data_AD_0m_a _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H27 N2, Br' _chemical_formula_sum 'C20 H27 Br N2' _chemical_formula_weight 375.34 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3429(8) _cell_length_b 16.4241(13) _cell_length_c 10.7998(8) _cell_angle_alpha 90 _cell_angle_beta 104.481(2) _cell_angle_gamma 90 _cell_volume 1776.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 2.309 _cell_measurement_theta_max 25.483 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_F_000 784 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 2.316 _shelx_estimated_absorpt_T_min 0.723 _shelx_estimated_absorpt_T_max 0.934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'SADABS. Ver. 2014/5. (Krause et al., 2015)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Microfocus sealed tube' _diffrn_measurement_device_type 'Bruker AXS D8 Quest diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 69444 _diffrn_reflns_av_unetI/netI 0.0572 _diffrn_reflns_av_R_equivalents 0.1216 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.382 _diffrn_reflns_theta_max 28.345 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4412 _reflns_number_gt 2815 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex3 v2017.3-0 (Bruker, 2017)' _computing_cell_refinement 'SAINT V8.38A (Bruker, 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2015)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+1.9140P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4412 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7403(2) 0.40367(12) 0.6090(2) 0.0222(5) Uani 1 1 d . . . . . N2 N 0.8299(2) 0.34475(13) 0.4689(2) 0.0279(5) Uani 1 1 d . . . . . C1 C 0.8446(3) 0.40109(15) 0.5581(3) 0.0270(6) Uani 1 1 d . . . . . H1 H 0.918873 0.434837 0.582509 0.032 Uiso 1 1 calc R U . . . C2 C 0.7070(2) 0.30730(15) 0.4571(3) 0.0251(6) Uani 1 1 d . . . . . C3 C 0.6447(3) 0.24483(16) 0.3785(3) 0.0319(6) Uani 1 1 d . . . . . H3 H 0.684677 0.219361 0.320757 0.038 Uiso 1 1 calc R U . . . C4 C 0.5206(3) 0.22256(17) 0.3905(3) 0.0356(7) Uani 1 1 d . . . . . H4 H 0.475627 0.180457 0.340079 0.043 Uiso 1 1 calc R U . . . C5 C 0.4604(3) 0.26104(17) 0.4759(3) 0.0337(7) Uani 1 1 d . . . . . H5 H 0.375346 0.244645 0.479521 0.040 Uiso 1 1 calc R U . . . C6 C 0.5219(3) 0.32246(16) 0.5550(3) 0.0281(6) Uani 1 1 d . . . . . H6 H 0.481104 0.347720 0.612359 0.034 Uiso 1 1 calc R U . . . C7 C 0.6486(2) 0.34503(14) 0.5450(2) 0.0223(5) Uani 1 1 d . . . . . C8 C 0.9271(3) 0.3308(2) 0.3913(3) 0.0469(9) Uani 1 1 d . . . . . H8 H 0.999163 0.370538 0.419613 0.056 Uiso 1 1 calc R U . . . C9 C 0.9884(4) 0.2476(3) 0.4185(5) 0.0891(16) Uani 1 1 d . . . . . H9A H 1.023791 0.241134 0.508987 0.134 Uiso 1 1 calc R U . . . H9B H 1.058990 0.241616 0.375977 0.134 Uiso 1 1 calc R U . . . H9C H 0.921421 0.206861 0.387809 0.134 Uiso 1 1 calc R U . . . C10 C 0.8620(5) 0.3490(3) 0.2524(4) 0.0798(14) Uani 1 1 d . . . . . H10A H 0.792055 0.310261 0.220503 0.120 Uiso 1 1 calc R U . . . H10B H 0.927493 0.345350 0.203429 0.120 Uiso 1 1 calc R U . . . H10C H 0.825001 0.402933 0.244991 0.120 Uiso 1 1 calc R U . . . C11 C 0.7240(2) 0.46117(15) 0.7113(2) 0.0215(5) Uani 1 1 d . . . . . C12 C 0.6963(3) 0.41267(16) 0.8225(2) 0.0270(6) Uani 1 1 d . . . . . H12A H 0.769933 0.375822 0.856510 0.032 Uiso 1 1 calc R U . . . H12B H 0.615788 0.380560 0.792962 0.032 Uiso 1 1 calc R U . . . C13 C 0.6082(3) 0.51883(15) 0.6567(2) 0.0259(6) Uani 1 1 d . . . . . H13A H 0.526734 0.487917 0.625140 0.031 Uiso 1 1 calc R U . . . H13B H 0.626105 0.549357 0.585851 0.031 Uiso 1 1 calc R U . . . C14 C 0.8516(2) 0.51056(16) 0.7581(2) 0.0262(6) Uani 1 1 d . . . . . H14A H 0.869823 0.541375 0.687742 0.031 Uiso 1 1 calc R U . . . H14B H 0.926356 0.474312 0.790974 0.031 Uiso 1 1 calc R U . . . C15 C 0.6794(3) 0.47155(17) 0.9270(3) 0.0308(6) Uani 1 1 d . . . . . H15 H 0.660744 0.440687 0.998266 0.037 Uiso 1 1 calc R U . . . C16 C 0.5628(3) 0.52880(18) 0.8718(3) 0.0342(7) Uani 1 1 d . . . . . H16A H 0.481565 0.497457 0.841589 0.041 Uiso 1 1 calc R U . . . H16B H 0.549967 0.565679 0.937893 0.041 Uiso 1 1 calc R U . . . C17 C 0.8072(3) 0.52068(19) 0.9745(3) 0.0356(7) Uani 1 1 d . . . . . H17A H 0.797566 0.557611 1.041741 0.043 Uiso 1 1 calc R U . . . H17B H 0.881350 0.484349 1.009382 0.043 Uiso 1 1 calc R U . . . C18 C 0.8346(3) 0.56865(17) 0.8637(3) 0.0321(6) Uani 1 1 d . . . . . H18 H 0.916791 0.600282 0.894072 0.039 Uiso 1 1 calc R U . . . C19 C 0.7194(3) 0.62642(17) 0.8092(3) 0.0366(7) Uani 1 1 d . . . . . H19A H 0.737969 0.657333 0.739119 0.044 Uiso 1 1 calc R U . . . H19B H 0.708829 0.664404 0.874784 0.044 Uiso 1 1 calc R U . . . C20 C 0.5917(3) 0.57724(16) 0.7619(3) 0.0323(6) Uani 1 1 d . . . . . H20 H 0.517157 0.614322 0.727470 0.039 Uiso 1 1 calc R U . . . Br1 Br 0.79005(3) 0.57877(2) 0.35804(4) 0.05647(14) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0226(11) 0.0187(11) 0.0276(11) -0.0022(9) 0.0105(9) -0.0007(8) N2 0.0278(12) 0.0234(11) 0.0365(13) -0.0056(10) 0.0157(10) -0.0024(9) C1 0.0258(14) 0.0231(14) 0.0348(15) -0.0037(12) 0.0128(12) -0.0039(11) C2 0.0257(13) 0.0171(12) 0.0327(15) 0.0012(11) 0.0077(11) -0.0003(10) C3 0.0412(16) 0.0187(13) 0.0367(16) -0.0033(12) 0.0112(13) 0.0001(12) C4 0.0390(16) 0.0221(14) 0.0428(18) -0.0034(13) 0.0047(13) -0.0092(12) C5 0.0281(15) 0.0297(15) 0.0421(17) 0.0022(13) 0.0069(13) -0.0097(12) C6 0.0254(14) 0.0252(14) 0.0350(15) 0.0024(12) 0.0099(12) -0.0018(11) C7 0.0227(13) 0.0146(12) 0.0286(14) 0.0014(10) 0.0045(11) -0.0011(10) C8 0.0439(18) 0.048(2) 0.061(2) -0.0246(17) 0.0354(17) -0.0162(15) C9 0.062(3) 0.070(3) 0.147(5) -0.041(3) 0.048(3) 0.012(2) C10 0.101(3) 0.101(3) 0.055(3) -0.026(2) 0.053(2) -0.047(3) C11 0.0218(13) 0.0195(12) 0.0242(13) -0.0012(11) 0.0074(10) 0.0007(10) C12 0.0234(13) 0.0260(14) 0.0326(15) 0.0072(12) 0.0087(11) 0.0020(11) C13 0.0266(14) 0.0230(13) 0.0257(14) 0.0031(11) 0.0019(11) 0.0020(11) C14 0.0214(13) 0.0293(14) 0.0288(14) -0.0040(12) 0.0079(11) -0.0041(11) C15 0.0299(15) 0.0416(16) 0.0225(14) 0.0041(12) 0.0095(11) 0.0011(12) C16 0.0268(14) 0.0418(17) 0.0364(16) -0.0080(14) 0.0123(12) 0.0038(13) C17 0.0294(15) 0.0496(18) 0.0264(15) -0.0050(14) 0.0044(12) 0.0017(13) C18 0.0288(14) 0.0358(16) 0.0307(15) -0.0088(13) 0.0056(12) -0.0088(12) C19 0.0485(18) 0.0244(14) 0.0377(17) -0.0071(13) 0.0123(14) -0.0018(13) C20 0.0311(14) 0.0274(14) 0.0359(16) -0.0025(13) 0.0035(12) 0.0121(12) Br1 0.0449(2) 0.0641(3) 0.0601(2) 0.0042(2) 0.01255(16) -0.00527(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.328(3) . ? N1 C7 1.406(3) . ? N1 C11 1.495(3) . ? N2 C1 1.317(3) . ? N2 C2 1.388(3) . ? N2 C8 1.478(3) . ? C1 H1 0.9300 . ? C2 C3 1.384(4) . ? C2 C7 1.392(4) . ? C3 C4 1.371(4) . ? C3 H3 0.9300 . ? C4 C5 1.387(4) . ? C4 H4 0.9300 . ? C5 C6 1.372(4) . ? C5 H5 0.9300 . ? C6 C7 1.392(4) . ? C6 H6 0.9300 . ? C8 C9 1.505(5) . ? C8 C10 1.513(5) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C14 1.524(3) . ? C11 C13 1.525(3) . ? C11 C12 1.527(3) . ? C12 C15 1.529(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C20 1.529(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C18 1.530(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C17 1.524(4) . ? C15 C16 1.527(4) . ? C15 H15 0.9800 . ? C16 C20 1.520(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.518(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.522(4) . ? C18 H18 0.9800 . ? C19 C20 1.523(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C7 107.0(2) . . ? C1 N1 C11 125.4(2) . . ? C7 N1 C11 127.5(2) . . ? C1 N2 C2 108.3(2) . . ? C1 N2 C8 123.5(2) . . ? C2 N2 C8 128.0(2) . . ? N2 C1 N1 111.6(2) . . ? N2 C1 H1 124.2 . . ? N1 C1 H1 124.2 . . ? C3 C2 N2 131.3(2) . . ? C3 C2 C7 122.2(2) . . ? N2 C2 C7 106.5(2) . . ? C4 C3 C2 116.3(3) . . ? C4 C3 H3 121.8 . . ? C2 C3 H3 121.8 . . ? C3 C4 C5 121.8(3) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 122.2(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 116.5(3) . . ? C5 C6 H6 121.7 . . ? C7 C6 H6 121.7 . . ? C6 C7 C2 120.8(2) . . ? C6 C7 N1 132.6(2) . . ? C2 C7 N1 106.6(2) . . ? N2 C8 C9 110.1(3) . . ? N2 C8 C10 109.5(3) . . ? C9 C8 C10 115.7(3) . . ? N2 C8 H8 107.0 . . ? C9 C8 H8 107.0 . . ? C10 C8 H8 107.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C14 109.46(19) . . ? N1 C11 C13 109.2(2) . . ? C14 C11 C13 109.2(2) . . ? N1 C11 C12 109.3(2) . . ? C14 C11 C12 109.5(2) . . ? C13 C11 C12 110.2(2) . . ? C11 C12 C15 109.2(2) . . ? C11 C12 H12A 109.8 . . ? C15 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? C15 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C11 C13 C20 109.0(2) . . ? C11 C13 H13A 109.9 . . ? C20 C13 H13A 109.9 . . ? C11 C13 H13B 109.9 . . ? C20 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C11 C14 C18 109.1(2) . . ? C11 C14 H14A 109.9 . . ? C18 C14 H14A 109.9 . . ? C11 C14 H14B 109.9 . . ? C18 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C17 C15 C16 109.8(2) . . ? C17 C15 C12 109.5(2) . . ? C16 C15 C12 109.0(2) . . ? C17 C15 H15 109.5 . . ? C16 C15 H15 109.5 . . ? C12 C15 H15 109.5 . . ? C20 C16 C15 109.7(2) . . ? C20 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? C20 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C18 C17 C15 109.1(2) . . ? C18 C17 H17A 109.9 . . ? C15 C17 H17A 109.9 . . ? C18 C17 H17B 109.9 . . ? C15 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C17 C18 C19 110.2(2) . . ? C17 C18 C14 110.1(2) . . ? C19 C18 C14 109.0(2) . . ? C17 C18 H18 109.2 . . ? C19 C18 H18 109.2 . . ? C14 C18 H18 109.2 . . ? C18 C19 C20 109.2(2) . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? C16 C20 C19 109.8(2) . . ? C16 C20 C13 109.4(2) . . ? C19 C20 C13 109.5(2) . . ? C16 C20 H20 109.4 . . ? C19 C20 H20 109.4 . . ? C13 C20 H20 109.4 . . ? _refine_diff_density_max 0.326 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.068 _shelx_res_file ; TITL AD_0m_a.res in P2(1)/n AD_0m_a.res created by SHELXL-2016/6 at 08:03:43 on 24-Aug-2019 CELL 0.71073 10.3429 16.4241 10.7998 90.000 104.481 90.000 ZERR 4.000 0.0008 0.0013 0.0008 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N Br UNIT 80 108 8 4 OMIT -1 0 1 OMIT 0 1 1 OMIT -1 1 1 L.S. 3 ACTA BOND $H FMAP 2 PLAN 10 SIZE 0.15 0.077 0.030 TEMP 23.000 WGHT 0.026700 1.914000 FVAR 0.44802 N1 3 0.740317 0.403669 0.608981 11.00000 0.02256 0.01868 = 0.02764 -0.00223 0.01048 -0.00074 N2 3 0.829854 0.344755 0.468869 11.00000 0.02782 0.02341 = 0.03647 -0.00564 0.01571 -0.00242 C1 1 0.844646 0.401086 0.558133 11.00000 0.02585 0.02312 = 0.03477 -0.00372 0.01277 -0.00386 AFIX 43 H1 2 0.918873 0.434837 0.582509 11.00000 -1.20000 AFIX 0 C2 1 0.707025 0.307301 0.457117 11.00000 0.02571 0.01710 = 0.03268 0.00117 0.00775 -0.00027 C3 1 0.644653 0.244830 0.378536 11.00000 0.04116 0.01868 = 0.03675 -0.00326 0.01121 0.00010 AFIX 43 H3 2 0.684677 0.219361 0.320757 11.00000 -1.20000 AFIX 0 C4 1 0.520628 0.222555 0.390546 11.00000 0.03903 0.02215 = 0.04280 -0.00343 0.00467 -0.00923 AFIX 43 H4 2 0.475627 0.180457 0.340079 11.00000 -1.20000 AFIX 0 C5 1 0.460372 0.261045 0.475858 11.00000 0.02815 0.02972 = 0.04214 0.00223 0.00691 -0.00972 AFIX 43 H5 2 0.375346 0.244645 0.479521 11.00000 -1.20000 AFIX 0 C6 1 0.521916 0.322463 0.554993 11.00000 0.02536 0.02517 = 0.03498 0.00239 0.00990 -0.00179 AFIX 43 H6 2 0.481104 0.347720 0.612359 11.00000 -1.20000 AFIX 0 C7 1 0.648599 0.345025 0.544991 11.00000 0.02269 0.01456 = 0.02861 0.00137 0.00450 -0.00109 C8 1 0.927065 0.330846 0.391345 11.00000 0.04393 0.04773 = 0.06099 -0.02463 0.03535 -0.01617 AFIX 13 H8 2 0.999163 0.370538 0.419613 11.00000 -1.20000 AFIX 0 C9 1 0.988367 0.247574 0.418487 11.00000 0.06208 0.07018 = 0.14687 -0.04081 0.04823 0.01214 AFIX 137 H9A 2 1.023791 0.241134 0.508987 11.00000 -1.50000 H9B 2 1.058990 0.241616 0.375977 11.00000 -1.50000 H9C 2 0.921421 0.206861 0.387809 11.00000 -1.50000 AFIX 0 C10 1 0.861952 0.349007 0.252364 11.00000 0.10106 0.10146 = 0.05470 -0.02573 0.05299 -0.04654 AFIX 137 H10A 2 0.792055 0.310261 0.220503 11.00000 -1.50000 H10B 2 0.927493 0.345350 0.203429 11.00000 -1.50000 H10C 2 0.825001 0.402933 0.244991 11.00000 -1.50000 AFIX 0 C11 1 0.724014 0.461174 0.711306 11.00000 0.02185 0.01947 = 0.02416 -0.00118 0.00743 0.00072 C12 1 0.696322 0.412671 0.822525 11.00000 0.02340 0.02601 = 0.03259 0.00717 0.00869 0.00201 AFIX 23 H12A 2 0.769933 0.375822 0.856510 11.00000 -1.20000 H12B 2 0.615788 0.380560 0.792962 11.00000 -1.20000 AFIX 0 C13 1 0.608249 0.518829 0.656657 11.00000 0.02660 0.02296 = 0.02570 0.00313 0.00191 0.00197 AFIX 23 H13A 2 0.526734 0.487917 0.625140 11.00000 -1.20000 H13B 2 0.626105 0.549357 0.585851 11.00000 -1.20000 AFIX 0 C14 1 0.851606 0.510562 0.758118 11.00000 0.02144 0.02934 = 0.02877 -0.00398 0.00792 -0.00413 AFIX 23 H14A 2 0.869823 0.541375 0.687742 11.00000 -1.20000 H14B 2 0.926356 0.474312 0.790974 11.00000 -1.20000 AFIX 0 C15 1 0.679378 0.471549 0.927014 11.00000 0.02986 0.04163 = 0.02252 0.00412 0.00948 0.00109 AFIX 13 H15 2 0.660744 0.440687 0.998266 11.00000 -1.20000 AFIX 0 C16 1 0.562833 0.528797 0.871847 11.00000 0.02677 0.04184 = 0.03643 -0.00798 0.01232 0.00376 AFIX 23 H16A 2 0.481565 0.497457 0.841589 11.00000 -1.20000 H16B 2 0.549967 0.565679 0.937893 11.00000 -1.20000 AFIX 0 C17 1 0.807234 0.520676 0.974548 11.00000 0.02944 0.04955 = 0.02641 -0.00500 0.00441 0.00166 AFIX 23 H17A 2 0.797566 0.557611 1.041741 11.00000 -1.20000 H17B 2 0.881350 0.484349 1.009382 11.00000 -1.20000 AFIX 0 C18 1 0.834623 0.568647 0.863698 11.00000 0.02877 0.03579 = 0.03070 -0.00883 0.00556 -0.00881 AFIX 13 H18 2 0.916791 0.600282 0.894072 11.00000 -1.20000 AFIX 0 C19 1 0.719419 0.626420 0.809249 11.00000 0.04851 0.02439 = 0.03766 -0.00706 0.01227 -0.00179 AFIX 23 H19A 2 0.737969 0.657333 0.739119 11.00000 -1.20000 H19B 2 0.708829 0.664404 0.874784 11.00000 -1.20000 AFIX 0 C20 1 0.591717 0.577240 0.761874 11.00000 0.03112 0.02743 = 0.03587 -0.00252 0.00348 0.01206 AFIX 13 H20 2 0.517157 0.614322 0.727470 11.00000 -1.20000 AFIX 0 BR1 4 0.790048 0.578767 0.358042 11.00000 0.04489 0.06407 = 0.06014 0.00422 0.01255 -0.00527 HKLF 4 REM AD_0m_a.res in P2(1)/n REM R1 = 0.0492 for 2815 Fo > 4sig(Fo) and 0.1028 for all 4412 data REM 210 parameters refined using 0 restraints END WGHT 0.0265 1.9132 REM Highest difference peak 0.326, deepest hole -0.456, 1-sigma level 0.068 Q1 1 0.8171 0.6343 0.4137 11.00000 0.05 0.33 Q2 1 0.7851 0.6394 0.4028 11.00000 0.05 0.32 Q3 1 0.7396 0.6359 0.2765 11.00000 0.05 0.30 Q4 1 0.7457 0.5111 0.3804 11.00000 0.05 0.29 Q5 1 0.9987 0.3243 0.2399 11.00000 0.05 0.27 Q6 1 0.8347 0.6416 0.3372 11.00000 0.05 0.27 Q7 1 0.8913 0.1713 0.4812 11.00000 0.05 0.26 Q8 1 0.7649 0.3225 0.4596 11.00000 0.05 0.26 Q9 1 0.6756 0.2135 0.3462 11.00000 0.05 0.25 Q10 1 0.8179 0.5012 0.3369 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122.69 17.00 -8 2 0 162.88 22.70 8 2 0 85.59 13.80 8 2 0 78.29 13.20 -8 2 0 113.19 14.10 -8 2 0 117.49 12.60 9 -2 0 136.19 19.40 -9 -2 0 160.98 27.60 -9 -2 0 132.69 15.70 9 -2 0 144.89 14.90 -9 -2 0 189.78 30.60 9 -2 0 160.58 21.50 9 -2 0 151.68 18.00 -9 -2 0 171.88 28.20 9 -2 0 154.48 18.80 -9 -2 0 132.49 17.90 9 -2 0 131.09 19.30 -9 2 0 124.29 18.50 9 2 0 129.79 17.80 -9 2 0 181.58 26.20 -9 2 0 182.28 26.00 9 2 0 121.89 18.10 9 2 0 135.79 17.70 -9 2 0 156.98 19.30 -9 2 0 156.48 15.50 -9 2 0 125.89 16.50 9 2 0 152.98 21.50 10 -2 0 91.09 25.10 -10 -2 0 52.89 22.50 -10 -2 0 48.00 23.40 10 -2 0 62.39 13.50 10 -2 0 47.70 13.00 -10 -2 0 12.90 25.80 -10 -2 0 64.59 17.00 -10 -2 0 60.09 9.90 10 2 0 55.09 17.50 -10 2 0 39.70 9.10 -10 2 0 68.19 15.00 -10 2 0 45.70 21.70 10 2 0 48.00 12.20 10 2 0 42.80 12.00 -10 2 0 76.89 29.30 -10 2 0 69.19 21.60 -10 2 0 47.80 13.60 -11 -2 0 115.59 30.00 -11 -2 0 115.19 45.00 11 -2 0 125.79 18.20 -11 -2 0 100.49 60.39 -11 2 0 97.39 27.70 -11 2 0 99.59 14.90 -11 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215.18 20.70 5 3 0 205.38 21.60 -5 3 0 211.18 21.00 5 3 0 207.98 20.90 -5 3 0 245.28 19.50 -5 3 0 224.28 21.10 5 3 0 210.88 22.70 5 3 0 219.98 19.70 5 3 0 191.18 21.10 6 -3 0 1594.84 126.19 6 -3 0 1584.64 126.59 6 -3 0 1492.55 126.99 -6 -3 0 1578.44 130.69 6 -3 0 1437.96 127.09 -6 -3 0 1479.05 125.39 6 -3 0 1301.77 126.09 -6 -3 0 1474.05 129.99 6 -3 0 1544.95 127.59 -6 -3 0 1598.64 129.79 -6 -3 0 1460.85 126.29 -6 3 0 1344.47 127.79 6 3 0 1387.16 126.09 6 3 0 1520.25 124.99 6 3 0 1488.15 125.39 6 3 0 1515.05 125.39 6 3 0 1554.34 128.59 -6 3 0 1506.65 126.19 -6 3 0 1534.85 125.79 -6 3 0 1392.66 124.79 6 3 0 1431.46 126.19 6 3 0 1486.55 127.19 6 3 0 1295.07 126.49 -6 3 0 1530.25 126.29 -6 3 0 1382.76 127.09 -6 3 0 1436.46 126.19 -7 -3 0 0.30 16.80 -7 -3 0 11.70 8.30 7 -3 0 1.30 8.00 -7 -3 0 2.40 13.60 -7 -3 0 -0.40 5.60 -7 -3 0 9.00 5.70 7 -3 0 9.40 8.20 -7 -3 0 -7.50 13.80 7 -3 0 3.00 3.70 7 -3 0 6.50 7.30 7 -3 0 11.90 6.20 -7 -3 0 3.10 2.80 7 -3 0 6.40 8.10 7 3 0 0.90 10.20 -7 3 0 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