data_x1209016 _audit_creation_date 2012-09-25 _audit_creation_method ; Olex2 1.2-beta (compiled Aug 15 2012 15:59:22, GUI svn.r4314) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H19 O4 P' _chemical_formula_sum 'C12 H19 O4 P' _chemical_formula_weight 258.24 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z' _cell_length_a 10.6837(3) _cell_length_b 5.7318(2) _cell_length_c 11.1098(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.432(3) _cell_angle_gamma 90.00 _cell_volume 652.54(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2870 _cell_measurement_temperature 100 _cell_measurement_theta_max 66.73 _cell_measurement_theta_min 4.15 _exptl_absorpt_coefficient_mu 1.896 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.5879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; ? was used for absorption correction. wR2(int) was 0.1082 before and 0.0617 after correction. The Ratio of minimum to maximum transmission is 0.7810. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 276 _exptl_crystal_size_max 0.322 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.035 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_unetI/netI 0.0680 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4356 _diffrn_reflns_theta_full 66.79 _diffrn_reflns_theta_max 66.79 _diffrn_reflns_theta_min 4.15 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_number_gt 1990 _reflns_number_total 2176 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 0.430 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.065 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 159 _refine_ls_number_reflns 2176 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0474 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1135 _refine_ls_wR_factor_ref 0.1174 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap 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 P1 P -0.04196(7) 0.33714(15) 0.20594(7) 0.0204(2) Uani 1 1 d . . . O1 O 0.0725(2) 0.7390(4) 0.2899(2) 0.0258(6) Uani 1 1 d . . . H1 H 0.0432 0.8508 0.2413 0.039 Uiso 1 1 calc R . . O2 O -0.0230(2) 0.1166(4) 0.1448(2) 0.0245(6) Uani 1 1 d . . . O3 O -0.0596(2) 0.2916(4) 0.3385(2) 0.0272(6) Uani 1 1 d . . . O4 O -0.1708(2) 0.4753(4) 0.1384(2) 0.0235(6) Uani 1 1 d . . . C1 C 0.6522(4) 1.0167(8) 0.2071(4) 0.0375(9) Uani 1 1 d . . . H1A H 0.6566 1.1635 0.2534 0.056 Uiso 1 1 calc R . . H1B H 0.6383 1.0503 0.1178 0.056 Uiso 1 1 calc R . . H1C H 0.7342 0.9309 0.2395 0.056 Uiso 1 1 calc R . . C2 C 0.5404(3) 0.8709(7) 0.2236(3) 0.0294(9) Uani 1 1 d . . . C3 C 0.4700(3) 0.9365(7) 0.3041(3) 0.0294(8) Uani 1 1 d . . . H3 H 0.4908 1.0795 0.3485 0.035 Uiso 1 1 calc R . . C4 C 0.3697(3) 0.8008(7) 0.3229(3) 0.0275(8) Uani 1 1 d . . . H4 H 0.3237 0.8514 0.3799 0.033 Uiso 1 1 calc R . . C5 C 0.3356(3) 0.5905(7) 0.2585(3) 0.0241(8) Uani 1 1 d . . . C6 C 0.4067(3) 0.5249(7) 0.1768(3) 0.0299(8) Uani 1 1 d . . . H6 H 0.3858 0.3829 0.1314 0.036 Uiso 1 1 calc R . . C7 C 0.5070(4) 0.6614(8) 0.1600(4) 0.0332(9) Uani 1 1 d . . . H7 H 0.5540 0.6109 0.1039 0.040 Uiso 1 1 calc R . . C8 C 0.2290(3) 0.4325(7) 0.2785(3) 0.0245(7) Uani 1 1 d . . . H8 H 0.2324 0.2833 0.2329 0.029 Uiso 1 1 calc R . . C9 C 0.2502(3) 0.3721(7) 0.4171(3) 0.0292(9) Uani 1 1 d . . . H9A H 0.2396 0.5130 0.4632 0.044 Uiso 1 1 calc R . . H9B H 0.3384 0.3097 0.4521 0.044 Uiso 1 1 calc R . . H9C H 0.1861 0.2549 0.4246 0.044 Uiso 1 1 calc R . . C10 C 0.0932(3) 0.5439(6) 0.2192(3) 0.0218(7) Uani 1 1 d . . . H10 H 0.0898 0.5990 0.1330 0.026 Uiso 1 1 calc R . . C11 C -0.1177(4) 0.4585(7) 0.4068(3) 0.0291(8) Uani 1 1 d . . . H11A H -0.2102 0.4795 0.3622 0.044 Uiso 1 1 calc R . . H11B H -0.0724 0.6086 0.4125 0.044 Uiso 1 1 calc R . . H11C H -0.1092 0.3992 0.4915 0.044 Uiso 1 1 calc R . . C12 C -0.1953(4) 0.5466(8) 0.0093(3) 0.0326(9) Uani 1 1 d . . . H12A H -0.2844 0.5027 -0.0377 0.049 Uiso 1 1 calc R . . H12B H -0.1330 0.4693 -0.0275 0.049 Uiso 1 1 calc R . . H12C H -0.1852 0.7161 0.0054 0.049 Uiso 1 1 calc R . . 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 P1 0.0195(4) 0.0168(4) 0.0251(4) 0.0005(4) 0.0065(3) -0.0004(4) O1 0.0293(13) 0.0163(13) 0.0310(13) -0.0012(10) 0.0073(10) 0.0019(10) O2 0.0245(12) 0.0212(14) 0.0284(13) -0.0004(10) 0.0085(10) -0.0006(10) O3 0.0260(12) 0.0229(17) 0.0314(13) 0.0015(10) 0.0059(9) -0.0013(10) O4 0.0241(11) 0.0220(15) 0.0252(12) 0.0017(10) 0.0080(9) 0.0001(10) C1 0.0296(18) 0.030(2) 0.052(2) 0.0001(18) 0.0099(17) -0.0085(17) C2 0.0234(16) 0.029(3) 0.0338(18) 0.0010(17) 0.0055(14) -0.0014(16) C3 0.0282(17) 0.0190(19) 0.037(2) -0.0034(16) 0.0020(14) -0.0031(15) C4 0.0255(16) 0.027(2) 0.0291(17) 0.0000(16) 0.0058(13) 0.0025(15) C5 0.0217(16) 0.025(2) 0.0236(16) 0.0025(14) 0.0036(13) 0.0015(14) C6 0.0287(18) 0.024(2) 0.035(2) -0.0060(16) 0.0057(15) -0.0042(16) C7 0.0299(19) 0.036(2) 0.036(2) -0.0045(18) 0.0138(15) -0.0043(16) C8 0.0266(17) 0.0184(18) 0.0276(17) -0.0023(15) 0.0064(13) -0.0002(14) C9 0.0247(16) 0.029(2) 0.0337(18) 0.0051(16) 0.0083(13) 0.0001(14) C10 0.0246(17) 0.0172(18) 0.0246(16) 0.0002(14) 0.0086(13) -0.0039(14) C11 0.0355(19) 0.030(2) 0.0266(17) -0.0053(16) 0.0159(15) -0.0028(16) C12 0.0318(19) 0.038(3) 0.0271(18) 0.0058(17) 0.0063(15) 0.0077(17) _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 P1 O2 1.476(3) . ? P1 O3 1.559(2) . ? P1 O4 1.582(2) . ? P1 C10 1.841(3) . ? O1 H1 0.8400 . ? O1 C10 1.419(4) . ? O3 C11 1.464(4) . ? O4 C12 1.442(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C2 1.511(5) . ? C2 C3 1.373(5) . ? C2 C7 1.388(6) . ? C3 H3 0.9500 . ? C3 C4 1.387(5) . ? C4 H4 0.9500 . ? C4 C5 1.396(5) . ? C5 C6 1.391(5) . ? C5 C8 1.519(5) . ? C6 H6 0.9500 . ? C6 C7 1.381(5) . ? C7 H7 0.9500 . ? C8 H8 1.0000 . ? C8 C9 1.530(5) . ? C8 C10 1.552(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 P1 O3 111.10(14) . . ? O2 P1 O4 115.15(13) . . ? O2 P1 C10 112.46(15) . . ? O3 P1 O4 102.14(12) . . ? O3 P1 C10 109.50(14) . . ? O4 P1 C10 105.87(15) . . ? C10 O1 H1 109.5 . . ? C11 O3 P1 124.2(2) . . ? C12 O4 P1 120.1(2) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? C3 C2 C1 121.6(4) . . ? C3 C2 C7 117.3(3) . . ? C7 C2 C1 121.0(3) . . ? C2 C3 H3 118.9 . . ? C2 C3 C4 122.2(4) . . ? C4 C3 H3 118.9 . . ? C3 C4 H4 119.8 . . ? C3 C4 C5 120.5(3) . . ? C5 C4 H4 119.8 . . ? C4 C5 C8 122.5(3) . . ? C6 C5 C4 117.2(3) . . ? C6 C5 C8 120.3(3) . . ? C5 C6 H6 119.2 . . ? C7 C6 C5 121.5(4) . . ? C7 C6 H6 119.2 . . ? C2 C7 H7 119.4 . . ? C6 C7 C2 121.3(3) . . ? C6 C7 H7 119.4 . . ? C5 C8 H8 107.4 . . ? C5 C8 C9 112.2(3) . . ? C5 C8 C10 110.0(3) . . ? C9 C8 H8 107.4 . . ? C9 C8 C10 112.0(3) . . ? C10 C8 H8 107.4 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P1 C10 H10 108.2 . . ? O1 C10 P1 108.1(2) . . ? O1 C10 C8 111.2(3) . . ? O1 C10 H10 108.2 . . ? C8 C10 P1 112.8(3) . . ? C8 C10 H10 108.2 . . ? O3 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? O3 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O4 C12 H12A 109.5 . . ? O4 C12 H12B 109.5 . . ? O4 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P1 O3 C11 -161.0(2) . . . . ? O2 P1 O4 C12 -57.7(3) . . . . ? O2 P1 C10 O1 -174.2(2) . . . . ? O2 P1 C10 C8 -50.8(3) . . . . ? O3 P1 O4 C12 -178.2(3) . . . . ? O3 P1 C10 O1 -50.2(2) . . . . ? O3 P1 C10 C8 73.2(3) . . . . ? O4 P1 O3 C11 -37.7(3) . . . . ? O4 P1 C10 O1 59.2(2) . . . . ? O4 P1 C10 C8 -177.4(2) . . . . ? C1 C2 C3 C4 -178.1(3) . . . . ? C1 C2 C7 C6 178.6(4) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C3 C2 C7 C6 0.2(6) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C3 C4 C5 C8 178.2(3) . . . . ? C4 C5 C6 C7 0.2(5) . . . . ? C4 C5 C8 C9 -53.4(4) . . . . ? C4 C5 C8 C10 72.0(4) . . . . ? C5 C6 C7 C2 -0.4(6) . . . . ? C5 C8 C10 P1 166.5(2) . . . . ? C5 C8 C10 O1 -71.9(3) . . . . ? C6 C5 C8 C9 124.4(4) . . . . ? C6 C5 C8 C10 -110.1(4) . . . . ? C7 C2 C3 C4 0.3(6) . . . . ? C8 C5 C6 C7 -177.8(3) . . . . ? C9 C8 C10 P1 -68.0(4) . . . . ? C9 C8 C10 O1 53.7(4) . . . . ? C10 P1 O3 C11 74.2(3) . . . . ? C10 P1 O4 C12 67.2(3) . . . . ? _shelx_res_file ; TITL CELL 1.54178 10.6837 5.7318 11.1098 90 106.432 90 ZERR 2 0.0003 0.0002 0.0004 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O P UNIT 24 38 8 2 L.S. 4 PLAN 3 TEMP -173.15 BOND $H CONF fmap 2 acta REM C:/Users/pwhite/My%20Structures/UNC/Johnson/x1209016/x1209016.hkl WGHT 0.058600 FVAR 0.32071 P1 4 -0.041956 0.337141 0.205942 11.00000 0.01954 0.01680 = 0.02507 0.00052 0.00649 -0.00040 O1 3 0.072548 0.738957 0.289950 11.00000 0.02930 0.01625 = 0.03099 -0.00122 0.00732 0.00190 AFIX 147 H1 2 0.043228 0.850836 0.241309 11.00000 -1.50000 AFIX 0 O2 3 -0.023044 0.116571 0.144838 11.00000 0.02449 0.02118 = 0.02841 -0.00044 0.00852 -0.00062 O3 3 -0.059593 0.291556 0.338529 11.00000 0.02602 0.02288 = 0.03142 0.00147 0.00588 -0.00134 O4 3 -0.170848 0.475324 0.138432 11.00000 0.02406 0.02199 = 0.02519 0.00170 0.00800 0.00007 C1 1 0.652185 1.016685 0.207108 11.00000 0.02965 0.02972 = 0.05214 0.00012 0.00995 -0.00847 AFIX 137 H1A 2 0.656578 1.163452 0.253371 11.00000 -1.50000 H1B 2 0.638324 1.050298 0.117799 11.00000 -1.50000 H1C 2 0.734179 0.930864 0.239455 11.00000 -1.50000 AFIX 0 C2 1 0.540353 0.870881 0.223608 11.00000 0.02342 0.02949 = 0.03384 0.00101 0.00553 -0.00136 C3 1 0.470039 0.936451 0.304115 11.00000 0.02820 0.01896 = 0.03655 -0.00344 0.00204 -0.00311 AFIX 43 H3 2 0.490845 1.079498 0.348466 11.00000 -1.20000 AFIX 0 C4 1 0.369655 0.800835 0.322856 11.00000 0.02545 0.02683 = 0.02905 0.00001 0.00581 0.00246 AFIX 43 H4 2 0.323720 0.851449 0.379894 11.00000 -1.20000 AFIX 0 C5 1 0.335610 0.590487 0.258519 11.00000 0.02166 0.02550 = 0.02358 0.00255 0.00363 0.00148 C6 1 0.406718 0.524898 0.176775 11.00000 0.02867 0.02447 = 0.03454 -0.00598 0.00567 -0.00424 AFIX 43 H6 2 0.385838 0.382910 0.131412 11.00000 -1.20000 AFIX 0 C7 1 0.506984 0.661376 0.160005 11.00000 0.02994 0.03635 = 0.03614 -0.00447 0.01377 -0.00425 AFIX 43 H7 2 0.554011 0.610885 0.103864 11.00000 -1.20000 AFIX 0 C8 1 0.229045 0.432518 0.278544 11.00000 0.02663 0.01842 = 0.02757 -0.00227 0.00645 -0.00019 AFIX 13 H8 2 0.232392 0.283291 0.232925 11.00000 -1.20000 AFIX 0 C9 1 0.250195 0.372100 0.417059 11.00000 0.02474 0.02905 = 0.03374 0.00510 0.00831 0.00011 AFIX 137 H9A 2 0.239641 0.513001 0.463197 11.00000 -1.50000 H9B 2 0.338433 0.309704 0.452055 11.00000 -1.50000 H9C 2 0.186055 0.254908 0.424619 11.00000 -1.50000 AFIX 0 C10 1 0.093160 0.543861 0.219217 11.00000 0.02457 0.01716 = 0.02458 0.00018 0.00862 -0.00386 AFIX 13 H10 2 0.089845 0.599032 0.132979 11.00000 -1.20000 AFIX 0 C11 1 -0.117657 0.458524 0.406821 11.00000 0.03546 0.02955 = 0.02660 -0.00530 0.01591 -0.00276 AFIX 137 H11A 2 -0.210208 0.479522 0.362247 11.00000 -1.50000 H11B 2 -0.072419 0.608606 0.412452 11.00000 -1.50000 H11C 2 -0.109217 0.399230 0.491486 11.00000 -1.50000 AFIX 0 C12 1 -0.195345 0.546556 0.009318 11.00000 0.03184 0.03775 = 0.02711 0.00581 0.00633 0.00768 AFIX 137 H12A 2 -0.284412 0.502701 -0.037717 11.00000 -1.50000 H12B 2 -0.133036 0.469281 -0.027478 11.00000 -1.50000 H12C 2 -0.185232 0.716085 0.005423 11.00000 -1.50000 HKLF 4 REM REM R1 = 0.0474 for 1990 Fo > 4sig(Fo) and 0.0532 for all 2176 data REM 159 parameters refined using 1 restraints END WGHT 0.0586 0.0000 REM Highest difference peak 0.430, deepest hole -0.340, 1-sigma level 0.065 Q1 1 0.0333 0.4271 0.2043 11.00000 0.05 0.43 Q2 1 -0.0519 0.3549 0.2742 11.00000 0.05 0.38 Q3 1 0.0358 0.2449 0.2032 11.00000 0.05 0.33 REM The information below was added by Olex2. REM REM R1 = 0.0474 for 1990 Fo > 4sig(Fo) and n/a for all 4361 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.43, deepest hole -0.34 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = n/a REM R1_gt = 0.0474 REM wR_ref = 0.1174 REM GOOF = 1.092 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 4361 REM Reflections_gt = 1990 REM Parameters = n/a REM Hole = 0.43 REM Peak = -0.34 REM Flack = 0.04(4) ; _shelx_res_file_MD5 5750e4aacec650335c09092f42a2211c