############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section E. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section E, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method 'SHELXL-2014/7' _chemical_name_systematic ;\ N-(4,4-Diphenylbut-3-en-1-yl)-N-iodomethyl-N,N-\ dimethylammonium iodide ; _chemical_name_common ? _chemical_formula_moiety 'C19 H23 I N+, I-' _chemical_formula_sum 'C19 H23 I2 N' _chemical_formula_iupac 'C19 H23 I N+, I-' _chemical_formula_weight 519.18 _chemical_melting_point_gt 425 _chemical_melting_point_lt 427 _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_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.9254(2) _cell_length_b 13.6161(3) _cell_length_c 9.4632(2) _cell_angle_alpha 90 _cell_angle_beta 103.3200(10) _cell_angle_gamma 90 _cell_volume 993.73(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4987 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.34 _cell_measurement_temperature 298(2) _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.188 _exptl_crystal_size_min 0.122 _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 3.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2012) ; _shelx_estimated_absorpt_T_min 0.530 _shelx_estimated_absorpt_T_max 0.699 _exptl_absorpt_correction_T_min 0.6241 _exptl_absorpt_correction_T_max 0.7452 _diffrn_ambient_temperature 298(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 5791 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_theta_min 2.212 _diffrn_reflns_theta_max 25.339 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _refine_special_details ; Refined as a 2-component inversion twin. ; _reflns_number_total 3085 _reflns_number_gt 3013 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0178 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0383 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_number_reflns 3085 _refine_ls_number_parameters 202 _refine_ls_number_restraints 1 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+0.0203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.265 _refine_diff_density_min -0.462 _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.02(3) 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2008) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I I1 -0.65685(3) 0.06224(2) 0.13054(3) 0.04839(9) Uani d 1 . . I I2 0.06519(4) 0.44189(2) 0.91487(3) 0.04368(9) Uani d 1 . . N N1 -0.3770(4) 0.2023(3) 0.0555(4) 0.0376(8) Uani d 1 . . C C1 -0.1849(5) 0.2322(4) 0.0948(5) 0.0402(10) Uani d 1 . . H H1A -0.1144 0.1733 0.1019 0.048 Uiso calc 1 . . H H1B -0.1609 0.2719 0.0166 0.048 Uiso calc 1 . . C C2 -0.1311(5) 0.2891(3) 0.2358(5) 0.0409(11) Uani d 1 . . H H2A -0.1888 0.3524 0.2249 0.049 Uiso calc 1 . . H H2B -0.1676 0.2536 0.3124 0.049 Uiso calc 1 . . C C3 0.0613(6) 0.3044(3) 0.2779(5) 0.0382(10) Uani d 1 . . H H3 0.1101 0.3408 0.2143 0.046 Uiso calc 1 . . C C4 0.1686(5) 0.2711(3) 0.3970(4) 0.0329(9) Uani d 1 . . C C5 0.3545(5) 0.3021(3) 0.4380(4) 0.0349(9) Uani d 1 . . C C6 0.4815(6) 0.2388(4) 0.5116(5) 0.0457(11) Uani d 1 . . H H6 0.4514 0.1752 0.5318 0.055 Uiso calc 1 . . C C7 0.6528(6) 0.2687(4) 0.5557(5) 0.0546(13) Uani d 1 . . H H7 0.7362 0.2248 0.6040 0.065 Uiso calc 1 . . C C8 0.7001(6) 0.3612(5) 0.5292(6) 0.0598(15) Uani d 1 . . H H8 0.8148 0.3812 0.5610 0.072 Uiso calc 1 . . C C9 0.5768(7) 0.4253(4) 0.4549(7) 0.0661(16) Uani d 1 . . H H9 0.6087 0.4887 0.4357 0.079 Uiso calc 1 . . C C10 0.4056(6) 0.3959(4) 0.4085(6) 0.0532(13) Uani d 1 . . H H10 0.3239 0.4395 0.3569 0.064 Uiso calc 1 . . C C11 0.1128(5) 0.2030(3) 0.5013(4) 0.0326(9) Uani d 1 . . C C12 0.0439(6) 0.1106(3) 0.4575(5) 0.0422(10) Uani d 1 . . H H12 0.0314 0.0909 0.3616 0.051 Uiso calc 1 . . C C13 -0.0060(6) 0.0480(3) 0.5561(5) 0.0500(12) Uani d 1 . . H H13 -0.0522 -0.0134 0.5258 0.060 Uiso calc 1 . . C C14 0.0124(6) 0.0761(4) 0.6978(5) 0.0523(13) Uani d 1 . . H H14 -0.0198 0.0334 0.7637 0.063 Uiso calc 1 . . C C15 0.0784(6) 0.1674(4) 0.7431(5) 0.0467(12) Uani d 1 . . H H15 0.0883 0.1871 0.8388 0.056 Uiso calc 1 . . C C16 0.1298(5) 0.2295(4) 0.6457(5) 0.0403(10) Uani d 1 . . H H16 0.1768 0.2905 0.6774 0.048 Uiso calc 1 . . C C17 -0.4036(5) 0.1302(3) 0.1685(5) 0.0411(10) Uani d 1 . . H H17A -0.3821 0.1637 0.2614 0.049 Uiso calc 1 . . H H17B -0.3174 0.0787 0.1761 0.049 Uiso calc 1 . . C C18 -0.4928(7) 0.2892(4) 0.0510(7) 0.0633(15) Uani d 1 . . H H18A -0.6106 0.2703 0.0100 0.095 Uiso calc 1 . . H H18B -0.4590 0.3397 -0.0076 0.095 Uiso calc 1 . . H H18C -0.4832 0.3135 0.1478 0.095 Uiso calc 1 . . C C19 -0.4089(7) 0.1546(5) -0.0910(5) 0.0596(14) Uani d 1 . . H H19A -0.5290 0.1369 -0.1218 0.089 Uiso calc 1 . . H H19B -0.3385 0.0967 -0.0855 0.089 Uiso calc 1 . . H H19C -0.3796 0.1997 -0.1596 0.089 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.03965(16) 0.05161(19) 0.05521(18) -0.00709(15) 0.01359(13) -0.00180(15) I2 0.04705(17) 0.03979(15) 0.04515(16) 0.00372(15) 0.01257(12) 0.00767(14) N1 0.0317(17) 0.043(2) 0.0351(19) -0.0020(17) 0.0010(15) 0.0047(16) C1 0.029(2) 0.051(3) 0.039(2) -0.005(2) 0.0042(18) 0.006(2) C2 0.035(2) 0.043(3) 0.042(3) 0.001(2) 0.004(2) -0.001(2) C3 0.038(2) 0.037(2) 0.038(2) -0.004(2) 0.0058(19) 0.003(2) C4 0.034(2) 0.031(2) 0.033(2) -0.0022(18) 0.0073(18) -0.0027(18) C5 0.033(2) 0.037(2) 0.035(2) -0.002(2) 0.0087(18) -0.0047(19) C6 0.037(3) 0.055(3) 0.046(3) 0.003(2) 0.012(2) 0.011(2) C7 0.033(2) 0.083(4) 0.049(3) 0.007(3) 0.010(2) 0.009(3) C8 0.034(3) 0.080(4) 0.065(4) -0.009(3) 0.011(3) -0.014(3) C9 0.049(3) 0.048(4) 0.103(4) -0.019(3) 0.021(3) -0.017(3) C10 0.040(3) 0.037(2) 0.082(4) -0.003(2) 0.012(3) 0.003(3) C11 0.0266(19) 0.035(2) 0.035(2) 0.0031(18) 0.0054(17) 0.0010(18) C12 0.043(2) 0.040(2) 0.045(2) -0.002(2) 0.013(2) -0.004(2) C13 0.054(3) 0.032(3) 0.068(3) -0.001(2) 0.022(2) 0.004(2) C14 0.046(3) 0.054(3) 0.061(3) 0.009(3) 0.019(2) 0.023(3) C15 0.043(3) 0.065(3) 0.031(2) 0.007(3) 0.008(2) 0.007(2) C16 0.031(2) 0.048(3) 0.040(2) -0.004(2) 0.0043(19) -0.004(2) C17 0.035(2) 0.049(3) 0.037(2) -0.005(2) 0.0035(18) 0.005(2) C18 0.041(3) 0.049(3) 0.091(4) 0.009(3) -0.002(3) 0.013(3) C19 0.055(3) 0.084(4) 0.036(3) -0.014(3) 0.003(2) 0.001(3) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 C17 . 2.164(4) ? I1 I2 2_446 3.5640(4) ? N1 C18 . 1.492(6) ? N1 C19 . 1.499(6) ? N1 C17 . 1.502(5) ? N1 C1 . 1.536(5) ? C1 C2 . 1.517(6) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 C3 . 1.499(6) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 C4 . 1.326(6) ? C3 H3 . 0.9300 ? C4 C11 . 1.493(6) ? C4 C5 . 1.495(6) ? C5 C6 . 1.385(6) ? C5 C10 . 1.388(6) ? C6 C7 . 1.387(7) ? C6 H6 . 0.9300 ? C7 C8 . 1.353(8) ? C7 H7 . 0.9300 ? C8 C9 . 1.376(8) ? C8 H8 . 0.9300 ? C9 C10 . 1.386(7) ? C9 H9 . 0.9300 ? C10 H10 . 0.9300 ? C11 C16 . 1.390(6) ? C11 C12 . 1.396(6) ? C12 C13 . 1.387(6) ? C12 H12 . 0.9300 ? C13 C14 . 1.370(7) ? C13 H13 . 0.9300 ? C14 C15 . 1.379(7) ? C14 H14 . 0.9300 ? C15 C16 . 1.379(6) ? C15 H15 . 0.9300 ? C16 H16 . 0.9300 ? C17 H17A . 0.9700 ? C17 H17B . 0.9700 ? C18 H18A . 0.9600 ? C18 H18B . 0.9600 ? C18 H18C . 0.9600 ? C19 H19A . 0.9600 ? C19 H19B . 0.9600 ? C19 H19C . 0.9600 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C17 I1 I2 . 2_446 176.81(12) ? C18 N1 C19 . . 110.2(4) ? C18 N1 C17 . . 110.7(4) ? C19 N1 C17 . . 110.7(4) ? C18 N1 C1 . . 111.4(4) ? C19 N1 C1 . . 106.6(3) ? C17 N1 C1 . . 107.1(3) ? C2 C1 N1 . . 114.2(3) ? C2 C1 H1A . . 108.7 ? N1 C1 H1A . . 108.7 ? C2 C1 H1B . . 108.7 ? N1 C1 H1B . . 108.7 ? H1A C1 H1B . . 107.6 ? C3 C2 C1 . . 111.6(4) ? C3 C2 H2A . . 109.3 ? C1 C2 H2A . . 109.3 ? C3 C2 H2B . . 109.3 ? C1 C2 H2B . . 109.3 ? H2A C2 H2B . . 108.0 ? C4 C3 C2 . . 126.3(4) ? C4 C3 H3 . . 116.8 ? C2 C3 H3 . . 116.8 ? C3 C4 C11 . . 123.0(4) ? C3 C4 C5 . . 121.6(4) ? C11 C4 C5 . . 115.3(3) ? C6 C5 C10 . . 117.5(4) ? C6 C5 C4 . . 120.9(4) ? C10 C5 C4 . . 121.6(4) ? C5 C6 C7 . . 121.1(5) ? C5 C6 H6 . . 119.4 ? C7 C6 H6 . . 119.4 ? C8 C7 C6 . . 120.7(5) ? C8 C7 H7 . . 119.6 ? C6 C7 H7 . . 119.6 ? C7 C8 C9 . . 119.4(5) ? C7 C8 H8 . . 120.3 ? C9 C8 H8 . . 120.3 ? C8 C9 C10 . . 120.5(5) ? C8 C9 H9 . . 119.8 ? C10 C9 H9 . . 119.8 ? C9 C10 C5 . . 120.8(5) ? C9 C10 H10 . . 119.6 ? C5 C10 H10 . . 119.6 ? C16 C11 C12 . . 118.0(4) ? C16 C11 C4 . . 120.8(4) ? C12 C11 C4 . . 121.2(4) ? C13 C12 C11 . . 120.5(4) ? C13 C12 H12 . . 119.8 ? C11 C12 H12 . . 119.8 ? C14 C13 C12 . . 120.3(5) ? C14 C13 H13 . . 119.9 ? C12 C13 H13 . . 119.9 ? C13 C14 C15 . . 120.2(4) ? C13 C14 H14 . . 119.9 ? C15 C14 H14 . . 119.9 ? C14 C15 C16 . . 119.7(4) ? C14 C15 H15 . . 120.2 ? C16 C15 H15 . . 120.2 ? C15 C16 C11 . . 121.4(4) ? C15 C16 H16 . . 119.3 ? C11 C16 H16 . . 119.3 ? N1 C17 I1 . . 116.0(3) ? N1 C17 H17A . . 108.3 ? I1 C17 H17A . . 108.3 ? N1 C17 H17B . . 108.3 ? I1 C17 H17B . . 108.3 ? H17A C17 H17B . . 107.4 ? N1 C18 H18A . . 109.5 ? N1 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? N1 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? N1 C19 H19A . . 109.5 ? N1 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? N1 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C18 N1 C1 C2 . . . . 55.2(5) ? C19 N1 C1 C2 . . . . 175.5(4) ? C17 N1 C1 C2 . . . . -65.9(5) ? N1 C1 C2 C3 . . . . 172.5(4) ? C1 C2 C3 C4 . . . . -117.9(5) ? C2 C3 C4 C11 . . . . 6.6(7) ? C2 C3 C4 C5 . . . . -171.6(4) ? C3 C4 C5 C6 . . . . -148.1(5) ? C11 C4 C5 C6 . . . . 33.5(5) ? C3 C4 C5 C10 . . . . 34.0(6) ? C11 C4 C5 C10 . . . . -144.3(4) ? C10 C5 C6 C7 . . . . 0.9(7) ? C4 C5 C6 C7 . . . . -177.0(4) ? C5 C6 C7 C8 . . . . 0.7(7) ? C6 C7 C8 C9 . . . . -1.4(8) ? C7 C8 C9 C10 . . . . 0.5(9) ? C8 C9 C10 C5 . . . . 1.1(9) ? C6 C5 C10 C9 . . . . -1.8(8) ? C4 C5 C10 C9 . . . . 176.1(5) ? C3 C4 C11 C16 . . . . -120.5(5) ? C5 C4 C11 C16 . . . . 57.8(5) ? C3 C4 C11 C12 . . . . 60.2(6) ? C5 C4 C11 C12 . . . . -121.5(4) ? C16 C11 C12 C13 . . . . 0.2(6) ? C4 C11 C12 C13 . . . . 179.5(4) ? C11 C12 C13 C14 . . . . -0.3(7) ? C12 C13 C14 C15 . . . . 0.9(7) ? C13 C14 C15 C16 . . . . -1.5(7) ? C14 C15 C16 C11 . . . . 1.5(7) ? C12 C11 C16 C15 . . . . -0.8(6) ? C4 C11 C16 C15 . . . . 179.9(4) ? C18 N1 C17 I1 . . . . 64.6(4) ? C19 N1 C17 I1 . . . . -57.9(4) ? C1 N1 C17 I1 . . . . -173.8(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C17 H17B I2 2_546 0.97 3.00 3.919(5) 159 C7 H7 Cg 1_655 0.93 2.84 3.030(5) 143 _shelx_hkl_file ; 1 0 0 49.26 1.22 1 0 0 47.54 1.23 -1 0 0 46.82 1.23 2 0 0 199.54 4.85 2 0 0 194.44 4.86 -2 0 0 196.68 4.87 -2 0 0 194.96 4.86 3 0 0 376.16 9.19 -3 0 0 373.47 9.19 3 0 0 374.02 9.19 -4 0 0 196.90 5.02 4 0 0 196.14 4.96 -5 0 0 23.33 0.89 5 0 0 22.46 0.80 -6 0 0 7.30 0.49 6 0 0 7.83 0.44 7 0 0 90.98 2.61 -7 0 0 91.07 2.74 -8 0 0 10.49 0.71 -9 0 0 -0.05 0.16 0 -1 0 0.20 0.03 1 -1 0 94.55 2.25 1 -1 0 91.24 2.18 -1 -1 0 91.19 2.23 1 1 0 87.50 2.22 -1 1 0 86.85 2.25 1 1 0 86.63 2.25 2 -1 0 479.15 11.70 -2 -1 0 512.42 11.72 2 1 0 474.26 11.78 -2 1 0 485.23 11.73 2 1 0 465.49 11.70 3 -1 0 177.12 4.26 -3 1 0 169.84 4.35 3 1 0 171.28 4.32 3 1 0 166.91 4.33 -4 -1 0 107.34 2.73 4 -1 0 102.63 2.63 4 1 0 99.72 2.70 4 1 0 98.88 2.71 -4 1 0 97.58 2.74 -5 -1 0 223.89 5.56 5 -1 0 215.15 5.45 -5 1 0 207.59 5.57 5 1 0 215.97 5.53 -6 -1 0 9.63 0.57 6 -1 0 9.66 0.48 -6 1 0 10.76 0.62 6 1 0 10.64 0.54 7 -1 0 12.28 0.59 -7 -1 0 11.89 0.68 -7 1 0 11.32 0.70 7 1 0 11.51 0.63 -8 -1 0 19.20 0.97 -8 1 0 21.01 1.03 8 1 0 19.98 0.91 -9 -1 0 8.89 0.68 -9 1 0 10.10 0.74 0 -2 0 79.20 2.24 0 2 0 97.21 2.24 0 2 0 93.89 2.25 -1 -2 0 190.84 4.76 1 2 0 196.30 4.81 1 2 0 195.86 4.75 -2 -2 0 75.46 2.01 2 -2 0 75.54 1.90 2 2 0 78.33 2.05 2 2 0 78.28 2.00 -2 2 0 79.75 2.06 3 -2 0 432.28 10.40 3 2 0 426.85 10.56 -3 2 0 426.32 10.53 3 2 0 426.55 10.46 4 -2 0 23.92 0.78 4 2 0 28.76 0.91 4 2 0 28.12 0.93 -4 2 0 27.06 0.95 -5 -2 0 10.89 0.54 5 -2 0 11.61 0.44 5 2 0 8.87 0.50 -5 2 0 9.59 0.55 5 2 0 9.70 0.51 -6 -2 0 58.11 1.85 6 -2 0 59.98 1.70 -6 2 0 59.01 1.92 6 2 0 61.61 1.87 -7 -2 0 31.37 1.22 -7 2 0 31.53 1.29 7 2 0 31.62 1.21 -8 -2 0 18.91 0.94 -8 2 0 18.22 0.99 8 2 0 18.60 0.91 -9 2 0 14.10 0.91 0 -3 0 -0.41 0.07 0 3 0 -0.46 0.05 0 3 0 -0.40 0.08 -1 -3 0 305.93 7.57 -1 3 0 315.06 7.52 1 3 0 299.81 7.57 1 3 0 314.92 7.64 -1 3 0 316.46 7.61 -2 -3 0 310.76 7.62 -2 3 0 310.37 7.67 2 3 0 311.49 7.70 2 3 0 310.37 7.60 3 3 0 142.04 3.62 -3 3 0 146.69 3.48 3 3 0 142.74 3.71 -3 3 0 136.85 3.71 4 -3 0 324.24 7.83 4 3 0 328.81 7.98 -4 3 0 320.45 7.83 -4 3 0 313.01 8.06 4 3 0 317.67 8.07 5 -3 0 58.67 1.54 -5 3 0 55.23 1.79 -5 3 0 56.68 1.53 5 3 0 55.88 1.75 5 3 0 55.95 1.69 -6 -3 0 63.84 1.90 6 3 0 61.42 1.87 6 3 0 60.11 1.92 -6 3 0 59.18 1.97 -7 -3 0 20.86 0.92 7 3 0 21.25 0.95 -7 3 0 19.83 0.98 -8 -3 0 17.67 0.90 8 3 0 18.81 0.93 -8 3 0 16.90 0.96 9 3 0 2.22 0.43 -9 3 0 2.11 0.42 0 4 0 22.24 0.69 0 4 0 22.60 0.73 -1 -4 0 305.80 7.76 -1 4 0 326.31 7.66 -1 4 0 323.05 7.76 1 4 0 307.43 7.72 1 4 0 310.69 7.77 2 4 0 180.25 4.49 2 4 0 176.86 4.59 -2 4 0 182.02 4.58 3 4 0 126.48 3.20 -3 4 0 121.61 3.31 3 4 0 124.65 3.32 4 4 0 9.92 0.52 4 4 0 9.64 0.45 -4 4 0 9.44 0.53 -5 4 0 4.11 0.38 5 4 0 4.07 0.36 5 4 0 4.43 0.33 6 4 0 182.47 4.92 -6 4 0 179.91 4.96 6 4 0 183.17 4.79 -7 -4 0 2.35 0.34 7 4 0 2.78 0.33 -7 4 0 2.87 0.44 7 4 0 2.55 0.38 8 4 0 12.80 0.77 -8 4 0 10.26 0.76 -9 4 0 20.19 1.14 0 5 0 -0.13 0.08 0 5 0 -0.06 0.06 -1 5 0 299.31 7.23 1 5 0 286.12 7.30 -1 5 0 301.36 7.35 1 5 0 296.00 7.36 2 5 0 69.84 1.91 2 5 0 71.43 2.00 3 5 0 155.02 3.98 3 5 0 151.83 4.11 -3 5 0 161.05 4.13 4 5 0 192.95 5.03 -4 5 0 200.73 5.22 4 5 0 201.50 5.21 -5 5 0 16.45 0.81 5 5 0 15.89 0.78 5 5 0 18.11 0.71 6 5 0 26.31 1.11 6 5 0 26.79 0.99 -6 5 0 26.24 1.15 -7 -5 0 13.86 0.74 7 5 0 15.44 0.74 7 5 0 15.47 0.84 -7 5 0 15.45 0.88 8 5 0 12.55 0.80 -8 5 0 11.90 0.84 0 6 0 409.56 9.90 0 6 0 394.78 9.91 1 6 0 167.74 4.39 -1 6 0 175.66 4.30 -1 6 0 171.95 4.44 1 6 0 172.07 4.42 2 -6 0 109.95 2.71 -2 6 0 108.84 2.98 2 6 0 107.40 2.88 2 6 0 110.90 2.97 3 6 0 85.34 2.32 -3 6 0 85.72 2.47 4 6 0 23.77 0.97 4 6 0 25.24 0.87 -4 6 0 23.73 0.99 5 6 0 9.63 0.60 -5 6 0 8.84 0.61 5 6 0 10.03 0.50 6 6 0 62.42 2.04 6 6 0 59.30 1.84 -6 6 0 59.67 2.05 7 6 0 19.41 0.93 7 6 0 20.01 1.01 -7 6 0 21.29 1.09 8 6 0 13.67 0.88 -8 6 0 13.85 0.92 0 7 0 0.04 0.08 0 7 0 -0.12 0.09 1 7 0 59.01 1.71 1 7 0 58.78 1.71 -1 7 0 57.85 1.58 -1 7 0 56.88 1.73 2 -7 0 193.24 4.77 2 7 0 193.73 5.04 -2 7 0 193.63 5.05 2 7 0 194.02 4.95 3 7 0 41.89 1.30 3 7 0 41.74 1.42 -3 7 0 42.61 1.45 4 7 0 58.84 1.74 4 7 0 59.70 1.92 -4 7 0 60.04 1.93 5 7 0 104.88 3.10 5 7 0 104.65 2.87 -5 7 0 104.14 3.11 -6 7 0 17.12 0.92 6 7 0 15.49 0.86 6 7 0 15.67 0.72 -7 7 0 1.02 0.29 7 7 0 0.37 0.22 8 7 0 13.39 0.90 -8 7 0 13.96 0.95 0 8 0 423.62 10.61 0 8 0 428.89 10.56 -1 8 0 43.81 1.45 -1 8 0 44.19 1.29 1 8 0 44.67 1.40 1 8 0 44.78 1.42 2 -8 0 21.80 0.67 2 8 0 23.26 0.90 2 8 0 22.30 0.85 -2 8 0 22.37 0.68 3 8 0 149.63 3.88 -3 8 0 144.68 4.03 3 8 0 145.11 4.02 -4 8 0 29.03 1.21 4 8 0 30.99 1.21 4 8 0 29.13 1.03 5 8 0 20.20 0.98 -5 8 0 19.30 0.99 5 8 0 20.83 0.82 6 8 0 0.36 0.18 -6 8 0 0.54 0.24 -7 8 0 44.34 1.81 7 8 0 44.60 1.78 8 8 0 5.17 0.58 -8 8 0 6.00 0.66 0 9 0 0.09 0.12 0 9 0 0.01 0.08 1 9 0 26.56 1.03 1 9 0 26.73 1.01 -1 9 0 27.80 0.91 -1 9 0 29.11 1.08 2 -9 0 190.62 4.78 2 9 0 192.25 5.08 -2 9 0 184.38 5.08 2 9 0 190.92 5.00 -2 9 0 197.03 4.80 3 9 0 36.44 1.23 -3 9 0 35.93 1.37 3 9 0 36.15 1.35 4 9 0 30.32 1.08 4 9 0 30.21 1.24 -4 9 0 31.34 1.28 5 9 0 85.33 2.44 5 9 0 83.21 2.68 -5 9 0 84.03 2.73 -6 9 0 1.26 0.34 6 9 0 2.03 0.39 -7 9 0 2.92 0.51 7 9 0 2.75 0.50 0 10 0 119.02 3.22 0 10 0 117.35 3.34 -1 10 0 40.09 1.46 1 10 0 40.60 1.40 1 10 0 42.19 1.44 -1 10 0 42.94 1.30 2 -10 0 29.99 0.91 -2 10 0 29.38 0.94 2 10 0 27.66 1.12 2 10 0 29.65 1.11 -2 10 0 29.84 1.20 3 10 0 40.19 1.49 3 10 0 40.98 1.37 -3 10 0 40.19 1.52 4 10 0 7.82 0.61 4 10 0 8.81 0.51 -4 10 0 8.94 0.65 -5 10 0 4.98 0.53 5 10 0 4.79 0.51 6 10 0 19.51 1.07 -6 10 0 20.13 1.12 7 10 0 13.32 0.92 -7 10 0 14.47 1.00 0 11 0 0.05 0.12 0 11 0 -0.12 0.16 1 11 0 36.15 1.29 -1 11 0 35.61 1.17 -1 11 0 33.67 1.34 1 11 0 35.75 1.33 -2 11 0 33.61 1.38 2 11 0 36.37 1.35 2 11 0 35.65 1.30 3 11 0 25.71 1.01 -3 11 0 24.99 1.14 3 11 0 23.95 1.10 4 11 0 45.41 1.53 4 11 0 44.48 1.72 -4 11 0 47.90 1.78 5 11 0 17.91 1.01 -5 11 0 18.33 1.04 6 11 0 5.63 0.60 -6 11 0 6.91 0.66 0 12 0 14.30 0.71 0 12 0 14.03 0.79 1 12 0 71.27 2.20 -1 12 0 68.40 2.04 1 12 0 69.35 2.23 -1 12 0 68.90 2.28 2 12 0 26.29 1.14 2 12 0 26.23 1.11 -2 12 0 27.98 1.22 3 12 0 7.88 0.62 -3 12 0 7.71 0.65 3 12 0 7.30 0.51 -4 12 0 9.33 0.72 4 12 0 7.89 0.67 -5 12 0 2.12 0.44 5 12 0 2.04 0.44 -6 12 0 21.01 1.21 6 12 0 19.63 1.16 0 13 0 -0.01 0.17 0 13 0 -0.16 0.11 1 13 0 26.90 1.13 1 13 0 25.43 1.14 -1 13 0 25.26 1.19 2 13 0 6.17 0.53 2 13 0 6.69 0.56 -2 13 0 6.68 0.60 -3 13 0 16.80 1.00 3 13 0 18.41 1.00 4 13 0 37.78 1.62 -4 13 0 37.84 1.66 5 13 0 1.29 0.40 -5 13 0 1.12 0.37 0 14 0 25.26 1.07 0 14 0 25.52 1.21 -1 14 0 25.95 1.26 1 14 0 27.12 1.22 1 14 0 27.83 1.18 -2 14 0 10.54 0.80 2 14 0 11.65 0.73 2 14 0 11.95 0.78 -3 14 0 6.87 0.69 3 14 0 8.12 0.69 -4 14 0 4.35 0.64 4 14 0 4.89 0.60 0 15 0 0.07 0.23 -1 15 0 7.31 0.68 1 15 0 7.42 0.59 1 15 0 6.30 0.63 -2 15 0 11.96 0.90 2 15 0 10.80 0.76 3 15 0 12.64 0.89 -3 15 0 16.57 1.04 0 16 0 26.31 1.33 1 16 0 2.46 0.46 -1 16 0 2.29 0.49 -2 16 0 1.24 0.42 2 16 0 1.44 0.36 -9 0 1 1.41 0.36 -8 0 1 45.82 1.72 -7 0 1 39.01 1.46 7 0 -1 38.54 1.32 -7 0 1 38.85 1.33 6 0 -1 -0.05 0.09 -6 0 1 0.12 0.11 -6 0 1 -0.12 0.10 5 0 -1 202.80 5.28 -5 0 1 200.10 5.28 5 0 -1 206.92 5.19 4 0 -1 17.97 0.65 4 0 -1 19.35 0.73 3 0 -1 12.58 0.45 -3 0 1 11.77 0.45 2 0 -1 336.39 8.17 -2 0 1 331.09 8.16 -1 0 1 51.60 1.33 -1 0 1 49.99 1.31 1 0 -1 50.38 1.33 0 0 1 267.33 6.38 0 0 -1 254.91 6.31 1 0 1 7.36 0.28 1 0 1 8.72 0.31 -1 0 -1 7.49 0.28 2 0 1 496.83 12.32 -2 0 -1 515.09 12.25 3 0 1 250.18 6.16 -3 0 -1 244.40 6.13 -4 0 -1 57.65 1.68 4 0 1 58.79 1.65 5 0 1 34.82 1.14 -5 0 -1 35.69 1.19 6 0 1 2.03 0.24 -6 0 -1 1.79 0.30 7 0 1 97.53 2.80 -7 0 -1 98.03 2.89 -8 0 -1 0.02 0.15 -9 -1 1 4.37 0.51 -9 1 1 4.87 0.53 -8 -1 1 3.65 0.49 -8 -1 1 3.91 0.41 -8 1 1 4.03 0.48 8 1 -1 4.14 0.42 -7 -1 1 55.27 1.89 -7 -1 1 55.62 1.80 -7 1 1 55.91 1.73 7 1 -1 57.34 1.80 -7 1 1 58.24 1.93 -6 -1 1 17.58 0.83 6 1 -1 18.46 0.76 -6 1 1 19.19 0.86 6 1 -1 18.66 0.83 -6 1 1 17.71 0.71 5 -1 -1 89.53 2.37 5 1 -1 86.34 2.48 -5 1 1 88.72 2.52 5 1 -1 87.29 2.42 -5 1 1 85.48 2.35 4 -1 -1 153.67 4.06 -4 1 1 158.76 4.07 4 1 -1 156.73 4.04 4 1 -1 153.98 4.00 -4 1 1 153.99 3.94 3 -1 -1 462.55 11.58 -3 1 1 480.66 11.59 -3 1 1 482.00 11.53 3 1 -1 477.66 11.59 3 1 -1 461.53 11.56 2 -1 -1 266.74 6.41 2 1 -1 255.41 6.39 2 1 -1 258.07 6.41 -2 1 1 257.93 6.35 -1 -1 1 41.37 1.09 1 -1 -1 39.22 1.08 -1 1 1 40.00 1.06 -1 1 1 41.77 1.09 1 1 -1 39.25 1.09 0 -1 -1 241.70 6.55 0 -1 1 290.15 6.63 0 -1 1 282.27 6.64 0 1 1 294.92 6.66 0 1 -1 276.51 6.62 0 1 1 250.49 6.55 -1 -1 -1 67.97 1.64 1 -1 1 66.58 1.72 -1 -1 -1 67.19 1.64 1 -1 1 67.91 1.70 -1 1 -1 62.29 1.71 1 1 1 64.28 1.74 2 -1 1 398.60 9.66 -2 -1 -1 391.07 9.60 -2 -1 -1 392.92 9.61 2 1 1 401.42 9.72 -2 1 -1 397.17 9.66 -3 -1 -1 0.41 0.10 3 -1 1 0.22 0.08 -3 1 -1 0.22 0.10 3 1 1 0.12 0.08 -4 -1 -1 112.35 2.99 4 -1 1 114.99 2.96 -4 1 -1 113.61 3.05 4 1 1 114.01 3.04 -5 -1 -1 227.59 5.70 5 -1 1 227.37 5.65 5 1 1 220.42 5.72 -5 1 -1 214.90 5.73 6 -1 1 18.43 0.72 -6 -1 -1 17.49 0.78 6 1 1 17.58 0.77 -6 1 -1 18.12 0.83 -7 -1 -1 20.41 0.91 7 1 1 19.57 0.87 -7 1 -1 20.20 0.94 -8 -1 -1 20.42 0.97 -8 1 -1 19.25 0.99 -9 1 -1 6.12 0.59 -9 -2 1 14.68 0.88 -9 2 1 13.06 0.88 -8 -2 1 18.36 0.92 -8 -2 1 18.06 0.95 8 2 -1 20.76 0.94 -8 2 1 18.17 0.99 -7 -2 1 43.19 1.55 7 2 -1 42.81 1.53 7 2 -1 44.50 1.52 -7 2 1 43.81 1.62 6 2 -1 59.60 1.85 -6 2 1 59.78 1.95 6 2 -1 58.71 1.87 -6 2 1 61.79 1.72 -5 2 1 221.05 5.54 5 2 -1 218.35 5.68 5 2 -1 222.10 5.69 -5 2 1 223.05 5.75 -4 2 1 56.22 1.71 4 2 -1 57.85 1.68 4 2 -1 57.87 1.68 -4 2 1 57.21 1.54 3 2 -1 110.98 2.90 3 2 -1 111.29 2.92 -3 2 1 110.65 2.93 -3 2 1 110.63 2.79 2 2 -1 323.85 8.26 -2 2 1 341.08 8.24 -2 2 1 338.49 8.16 2 2 -1 336.87 8.23 -1 -2 1 439.19 10.44 1 -2 -1 453.66 10.40 -1 -2 1 449.86 10.48 -1 2 1 393.69 10.41 1 2 -1 414.70 10.43 -1 2 1 427.49 10.40 -1 2 1 426.89 10.40 0 -2 -1 358.80 9.08 0 -2 1 389.57 9.18 0 -2 1 387.72 9.18 0 2 1 392.80 9.20 0 2 1 358.02 9.08 -1 -2 -1 556.51 14.39 1 -2 1 590.21 14.52 1 2 1 693.64 14.61 -1 2 -1 617.92 14.51 1 2 1 543.09 14.38 -2 -2 -1 181.53 4.22 2 -2 1 181.96 4.22 2 2 1 162.74 4.20 2 2 1 165.20 4.34 -2 2 -1 163.07 4.31 -3 -2 -1 99.04 2.71 3 -2 1 102.72 2.69 -3 2 -1 108.97 2.83 3 2 1 109.52 2.72 3 2 1 111.52 2.84 4 -2 1 188.33 4.68 -4 -2 -1 185.64 4.73 -4 2 -1 185.12 4.84 4 2 1 188.49 4.84 -5 -2 -1 24.20 0.90 5 -2 1 25.82 0.84 -5 2 -1 26.83 1.01 5 2 1 26.97 0.97 6 -2 1 12.52 0.54 -6 -2 -1 12.88 0.63 6 2 1 12.42 0.65 -6 2 -1 11.15 0.65 -7 -2 -1 33.28 1.27 -7 2 -1 36.03 1.38 7 2 1 36.07 1.33 -8 2 -1 11.76 0.76 8 2 1 12.79 0.74 -9 -3 1 10.09 0.73 -9 -3 1 10.59 0.74 -9 3 1 9.68 0.78 9 3 -1 10.54 0.74 -8 -3 1 24.26 1.11 -8 -3 1 24.29 1.11 8 3 -1 25.97 1.11 -8 3 1 24.40 1.19 7 3 -1 27.16 1.10 -7 3 1 25.93 1.17 7 3 -1 27.28 1.10 6 3 -1 4.72 0.41 -6 3 1 5.10 0.46 6 3 -1 5.23 0.42 -5 3 1 7.76 0.34 5 3 -1 7.74 0.47 5 3 -1 8.09 0.47 4 3 -1 283.32 7.07 -4 3 1 270.92 7.12 4 3 -1 284.21 7.14 -4 3 1 287.89 6.91 3 3 -1 38.67 1.21 -3 3 1 39.76 1.23 -3 3 1 38.65 1.04 3 3 -1 40.44 1.19 2 3 -1 251.19 6.28 -2 3 1 257.79 6.18 2 3 -1 248.84 6.32 -2 3 1 254.78 6.29 1 3 -1 959.53 21.84 -1 3 1 906.24 21.70 -1 3 1 866.53 21.76 1 3 -1 869.65 21.73 0 -3 1 173.70 4.22 0 -3 -1 173.81 4.17 0 3 1 168.98 4.24 0 3 -1 165.80 4.26 0 3 1 168.37 4.17 1 -3 1 62.15 1.57 -1 -3 -1 62.09 1.55 1 3 1 60.83 1.68 1 3 1 60.38 1.55 2 -3 1 81.29 2.00 -2 -3 -1 82.06 2.03 -2 3 -1 78.05 2.16 2 3 1 80.12 2.02 2 3 1 76.33 2.16 3 -3 1 304.26 7.19 -3 3 -1 289.13 7.37 3 3 1 291.38 7.40 3 3 1 292.83 7.22 4 -3 1 40.66 1.18 4 3 1 45.30 1.28 4 3 1 44.06 1.40 -4 3 -1 44.66 1.41 -5 -3 -1 54.97 1.65 5 -3 1 54.76 1.53 -5 3 -1 57.52 1.79 5 3 1 57.78 1.77 -6 -3 -1 67.07 2.00 6 3 1 68.00 2.10 -6 3 -1 66.28 2.13 -7 -3 -1 14.48 0.72 -7 3 -1 14.49 0.81 7 3 1 15.15 0.78 8 3 1 4.48 0.46 -8 3 -1 3.55 0.50 -9 -4 1 18.63 1.04 -9 4 1 20.02 1.14 9 4 -1 19.65 1.04 -8 -4 1 1.02 0.29 8 4 -1 0.89 0.26 -8 4 1 1.12 0.33 8 4 -1 0.76 0.25 7 4 -1 19.44 0.94 -7 4 1 22.68 1.07 7 4 -1 21.33 0.94 6 4 -1 140.70 3.95 6 4 -1 142.80 3.88 -6 4 1 145.66 4.03 5 4 -1 5.87 0.42 -5 4 1 5.35 0.43 5 4 -1 4.95 0.37 -5 4 1 5.52 0.25 4 4 -1 61.26 1.88 -4 4 1 64.34 1.91 -4 4 1 63.90 1.61 4 4 -1 63.19 1.83 -3 4 1 87.66 2.46 3 4 -1 90.79 2.43 3 4 -1 89.98 2.47 2 4 -1 182.32 4.69 2 4 -1 182.30 4.65 -2 4 1 181.60 4.66 -2 4 1 188.76 4.50 1 4 -1 35.92 1.11 -1 4 1 36.50 1.07 1 4 -1 36.73 1.08 -1 4 1 38.14 1.02 0 -4 1 27.87 0.80 0 -4 -1 27.65 0.78 0 4 -1 27.84 0.80 0 4 1 26.48 0.79 0 4 -1 26.87 0.87 0 4 1 26.69 0.82 1 -4 1 852.92 21.24 -1 -4 -1 831.95 21.12 1 4 1 770.42 21.13 1 4 1 939.41 21.39 -1 4 -1 1000.00 21.30 -2 -4 -1 56.90 1.51 2 -4 1 57.19 1.45 -2 4 -1 56.79 1.66 2 4 1 57.75 1.50 3 4 1 81.35 2.29 -3 4 -1 80.26 2.29 3 4 1 81.07 2.11 4 -4 1 208.62 5.12 4 4 1 210.53 5.25 4 4 1 211.94 5.46 -4 4 -1 205.14 5.44 -5 -4 -1 2.58 0.26 -5 4 -1 2.42 0.34 5 4 1 2.85 0.32 5 4 1 2.77 0.25 -6 -4 -1 9.56 0.54 6 4 1 12.14 0.67 -6 4 -1 10.26 0.66 7 4 1 2.52 0.39 -7 4 -1 2.35 0.38 -8 4 -1 35.27 1.50 8 4 1 34.71 1.44 -9 5 1 4.92 0.60 -8 -5 1 14.66 0.85 8 5 -1 15.37 0.82 8 5 -1 16.17 0.90 -8 5 1 14.25 0.92 -7 5 1 10.14 0.71 7 5 -1 10.32 0.66 7 5 -1 9.66 0.60 6 5 -1 4.39 0.38 6 5 -1 5.15 0.46 -6 5 1 5.41 0.49 -5 5 1 5.30 0.44 5 5 -1 5.74 0.39 5 5 -1 5.43 0.43 4 5 -1 292.64 7.42 4 5 -1 287.76 7.29 -4 5 1 289.77 7.40 3 5 -1 90.28 2.51 3 5 -1 91.17 2.56 -3 5 1 94.65 2.58 2 5 -1 68.21 1.96 2 5 -1 71.69 1.96 -2 5 1 68.70 1.96 -2 5 1 69.10 1.77 1 5 -1 500.68 12.23 -1 5 1 504.93 12.14 -1 5 1 495.77 12.15 1 5 -1 490.73 12.21 0 -5 1 95.69 2.51 0 5 1 97.70 2.52 0 5 -1 98.00 2.61 0 5 1 98.64 2.55 0 5 -1 95.65 2.52 -1 -5 -1 21.95 0.68 1 -5 1 22.29 0.67 1 5 1 22.53 0.78 1 5 1 23.28 0.71 -1 5 -1 22.62 0.81 -2 -5 -1 149.52 3.68 2 -5 1 148.37 3.61 2 5 1 146.54 3.85 2 5 1 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4 27.23 0.98 -2 -2 -4 26.74 0.79 2 2 4 29.63 0.79 2 2 4 28.90 1.04 -2 2 -4 28.06 0.97 -3 -2 -4 78.25 2.05 3 -2 4 81.43 2.27 3 2 4 78.10 2.33 -3 2 -4 77.71 2.23 -4 -2 -4 81.17 2.20 4 -2 4 84.57 2.39 4 2 4 82.65 2.46 -4 2 -4 84.00 2.39 5 -2 4 65.87 1.99 -5 2 -4 66.30 2.03 5 2 4 64.01 2.09 6 2 4 25.98 1.13 -6 2 -4 27.27 1.12 7 2 4 17.73 0.94 -9 -3 4 4.69 0.54 -9 3 4 5.56 0.63 9 3 -4 5.74 0.60 -8 -3 4 14.16 0.83 -8 3 4 13.60 0.89 8 3 -4 14.55 0.87 -7 -3 4 73.38 2.38 -7 3 4 74.09 2.47 7 3 -4 75.87 2.45 6 -3 -4 64.05 2.13 -6 -3 4 65.77 2.09 -6 3 4 64.77 1.94 -6 3 4 65.22 2.14 6 3 -4 65.00 2.12 5 -3 -4 43.05 1.51 -5 -3 4 43.36 1.48 -5 3 4 43.77 1.38 -5 3 4 42.22 1.50 5 3 -4 43.42 1.53 -4 -3 4 151.33 4.03 4 -3 -4 150.35 4.02 -4 3 4 148.24 3.94 4 3 -4 146.62 4.04 3 -3 -4 5.00 0.35 -3 -3 4 4.96 0.36 -3 3 4 4.49 0.34 3 3 -4 4.29 0.36 -2 -3 4 213.95 5.58 2 -3 -4 215.04 5.48 2 3 -4 218.78 5.60 -2 3 4 219.34 5.58 1 -3 -4 153.56 3.93 -1 -3 4 155.34 4.09 1 3 -4 156.09 4.09 -1 3 4 156.95 4.10 0 -3 -4 260.99 6.34 0 -3 4 259.12 6.58 0 3 -4 260.24 6.58 0 3 4 260.56 6.34 0 3 4 254.78 6.62 1 -3 4 213.32 5.40 1 3 4 215.31 5.47 -1 3 -4 201.64 5.37 2 -3 4 76.60 2.12 2 3 4 72.73 2.19 -2 3 -4 72.54 2.13 3 -3 4 81.36 2.27 -3 -3 -4 81.55 2.02 3 3 4 77.23 2.37 -3 3 -4 79.61 2.31 4 -3 4 47.84 1.53 -4 3 -4 50.74 1.62 4 3 4 49.75 1.68 5 -3 4 9.88 0.52 -5 3 -4 8.68 0.59 5 3 4 9.71 0.62 -6 3 -4 2.74 0.40 6 3 4 2.66 0.40 -7 3 -4 0.74 0.28 7 3 4 1.35 0.32 -9 -4 4 34.22 1.51 9 4 -4 34.10 1.51 -9 4 4 32.61 1.57 -8 -4 4 2.75 0.44 -8 4 4 3.38 0.52 8 4 -4 3.22 0.47 -7 -4 4 4.70 0.47 7 4 -4 4.89 0.49 -7 4 4 5.05 0.52 -6 -4 4 28.12 1.16 -6 4 4 27.99 1.19 6 4 -4 28.51 1.18 -6 4 4 27.42 1.01 -5 -4 4 43.56 1.51 5 4 -4 42.30 1.53 -5 4 4 43.81 1.53 -5 4 4 42.97 1.38 -4 -4 4 167.10 4.37 -4 4 4 156.93 4.32 4 4 -4 163.45 4.39 -4 4 4 159.28 4.24 -3 -4 4 3.08 0.31 3 -4 -4 3.08 0.29 -3 4 4 3.34 0.29 -3 4 4 3.09 0.28 3 4 -4 3.16 0.32 -2 -4 4 312.73 7.88 2 -4 -4 315.61 7.76 -2 4 4 307.29 7.86 -2 4 4 312.55 7.75 2 4 -4 309.92 7.89 -1 -4 4 231.69 6.07 1 -4 -4 226.55 5.89 -1 4 4 241.70 5.90 -1 4 4 241.00 6.10 1 4 -4 248.60 6.13 0 -4 4 11.07 0.54 0 4 4 12.49 0.59 0 4 -4 11.78 0.59 0 4 4 12.34 0.40 0 4 4 12.38 0.41 1 -4 4 76.87 2.20 -1 4 -4 78.46 2.25 2 -4 4 2.23 0.25 2 4 4 1.79 0.28 -2 4 -4 2.00 0.29 3 -4 4 138.12 3.64 -3 4 -4 136.62 3.74 3 4 4 135.85 3.80 4 -4 4 0.41 0.14 4 4 4 0.26 0.16 -4 4 -4 0.07 0.16 5 4 4 16.37 0.85 -5 4 -4 16.11 0.83 6 4 4 50.35 1.86 -6 4 -4 52.88 1.85 7 4 4 2.04 0.40 -7 4 -4 1.88 0.38 -8 -5 4 9.37 0.73 -8 5 4 9.54 0.77 8 5 -4 10.19 0.74 -7 -5 4 34.19 1.44 -7 5 4 37.14 1.52 7 5 -4 35.86 1.45 -6 -5 4 63.33 2.07 -6 5 4 60.57 2.06 6 5 -4 58.84 2.04 -5 -5 4 37.18 1.37 -5 5 4 36.75 1.19 -5 5 4 35.67 1.35 5 5 -4 35.55 1.36 -4 -5 4 118.71 3.33 -4 5 4 117.36 3.28 -4 5 4 118.07 3.17 4 5 -4 115.83 3.34 -3 -5 4 33.33 1.20 3 5 -4 32.83 1.23 -3 5 4 34.28 1.16 -3 5 4 33.51 1.11 -2 -5 4 56.01 1.66 -2 5 4 50.16 1.59 -2 5 4 52.99 1.55 2 5 -4 50.78 1.68 -1 -5 4 24.12 0.92 -1 5 4 24.89 0.93 -1 5 4 25.88 0.81 1 5 -4 25.89 1.00 0 -5 4 67.58 2.03 0 5 -4 70.81 2.13 0 5 4 73.16 1.83 0 5 4 71.76 1.84 0 5 4 71.39 2.10 1 -5 4 297.76 7.51 1 5 4 296.86 7.62 -1 5 -4 299.07 7.59 2 -5 4 16.64 0.68 -2 5 -4 15.47 0.75 2 5 4 16.88 0.78 3 -5 4 77.10 2.19 3 5 4 78.32 2.39 -3 5 -4 77.87 2.35 4 -5 4 39.77 1.25 4 5 4 38.29 1.46 -4 5 -4 39.01 1.45 5 5 4 27.81 1.23 -5 5 -4 29.52 1.22 -6 5 -4 0.30 0.24 6 5 4 0.62 0.24 -7 5 -4 1.69 0.37 7 5 4 0.71 0.29 -8 -6 4 7.85 0.71 -8 6 4 10.33 0.77 8 6 -4 8.84 0.70 -7 -6 4 13.08 0.83 -7 6 4 12.65 0.83 7 6 -4 12.77 0.79 -6 -6 4 30.28 1.29 6 6 -4 30.31 1.27 -6 6 4 30.54 1.30 -5 -6 4 14.70 0.79 5 6 -4 14.33 0.78 -5 6 4 13.24 0.75 -4 -6 4 94.21 2.75 4 6 -4 92.50 2.78 -4 6 4 91.28 2.70 -4 6 4 91.85 2.54 -3 -6 4 123.01 3.39 -3 6 4 120.04 3.30 3 6 -4 117.61 3.42 -3 6 4 122.10 3.25 -2 -6 4 127.20 3.50 -2 6 4 128.00 3.44 2 6 -4 127.58 3.57 -2 6 4 128.84 3.40 -1 -6 4 78.48 2.19 -1 6 4 75.36 2.04 1 6 -4 72.19 2.26 -1 6 4 72.74 2.17 0 -6 4 125.53 3.38 0 6 4 127.15 3.16 0 6 -4 120.80 3.48 0 6 4 128.25 3.16 0 6 4 124.64 3.44 1 -6 4 25.43 0.90 1 6 4 23.23 0.98 -1 6 -4 25.26 1.02 2 -6 4 18.59 0.73 -2 6 -4 17.80 0.85 2 6 4 18.06 0.84 3 -6 4 46.84 1.43 -3 6 -4 47.62 1.64 3 6 4 45.62 1.64 -4 6 -4 43.88 1.56 4 6 4 37.51 1.51 5 6 4 25.64 1.16 -5 6 -4 24.32 1.15 -6 6 -4 20.45 1.08 6 6 4 21.79 1.11 -7 6 -4 11.00 0.82 7 6 4 10.69 0.78 -8 -7 4 24.61 1.26 8 7 -4 24.84 1.22 -8 7 4 22.82 1.25 -7 -7 4 15.52 0.94 -7 7 4 14.97 0.92 7 7 -4 14.87 0.88 -6 -7 4 22.63 1.11 -6 7 4 22.88 1.09 6 7 -4 21.95 1.06 -5 -7 4 58.42 2.01 -5 7 4 59.61 1.98 5 7 -4 58.01 2.00 -4 -7 4 17.68 0.85 4 7 -4 16.19 0.85 -4 7 4 16.68 0.67 -4 7 4 17.03 0.81 -3 -7 4 1.41 0.27 -3 7 4 2.51 0.26 3 7 -4 3.02 0.40 -3 7 4 1.55 0.26 -2 -7 4 58.74 1.91 -2 7 4 63.92 1.86 2 7 -4 62.48 2.02 -2 7 4 63.75 1.85 -1 -7 4 77.18 2.30 -1 7 4 81.77 2.19 1 7 -4 79.57 2.44 -1 7 4 79.95 2.32 0 -7 4 66.59 1.91 0 7 -4 64.74 2.05 0 7 4 63.62 1.72 0 7 4 60.19 1.95 1 -7 4 23.48 0.87 -1 7 -4 22.21 1.00 1 7 4 23.60 0.98 2 -7 4 157.50 4.09 -2 7 -4 153.75 4.30 2 7 4 154.28 4.29 3 -7 4 14.70 0.61 3 7 4 13.57 0.78 -3 7 -4 13.00 0.77 4 7 4 8.25 0.62 -4 7 -4 9.51 0.67 -5 7 -4 27.65 1.26 5 7 4 25.00 1.20 6 7 4 8.56 0.69 -6 7 -4 7.57 0.69 -8 -8 4 5.97 0.67 8 8 -4 6.75 0.64 -8 8 4 6.06 0.63 -7 -8 4 18.90 1.08 7 8 -4 18.76 1.02 -7 8 4 19.92 1.08 -6 -8 4 32.64 1.45 6 8 -4 34.95 1.44 -6 8 4 36.55 1.48 -5 -8 4 0.09 0.16 5 8 -4 0.20 0.16 -5 8 4 0.32 0.18 -4 -8 4 9.76 0.63 -4 8 4 8.28 0.57 4 8 -4 9.00 0.63 -3 -8 4 209.03 5.52 -3 8 4 206.14 5.31 3 8 -4 201.29 5.55 -3 8 4 207.15 5.42 -2 -8 4 8.61 0.54 2 8 -4 9.01 0.61 -2 8 4 9.14 0.50 -2 8 4 8.57 0.49 -1 -8 4 10.40 0.58 -1 8 4 12.19 0.54 1 8 -4 10.49 0.68 -1 8 4 12.28 0.62 0 -8 4 98.60 2.75 0 8 -4 94.37 2.91 0 8 4 99.74 2.57 0 8 4 96.18 2.81 1 -8 4 14.75 0.65 -1 8 -4 14.84 0.81 1 8 4 15.15 0.77 2 -8 4 5.60 0.39 -2 8 -4 5.34 0.53 2 8 4 6.25 0.51 3 8 4 7.24 0.57 -3 8 -4 8.04 0.63 4 8 4 42.68 1.64 -4 8 -4 41.22 1.64 -5 8 -4 20.49 1.10 5 8 4 19.64 1.07 -6 8 -4 0.02 0.21 6 8 4 0.38 0.20 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4 -5 141.21 3.90 2 -4 5 1.68 0.27 -2 4 -5 1.63 0.29 2 4 5 1.15 0.26 3 -4 5 34.28 1.21 -3 4 -5 34.09 1.27 4 -4 5 0.82 0.22 -4 4 -5 0.19 0.17 4 4 5 0.31 0.19 5 4 5 42.69 1.65 -5 4 -5 43.29 1.58 -6 4 -5 25.58 1.17 6 4 5 25.74 1.23 7 4 5 0.10 0.21 -8 -5 5 1.16 0.36 -8 5 5 1.38 0.37 8 5 -5 1.50 0.37 -7 -5 5 54.38 1.97 7 5 -5 51.29 1.95 -7 5 5 54.66 1.99 -6 -5 5 2.69 0.43 -6 5 5 2.07 0.36 6 5 -5 1.92 0.36 -5 -5 5 23.25 1.06 -5 5 5 23.74 0.95 5 5 -5 25.33 1.11 -5 5 5 22.76 1.02 -4 -5 5 171.08 4.70 4 5 -5 172.96 4.74 -4 5 5 173.29 4.58 -4 5 5 171.46 4.62 -3 -5 5 11.86 0.63 3 5 -5 10.21 0.64 -3 5 5 11.05 0.58 -3 5 5 11.03 0.57 -2 -5 5 2.89 0.33 -2 5 5 2.36 0.29 -2 5 5 1.90 0.23 2 5 -5 1.56 0.27 -1 -5 5 57.89 1.88 1 5 -5 62.07 1.96 -1 5 5 62.97 1.71 -1 5 5 62.25 1.93 0 -5 5 87.71 2.52 0 5 5 85.84 2.58 0 5 -5 86.04 2.59 0 5 5 89.47 2.24 0 5 5 86.82 2.23 1 -5 5 45.68 1.47 1 5 5 44.32 1.54 -1 5 -5 43.11 1.52 2 -5 5 28.67 1.05 2 5 5 27.65 1.15 -2 5 -5 27.09 1.11 3 -5 5 148.55 3.96 3 5 5 142.76 4.14 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4.37 0.62 -8 7 5 4.67 0.55 -7 -7 5 6.85 0.64 -7 7 5 5.52 0.56 7 7 -5 6.75 0.61 -6 -7 5 47.32 1.80 6 7 -5 46.51 1.78 -6 7 5 46.33 1.75 -5 -7 5 38.85 1.51 5 7 -5 36.91 1.50 -5 7 5 36.80 1.43 -4 -7 5 24.43 1.06 -4 7 5 22.95 0.98 -4 7 5 21.35 0.89 4 7 -5 21.24 1.05 -3 -7 5 64.62 2.11 3 7 -5 65.18 2.19 -3 7 5 67.16 2.03 -3 7 5 68.53 2.04 -2 -7 5 17.57 0.83 2 7 -5 20.01 0.95 -2 7 5 18.61 0.76 -2 7 5 18.73 0.83 -1 -7 5 35.31 1.28 1 7 -5 35.96 1.39 -1 7 5 34.99 1.29 -1 7 5 37.89 1.14 0 -7 5 30.40 1.12 0 7 -5 28.99 1.22 0 7 5 30.44 0.89 0 7 5 29.76 1.18 1 -7 5 44.68 1.51 1 7 5 46.27 1.64 -1 7 -5 49.09 1.69 2 -7 5 88.23 2.56 -2 7 -5 91.17 2.77 2 7 5 89.40 2.76 3 7 5 20.86 1.05 -3 7 -5 23.11 1.08 -4 7 -5 14.14 0.85 4 7 5 13.26 0.83 5 7 5 27.25 1.29 -5 7 -5 26.32 1.27 -6 7 -5 3.59 0.55 6 7 5 3.63 0.57 -7 -8 5 5.90 0.64 7 8 -5 5.76 0.61 -7 8 5 6.83 0.63 -6 -8 5 1.66 0.38 -6 8 5 2.87 0.43 6 8 -5 3.32 0.49 -5 -8 5 18.34 0.98 -5 8 5 18.15 0.92 5 8 -5 18.53 1.00 -4 8 5 6.10 0.48 4 8 -5 6.33 0.55 -4 8 5 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9 8.32 0.71 4 1 -9 7.64 0.62 -4 1 9 8.12 0.68 3 -1 -9 10.28 0.67 -3 -1 9 10.17 0.76 -3 1 9 8.80 0.73 3 1 -9 10.20 0.68 2 -1 -9 15.27 0.76 -2 -1 9 14.20 0.89 -2 1 9 12.83 0.86 2 1 -9 12.60 0.75 1 -1 -9 55.95 1.82 -1 -1 9 56.05 2.07 -1 1 9 54.44 2.09 1 1 -9 58.78 1.91 0 -1 9 5.18 0.55 0 1 -9 4.63 0.43 0 1 9 5.79 0.59 1 -1 9 15.10 0.95 1 1 9 17.33 1.00 2 -1 9 22.54 1.18 2 1 9 23.85 1.22 3 -1 9 6.90 0.64 3 1 9 3.48 0.55 7 -2 -9 1.08 0.34 -7 -2 9 0.95 0.36 -7 2 9 0.73 0.32 7 2 -9 0.29 0.26 -6 -2 9 5.73 0.63 6 -2 -9 5.81 0.59 -6 2 9 7.80 0.71 6 2 -9 7.73 0.69 -5 -2 9 21.03 1.17 5 -2 -9 23.23 1.14 -5 2 9 22.61 1.16 5 2 -9 20.44 1.11 -4 -2 9 26.37 1.27 4 -2 -9 22.81 1.10 -4 2 9 24.64 1.24 4 2 -9 24.57 1.18 -3 -2 9 31.45 1.43 3 -2 -9 30.44 1.26 -3 2 9 32.52 1.44 3 2 -9 32.80 1.36 2 -2 -9 24.68 1.06 -2 -2 9 26.80 1.28 -2 2 9 26.77 1.29 2 2 -9 29.08 1.20 -1 -2 9 12.89 0.85 1 2 -9 12.58 0.74 -1 2 9 13.45 0.88 0 -2 9 4.11 0.51 0 2 -9 3.83 0.42 0 2 9 3.78 0.55 1 -2 9 12.59 0.83 1 2 9 12.48 0.87 2 -2 9 7.69 0.65 2 2 9 6.85 0.66 3 -2 9 11.25 0.80 3 2 9 10.92 0.82 7 -3 -9 28.81 1.41 -7 -3 9 28.68 1.44 -7 3 9 27.21 1.35 7 3 -9 27.94 1.45 6 -3 -9 5.00 0.57 -6 -3 9 4.96 0.61 6 3 -9 6.23 0.63 -6 3 9 5.08 0.59 5 -3 -9 1.71 0.36 -5 -3 9 0.87 0.31 -5 3 9 1.05 0.33 5 3 -9 1.64 0.39 -4 -3 9 15.62 0.97 4 -3 -9 15.28 0.85 4 3 -9 15.87 0.93 -4 3 9 14.94 0.93 -3 -3 9 10.86 0.80 3 -3 -9 12.37 0.71 3 3 -9 10.99 0.75 -3 3 9 10.52 0.79 -2 -3 9 7.04 0.65 -2 3 9 6.23 0.61 2 3 -9 7.49 0.61 -1 -3 9 4.64 0.54 1 3 -9 5.69 0.52 -1 3 9 5.61 0.59 0 -3 9 58.97 2.16 0 3 -9 59.83 2.03 0 3 9 61.99 2.26 1 -3 9 17.53 0.99 -1 3 -9 16.34 0.88 1 3 9 18.04 1.05 2 -3 9 3.97 0.55 2 3 9 4.93 0.57 3 -3 9 9.88 0.74 3 3 9 10.25 0.81 -6 -4 9 0.80 0.33 6 -4 -9 1.14 0.32 6 4 -9 0.55 0.26 -6 4 9 1.16 0.35 5 -4 -9 32.88 1.43 -5 -4 9 35.02 1.57 5 4 -9 33.46 1.52 -5 4 9 35.82 1.52 4 -4 -9 10.94 0.70 -4 -4 9 10.27 0.79 4 4 -9 9.09 0.73 -4 4 9 11.48 0.81 3 -4 -9 1.53 0.31 -3 -4 9 1.59 0.40 -3 4 9 1.46 0.35 3 4 -9 1.28 0.33 -2 -4 9 50.59 1.96 -2 4 9 53.83 1.99 2 4 -9 49.39 1.87 -1 -4 9 0.43 0.24 1 4 -9 -0.03 0.17 -1 4 9 0.00 0.20 0 -4 9 2.97 0.46 0 4 -9 2.74 0.42 0 4 9 2.91 0.49 1 -4 9 4.22 0.53 -1 4 -9 4.90 0.51 1 4 9 4.55 0.55 2 -4 9 12.87 0.84 2 4 9 15.59 0.97 3 -4 9 10.30 0.76 3 4 9 10.98 0.85 6 -5 -9 2.95 0.49 -6 -5 9 3.91 0.62 -6 5 9 3.25 0.51 6 5 -9 3.15 0.55 -6 5 9 3.22 0.52 -5 -5 9 2.86 0.50 5 -5 -9 2.44 0.41 -5 5 9 3.42 0.49 5 5 -9 2.14 0.45 -5 5 9 2.60 0.47 -4 -5 9 13.56 0.90 4 -5 -9 12.15 0.75 4 5 -9 11.80 0.84 -4 5 9 13.22 0.85 -3 -5 9 21.30 1.13 -3 5 9 20.60 1.11 3 5 -9 20.38 1.10 -2 -5 9 7.74 0.68 2 5 -9 7.43 0.65 -2 5 9 7.68 0.69 -1 -5 9 4.44 0.54 1 5 -9 4.52 0.51 -1 5 9 3.72 0.59 0 -5 9 35.99 1.55 0 5 -9 39.42 1.56 0 5 9 36.09 1.63 1 -5 9 7.53 0.65 -1 5 -9 7.51 0.62 1 5 9 7.78 0.72 2 -5 9 2.74 0.45 -2 5 -9 3.34 0.48 2 5 9 3.78 0.57 3 -5 9 11.18 0.79 3 5 9 10.05 0.85 -6 -6 9 4.87 0.70 6 6 -9 4.26 0.65 -6 6 9 4.52 0.53 -5 -6 9 17.32 1.07 5 6 -9 18.93 1.11 -5 6 9 15.59 0.91 -5 6 9 16.01 0.97 -4 -6 9 11.12 0.83 -4 6 9 11.19 0.72 -4 6 9 10.71 0.78 4 6 -9 10.66 0.81 -3 -6 9 21.92 1.18 3 6 -9 21.28 1.15 -3 6 9 22.99 1.17 -2 -6 9 21.73 1.14 2 6 -9 20.89 1.14 -2 6 9 21.40 1.16 -1 -6 9 11.78 0.81 -1 6 9 10.40 0.83 1 6 -9 10.90 0.78 0 -6 9 4.51 0.54 0 6 -9 3.87 0.54 0 6 9 3.82 0.57 1 -6 9 4.87 0.52 -1 6 -9 4.07 0.56 1 6 9 3.71 0.58 2 -6 9 8.43 0.68 2 6 9 8.45 0.77 -2 6 -9 10.17 0.73 -5 -7 9 7.00 0.71 -5 7 9 6.62 0.57 -5 7 9 5.96 0.62 5 7 -9 5.50 0.66 -4 -7 9 2.67 0.50 -4 7 9 2.94 0.49 4 7 -9 2.33 0.49 -3 -7 9 6.59 0.65 -3 7 9 6.08 0.64 3 7 -9 6.20 0.64 -2 -7 9 5.47 0.60 2 7 -9 5.31 0.59 -2 7 9 5.98 0.62 -1 -7 9 26.71 1.27 -1 7 9 22.46 1.24 1 7 -9 23.21 1.21 0 -7 9 10.03 0.75 0 7 9 10.57 0.82 0 7 -9 10.03 0.77 1 -7 9 6.72 0.63 1 7 9 6.59 0.70 -1 7 -9 7.61 0.70 2 -7 9 10.03 0.75 -2 7 -9 11.24 0.82 2 7 9 10.70 0.88 -5 -8 9 0.76 0.32 5 8 -9 0.33 0.28 -4 -8 9 15.14 1.00 4 8 -9 15.28 1.05 -4 8 9 14.75 0.92 -3 -8 9 23.48 1.24 3 8 -9 22.26 1.24 -3 8 9 20.51 1.14 -2 -8 9 -0.10 0.17 -2 8 9 0.26 0.25 2 8 -9 -0.07 0.20 -1 -8 9 5.58 0.61 1 8 -9 6.37 0.64 -1 8 9 5.11 0.62 0 -8 9 2.78 0.48 0 8 -9 2.87 0.50 0 8 9 2.65 0.51 1 -8 9 10.16 0.76 -1 8 -9 10.83 0.85 1 8 9 9.69 0.84 -4 -9 9 3.68 0.58 4 9 -9 3.06 0.56 -4 9 9 3.04 0.51 -3 -9 9 2.33 0.49 -3 9 9 1.62 0.40 3 9 -9 2.24 0.47 -2 -9 9 4.48 0.62 2 9 -9 2.69 0.50 -2 9 9 3.32 0.54 -1 -9 9 19.12 1.10 -1 9 9 18.49 1.11 1 9 -9 18.58 1.14 0 -9 9 3.46 0.54 0 9 9 2.78 0.53 0 9 -9 2.58 0.50 -2 -10 9 9.43 0.76 2 10 -9 9.80 0.84 -2 10 9 7.93 0.74 6 0 -10 0.23 0.21 -6 0 10 0.15 0.26 -5 0 10 0.46 0.31 5 0 -10 0.42 0.25 -4 0 10 30.84 1.49 4 0 -10 32.53 1.40 -3 0 10 4.00 0.58 3 0 -10 4.42 0.47 2 0 -10 -0.07 0.17 -2 0 10 0.16 0.22 -1 0 10 39.46 1.72 0 0 10 0.87 0.33 1 0 10 1.11 0.33 2 0 10 4.21 0.60 -6 -1 10 23.91 1.32 6 -1 -10 25.09 1.30 6 1 -10 23.63 1.27 -6 1 10 23.77 1.30 5 -1 -10 5.21 0.57 -5 -1 10 5.06 0.70 -5 1 10 3.43 0.57 5 1 -10 4.55 0.54 4 -1 -10 1.90 0.38 -4 -1 10 2.98 0.56 4 1 -10 2.26 0.42 -4 1 10 1.54 0.41 -3 -1 10 12.88 0.92 3 -1 -10 13.68 0.81 3 1 -10 13.53 0.84 -3 1 10 14.32 0.96 -2 -1 10 6.20 0.65 -2 1 10 5.56 0.64 2 1 -10 4.87 0.50 -1 -1 10 5.16 0.70 -1 1 10 4.37 0.63 0 -1 10 4.86 0.57 0 1 10 5.18 0.60 1 -1 10 21.36 1.20 1 1 10 23.77 1.27 2 -1 10 7.67 0.70 2 1 10 7.58 0.71 -6 -2 10 -0.05 0.21 6 -2 -10 0.06 0.21 6 2 -10 0.14 0.24 -6 2 10 -0.12 0.21 5 -2 -10 6.53 0.63 -5 -2 10 6.87 0.71 5 2 -10 8.50 0.72 -5 2 10 6.96 0.70 -4 -2 10 12.32 0.91 4 -2 -10 11.26 0.77 4 2 -10 11.84 0.82 -4 2 10 12.04 0.89 3 -2 -10 15.75 0.87 -3 -2 10 17.92 1.08 -3 2 10 17.60 1.07 3 2 -10 16.83 0.95 -2 -2 10 18.78 1.11 2 2 -10 17.78 0.97 -2 2 10 18.45 1.10 -1 -2 10 15.37 0.98 1 2 -10 14.00 0.84 -1 2 10 15.35 1.00 0 -2 10 5.96 0.66 0 2 10 5.01 0.60 1 -2 10 5.69 0.60 1 2 10 4.64 0.58 2 -2 10 2.29 0.47 2 2 10 3.08 0.54 -6 -3 10 5.70 0.67 6 -3 -10 5.59 0.61 -6 3 10 4.80 0.68 6 3 -10 4.90 0.68 -5 -3 10 15.32 1.04 5 -3 -10 14.83 0.91 5 3 -10 15.80 1.00 -5 3 10 15.87 1.01 4 -3 -10 8.00 0.64 -4 -3 10 8.07 0.76 4 3 -10 7.43 0.68 -4 3 10 7.76 0.73 -3 -3 10 5.07 0.61 -3 3 10 6.61 0.69 3 3 -10 6.44 0.61 -2 -3 10 9.16 0.76 -2 3 10 7.85 0.73 2 3 -10 7.71 0.66 -1 -3 10 3.62 0.56 -1 3 10 4.42 0.64 1 3 -10 4.24 0.49 0 -3 10 21.17 1.15 0 3 -10 19.09 1.07 0 3 10 19.64 1.16 1 -3 10 5.60 0.60 1 3 10 6.33 0.67 2 -3 10 3.86 0.58 2 3 10 4.25 0.63 5 -4 -10 11.02 0.79 -5 -4 10 12.72 0.94 -5 4 10 11.65 0.87 5 4 -10 10.65 0.84 -4 -4 10 1.09 0.38 4 4 -10 0.80 0.32 -4 4 10 1.08 0.36 -3 -4 10 18.43 1.10 3 4 -10 16.05 0.99 -3 4 10 17.72 1.08 -2 -4 10 36.40 1.64 -2 4 10 36.95 1.67 2 4 -10 36.62 1.56 -1 -4 10 0.32 0.26 1 4 -10 0.37 0.23 -1 4 10 0.62 0.34 0 -4 10 9.50 0.76 0 4 10 8.48 0.78 0 4 -10 9.78 0.72 1 -4 10 2.55 0.46 1 4 10 2.38 0.52 -5 -5 10 15.04 1.05 5 5 -10 13.67 0.98 -5 5 10 14.46 0.97 -5 5 10 16.67 0.94 -4 -5 10 9.34 0.82 4 5 -10 9.16 0.79 -4 5 10 8.46 0.74 -3 -5 10 3.09 0.55 -3 5 10 5.28 0.60 3 5 -10 3.36 0.54 -2 -5 10 2.14 0.45 -2 5 10 3.11 0.53 2 5 -10 2.83 0.48 -1 -5 10 0.85 0.32 1 5 -10 0.76 0.31 -1 5 10 0.47 0.31 0 -5 10 19.64 1.11 0 5 10 18.68 1.17 0 5 -10 18.71 1.04 1 -5 10 3.05 0.53 1 5 10 2.66 0.53 -4 -6 10 9.22 0.80 -4 6 10 9.04 0.78 4 6 -10 8.71 0.78 -3 -6 10 8.47 0.76 3 6 -10 8.25 0.73 -3 6 10 8.11 0.75 -2 -6 10 9.23 0.78 2 6 -10 7.78 0.70 -2 6 10 8.36 0.78 -1 -6 10 13.54 0.92 -1 6 10 13.32 0.96 1 6 -10 12.99 0.90 0 -6 10 3.16 0.53 0 6 -10 2.73 0.47 0 6 10 2.92 0.58 -3 -7 10 8.30 0.77 -3 7 10 7.33 0.74 3 7 -10 6.58 0.70 -2 -7 10 1.30 0.40 2 7 -10 0.81 0.35 -2 7 10 1.38 0.40 -1 -7 10 2.62 0.50 -1 7 10 3.72 0.60 1 7 -10 3.13 0.53 0 -7 10 4.26 0.62 0 7 10 3.78 0.61 0 7 -10 4.51 0.61 -4 0 11 9.15 0.84 4 0 -11 8.24 0.70 -3 0 11 1.19 0.39 -2 0 11 12.95 0.97 -1 0 11 30.64 1.52 0 0 11 1.03 0.35 4 -1 -11 11.34 0.80 -4 -1 11 11.84 0.94 -4 1 11 11.13 0.91 4 1 -11 11.91 0.84 -3 -1 11 10.79 0.90 -3 1 11 9.06 0.83 3 1 -11 9.76 0.74 -2 -1 11 3.54 0.57 -2 1 11 4.05 0.66 -1 -1 11 3.76 0.62 -1 1 11 3.31 0.58 0 -1 11 0.31 0.25 0 1 11 1.07 0.36 -4 -2 11 6.72 0.74 4 2 -11 6.17 0.64 -4 2 11 5.93 0.68 -3 -2 11 5.80 0.67 3 2 -11 4.81 0.55 -3 2 11 4.61 0.68 -2 -2 11 4.58 0.67 2 2 -11 4.85 0.58 -2 2 11 6.41 0.71 -1 -2 11 10.47 0.86 -1 2 11 10.13 0.86 -3 -3 11 0.55 0.29 -3 3 11 1.47 0.41 3 3 -11 1.12 0.34 -2 -3 11 11.72 0.91 2 3 -11 9.77 0.76 -2 3 11 10.34 0.89 -1 -3 11 0.47 0.29 -1 3 11 0.11 0.26 3 4 -11 10.70 0.81 -2 -4 11 4.12 0.65 -2 4 11 4.03 0.65 2 4 -11 4.59 0.57 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 66196 _shelx_res_file ; Compound_I.res created by SHELXL-2014/7 TITL Compound_I CELL 0.71073 7.9254 13.6161 9.4632 90.000 103.320 90.000 ZERR 2.00 0.0002 0.0003 0.0002 0.000 0.001 0.000 LATT -1 SYMM -x, y+1/2, -z SFAC C H N I UNIT 38 46 2 4 OMIT -1 3 1 OMIT 0 -1 2 OMIT 0 1 2 OMIT 1 -4 1 OMIT 1 -2 1 TEMP 25 SIZE 0.122 0.188 0.230 ACTA BOND $H EQIV $7 -1-x, -1/2+y, 1-z BIND I1 I2_$7 EQIV $1 -1+x, y, z HTAB C2 C7_$1 HTAB C2 C8_$1 HTAB C17 C6_$1 HTAB C17 C7_$1 EQIV $2 1+x,y,z HTAB C7 C14_$2 HTAB C7 C15_$2 HTAB C7 C16_$2 EQIV $3 -1+x,y,-1+z HTAB C19 C6_$3 HTAB C19 C7_$3 EQIV $4 1-x, 1/2+y ,1-z HTAB C8 C13_$4 EQIV $5 -x, y-1/2, -z+1 HTAB C1 I2_$5 HTAB C17 I2_$5 HTAB C19 I2_$5 EQIV $6 x, y, z-1 HTAB C1 I2_$6 HTAB C3 I2_$6 MPLA 5 C2 > C5 C11 MPLA 6 C5 > C10 MPLA 6 C11 > C16 L.S. 20 TWIN FMAP 2 PLAN 5 CONF WGHT 0.013800 0.020300 BASF 0.02468 FVAR 0.18750 I1 4 -0.656852 0.062244 0.130545 11.00000 0.03965 0.05161 = 0.05521 -0.00180 0.01359 -0.00709 I2 4 0.065188 0.441892 0.914871 11.00000 0.04705 0.03979 = 0.04515 0.00767 0.01257 0.00372 N1 3 -0.376995 0.202293 0.055545 11.00000 0.03173 0.04277 = 0.03505 0.00468 0.00101 -0.00196 C1 1 -0.184897 0.232164 0.094807 11.00000 0.02919 0.05088 = 0.03871 0.00574 0.00424 -0.00455 AFIX 23 H1A 2 -0.114438 0.173326 0.101911 11.00000 -1.20000 H1B 2 -0.160906 0.271904 0.016640 11.00000 -1.20000 AFIX 0 C2 1 -0.131097 0.289125 0.235773 11.00000 0.03519 0.04293 = 0.04210 -0.00062 0.00409 0.00089 AFIX 23 H2A 2 -0.188824 0.352417 0.224883 11.00000 -1.20000 H2B 2 -0.167569 0.253566 0.312435 11.00000 -1.20000 AFIX 0 C3 1 0.061289 0.304429 0.277881 11.00000 0.03829 0.03737 = 0.03752 0.00314 0.00575 -0.00430 AFIX 43 H3 2 0.110129 0.340817 0.214280 11.00000 -1.20000 AFIX 0 C4 1 0.168585 0.271111 0.397028 11.00000 0.03426 0.03123 = 0.03314 -0.00272 0.00734 -0.00220 C5 1 0.354474 0.302091 0.438042 11.00000 0.03284 0.03715 = 0.03519 -0.00471 0.00868 -0.00198 C6 1 0.481515 0.238810 0.511607 11.00000 0.03748 0.05452 = 0.04624 0.01147 0.01218 0.00349 AFIX 43 H6 2 0.451414 0.175181 0.531770 11.00000 -1.20000 AFIX 0 C7 1 0.652849 0.268726 0.555709 11.00000 0.03266 0.08289 = 0.04873 0.00923 0.01050 0.00688 AFIX 43 H7 2 0.736218 0.224752 0.604023 11.00000 -1.20000 AFIX 0 C8 1 0.700094 0.361163 0.529243 11.00000 0.03372 0.08022 = 0.06535 -0.01412 0.01143 -0.00926 AFIX 43 H8 2 0.814766 0.381208 0.560990 11.00000 -1.20000 AFIX 0 C9 1 0.576816 0.425260 0.454879 11.00000 0.04894 0.04810 = 0.10269 -0.01718 0.02063 -0.01877 AFIX 43 H9 2 0.608670 0.488732 0.435657 11.00000 -1.20000 AFIX 0 C10 1 0.405590 0.395872 0.408460 11.00000 0.04025 0.03672 = 0.08157 0.00291 0.01188 -0.00298 AFIX 43 H10 2 0.323946 0.439528 0.356858 11.00000 -1.20000 AFIX 0 C11 1 0.112801 0.203014 0.501302 11.00000 0.02660 0.03504 = 0.03545 0.00097 0.00541 0.00312 C12 1 0.043897 0.110570 0.457504 11.00000 0.04333 0.03978 = 0.04468 -0.00377 0.01273 -0.00151 AFIX 43 H12 2 0.031400 0.090852 0.361554 11.00000 -1.20000 AFIX 0 C13 1 -0.006031 0.047956 0.556055 11.00000 0.05360 0.03228 = 0.06799 0.00367 0.02208 -0.00134 AFIX 43 H13 2 -0.052211 -0.013369 0.525792 11.00000 -1.20000 AFIX 0 C14 1 0.012388 0.076059 0.697805 11.00000 0.04554 0.05352 = 0.06121 0.02344 0.01904 0.00922 AFIX 43 H14 2 -0.019751 0.033381 0.763723 11.00000 -1.20000 AFIX 0 C15 1 0.078432 0.167428 0.743067 11.00000 0.04349 0.06526 = 0.03116 0.00703 0.00809 0.00723 AFIX 43 H15 2 0.088291 0.187060 0.838755 11.00000 -1.20000 AFIX 0 C16 1 0.129789 0.229549 0.645741 11.00000 0.03118 0.04790 = 0.03979 -0.00415 0.00429 -0.00423 AFIX 43 H16 2 0.176765 0.290462 0.677410 11.00000 -1.20000 AFIX 0 C17 1 -0.403564 0.130167 0.168523 11.00000 0.03465 0.04947 = 0.03687 0.00542 0.00346 -0.00496 AFIX 23 H17A 2 -0.382087 0.163651 0.261432 11.00000 -1.20000 H17B 2 -0.317378 0.078663 0.176134 11.00000 -1.20000 AFIX 0 C18 1 -0.492781 0.289213 0.051041 11.00000 0.04088 0.04936 = 0.09105 0.01276 -0.00233 0.00925 AFIX 137 H18A 2 -0.610589 0.270308 0.010049 11.00000 -1.50000 H18B 2 -0.459001 0.339740 -0.007617 11.00000 -1.50000 H18C 2 -0.483243 0.313511 0.147795 11.00000 -1.50000 AFIX 0 C19 1 -0.408912 0.154608 -0.091027 11.00000 0.05496 0.08412 = 0.03595 0.00063 0.00302 -0.01430 AFIX 137 H19A 2 -0.529037 0.136888 -0.121766 11.00000 -1.50000 H19B 2 -0.338534 0.096726 -0.085532 11.00000 -1.50000 H19C 2 -0.379601 0.199678 -0.159637 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM Compound_I REM R1 = 0.0172 for 3013 Fo > 4sig(Fo) and 0.0178 for all 3085 data REM 202 parameters refined using 1 restraints END WGHT 0.0138 0.0203 REM Highest difference peak 0.265, deepest hole -0.462, 1-sigma level 0.065 Q1 1 -0.5801 0.0505 0.2143 11.00000 0.05 0.27 Q2 1 0.1239 0.0518 0.9554 11.00000 0.05 0.23 Q3 1 -0.0722 -0.0678 0.5404 11.00000 0.05 0.21 Q4 1 0.5622 0.0834 0.4719 11.00000 0.05 0.21 Q5 1 0.1502 0.1204 0.8206 11.00000 0.05 0.21 ; _shelx_res_checksum 48955 data_II _audit_creation_method 'SHELXL-2014/7' _chemical_name_systematic ;\ N-(5,5-Diphenylpent-4-en-1-yl)-N-iodomethyl-N,N-\ dimethylammonium iodide ; _chemical_name_common ? _chemical_formula_moiety 'C20 H25 I N +, I-' _chemical_formula_sum 'C20 H25 I2 N' _chemical_formula_iupac 'C20 H25 I N +, I-' _chemical_formula_weight 533.21 _chemical_melting_point_gt 430 _chemical_melting_point_lt 431 _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_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.778(7) _cell_length_b 6.6323(12) _cell_length_c 17.021(3) _cell_angle_alpha 90 _cell_angle_beta 100.567(4) _cell_angle_gamma 90 _cell_volume 4192.3(13) _cell_formula_units_Z 8 _cell_measurement_reflns_used 4726 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.32 _cell_measurement_temperature 298(2) _exptl_crystal_description 'platy-prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.205 _exptl_crystal_size_mid 0.195 _exptl_crystal_size_min 0.077 _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 3.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2012) ; _shelx_estimated_absorpt_T_min 0.578 _shelx_estimated_absorpt_T_max 0.802 _exptl_absorpt_correction_T_min 0.3492 _exptl_absorpt_correction_T_max 0.7452 _diffrn_ambient_temperature 298(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_reflns_number 16925 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_theta_min 2.194 _diffrn_reflns_theta_max 25.347 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _refine_special_details ? _reflns_number_total 3808 _reflns_number_gt 3114 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_gt 0.1312 _refine_ls_wR_factor_ref 0.1450 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_number_reflns 3808 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0918P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.902 _refine_diff_density_min -1.984 _refine_ls_extinction_method none _refine_ls_extinction_coef . 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2008) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I I1 0.25244(2) -0.01229(6) 0.13640(2) 0.04488(19) Uani d 1 . . I I2 0.30512(2) 0.07869(7) 0.42246(3) 0.04999(19) Uani d 1 . . N N1 0.31227(12) 0.3200(8) 0.1496(2) 0.0383(11) Uani d 1 . . C C1 0.32956(18) 0.4989(9) 0.1981(4) 0.0446(15) Uani d 1 . . H H1A 0.3463 0.5629 0.1690 0.053 Uiso calc 1 . . H H1B 0.3109 0.5965 0.2029 0.053 Uiso calc 1 . . C C2 0.34941(19) 0.4459(10) 0.2810(4) 0.0503(16) Uani d 1 . . H H2A 0.3713 0.3736 0.2770 0.060 Uiso calc 1 . . H H2B 0.3345 0.3583 0.3069 0.060 Uiso calc 1 . . C C3 0.35877(18) 0.6363(11) 0.3312(4) 0.0498(15) Uani d 1 . . H H3A 0.3769 0.7134 0.3107 0.060 Uiso calc 1 . . H H3B 0.3375 0.7199 0.3284 0.060 Uiso calc 1 . . C C4 0.37268(18) 0.5764(12) 0.4160(4) 0.0536(17) Uani d 1 . . H H4 0.3577 0.4935 0.4394 0.064 Uiso calc 1 . . C C5 0.40427(16) 0.6276(11) 0.4628(3) 0.0476(15) Uani d 1 . . C C6 0.41456(18) 0.5452(12) 0.5446(4) 0.0537(18) Uani d 1 . . C C7 0.4042(2) 0.3523(14) 0.5653(4) 0.066(2) Uani d 1 . . H H7 0.3905 0.2719 0.5265 0.080 Uiso calc 1 . . C C8 0.4140(2) 0.2791(17) 0.6421(5) 0.083(3) Uani d 1 . . H H8 0.4068 0.1506 0.6544 0.099 Uiso calc 1 . . C C9 0.4346(2) 0.396(2) 0.7012(5) 0.095(4) Uani d 1 . . H H9 0.4411 0.3468 0.7530 0.114 Uiso calc 1 . . C C10 0.4453(2) 0.586(2) 0.6822(5) 0.098(4) Uani d 1 . . H H10 0.4592 0.6652 0.7213 0.117 Uiso calc 1 . . C C11 0.43528(19) 0.6603(16) 0.6054(4) 0.073(2) Uani d 1 . . H H11 0.4425 0.7893 0.5937 0.088 Uiso calc 1 . . C C12 0.42943(16) 0.7710(12) 0.4341(3) 0.0494(16) Uani d 1 . . C C13 0.4190(2) 0.9644(13) 0.4097(5) 0.067(2) Uani d 1 . . H H13 0.3957 1.0067 0.4121 0.080 Uiso calc 1 . . C C14 0.4417(3) 1.0942(16) 0.3824(6) 0.087(3) Uani d 1 . . H H14 0.4339 1.2226 0.3655 0.104 Uiso calc 1 . . C C15 0.4761(3) 1.036(2) 0.3796(7) 0.097(4) Uani d 1 . . H H15 0.4914 1.1257 0.3604 0.117 Uiso calc 1 . . C C16 0.4882(2) 0.849(2) 0.4045(5) 0.091(3) Uani d 1 . . H H16 0.5118 0.8115 0.4026 0.109 Uiso calc 1 . . C C17 0.46478(18) 0.7137(15) 0.4330(4) 0.067(2) Uani d 1 . . H H17 0.4729 0.5865 0.4509 0.080 Uiso calc 1 . . C C18 0.28176(16) 0.2484(10) 0.1869(3) 0.0425(14) Uani d 1 . . H H18A 0.2648 0.3587 0.1853 0.051 Uiso calc 1 . . H H18B 0.2911 0.2201 0.2428 0.051 Uiso calc 1 . . C C19 0.33945(17) 0.1549(11) 0.1464(4) 0.0509(16) Uani d 1 . . H H19A 0.3288 0.0516 0.1101 0.076 Uiso calc 1 . . H H19B 0.3468 0.0982 0.1988 0.076 Uiso calc 1 . . H H19C 0.3601 0.2098 0.1283 0.076 Uiso calc 1 . . C C20 0.29821(18) 0.3908(10) 0.0658(3) 0.0495(16) Uani d 1 . . H H20A 0.2870 0.2801 0.0343 0.074 Uiso calc 1 . . H H20B 0.3178 0.4416 0.0427 0.074 Uiso calc 1 . . H H20C 0.2808 0.4959 0.0668 0.074 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0501(3) 0.0520(3) 0.0289(3) -0.01023(17) -0.00240(18) 0.00087(16) I2 0.0512(3) 0.0512(3) 0.0461(3) 0.00415(19) 0.0052(2) 0.01397(19) N1 0.041(3) 0.050(3) 0.021(2) -0.003(2) -0.0006(19) -0.002(2) C1 0.052(4) 0.047(4) 0.033(3) -0.013(3) 0.001(3) -0.003(3) C2 0.052(4) 0.062(4) 0.031(3) -0.008(3) -0.009(3) -0.005(3) C3 0.044(3) 0.062(4) 0.039(3) -0.010(3) -0.003(3) -0.011(3) C4 0.047(4) 0.082(5) 0.028(3) -0.012(3) -0.001(3) -0.011(3) C5 0.042(3) 0.067(4) 0.031(3) -0.009(3) 0.000(2) -0.019(3) C6 0.035(3) 0.089(5) 0.036(3) 0.001(3) 0.004(3) -0.008(3) C7 0.064(5) 0.088(6) 0.046(4) 0.000(4) 0.008(3) -0.002(4) C8 0.066(5) 0.126(8) 0.058(5) 0.013(5) 0.018(4) 0.021(5) C9 0.051(5) 0.188(12) 0.044(5) 0.007(6) 0.002(4) 0.014(6) C10 0.059(5) 0.190(12) 0.039(4) -0.033(7) -0.004(4) -0.024(6) C11 0.057(4) 0.118(7) 0.042(4) -0.023(5) 0.001(3) -0.021(4) C12 0.040(3) 0.075(5) 0.029(3) -0.008(3) -0.003(2) -0.016(3) C13 0.057(5) 0.075(5) 0.061(5) -0.012(4) -0.007(4) -0.020(4) C14 0.079(6) 0.092(7) 0.079(6) -0.027(5) -0.014(5) 0.009(5) C15 0.073(7) 0.136(10) 0.076(6) -0.044(6) -0.004(5) 0.025(7) C16 0.047(4) 0.167(11) 0.056(5) -0.019(6) 0.004(4) -0.005(6) C17 0.043(4) 0.111(7) 0.042(4) -0.004(4) -0.002(3) -0.004(4) C18 0.044(3) 0.058(4) 0.025(3) -0.009(3) 0.003(2) -0.004(3) C19 0.048(4) 0.058(4) 0.044(3) 0.005(3) 0.002(3) -0.011(3) C20 0.057(4) 0.061(4) 0.028(3) -0.004(3) 0.000(3) 0.006(3) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 C18 . 2.146(6) ? I1 I2 4_545 3.5058(7) ? N1 C18 . 1.492(7) ? N1 C20 . 1.504(7) ? N1 C19 . 1.509(8) ? N1 C1 . 1.522(8) ? C1 C2 . 1.513(9) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 C3 . 1.530(9) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 C4 . 1.496(9) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 C5 . 1.351(9) ? C4 H4 . 0.9300 ? C5 C6 . 1.480(10) ? C5 C12 . 1.489(9) ? C6 C7 . 1.402(12) ? C6 C11 . 1.404(10) ? C7 C8 . 1.379(11) ? C7 H7 . 0.9300 ? C8 C9 . 1.390(14) ? C8 H8 . 0.9300 ? C9 C10 . 1.381(16) ? C9 H9 . 0.9300 ? C10 C11 . 1.382(12) ? C10 H10 . 0.9300 ? C11 H11 . 0.9300 ? C12 C13 . 1.383(11) ? C12 C17 . 1.392(9) ? C13 C14 . 1.357(12) ? C13 H13 . 0.9300 ? C14 C15 . 1.361(14) ? C14 H14 . 0.9300 ? C15 C16 . 1.363(16) ? C15 H15 . 0.9300 ? C16 C17 . 1.410(13) ? C16 H16 . 0.9300 ? C17 H17 . 0.9300 ? C18 H18A . 0.9700 ? C18 H18B . 0.9700 ? C19 H19A . 0.9600 ? C19 H19B . 0.9600 ? C19 H19C . 0.9600 ? C20 H20A . 0.9600 ? C20 H20B . 0.9600 ? C20 H20C . 0.9600 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C18 I1 I2 . 4_545 170.16(15) ? C18 N1 C20 . . 109.7(4) ? C18 N1 C19 . . 111.6(5) ? C20 N1 C19 . . 108.5(5) ? C18 N1 C1 . . 107.8(4) ? C20 N1 C1 . . 108.2(5) ? C19 N1 C1 . . 111.0(5) ? C2 C1 N1 . . 114.4(5) ? C2 C1 H1A . . 108.6 ? N1 C1 H1A . . 108.6 ? C2 C1 H1B . . 108.6 ? N1 C1 H1B . . 108.6 ? H1A C1 H1B . . 107.6 ? C1 C2 C3 . . 110.7(6) ? C1 C2 H2A . . 109.5 ? C3 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? C3 C2 H2B . . 109.5 ? H2A C2 H2B . . 108.1 ? C4 C3 C2 . . 108.9(6) ? C4 C3 H3A . . 109.9 ? C2 C3 H3A . . 109.9 ? C4 C3 H3B . . 109.9 ? C2 C3 H3B . . 109.9 ? H3A C3 H3B . . 108.3 ? C5 C4 C3 . . 128.2(7) ? C5 C4 H4 . . 115.9 ? C3 C4 H4 . . 115.9 ? C4 C5 C6 . . 120.9(6) ? C4 C5 C12 . . 121.0(6) ? C6 C5 C12 . . 118.1(5) ? C7 C6 C11 . . 117.0(7) ? C7 C6 C5 . . 122.5(6) ? C11 C6 C5 . . 120.5(7) ? C8 C7 C6 . . 121.4(8) ? C8 C7 H7 . . 119.3 ? C6 C7 H7 . . 119.3 ? C7 C8 C9 . . 120.4(10) ? C7 C8 H8 . . 119.8 ? C9 C8 H8 . . 119.8 ? C10 C9 C8 . . 119.3(8) ? C10 C9 H9 . . 120.3 ? C8 C9 H9 . . 120.3 ? C9 C10 C11 . . 120.3(9) ? C9 C10 H10 . . 119.9 ? C11 C10 H10 . . 119.9 ? C10 C11 C6 . . 121.6(9) ? C10 C11 H11 . . 119.2 ? C6 C11 H11 . . 119.2 ? C13 C12 C17 . . 118.1(7) ? C13 C12 C5 . . 121.8(6) ? C17 C12 C5 . . 120.1(7) ? C14 C13 C12 . . 121.8(8) ? C14 C13 H13 . . 119.1 ? C12 C13 H13 . . 119.1 ? C13 C14 C15 . . 120.0(10) ? C13 C14 H14 . . 120.0 ? C15 C14 H14 . . 120.0 ? C14 C15 C16 . . 121.0(9) ? C14 C15 H15 . . 119.5 ? C16 C15 H15 . . 119.5 ? C15 C16 C17 . . 119.3(9) ? C15 C16 H16 . . 120.3 ? C17 C16 H16 . . 120.3 ? C12 C17 C16 . . 119.7(9) ? C12 C17 H17 . . 120.1 ? C16 C17 H17 . . 120.1 ? N1 C18 I1 . . 117.9(4) ? N1 C18 H18A . . 107.8 ? I1 C18 H18A . . 107.8 ? N1 C18 H18B . . 107.8 ? I1 C18 H18B . . 107.8 ? H18A C18 H18B . . 107.2 ? N1 C19 H19A . . 109.5 ? N1 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? N1 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? N1 C20 H20A . . 109.5 ? N1 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? N1 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C18 N1 C1 C2 . . . . 69.2(7) ? C20 N1 C1 C2 . . . . -172.2(5) ? C19 N1 C1 C2 . . . . -53.3(7) ? N1 C1 C2 C3 . . . . -167.8(5) ? C1 C2 C3 C4 . . . . 170.6(6) ? C2 C3 C4 C5 . . . . 124.9(8) ? C3 C4 C5 C6 . . . . -176.7(7) ? C3 C4 C5 C12 . . . . 4.3(12) ? C4 C5 C6 C7 . . . . 32.1(11) ? C12 C5 C6 C7 . . . . -148.9(7) ? C4 C5 C6 C11 . . . . -147.5(7) ? C12 C5 C6 C11 . . . . 31.5(10) ? C11 C6 C7 C8 . . . . 0.0(11) ? C5 C6 C7 C8 . . . . -179.7(7) ? C6 C7 C8 C9 . . . . 0.0(12) ? C7 C8 C9 C10 . . . . -0.2(14) ? C8 C9 C10 C11 . . . . 0.6(15) ? C9 C10 C11 C6 . . . . -0.7(14) ? C7 C6 C11 C10 . . . . 0.4(12) ? C5 C6 C11 C10 . . . . -179.9(8) ? C4 C5 C12 C13 . . . . 57.8(9) ? C6 C5 C12 C13 . . . . -121.2(7) ? C4 C5 C12 C17 . . . . -123.6(8) ? C6 C5 C12 C17 . . . . 57.4(8) ? C17 C12 C13 C14 . . . . 2.5(11) ? C5 C12 C13 C14 . . . . -179.0(7) ? C12 C13 C14 C15 . . . . -1.0(14) ? C13 C14 C15 C16 . . . . -0.4(16) ? C14 C15 C16 C17 . . . . 0.4(16) ? C13 C12 C17 C16 . . . . -2.5(10) ? C5 C12 C17 C16 . . . . 179.0(6) ? C15 C16 C17 C12 . . . . 1.1(13) ? C20 N1 C18 I1 . . . . 64.9(6) ? C19 N1 C18 I1 . . . . -55.4(5) ? C1 N1 C18 I1 . . . . -177.5(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C2 H2B I2 . 0.97 3.06 4.001(7) 165 _shelx_hkl_file ; 2 0 0 -0.17 0.02 2 0 0 -0.17 0.01 -2 0 0 -0.20 0.01 4 0 0 114.41 12.28 -4 0 0 126.27 12.29 4 0 0 113.04 11.01 4 0 0 115.46 11.14 -4 0 0 114.82 11.14 6 0 0 81.38 8.25 -6 0 0 99.98 9.19 -6 0 0 82.31 8.34 6 0 0 84.34 9.18 -8 0 0 50.79 4.98 8 0 0 51.66 4.92 8 0 0 51.41 5.45 10 0 0 0.80 0.21 -10 0 0 1.69 0.26 10 0 0 0.88 0.27 -10 0 0 1.37 0.32 -12 0 0 72.74 6.43 12 0 0 64.55 6.34 12 0 0 63.12 7.00 14 0 0 52.42 5.66 -14 0 0 54.90 5.22 14 0 0 53.45 5.15 16 0 0 226.71 24.39 16 0 0 224.21 21.92 -16 0 0 245.83 22.19 18 0 0 341.43 32.83 18 0 0 341.26 36.57 -18 0 0 362.08 33.23 20 0 0 184.59 19.08 -20 0 0 184.28 17.41 20 0 0 174.01 17.20 -22 0 0 82.76 7.70 22 0 0 79.81 8.31 22 0 0 72.62 7.58 -24 0 0 8.56 1.16 24 0 0 8.18 0.97 24 0 0 8.30 1.13 26 0 0 1.20 0.42 -26 0 0 1.50 0.52 26 0 0 1.80 0.31 28 0 0 0.71 0.35 -28 0 0 1.44 0.47 -30 0 0 2.82 0.72 30 0 0 2.35 0.62 32 0 0 29.64 3.13 -32 0 0 28.78 3.14 -34 0 0 38.91 4.02 34 0 0 36.96 3.96 36 0 0 38.22 4.13 -36 0 0 40.85 4.19 38 0 0 30.36 3.27 -38 0 0 29.26 3.26 -40 0 0 5.70 1.09 40 0 0 3.68 0.89 42 0 0 0.67 0.44 -42 0 0 0.86 0.58 44 0 0 -0.26 0.38 -44 0 0 -0.89 0.39 -1 -1 0 0.46 0.14 1 -1 0 0.94 0.22 1 -1 0 0.45 0.12 -1 -1 0 0.37 0.18 -1 1 0 0.56 0.12 -1 1 0 0.38 0.13 1 1 0 0.21 0.12 3 -1 0 14.47 1.37 -3 -1 0 12.73 1.54 3 -1 0 13.42 1.57 3 -1 0 15.84 1.40 -3 -1 0 13.27 1.41 3 1 0 14.79 1.39 -3 1 0 14.52 1.37 -5 -1 0 240.23 25.37 5 -1 0 244.77 22.94 -5 -1 0 220.23 22.98 5 -1 0 271.95 22.72 5 1 0 211.18 25.35 -5 1 0 245.36 22.93 5 1 0 257.02 22.72 -7 -1 0 49.10 5.16 7 -1 0 55.16 5.10 7 -1 0 51.38 5.11 -7 -1 0 54.20 5.64 -7 1 0 55.86 5.11 7 1 0 53.08 5.62 7 1 0 53.55 5.09 -9 -1 0 13.86 1.37 9 -1 0 13.81 1.32 -9 -1 0 13.43 1.39 9 1 0 10.75 1.37 -9 1 0 13.90 1.30 9 1 0 12.61 1.32 11 -1 0 25.55 2.61 11 -1 0 28.29 2.88 -11 -1 0 24.87 2.66 11 1 0 26.81 2.61 -11 1 0 26.07 2.60 -13 -1 0 41.94 4.49 13 -1 0 51.51 4.91 13 -1 0 44.97 4.43 13 1 0 45.47 4.42 -13 1 0 43.66 4.44 -15 -1 0 21.85 2.20 15 -1 0 20.58 2.33 15 -1 0 21.50 2.16 15 1 0 19.37 2.12 -15 1 0 22.44 2.14 17 -1 0 0.14 0.19 17 -1 0 0.21 0.21 -17 -1 0 -0.07 0.20 -17 1 0 -0.08 0.18 17 1 0 0.20 0.19 19 -1 0 21.52 2.04 -19 -1 0 22.44 2.10 19 -1 0 15.82 2.12 19 1 0 19.28 1.99 -19 1 0 19.99 2.00 -21 -1 0 35.16 3.60 21 -1 0 30.74 3.79 21 -1 0 36.78 3.54 -21 1 0 38.70 3.55 21 1 0 36.73 3.52 -23 -1 0 82.77 7.56 23 -1 0 68.97 8.13 23 -1 0 76.47 7.43 -23 1 0 84.37 7.48 23 1 0 72.90 7.39 25 -1 0 38.72 4.44 25 -1 0 41.38 4.15 -25 -1 0 40.12 4.21 -25 1 0 44.14 4.15 25 1 0 41.88 4.12 27 -1 0 5.21 0.75 -27 -1 0 4.15 0.89 27 -1 0 5.10 0.89 -27 1 0 5.62 0.86 27 1 0 4.06 0.77 29 -1 0 0.12 0.32 29 -1 0 0.50 0.26 -29 -1 0 0.15 0.46 -29 1 0 -0.14 0.34 29 1 0 0.05 0.29 31 -1 0 0.70 0.42 -31 -1 0 1.90 0.65 31 1 0 1.51 0.46 -31 1 0 1.23 0.50 -33 -1 0 4.25 0.95 33 -1 0 4.74 0.89 33 1 0 4.29 0.83 -33 1 0 3.84 0.79 -35 -1 0 1.10 0.54 35 -1 0 0.56 0.38 -35 1 0 0.61 0.43 35 1 0 0.73 0.32 -37 -1 0 6.99 1.32 37 -1 0 10.02 1.42 -37 1 0 8.74 1.33 37 1 0 7.67 1.26 39 -1 0 12.41 1.72 -39 -1 0 9.46 1.65 -39 1 0 11.93 1.63 39 1 0 10.79 1.62 -41 -1 0 9.37 1.60 41 -1 0 10.50 1.57 41 1 0 8.65 1.48 -41 1 0 10.31 1.50 -43 -1 0 5.87 1.21 43 -1 0 5.33 1.05 43 1 0 4.03 0.97 0 -2 0 291.59 32.67 0 -2 0 339.99 29.53 0 2 0 298.73 29.18 -2 -2 0 251.87 29.23 2 -2 0 295.20 26.40 2 -2 0 244.92 29.23 -2 -2 0 292.17 26.44 -2 2 0 306.56 26.41 -2 2 0 265.51 26.12 2 2 0 284.26 26.13 4 -2 0 114.30 12.88 -4 -2 0 115.44 12.87 -4 -2 0 122.37 11.65 4 -2 0 125.19 11.60 4 2 0 123.78 11.50 -4 2 0 122.08 11.58 -4 2 0 126.21 11.50 -6 -2 0 42.39 4.73 -6 -2 0 40.91 4.30 6 -2 0 38.58 4.74 6 -2 0 44.72 4.21 -6 2 0 43.68 4.21 -6 2 0 50.39 4.26 6 2 0 47.05 4.25 8 -2 0 34.64 3.57 8 -2 0 39.89 3.63 8 -2 0 37.05 4.05 -8 -2 0 37.09 4.01 -8 -2 0 36.73 3.68 -8 2 0 37.58 3.57 8 2 0 38.80 3.62 10 -2 0 36.59 3.57 -10 -2 0 35.30 3.93 -10 -2 0 35.23 3.64 10 -2 0 42.14 4.00 -10 2 0 35.10 3.52 10 2 0 36.48 3.57 12 -2 0 60.37 5.79 -12 -2 0 61.58 6.38 -12 -2 0 61.75 5.90 -12 2 0 57.95 5.75 12 2 0 58.85 5.78 -14 -2 0 110.16 10.35 14 -2 0 111.38 10.19 -14 -2 0 101.53 11.25 14 2 0 100.75 10.16 -14 2 0 110.23 10.20 16 -2 0 129.50 11.97 -16 -2 0 117.79 13.21 -16 -2 0 117.70 12.14 16 2 0 125.37 11.96 -16 2 0 133.92 12.01 16 2 0 128.25 13.21 18 -2 0 140.76 15.45 18 -2 0 148.70 13.89 -18 -2 0 131.68 14.09 -18 2 0 153.82 13.96 18 2 0 152.69 13.90 20 -2 0 106.56 10.46 20 -2 0 123.36 11.62 -20 -2 0 97.89 10.61 -20 2 0 116.42 10.49 20 2 0 97.50 10.42 -22 -2 0 53.10 5.19 22 -2 0 42.97 5.51 22 -2 0 53.83 5.08 22 2 0 51.32 5.04 -22 2 0 56.86 5.03 24 -2 0 18.51 2.60 -24 -2 0 26.95 2.65 24 -2 0 25.86 2.53 24 2 0 22.60 2.45 -24 2 0 26.88 2.43 26 -2 0 7.52 1.16 26 -2 0 8.32 1.22 -26 -2 0 11.76 1.48 26 2 0 9.11 1.22 -26 2 0 8.80 1.13 28 -2 0 0.15 0.27 28 -2 0 0.25 0.32 -28 -2 0 0.73 0.52 -28 2 0 -0.03 0.29 28 2 0 0.55 0.31 30 -2 0 9.48 1.40 -30 -2 0 10.21 1.54 30 -2 0 8.66 1.30 30 2 0 8.90 1.32 -30 2 0 10.93 1.31 32 -2 0 6.71 1.12 -32 -2 0 6.16 1.16 32 -2 0 5.50 0.94 -32 2 0 7.34 1.00 32 2 0 5.51 0.97 -34 -2 0 10.94 1.70 34 -2 0 9.89 1.53 34 2 0 12.25 1.59 -36 -2 0 22.91 2.62 36 -2 0 20.88 2.43 36 2 0 20.00 2.36 38 -2 0 11.49 1.60 -38 -2 0 11.96 1.82 38 2 0 7.91 1.40 40 -2 0 7.94 1.45 -40 -2 0 9.37 1.65 40 2 0 9.37 1.44 42 -2 0 2.23 0.81 -42 -2 0 3.24 1.03 42 2 0 3.30 0.78 -1 -3 0 5.80 0.64 1 -3 0 5.30 0.61 1 -3 0 5.32 0.85 -1 -3 0 4.86 0.82 -1 3 0 4.98 0.61 1 3 0 4.82 0.61 -3 -3 0 0.67 0.31 3 -3 0 0.59 0.17 -3 -3 0 0.82 0.25 3 -3 0 0.50 0.31 3 3 0 0.79 0.22 -3 3 0 0.74 0.21 5 -3 0 0.13 0.25 5 -3 0 0.12 0.11 -5 -3 0 -0.03 0.24 -5 -3 0 0.07 0.15 5 3 0 0.14 0.15 -5 3 0 0.04 0.15 -7 -3 0 17.25 2.01 -7 -3 0 18.67 1.84 7 3 0 17.85 1.79 -7 3 0 16.76 1.70 -7 3 0 16.67 1.77 9 -3 0 4.91 0.85 -9 -3 0 6.66 0.86 -9 -3 0 5.34 0.80 -9 3 0 5.14 0.56 9 3 0 5.55 0.73 -9 3 0 5.71 0.74 -11 -3 0 -0.04 0.19 11 -3 0 0.33 0.31 11 -3 0 0.14 0.18 -11 -3 0 0.27 0.23 -11 3 0 0.32 0.09 11 3 0 0.14 0.18 -11 3 0 0.26 0.20 -13 -3 0 1.11 0.33 13 -3 0 0.62 0.30 -13 -3 0 1.47 0.44 13 -3 0 0.99 0.36 -13 3 0 1.14 0.18 13 3 0 1.09 0.32 -13 3 0 1.62 0.39 -15 -3 0 0.16 0.19 15 -3 0 0.05 0.19 15 -3 0 -0.35 0.22 -15 -3 0 -0.05 0.24 -15 3 0 0.18 0.09 15 3 0 0.26 0.23 17 -3 0 0.14 0.23 17 -3 0 -0.39 0.21 -17 -3 0 -0.04 0.16 -17 -3 0 0.26 0.31 17 3 0 0.00 0.18 -17 3 0 -0.09 0.09 19 -3 0 9.52 1.21 19 -3 0 9.99 1.21 -19 -3 0 8.14 1.29 -19 -3 0 9.29 1.07 -19 3 0 8.49 0.94 19 3 0 8.70 1.20 21 -3 0 11.75 1.44 21 -3 0 13.40 1.56 -21 -3 0 13.20 1.72 21 3 0 12.88 1.46 -21 3 0 12.03 1.30 23 -3 0 5.83 0.97 23 -3 0 6.19 0.99 -23 -3 0 5.57 1.06 -23 3 0 7.35 0.78 23 3 0 7.01 1.05 25 -3 0 1.02 0.46 25 -3 0 0.84 0.37 -25 -3 0 1.06 0.56 25 3 0 1.12 0.39 27 -3 0 2.62 0.64 -27 -3 0 0.60 0.60 27 -3 0 1.98 0.50 27 3 0 1.98 0.52 -29 -3 0 2.86 0.84 29 -3 0 3.09 0.73 29 -3 0 2.91 0.61 29 3 0 3.17 0.69 -31 -3 0 1.00 0.54 31 -3 0 0.21 0.39 31 -3 0 0.53 0.32 31 3 0 1.12 0.42 33 -3 0 1.55 0.58 33 -3 0 1.87 0.51 -33 -3 0 1.36 0.71 33 3 0 2.09 0.59 -35 -3 0 0.26 0.58 35 -3 0 1.25 0.56 35 3 0 0.75 0.43 -37 -3 0 1.37 0.79 37 -3 0 1.65 0.64 37 3 0 2.32 0.64 -39 -3 0 0.60 0.73 39 -3 0 2.35 0.75 39 3 0 1.73 0.54 41 -3 0 2.36 0.73 -41 -3 0 1.55 0.83 41 3 0 1.60 0.60 0 -4 0 11.59 1.69 0 -4 0 13.43 1.33 0 4 0 11.28 1.31 -2 -4 0 26.25 2.47 2 -4 0 18.59 2.75 2 -4 0 26.19 2.42 -2 -4 0 23.90 2.80 2 4 0 24.70 2.43 -2 4 0 23.29 2.41 4 -4 0 44.32 5.61 -4 -4 0 50.15 5.64 4 -4 0 53.22 4.97 -4 -4 0 55.32 5.06 -4 4 0 49.88 4.96 4 4 0 52.93 4.98 6 -4 0 58.53 7.38 -6 -4 0 66.33 7.41 -6 -4 0 73.18 6.70 6 -4 0 69.63 6.56 6 4 0 69.09 6.58 -6 4 0 71.14 6.57 8 -4 0 69.39 8.35 -8 -4 0 80.21 8.38 -8 -4 0 82.14 7.60 8 -4 0 73.50 7.41 8 4 0 82.85 7.46 -8 4 0 77.70 7.44 -10 -4 0 79.39 7.25 10 -4 0 62.64 7.92 -10 -4 0 76.61 7.96 10 -4 0 71.81 7.02 -10 4 0 73.68 7.08 10 4 0 77.59 7.10 -12 -4 0 60.94 5.77 12 -4 0 56.77 5.51 -12 -4 0 63.75 6.30 12 -4 0 45.58 6.25 12 4 0 58.87 5.62 -12 4 0 61.49 5.63 -14 -4 0 25.20 3.13 14 -4 0 29.05 3.19 -14 -4 0 27.18 2.96 -14 4 0 27.69 2.84 14 4 0 29.74 2.86 -16 -4 0 6.30 1.12 16 -4 0 7.91 1.24 -16 -4 0 7.07 1.09 16 4 0 9.00 1.10 -16 4 0 8.17 1.07 -18 -4 0 5.47 1.05 18 -4 0 6.74 1.11 18 -4 0 6.78 1.01 -18 -4 0 7.80 0.96 -18 4 0 7.43 1.05 18 4 0 6.89 1.00 -20 -4 0 2.87 0.75 20 -4 0 3.68 0.75 20 -4 0 2.81 0.63 20 4 0 3.33 0.67 -20 4 0 3.96 0.75 -22 -4 0 20.98 2.17 22 -4 0 18.25 2.10 22 -4 0 15.31 1.93 22 4 0 15.92 1.91 -24 -4 0 38.49 3.83 24 -4 0 35.33 3.61 24 -4 0 35.66 3.90 24 4 0 30.29 3.55 26 -4 0 22.08 2.40 26 -4 0 20.98 2.29 -26 -4 0 16.77 2.52 26 4 0 18.45 2.20 28 -4 0 27.35 2.74 28 -4 0 24.97 2.83 -28 -4 0 24.19 2.85 28 4 0 21.31 2.61 -30 -4 0 17.26 2.23 30 -4 0 13.39 1.81 30 -4 0 15.89 2.03 30 4 0 15.15 1.77 32 -4 0 3.22 0.82 -32 -4 0 5.53 1.15 32 -4 0 3.33 0.73 32 4 0 3.28 0.76 34 -4 0 2.42 0.70 34 -4 0 1.99 0.55 -34 -4 0 2.01 0.89 34 4 0 1.33 0.50 -36 -4 0 1.13 0.74 36 -4 0 1.47 0.64 36 -4 0 1.81 0.58 36 4 0 0.92 0.46 38 -4 0 0.62 0.63 -38 -4 0 -0.05 0.58 38 4 0 2.10 0.58 1 -5 0 0.82 0.57 -1 -5 0 1.39 0.37 1 -5 0 1.72 0.38 -1 -5 0 1.75 0.64 -1 5 0 1.15 0.36 1 5 0 1.40 0.39 -3 -5 0 12.32 1.43 3 -5 0 11.71 1.36 -3 -5 0 14.78 1.92 3 -5 0 10.60 1.84 -3 5 0 12.64 1.41 3 5 0 13.71 1.43 -5 -5 0 19.97 2.11 5 -5 0 19.09 1.98 5 -5 0 16.26 2.38 -5 -5 0 20.76 2.44 5 5 0 21.91 2.08 -5 5 0 18.46 2.04 -7 -5 0 4.72 0.96 7 -5 0 4.90 0.58 7 -5 0 4.09 0.96 -7 -5 0 5.39 0.85 7 5 0 4.75 0.76 -7 5 0 4.07 0.69 9 -5 0 2.20 0.68 -9 -5 0 2.59 0.59 -9 -5 0 1.88 0.63 9 5 0 1.85 0.47 -9 5 0 1.57 0.42 -11 -5 0 11.53 1.65 11 -5 0 11.88 1.89 -11 -5 0 14.62 1.78 11 5 0 13.32 1.49 -11 5 0 13.02 1.48 -13 -5 0 23.11 2.38 -13 -5 0 22.98 2.53 13 -5 0 18.58 2.49 13 5 0 19.69 2.20 -13 5 0 19.62 2.17 -15 -5 0 7.93 1.33 15 -5 0 7.77 1.41 -15 -5 0 10.05 1.42 15 5 0 10.21 1.30 -15 5 0 10.28 1.19 -17 -5 0 1.18 0.48 -17 -5 0 1.95 0.61 17 -5 0 2.18 0.63 17 5 0 1.95 0.52 -17 5 0 1.66 0.45 19 -5 0 0.02 0.33 -19 -5 0 -0.35 0.34 -19 5 0 -0.46 0.17 19 5 0 0.29 0.28 21 -5 0 1.84 0.61 -21 -5 0 1.29 0.60 -21 5 0 2.69 0.58 21 5 0 1.80 0.52 -23 -5 0 2.18 0.74 23 -5 0 1.47 0.53 -23 5 0 1.38 0.49 23 5 0 2.69 0.60 -25 -5 0 -0.01 0.37 25 -5 0 0.13 0.31 25 5 0 0.70 0.38 -25 5 0 0.36 0.28 27 -5 0 1.40 0.48 -27 -5 0 1.23 0.60 -27 5 0 0.72 0.45 27 5 0 2.54 0.62 29 -5 0 4.70 0.90 -29 -5 0 3.37 1.03 29 -5 0 4.56 0.97 -29 5 0 6.12 1.03 29 5 0 4.98 0.90 -31 -5 0 7.23 1.40 31 -5 0 5.31 1.03 31 -5 0 6.51 1.20 -31 5 0 8.19 1.26 31 5 0 8.10 1.24 33 -5 0 4.43 0.99 33 -5 0 3.45 0.82 -33 -5 0 4.51 1.18 -33 5 0 3.95 0.95 33 5 0 4.28 0.86 0 -6 0 -0.16 0.42 0 6 0 -0.50 0.19 2 -6 0 0.72 0.51 -2 -6 0 0.70 0.53 -2 -6 0 0.70 0.34 2 6 0 0.88 0.34 -2 6 0 0.28 0.27 4 -6 0 7.29 1.34 -4 -6 0 6.84 1.02 -4 -6 0 7.80 1.33 -4 6 0 5.65 0.93 4 6 0 6.41 0.96 -6 -6 0 22.37 2.64 -6 -6 0 20.00 2.27 6 -6 0 19.31 2.61 -6 6 0 19.88 2.22 6 6 0 21.58 2.23 8 -6 0 39.73 4.86 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2 -2 -19 -0.19 0.55 -2 -2 19 0.59 0.64 -2 2 19 -0.01 0.33 2 2 -19 0.47 0.49 0 -2 19 0.00 0.54 0 -2 19 0.55 0.40 0 -2 -19 0.27 0.59 0 2 19 0.01 0.39 0 2 -19 0.64 0.70 2 -2 19 3.31 1.00 -2 -2 -19 1.94 0.85 2 -2 19 2.81 0.77 2 2 19 3.42 0.88 -2 2 -19 2.41 0.93 4 2 19 3.45 0.87 -7 -3 19 0.38 0.37 -7 3 19 0.26 0.40 -18 0 20 7.46 1.20 -16 0 20 5.20 0.96 16 0 -20 4.75 1.13 -14 0 20 3.02 0.73 14 0 -20 2.52 0.83 -12 0 20 -0.40 0.26 12 0 -20 -0.54 0.41 -10 0 20 -0.27 0.27 10 0 -20 0.05 0.44 8 0 -20 0.80 0.55 -8 0 20 1.14 0.48 -6 0 20 -0.17 0.30 6 0 -20 -0.09 0.51 -4 0 20 -0.02 0.36 4 0 -20 0.44 0.64 -2 0 20 3.53 0.83 2 0 -20 2.66 0.99 0 0 20 5.26 1.06 -15 -1 20 10.02 1.49 -15 1 20 11.37 1.60 -13 -1 20 17.17 1.97 13 -1 -20 17.55 2.53 -13 1 20 14.70 2.12 13 1 -20 15.46 2.52 11 -1 -20 17.90 2.75 -11 -1 20 19.61 2.20 11 1 -20 20.83 2.67 -11 1 20 16.61 2.40 -9 -1 20 10.49 1.63 9 -1 -20 13.05 2.13 -9 1 20 13.34 1.83 9 1 -20 13.78 2.21 -7 -1 20 3.34 0.80 7 -1 -20 3.39 1.04 7 1 -20 4.58 1.25 -7 1 20 4.03 0.89 -5 -1 20 1.97 0.60 5 -1 -20 1.15 0.78 -5 1 20 1.76 0.65 5 1 -20 0.42 0.62 -3 -1 20 3.45 0.77 3 -1 -20 1.55 0.84 3 1 -20 1.34 0.82 -3 1 20 1.42 0.62 -1 -1 20 3.75 0.80 -1 1 20 2.28 0.74 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 10903 _shelx_res_file ; Compound_I.res created by SHELXL-2014/7 TITL Compound I CELL 0.71073 37.7778 6.6323 17.0210 90.000 100.567 90.000 ZERR 8.00 0.0068 0.0012 0.0031 0.000 0.004 0.000 LATT 7 SYMM -x, y, -z+1/2 SFAC C H N I UNIT 160 200 8 16 OMIT 2 0 0 OMIT 2 0 2 OMIT 5 1 7 OMIT 4 0 6 OMIT 4 0 4 OMIT 4 0 2 OMIT 8 0 6 TEMP 25 SIZE 0.077 0.195 0.205 L.S. 20 BOND $H BIND I1 I2_$1 EQIV $1 -x+1/2, y-1/2, -z+1/2 HTAB C2 I2 HTAB C18 I2 EQIV $2 x, -y, z-1/2 HTAB C20 I2_$2 EQIV $3 x, -y+1, z-1/2 HTAB C1 C8_$3 HTAB C19 C11_$3 EQIV $4 x, -y+1, z+1/2 HTAB C9 C17_$4 EQIV $5 -x+1, -y+1, -z+1 HTAB C16 C8_$5 ACTA CONF BOND FMAP 2 PLAN 5 MPLA 6 C3 > C6 C12 MPLA 6 C6 > C11 MPLA 6 C12 > C17 WGHT 0.091800 FVAR 0.03825 I1 4 0.252436 -0.012290 0.136404 11.00000 0.05007 0.05196 = 0.02894 0.00087 -0.00240 -0.01023 I2 4 0.305117 0.078694 0.422462 11.00000 0.05124 0.05122 = 0.04607 0.01397 0.00516 0.00415 N1 3 0.312274 0.320001 0.149626 11.00000 0.04073 0.05037 = 0.02145 -0.00163 -0.00061 -0.00328 C1 1 0.329564 0.498943 0.198068 11.00000 0.05174 0.04684 = 0.03266 -0.00292 0.00133 -0.01336 AFIX 23 H1A 2 0.346319 0.562912 0.168971 11.00000 -1.20000 H1B 2 0.310946 0.596492 0.202854 11.00000 -1.20000 AFIX 0 C2 1 0.349414 0.445875 0.280984 11.00000 0.05175 0.06204 = 0.03092 -0.00466 -0.00878 -0.00776 AFIX 23 H2A 2 0.371344 0.373609 0.277047 11.00000 -1.20000 H2B 2 0.334502 0.358305 0.306925 11.00000 -1.20000 AFIX 0 C3 1 0.358765 0.636310 0.331198 11.00000 0.04429 0.06215 = 0.03900 -0.01099 -0.00307 -0.00987 AFIX 23 H3A 2 0.376908 0.713439 0.310698 11.00000 -1.20000 H3B 2 0.337506 0.719934 0.328408 11.00000 -1.20000 AFIX 0 C4 1 0.372682 0.576409 0.415964 11.00000 0.04676 0.08250 = 0.02839 -0.01051 -0.00122 -0.01227 AFIX 43 H4 2 0.357699 0.493473 0.439400 11.00000 -1.20000 AFIX 0 C5 1 0.404269 0.627583 0.462772 11.00000 0.04198 0.06697 = 0.03123 -0.01940 0.00020 -0.00902 C6 1 0.414557 0.545170 0.544551 11.00000 0.03536 0.08888 = 0.03590 -0.00807 0.00372 0.00086 C7 1 0.404223 0.352259 0.565314 11.00000 0.06400 0.08824 = 0.04575 -0.00154 0.00762 -0.00037 AFIX 43 H7 2 0.390468 0.271875 0.526494 11.00000 -1.20000 AFIX 0 C8 1 0.414016 0.279098 0.642081 11.00000 0.06629 0.12597 = 0.05828 0.02060 0.01793 0.01326 AFIX 43 H8 2 0.406808 0.150622 0.654376 11.00000 -1.20000 AFIX 0 C9 1 0.434584 0.396120 0.701178 11.00000 0.05077 0.18832 = 0.04439 0.01367 0.00236 0.00687 AFIX 43 H9 2 0.441090 0.346801 0.752964 11.00000 -1.20000 AFIX 0 C10 1 0.445268 0.586428 0.682218 11.00000 0.05899 0.18970 = 0.03921 -0.02418 -0.00426 -0.03280 AFIX 43 H10 2 0.459238 0.665193 0.721287 11.00000 -1.20000 AFIX 0 C11 1 0.435277 0.660272 0.605395 11.00000 0.05680 0.11809 = 0.04192 -0.02106 0.00067 -0.02320 AFIX 43 H11 2 0.442454 0.789302 0.593744 11.00000 -1.20000 AFIX 0 C12 1 0.429432 0.771003 0.434081 11.00000 0.04017 0.07518 = 0.02914 -0.01590 -0.00336 -0.00791 C13 1 0.418988 0.964395 0.409685 11.00000 0.05712 0.07530 = 0.06074 -0.02013 -0.00739 -0.01173 AFIX 43 H13 2 0.395737 1.006675 0.412073 11.00000 -1.20000 AFIX 0 C14 1 0.441735 1.094164 0.382358 11.00000 0.07889 0.09208 = 0.07947 0.00923 -0.01353 -0.02673 AFIX 43 H14 2 0.433877 1.222623 0.365522 11.00000 -1.20000 AFIX 0 C15 1 0.476059 1.036229 0.379599 11.00000 0.07267 0.13637 = 0.07621 0.02528 -0.00407 -0.04357 AFIX 43 H15 2 0.491435 1.125658 0.360448 11.00000 -1.20000 AFIX 0 C16 1 0.488239 0.849264 0.404458 11.00000 0.04743 0.16670 = 0.05577 -0.00477 0.00415 -0.01930 AFIX 43 H16 2 0.511784 0.811507 0.402639 11.00000 -1.20000 AFIX 0 C17 1 0.464780 0.713699 0.432956 11.00000 0.04321 0.11078 = 0.04201 -0.00399 -0.00187 -0.00423 AFIX 43 H17 2 0.472886 0.586486 0.450935 11.00000 -1.20000 AFIX 0 C18 1 0.281755 0.248385 0.186934 11.00000 0.04371 0.05762 = 0.02502 -0.00389 0.00290 -0.00863 AFIX 23 H18A 2 0.264778 0.358698 0.185304 11.00000 -1.20000 H18B 2 0.291149 0.220115 0.242779 11.00000 -1.20000 AFIX 0 C19 1 0.339448 0.154888 0.146437 11.00000 0.04780 0.05807 = 0.04423 -0.01124 0.00180 0.00538 AFIX 137 H19A 2 0.328795 0.051601 0.110147 11.00000 -1.50000 H19B 2 0.346782 0.098198 0.198789 11.00000 -1.50000 H19C 2 0.360058 0.209809 0.128347 11.00000 -1.50000 AFIX 0 C20 1 0.298207 0.390799 0.065771 11.00000 0.05660 0.06090 = 0.02794 0.00647 0.00000 -0.00420 AFIX 137 H20A 2 0.287027 0.280066 0.034307 11.00000 -1.50000 H20B 2 0.317786 0.441604 0.042687 11.00000 -1.50000 H20C 2 0.280828 0.495919 0.066795 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM Compound I REM R1 = 0.0522 for 3114 Fo > 4sig(Fo) and 0.0633 for all 3808 data REM 210 parameters refined using 0 restraints END WGHT 0.0918 0.0000 REM Highest difference peak 1.902, deepest hole -1.984, 1-sigma level 0.199 Q1 1 0.2717 0.0786 0.1191 11.00000 0.05 1.90 Q2 1 0.2723 -0.0968 0.1208 11.00000 0.05 1.72 Q3 1 0.2324 0.0689 0.1565 11.00000 0.05 1.72 Q4 1 0.2872 0.1772 0.4370 11.00000 0.05 1.72 Q5 1 0.2878 -0.0182 0.4380 11.00000 0.05 1.71 ; _shelx_res_checksum 41700 data_III _audit_creation_method SHELXL-2014 _chemical_name_systematic ;\ N-(6,6-Diphenylhex-5-en-1-yl)-N-iodomethyl-N,N-\ dimethylammonium iodide ; _chemical_name_common ? _chemical_formula_moiety 'C21 H27 I N+, I-' _chemical_formula_sum 'C21 H27 I2 N' _chemical_formula_iupac 'C21 H27 I N+, I-' _chemical_formula_weight 547.23 _chemical_melting_point_gt 429 _chemical_melting_point_lt 431 _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_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9423(12) _cell_length_b 24.058(3) _cell_length_c 10.3749(13) _cell_angle_alpha 90 _cell_angle_beta 103.656(3) _cell_angle_gamma 90 _cell_volume 2168.9(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3046 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.43 _cell_measurement_temperature 298(2) _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.322 _exptl_crystal_size_mid 0.222 _exptl_crystal_size_min 0.042 _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 2.902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (TWINABS; Bruker, 2012) ; _shelx_estimated_absorpt_T_min 0.455 _shelx_estimated_absorpt_T_max 0.888 _exptl_absorpt_correction_T_min 0.2730 _exptl_absorpt_correction_T_max 0.4288 _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 3961 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_theta_min 1.693 _diffrn_reflns_theta_max 25.359 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _refine_special_details ; Refined as a 2-component twin. The studied crystal was a nonmerohedral twin with a ratio of two major domains of 0.374(2):0.626 (2). The two domains were rotated from each other by 180.0\% about the recipocal axis (1 0 0), which was determined by the CELL NOW program (Sheldrick, 2004). The final refinement was carried out using twinned data set. ; _reflns_number_total 3961 _reflns_number_gt 2941 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_gt 0.1235 _refine_ls_wR_factor_ref 0.1383 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_number_reflns 3961 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+2.9321P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.816 _refine_diff_density_min -0.804 _refine_ls_extinction_method none _refine_ls_extinction_coef . 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2008) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015), PLATON (Spek, 2009) and publCIF (Westrip, 2010) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I I1 -0.29957(8) 0.44339(3) 0.01740(6) 0.0597(2) Uani d 1 . . I I2 0.17494(8) 0.51476(3) 0.26901(6) 0.0598(2) Uani d 1 . . N N1 -0.3411(8) 0.4415(4) 0.3070(7) 0.056(2) Uani d 1 . . C C1 -0.1733(11) 0.4319(4) 0.3631(10) 0.063(3) Uani d 1 . . H H1A -0.1159 0.4525 0.3103 0.076 Uiso calc 1 . . H H1B -0.1459 0.4469 0.4524 0.076 Uiso calc 1 . . C C2 -0.1252(12) 0.3731(4) 0.3678(12) 0.072(3) Uani d 1 . . H H2A -0.1407 0.3584 0.2786 0.087 Uiso calc 1 . . H H2B -0.1860 0.3512 0.4153 0.087 Uiso calc 1 . . C C3 0.0467(11) 0.3699(4) 0.4394(11) 0.068(3) Uani d 1 . . H H3A 0.1029 0.3971 0.4001 0.082 Uiso calc 1 . . H H3B 0.0578 0.3800 0.5317 0.082 Uiso calc 1 . . C C4 0.1182(12) 0.3134(4) 0.4333(15) 0.091(4) Uani d 1 . . H H4A 0.1013 0.3019 0.3413 0.109 Uiso calc 1 . . H H4B 0.0681 0.2866 0.4789 0.109 Uiso calc 1 . . C C5 0.2892(10) 0.3135(4) 0.4957(12) 0.068(3) Uani d 1 . . H H5 0.3381 0.3478 0.5120 0.082 Uiso calc 1 . . C C6 0.3743(10) 0.2685(3) 0.5287(10) 0.055(2) Uani d 1 . . C C7 0.5451(11) 0.2703(3) 0.5813(9) 0.052(2) Uani d 1 . . C C8 0.6398(11) 0.2322(4) 0.5435(11) 0.066(3) Uani d 1 . . H H8 0.5966 0.2031 0.4881 0.080 Uiso calc 1 . . C C9 0.8003(12) 0.2359(5) 0.5862(14) 0.091(4) Uani d 1 . . H H9 0.8636 0.2109 0.5560 0.109 Uiso calc 1 . . C C10 0.8623(15) 0.2778(5) 0.6747(14) 0.097(5) Uani d 1 . . H H10 0.9683 0.2798 0.7079 0.116 Uiso calc 1 . . C C11 0.7701(16) 0.3158(5) 0.7133(14) 0.094(4) Uani d 1 . . H H11 0.8128 0.3446 0.7699 0.113 Uiso calc 1 . . C C12 0.6122(14) 0.3116(5) 0.6681(11) 0.079(3) Uani d 1 . . H H12 0.5495 0.3373 0.6969 0.094 Uiso calc 1 . . C C13 0.3026(11) 0.2115(3) 0.5086(10) 0.055(2) Uani d 1 . . C C14 0.2723(13) 0.1847(4) 0.6156(12) 0.074(3) Uani d 1 . . H H14 0.2993 0.2012 0.6990 0.089 Uiso calc 1 . . C C15 0.2004(14) 0.1323(4) 0.6000(16) 0.088(4) Uani d 1 . . H H15 0.1840 0.1135 0.6738 0.105 Uiso calc 1 . . C C16 0.1551(14) 0.1091(5) 0.4782(18) 0.095(4) Uani d 1 . . H H16 0.1010 0.0757 0.4681 0.114 Uiso calc 1 . . C C17 0.1888(18) 0.1347(6) 0.3678(16) 0.116(6) Uani d 1 . . H H17 0.1614 0.1184 0.2842 0.139 Uiso calc 1 . . C C18 0.2659(17) 0.1861(5) 0.3880(12) 0.091(4) Uani d 1 . . H H18 0.2926 0.2034 0.3164 0.109 Uiso calc 1 . . C C19 -0.4077(11) 0.4192(4) 0.1718(10) 0.065(3) Uani d 1 . . H H19A -0.5148 0.4304 0.1460 0.078 Uiso calc 1 . . H H19B -0.4058 0.3789 0.1771 0.078 Uiso calc 1 . . C C20 -0.3648(13) 0.5048(4) 0.3059(11) 0.074(3) Uani d 1 . . H H20A -0.4723 0.5131 0.2740 0.111 Uiso calc 1 . . H H20B -0.3078 0.5218 0.2488 0.111 Uiso calc 1 . . H H20C -0.3294 0.5191 0.3943 0.111 Uiso calc 1 . . C C21 -0.4312(12) 0.4165(5) 0.3995(10) 0.071(3) Uani d 1 . . H H21A -0.5382 0.4256 0.3684 0.107 Uiso calc 1 . . H H21B -0.3936 0.4313 0.4872 0.107 Uiso calc 1 . . H H21C -0.4189 0.3769 0.4015 0.107 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I1 0.0559(4) 0.0659(4) 0.0605(4) 0.0039(3) 0.0202(3) 0.0118(3) I2 0.0586(4) 0.0618(4) 0.0632(4) 0.0015(3) 0.0228(3) 0.0043(3) N1 0.041(4) 0.081(6) 0.046(4) 0.002(4) 0.012(4) 0.020(4) C1 0.045(5) 0.078(7) 0.069(6) -0.006(5) 0.015(5) 0.014(5) C2 0.058(6) 0.056(6) 0.106(9) 0.003(5) 0.024(6) -0.001(6) C3 0.057(6) 0.069(6) 0.075(7) 0.012(5) 0.007(6) 0.017(6) C4 0.054(7) 0.065(7) 0.158(12) 0.006(5) 0.036(8) 0.023(8) C5 0.040(5) 0.043(5) 0.123(9) 0.002(4) 0.022(6) 0.012(6) C6 0.047(5) 0.038(5) 0.082(7) 0.005(4) 0.019(5) 0.010(5) C7 0.052(6) 0.038(5) 0.069(6) -0.002(4) 0.019(5) 0.010(4) C8 0.051(6) 0.055(6) 0.090(7) 0.004(5) 0.009(6) -0.006(5) C9 0.051(7) 0.083(8) 0.140(11) 0.017(6) 0.026(8) 0.022(8) C10 0.066(8) 0.077(8) 0.129(11) -0.028(7) -0.014(8) 0.022(8) C11 0.100(10) 0.054(7) 0.116(11) -0.008(7) -0.001(9) -0.007(7) C12 0.075(8) 0.074(7) 0.087(8) -0.007(6) 0.019(7) -0.002(7) C13 0.056(6) 0.040(5) 0.067(6) 0.012(4) 0.011(5) 0.014(5) C14 0.079(8) 0.053(6) 0.101(9) -0.004(6) 0.043(7) -0.012(6) C15 0.085(9) 0.041(6) 0.152(13) -0.009(6) 0.058(9) 0.011(7) C16 0.053(7) 0.063(7) 0.155(14) -0.001(6) -0.004(9) -0.005(10) C17 0.135(14) 0.072(9) 0.108(11) 0.001(9) -0.038(10) -0.002(8) C18 0.116(11) 0.069(8) 0.075(8) -0.001(8) -0.002(7) 0.001(7) C19 0.049(6) 0.080(7) 0.073(7) -0.005(5) 0.029(5) 0.024(6) C20 0.066(7) 0.071(7) 0.089(8) 0.009(6) 0.027(6) 0.008(6) C21 0.056(6) 0.091(8) 0.072(7) -0.006(6) 0.025(6) 0.032(6) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 C19 . 2.138(9) ? I1 I2 3_565 3.5565(9) ? N1 C19 . 1.489(12) ? N1 C1 . 1.494(12) ? N1 C21 . 1.515(11) ? N1 C20 . 1.537(12) ? C1 C2 . 1.477(13) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 C3 . 1.543(13) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 C4 . 1.510(14) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 C5 . 1.514(14) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 C6 . 1.323(12) ? C5 H5 . 0.9300 ? C6 C7 . 1.497(12) ? C6 C13 . 1.507(12) ? C7 C8 . 1.366(12) ? C7 C12 . 1.379(14) ? C8 C9 . 1.401(14) ? C8 H8 . 0.9300 ? C9 C10 . 1.388(17) ? C9 H9 . 0.9300 ? C10 C11 . 1.353(18) ? C10 H10 . 0.9300 ? C11 C12 . 1.383(16) ? C11 H11 . 0.9300 ? C12 H12 . 0.9300 ? C13 C18 . 1.360(14) ? C13 C14 . 1.365(14) ? C14 C15 . 1.407(14) ? C14 H14 . 0.9300 ? C15 C16 . 1.353(18) ? C15 H15 . 0.9300 ? C16 C17 . 1.39(2) ? C16 H16 . 0.9300 ? C17 C18 . 1.409(17) ? C17 H17 . 0.9300 ? C18 H18 . 0.9300 ? C19 H19A . 0.9700 ? C19 H19B . 0.9700 ? C20 H20A . 0.9600 ? C20 H20B . 0.9600 ? C20 H20C . 0.9600 ? C21 H21A . 0.9600 ? C21 H21B . 0.9600 ? C21 H21C . 0.9600 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C19 I1 I2 . 3_565 171.6(3) ? C19 N1 C1 . . 116.9(8) ? C19 N1 C21 . . 107.4(7) ? C1 N1 C21 . . 109.1(7) ? C19 N1 C20 . . 109.1(7) ? C1 N1 C20 . . 106.3(7) ? C21 N1 C20 . . 107.8(8) ? C2 C1 N1 . . 114.8(8) ? C2 C1 H1A . . 108.6 ? N1 C1 H1A . . 108.6 ? C2 C1 H1B . . 108.6 ? N1 C1 H1B . . 108.6 ? H1A C1 H1B . . 107.5 ? C1 C2 C3 . . 108.2(8) ? C1 C2 H2A . . 110.1 ? C3 C2 H2A . . 110.1 ? C1 C2 H2B . . 110.1 ? C3 C2 H2B . . 110.1 ? H2A C2 H2B . . 108.4 ? C4 C3 C2 . . 114.0(9) ? C4 C3 H3A . . 108.7 ? C2 C3 H3A . . 108.7 ? C4 C3 H3B . . 108.7 ? C2 C3 H3B . . 108.7 ? H3A C3 H3B . . 107.6 ? C3 C4 C5 . . 112.1(9) ? C3 C4 H4A . . 109.2 ? C5 C4 H4A . . 109.2 ? C3 C4 H4B . . 109.2 ? C5 C4 H4B . . 109.2 ? H4A C4 H4B . . 107.9 ? C6 C5 C4 . . 124.8(9) ? C6 C5 H5 . . 117.6 ? C4 C5 H5 . . 117.6 ? C5 C6 C7 . . 123.1(8) ? C5 C6 C13 . . 120.7(8) ? C7 C6 C13 . . 116.2(7) ? C8 C7 C12 . . 117.9(10) ? C8 C7 C6 . . 121.6(9) ? C12 C7 C6 . . 120.5(9) ? C7 C8 C9 . . 121.6(10) ? C7 C8 H8 . . 119.2 ? C9 C8 H8 . . 119.2 ? C10 C9 C8 . . 118.4(11) ? C10 C9 H9 . . 120.8 ? C8 C9 H9 . . 120.8 ? C11 C10 C9 . . 120.6(11) ? C11 C10 H10 . . 119.7 ? C9 C10 H10 . . 119.7 ? C10 C11 C12 . . 119.7(12) ? C10 C11 H11 . . 120.1 ? C12 C11 H11 . . 120.1 ? C7 C12 C11 . . 121.7(12) ? C7 C12 H12 . . 119.1 ? C11 C12 H12 . . 119.1 ? C18 C13 C14 . . 119.1(9) ? C18 C13 C6 . . 122.5(9) ? C14 C13 C6 . . 118.4(9) ? C13 C14 C15 . . 120.1(12) ? C13 C14 H14 . . 119.9 ? C15 C14 H14 . . 119.9 ? C16 C15 C14 . . 120.4(12) ? C16 C15 H15 . . 119.8 ? C14 C15 H15 . . 119.8 ? C15 C16 C17 . . 120.6(11) ? C15 C16 H16 . . 119.7 ? C17 C16 H16 . . 119.7 ? C16 C17 C18 . . 117.3(13) ? C16 C17 H17 . . 121.3 ? C18 C17 H17 . . 121.3 ? C13 C18 C17 . . 122.2(13) ? C13 C18 H18 . . 118.9 ? C17 C18 H18 . . 118.9 ? N1 C19 I1 . . 117.2(6) ? N1 C19 H19A . . 108.0 ? I1 C19 H19A . . 108.0 ? N1 C19 H19B . . 108.0 ? I1 C19 H19B . . 108.0 ? H19A C19 H19B . . 107.2 ? N1 C20 H20A . . 109.5 ? N1 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? N1 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? N1 C21 H21A . . 109.5 ? N1 C21 H21B . . 109.5 ? H21A C21 H21B . . 109.5 ? N1 C21 H21C . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C19 N1 C1 C2 . . . . -55.7(12) ? C21 N1 C1 C2 . . . . 66.3(12) ? C20 N1 C1 C2 . . . . -177.7(9) ? N1 C1 C2 C3 . . . . -174.9(8) ? C1 C2 C3 C4 . . . . -171.1(10) ? C2 C3 C4 C5 . . . . 175.7(10) ? C3 C4 C5 C6 . . . . 165.3(12) ? C4 C5 C6 C7 . . . . 175.5(11) ? C4 C5 C6 C13 . . . . -1.5(18) ? C5 C6 C7 C8 . . . . -140.0(11) ? C13 C6 C7 C8 . . . . 37.2(13) ? C5 C6 C7 C12 . . . . 38.6(15) ? C13 C6 C7 C12 . . . . -144.2(10) ? C12 C7 C8 C9 . . . . -2.7(16) ? C6 C7 C8 C9 . . . . 175.9(10) ? C7 C8 C9 C10 . . . . 3.5(18) ? C8 C9 C10 C11 . . . . -3.4(19) ? C9 C10 C11 C12 . . . . 3(2) ? C8 C7 C12 C11 . . . . 1.8(16) ? C6 C7 C12 C11 . . . . -176.9(10) ? C10 C11 C12 C7 . . . . -2(2) ? C5 C6 C13 C18 . . . . 78.5(15) ? C7 C6 C13 C18 . . . . -98.8(13) ? C5 C6 C13 C14 . . . . -100.9(13) ? C7 C6 C13 C14 . . . . 81.9(12) ? C18 C13 C14 C15 . . . . -1.6(16) ? C6 C13 C14 C15 . . . . 177.7(9) ? C13 C14 C15 C16 . . . . -2.7(18) ? C14 C15 C16 C17 . . . . 4.7(19) ? C15 C16 C17 C18 . . . . -2(2) ? C14 C13 C18 C17 . . . . 4.0(19) ? C6 C13 C18 C17 . . . . -175.3(11) ? C16 C17 C18 C13 . . . . -2(2) ? C1 N1 C19 I1 . . . . -54.3(10) ? C21 N1 C19 I1 . . . . -177.2(7) ? C20 N1 C19 I1 . . . . 66.3(9) ? _shelx_hkl_file ; 1 0 0 19.8891 1.52573 -2 1 0 0 19.8891 1.52573 1 2 0 0 9999.99 451.601 -2 2 0 0 9999.99 451.601 1 3 0 0 147.832 9.33590 -2 3 0 0 147.832 9.33590 1 4 0 0 263.588 15.3373 -2 4 0 0 263.588 15.3373 1 5 0 0 14.4537 3.50324 -2 5 0 0 14.4537 3.50324 1 6 0 0 907.380 46.3802 -2 6 0 0 907.380 46.3802 1 7 0 0 238.760 21.3825 -2 7 0 0 238.760 21.3825 1 8 0 0 353.329 22.4382 -2 8 0 0 353.329 22.4382 1 9 0 0 125.435 18.8744 -2 9 0 0 125.435 18.8744 1 10 0 0 16.3665 9.31885 -2 10 0 0 16.3665 9.31885 1 0 1 0 -0.0518 0.07424 -2 0 1 0 -0.0518 0.07424 1 1 1 0 240.244 6.86320 -2 1 1 0 240.244 6.86320 1 2 1 0 157.200 6.34771 -2 2 1 0 157.200 6.34771 1 3 1 0 51.7578 3.31521 -2 3 1 0 51.7578 3.31521 1 4 1 0 83.3477 4.86032 -2 4 1 0 83.3477 4.86032 1 5 1 0 20.2210 2.64219 -2 5 1 0 20.2210 2.64219 1 6 1 0 9.20636 2.66976 -2 6 1 0 9.20636 2.66976 1 7 1 0 25.9574 3.53982 -2 7 1 0 25.9574 3.53982 1 8 1 0 6.97232 2.85473 -2 8 1 0 6.97232 2.85473 1 9 1 0 6.87519 3.76849 -2 9 1 0 6.87519 3.76849 1 10 1 0 -9.3552 4.76154 -2 10 1 0 -9.3552 4.76154 1 0 2 0 2276.04 103.203 -2 0 2 0 2276.04 103.203 1 1 2 0 98.0748 2.50313 -2 1 2 0 98.0748 2.50313 1 2 2 0 1888.85 61.1766 -2 2 2 0 1888.85 61.1766 1 3 2 0 250.507 9.90368 -2 3 2 0 250.507 9.90368 1 4 2 0 20.7263 2.45881 -2 4 2 0 20.7263 2.45881 1 5 2 0 0.01354 1.57403 -2 5 2 0 0.01354 1.57403 1 6 2 0 665.967 24.7397 -2 6 2 0 665.967 24.7397 1 7 2 0 147.063 8.29201 -2 7 2 0 147.063 8.29201 1 8 2 0 288.982 13.5431 -2 8 2 0 288.982 13.5431 1 9 2 0 87.5411 7.89557 -2 9 2 0 87.5411 7.89557 1 10 2 0 3.50737 5.68051 -2 10 2 0 3.50737 5.68051 1 0 3 0 1.14544 0.28519 -2 0 3 0 1.14544 0.28519 1 1 3 0 3370.65 76.0381 -2 1 3 0 3370.65 76.0381 1 2 3 0 1077.21 35.3982 -2 2 3 0 1077.21 35.3982 1 3 3 0 380.630 13.8337 -2 3 3 0 380.630 13.8337 1 4 3 0 609.840 21.7926 -2 4 3 0 609.840 21.7926 1 5 3 0 37.2477 3.39037 -2 5 3 0 37.2477 3.39037 1 6 3 0 358.672 14.8237 -2 6 3 0 358.672 14.8237 1 7 3 0 102.638 6.68575 -2 7 3 0 102.638 6.68575 1 8 3 0 82.4150 6.21386 -2 8 3 0 82.4150 6.21386 1 9 3 0 79.0391 7.73474 -2 9 3 0 79.0391 7.73474 1 10 3 0 -4.7574 5.43319 -2 10 3 0 -4.7574 5.43319 1 0 4 0 2660.16 98.0254 -2 0 4 0 2660.16 98.0254 1 1 4 0 11.7036 0.90553 -2 1 4 0 11.7036 0.90553 1 2 4 0 972.749 28.7614 -2 2 4 0 972.749 28.7614 1 3 4 0 272.289 10.4096 -2 3 4 0 272.289 10.4096 1 4 4 0 87.6582 4.92773 -2 4 4 0 87.6582 4.92773 1 5 4 0 127.814 6.85843 -2 5 4 0 127.814 6.85843 1 6 4 0 433.110 17.5826 -2 6 4 0 433.110 17.5826 1 7 4 0 3.57266 2.55444 -2 7 4 0 3.57266 2.55444 1 8 4 0 68.8395 6.89061 -2 8 4 0 68.8395 6.89061 1 9 4 0 42.7690 5.97315 -2 9 4 0 42.7690 5.97315 1 10 4 0 3.94877 5.94690 -2 10 4 0 3.94877 5.94690 1 0 5 0 -0.5607 0.39802 -2 0 5 0 -0.5607 0.39802 1 1 5 0 7799.53 222.040 -2 1 5 0 7799.53 222.040 1 2 5 0 12.1555 1.38326 -2 2 5 0 12.1555 1.38326 1 3 5 0 554.021 19.4553 -2 3 5 0 554.021 19.4553 1 4 5 0 115.893 5.95785 -2 4 5 0 115.893 5.95785 1 5 5 0 66.6131 4.67121 -2 5 5 0 66.6131 4.67121 1 6 5 0 205.048 9.84565 -2 6 5 0 205.048 9.84565 1 7 5 0 335.271 14.8004 -2 7 5 0 335.271 14.8004 1 8 5 0 86.8204 8.01635 -2 8 5 0 86.8204 8.01635 1 9 5 0 67.8100 7.97959 -2 9 5 0 67.8100 7.97959 1 10 5 0 10.6200 4.29696 -2 10 5 0 10.6200 4.29696 1 0 6 0 68.0678 3.64454 -2 0 6 0 68.0678 3.64454 1 1 6 0 1056.82 30.9896 -2 1 6 0 1056.82 30.9896 1 2 6 0 247.694 8.34806 -2 2 6 0 247.694 8.34806 1 3 6 0 1660.61 48.8111 -2 3 6 0 1660.61 48.8111 1 4 6 0 16.0857 2.11367 -2 4 6 0 16.0857 2.11367 1 5 6 0 483.847 18.5831 -2 5 6 0 483.847 18.5831 1 6 6 0 75.0868 5.29925 -2 6 6 0 75.0868 5.29925 1 7 6 0 10.2067 2.88772 -2 7 6 0 10.2067 2.88772 1 8 6 0 0.79124 3.70884 -2 8 6 0 0.79124 3.70884 1 9 6 0 26.3773 5.40376 -2 9 6 0 26.3773 5.40376 1 10 6 0 11.3568 4.56423 -2 10 6 0 11.3568 4.56423 1 0 7 0 4.90266 1.25714 -2 0 7 0 4.90266 1.25714 1 1 7 0 1578.99 45.9388 -2 1 7 0 1578.99 45.9388 1 2 7 0 106.449 4.36974 -2 2 7 0 106.449 4.36974 1 3 7 0 211.362 7.78099 -2 3 7 0 211.362 7.78099 1 4 7 0 12.2715 2.08171 -2 4 7 0 12.2715 2.08171 1 5 7 0 146.342 7.55994 -2 5 7 0 146.342 7.55994 1 6 7 0 3.30140 2.08110 -2 6 7 0 3.30140 2.08110 1 7 7 0 174.612 9.30377 -2 7 7 0 174.612 9.30377 1 8 7 0 43.9077 6.19060 -2 8 7 0 43.9077 6.19060 1 9 7 0 21.6812 5.58199 -2 9 7 0 21.6812 5.58199 1 10 7 0 19.1813 5.11537 -2 10 7 0 19.1813 5.11537 1 0 8 0 162.925 7.43356 -2 0 8 0 162.925 7.43356 1 1 8 0 1183.40 34.8246 -2 1 8 0 1183.40 34.8246 1 2 8 0 448.994 14.2550 -2 2 8 0 448.994 14.2550 1 3 8 0 2864.35 92.5510 -2 3 8 0 2864.35 92.5510 1 4 8 0 329.134 12.9260 -2 4 8 0 329.134 12.9260 1 5 8 0 1438.27 49.0622 -2 5 8 0 1438.27 49.0622 1 6 8 0 89.9067 5.91508 -2 6 8 0 89.9067 5.91508 1 7 8 0 145.109 10.5698 -2 7 8 0 145.109 10.5698 1 8 8 0 5.73875 4.39053 -2 8 8 0 5.73875 4.39053 1 9 8 0 8.23326 4.71505 -2 9 8 0 8.23326 4.71505 1 10 8 0 37.3524 6.27627 -2 10 8 0 37.3524 6.27627 1 0 9 0 -0.5032 1.26271 -2 0 9 0 -0.5032 1.26271 1 1 9 0 546.280 16.9354 -2 1 9 0 546.280 16.9354 1 2 9 0 760.564 23.2696 -2 2 9 0 760.564 23.2696 1 3 9 0 104.955 4.76609 -2 3 9 0 104.955 4.76609 1 4 9 0 136.334 6.71712 -2 4 9 0 136.334 6.71712 1 5 9 0 92.4468 5.70272 -2 5 9 0 92.4468 5.70272 1 6 9 0 11.5349 2.07140 -2 6 9 0 11.5349 2.07140 1 7 9 0 53.1019 6.39072 -2 7 9 0 53.1019 6.39072 1 8 9 0 8.94170 4.44427 -2 8 9 0 8.94170 4.44427 1 9 9 0 9.55314 4.65182 -2 9 9 0 9.55314 4.65182 1 0 10 0 2.75951 1.44058 -2 0 10 0 2.75951 1.44058 1 1 10 0 262.185 8.98923 -2 1 10 0 262.185 8.98923 1 2 10 0 65.5789 3.40822 -2 2 10 0 65.5789 3.40822 1 3 10 0 1168.06 35.3321 -2 3 10 0 1168.06 35.3321 1 4 10 0 112.867 6.03774 -2 4 10 0 112.867 6.03774 1 5 10 0 541.368 20.6814 -2 5 10 0 541.368 20.6814 1 6 10 0 1.30274 2.08918 -2 6 10 0 1.30274 2.08918 1 7 10 0 28.1947 5.26514 -2 7 10 0 28.1947 5.26514 1 8 10 0 11.0892 4.58022 -2 8 10 0 11.0892 4.58022 1 9 10 0 10.8833 5.23312 -2 9 10 0 10.8833 5.23312 1 0 11 0 6.59523 1.73346 -2 0 11 0 6.59523 1.73346 1 1 11 0 124.117 5.14557 -2 1 11 0 124.117 5.14557 1 2 11 0 1044.63 31.6374 -2 2 11 0 1044.63 31.6374 1 3 11 0 60.4595 3.56750 -2 3 11 0 60.4595 3.56750 1 4 11 0 1072.68 37.1293 -2 4 11 0 1072.68 37.1293 1 5 11 0 85.2646 5.37538 -2 5 11 0 85.2646 5.37538 1 6 11 0 190.202 9.54307 -2 6 11 0 190.202 9.54307 1 7 11 0 2.05529 3.70751 -2 7 11 0 2.05529 3.70751 1 8 11 0 -4.7194 4.01993 -2 8 11 0 -4.7194 4.01993 1 9 11 0 9.00392 5.08382 -2 9 11 0 9.00392 5.08382 1 0 12 0 18.2248 2.48431 -2 0 12 0 18.2248 2.48431 1 1 12 0 -0.3685 0.96518 -2 1 12 0 -0.3685 0.96518 1 2 12 0 33.8300 2.71553 -2 2 12 0 33.8300 2.71553 1 3 12 0 285.116 10.3722 -2 3 12 0 285.116 10.3722 1 4 12 0 42.3458 3.30596 -2 4 12 0 42.3458 3.30596 1 5 12 0 246.411 11.1861 -2 5 12 0 246.411 11.1861 1 6 12 0 5.12406 3.48130 -2 6 12 0 5.12406 3.48130 1 7 12 0 2.84835 3.88501 -2 7 12 0 2.84835 3.88501 1 8 12 0 1.75385 4.19260 -2 8 12 0 1.75385 4.19260 1 9 12 0 4.02416 4.75988 -2 9 12 0 4.02416 4.75988 1 0 13 0 3.41198 1.79351 -2 0 13 0 3.41198 1.79351 1 1 13 0 16.2927 1.64229 -2 1 13 0 16.2927 1.64229 1 2 13 0 1085.83 33.1797 -2 2 13 0 1085.83 33.1797 1 3 13 0 64.2494 3.78692 -2 3 13 0 64.2494 3.78692 1 4 13 0 1407.12 42.8843 -2 4 13 0 1407.12 42.8843 1 5 13 0 35.8009 3.44481 -2 5 13 0 35.8009 3.44481 1 6 13 0 383.126 19.8106 -2 6 13 0 383.126 19.8106 1 7 13 0 13.3175 4.46333 -2 7 13 0 13.3175 4.46333 1 8 13 0 3.05802 4.28205 -2 8 13 0 3.05802 4.28205 1 9 13 0 -1.5681 4.82442 -2 9 13 0 -1.5681 4.82442 1 0 14 0 293.132 13.3848 -2 0 14 0 293.132 13.3848 1 1 14 0 1.55359 1.07339 -2 1 14 0 1.55359 1.07339 1 2 14 0 22.1585 2.45090 -2 2 14 0 22.1585 2.45090 1 3 14 0 0.73152 1.18560 -2 3 14 0 0.73152 1.18560 1 4 14 0 16.8401 2.32401 -2 4 14 0 16.8401 2.32401 1 5 14 0 1.11780 1.41557 -2 5 14 0 1.11780 1.41557 1 6 14 0 34.5431 5.34278 -2 6 14 0 34.5431 5.34278 1 7 14 0 -4.9625 3.78640 -2 7 14 0 -4.9625 3.78640 1 8 14 0 11.4979 4.75104 -2 8 14 0 11.4979 4.75104 1 9 14 0 6.29256 4.60432 -2 9 14 0 6.29256 4.60432 1 0 15 0 4.75840 1.97671 -2 0 15 0 4.75840 1.97671 1 1 15 0 28.1904 2.37420 -2 1 15 0 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112.937 8.42695 1 -7 8 10 0.35877 5.25433 -2 3 8 10 0.35877 5.25433 1 3 9 10 -7.3225 7.69312 -2 -7 9 10 -7.3225 7.69312 1 2 9 10 12.0190 6.72067 -2 -6 9 10 12.0190 6.72067 1 1 9 10 29.7363 6.80832 -2 -5 9 10 29.7363 6.80832 1 0 9 10 12.0547 6.46850 -2 -4 9 10 12.0547 6.46850 1 -1 9 10 15.2061 6.01152 -2 -3 9 10 15.2061 6.01152 1 -2 9 10 18.6764 4.45243 -2 -2 9 10 18.6764 4.45243 1 -3 9 10 9.62655 4.17546 -2 -1 9 10 9.62655 4.17546 1 -4 9 10 25.6400 4.80135 -2 0 9 10 25.6400 4.80135 1 -5 9 10 34.4011 5.53525 -2 1 9 10 34.4011 5.53525 1 -6 9 10 26.4729 5.14159 -2 2 9 10 26.4729 5.14159 1 -7 9 10 0.22762 4.51648 -2 3 9 10 0.22762 4.51648 1 3 10 10 15.2829 9.35569 -2 -7 10 10 15.2829 9.35569 1 2 10 10 65.9766 9.56813 -2 -6 10 10 65.9766 9.56813 1 1 10 10 11.9412 6.20607 -2 -5 10 10 11.9412 6.20607 1 0 10 10 80.2276 9.72449 -2 -4 10 10 80.2276 9.72449 1 -1 10 10 14.1037 6.31889 -2 -3 10 10 14.1037 6.31889 1 -2 10 10 33.1752 6.22519 -2 -2 10 10 33.1752 6.22519 1 -3 10 10 13.7019 4.40300 -2 -1 10 10 13.7019 4.40300 1 -4 10 10 43.1928 5.77504 -2 0 10 10 43.1928 5.77504 1 -5 10 10 7.94292 4.68846 -2 1 10 10 7.94292 4.68846 1 -6 10 10 59.1491 6.43319 -2 2 10 10 59.1491 6.43319 1 -7 10 10 23.9247 5.44612 -2 3 10 10 23.9247 5.44612 1 2 11 10 36.5034 8.22391 -2 -6 11 10 36.5034 8.22391 1 1 11 10 87.6837 10.6914 -2 -5 11 10 87.6837 10.6914 1 0 11 10 20.3401 6.54602 -2 -4 11 10 20.3401 6.54602 1 -1 11 10 32.1167 7.81564 -2 -3 11 10 32.1167 7.81564 1 -2 11 10 12.1735 5.57789 -2 -2 11 10 12.1735 5.57789 1 -3 11 10 31.5861 5.16494 -2 -1 11 10 31.5861 5.16494 1 -4 11 10 8.90503 4.41994 -2 0 11 10 8.90503 4.41994 1 -5 11 10 84.1727 7.37576 -2 1 11 10 84.1727 7.37576 1 -6 11 10 17.9288 4.91536 -2 2 11 10 17.9288 4.91536 1 2 12 10 30.5903 7.67844 -2 -6 12 10 30.5903 7.67844 1 1 12 10 14.5342 6.88792 -2 -5 12 10 14.5342 6.88792 1 0 12 10 32.6578 7.31876 -2 -4 12 10 32.6578 7.31876 1 -1 12 10 -0.7441 8.05912 -2 -3 12 10 -0.7441 8.05912 1 -2 12 10 14.4931 5.57336 -2 -2 12 10 14.4931 5.57336 1 -3 12 10 7.81046 4.15183 -2 -1 12 10 7.81046 4.15183 1 -4 12 10 8.33964 4.60673 -2 0 12 10 8.33964 4.60673 1 -5 12 10 4.71777 5.03474 -2 1 12 10 4.71777 5.03474 1 -6 12 10 24.2008 5.05045 -2 2 12 10 24.2008 5.05045 1 2 13 10 14.1132 7.01997 -2 -6 13 10 14.1132 7.01997 1 1 13 10 73.1505 9.85248 -2 -5 13 10 73.1505 9.85248 1 0 13 10 16.4102 6.58667 -2 -4 13 10 16.4102 6.58667 1 -1 13 10 54.2018 7.79613 -2 -3 13 10 54.2018 7.79613 1 -2 13 10 11.1187 5.45577 -2 -2 13 10 11.1187 5.45577 1 -3 13 10 43.4981 5.60661 -2 -1 13 10 43.4981 5.60661 1 -4 13 10 -2.0865 4.79042 -2 0 13 10 -2.0865 4.79042 1 -5 13 10 84.8349 7.49714 -2 1 13 10 84.8349 7.49714 1 -6 13 10 24.3004 5.50258 -2 2 13 10 24.3004 5.50258 1 1 14 10 15.8646 6.50576 -2 -5 14 10 15.8646 6.50576 1 0 14 10 7.11166 6.97903 -2 -4 14 10 7.11166 6.97903 1 -1 14 10 8.37444 7.08606 -2 -3 14 10 8.37444 7.08606 1 -2 14 10 -1.4784 6.67241 -2 -2 14 10 -1.4784 6.67241 1 -3 14 10 19.5441 5.72740 -2 -1 14 10 19.5441 5.72740 1 -4 14 10 6.99659 4.51506 -2 0 14 10 6.99659 4.51506 1 -5 14 10 12.2338 4.97322 -2 1 14 10 12.2338 4.97322 1 1 15 10 80.5369 9.83064 -2 -5 15 10 80.5369 9.83064 1 0 15 10 12.4948 6.58816 -2 -4 15 10 12.4948 6.58816 1 -1 15 10 49.3623 7.86360 -2 -3 15 10 49.3623 7.86360 1 -2 15 10 16.5812 6.98533 -2 -2 15 10 16.5812 6.98533 1 -3 15 10 29.8036 6.09739 -2 -1 15 10 29.8036 6.09739 1 -4 15 10 6.05867 4.46703 -2 0 15 10 6.05867 4.46703 1 -5 15 10 56.8465 6.42430 -2 1 15 10 56.8465 6.42430 1 0 16 10 -5.8067 6.64831 -2 -4 16 10 -5.8067 6.64831 1 -1 16 10 37.6800 6.83201 -2 -3 16 10 37.6800 6.83201 1 -2 16 10 1.77511 5.47754 -2 -2 16 10 1.77511 5.47754 1 -3 16 10 38.0491 6.79330 -2 -1 16 10 38.0491 6.79330 1 -4 16 10 16.3139 4.77523 -2 0 16 10 16.3139 4.77523 1 -1 17 10 18.0648 6.55707 -2 -3 17 10 18.0648 6.55707 1 -2 17 10 14.6680 5.62728 -2 -2 17 10 14.6680 5.62728 1 -3 17 10 23.1014 6.20823 -2 -1 17 10 23.1014 6.20823 1 -7 0 11 6.06737 5.49902 1 -6 0 11 5.58889 5.12347 1 -5 0 11 0.80918 5.27000 1 -4 0 11 1.28853 2.46004 1 -3 0 11 -2.4845 2.52734 1 -2 0 11 -4.5876 4.66502 1 -1 0 11 1.15316 4.98088 1 0 0 11 2.59381 3.85500 1 1 0 11 0.61530 5.93880 1 2 0 11 0.31368 5.23682 1 -7 1 11 1.80873 3.79600 1 -6 1 11 90.0495 9.59140 1 -5 1 11 14.9452 4.48598 1 -4 1 11 22.7146 3.46576 1 -3 1 11 6.02436 2.59782 1 -2 1 11 5.83501 2.81399 1 -1 1 11 10.7102 5.67091 1 0 1 11 45.4082 6.06483 1 1 1 11 57.3104 7.61516 1 2 1 11 10.3519 4.88421 1 -7 2 11 19.7772 5.34647 1 -6 2 11 2.91613 3.25790 1 -5 2 11 20.9460 7.52600 1 -4 2 11 3.74165 3.25287 1 -3 2 11 6.39556 3.09273 1 -2 2 11 13.4595 3.50053 1 -1 2 11 2.89144 2.53178 1 0 2 11 19.6379 5.49931 1 1 2 11 6.77128 3.45071 1 2 2 11 6.24946 3.73898 1 -7 3 11 -9.2670 3.48888 1 -6 3 11 35.0471 10.6739 1 -5 3 11 21.1477 7.95185 1 -4 3 11 5.47478 3.62451 1 -3 3 11 5.44612 3.00949 1 -2 3 11 10.5990 3.04326 1 -1 3 11 -0.4322 2.05224 1 0 3 11 25.7431 6.26690 1 1 3 11 26.6303 6.67642 1 2 3 11 9.14686 3.21452 1 -6 4 11 3.39555 6.61765 1 -5 4 11 46.0666 7.58731 1 -4 4 11 1.72840 2.98659 1 -3 4 11 7.70916 3.03549 1 -2 4 11 11.6577 3.37273 1 -1 4 11 3.44282 2.33272 1 0 4 11 24.2778 4.45037 1 1 4 11 8.33271 4.27133 1 2 4 11 8.77211 3.31625 1 -6 5 11 0.84068 5.35780 1 -5 5 11 20.7013 5.03166 1 -4 5 11 6.16696 3.50356 1 -3 5 11 33.3181 6.73140 1 -2 5 11 7.58528 2.55240 1 -1 5 11 3.46442 2.55160 1 0 5 11 6.54093 2.87480 1 1 5 11 10.7671 3.01136 1 2 5 11 2.54182 3.74341 1 -6 6 11 11.0856 6.48477 1 -5 6 11 29.1730 6.37167 1 -4 6 11 0.14536 4.32781 1 -3 6 11 5.05469 4.25610 1 -2 6 11 4.91445 2.52867 1 -1 6 11 -1.3566 2.57006 1 0 6 11 15.7216 3.49888 1 1 6 11 10.7031 2.98911 1 2 6 11 20.2325 3.82551 1 -6 7 11 -6.1144 4.19391 1 -5 7 11 27.1531 5.75399 1 -4 7 11 4.79378 3.63845 1 -3 7 11 51.0860 6.27324 1 -2 7 11 8.95360 3.01137 1 -1 7 11 18.7437 4.00125 1 0 7 11 5.65328 3.31606 1 1 7 11 0.05145 2.71789 1 2 7 11 6.15191 3.20041 1 -6 8 11 -3.5363 3.24382 1 -5 8 11 3.12317 3.44397 1 -4 8 11 12.1654 4.71965 1 -3 8 11 2.80885 2.70684 1 -2 8 11 4.00456 2.79380 1 -1 8 11 4.00921 2.94836 1 0 8 11 5.19693 2.85683 1 1 8 11 4.86270 2.82098 1 -5 9 11 27.8803 6.13988 1 -4 9 11 14.4897 5.22802 1 -3 9 11 45.3992 5.89175 1 -2 9 11 10.9711 4.19344 1 -1 9 11 25.9592 4.48234 1 0 9 11 4.92549 2.62601 1 1 9 11 0.58621 2.67402 1 -5 10 11 -0.2803 3.77958 1 -4 10 11 28.7462 7.27401 1 -3 10 11 2.26136 3.05936 1 -2 10 11 20.0568 4.90535 1 -1 10 11 9.07745 3.10403 1 0 10 11 4.96234 3.14288 1 1 10 11 -5.4152 2.47643 1 -5 11 11 12.2045 4.41747 1 -4 11 11 8.20142 4.31474 1 -3 11 11 11.7568 4.00575 1 -2 11 11 9.16439 4.06572 1 -1 11 11 7.51132 2.74318 1 0 11 11 5.39400 2.87854 1 -4 12 11 38.1580 8.30010 1 -3 12 11 3.43734 3.18202 1 -2 12 11 19.9531 5.02656 1 -1 12 11 7.85180 3.61997 1 0 12 11 6.12589 2.96579 1 -3 13 11 5.53517 3.10130 1 -2 13 11 7.90184 3.88113 1 -1 13 11 1.49840 2.95745 1 -2 0 12 4.60053 11.9477 -2 -3 0 12 4.60053 11.9477 1 -3 0 12 43.3198 13.9783 -2 -2 0 12 43.3198 13.9783 1 -4 0 12 18.5800 12.0946 -2 -1 0 12 18.5800 12.0946 1 -5 0 12 -6.9589 10.4892 -2 0 0 12 -6.9589 10.4892 1 -2 1 12 -0.6779 7.83222 -2 -3 1 12 -0.6779 7.83222 1 -3 1 12 -4.5079 8.56208 -2 -2 1 12 -4.5079 8.56208 1 -4 1 12 1.95174 7.86153 -2 -1 1 12 1.95174 7.86153 1 -5 1 12 17.5697 7.61910 -2 0 1 12 17.5697 7.61910 1 0 2 12 12.5976 8.60239 -2 -5 2 12 12.5976 8.60239 1 -1 2 12 21.2297 10.9429 -2 -4 2 12 21.2297 10.9429 1 -2 2 12 17.9844 12.8618 -2 -3 2 12 17.9844 12.8618 1 -3 2 12 33.4358 9.34975 -2 -2 2 12 33.4358 9.34975 1 -4 2 12 46.4530 9.27236 -2 -1 2 12 46.4530 9.27236 1 -5 2 12 25.7600 8.04715 -2 0 2 12 25.7600 8.04715 1 0 3 12 21.4675 9.41417 -2 -5 3 12 21.4675 9.41417 1 -1 3 12 13.8578 6.77323 -2 -4 3 12 13.8578 6.77323 1 -2 3 12 22.1559 12.2782 -2 -3 3 12 22.1559 12.2782 1 -3 3 12 13.0995 8.53791 -2 -2 3 12 13.0995 8.53791 1 -4 3 12 6.51079 7.94385 -2 -1 3 12 6.51079 7.94385 1 -5 3 12 7.43508 6.45449 -2 0 3 12 7.43508 6.45449 1 -1 4 12 30.7154 7.87725 -2 -4 4 12 30.7154 7.87725 1 -2 4 12 1.89811 6.28017 -2 -3 4 12 1.89811 6.28017 1 -3 4 12 8.58158 8.28139 -2 -2 4 12 8.58158 8.28139 1 -4 4 12 39.8075 9.19383 -2 -1 4 12 39.8075 9.19383 1 0 4 12 4.73472 4.12877 1 -1 5 12 14.5466 7.37585 -2 -4 5 12 14.5466 7.37585 1 -2 5 12 35.8287 7.47816 -2 -3 5 12 35.8287 7.47816 1 -3 5 12 15.4969 5.59056 -2 -2 5 12 15.4969 5.59056 1 -4 5 12 23.5716 8.72103 -2 -1 5 12 23.5716 8.72103 1 -1 6 12 21.6991 7.36602 -2 -4 6 12 21.6991 7.36602 1 -2 6 12 5.43157 6.33653 -2 -3 6 12 5.43157 6.33653 1 -3 6 12 10.6332 6.32895 -2 -2 6 12 10.6332 6.32895 1 -4 6 12 38.2183 5.97075 -2 -1 6 12 38.2183 5.97075 1 -2 7 12 22.5840 6.80452 -2 -3 7 12 22.5840 6.80452 1 -3 7 12 13.3406 6.57036 -2 -2 7 12 13.3406 6.57036 1 -1 7 12 7.76828 3.38339 1 -2 8 12 7.87463 10.0820 -2 -3 8 12 7.87463 10.0820 1 -3 8 12 11.0868 9.46450 -2 -2 8 12 11.0868 9.46450 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 87747 _shelx_res_file ; TITL Compound_I CELL 0.71073 8.9423 24.0583 10.3749 90.000 103.656 90.000 ZERR 4.00 0.0012 0.0029 0.0013 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N I UNIT 84 108 4 8 LIST 8 TEMP 25 SIZE 0.042 0.222 0.322 MERG 0 OMIT -1 16 3 OMIT 1 6 2 OMIT 1 0 0 OMIT -1 9 5 OMIT 2 3 2 OMIT -1 10 3 OMIT 0 1 2 OMIT -1 15 3 OMIT -3 3 2 OMIT 0 16 3 OMIT 0 10 3 ACTA L.S. 20 BOND BOND $H EQIV $1 -x,-y+1,-z BIND I1 I2_$1 CONF HTAB C1 I2 EQIV $2 -x, -y+1, -z+1 HTAB C1 I2_$2 HTAB C21 I2_$2 EQIV $3 x-1,y,z HTAB C20 I2_$3 EQIV $4 x-1, -y+1/2, z-1/2 HTAB C2 C9_$4 HTAB C4 C10_$4 HTAB C19 C8_$4 HTAB C19 C15_$4 EQIV $5 x-1, y, Z HTAB C4 C10_$5 EQIV $6 x+1, -y+1/2, z+1/2 HTAB C10 C17_$6 HTAB C10 C18_$6 MPLA 6 C7 > C12 MPLA 6 C4 > C7 C13 MPLA 6 C13 > C18 FMAP 2 PLAN 5 WGHT 0.051500 2.932100 BASF 0.37374 FVAR 0.26204 I1 4 -0.299571 0.443388 0.017398 11.00000 0.05591 0.06585 = 0.06053 0.01177 0.02018 0.00392 I2 4 0.174936 0.514763 0.269008 11.00000 0.05856 0.06185 = 0.06316 0.00425 0.02282 0.00153 N1 3 -0.341123 0.441545 0.307039 11.00000 0.04052 0.08110 = 0.04639 0.02004 0.01167 0.00214 C1 1 -0.173345 0.431911 0.363077 11.00000 0.04479 0.07771 = 0.06871 0.01381 0.01505 -0.00593 AFIX 23 H1A 2 -0.115901 0.452466 0.310311 11.00000 -1.20000 H1B 2 -0.145922 0.446889 0.452368 11.00000 -1.20000 AFIX 0 C2 1 -0.125195 0.373056 0.367808 11.00000 0.05789 0.05567 = 0.10559 -0.00108 0.02417 0.00333 AFIX 23 H2A 2 -0.140674 0.358352 0.278574 11.00000 -1.20000 H2B 2 -0.185959 0.351182 0.415261 11.00000 -1.20000 AFIX 0 C3 1 0.046655 0.369931 0.439369 11.00000 0.05689 0.06915 = 0.07474 0.01748 0.00707 0.01200 AFIX 23 H3A 2 0.102868 0.397059 0.400137 11.00000 -1.20000 H3B 2 0.057787 0.380034 0.531665 11.00000 -1.20000 AFIX 0 C4 1 0.118211 0.313432 0.433252 11.00000 0.05432 0.06537 = 0.15825 0.02278 0.03580 0.00632 AFIX 23 H4A 2 0.101251 0.301926 0.341327 11.00000 -1.20000 H4B 2 0.068119 0.286629 0.478899 11.00000 -1.20000 AFIX 0 C5 1 0.289247 0.313544 0.495665 11.00000 0.04027 0.04260 = 0.12338 0.01160 0.02172 0.00238 AFIX 43 H5 2 0.338120 0.347825 0.511957 11.00000 -1.20000 AFIX 0 C6 1 0.374302 0.268455 0.528736 11.00000 0.04657 0.03773 = 0.08246 0.00982 0.01933 0.00464 C7 1 0.545150 0.270268 0.581340 11.00000 0.05200 0.03750 = 0.06946 0.01012 0.01917 -0.00217 C8 1 0.639764 0.232173 0.543503 11.00000 0.05082 0.05472 = 0.09029 -0.00630 0.00946 0.00432 AFIX 43 H8 2 0.596613 0.203076 0.488072 11.00000 -1.20000 AFIX 0 C9 1 0.800268 0.235888 0.586207 11.00000 0.05128 0.08327 = 0.13995 0.02244 0.02596 0.01688 AFIX 43 H9 2 0.863645 0.210902 0.555973 11.00000 -1.20000 AFIX 0 C10 1 0.862309 0.277779 0.674739 11.00000 0.06607 0.07740 = 0.12923 0.02184 -0.01375 -0.02837 AFIX 43 H10 2 0.968295 0.279754 0.707900 11.00000 -1.20000 AFIX 0 C11 1 0.770102 0.315764 0.713260 11.00000 0.09975 0.05390 = 0.11581 -0.00660 -0.00079 -0.00768 AFIX 43 H11 2 0.812752 0.344568 0.769877 11.00000 -1.20000 AFIX 0 C12 1 0.612191 0.311571 0.668084 11.00000 0.07495 0.07398 = 0.08728 -0.00194 0.01922 -0.00707 AFIX 43 H12 2 0.549546 0.337270 0.696939 11.00000 -1.20000 AFIX 0 C13 1 0.302627 0.211451 0.508564 11.00000 0.05569 0.04032 = 0.06685 0.01374 0.01114 0.01160 C14 1 0.272336 0.184718 0.615604 11.00000 0.07869 0.05314 = 0.10108 -0.01162 0.04273 -0.00371 AFIX 43 H14 2 0.299259 0.201164 0.699008 11.00000 -1.20000 AFIX 0 C15 1 0.200450 0.132320 0.600004 11.00000 0.08525 0.04148 = 0.15172 0.01067 0.05844 -0.00917 AFIX 43 H15 2 0.183994 0.113545 0.673790 11.00000 -1.20000 AFIX 0 C16 1 0.155125 0.109093 0.478226 11.00000 0.05334 0.06270 = 0.15539 -0.00518 -0.00423 -0.00150 AFIX 43 H16 2 0.101007 0.075745 0.468073 11.00000 -1.20000 AFIX 0 C17 1 0.188771 0.134674 0.367811 11.00000 0.13541 0.07178 = 0.10801 -0.00217 -0.03793 0.00088 AFIX 43 H17 2 0.161408 0.118408 0.284222 11.00000 -1.20000 AFIX 0 C18 1 0.265874 0.186143 0.387965 11.00000 0.11616 0.06886 = 0.07479 0.00077 -0.00228 -0.00097 AFIX 43 H18 2 0.292559 0.203408 0.316370 11.00000 -1.20000 AFIX 0 C19 1 -0.407728 0.419204 0.171794 11.00000 0.04898 0.07983 = 0.07276 0.02372 0.02925 -0.00538 AFIX 23 H19A 2 -0.514843 0.430419 0.145959 11.00000 -1.20000 H19B 2 -0.405807 0.378947 0.177098 11.00000 -1.20000 AFIX 0 C20 1 -0.364849 0.504813 0.305935 11.00000 0.06646 0.07094 = 0.08877 0.00828 0.02679 0.00903 AFIX 137 H20A 2 -0.472253 0.513096 0.274030 11.00000 -1.50000 H20B 2 -0.307766 0.521785 0.248796 11.00000 -1.50000 H20C 2 -0.329352 0.519089 0.394290 11.00000 -1.50000 AFIX 0 C21 1 -0.431224 0.416523 0.399495 11.00000 0.05588 0.09105 = 0.07234 0.03158 0.02495 -0.00580 AFIX 137 H21A 2 -0.538229 0.425589 0.368350 11.00000 -1.50000 H21B 2 -0.393620 0.431260 0.487162 11.00000 -1.50000 H21C 2 -0.418898 0.376870 0.401543 11.00000 -1.50000 AFIX 0 HKLF 5 REM Compound_I REM R1 = 0.0595 for 2941 Fo > 4sig(Fo) and 0.0864 for all 3961 data REM 220 parameters refined using 0 restraints END WGHT 0.0517 2.9131 REM Highest difference peak 0.816, deepest hole -0.804, 1-sigma level 0.143 Q1 1 -0.3403 0.4398 -0.1109 11.00000 0.05 0.82 Q2 1 0.1634 0.5169 0.3722 11.00000 0.05 0.77 Q3 1 -0.2017 0.4887 0.3158 11.00000 0.05 0.65 Q4 1 0.2072 0.5575 0.2216 11.00000 0.05 0.61 Q5 1 -0.3368 0.4012 0.1093 11.00000 0.05 0.55 ; _shelx_res_checksum 50552 _shelxl_version_number 201.4 data_Global _journal_date_recd_electronic 2015-07-22 _journal_date_accepted 2015-09-14 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2015 _journal_volume 71 _journal_issue 10 _journal_page_first 1230 _journal_page_last 1235 _journal_paper_category GO _journal_paper_doi 10.1107/S2056989015017181 _journal_coeditor_code SU5179 _publ_contact_author_name 'Luz Amalia R\'ios-V\'asquez' _publ_contact_author_address ; Departamento de Qu\'imica, Universidad de Caldas, Manizales, Caldas, Colombia ; _publ_contact_author_email amalia.rios@ucaldas.edu.co _publ_contact_author_fax '(+57)68781520' _publ_contact_author_phone '3117339680' _publ_section_title ; Crystal structures of three new N-halomethylated quaternary ammonium salts ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'M\'unera-Orozco, Carolina' . ; Departamento de Qu\'imica, Universidad de Caldas, Manizales, Caldas, Colombia ; 'Ocampo-Cardona, Rogelio' . ; Departamento de Qu\'imica, Universidad de Caldas, Manizales, Caldas, Colombia ; 'Cede\~no, David L.' ; Current address: Millennium Pain Center, Basic Science, 1015 S Mercer Ave Bloomington, IL 61701 USA. ; ; Department of Chemistry, Illinois State University, Normal, Illinois, USA ; 'Toscano, Rub\'en A.' . ; Instituto de Qu\'imica, UNAM, Circuito Exterior, Ciudad Universitaria, Delegaci\'on Coyoac\'an, C.P. 04510, M\'exico, D.F., Mexico ; 'R\'ios-V\'asquez, Luz Amalia' . ; Departamento de Qu\'imica, Universidad de Caldas, Manizales, Caldas, Colombia ; _publ_section_synopsis ; In the crystals of the title N-halomethylated quaternary ammonium salts, there are short I...I^-^ interactions of 3.564(4), 3.506(1) and 3.55781) \%A for compounds (I), (II) and (III), respectively. In (I), molecules are linked by C---H...I^-^ and C---H...\p interactions, together with the I...I^-^ short contacts, forming ribbons along [100]. In (II), there are only C---H...I^-^ interactions, which together with the I...I^-^ short contacts, lead to the formation of helices along [010]. In (III), apart from the I...I^-^ short contacts, there are no other significant intermolecular interactions present. ;