data_Baran313 _audit_creation_date 2013-09-26 _audit_creation_method ; Olex2 1.2-beta (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _shelxl_version_number 2013-3 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common 'RRVI N oxide diol' _chemical_name_systematic 3-(N,N-diethylamine)-propan-1,2-diol-N-oxide _chemical_formula_moiety 'C7 H17 N O3' _chemical_formula_sum 'C7 H17 N O3' _chemical_formula_weight 163.21 _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' 0.0033 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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_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 5.6142(5) _cell_length_b 12.7026(8) _cell_length_c 12.0019(8) _cell_angle_alpha 90 _cell_angle_beta 95.341(3) _cell_angle_gamma 90 _cell_volume 852.20(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2998 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.367 _cell_measurement_theta_min 2.340 _shelx_estimated_absorpt_T_max 0.992 _shelx_estimated_absorpt_T_min 0.969 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1524 before and 0.0322 after correction. The Ratio of minimum to maximum transmission is 0.8719. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'Colorless' _exptl_crystal_colour_lustre Clear _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not measured' _exptl_crystal_description 'Plate' _exptl_crystal_F_000 360 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_unetI/netI 0.0234 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5994 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 26.402 _diffrn_reflns_theta_min 2.340 _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX II TXS' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1515 _reflns_number_total 1740 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _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 ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.315 _refine_diff_density_min -0.188 _refine_diff_density_rms 0.039 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1740 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0324 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.3061P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.0872 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances O1-H1 0.9 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O2A) = Uanis(O2) 4. Others Sof(H2B)=Sof(O2A)=Sof(H2AA)=1-FVAR(1) Sof(O2)=Sof(H2)=Sof(H2A)=FVAR(1) 5.a Ternary CH refined with riding coordinates: C2(H2A), C2(H2B) 5.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B) 5.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C7(H7A,H7B,H7C) 5.d Idealised tetrahedral OH refined as rotating group: O2A(H2AA) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.42287(15) 0.37267(7) 1.09526(7) 0.0187(2) Uani 1 1 d D . . . . H1 H 0.351(3) 0.3358(13) 1.1453(13) 0.037(5) Uiso 1 1 d D . . . . O2 O 0.06975(16) 0.38872(7) 0.82368(7) 0.0154(2) Uani 0.9451(19) 1 d . . P A 1 H2 H -0.048(3) 0.3433(14) 0.8035(14) 0.033(5) Uiso 0.9451(19) 1 d . . P A 1 O3 O 0.75424(14) 0.24107(6) 0.76095(7) 0.0160(2) Uani 1 1 d . . . . . N1 N 0.50908(17) 0.25587(7) 0.76853(7) 0.0119(2) Uani 1 1 d . . . . . C1 C 0.2512(2) 0.40926(9) 1.00985(9) 0.0137(3) Uani 1 1 d . . . . . H1A H 0.2943 0.4816 0.9886 0.016 Uiso 1 1 calc R U . . . H1B H 0.0927 0.4124 1.0397 0.016 Uiso 1 1 calc R U . . . C2 C 0.2326(2) 0.33959(8) 0.90536(9) 0.0122(2) Uani 1 1 d . . . . . H2A H 0.1699 0.2687 0.9242 0.015 Uiso 0.9451(19) 1 calc R U P A 1 H2B H 0.1365 0.3802 0.8456 0.015 Uiso 0.0549(19) 1 calc R U P A 2 C3 C 0.4815(2) 0.32790(9) 0.86662(9) 0.0137(3) Uani 1 1 d . . . . . H3A H 0.5381 0.3988 0.8471 0.016 Uiso 1 1 calc R U . . . H3B H 0.5895 0.3023 0.9308 0.016 Uiso 1 1 calc R U . . . C4 C 0.3952(2) 0.14978(9) 0.78344(9) 0.0155(3) Uani 1 1 d . . . . . H4A H 0.4189 0.1051 0.7178 0.019 Uiso 1 1 calc R U . . . H4B H 0.2209 0.1592 0.7866 0.019 Uiso 1 1 calc R U . . . C5 C 0.4983(2) 0.09451(10) 0.88843(11) 0.0221(3) Uani 1 1 d . . . . . H5A H 0.4437 0.0212 0.8871 0.033 Uiso 1 1 calc R U . . . H5B H 0.4446 0.1302 0.9541 0.033 Uiso 1 1 calc R U . . . H5C H 0.6733 0.0963 0.8923 0.033 Uiso 1 1 calc R U . . . C6 C 0.3995(2) 0.30168(9) 0.65922(9) 0.0158(3) Uani 1 1 d . . . . . H6A H 0.4107 0.2492 0.5989 0.019 Uiso 1 1 calc R U . . . H6B H 0.2279 0.3160 0.6653 0.019 Uiso 1 1 calc R U . . . C7 C 0.5204(3) 0.40222(11) 0.62779(11) 0.0264(3) Uani 1 1 d . . . . . H7A H 0.4597 0.4228 0.5517 0.040 Uiso 1 1 calc R U . . . H7B H 0.6935 0.3909 0.6310 0.040 Uiso 1 1 calc R U . . . H7C H 0.4862 0.4582 0.6802 0.040 Uiso 1 1 calc R U . . . O2A O 0.096(3) 0.2503(11) 0.9269(12) 0.0154(2) Uani 0.0549(19) 1 d . . P A 2 H2AA H -0.0156 0.2433 0.8757 0.023 Uiso 0.0549(19) 1 calc R U P A 2 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 O1 0.0129(5) 0.0298(5) 0.0130(4) 0.0056(4) -0.0004(3) 0.0005(4) O2 0.0102(5) 0.0172(4) 0.0178(4) 0.0021(3) -0.0045(3) 0.0001(3) O3 0.0075(4) 0.0216(4) 0.0187(4) -0.0054(3) 0.0001(3) 0.0010(3) N1 0.0082(5) 0.0143(5) 0.0130(4) -0.0008(4) -0.0003(4) -0.0006(4) C1 0.0110(6) 0.0161(5) 0.0140(5) 0.0014(4) 0.0004(4) 0.0006(4) C2 0.0095(6) 0.0118(5) 0.0148(5) 0.0026(4) -0.0015(4) -0.0003(4) C3 0.0118(6) 0.0152(5) 0.0136(5) -0.0036(4) -0.0007(4) -0.0009(4) C4 0.0164(6) 0.0126(5) 0.0172(5) -0.0010(4) -0.0003(4) -0.0033(4) C5 0.0249(7) 0.0177(6) 0.0233(6) 0.0049(5) 0.0006(5) 0.0035(5) C6 0.0146(6) 0.0202(6) 0.0120(5) 0.0024(4) -0.0019(4) -0.0008(5) C7 0.0260(8) 0.0265(7) 0.0263(7) 0.0112(5) 0.0008(6) -0.0044(5) O2A 0.0102(5) 0.0172(4) 0.0178(4) 0.0021(3) -0.0045(3) 0.0001(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 O1 H1 0.889(14) . ? O1 C1 1.4186(13) . ? O2 H2 0.89(2) . ? O2 C2 1.4210(14) . ? O3 N1 1.4005(12) . ? N1 C3 1.5104(14) . ? N1 C4 1.5095(14) . ? N1 C6 1.5126(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.5305(15) . ? C2 H2A 1.0000 . ? C2 H2B 1.0000 . ? C2 C3 1.5205(16) . ? C2 O2A 1.407(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.5099(16) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.5104(17) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O2A H2AA 0.8400 . ? 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 C1 O1 H1 109.8(11) . . ? C2 O2 H2 108.4(11) . . ? O3 N1 C3 107.74(8) . . ? O3 N1 C4 108.52(8) . . ? O3 N1 C6 108.54(8) . . ? C3 N1 C6 112.34(9) . . ? C4 N1 C3 111.91(8) . . ? C4 N1 C6 107.68(8) . . ? O1 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? O1 C1 C2 113.12(9) . . ? H1A C1 H1B 107.8 . . ? C2 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? O2 C2 C1 107.57(9) . . ? O2 C2 H2A 109.5 . . ? O2 C2 C3 112.48(9) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 106.3 . . ? C3 C2 C1 108.21(9) . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 106.3 . . ? O2A C2 C1 108.2(6) . . ? O2A C2 H2B 106.3 . . ? O2A C2 C3 120.7(6) . . ? N1 C3 C2 117.48(9) . . ? N1 C3 H3A 107.9 . . ? N1 C3 H3B 107.9 . . ? C2 C3 H3A 107.9 . . ? C2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? N1 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? N1 C4 C5 112.36(9) . . ? H4A C4 H4B 107.9 . . ? C5 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 H6A 109.1 . . ? N1 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C7 C6 N1 112.71(10) . . ? C7 C6 H6A 109.1 . . ? C7 C6 H6B 109.1 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 O2A H2AA 109.5 . . ? 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 O1 H1 O3 0.889(14) 1.820(14) 2.6997(12) 170.0(16) 4_566 O2 H2 O3 0.89(2) 1.75(2) 2.6408(12) 171.6(17) 1_455 O2A H2AA O3 0.84 1.80 2.636(14) 174.2 1_455 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 O1 C1 C2 O2 -175.58(9) . . . . ? O1 C1 C2 C3 -53.82(12) . . . . ? O1 C1 C2 O2A 78.5(6) . . . . ? O2 C2 C3 N1 -65.34(12) . . . . ? O3 N1 C3 C2 -168.88(9) . . . . ? O3 N1 C4 C5 60.51(12) . . . . ? O3 N1 C6 C7 -55.72(12) . . . . ? C1 C2 C3 N1 175.98(9) . . . . ? C3 N1 C4 C5 -58.25(12) . . . . ? C3 N1 C6 C7 63.31(13) . . . . ? C4 N1 C3 C2 -49.66(12) . . . . ? C4 N1 C6 C7 -173.02(10) . . . . ? C6 N1 C3 C2 71.61(12) . . . . ? C6 N1 C4 C5 177.82(10) . . . . ? O2A C2 C3 N1 50.7(7) . . . . ? _shelx_res_file ; TITL baran313 in P2(1)/n CELL 0.71073 5.6142 12.7026 12.0019 90 95.341 90 ZERR 4 0.0005 0.0008 0.0008 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 28 68 4 12 EQIV $1 -0.5+X,0.5-Y,0.5+Z EQIV $2 -1+X,+Y,+Z DFIX 0.9 O1 H1 EADP O2A O2 L.S. 10 PLAN 10 SIZE 0.08 0.15 0.32 TEMP -173.15 HTAB O1 O3_$1 HTAB O2A O3_$2 HTAB O2 O3_$2 REM Solution 1 R1 0.129 Rweak 0.004, Alpha = 0.0732 in P2(1)/n REM Formula: C7 N O3 BOND $H MORE -1 CONF fmap 2 acta 50 REM C:\Documents%20and%20Settings\Daley%20Group\Desktop\Frames\baran313\w REM ork\baran313_a.hkl WGHT 0.042500 0.306100 FVAR 0.93429 0.94505 O1 4 0.422869 0.372665 1.095265 11.00000 0.01287 0.02985 = 0.01304 0.00556 -0.00041 0.00054 H1 2 0.350633 0.335843 1.145340 11.00000 0.03692 PART 1 O2 4 0.069752 0.388717 0.823676 21.00000 0.01016 0.01717 = 0.01781 0.00209 -0.00452 0.00014 H2 2 -0.048058 0.343347 0.803470 21.00000 0.03256 PART 0 O3 4 0.754235 0.241071 0.760946 11.00000 0.00751 0.02159 = 0.01871 -0.00539 0.00011 0.00096 N1 3 0.509075 0.255872 0.768531 11.00000 0.00816 0.01432 = 0.01304 -0.00076 -0.00029 -0.00062 C1 1 0.251159 0.409261 1.009852 11.00000 0.01098 0.01608 = 0.01400 0.00142 0.00039 0.00063 AFIX 23 H1A 2 0.294257 0.481613 0.988550 11.00000 -1.20000 H1B 2 0.092749 0.412430 1.039690 11.00000 -1.20000 AFIX 0 C2 1 0.232561 0.339592 0.905358 11.00000 0.00951 0.01177 = 0.01479 0.00257 -0.00152 -0.00034 PART 1 AFIX 13 H2A 2 0.169885 0.268726 0.924186 21.00000 -1.20000 AFIX 13 PART 0 PART 2 H2B 2 0.136456 0.380199 0.845571 -21.00000 -1.20000 AFIX 0 PART 0 C3 1 0.481475 0.327905 0.866621 11.00000 0.01182 0.01522 = 0.01362 -0.00360 -0.00073 -0.00093 AFIX 23 H3A 2 0.538065 0.398774 0.847097 11.00000 -1.20000 H3B 2 0.589494 0.302320 0.930821 11.00000 -1.20000 AFIX 0 C4 1 0.395169 0.149778 0.783444 11.00000 0.01644 0.01260 = 0.01715 -0.00102 -0.00034 -0.00334 AFIX 23 H4A 2 0.418928 0.105083 0.717816 11.00000 -1.20000 H4B 2 0.220883 0.159202 0.786605 11.00000 -1.20000 AFIX 0 C5 1 0.498264 0.094510 0.888427 11.00000 0.02486 0.01766 = 0.02333 0.00492 0.00058 0.00347 AFIX 137 H5A 2 0.443720 0.021195 0.887097 11.00000 -1.50000 H5B 2 0.444640 0.130161 0.954062 11.00000 -1.50000 H5C 2 0.673346 0.096299 0.892265 11.00000 -1.50000 AFIX 0 C6 1 0.399510 0.301680 0.659220 11.00000 0.01461 0.02024 = 0.01197 0.00242 -0.00186 -0.00079 AFIX 23 H6A 2 0.410683 0.249198 0.598948 11.00000 -1.20000 H6B 2 0.227866 0.315975 0.665327 11.00000 -1.20000 AFIX 0 C7 1 0.520366 0.402218 0.627789 11.00000 0.02596 0.02652 = 0.02628 0.01123 0.00077 -0.00440 AFIX 137 H7A 2 0.459734 0.422816 0.551701 11.00000 -1.50000 H7B 2 0.693547 0.390917 0.631028 11.00000 -1.50000 H7C 2 0.486232 0.458153 0.680246 11.00000 -1.50000 AFIX 0 PART 2 O2A 4 0.095943 0.250297 0.926899 -21.00000 0.01016 0.01717 = 0.01781 0.00209 -0.00452 0.00014 AFIX 147 H2AA 2 -0.015564 0.243267 0.875720 -21.00000 -1.50000 AFIX 0 HKLF 4 REM baran313 in P2(1)/n REM R1 = 0.0324 for 1515 Fo > 4sig(Fo) and 0.0383 for all 1740 data REM 115 parameters refined using 1 restraints END WGHT 0.0376 0.3052 REM Highest difference peak 0.315, deepest hole -0.188, 1-sigma level 0.039 Q1 1 0.2477 0.3720 0.9569 11.00000 0.05 0.32 Q2 1 0.4559 0.2824 0.7134 11.00000 0.05 0.25 Q3 1 0.4519 0.2014 0.7773 11.00000 0.05 0.25 Q4 1 0.4612 0.3552 0.6542 11.00000 0.05 0.24 Q5 1 0.3552 0.3390 0.8844 11.00000 0.05 0.22 Q6 1 0.4841 0.2928 0.8198 11.00000 0.05 0.19 Q7 1 0.4485 0.1263 0.8354 11.00000 0.05 0.19 Q8 1 0.4896 0.1180 0.7332 11.00000 0.05 0.18 Q9 1 0.4616 0.2235 0.6182 11.00000 0.05 0.16 Q10 1 0.3269 0.3980 1.0485 11.00000 0.05 0.14 ; _shelx_res_checksum 14257 _shelx_hkl_file ; -1 0 0 -3.40 0.50 1 0 0 -2.70 0.60 2 0 0 2123.89 52.69 -2 0 0 2099.09 52.79 3 0 0 -0.80 1.10 -3 0 0 -0.50 1.10 4 0 0 1302.87 33.00 -4 0 0 1230.18 33.00 -5 0 0 -0.60 2.00 -6 0 0 339.07 11.80 0 -1 0 -6.80 0.10 0 -1 0 -6.70 0.10 0 1 0 -6.60 0.10 0 1 0 -6.70 0.10 -1 -1 0 7.50 0.80 1 -1 0 6.70 0.80 1 1 0 6.90 0.80 -1 1 0 6.00 0.80 2 -1 0 432.76 11.80 -2 -1 0 446.36 11.80 2 1 0 434.66 11.80 -2 1 0 456.85 11.90 -3 -1 0 17.10 1.80 3 -1 0 22.10 2.00 3 1 0 21.90 1.90 -3 1 0 22.00 2.00 4 -1 0 118.99 4.90 -4 -1 0 115.89 5.00 -4 1 0 116.99 5.10 4 1 0 106.59 4.70 -5 -1 0 6.10 2.30 -5 1 0 6.00 2.10 -6 -1 0 60.79 4.90 -6 1 0 53.49 4.80 0 -2 0 4228.58 118.39 0 -2 0 4555.34 120.29 0 2 0 4540.55 120.49 0 2 0 4626.14 119.69 1 -2 0 2644.74 64.69 -1 -2 0 2515.45 64.29 1 2 0 2479.85 63.99 -1 2 0 2753.82 64.69 -1 2 0 2423.96 64.29 -2 -2 0 59.99 2.50 2 -2 0 55.89 2.50 2 2 0 58.79 2.50 -2 2 0 56.49 2.70 -3 -2 0 27.10 2.10 3 -2 0 21.30 1.80 -3 2 0 20.60 2.00 3 2 0 21.10 1.90 4 -2 0 163.48 5.90 -4 -2 0 166.18 6.00 4 2 0 165.48 6.00 -4 2 0 160.68 6.20 -5 -2 0 382.06 12.00 -5 2 0 388.36 12.30 -6 -2 0 19.60 3.40 -6 2 0 20.40 3.60 0 -3 0 -1.00 0.40 0 -3 0 -1.20 0.30 0 3 0 -1.70 0.40 0 3 0 -0.40 0.40 1 -3 0 344.67 9.10 -1 -3 0 355.26 9.00 -1 3 0 341.77 9.00 1 3 0 350.56 9.10 -1 3 0 348.67 9.10 2 -3 0 37.00 2.10 -2 -3 0 38.10 2.10 2 3 0 35.10 2.10 -2 3 0 38.50 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6.30 2 7 0 224.88 6.60 -2 7 0 216.58 6.80 -3 -7 0 13.90 1.50 3 -7 0 15.90 1.80 3 7 0 12.30 1.90 -3 7 0 11.10 2.10 -3 7 0 11.20 1.40 -4 -7 0 179.68 6.20 4 -7 0 167.78 6.30 -4 7 0 181.78 7.20 -5 -7 0 6.70 2.10 -5 7 0 7.90 3.10 -6 -7 0 3.70 2.70 -6 7 0 8.70 4.00 0 -8 0 1146.39 28.40 0 8 0 1126.39 28.50 0 8 0 1127.99 28.50 1 -8 0 163.18 4.90 1 -8 0 167.78 4.70 -1 -8 0 166.08 4.60 1 8 0 164.38 4.60 -1 8 0 154.78 5.10 -1 8 0 167.28 4.80 1 8 0 163.28 5.00 -2 -8 0 65.19 2.50 2 -8 0 72.79 2.80 -2 8 0 73.29 3.40 2 8 0 65.59 3.10 -2 8 0 66.39 2.60 3 -8 0 17.40 1.90 -3 -8 0 15.80 1.50 3 8 0 16.10 2.20 -3 8 0 16.40 2.40 -3 8 0 13.60 1.50 4 -8 0 50.99 3.40 -4 -8 0 38.30 2.70 -4 8 0 39.80 3.80 -5 -8 0 0.70 1.90 -5 8 0 -1.00 2.50 -6 -8 0 54.59 4.20 -6 8 0 50.69 5.30 0 -9 0 0.00 0.60 0 9 0 1.40 0.80 0 9 0 1.40 0.70 -1 -9 0 12.90 1.00 1 -9 0 13.40 1.10 1 -9 0 13.50 1.30 1 9 0 13.10 1.30 -1 9 0 12.40 1.50 1 9 0 12.30 1.00 -1 9 0 13.00 1.10 2 -9 0 35.40 2.00 -2 -9 0 35.00 1.80 2 9 0 36.70 1.70 -2 9 0 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5.90 2.90 -6 5 -4 6.30 3.90 -6 -6 4 14.90 3.40 -6 6 4 21.70 3.90 5 -6 -4 17.60 3.10 -5 -6 4 20.50 2.90 -5 6 4 24.20 3.60 4 -6 -4 655.13 17.80 -4 -6 4 616.84 17.60 -4 6 4 634.84 18.20 -3 -6 4 24.90 2.20 3 -6 -4 26.50 2.20 3 6 -4 23.80 2.70 -3 6 4 25.70 2.50 2 -6 -4 120.69 4.20 -2 -6 4 124.69 4.20 2 6 -4 131.99 4.80 -2 6 4 127.29 4.60 1 -6 -4 20.70 1.20 -1 -6 4 17.40 1.30 1 6 -4 19.10 1.30 1 6 -4 24.10 1.80 -1 6 4 20.10 1.10 -1 6 4 19.10 1.40 0 -6 4 610.54 15.90 0 6 -4 607.84 15.90 0 6 -4 633.84 16.10 0 6 4 617.24 15.30 0 6 4 615.04 15.50 1 -6 4 100.89 3.40 1 -6 4 99.59 3.20 -1 6 -4 104.19 3.40 -1 6 -4 98.29 3.60 -2 -6 -4 684.43 16.70 2 -6 4 666.23 17.60 -2 -6 -4 655.13 16.70 2 -6 4 676.53 17.50 2 6 4 669.83 17.00 -2 6 -4 681.63 18.00 -2 6 -4 677.23 17.50 3 -6 4 11.20 1.50 -3 -6 -4 8.80 1.10 -3 6 -4 6.30 1.30 -3 6 -4 8.00 2.00 3 6 4 9.60 1.40 -4 -6 -4 203.78 6.50 4 6 4 195.58 6.60 -4 6 -4 208.78 7.90 -5 -6 -4 6.10 2.00 -5 6 -4 3.50 3.00 -6 -6 -4 96.99 6.00 -6 6 -4 95.49 6.90 -6 -7 4 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2 5 899.71 22.30 1 2 5 893.01 22.20 2 -2 5 1884.71 47.90 -2 -2 -5 1907.51 47.50 2 -2 5 1966.70 48.00 -2 -2 -5 1921.41 47.90 -2 2 -5 1925.41 48.20 2 2 5 1930.51 47.70 -2 2 -5 1909.71 47.80 3 -2 5 -0.80 0.90 -3 -2 -5 0.90 0.70 -3 -2 -5 -0.30 1.10 -3 2 -5 0.10 0.80 3 2 5 -0.20 0.90 -3 2 -5 0.10 1.30 -4 -2 -5 455.45 12.10 -4 -2 -5 457.45 13.10 -4 2 -5 446.66 12.30 4 2 5 458.85 12.50 -4 2 -5 429.06 13.30 -5 -2 -5 124.29 4.70 -5 -2 -5 118.89 5.90 -5 2 -5 126.19 4.90 -5 2 -5 117.09 6.40 -6 -2 -5 31.00 4.10 -6 2 -5 39.80 4.80 -6 -3 5 84.99 5.90 -6 3 5 89.79 6.30 -5 -3 5 346.27 11.30 -5 3 5 347.67 11.70 -4 -3 5 6.60 1.90 4 -3 -5 9.80 2.30 4 3 -5 9.70 2.70 -4 3 5 11.70 2.30 -3 -3 5 21.50 2.10 3 -3 -5 21.20 2.30 -3 3 5 23.80 2.30 3 3 -5 21.60 2.50 -2 -3 5 31.60 2.20 2 -3 -5 37.00 2.40 -2 3 5 25.50 1.90 2 3 -5 27.30 2.10 1 -3 -5 506.55 13.10 -1 -3 5 488.55 13.10 -1 3 5 510.15 13.00 1 3 -5 493.85 13.40 0 -3 -5 1043.20 26.40 0 -3 -5 1090.79 26.20 0 -3 5 1071.79 26.70 0 3 -5 1056.29 26.60 0 3 5 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151.88 5.20 -1 5 -10 149.79 5.40 -1 5 -10 146.09 5.60 2 -5 10 25.30 2.30 -2 5 -10 23.10 2.30 -2 5 -10 30.80 2.80 3 -5 10 0.60 1.70 -3 5 -10 0.80 1.90 -3 5 -10 -2.90 2.20 -4 -5 -10 29.80 2.30 -4 5 -10 29.40 4.00 -4 -6 10 10.70 2.30 -4 6 10 11.20 2.80 -3 -6 10 32.50 2.80 -3 6 10 43.40 3.30 2 -6 -10 12.00 1.90 -2 -6 10 9.70 1.70 -2 6 10 14.30 1.80 2 6 -10 11.40 1.70 -1 -6 10 92.79 4.00 1 -6 -10 99.59 3.50 1 -6 -10 101.39 2.90 1 6 -10 97.29 5.40 -1 6 10 96.49 3.20 1 6 -10 99.99 3.90 0 -6 10 21.80 2.00 0 6 10 21.10 1.00 0 6 -10 19.80 1.80 0 6 -10 19.30 2.60 1 -6 10 38.30 2.60 -1 6 -10 38.50 3.10 -1 6 -10 27.90 2.50 2 -6 10 93.19 4.30 -2 6 -10 94.19 4.80 -2 6 -10 93.89 4.50 3 -6 10 19.30 2.60 -3 6 -10 11.90 2.80 -4 6 -10 -0.10 3.20 -4 -7 10 0.20 2.00 -3 -7 10 -0.30 1.50 3 7 -10 -0.30 1.50 2 -7 -10 132.29 4.90 -2 -7 10 134.59 5.20 -2 7 10 134.19 4.90 2 7 -10 139.79 5.00 1 -7 -10 4.00 0.50 -1 -7 10 4.20 1.30 1 -7 -10 2.40 0.80 -1 7 10 3.70 0.80 1 7 -10 3.40 1.40 0 -7 10 64.89 3.20 0 7 -10 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146.69 6.30 1 -11 10 14.60 2.60 -1 11 -10 17.90 3.20 -5 0 11 35.10 4.00 -4 0 11 1.90 2.20 4 0 -11 0.70 3.80 -3 0 11 163.28 6.10 3 0 -11 160.78 7.40 2 0 -11 0.40 2.20 -2 0 11 0.30 1.20 1 0 -11 89.49 4.70 1 0 -11 88.59 3.30 -1 0 11 95.39 3.60 0 0 -11 -1.40 1.50 0 0 -11 -0.40 0.90 0 0 11 1.60 0.90 -1 0 -11 77.19 3.70 1 0 11 83.09 3.20 -1 0 -11 78.79 3.40 -2 0 -11 0.10 1.30 -2 0 -11 -1.90 1.40 2 0 11 0.40 1.20 -3 0 -11 10.20 2.30 -4 0 -11 -1.30 2.70 -5 -1 11 51.99 4.70 -5 1 11 53.29 4.60 -4 -1 11 2.20 2.20 4 -1 -11 0.30 3.60 -4 1 11 -0.80 2.10 -3 -1 11 64.69 3.90 3 -1 -11 75.69 5.10 3 1 -11 74.69 5.30 -3 1 11 64.49 3.90 -2 -1 11 16.90 1.90 2 -1 -11 15.20 2.70 2 1 -11 14.50 2.80 -2 1 11 13.10 1.80 1 -1 -11 112.49 3.70 1 -1 -11 105.49 5.00 -1 -1 11 116.29 4.20 1 1 -11 115.39 5.20 1 1 -11 114.69 3.90 -1 1 11 110.89 3.90 0 -1 -11 324.87 9.70 0 -1 11 333.57 9.20 0 -1 -11 321.47 8.90 0 1 -11 324.07 9.10 0 1 -11 333.47 9.90 0 1 11 332.87 9.00 1 -1 11 184.68 5.70 -1 -1 -11 172.18 5.70 -1 -1 -11 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