data_publication_text _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _publ_contact_author_name 'J. M. Shreeve' _publ_contact_author_address ; Department of Chemistry University of Idaho Moscow ID 83844-2343 UNITED STATES OF AMERICA ; _publ_contact_author_email JSHREEVE@UIDAHO.EDU loop_ _publ_author_name _publ_author_address 'Ruihu Wang.' ;Department of Chemistry, University of Idaho, Moscow, ID 83843-2343 ; 'Ji-Chang Xiao.' ;Department of Chemistry, University of Idaho, Moscow, ID 83843-2343 ; B.Twamley ;Department of Chemistry, University of Idaho, Moscow, ID 83843-2343 ; J.M.Shreeve ;Department of Chemistry, University of Idaho, Moscow, ID 83843-2343 ; _publ_section_title ;Pyridyl-functionalized Imidazolium-based Ionic liquids and Palladium(II) Complex Catalyzed Highly Recyclable and Efficient Heck Reactions ; data_bt789 _database_code_depnum_ccdc_archive 'CCDC 286255' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (R2PdCl2)(NTf)2 _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 Cl2 N6 Pd, 2(C2 F6 N O4 S2)' _chemical_formula_sum 'C30 H36 Cl2 F12 N8 O8 Pd S4' _chemical_formula_weight 1170.21 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 8.8615(12) _cell_length_b 24.322(3) _cell_length_c 11.2807(16) _cell_angle_alpha 90.00 _cell_angle_beta 111.633(2) _cell_angle_gamma 90.00 _cell_volume 2260.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 87(2) _cell_measurement_reflns_used 6939 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 30.01 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7302 _exptl_absorpt_correction_T_max 0.9759 _exptl_absorpt_process_details 'SADABS; Bruker, 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 87(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33709 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4080 _reflns_number_gt 3829 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART v. 5.626' _computing_cell_refinement 'Bruker SAINT+ v. 6.45a' _computing_data_reduction 'Bruker SAINT+ v. 6.45a' _computing_structure_solution 'XS, Bruker SHELXTL v. 6.12' _computing_structure_refinement 'XL, Bruker SHELXTL v. 6.12' _computing_molecular_graphics 'XP, Bruker SHELXTL v. 6.12' _computing_publication_material 'XCIF, Bruker SHELXTL v. 6.12' _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^)+(0.0316P)^2^+6.1609P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4080 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _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 Pd1 Pd 0.5000 0.0000 1.0000 0.01433(10) Uani 1 2 d S . . C2 C 0.8552(4) 0.00207(14) 1.1002(3) 0.0199(6) Uani 1 1 d . . . H2 H 0.8405 -0.0365 1.1030 0.024 Uiso 1 1 calc R . . C3 C 1.0114(4) 0.02319(15) 1.1423(3) 0.0228(7) Uani 1 1 d . . . H3 H 1.1021 -0.0007 1.1752 0.027 Uiso 1 1 calc R . . C4 C 1.0349(4) 0.07880(15) 1.1365(3) 0.0238(7) Uani 1 1 d . . . H4 H 1.1414 0.0937 1.1647 0.029 Uiso 1 1 calc R . . C5 C 0.8998(4) 0.11274(14) 1.0886(3) 0.0209(7) Uani 1 1 d . . . H5 H 0.9124 0.1513 1.0831 0.025 Uiso 1 1 calc R . . C6 C 0.7467(4) 0.08948(13) 1.0489(3) 0.0165(6) Uani 1 1 d . . . C7 C 0.6007(4) 0.12470(12) 1.0013(3) 0.0165(6) Uani 1 1 d . . . C9 C 0.4147(4) 0.18484(13) 1.0009(3) 0.0244(7) Uani 1 1 d . . . H9 H 0.3559 0.2111 1.0292 0.029 Uiso 1 1 calc R . . C10 C 0.3736(4) 0.16539(13) 0.8815(3) 0.0226(7) Uani 1 1 d . . . H10 H 0.2809 0.1756 0.8097 0.027 Uiso 1 1 calc R . . C12 C 0.4995(4) 0.10082(13) 0.7681(3) 0.0195(6) Uani 1 1 d . . . H12A H 0.5864 0.0727 0.7952 0.023 Uiso 1 1 calc R . . H12B H 0.5294 0.1285 0.7163 0.023 Uiso 1 1 calc R . . C13 C 0.3421(4) 0.07360(14) 0.6860(3) 0.0237(7) Uani 1 1 d . . . H13A H 0.2549 0.1015 0.6562 0.028 Uiso 1 1 calc R . . H13B H 0.3105 0.0460 0.7371 0.028 Uiso 1 1 calc R . . C14 C 0.3615(4) 0.04575(15) 0.5718(3) 0.0282(8) Uani 1 1 d . . . H14A H 0.4523 0.0191 0.6023 0.034 Uiso 1 1 calc R . . H14B H 0.3896 0.0738 0.5197 0.034 Uiso 1 1 calc R . . C15 C 0.2080(5) 0.01579(18) 0.4890(4) 0.0421(10) Uani 1 1 d . . . H15A H 0.1792 -0.0118 0.5403 0.063 Uiso 1 1 calc R . . H15B H 0.2268 -0.0023 0.4181 0.063 Uiso 1 1 calc R . . H15C H 0.1189 0.0423 0.4552 0.063 Uiso 1 1 calc R . . C16 C 0.6428(4) 0.16809(15) 1.2121(3) 0.0271(7) Uani 1 1 d . . . H16A H 0.6857 0.1329 1.2529 0.041 Uiso 1 1 calc R . . H16B H 0.5670 0.1831 1.2488 0.041 Uiso 1 1 calc R . . H16C H 0.7326 0.1940 1.2263 0.041 Uiso 1 1 calc R . . C17 C 0.2580(4) 0.21230(15) 0.4223(3) 0.0299(8) Uani 1 1 d . . . Cl1 Cl 0.44239(9) 0.04457(3) 1.15784(7) 0.01937(17) Uani 1 1 d . . . F1 F 0.1954(3) 0.16218(10) 0.4159(2) 0.0491(6) Uani 1 1 d . . . F2 F 0.4173(3) 0.20813(11) 0.4634(2) 0.0492(7) Uani 1 1 d . . . F3 F 0.2175(3) 0.24192(10) 0.50429(19) 0.0367(5) Uani 1 1 d . . . F4 F 0.2505(3) 0.30487(9) 0.0129(2) 0.0374(5) Uani 1 1 d . . . F5 F 0.2011(3) 0.38438(9) 0.0730(2) 0.0442(6) Uani 1 1 d . . . F6 F 0.4320(3) 0.36856(10) 0.0570(3) 0.0467(6) Uani 1 1 d . . . N1 N 0.7236(3) 0.03482(11) 1.0554(2) 0.0164(5) Uani 1 1 d . . . C19 C 0.3148(5) 0.34687(15) 0.0906(4) 0.0336(9) Uani 1 1 d . . . N8 N 0.5576(3) 0.15963(11) 1.0744(3) 0.0210(6) Uani 1 1 d . . . N11 N 0.4907(3) 0.12783(11) 0.8823(3) 0.0192(6) Uani 1 1 d . . . N18 N 0.2513(4) 0.30312(12) 0.2868(3) 0.0276(6) Uani 1 1 d . . . O1 O 0.2341(3) 0.20779(10) 0.1865(2) 0.0282(5) Uani 1 1 d . . . O2 O 0.0078(3) 0.24652(10) 0.2356(2) 0.0277(5) Uani 1 1 d . . . O3 O 0.4573(3) 0.37458(11) 0.3251(3) 0.0423(7) Uani 1 1 d . . . O4 O 0.5185(3) 0.28364(10) 0.2577(3) 0.0342(6) Uani 1 1 d . . . S1 S 0.17824(9) 0.24311(3) 0.26277(8) 0.02005(18) Uani 1 1 d . . . S2 S 0.40252(10) 0.32434(4) 0.25791(9) 0.0282(2) 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 Pd1 0.00913(16) 0.01564(17) 0.01920(18) -0.00033(13) 0.00637(12) 0.00089(12) C2 0.0170(15) 0.0251(16) 0.0190(15) -0.0005(13) 0.0083(12) 0.0042(13) C3 0.0115(14) 0.0361(19) 0.0200(16) -0.0019(14) 0.0050(13) 0.0055(13) C4 0.0107(14) 0.037(2) 0.0231(17) -0.0072(14) 0.0052(13) -0.0010(13) C5 0.0156(15) 0.0250(17) 0.0214(16) -0.0066(13) 0.0059(13) -0.0047(13) C6 0.0138(14) 0.0220(16) 0.0135(14) -0.0024(12) 0.0050(12) -0.0005(12) C7 0.0128(14) 0.0159(15) 0.0211(16) -0.0021(12) 0.0064(12) -0.0033(11) C9 0.0225(17) 0.0170(16) 0.039(2) 0.0028(14) 0.0170(15) 0.0049(13) C10 0.0145(15) 0.0222(17) 0.0326(18) 0.0064(14) 0.0104(14) 0.0058(13) C12 0.0184(15) 0.0215(16) 0.0200(16) 0.0001(13) 0.0086(13) -0.0010(12) C13 0.0153(15) 0.0276(18) 0.0248(17) 0.0027(14) 0.0033(13) -0.0005(13) C14 0.0249(18) 0.0331(19) 0.0217(17) 0.0025(15) 0.0029(14) 0.0012(15) C15 0.038(2) 0.044(2) 0.032(2) -0.0082(18) -0.0019(18) -0.0048(18) C16 0.0289(18) 0.0270(18) 0.0277(18) -0.0069(14) 0.0132(15) -0.0014(14) C17 0.0287(19) 0.033(2) 0.0242(18) 0.0015(15) 0.0055(15) 0.0096(16) Cl1 0.0164(4) 0.0212(4) 0.0226(4) -0.0026(3) 0.0096(3) 0.0006(3) F1 0.0714(18) 0.0351(13) 0.0388(13) 0.0119(10) 0.0181(13) 0.0061(12) F2 0.0258(12) 0.0790(18) 0.0328(12) -0.0007(12) -0.0008(10) 0.0286(12) F3 0.0308(11) 0.0568(14) 0.0189(10) -0.0040(9) 0.0049(9) 0.0131(10) F4 0.0345(12) 0.0378(12) 0.0381(12) -0.0007(10) 0.0111(10) -0.0012(10) F5 0.0444(14) 0.0335(12) 0.0663(16) 0.0137(11) 0.0341(13) 0.0125(10) F6 0.0376(13) 0.0515(15) 0.0631(16) 0.0009(12) 0.0327(12) -0.0105(11) N1 0.0128(12) 0.0213(14) 0.0155(12) -0.0017(10) 0.0055(10) 0.0006(10) C19 0.0299(19) 0.0262(19) 0.052(2) -0.0033(17) 0.0233(18) -0.0028(15) N8 0.0184(13) 0.0195(14) 0.0269(15) -0.0030(11) 0.0104(12) -0.0004(11) N11 0.0128(12) 0.0208(14) 0.0245(14) 0.0008(11) 0.0075(11) -0.0002(10) N18 0.0254(15) 0.0224(15) 0.0398(17) -0.0039(13) 0.0178(13) 0.0017(12) O1 0.0310(13) 0.0277(13) 0.0277(13) -0.0080(10) 0.0129(11) -0.0062(10) O2 0.0144(11) 0.0418(15) 0.0233(12) 0.0030(10) 0.0029(10) -0.0006(10) O3 0.0422(16) 0.0326(15) 0.0559(18) -0.0168(13) 0.0227(14) -0.0123(12) O4 0.0178(12) 0.0327(14) 0.0512(17) -0.0072(12) 0.0115(12) 0.0006(10) S1 0.0147(4) 0.0232(4) 0.0201(4) -0.0022(3) 0.0039(3) -0.0002(3) S2 0.0205(4) 0.0252(4) 0.0408(5) -0.0098(4) 0.0136(4) -0.0042(3) _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 Pd1 N1 2.030(2) 3_657 ? Pd1 N1 2.030(2) . ? Pd1 Cl1 2.2970(8) . ? Pd1 Cl1 2.2970(8) 3_657 ? C2 N1 1.348(4) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 C4 1.374(5) . ? C3 H3 0.9500 . ? C4 C5 1.389(5) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 N1 1.351(4) . ? C6 C7 1.477(4) . ? C7 N8 1.334(4) . ? C7 N11 1.339(4) . ? C9 C10 1.345(5) . ? C9 N8 1.376(4) . ? C9 H9 0.9500 . ? C10 N11 1.380(4) . ? C10 H10 0.9500 . ? C12 N11 1.473(4) . ? C12 C13 1.513(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.520(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.523(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N8 1.469(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 F2 1.318(4) . ? C17 F3 1.322(4) . ? C17 F1 1.330(5) . ? C17 S1 1.834(4) . ? F4 C19 1.330(4) . ? F5 C19 1.319(4) . ? F6 C19 1.338(4) . ? C19 S2 1.840(4) . ? N18 S2 1.578(3) . ? N18 S1 1.579(3) . ? O1 S1 1.427(2) . ? O2 S1 1.428(2) . ? O3 S2 1.425(3) . ? O4 S2 1.428(3) . ? 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 Pd1 N1 180.0 3_657 . ? N1 Pd1 Cl1 88.00(7) 3_657 . ? N1 Pd1 Cl1 92.00(7) . . ? N1 Pd1 Cl1 92.00(7) 3_657 3_657 ? N1 Pd1 Cl1 88.00(7) . 3_657 ? Cl1 Pd1 Cl1 180.0 . 3_657 ? N1 C2 C3 121.8(3) . . ? N1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 118.7(3) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 119.0(3) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? N1 C6 C5 122.3(3) . . ? N1 C6 C7 117.4(3) . . ? C5 C6 C7 120.2(3) . . ? N8 C7 N11 108.4(3) . . ? N8 C7 C6 123.8(3) . . ? N11 C7 C6 127.9(3) . . ? C10 C9 N8 107.2(3) . . ? C10 C9 H9 126.4 . . ? N8 C9 H9 126.4 . . ? C9 C10 N11 107.5(3) . . ? C9 C10 H10 126.2 . . ? N11 C10 H10 126.2 . . ? N11 C12 C13 113.3(3) . . ? N11 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N11 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 110.3(3) . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 112.2(3) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N8 C16 H16A 109.5 . . ? N8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F2 C17 F3 109.1(3) . . ? F2 C17 F1 108.6(3) . . ? F3 C17 F1 108.8(3) . . ? F2 C17 S1 110.6(3) . . ? F3 C17 S1 111.0(2) . . ? F1 C17 S1 108.6(2) . . ? C2 N1 C6 118.3(3) . . ? C2 N1 Pd1 118.7(2) . . ? C6 N1 Pd1 123.0(2) . . ? F5 C19 F4 108.3(3) . . ? F5 C19 F6 108.3(3) . . ? F4 C19 F6 107.8(3) . . ? F5 C19 S2 111.8(3) . . ? F4 C19 S2 111.3(3) . . ? F6 C19 S2 109.2(3) . . ? C7 N8 C9 108.7(3) . . ? C7 N8 C16 126.2(3) . . ? C9 N8 C16 125.1(3) . . ? C7 N11 C10 108.2(3) . . ? C7 N11 C12 126.7(3) . . ? C10 N11 C12 124.9(3) . . ? S2 N18 S1 126.36(18) . . ? O1 S1 O2 118.68(15) . . ? O1 S1 N18 116.62(15) . . ? O2 S1 N18 108.51(15) . . ? O1 S1 C17 104.58(16) . . ? O2 S1 C17 103.23(16) . . ? N18 S1 C17 102.96(17) . . ? O3 S2 O4 119.40(17) . . ? O3 S2 N18 108.66(16) . . ? O4 S2 N18 116.12(16) . . ? O3 S2 C19 102.84(18) . . ? O4 S2 C19 103.68(17) . . ? N18 S2 C19 103.85(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C9 H9 O1 0.95 2.39 3.118(4) 132.8 1_556 C10 H10 O4 0.95 2.39 3.186(4) 140.8 4_566 C12 H12B N18 0.99 2.47 3.184(4) 128.5 4_666 C16 H16B O4 0.98 2.49 3.130(4) 122.5 1_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.178 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.083