# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 #TrackingRef '5232_web_deposit_cif_file_0_JohnBeck_1304367608.cif' #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name ' Joseph A. R. Schmidt ' _publ_contact_author_address ; 2801 W. Bancroft St. MS 602 Department of Chemistry The University of Toledo Toledo, OH 43606-3390 ; _publ_contact_author_email ' Joseph.Schmidt@utoledo.edu ' _publ_contact_author_fax ' (419) 530-4033 ' #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Hydroamination of 1,1-dimethylallene with primary aryl amines under mild conditions: An atom-economical route to N-(1,1-dimethyl-2-propenyl)-anilines ; loop_ _publ_author_name _publ_author_address J.F.Beck ; 2801 W. Bancroft St. MS 602 Department of Chemistry The University of Toledo Toledo, OH 43606-3390 ; J.A.R.Schmidt ; 2801 W. Bancroft St. MS 602 Department of Chemistry The University of Toledo Toledo, OH 43606-3390 ; #------------------------------------------------------------------------------ # TEXT _publ_section_references ; SMART: Area-Detector Software Package,v5.625; Bruker AXS, Inc.: Madison, WI, (1997-2001) SAINT: SAX Area-Detector Integration Program, V6.22; Bruker AXS, Inc.: Madison, WI, (1997-2001) XPREP: Reciprocal Space Exploration Program, v6.12; Bruker AXS, Inc.: Madison, WI, (2001) SADABS: Bruker/Siemens Area Detector Absorption Program, v2.03; Bruker AXS, Inc.: Madison, WI, (2001) SHELXL-97: Structure Solution Program, v6.10; Bruker AXS, Inc.: Madison, WI, (2000) ; data_[(3IPtbu)Pd(allyl)]OTf _database_code_depnum_ccdc_archive 'CCDC 823823' #TrackingRef '5232_web_deposit_cif_file_0_JohnBeck_1304367608.cif' #------------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H39 F3 N O3 P Pd S' _chemical_formula_weight 591.97 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' P P 0.1023 0.0942 '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' 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)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.227(2) _cell_length_b 8.4499(17) _cell_length_c 27.587(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.82(3) _cell_angle_gamma 90.00 _cell_volume 2615.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.210 _cell_measurement_theta_max 26.253 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.206 _exptl_crystal_size_mid 0.134 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.940324 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30828 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5334 _reflns_number_gt 4490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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^)+(0.0340P)^2^+3.1107P] 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 5334 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Pd1 Pd 0.115459(18) 0.41408(2) 0.129750(8) 0.01823(8) Uani 1 1 d . . . P1 P 0.30298(6) 0.52142(8) 0.11580(2) 0.01670(15) Uani 1 1 d . . . S1 S -0.21188(8) -0.09939(10) 0.12436(3) 0.0358(2) Uani 1 1 d . . . N1 N 0.16825(19) 0.3375(3) 0.20096(8) 0.0156(5) Uani 1 1 d . . . C1 C 0.2374(2) 0.4170(3) 0.22916(10) 0.0168(5) Uani 1 1 d . . . H1A H 0.2484 0.3787 0.2606 0.020 Uiso 1 1 calc R . . C16 C 0.2210(3) 0.0944(3) 0.24976(11) 0.0255(7) Uani 1 1 d . . . H16A H 0.2886 0.0745 0.2302 0.038 Uiso 1 1 calc R . . H16B H 0.1903 -0.0043 0.2613 0.038 Uiso 1 1 calc R . . H16C H 0.2449 0.1594 0.2769 0.038 Uiso 1 1 calc R . . C2 C 0.3016(2) 0.5624(3) 0.21734(10) 0.0156(5) Uani 1 1 d . . . C11 C 0.4331(3) 0.3810(3) 0.10854(10) 0.0214(6) Uani 1 1 d . . . C6 C 0.3489(2) 0.6617(3) 0.25956(10) 0.0190(6) Uani 1 1 d . . . H6A H 0.3811 0.5954 0.2855 0.023 Uiso 1 1 calc R . . H6B H 0.2869 0.7287 0.2722 0.023 Uiso 1 1 calc R . . C3 C 0.3381(2) 0.6172(3) 0.17451(10) 0.0171(6) Uani 1 1 d . . . C10 C 0.4254(3) 0.7665(4) 0.06214(11) 0.0283(7) Uani 1 1 d . . . H10A H 0.4166 0.8479 0.0380 0.042 Uiso 1 1 calc R . . H10B H 0.4822 0.6896 0.0518 0.042 Uiso 1 1 calc R . . H10C H 0.4528 0.8125 0.0923 0.042 Uiso 1 1 calc R . . C9 C 0.2618(3) 0.6229(4) 0.01899(11) 0.0310(7) Uani 1 1 d . . . H9A H 0.2631 0.7073 -0.0043 0.047 Uiso 1 1 calc R . . H9B H 0.1821 0.5829 0.0210 0.047 Uiso 1 1 calc R . . H9C H 0.3138 0.5395 0.0091 0.047 Uiso 1 1 calc R . . C15 C 0.1244(2) 0.1794(3) 0.21941(10) 0.0191(6) Uani 1 1 d . . . C17 C 0.0158(3) 0.2092(4) 0.25004(11) 0.0260(7) Uani 1 1 d . . . H17A H -0.0449 0.2615 0.2307 0.039 Uiso 1 1 calc R . . H17B H 0.0383 0.2749 0.2772 0.039 Uiso 1 1 calc R . . H17C H -0.0142 0.1101 0.2615 0.039 Uiso 1 1 calc R . . C5 C 0.4468(3) 0.7605(3) 0.23694(10) 0.0228(6) Uani 1 1 d . . . H5A H 0.4475 0.8670 0.2500 0.027 Uiso 1 1 calc R . . H5B H 0.5243 0.7128 0.2432 0.027 Uiso 1 1 calc R . . C18 C 0.0916(3) 0.0778(3) 0.17558(11) 0.0274(7) Uani 1 1 d . . . H18A H 0.1612 0.0596 0.1570 0.041 Uiso 1 1 calc R . . H18B H 0.0323 0.1312 0.1558 0.041 Uiso 1 1 calc R . . H18C H 0.0604 -0.0217 0.1862 0.041 Uiso 1 1 calc R . . C4 C 0.4162(3) 0.7626(3) 0.18267(10) 0.0222(6) Uani 1 1 d . . . H4A H 0.3734 0.8584 0.1736 0.027 Uiso 1 1 calc R . . H4B H 0.4878 0.7558 0.1640 0.027 Uiso 1 1 calc R . . C7 C 0.3044(3) 0.6856(3) 0.06903(10) 0.0230(6) Uani 1 1 d . . . C8 C 0.2143(3) 0.8093(4) 0.08574(12) 0.0318(7) Uani 1 1 d . . . H8A H 0.2117 0.8961 0.0633 0.048 Uiso 1 1 calc R . . H8B H 0.2381 0.8473 0.1174 0.048 Uiso 1 1 calc R . . H8C H 0.1367 0.7619 0.0870 0.048 Uiso 1 1 calc R . . C12 C 0.4390(3) 0.3269(4) 0.05582(11) 0.0339(8) Uani 1 1 d . . . H12A H 0.5055 0.2568 0.0525 0.051 Uiso 1 1 calc R . . H12B H 0.4485 0.4174 0.0353 0.051 Uiso 1 1 calc R . . H12C H 0.3667 0.2726 0.0466 0.051 Uiso 1 1 calc R . . C13 C 0.5537(3) 0.4506(4) 0.12575(12) 0.0300(7) Uani 1 1 d . . . H13A H 0.6155 0.3741 0.1210 0.045 Uiso 1 1 calc R . . H13B H 0.5510 0.4767 0.1596 0.045 Uiso 1 1 calc R . . H13C H 0.5700 0.5443 0.1074 0.045 Uiso 1 1 calc R . . O1 O -0.2024(2) 0.0657(3) 0.13348(11) 0.0556(8) Uani 1 1 d . . . O2 O -0.1010(2) -0.1876(3) 0.13145(11) 0.0548(7) Uani 1 1 d . . . F1 F -0.3335(2) -0.0372(3) 0.04384(10) 0.0756(8) Uani 1 1 d . . . C22 C -0.0848(3) 0.4069(4) 0.13657(12) 0.0296(7) Uani 1 1 d . . . H22A H -0.1162 0.3261 0.1576 0.036 Uiso 1 1 calc R . . H22B H -0.1253 0.5079 0.1387 0.036 Uiso 1 1 calc R . . F2 F -0.2485(3) -0.2612(3) 0.04523(9) 0.0731(8) Uani 1 1 d . . . C14 C 0.4085(3) 0.2344(3) 0.13942(11) 0.0239(6) Uani 1 1 d . . . H14A H 0.4730 0.1605 0.1368 0.036 Uiso 1 1 calc R . . H14B H 0.3356 0.1856 0.1281 0.036 Uiso 1 1 calc R . . H14C H 0.4017 0.2652 0.1727 0.036 Uiso 1 1 calc R . . F3 F -0.1452(2) -0.0486(4) 0.03640(9) 0.0809(9) Uani 1 1 d . . . O3 O -0.3140(2) -0.1753(4) 0.14334(10) 0.0603(8) Uani 1 1 d . . . C20 C 0.0202(3) 0.4595(4) 0.06410(12) 0.0349(8) Uani 1 1 d . . . H20A H -0.0083 0.5670 0.0594 0.042 Uiso 1 1 calc R . . H20B H 0.0529 0.4140 0.0351 0.042 Uiso 1 1 calc R . . C21 C -0.0523(3) 0.3594(4) 0.09122(12) 0.0367(8) Uani 1 1 d . . . H21A H -0.0690 0.2512 0.0801 0.044 Uiso 1 1 calc R . . C23 C -0.2347(4) -0.1131(5) 0.05929(14) 0.0460(9) 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 0.01781(12) 0.02152(12) 0.01513(12) 0.00034(9) -0.00301(8) -0.00425(8) P1 0.0189(3) 0.0192(3) 0.0119(3) -0.0007(3) 0.0000(3) -0.0035(3) S1 0.0425(5) 0.0410(5) 0.0239(4) -0.0016(3) 0.0011(4) -0.0227(4) N1 0.0156(11) 0.0161(11) 0.0151(12) 0.0000(9) 0.0019(9) -0.0001(9) C1 0.0198(13) 0.0184(13) 0.0123(13) 0.0021(11) 0.0020(11) 0.0020(11) C16 0.0259(15) 0.0166(13) 0.0340(18) 0.0045(12) 0.0008(13) -0.0009(12) C2 0.0148(12) 0.0171(13) 0.0148(14) -0.0015(10) -0.0010(10) 0.0012(10) C11 0.0220(14) 0.0242(14) 0.0182(15) -0.0027(11) 0.0039(12) -0.0006(11) C6 0.0213(14) 0.0202(13) 0.0154(14) -0.0019(11) -0.0011(11) -0.0037(11) C3 0.0167(13) 0.0176(13) 0.0169(14) -0.0023(11) -0.0004(11) -0.0014(10) C10 0.0331(17) 0.0300(16) 0.0220(16) 0.0040(13) 0.0033(13) -0.0085(13) C9 0.0377(18) 0.0388(18) 0.0166(16) 0.0057(13) -0.0008(13) -0.0071(14) C15 0.0185(13) 0.0158(13) 0.0231(15) 0.0007(11) 0.0028(11) -0.0027(11) C17 0.0214(15) 0.0260(15) 0.0310(17) 0.0039(13) 0.0076(13) -0.0022(12) C5 0.0231(15) 0.0226(14) 0.0225(16) -0.0029(12) -0.0021(12) -0.0048(12) C18 0.0332(17) 0.0180(14) 0.0309(17) -0.0041(12) 0.0013(14) -0.0073(12) C4 0.0262(15) 0.0219(14) 0.0186(15) -0.0023(12) 0.0018(12) -0.0069(12) C7 0.0301(16) 0.0242(14) 0.0147(14) 0.0043(12) 0.0007(12) -0.0027(12) C8 0.0375(18) 0.0296(16) 0.0284(18) 0.0077(14) 0.0008(14) 0.0063(14) C12 0.046(2) 0.0333(17) 0.0224(17) -0.0056(14) 0.0077(15) 0.0081(15) C13 0.0210(15) 0.0332(17) 0.0360(19) -0.0009(14) 0.0051(13) -0.0024(13) O1 0.0486(16) 0.0448(15) 0.074(2) -0.0259(14) 0.0161(15) -0.0128(13) O2 0.0484(16) 0.0456(15) 0.069(2) 0.0083(14) -0.0262(14) -0.0056(13) F1 0.0671(17) 0.0846(19) 0.0733(19) 0.0358(15) -0.0286(14) -0.0062(15) C22 0.0172(14) 0.0385(18) 0.0328(18) 0.0041(14) -0.0062(13) 0.0006(13) F2 0.092(2) 0.0724(17) 0.0535(16) -0.0305(14) -0.0192(14) -0.0023(15) C14 0.0230(15) 0.0253(15) 0.0236(16) 0.0004(12) 0.0035(12) 0.0024(12) F3 0.0710(18) 0.132(3) 0.0407(14) 0.0150(15) 0.0199(13) -0.0215(17) O3 0.0542(17) 0.087(2) 0.0403(16) 0.0047(15) 0.0059(13) -0.0427(16) C20 0.0298(17) 0.051(2) 0.0235(17) 0.0070(15) -0.0111(14) -0.0096(15) C21 0.0269(17) 0.047(2) 0.035(2) 0.0040(16) -0.0132(15) -0.0079(15) C23 0.047(2) 0.058(2) 0.033(2) 0.0032(18) -0.0029(18) -0.0089(19) _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 C20 2.109(3) . ? Pd1 N1 2.134(2) . ? Pd1 C21 2.182(3) . ? Pd1 C22 2.262(3) . ? Pd1 P1 2.3356(8) . ? P1 C3 1.842(3) . ? P1 C7 1.895(3) . ? P1 C11 1.898(3) . ? S1 O1 1.421(3) . ? S1 O3 1.428(3) . ? S1 O2 1.458(3) . ? S1 C23 1.809(4) . ? N1 C1 1.273(3) . ? N1 C15 1.517(3) . ? C1 C2 1.467(4) . ? C16 C15 1.529(4) . ? C2 C3 1.345(4) . ? C2 C6 1.517(4) . ? C11 C12 1.528(4) . ? C11 C14 1.534(4) . ? C11 C13 1.537(4) . ? C6 C5 1.529(4) . ? C3 C4 1.522(4) . ? C10 C7 1.538(4) . ? C9 C7 1.540(4) . ? C15 C18 1.519(4) . ? C15 C17 1.526(4) . ? C5 C4 1.526(4) . ? C7 C8 1.536(4) . ? F1 C23 1.339(5) . ? C22 C21 1.374(5) . ? F2 C23 1.318(5) . ? F3 C23 1.322(4) . ? C20 C21 1.406(5) . ? 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 C20 Pd1 N1 164.57(10) . . ? C20 Pd1 C21 38.19(12) . . ? N1 Pd1 C21 126.45(11) . . ? C20 Pd1 C22 66.30(13) . . ? N1 Pd1 C22 99.38(10) . . ? C21 Pd1 C22 35.96(12) . . ? C20 Pd1 P1 102.89(9) . . ? N1 Pd1 P1 92.52(6) . . ? C21 Pd1 P1 140.39(9) . . ? C22 Pd1 P1 158.02(8) . . ? C3 P1 C7 105.72(13) . . ? C3 P1 C11 102.91(13) . . ? C7 P1 C11 111.27(13) . . ? C3 P1 Pd1 101.23(9) . . ? C7 P1 Pd1 115.06(10) . . ? C11 P1 Pd1 118.40(9) . . ? O1 S1 O3 115.63(18) . . ? O1 S1 O2 114.78(16) . . ? O3 S1 O2 114.40(18) . . ? O1 S1 C23 104.26(19) . . ? O3 S1 C23 104.18(17) . . ? O2 S1 C23 101.17(18) . . ? C1 N1 C15 117.2(2) . . ? C1 N1 Pd1 123.27(18) . . ? C15 N1 Pd1 119.48(16) . . ? N1 C1 C2 126.9(2) . . ? C3 C2 C1 130.5(2) . . ? C3 C2 C6 112.0(2) . . ? C1 C2 C6 117.1(2) . . ? C12 C11 C14 107.5(2) . . ? C12 C11 C13 110.1(2) . . ? C14 C11 C13 108.0(2) . . ? C12 C11 P1 110.1(2) . . ? C14 C11 P1 107.09(18) . . ? C13 C11 P1 113.7(2) . . ? C2 C6 C5 103.1(2) . . ? C2 C3 C4 109.8(2) . . ? C2 C3 P1 124.0(2) . . ? C4 C3 P1 126.2(2) . . ? N1 C15 C18 107.7(2) . . ? N1 C15 C17 108.3(2) . . ? C18 C15 C17 110.9(2) . . ? N1 C15 C16 111.4(2) . . ? C18 C15 C16 108.7(2) . . ? C17 C15 C16 109.9(2) . . ? C4 C5 C6 105.4(2) . . ? C3 C4 C5 104.3(2) . . ? C8 C7 C10 109.1(2) . . ? C8 C7 C9 108.3(3) . . ? C10 C7 C9 107.0(2) . . ? C8 C7 P1 105.92(19) . . ? C10 C7 P1 115.9(2) . . ? C9 C7 P1 110.4(2) . . ? C21 C22 Pd1 68.84(18) . . ? C21 C20 Pd1 73.72(19) . . ? C22 C21 C20 118.9(3) . . ? C22 C21 Pd1 75.19(19) . . ? C20 C21 Pd1 68.09(18) . . ? F2 C23 F3 109.6(4) . . ? F2 C23 F1 105.8(3) . . ? F3 C23 F1 106.6(3) . . ? F2 C23 S1 111.4(3) . . ? F3 C23 S1 111.2(3) . . ? F1 C23 S1 112.0(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.669 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.083