15 C4 109.3(3) . . ? C18 C15 C4 111.9(3) . . ? C16 C15 C17 109.0(3) . . ? C18 C15 C17 108.8(4) . . ? C4 C15 C17 109.2(3) . . ? C21 C19 C20 109.4(4) . . ? C21 C19 C22 108.0(4) . . ? C20 C19 C22 107.8(4) . . ? C21 C19 C10 108.3(3) . . ? C20 C19 C10 110.7(3) . . ? C22 C19 C10 112.5(3) . . ? O2 C23 C24 107.7(3) . . ? C25 C24 C23 116.5(3) . . ? C24 C25 Se2 133.9(4) . . ? C24 C25 Se1 111.9(3) . . ? Se2 C25 Se1 45.4(3) . . ? C31 C26 C27 119.7(6) . . ? C31 C26 Se2 160.9(5) . . ? C27 C26 Se2 74.3(5) . . ? C31 C26 Se1 120.9(5) . . ? C27 C26 Se1 119.3(5) . . ? Se2 C26 Se1 46.1(2) . . ? C26 C27 C28 120.3(7) . . ? C26 C27 Se2 64.7(4) . . ? C28 C27 Se2 168.6(7) . . ? C27 C28 C29 117.7(8) . . ? C30 C29 C28 119.6(8) . . ? C31 C30 C29 119.8(8) . . ? C26 C31 C30 122.9(7) . . ? Cl1 C32 Cl1 114.0(4) 2_756 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.805 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.060