data_mo_dd19210_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H23 N5' _chemical_formula_weight 441.52 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 6.1532(3) _cell_length_b 13.1141(6) _cell_length_c 15.5713(8) _cell_angle_alpha 109.057(2) _cell_angle_beta 90.519(2) _cell_angle_gamma 99.450(2) _cell_volume 1168.87(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5289 _cell_measurement_theta_min 5.000 _cell_measurement_theta_max 54.290 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_F_000 464 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.076 _shelx_estimated_absorpt_T_min 0.989 _shelx_estimated_absorpt_T_max 0.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6289 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17080 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.774 _diffrn_reflns_theta_max 25.495 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 4348 _reflns_number_gt 3140 _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0461P)^2^+0.2626P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.059(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4348 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _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 1.2855(2) 0.65696(11) 0.91044(10) 0.0470(4) Uani 1 1 d . . . . . N2 N 0.3435(3) 0.72395(17) 0.66589(14) 0.0813(6) Uani 1 1 d . . . . . N3 N 1.0039(2) 0.51729(11) 0.82658(9) 0.0421(4) Uani 1 1 d . . . . . N4 N -0.3022(4) -0.08633(17) 0.25445(17) 0.1039(8) Uani 1 1 d . . . . . N5 N 0.2554(4) -0.07715(16) 0.42450(15) 0.0887(7) Uani 1 1 d . . . . . C1 C 1.3734(3) 0.76528(15) 0.95086(12) 0.0488(5) Uani 1 1 d . . . . . C2 C 1.2721(3) 0.84581(15) 0.94119(13) 0.0537(5) Uani 1 1 d . . . . . H2 H 1.3315 0.9188 0.9726 0.064 Uiso 1 1 calc R U . . . C3 C 1.0791(3) 0.82001(14) 0.88435(12) 0.0481(4) Uani 1 1 d . . . . . C4 C 0.9733(3) 0.90274(15) 0.87114(14) 0.0568(5) Uani 1 1 d . . . . . H4 H 1.0352 0.9758 0.9009 0.068 Uiso 1 1 calc R U . . . C5 C 0.7856(3) 0.87942(15) 0.81686(13) 0.0540(5) Uani 1 1 d . . . . . C6 C 0.7011(3) 0.76732(15) 0.76839(12) 0.0488(5) Uani 1 1 d . . . . . C7 C 0.8017(3) 0.68207(14) 0.77594(11) 0.0435(4) Uani 1 1 d . . . . . C8 C 0.9877(3) 0.70767(13) 0.83908(11) 0.0418(4) Uani 1 1 d . . . . . C9 C 1.0981(3) 0.62903(13) 0.85991(11) 0.0417(4) Uani 1 1 d . . . . . C10 C 1.5815(3) 0.78805(17) 1.00995(13) 0.0609(5) Uani 1 1 d . . . . . H10A H 1.5448 0.7901 1.0702 0.091 Uiso 1 1 calc R U . . . H10B H 1.6665 0.8574 1.0126 0.091 Uiso 1 1 calc R U . . . H10C H 1.6663 0.7312 0.9849 0.091 Uiso 1 1 calc R U . . . C11 C 0.6682(4) 0.96780(17) 0.80747(16) 0.0714(6) Uani 1 1 d . . . . . H11A H 0.6457 0.9589 0.7442 0.107 Uiso 1 1 calc R U . . . H11B H 0.7562 1.0383 0.8386 0.107 Uiso 1 1 calc R U . . . H11C H 0.5280 0.9625 0.8337 0.107 Uiso 1 1 calc R U . . . C12 C 0.5035(3) 0.74128(16) 0.71010(14) 0.0579(5) Uani 1 1 d . . . . . C13 C 0.8072(3) 0.48996(14) 0.87372(12) 0.0474(4) Uani 1 1 d . . . . . H13A H 0.7042 0.5384 0.8732 0.057 Uiso 1 1 calc R U . . . H13B H 0.8508 0.5016 0.9367 0.057 Uiso 1 1 calc R U . . . C14 C 0.6942(3) 0.37233(15) 0.82884(14) 0.0561(5) Uani 1 1 d . . . . . H14A H 0.5747 0.3552 0.8649 0.067 Uiso 1 1 calc R U . . . H14B H 0.6309 0.3636 0.7690 0.067 Uiso 1 1 calc R U . . . C15 C 0.8525(3) 0.29306(16) 0.81923(17) 0.0687(6) Uani 1 1 d . . . . . H15A H 0.8983 0.2928 0.8789 0.082 Uiso 1 1 calc R U . . . H15B H 0.7794 0.2196 0.7839 0.082 Uiso 1 1 calc R U . . . C16 C 1.0525(3) 0.32636(15) 0.77241(16) 0.0670(6) Uani 1 1 d . . . . . H16A H 1.1574 0.2779 0.7697 0.080 Uiso 1 1 calc R U . . . H16B H 1.0081 0.3193 0.7105 0.080 Uiso 1 1 calc R U . . . C17 C 1.1609(3) 0.44315(14) 0.82290(14) 0.0547(5) Uani 1 1 d . . . . . H17A H 1.2097 0.4499 0.8842 0.066 Uiso 1 1 calc R U . . . H17B H 1.2893 0.4630 0.7922 0.066 Uiso 1 1 calc R U . . . C18 C 0.7078(3) 0.57480(15) 0.71612(12) 0.0470(4) Uani 1 1 d . . . . . C19 C 0.6019(3) 0.49634(15) 0.65989(13) 0.0528(5) Uani 1 1 d . . . . . C20 C 0.4625(3) 0.40499(15) 0.59520(12) 0.0526(5) Uani 1 1 d . . . . . C21 C 0.2762(4) 0.42233(17) 0.55430(15) 0.0684(6) Uani 1 1 d . . . . . H21 H 0.2461 0.4930 0.5685 0.082 Uiso 1 1 calc R U . . . C22 C 0.1366(4) 0.33627(16) 0.49336(15) 0.0664(6) Uani 1 1 d . . . . . H22 H 0.0138 0.3494 0.4662 0.080 Uiso 1 1 calc R U . . . C23 C 0.1761(3) 0.22936(15) 0.47145(12) 0.0521(5) Uani 1 1 d . . . . . C24 C 0.3637(3) 0.21194(16) 0.51214(14) 0.0598(5) Uani 1 1 d . . . . . H24 H 0.3934 0.1413 0.4985 0.072 Uiso 1 1 calc R U . . . C25 C 0.5046(3) 0.29875(16) 0.57221(13) 0.0590(5) Uani 1 1 d . . . . . H25 H 0.6302 0.2862 0.5979 0.071 Uiso 1 1 calc R U . . . C26 C 0.0185(3) 0.14412(16) 0.40628(13) 0.0573(5) Uani 1 1 d . . . . . H26 H -0.0911 0.1695 0.3816 0.069 Uiso 1 1 calc R U . . . C27 C 0.0043(3) 0.03440(15) 0.37556(13) 0.0541(5) Uani 1 1 d . . . . . C28 C -0.1683(4) -0.03238(17) 0.30887(16) 0.0699(6) Uani 1 1 d . . . . . C29 C 0.1472(4) -0.02555(17) 0.40367(13) 0.0599(5) 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 0.0412(8) 0.0439(9) 0.0493(9) 0.0103(7) -0.0038(7) 0.0001(7) N2 0.0765(13) 0.0886(15) 0.0872(14) 0.0353(12) -0.0132(11) 0.0266(11) N3 0.0369(7) 0.0339(8) 0.0510(8) 0.0094(6) -0.0023(6) 0.0038(6) N4 0.1068(17) 0.0610(13) 0.1199(19) 0.0006(12) -0.0542(15) 0.0128(12) N5 0.1032(16) 0.0676(13) 0.0944(15) 0.0211(11) -0.0216(12) 0.0261(12) C1 0.0438(10) 0.0463(11) 0.0455(10) 0.0078(8) 0.0009(8) -0.0061(8) C2 0.0534(11) 0.0386(10) 0.0571(12) 0.0067(9) 0.0003(9) -0.0060(9) C3 0.0493(10) 0.0388(10) 0.0504(11) 0.0110(8) 0.0040(8) 0.0001(8) C4 0.0683(13) 0.0353(10) 0.0635(12) 0.0151(9) 0.0081(10) 0.0028(9) C5 0.0638(12) 0.0449(11) 0.0583(12) 0.0218(9) 0.0106(10) 0.0132(9) C6 0.0530(11) 0.0473(11) 0.0504(10) 0.0205(9) 0.0039(9) 0.0118(9) C7 0.0455(10) 0.0388(10) 0.0452(10) 0.0134(8) 0.0026(8) 0.0060(8) C8 0.0407(9) 0.0372(9) 0.0440(9) 0.0106(8) 0.0033(8) 0.0037(7) C9 0.0385(9) 0.0379(9) 0.0434(9) 0.0089(8) 0.0024(8) 0.0012(7) C10 0.0490(11) 0.0606(12) 0.0592(12) 0.0093(10) -0.0074(9) -0.0070(9) C11 0.0889(16) 0.0553(13) 0.0822(15) 0.0319(11) 0.0152(13) 0.0279(12) C12 0.0589(13) 0.0591(13) 0.0639(13) 0.0279(10) 0.0016(11) 0.0179(10) C13 0.0430(10) 0.0463(10) 0.0546(11) 0.0195(9) 0.0011(8) 0.0070(8) C14 0.0478(11) 0.0479(11) 0.0750(13) 0.0274(10) -0.0024(10) 0.0008(9) C15 0.0682(14) 0.0403(11) 0.0965(17) 0.0250(11) -0.0104(12) 0.0024(10) C16 0.0565(12) 0.0415(11) 0.0948(16) 0.0094(11) -0.0030(11) 0.0135(9) C17 0.0427(10) 0.0428(10) 0.0741(13) 0.0116(9) -0.0020(9) 0.0113(8) C18 0.0486(10) 0.0459(11) 0.0483(10) 0.0181(9) -0.0049(8) 0.0088(8) C19 0.0550(11) 0.0491(11) 0.0530(11) 0.0167(9) -0.0095(9) 0.0071(9) C20 0.0569(11) 0.0472(11) 0.0489(11) 0.0124(9) -0.0127(9) 0.0039(9) C21 0.0742(14) 0.0456(12) 0.0788(15) 0.0132(10) -0.0267(12) 0.0101(10) C22 0.0655(13) 0.0519(12) 0.0766(14) 0.0148(11) -0.0272(11) 0.0115(10) C23 0.0535(11) 0.0482(11) 0.0503(11) 0.0119(9) -0.0100(9) 0.0068(9) C24 0.0635(12) 0.0485(11) 0.0611(12) 0.0085(9) -0.0174(10) 0.0132(10) C25 0.0576(12) 0.0541(12) 0.0602(12) 0.0114(10) -0.0175(10) 0.0129(10) C26 0.0564(12) 0.0547(12) 0.0561(12) 0.0123(9) -0.0141(9) 0.0102(9) C27 0.0598(12) 0.0484(11) 0.0493(11) 0.0097(9) -0.0082(9) 0.0104(9) C28 0.0754(15) 0.0483(12) 0.0759(15) 0.0077(11) -0.0210(12) 0.0110(11) C29 0.0700(13) 0.0502(12) 0.0536(12) 0.0095(10) -0.0070(10) 0.0105(10) _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 C9 1.319(2) . ? N1 C1 1.365(2) . ? N2 C12 1.143(2) . ? N3 C9 1.404(2) . ? N3 C17 1.468(2) . ? N3 C13 1.476(2) . ? N4 C28 1.141(3) . ? N5 C29 1.137(3) . ? C1 C2 1.358(3) . ? C1 C10 1.499(3) . ? C2 C3 1.401(3) . ? C2 H2 0.9300 . ? C3 C4 1.421(3) . ? C3 C8 1.423(2) . ? C4 C5 1.356(3) . ? C4 H4 0.9300 . ? C5 C6 1.421(3) . ? C5 C11 1.507(3) . ? C6 C7 1.399(2) . ? C6 C12 1.436(3) . ? C7 C8 1.424(2) . ? C7 C18 1.431(2) . ? C8 C9 1.440(2) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C13 C14 1.512(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.512(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.511(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.509(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.196(2) . ? C19 C20 1.430(3) . ? C20 C25 1.390(3) . ? C20 C21 1.392(3) . ? C21 C22 1.371(3) . ? C21 H21 0.9300 . ? C22 C23 1.394(3) . ? C22 H22 0.9300 . ? C23 C24 1.398(3) . ? C23 C26 1.451(3) . ? C24 C25 1.374(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.347(3) . ? C26 H26 0.9300 . ? C27 C29 1.424(3) . ? C27 C28 1.433(3) . ? 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 C9 N1 C1 119.54(15) . . ? C9 N3 C17 114.26(13) . . ? C9 N3 C13 112.98(13) . . ? C17 N3 C13 111.10(14) . . ? C2 C1 N1 121.77(17) . . ? C2 C1 C10 122.97(17) . . ? N1 C1 C10 115.18(17) . . ? C1 C2 C3 120.63(17) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 121.75(17) . . ? C2 C3 C8 118.66(16) . . ? C4 C3 C8 119.59(17) . . ? C5 C4 C3 122.63(17) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 117.51(17) . . ? C4 C5 C11 122.07(18) . . ? C6 C5 C11 120.42(19) . . ? C7 C6 C5 122.66(17) . . ? C7 C6 C12 119.13(17) . . ? C5 C6 C12 118.21(16) . . ? C6 C7 C8 118.93(16) . . ? C6 C7 C18 115.50(16) . . ? C8 C7 C18 125.55(15) . . ? C7 C8 C3 118.30(15) . . ? C7 C8 C9 125.56(15) . . ? C3 C8 C9 116.11(15) . . ? N1 C9 N3 117.43(15) . . ? N1 C9 C8 122.94(15) . . ? N3 C9 C8 119.63(15) . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C6 177.4(2) . . ? N3 C13 C14 111.53(14) . . ? N3 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N3 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 111.87(16) . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 109.84(16) . . ? C16 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? C16 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 110.74(17) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N3 C17 C16 109.91(15) . . ? N3 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? N3 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C7 166.74(18) . . ? C18 C19 C20 176.2(2) . . ? C25 C20 C21 118.49(17) . . ? C25 C20 C19 122.37(17) . . ? C21 C20 C19 119.14(17) . . ? C22 C21 C20 120.63(19) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 121.01(18) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C24 118.38(17) . . ? C22 C23 C26 116.72(17) . . ? C24 C23 C26 124.89(18) . . ? C25 C24 C23 120.32(18) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 121.14(18) . . ? C24 C25 H25 119.4 . . ? C20 C25 H25 119.4 . . ? C27 C26 C23 130.79(18) . . ? C27 C26 H26 114.6 . . ? C23 C26 H26 114.6 . . ? C26 C27 C29 126.02(18) . . ? C26 C27 C28 119.69(18) . . ? C29 C27 C28 114.29(17) . . ? N4 C28 C27 178.5(3) . . ? N5 C29 C27 177.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N1 C1 C2 0.6(3) . . . . ? C9 N1 C1 C10 177.52(16) . . . . ? N1 C1 C2 C3 -4.0(3) . . . . ? C10 C1 C2 C3 179.35(17) . . . . ? C1 C2 C3 C4 -178.28(17) . . . . ? C1 C2 C3 C8 1.8(3) . . . . ? C2 C3 C4 C5 -179.56(18) . . . . ? C8 C3 C4 C5 0.3(3) . . . . ? C3 C4 C5 C6 -3.3(3) . . . . ? C3 C4 C5 C11 176.59(17) . . . . ? C4 C5 C6 C7 1.0(3) . . . . ? C11 C5 C6 C7 -178.89(17) . . . . ? C4 C5 C6 C12 -179.53(18) . . . . ? C11 C5 C6 C12 0.6(3) . . . . ? C5 C6 C7 C8 4.2(3) . . . . ? C12 C6 C7 C8 -175.21(16) . . . . ? C5 C6 C7 C18 -174.32(16) . . . . ? C12 C6 C7 C18 6.2(2) . . . . ? C6 C7 C8 C3 -7.1(2) . . . . ? C18 C7 C8 C3 171.31(16) . . . . ? C6 C7 C8 C9 174.84(16) . . . . ? C18 C7 C8 C9 -6.8(3) . . . . ? C2 C3 C8 C7 -175.14(16) . . . . ? C4 C3 C8 C7 5.0(2) . . . . ? C2 C3 C8 C9 3.1(2) . . . . ? C4 C3 C8 C9 -176.77(15) . . . . ? C1 N1 C9 N3 -174.35(15) . . . . ? C1 N1 C9 C8 4.9(2) . . . . ? C17 N3 C9 N1 -21.8(2) . . . . ? C13 N3 C9 N1 106.56(17) . . . . ? C17 N3 C9 C8 158.98(15) . . . . ? C13 N3 C9 C8 -72.70(19) . . . . ? C7 C8 C9 N1 171.46(16) . . . . ? C3 C8 C9 N1 -6.6(2) . . . . ? C7 C8 C9 N3 -9.3(2) . . . . ? C3 C8 C9 N3 172.57(15) . . . . ? C9 N3 C13 C14 173.10(14) . . . . ? C17 N3 C13 C14 -56.96(19) . . . . ? N3 C13 C14 C15 53.4(2) . . . . ? C13 C14 C15 C16 -52.6(2) . . . . ? C14 C15 C16 C17 55.8(2) . . . . ? C9 N3 C17 C16 -170.83(16) . . . . ? C13 N3 C17 C16 59.9(2) . . . . ? C15 C16 C17 N3 -59.7(2) . . . . ? C6 C7 C18 C19 2.0(9) . . . . ? C8 C7 C18 C19 -176.4(8) . . . . ? C25 C20 C21 C22 0.5(3) . . . . ? C19 C20 C21 C22 -178.7(2) . . . . ? C20 C21 C22 C23 0.7(4) . . . . ? C21 C22 C23 C24 -1.0(3) . . . . ? C21 C22 C23 C26 179.9(2) . . . . ? C22 C23 C24 C25 0.0(3) . . . . ? C26 C23 C24 C25 179.1(2) . . . . ? C23 C24 C25 C20 1.2(3) . . . . ? C21 C20 C25 C24 -1.5(3) . . . . ? C19 C20 C25 C24 177.8(2) . . . . ? C22 C23 C26 C27 -175.9(2) . . . . ? C24 C23 C26 C27 5.0(4) . . . . ? C23 C26 C27 C29 1.5(4) . . . . ? C23 C26 C27 C28 -178.9(2) . . . . ? _refine_diff_density_max 0.159 _refine_diff_density_min -0.146 _refine_diff_density_rms 0.028 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_dd19210_0m_a.res in P-1 CELL 0.71073 6.1532 13.1141 15.5713 109.057 90.519 99.45 ZERR 2 0.0003 0.0006 0.0008 0.002 0.002 0.002 LATT 1 SFAC C H N UNIT 58 46 10 OMIT 0 1 0 OMIT 0 -1 1 OMIT -3.00 51.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 size 0.15 0.10 0.05 wpdb -1 mpla c19 > c24 mpla n1 c1 > c9 htab conf TEMP 20.15 WGHT 0.046100 0.262600 EXTI 0.058514 FVAR 1.70198 N1 3 1.285452 0.656962 0.910436 11.00000 0.04125 0.04387 = 0.04932 0.01034 -0.00383 0.00010 N2 3 0.343467 0.723952 0.665886 11.00000 0.07651 0.08862 = 0.08717 0.03528 -0.01316 0.02658 N3 3 1.003945 0.517294 0.826584 11.00000 0.03693 0.03390 = 0.05105 0.00936 -0.00230 0.00382 N4 3 -0.302209 -0.086332 0.254453 11.00000 0.10684 0.06102 = 0.11987 0.00061 -0.05420 0.01279 N5 3 0.255415 -0.077146 0.424496 11.00000 0.10321 0.06758 = 0.09437 0.02114 -0.02159 0.02614 C1 1 1.373427 0.765282 0.950864 11.00000 0.04376 0.04633 = 0.04554 0.00782 0.00086 -0.00608 C2 1 1.272143 0.845812 0.941191 11.00000 0.05336 0.03857 = 0.05710 0.00674 0.00032 -0.00601 AFIX 43 H2 2 1.331515 0.918788 0.972612 11.00000 -1.20000 AFIX 0 C3 1 1.079139 0.820008 0.884350 11.00000 0.04935 0.03885 = 0.05040 0.01095 0.00395 0.00008 C4 1 0.973288 0.902739 0.871135 11.00000 0.06833 0.03531 = 0.06352 0.01510 0.00809 0.00277 AFIX 43 H4 2 1.035207 0.975800 0.900891 11.00000 -1.20000 AFIX 0 C5 1 0.785574 0.879417 0.816865 11.00000 0.06376 0.04490 = 0.05829 0.02180 0.01058 0.01319 C6 1 0.701126 0.767323 0.768395 11.00000 0.05298 0.04729 = 0.05042 0.02050 0.00386 0.01180 C7 1 0.801687 0.682071 0.775942 11.00000 0.04549 0.03877 = 0.04521 0.01337 0.00256 0.00602 C8 1 0.987722 0.707667 0.839083 11.00000 0.04068 0.03722 = 0.04404 0.01058 0.00331 0.00367 C9 1 1.098127 0.629028 0.859906 11.00000 0.03852 0.03794 = 0.04335 0.00890 0.00241 0.00120 C10 1 1.581478 0.788048 1.009954 11.00000 0.04898 0.06056 = 0.05915 0.00926 -0.00745 -0.00699 AFIX 137 H10A 2 1.544850 0.790102 1.070225 11.00000 -1.50000 H10B 2 1.666486 0.857399 1.012573 11.00000 -1.50000 H10C 2 1.666300 0.731219 0.984897 11.00000 -1.50000 AFIX 0 C11 1 0.668233 0.967800 0.807467 11.00000 0.08894 0.05528 = 0.08218 0.03188 0.01522 0.02786 AFIX 137 H11A 2 0.645720 0.958884 0.744158 11.00000 -1.50000 H11B 2 0.756216 1.038344 0.838552 11.00000 -1.50000 H11C 2 0.527994 0.962489 0.833702 11.00000 -1.50000 AFIX 0 C12 1 0.503456 0.741283 0.710099 11.00000 0.05894 0.05909 = 0.06385 0.02792 0.00158 0.01794 C13 1 0.807226 0.489965 0.873724 11.00000 0.04296 0.04633 = 0.05458 0.01946 0.00108 0.00696 AFIX 23 H13A 2 0.704239 0.538427 0.873230 11.00000 -1.20000 H13B 2 0.850835 0.501595 0.936696 11.00000 -1.20000 AFIX 0 C14 1 0.694221 0.372334 0.828839 11.00000 0.04779 0.04788 = 0.07502 0.02741 -0.00241 0.00076 AFIX 23 H14A 2 0.574732 0.355246 0.864863 11.00000 -1.20000 H14B 2 0.630884 0.363589 0.769047 11.00000 -1.20000 AFIX 0 C15 1 0.852528 0.293057 0.819233 11.00000 0.06816 0.04026 = 0.09654 0.02497 -0.01039 0.00245 AFIX 23 H15A 2 0.898295 0.292846 0.878940 11.00000 -1.20000 H15B 2 0.779448 0.219552 0.783908 11.00000 -1.20000 AFIX 0 C16 1 1.052454 0.326356 0.772407 11.00000 0.05652 0.04145 = 0.09481 0.00937 -0.00297 0.01345 AFIX 23 H16A 2 1.157423 0.277881 0.769700 11.00000 -1.20000 H16B 2 1.008074 0.319347 0.710517 11.00000 -1.20000 AFIX 0 C17 1 1.160914 0.443152 0.822897 11.00000 0.04268 0.04277 = 0.07409 0.01161 -0.00203 0.01125 AFIX 23 H17A 2 1.209669 0.449892 0.884231 11.00000 -1.20000 H17B 2 1.289310 0.463038 0.792220 11.00000 -1.20000 AFIX 0 C18 1 0.707756 0.574801 0.716119 11.00000 0.04863 0.04590 = 0.04829 0.01815 -0.00492 0.00882 C19 1 0.601944 0.496344 0.659890 11.00000 0.05495 0.04912 = 0.05297 0.01669 -0.00949 0.00711 C20 1 0.462524 0.404993 0.595198 11.00000 0.05690 0.04723 = 0.04889 0.01237 -0.01267 0.00387 C21 1 0.276170 0.422335 0.554303 11.00000 0.07423 0.04563 = 0.07881 0.01318 -0.02670 0.01007 AFIX 43 H21 2 0.246079 0.492982 0.568475 11.00000 -1.20000 AFIX 0 C22 1 0.136646 0.336270 0.493355 11.00000 0.06554 0.05187 = 0.07659 0.01475 -0.02725 0.01152 AFIX 43 H22 2 0.013767 0.349432 0.466206 11.00000 -1.20000 AFIX 0 C23 1 0.176108 0.229358 0.471453 11.00000 0.05348 0.04819 = 0.05030 0.01190 -0.01001 0.00682 C24 1 0.363722 0.211945 0.512135 11.00000 0.06346 0.04847 = 0.06108 0.00853 -0.01738 0.01318 AFIX 43 H24 2 0.393350 0.141272 0.498475 11.00000 -1.20000 AFIX 0 C25 1 0.504583 0.298748 0.572214 11.00000 0.05758 0.05411 = 0.06021 0.01135 -0.01746 0.01294 AFIX 43 H25 2 0.630242 0.286172 0.597938 11.00000 -1.20000 AFIX 0 C26 1 0.018476 0.144121 0.406282 11.00000 0.05642 0.05465 = 0.05614 0.01231 -0.01411 0.01023 AFIX 43 H26 2 -0.091059 0.169465 0.381588 11.00000 -1.20000 AFIX 0 C27 1 0.004252 0.034396 0.375557 11.00000 0.05978 0.04845 = 0.04926 0.00970 -0.00822 0.01044 C28 1 -0.168267 -0.032381 0.308867 11.00000 0.07538 0.04827 = 0.07586 0.00770 -0.02097 0.01103 C29 1 0.147189 -0.025548 0.403675 11.00000 0.06996 0.05020 = 0.05360 0.00949 -0.00703 0.01045 HKLF 4 REM mo_dd19210_0m_a.res in P-1 REM R1 = 0.0480 for 3140 Fo > 4sig(Fo) and 0.0725 for all 4348 data REM 310 parameters refined using 0 restraints END WGHT 0.0450 0.2685 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.159, deepest hole -0.146, 1-sigma level 0.028 Q1 1 1.6026 0.7247 1.0349 11.00000 0.05 0.16 Q2 1 1.7096 0.7980 0.9672 11.00000 0.05 0.15 Q3 1 0.9965 0.7747 0.8809 11.00000 0.05 0.13 Q4 1 1.3262 0.4775 0.8391 11.00000 0.05 0.13 Q5 1 1.0651 0.7661 0.8416 11.00000 0.05 0.13 Q6 1 1.5686 0.8686 1.0614 11.00000 0.05 0.12 Q7 1 0.2912 0.2217 0.4757 11.00000 0.05 0.11 Q8 1 0.6476 0.5659 0.6594 11.00000 0.05 0.11 Q9 1 0.5019 0.9219 0.7441 11.00000 0.05 0.11 Q10 1 0.7596 0.5118 0.6865 11.00000 0.05 0.11 Q11 1 1.3176 0.6062 0.9358 11.00000 0.05 0.11 Q12 1 0.9088 0.6947 0.8192 11.00000 0.05 0.10 Q13 1 0.8012 1.0227 0.7836 11.00000 0.05 0.10 Q14 1 1.3892 0.6043 0.9020 11.00000 0.05 0.10 Q15 1 0.7003 0.8184 0.8113 11.00000 0.05 0.10 Q16 1 0.5159 0.3375 0.7993 11.00000 0.05 0.10 Q17 1 0.5706 0.5546 0.6978 11.00000 0.05 0.10 Q18 1 1.3512 0.5806 0.8656 11.00000 0.05 0.10 Q19 1 0.0696 0.3542 0.4212 11.00000 0.05 0.10 Q20 1 0.1904 0.2065 0.5139 11.00000 0.05 0.10 ; _shelx_res_checksum 14212 _shelx_hkl_file ; -1 0 0 2037.80 65.19 -1 0 0 2097.29 58.89 1 0 0 2122.79 64.69 1 0 0 1961.00 58.39 -2 0 0 1458.25 56.79 -2 0 0 1410.26 46.50 2 0 0 1374.16 55.19 -3 0 0 1266.37 46.30 -3 0 0 1233.18 58.79 -3 0 0 1266.67 40.30 3 0 0 1189.68 44.40 3 0 0 1181.78 56.49 -4 0 0 372.36 19.30 -4 0 0 335.47 31.90 -4 0 0 375.36 23.20 4 0 0 351.16 30.90 4 0 0 338.27 26.30 4 0 0 374.36 22.10 -5 0 0 0.50 7.10 -5 0 0 7.20 4.50 -5 0 0 1.70 4.40 5 0 0 0.40 5.50 5 0 0 12.10 5.40 5 0 0 -1.60 4.30 -6 0 0 309.67 25.10 -6 0 0 301.77 21.80 -6 0 0 342.07 40.20 6 0 0 275.37 29.70 6 0 0 285.57 25.40 -7 0 0 76.69 13.20 -7 0 0 68.79 14.50 -7 0 0 82.29 25.40 7 0 0 55.69 14.20 7 0 0 73.59 18.50 7 -1 0 31.90 11.20 7 -1 0 12.70 8.00 -7 1 0 11.60 8.50 -7 1 0 20.50 5.80 -7 1 0 32.30 11.70 6 -1 0 37.60 11.10 6 -1 0 23.50 7.80 -6 1 0 46.20 9.90 -6 1 0 27.80 6.10 -6 1 0 15.40 11.40 5 -1 0 51.39 9.90 5 -1 0 83.89 13.80 5 -1 0 103.49 17.90 -5 1 0 94.49 14.70 -5 1 0 93.79 22.30 -5 1 0 73.09 7.50 4 -1 0 408.16 25.10 4 -1 0 348.97 29.90 4 -1 0 427.86 28.50 4 -1 0 407.66 23.90 -4 1 0 380.76 23.60 -4 1 0 433.36 34.40 3 -1 0 282.57 17.70 3 -1 0 257.87 16.70 3 -1 0 259.77 18.70 3 -1 0 272.17 22.80 -3 1 0 276.07 23.60 -3 1 0 280.77 17.30 2 -1 0 96.99 8.30 2 -1 0 105.49 8.40 2 -1 0 83.69 10.20 -2 1 0 115.89 12.10 -2 1 0 96.39 8.30 1 -1 0 1991.90 55.19 1 -1 0 1769.32 53.59 1 -1 0 1742.13 56.09 -1 1 0 1929.31 55.09 -1 1 0 1875.81 56.79 0 1 0 0.20 0.50 0 1 0 -0.60 0.50 -1 -1 0 9.60 2.40 -1 -1 0 11.10 3.10 -1 -1 0 8.50 3.60 1 1 0 14.20 3.30 1 1 0 13.30 4.20 -2 -1 0 239.58 14.20 -2 -1 0 243.88 20.00 -2 -1 0 246.48 13.50 2 1 0 245.08 15.10 2 1 0 228.48 19.10 -3 -1 0 118.09 10.80 -3 -1 0 128.49 11.30 -3 -1 0 105.09 18.70 3 1 0 111.89 9.80 3 1 0 106.49 15.40 -4 -1 0 322.77 21.20 -4 -1 0 304.27 31.20 -4 -1 0 329.47 21.70 4 1 0 327.17 20.00 4 1 0 342.17 26.80 4 1 0 296.87 34.80 -5 -1 0 -5.20 4.00 -5 -1 0 9.10 4.90 -5 -1 0 2.40 8.10 5 1 0 -4.70 4.40 -6 -1 0 82.79 14.60 -6 -1 0 59.49 13.30 -6 -1 0 71.99 20.90 6 1 0 110.29 21.60 6 1 0 75.19 13.60 -7 -1 0 95.89 26.90 -7 -1 0 113.59 15.90 -7 -1 0 115.59 19.90 7 1 0 123.49 23.90 7 1 0 104.59 17.90 7 -2 0 60.09 13.60 7 -2 0 55.69 16.50 -7 2 0 39.80 20.50 -7 2 0 73.49 7.20 -7 2 0 59.09 6.60 6 -2 0 6.70 6.30 6 -2 0 14.80 8.50 -6 2 0 16.80 6.80 -6 2 0 9.70 3.30 -6 2 0 10.70 9.40 5 -2 0 19.60 5.80 5 -2 0 29.20 9.60 5 -2 0 28.20 8.90 -5 2 0 20.00 7.20 -5 2 0 22.80 10.00 4 -2 0 443.36 26.40 4 -2 0 448.46 28.10 4 -2 0 403.06 25.10 4 -2 0 432.26 32.50 -4 2 0 448.76 25.80 -4 2 0 467.85 34.90 3 -2 0 90.09 12.10 3 -2 0 110.09 11.00 3 -2 0 102.19 10.30 3 -2 0 115.59 11.30 -3 2 0 108.19 14.20 -3 2 0 111.59 10.70 2 -2 0 3970.50 115.49 2 -2 0 3785.72 118.09 2 -2 0 3768.52 112.79 2 -2 0 3939.51 115.09 -2 2 0 3978.20 115.59 -2 2 0 4017.90 119.29 -2 2 0 4027.50 104.49 1 -2 0 3570.84 99.79 1 -2 0 3657.63 102.29 1 -2 0 3517.25 97.19 1 -2 0 3583.64 99.69 -1 2 0 3647.64 101.79 -1 2 0 3616.84 102.39 0 -2 0 1061.29 37.30 0 -2 0 960.90 31.50 0 -2 0 981.70 32.40 0 2 0 1016.10 31.60 0 2 0 1090.79 37.80 0 2 0 1005.20 32.30 -1 -2 0 1334.97 48.80 -1 -2 0 1306.07 50.29 -1 -2 0 1380.56 41.70 1 2 0 1324.97 41.10 1 2 0 1420.16 53.99 -2 -2 0 61.69 8.80 -2 -2 0 58.89 6.40 -2 -2 0 59.59 12.50 2 2 0 57.09 11.80 2 2 0 47.20 6.70 2 2 0 57.99 5.80 -3 -2 0 16.80 5.90 -3 -2 0 7.40 6.80 -3 -2 0 11.00 4.10 3 2 0 6.50 5.70 3 2 0 14.80 4.40 -4 -2 0 8.10 8.10 -4 -2 0 4.50 3.40 -4 -2 0 3.30 4.70 4 2 0 -1.30 3.70 -5 -2 0 211.28 29.60 -5 -2 0 221.58 21.00 -5 -2 0 204.18 18.80 5 2 0 199.28 23.90 -6 -2 0 5.30 6.80 -6 -2 0 -3.20 5.80 -6 -2 0 -1.80 6.10 6 2 0 0.30 5.00 -7 -2 0 27.30 10.10 -7 -2 0 16.60 8.60 -7 -2 0 -11.70 13.90 7 2 0 31.80 13.20 7 2 0 17.30 9.00 7 -3 0 5.10 5.70 6 -3 0 46.80 12.80 6 -3 0 50.29 12.90 -6 3 0 43.80 17.30 5 -3 0 472.05 30.60 5 -3 0 492.85 32.70 -5 3 0 480.05 39.20 4 -3 0 -0.30 3.90 4 -3 0 -1.90 2.60 4 -3 0 7.30 4.00 -4 3 0 23.10 8.80 3 -3 0 161.78 12.90 3 -3 0 168.28 15.70 3 -3 0 188.58 14.90 3 -3 0 158.08 13.80 -3 3 0 183.08 8.90 -3 3 0 187.58 17.10 2 -3 0 71.79 6.20 2 -3 0 65.69 7.70 2 -3 0 79.09 8.10 2 -3 0 70.39 8.00 -2 3 0 74.99 8.10 -2 3 0 82.59 7.20 1 -3 0 2281.67 68.99 1 -3 0 2298.07 70.89 1 -3 0 2333.47 60.89 -1 3 0 2155.08 61.19 -1 3 0 2253.17 69.39 0 -3 0 1181.28 40.70 0 -3 0 1202.98 39.30 0 -3 0 1271.57 47.60 0 3 0 1217.08 40.30 0 3 0 1221.98 39.90 0 3 0 1290.17 48.10 -1 -3 0 88.79 7.10 -1 -3 0 80.79 10.80 -1 -3 0 91.59 11.10 1 3 0 96.29 11.20 1 3 0 93.89 7.10 1 3 0 91.49 10.80 -2 -3 0 80.79 7.90 -2 -3 0 80.09 11.70 -2 -3 0 70.29 14.50 2 3 0 96.99 10.90 2 3 0 98.79 7.90 2 3 0 94.29 13.40 -3 -3 0 228.58 20.70 -3 -3 0 264.07 17.20 -3 -3 0 258.97 26.80 3 3 0 253.17 17.70 3 3 0 242.48 24.30 3 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20 18.70 10.50 0 -7 20 9.00 15.90 1 6 -20 -11.00 6.40 -1 -6 20 -10.60 7.00 0 6 -20 -2.80 14.00 0 6 -20 20.30 10.90 0 -6 20 43.30 13.20 -1 6 -20 -17.90 8.50 -1 6 -20 5.40 9.10 1 -6 20 15.50 7.80 1 5 -20 11.40 9.40 -1 -5 20 1.60 9.60 0 5 -20 -8.70 9.40 0 -5 20 26.80 10.60 -1 -4 20 27.30 11.50 0 4 -20 20.10 13.60 0 -4 20 20.50 11.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 54718