# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_rjg120003_4f _database_code_depnum_ccdc_archive 'CCDC 905716' #TrackingRef 'rjg120003.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H17 I N4 O' _chemical_formula_sum 'C13 H17 I N4 O' _chemical_formula_weight 372.21 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 20.6041(14) _cell_length_b 10.2213(6) _cell_length_c 6.8832(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.370(7) _cell_angle_gamma 90.00 _cell_volume 1449.58(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2746 _cell_measurement_theta_min 2.8018 _cell_measurement_theta_max 28.5075 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 2.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5572 _exptl_absorpt_correction_T_max 0.9572 _exptl_absorpt_process_details ; 'Thu Jun 14 11:59:21 2012' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 2784 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2784 _reflns_number_gt 2450 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0470P)^2^+7.4793P] 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 2784 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 I I 0.21039(2) 1.12326(3) 0.36753(7) 0.03327(16) Uani 1 1 d . . . N1 N 0.21186(19) 0.8389(4) 0.4057(6) 0.0141(8) Uani 1 1 d . . . C2 C 0.1687(2) 0.9341(5) 0.3635(7) 0.0153(10) Uani 1 1 d . . . N3 N 0.1075(2) 0.9276(4) 0.3211(6) 0.0179(9) Uani 1 1 d . . . C4 C 0.0857(2) 0.8017(5) 0.3171(7) 0.0170(10) Uani 1 1 d . . . C5 C 0.1249(2) 0.6945(5) 0.3533(7) 0.0135(9) Uani 1 1 d . . . C6 C 0.1902(2) 0.7170(5) 0.3982(7) 0.0119(10) Uani 1 1 d . . . N7 N 0.08633(19) 0.5859(4) 0.3291(6) 0.0147(9) Uani 1 1 d . . . C7 C 0.1043(2) 0.4492(5) 0.3523(9) 0.0206(11) Uani 1 1 d . . . H7A H 0.0686 0.3935 0.3069 0.031 Uiso 1 1 calc R . . H7B H 0.1132 0.4311 0.4897 0.031 Uiso 1 1 calc R . . H7C H 0.1432 0.4309 0.2759 0.031 Uiso 1 1 calc R . . C8 C 0.0272(3) 0.6343(6) 0.2795(8) 0.0230(12) Uani 1 1 d . . . H8A H -0.0092 0.5798 0.2539 0.028 Uiso 1 1 calc R . . N9 N 0.02431(19) 0.7634(5) 0.2696(6) 0.0204(10) Uani 1 1 d . . . O10 O 0.22907(16) 0.6166(3) 0.4344(6) 0.0180(8) Uani 1 1 d . . . C11 C 0.2968(2) 0.6413(5) 0.4762(9) 0.0220(12) Uani 1 1 d . . . H11A H 0.3071 0.6133 0.6105 0.026 Uiso 1 1 calc R . . H11B H 0.3058 0.7361 0.4655 0.026 Uiso 1 1 calc R . . C12 C 0.3386(2) 0.5668(5) 0.3344(8) 0.0144(10) Uani 1 1 d . . . H12A H 0.3249 0.5914 0.1997 0.017 Uiso 1 1 calc R . . C13 C 0.4094(2) 0.6077(6) 0.3628(11) 0.0315(14) Uani 1 1 d . . . H13A H 0.4136 0.7027 0.3377 0.038 Uiso 1 1 calc R . . H13B H 0.4226 0.5913 0.4992 0.038 Uiso 1 1 calc R . . C14 C 0.4542(3) 0.5335(7) 0.2283(11) 0.0393(17) Uani 1 1 d . . . H14A H 0.4443 0.5573 0.0920 0.047 Uiso 1 1 calc R . . H14B H 0.4998 0.5586 0.2560 0.047 Uiso 1 1 calc R . . C15 C 0.4467(3) 0.3873(6) 0.2539(11) 0.0344(15) Uani 1 1 d . . . H15A H 0.4615 0.3624 0.3859 0.041 Uiso 1 1 calc R . . H15B H 0.4744 0.3414 0.1589 0.041 Uiso 1 1 calc R . . C16 C 0.3765(3) 0.3443(7) 0.2254(10) 0.0349(15) Uani 1 1 d . . . H16A H 0.3636 0.3578 0.0881 0.042 Uiso 1 1 calc R . . H16B H 0.3727 0.2499 0.2549 0.042 Uiso 1 1 calc R . . C17 C 0.3315(2) 0.4209(5) 0.3558(9) 0.0209(11) Uani 1 1 d . . . H17A H 0.2861 0.3962 0.3253 0.025 Uiso 1 1 calc R . . H17B H 0.3403 0.3965 0.4927 0.025 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 I 0.0448(3) 0.0198(2) 0.0353(2) 0.00090(17) -0.00131(19) -0.00403(17) N1 0.0109(18) 0.017(2) 0.015(2) 0.0014(17) 0.0013(17) 0.0002(17) C2 0.022(2) 0.012(2) 0.012(2) 0.001(2) 0.003(2) 0.000(2) N3 0.022(2) 0.018(2) 0.014(2) -0.0005(18) 0.0008(18) 0.0061(18) C4 0.018(2) 0.022(3) 0.011(2) 0.001(2) 0.0009(19) 0.004(2) C5 0.014(2) 0.016(2) 0.010(2) 0.002(2) 0.0024(19) -0.0001(19) C6 0.009(2) 0.015(2) 0.012(2) -0.001(2) 0.0010(18) 0.0024(18) N7 0.0085(18) 0.020(2) 0.016(2) -0.0026(18) -0.0008(16) -0.0017(16) C7 0.016(2) 0.018(3) 0.027(3) -0.003(2) 0.000(2) -0.004(2) C8 0.011(2) 0.038(3) 0.019(3) -0.001(3) -0.005(2) 0.000(2) N9 0.0107(18) 0.033(3) 0.018(2) 0.002(2) -0.0016(17) 0.0053(19) O10 0.0092(16) 0.0120(17) 0.033(2) -0.0038(16) -0.0034(15) 0.0010(13) C11 0.008(2) 0.023(3) 0.035(3) -0.010(2) -0.007(2) 0.000(2) C12 0.006(2) 0.017(2) 0.020(3) 0.004(2) 0.0003(19) 0.0001(18) C13 0.010(2) 0.024(3) 0.060(4) -0.008(3) 0.005(3) -0.005(2) C14 0.017(3) 0.045(4) 0.056(4) -0.003(4) 0.012(3) 0.001(3) C15 0.022(3) 0.036(4) 0.045(4) -0.011(3) 0.008(3) 0.008(3) C16 0.032(3) 0.032(3) 0.041(4) -0.018(3) -0.003(3) 0.009(3) C17 0.016(2) 0.012(2) 0.034(3) -0.001(2) 0.001(2) -0.003(2) _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 I C2 2.115(5) . ? N1 C2 1.348(6) . ? N1 C6 1.325(6) . ? C2 N3 1.295(7) . ? N3 C4 1.363(7) . ? C4 C5 1.383(7) . ? C4 N9 1.362(7) . ? C5 C6 1.397(6) . ? C5 N7 1.375(6) . ? C6 O10 1.324(6) . ? N7 C7 1.454(7) . ? N7 C8 1.357(7) . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 H8A 0.950 . ? C8 N9 1.323(8) . ? O10 C11 1.445(6) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 C12 1.512(7) . ? C12 H12A 1.000 . ? C12 C13 1.529(6) . ? C12 C17 1.506(7) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C13 C14 1.515(9) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.512(9) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.522(9) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.513(8) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? 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 C2 N1 C6 116.7(4) . . ? I C2 N1 113.0(3) . . ? I C2 N3 116.4(4) . . ? N1 C2 N3 130.7(5) . . ? C2 N3 C4 111.9(4) . . ? N3 C4 C5 123.6(4) . . ? N3 C4 N9 125.6(5) . . ? C5 C4 N9 110.8(5) . . ? C4 C5 C6 118.0(4) . . ? C4 C5 N7 106.4(4) . . ? C6 C5 N7 135.6(5) . . ? N1 C6 C5 119.1(4) . . ? N1 C6 O10 121.2(4) . . ? C5 C6 O10 119.7(4) . . ? C5 N7 C7 128.0(4) . . ? C5 N7 C8 104.7(4) . . ? C7 N7 C8 127.3(4) . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N7 C8 H8A 122.7 . . ? N7 C8 N9 114.6(5) . . ? H8A C8 N9 122.7 . . ? C4 N9 C8 103.5(4) . . ? C6 O10 C11 119.0(4) . . ? O10 C11 H11A 109.7 . . ? O10 C11 H11B 109.7 . . ? O10 C11 C12 109.7(4) . . ? H11A C11 H11B 108.2 . . ? H11A C11 C12 109.7 . . ? H11B C11 C12 109.7 . . ? C11 C12 H12A 108.2 . . ? C11 C12 C13 109.1(4) . . ? C11 C12 C17 112.3(4) . . ? H12A C12 C13 108.2 . . ? H12A C12 C17 108.2 . . ? C13 C12 C17 110.6(4) . . ? C12 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C12 C13 C14 111.7(5) . . ? H13A C13 H13B 107.9 . . ? H13A C13 C14 109.3 . . ? H13B C13 C14 109.3 . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C13 C14 C15 111.1(5) . . ? H14A C14 H14B 108.0 . . ? H14A C14 C15 109.4 . . ? H14B C14 C15 109.4 . . ? C14 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C14 C15 C16 111.6(5) . . ? H15A C15 H15B 108.0 . . ? H15A C15 C16 109.3 . . ? H15B C15 C16 109.3 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C15 C16 C17 111.1(5) . . ? H16A C16 H16B 108.0 . . ? H16A C16 C17 109.4 . . ? H16B C16 C17 109.4 . . ? C12 C17 C16 113.1(5) . . ? C12 C17 H17A 108.9 . . ? C12 C17 H17B 108.9 . . ? C16 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.8 . . ? 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 C6 N1 C2 I -177.3(3) . . . . ? C6 N1 C2 N3 2.3(8) . . . . ? I C2 N3 C4 178.3(3) . . . . ? N1 C2 N3 C4 -1.2(8) . . . . ? C2 N3 C4 C5 -0.3(7) . . . . ? C2 N3 C4 N9 -177.3(5) . . . . ? N3 C4 C5 C6 0.6(7) . . . . ? N3 C4 C5 N7 -177.9(4) . . . . ? N9 C4 C5 C6 178.0(4) . . . . ? N9 C4 C5 N7 -0.5(5) . . . . ? C2 N1 C6 C5 -1.7(7) . . . . ? C2 N1 C6 O10 179.0(4) . . . . ? C4 C5 C6 N1 0.4(7) . . . . ? C4 C5 C6 O10 179.8(4) . . . . ? N7 C5 C6 N1 178.4(5) . . . . ? N7 C5 C6 O10 -2.2(9) . . . . ? C4 C5 N7 C7 -179.4(5) . . . . ? C4 C5 N7 C8 0.3(5) . . . . ? C6 C5 N7 C7 2.5(9) . . . . ? C6 C5 N7 C8 -177.9(6) . . . . ? C5 N7 C8 N9 0.0(6) . . . . ? C7 N7 C8 N9 179.7(5) . . . . ? N7 C8 N9 C4 -0.3(6) . . . . ? N3 C4 N9 C8 177.8(5) . . . . ? C5 C4 N9 C8 0.5(6) . . . . ? N1 C6 O10 C11 -2.1(7) . . . . ? C5 C6 O10 C11 178.6(5) . . . . ? C6 O10 C11 C12 -123.3(5) . . . . ? O10 C11 C12 C13 172.6(5) . . . . ? O10 C11 C12 C17 -64.4(6) . . . . ? C11 C12 C13 C14 178.4(5) . . . . ? C17 C12 C13 C14 54.4(7) . . . . ? C12 C13 C14 C15 -55.8(8) . . . . ? C13 C14 C15 C16 55.5(8) . . . . ? C14 C15 C16 C17 -54.0(8) . . . . ? C11 C12 C17 C16 -175.8(5) . . . . ? C13 C12 C17 C16 -53.7(7) . . . . ? C15 C16 C17 C12 53.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.659 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.125 # Contents of RES file _computing_special_details ; TITL rjg120003 in P2(1)/c CELL 0.71073 20.6041 10.2213 6.8832 90.000 90.370 90.000 ZERR 4.00 0.0014 0.0006 0.0005 0.000 0.007 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O I N UNIT 52 68 4 4 16 TEMP -123 L.S. 8 BOND $H CONF REM colourless lath SIZE 0.30 0.10 0.02 FMAP 2 PLAN 5 OMIT -3 52 ACTA 50 REM EXTI 0.000000 WGHT 0.047000 7.479300 BASF 0.08133 FVAR 3.09366 I 4 0.210392 1.123265 0.367526 11.00000 0.04477 0.01976 = 0.03526 0.00090 -0.00131 -0.00403 N1 5 0.211857 0.838883 0.405653 11.00000 0.01094 0.01650 = 0.01486 0.00138 0.00131 0.00020 C2 1 0.168732 0.934112 0.363538 11.00000 0.02193 0.01228 = 0.01172 0.00069 0.00289 0.00043 N3 5 0.107495 0.927642 0.321090 11.00000 0.02247 0.01759 = 0.01372 -0.00052 0.00076 0.00611 C4 1 0.085717 0.801703 0.317090 11.00000 0.01820 0.02238 = 0.01053 0.00132 0.00090 0.00432 C5 1 0.124899 0.694527 0.353320 11.00000 0.01431 0.01605 = 0.01028 0.00158 0.00241 -0.00006 C6 1 0.190181 0.716976 0.398228 11.00000 0.00906 0.01453 = 0.01208 -0.00100 0.00105 0.00242 N7 5 0.086332 0.585887 0.329083 11.00000 0.00854 0.01999 = 0.01551 -0.00262 -0.00077 -0.00168 C7 1 0.104307 0.449201 0.352293 11.00000 0.01629 0.01842 = 0.02702 -0.00264 0.00004 -0.00382 AFIX 137 H7A 2 0.068599 0.393471 0.306909 11.00000 -1.50000 H7B 2 0.113202 0.431107 0.489724 11.00000 -1.50000 H7C 2 0.143237 0.430892 0.275892 11.00000 -1.50000 AFIX 0 C8 1 0.027177 0.634250 0.279480 11.00000 0.01127 0.03822 = 0.01941 -0.00149 -0.00529 0.00010 AFIX 43 H8A 2 -0.009243 0.579774 0.253882 11.00000 -1.20000 AFIX 0 N9 5 0.024309 0.763373 0.269638 11.00000 0.01074 0.03253 = 0.01803 0.00200 -0.00163 0.00526 O10 3 0.229068 0.616617 0.434416 11.00000 0.00924 0.01205 = 0.03268 -0.00379 -0.00337 0.00099 C11 1 0.296781 0.641253 0.476166 11.00000 0.00791 0.02323 = 0.03476 -0.00994 -0.00749 0.00040 AFIX 23 H11A 2 0.307129 0.613305 0.610548 11.00000 -1.20000 H11B 2 0.305797 0.736110 0.465526 11.00000 -1.20000 AFIX 0 C12 1 0.338620 0.566768 0.334422 11.00000 0.00585 0.01677 = 0.02047 0.00405 0.00032 0.00008 AFIX 13 H12A 2 0.324917 0.591417 0.199679 11.00000 -1.20000 AFIX 0 C13 1 0.409445 0.607709 0.362788 11.00000 0.00970 0.02449 = 0.06047 -0.00790 0.00539 -0.00549 AFIX 23 H13A 2 0.413634 0.702693 0.337671 11.00000 -1.20000 H13B 2 0.422617 0.591297 0.499198 11.00000 -1.20000 AFIX 0 C14 1 0.454245 0.533491 0.228319 11.00000 0.01733 0.04466 = 0.05593 -0.00308 0.01231 0.00101 AFIX 23 H14A 2 0.444270 0.557312 0.091950 11.00000 -1.20000 H14B 2 0.499772 0.558645 0.256031 11.00000 -1.20000 AFIX 0 C15 1 0.446661 0.387340 0.253944 11.00000 0.02235 0.03608 = 0.04473 -0.01141 0.00805 0.00830 AFIX 23 H15A 2 0.461458 0.362355 0.385943 11.00000 -1.20000 H15B 2 0.474432 0.341445 0.158922 11.00000 -1.20000 AFIX 0 C16 1 0.376514 0.344341 0.225430 11.00000 0.03201 0.03161 = 0.04112 -0.01809 -0.00280 0.00859 AFIX 23 H16A 2 0.363591 0.357752 0.088090 11.00000 -1.20000 H16B 2 0.372665 0.249871 0.254916 11.00000 -1.20000 AFIX 0 C17 1 0.331457 0.420887 0.355808 11.00000 0.01641 0.01200 = 0.03434 -0.00098 0.00092 -0.00342 AFIX 23 H17A 2 0.286062 0.396200 0.325283 11.00000 -1.20000 H17B 2 0.340268 0.396515 0.492658 11.00000 -1.20000 HKLF 5 REM rjg120003 in P2(1)/c REM R1 = 0.0428 for 2450 Fo > 4sig(Fo) and 0.0500 for all 2784 data REM 174 parameters refined using 0 restraints END WGHT 0.0473 7.4449 REM Highest difference peak 1.659, deepest hole -0.671, 1-sigma level 0.125 Q1 1 0.2103 1.1284 0.1336 11.00000 0.05 1.66 Q2 1 0.2411 1.0578 0.3943 11.00000 0.05 0.88 Q3 1 0.1883 1.0404 0.3571 11.00000 0.05 0.83 Q4 1 0.1574 1.1813 0.3384 11.00000 0.05 0.73 Q5 1 0.0601 0.6152 0.3219 11.00000 0.05 0.55 ; #===END