# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_d8v20106_0m _database_code_depnum_ccdc_archive 'CCDC 1996923' loop_ _audit_author_name _audit_author_address 'Chenxu Yan' ;East China University Of Science and Technology China ; _audit_update_record ; 2020-04-15 deposited with the CCDC. 2021-06-24 downloaded from the CCDC. ; _audit_creation_method SHELXL-2013 _chemical_name_systematic QM-NH2 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 N4' _chemical_formula_weight 338.40 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 monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.3713(4) _cell_length_b 11.8588(6) _cell_length_c 20.5481(14) _cell_angle_alpha 90 _cell_angle_beta 92.123(2) _cell_angle_gamma 90 _cell_volume 1794.97(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2482 _cell_measurement_theta_min 5.530 _cell_measurement_theta_max 49.243 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_F_000 712 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 0.076 _shelx_estimated_absorpt_T_min 0.987 _shelx_estimated_absorpt_T_max 0.992 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6497 _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 8798 _diffrn_reflns_av_unetI/netI 0.0467 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.624 _diffrn_reflns_theta_max 25.995 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 3494 _reflns_number_gt 2219 _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^)+(0.0564P)^2^+0.1439P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.027(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3494 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1346 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.24291(19) 0.44735(11) 0.38195(8) 0.0534(4) Uani 1 1 d . . . . . N2 N 0.5205(3) 1.15700(14) 0.29002(12) 0.0727(6) Uani 1 1 d . . . . . N3 N 0.2957(3) 0.64674(15) 0.63873(9) 0.0798(6) Uani 1 1 d . . . . . N4 N 0.1900(3) 0.30206(15) 0.67555(10) 0.0838(6) Uani 1 1 d . . . . . C1 C 0.1876(2) 0.34947(14) 0.41326(11) 0.0557(5) Uani 1 1 d . . . . . C2 C 0.1437(3) 0.25269(16) 0.37611(12) 0.0712(6) Uani 1 1 d . . . . . H2 H 0.1591 0.2528 0.3314 0.085 Uiso 1 1 calc R U . . . C3 C 0.0788(3) 0.15871(17) 0.40577(15) 0.0866(8) Uani 1 1 d . . . . . H3 H 0.0522 0.0946 0.3811 0.104 Uiso 1 1 calc R U . . . C4 C 0.0522(4) 0.15777(17) 0.47174(14) 0.0889(8) Uani 1 1 d . . . . . H4 H 0.0032 0.0943 0.4910 0.107 Uiso 1 1 calc R U . . . C5 C 0.0975(3) 0.24977(15) 0.50902(11) 0.0731(6) Uani 1 1 d . . . . . H5 H 0.0803 0.2475 0.5536 0.088 Uiso 1 1 calc R U . . . C6 C 0.1695(2) 0.34778(14) 0.48132(10) 0.0539(5) Uani 1 1 d . . . . . C7 C 0.2169(2) 0.44659(13) 0.51923(10) 0.0508(5) Uani 1 1 d . . . . . C8 C 0.2544(2) 0.54276(14) 0.48311(10) 0.0525(5) Uani 1 1 d . . . . . H8 H 0.2719 0.6102 0.5056 0.063 Uiso 1 1 calc R U . . . C9 C 0.2673(2) 0.54466(14) 0.41691(10) 0.0513(5) Uani 1 1 d . . . . . C10 C 0.2998(2) 0.64984(14) 0.38288(10) 0.0550(5) Uani 1 1 d . . . . . H10 H 0.2611 0.6550 0.3394 0.066 Uiso 1 1 calc R U . . . C11 C 0.3818(2) 0.73949(14) 0.41010(10) 0.0564(5) Uani 1 1 d . . . . . H11 H 0.4271 0.7309 0.4527 0.068 Uiso 1 1 calc R U . . . C12 C 0.4077(2) 0.84935(14) 0.38017(10) 0.0535(5) Uani 1 1 d . . . . . C13 C 0.5224(3) 0.92882(16) 0.41041(11) 0.0664(6) Uani 1 1 d . . . . . H13 H 0.5764 0.9121 0.4509 0.080 Uiso 1 1 calc R U . . . C14 C 0.5580(3) 1.03120(16) 0.38191(11) 0.0676(6) Uani 1 1 d . . . . . H14 H 0.6356 1.0821 0.4032 0.081 Uiso 1 1 calc R U . . . C15 C 0.4792(3) 1.05899(14) 0.32183(10) 0.0557(5) Uani 1 1 d . . . . . C16 C 0.3583(3) 0.98190(15) 0.29306(10) 0.0580(5) Uani 1 1 d . . . . . H16 H 0.2991 1.0001 0.2537 0.070 Uiso 1 1 calc R U . . . C17 C 0.3249(3) 0.88014(15) 0.32130(10) 0.0564(5) Uani 1 1 d . . . . . H17 H 0.2444 0.8303 0.3005 0.068 Uiso 1 1 calc R U . . . C18 C 0.2827(3) 0.44466(16) 0.31190(10) 0.0620(6) Uani 1 1 d . . . . . H18A H 0.3360 0.3722 0.3019 0.074 Uiso 1 1 calc R U . . . H18B H 0.3720 0.5023 0.3033 0.074 Uiso 1 1 calc R U . . . C19 C 0.1187(3) 0.46316(18) 0.26711(11) 0.0770(7) Uani 1 1 d . . . . . H19A H 0.1526 0.4548 0.2227 0.116 Uiso 1 1 calc R U . . . H19B H 0.0720 0.5377 0.2735 0.116 Uiso 1 1 calc R U . . . H19C H 0.0269 0.4087 0.2766 0.116 Uiso 1 1 calc R U . . . C20 C 0.2215(2) 0.45426(14) 0.58793(10) 0.0535(5) Uani 1 1 d . . . . . C21 C 0.2627(3) 0.56043(17) 0.61668(10) 0.0587(5) Uani 1 1 d . . . . . C22 C 0.2021(3) 0.36684(16) 0.63443(11) 0.0615(5) Uani 1 1 d . . . . . H2A H 0.577(3) 1.2078(18) 0.3128(10) 0.079(7) Uiso 1 1 d . . . . . H2B H 0.440(4) 1.180(2) 0.2545(13) 0.113(10) Uiso 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 0.0506(9) 0.0474(9) 0.0626(11) -0.0030(7) 0.0064(8) 0.0014(7) N2 0.0876(14) 0.0458(10) 0.0843(16) 0.0008(10) -0.0021(12) -0.0136(10) N3 0.0973(14) 0.0638(11) 0.0769(14) -0.0013(10) -0.0173(11) -0.0162(10) N4 0.1111(16) 0.0632(11) 0.0775(14) 0.0123(10) 0.0094(12) 0.0001(10) C1 0.0468(10) 0.0442(10) 0.0764(16) -0.0032(10) 0.0053(10) 0.0047(8) C2 0.0788(14) 0.0509(12) 0.0844(17) -0.0135(11) 0.0099(12) -0.0003(10) C3 0.1038(19) 0.0474(12) 0.109(2) -0.0165(13) 0.0057(16) -0.0053(12) C4 0.120(2) 0.0466(12) 0.100(2) 0.0033(12) 0.0050(17) -0.0135(12) C5 0.0904(15) 0.0461(11) 0.0826(17) 0.0041(10) -0.0004(13) -0.0052(10) C6 0.0494(10) 0.0414(10) 0.0708(15) 0.0024(9) 0.0005(10) 0.0037(8) C7 0.0412(9) 0.0439(10) 0.0670(14) 0.0020(9) -0.0019(9) 0.0033(8) C8 0.0509(11) 0.0448(10) 0.0615(14) -0.0017(9) -0.0028(9) -0.0009(8) C9 0.0411(9) 0.0455(10) 0.0670(14) -0.0016(9) 0.0008(9) 0.0012(8) C10 0.0565(11) 0.0481(10) 0.0603(13) 0.0025(9) 0.0022(10) 0.0005(9) C11 0.0544(11) 0.0547(11) 0.0598(13) 0.0040(9) -0.0031(9) -0.0005(9) C12 0.0535(11) 0.0467(10) 0.0601(13) -0.0013(9) -0.0001(9) 0.0001(8) C13 0.0709(13) 0.0604(12) 0.0666(14) -0.0001(10) -0.0174(11) -0.0066(10) C14 0.0694(13) 0.0520(11) 0.0804(16) -0.0068(11) -0.0127(12) -0.0129(10) C15 0.0587(11) 0.0440(10) 0.0645(14) -0.0044(9) 0.0035(10) -0.0009(8) C16 0.0667(12) 0.0498(11) 0.0568(13) -0.0011(9) -0.0052(10) -0.0019(9) C17 0.0596(11) 0.0478(10) 0.0611(13) -0.0036(9) -0.0081(10) -0.0048(9) C18 0.0603(12) 0.0583(12) 0.0682(15) -0.0071(10) 0.0120(11) 0.0039(9) C19 0.0735(15) 0.0852(15) 0.0720(16) -0.0106(12) -0.0015(12) 0.0008(12) C20 0.0521(11) 0.0454(10) 0.0627(14) 0.0026(9) -0.0029(9) 0.0003(8) C21 0.0579(12) 0.0591(12) 0.0584(14) 0.0061(10) -0.0077(10) -0.0040(10) C22 0.0648(12) 0.0530(11) 0.0667(15) -0.0001(11) 0.0018(11) 0.0019(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 1.368(2) . ? N1 C1 1.395(2) . ? N1 C18 1.480(2) . ? N2 C15 1.373(2) . ? N2 H2A 0.86(2) . ? N2 H2B 0.96(3) . ? N3 C21 1.142(2) . ? N4 C22 1.148(2) . ? C1 C2 1.409(3) . ? C1 C6 1.410(3) . ? C2 C3 1.365(3) . ? C2 H2 0.9300 . ? C3 C4 1.377(3) . ? C3 H3 0.9300 . ? C4 C5 1.367(3) . ? C4 H4 0.9300 . ? C5 C6 1.407(2) . ? C5 H5 0.9300 . ? C6 C7 1.443(2) . ? C7 C8 1.394(2) . ? C7 C20 1.414(3) . ? C8 C9 1.367(3) . ? C8 H8 0.9300 . ? C9 C10 1.454(2) . ? C10 C11 1.335(2) . ? C10 H10 0.9300 . ? C11 C12 1.456(2) . ? C11 H11 0.9300 . ? C12 C17 1.384(3) . ? C12 C13 1.397(3) . ? C13 C14 1.377(3) . ? C13 H13 0.9300 . ? C14 C15 1.384(3) . ? C14 H14 0.9300 . ? C15 C16 1.393(2) . ? C16 C17 1.365(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.508(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.419(3) . ? C20 C22 1.421(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 119.65(17) . . ? C9 N1 C18 120.14(15) . . ? C1 N1 C18 120.16(15) . . ? C15 N2 H2A 116.4(15) . . ? C15 N2 H2B 117.3(15) . . ? H2A N2 H2B 119(2) . . ? N1 C1 C2 119.52(19) . . ? N1 C1 C6 120.62(16) . . ? C2 C1 C6 119.83(17) . . ? C3 C2 C1 120.0(2) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.7(2) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.4(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 117.65(18) . . ? C5 C6 C7 122.69(19) . . ? C1 C6 C7 119.60(16) . . ? C8 C7 C20 118.76(16) . . ? C8 C7 C6 115.20(18) . . ? C20 C7 C6 126.00(16) . . ? C9 C8 C7 124.45(17) . . ? C9 C8 H8 117.8 . . ? C7 C8 H8 117.8 . . ? C8 C9 N1 119.73(16) . . ? C8 C9 C10 120.75(16) . . ? N1 C9 C10 119.48(18) . . ? C11 C10 C9 124.17(19) . . ? C11 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? C10 C11 C12 126.84(19) . . ? C10 C11 H11 116.6 . . ? C12 C11 H11 116.6 . . ? C17 C12 C13 116.82(17) . . ? C17 C12 C11 123.02(17) . . ? C13 C12 C11 120.16(19) . . ? C14 C13 C12 121.8(2) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 120.59(18) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? N2 C15 C14 122.19(19) . . ? N2 C15 C16 120.2(2) . . ? C14 C15 C16 117.58(17) . . ? C17 C16 C15 121.49(19) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C12 121.60(18) . . ? C16 C17 H17 119.2 . . ? C12 C17 H17 119.2 . . ? N1 C18 C19 114.03(16) . . ? N1 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? N1 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C7 C20 C21 118.02(16) . . ? C7 C20 C22 128.71(16) . . ? C21 C20 C22 113.13(18) . . ? N3 C21 C20 178.8(2) . . ? N4 C22 C20 174.8(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 173.23(16) . . . . ? C18 N1 C1 C2 -9.4(3) . . . . ? C9 N1 C1 C6 -4.7(3) . . . . ? C18 N1 C1 C6 172.67(16) . . . . ? N1 C1 C2 C3 -175.97(19) . . . . ? C6 C1 C2 C3 2.0(3) . . . . ? C1 C2 C3 C4 1.2(4) . . . . ? C2 C3 C4 C5 -2.6(4) . . . . ? C3 C4 C5 C6 0.9(4) . . . . ? C4 C5 C6 C1 2.2(3) . . . . ? C4 C5 C6 C7 179.4(2) . . . . ? N1 C1 C6 C5 174.35(16) . . . . ? C2 C1 C6 C5 -3.6(3) . . . . ? N1 C1 C6 C7 -2.9(3) . . . . ? C2 C1 C6 C7 179.15(17) . . . . ? C5 C6 C7 C8 -168.67(17) . . . . ? C1 C6 C7 C8 8.5(2) . . . . ? C5 C6 C7 C20 8.9(3) . . . . ? C1 C6 C7 C20 -173.95(17) . . . . ? C20 C7 C8 C9 175.04(16) . . . . ? C6 C7 C8 C9 -7.2(3) . . . . ? C7 C8 C9 N1 -0.1(3) . . . . ? C7 C8 C9 C10 177.53(16) . . . . ? C1 N1 C9 C8 6.3(2) . . . . ? C18 N1 C9 C8 -171.06(16) . . . . ? C1 N1 C9 C10 -171.37(15) . . . . ? C18 N1 C9 C10 11.3(2) . . . . ? C8 C9 C10 C11 25.1(3) . . . . ? N1 C9 C10 C11 -157.22(17) . . . . ? C9 C10 C11 C12 -175.61(16) . . . . ? C10 C11 C12 C17 10.0(3) . . . . ? C10 C11 C12 C13 -169.09(19) . . . . ? C17 C12 C13 C14 -2.7(3) . . . . ? C11 C12 C13 C14 176.44(18) . . . . ? C12 C13 C14 C15 0.4(3) . . . . ? C13 C14 C15 N2 -175.66(19) . . . . ? C13 C14 C15 C16 2.5(3) . . . . ? N2 C15 C16 C17 175.12(18) . . . . ? C14 C15 C16 C17 -3.1(3) . . . . ? C15 C16 C17 C12 0.8(3) . . . . ? C13 C12 C17 C16 2.1(3) . . . . ? C11 C12 C17 C16 -176.98(17) . . . . ? C9 N1 C18 C19 -95.8(2) . . . . ? C1 N1 C18 C19 86.8(2) . . . . ? C8 C7 C20 C21 0.6(3) . . . . ? C6 C7 C20 C21 -176.90(17) . . . . ? C8 C7 C20 C22 -174.69(18) . . . . ? C6 C7 C20 C22 7.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2B N4 0.96(3) 2.42(3) 3.358(3) 165(2) 4_575 N2 H2A N3 0.86(2) 2.19(2) 3.041(3) 172(2) 3_676 _refine_diff_density_max 0.113 _refine_diff_density_min -0.132 _refine_diff_density_rms 0.027 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_d8v20106_0m_a.res in P2(1)/c CELL 0.71073 7.3713 11.8588 20.5481 90 92.123 90 ZERR 4 0.0004 0.0006 0.0014 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N UNIT 88 72 16 OMIT -3.00 52.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 HTAB N2 N4_$2 EQIV $2 x, -y+3/2, z-1/2 HTAB N2 N3_$1 EQIV $1 -x+1, -y+2, -z+1 conf htab mpla n1 c1 > c9 mpla c12 > c17 wpdb -1 size 0.17 0.13 0.10 TEMP 19.96 WGHT 0.056400 0.143900 EXTI 0.026583 FVAR 1.12010 N1 3 0.242908 0.447347 0.381949 11.00000 0.05055 0.04743 = 0.06260 -0.00296 0.00640 0.00143 N2 3 0.520495 1.157000 0.290019 11.00000 0.08761 0.04577 = 0.08431 0.00080 -0.00211 -0.01359 N3 3 0.295699 0.646736 0.638726 11.00000 0.09732 0.06377 = 0.07691 -0.00128 -0.01733 -0.01622 N4 3 0.190015 0.302058 0.675550 11.00000 0.11107 0.06322 = 0.07754 0.01228 0.00940 0.00006 C1 1 0.187552 0.349471 0.413263 11.00000 0.04677 0.04419 = 0.07638 -0.00319 0.00526 0.00474 C2 1 0.143737 0.252686 0.376111 11.00000 0.07883 0.05092 = 0.08439 -0.01349 0.00985 -0.00030 AFIX 43 H2 2 0.159067 0.252827 0.331390 11.00000 -1.20000 AFIX 0 C3 1 0.078783 0.158709 0.405771 11.00000 0.10379 0.04736 = 0.10878 -0.01652 0.00566 -0.00526 AFIX 43 H3 2 0.052213 0.094615 0.381140 11.00000 -1.20000 AFIX 0 C4 1 0.052179 0.157774 0.471742 11.00000 0.12027 0.04663 = 0.10001 0.00335 0.00502 -0.01345 AFIX 43 H4 2 0.003199 0.094285 0.491031 11.00000 -1.20000 AFIX 0 C5 1 0.097452 0.249769 0.509019 11.00000 0.09036 0.04608 = 0.08257 0.00408 -0.00038 -0.00522 AFIX 43 H5 2 0.080287 0.247504 0.553611 11.00000 -1.20000 AFIX 0 C6 1 0.169457 0.347778 0.481321 11.00000 0.04939 0.04138 = 0.07082 0.00243 0.00053 0.00368 C7 1 0.216886 0.446588 0.519229 11.00000 0.04124 0.04385 = 0.06697 0.00204 -0.00186 0.00333 C8 1 0.254424 0.542755 0.483107 11.00000 0.05090 0.04481 = 0.06148 -0.00174 -0.00279 -0.00094 AFIX 43 H8 2 0.271891 0.610204 0.505564 11.00000 -1.20000 AFIX 0 C9 1 0.267310 0.544664 0.416906 11.00000 0.04112 0.04554 = 0.06702 -0.00161 0.00078 0.00118 C10 1 0.299848 0.649843 0.382881 11.00000 0.05647 0.04813 = 0.06035 0.00253 0.00217 0.00049 AFIX 43 H10 2 0.261120 0.655001 0.339392 11.00000 -1.20000 AFIX 0 C11 1 0.381788 0.739489 0.410103 11.00000 0.05441 0.05469 = 0.05980 0.00401 -0.00307 -0.00051 AFIX 43 H11 2 0.427089 0.730865 0.452657 11.00000 -1.20000 AFIX 0 C12 1 0.407680 0.849347 0.380165 11.00000 0.05347 0.04667 = 0.06012 -0.00131 -0.00015 0.00011 C13 1 0.522448 0.928824 0.410409 11.00000 0.07089 0.06035 = 0.06662 -0.00009 -0.01737 -0.00658 AFIX 43 H13 2 0.576361 0.912147 0.450903 11.00000 -1.20000 AFIX 0 C14 1 0.557960 1.031203 0.381910 11.00000 0.06944 0.05197 = 0.08036 -0.00678 -0.01273 -0.01289 AFIX 43 H14 2 0.635563 1.082124 0.403211 11.00000 -1.20000 AFIX 0 C15 1 0.479160 1.058989 0.321833 11.00000 0.05875 0.04397 = 0.06454 -0.00435 0.00354 -0.00086 C16 1 0.358319 0.981902 0.293056 11.00000 0.06671 0.04982 = 0.05681 -0.00112 -0.00522 -0.00191 AFIX 43 H16 2 0.299079 1.000148 0.253713 11.00000 -1.20000 AFIX 0 C17 1 0.324854 0.880142 0.321300 11.00000 0.05960 0.04775 = 0.06107 -0.00365 -0.00811 -0.00485 AFIX 43 H17 2 0.244438 0.830323 0.300464 11.00000 -1.20000 AFIX 0 C18 1 0.282678 0.444658 0.311899 11.00000 0.06034 0.05826 = 0.06818 -0.00713 0.01196 0.00387 AFIX 23 H18A 2 0.335954 0.372191 0.301904 11.00000 -1.20000 H18B 2 0.372046 0.502313 0.303346 11.00000 -1.20000 AFIX 0 C19 1 0.118656 0.463157 0.267109 11.00000 0.07347 0.08517 = 0.07205 -0.01065 -0.00147 0.00077 AFIX 137 H19A 2 0.152643 0.454810 0.222715 11.00000 -1.50000 H19B 2 0.071974 0.537744 0.273542 11.00000 -1.50000 H19C 2 0.026944 0.408694 0.276558 11.00000 -1.50000 AFIX 0 C20 1 0.221519 0.454259 0.587926 11.00000 0.05214 0.04539 = 0.06274 0.00255 -0.00289 0.00026 C21 1 0.262737 0.560435 0.616684 11.00000 0.05788 0.05907 = 0.05842 0.00610 -0.00769 -0.00396 C22 1 0.202061 0.366840 0.634430 11.00000 0.06481 0.05303 = 0.06672 -0.00006 0.00176 0.00191 H2A 2 0.577169 1.207812 0.312827 11.00000 0.07884 H2B 2 0.439902 1.180017 0.254488 11.00000 0.11325 HKLF 4 REM mo_d8v20106_0m_a.res in P2(1)/c REM R1 = 0.0490 for 2219 Fo > 4sig(Fo) and 0.0868 for all 3494 data REM 245 parameters refined using 0 restraints END WGHT 0.0464 0.1717 REM Instructions for potential hydrogen bonds HTAB N2 N3_$1 HTAB N2 N4_$2 REM Highest difference peak 0.113, deepest hole -0.132, 1-sigma level 0.027 Q1 1 0.1235 0.2658 0.3183 11.00000 0.05 0.11 Q2 1 0.0986 0.0770 0.5032 11.00000 0.05 0.10 Q3 1 -0.0098 0.1051 0.3517 11.00000 0.05 0.10 Q4 1 0.1709 0.1581 0.4868 11.00000 0.05 0.10 Q5 1 0.0781 0.2353 0.6320 11.00000 0.05 0.10 Q6 1 0.2922 0.4636 0.6308 11.00000 0.05 0.09 Q7 1 0.1943 0.6781 0.3280 11.00000 0.05 0.09 Q8 1 0.4733 0.9766 0.3006 11.00000 0.05 0.09 Q9 1 0.1784 0.4257 0.6112 11.00000 0.05 0.09 Q10 1 0.2612 0.5965 0.4028 11.00000 0.05 0.09 Q11 1 0.3024 0.8210 0.2866 11.00000 0.05 0.09 Q12 1 0.6821 0.9010 0.4425 11.00000 0.05 0.09 Q13 1 0.3619 1.0372 0.3251 11.00000 0.05 0.09 Q14 1 0.4201 0.8175 0.3959 11.00000 0.05 0.09 Q15 1 0.1633 0.4468 0.5561 11.00000 0.05 0.09 Q16 1 0.1741 0.3947 0.4036 11.00000 0.05 0.08 Q17 1 0.3586 0.9917 0.2247 11.00000 0.05 0.08 Q18 1 0.2299 0.2595 0.5114 11.00000 0.05 0.08 Q19 1 0.4396 1.0544 0.3720 11.00000 0.05 0.08 Q20 1 0.3888 0.7178 0.6306 11.00000 0.05 0.08 ; _shelx_res_checksum 99199 _shelx_hkl_file ; -1 0 0 1727.93 33.30 3 0 0 2010.10 47.70 -3 0 0 1991.70 47.80 4 0 0 1544.35 38.90 -4 0 0 1550.64 44.00 4 0 0 1520.45 43.40 5 0 0 36.00 6.50 -5 0 0 40.60 8.10 5 0 0 50.19 8.80 6 0 0 90.99 9.70 -6 0 0 83.99 13.00 -7 0 0 5.60 6.30 7 0 0 9.70 4.30 -8 0 0 9.90 6.30 8 0 0 3.00 4.70 9 0 0 11.50 6.20 0 -1 0 0.20 0.30 0 -1 0 -0.10 0.10 -1 -1 0 2116.39 37.30 1 -1 0 2154.58 42.10 -1 1 0 2090.49 42.00 3 -1 0 129.09 10.20 -3 -1 0 122.89 8.70 3 -1 0 127.59 8.30 -3 1 0 139.89 10.50 3 1 0 118.49 8.40 4 -1 0 850.21 32.00 4 -1 0 898.11 28.20 -4 -1 0 875.41 29.70 4 1 0 926.31 30.00 4 1 0 931.51 26.50 -4 1 0 922.11 33.10 -5 -1 0 27.30 6.60 5 -1 0 23.40 6.70 5 -1 0 18.60 5.10 5 1 0 28.90 6.30 5 1 0 26.30 5.30 -5 1 0 22.80 6.10 6 -1 0 110.29 11.30 -6 -1 0 102.39 12.20 6 1 0 96.59 11.70 -6 1 0 105.49 13.40 6 1 0 105.19 9.90 7 -1 0 79.49 10.10 -7 -1 0 60.49 11.50 -7 1 0 39.60 9.80 7 1 0 66.99 10.70 8 -1 0 11.40 6.40 -8 -1 0 19.00 7.80 -8 1 0 12.40 6.80 8 1 0 23.80 6.90 9 -1 0 0.30 4.40 9 1 0 7.60 5.60 0 -2 0 4406.26 75.49 1 -2 0 4002.00 81.39 1 -2 0 3951.90 71.69 -1 2 0 4086.59 75.59 1 2 0 4121.89 65.59 -2 -2 0 3084.89 56.09 2 -2 0 3193.08 65.69 2 -2 0 2971.10 60.09 2 2 0 3098.99 55.69 -2 2 0 3104.69 65.49 -3 -2 0 107.89 7.40 3 -2 0 103.59 8.00 3 -2 0 116.49 10.10 3 2 0 98.89 7.10 -3 2 0 106.39 9.80 4 -2 0 3127.79 68.39 4 -2 0 3046.90 75.19 -4 -2 0 3036.30 66.59 4 2 0 3106.29 66.29 4 2 0 3148.68 62.09 -4 2 0 3032.70 74.89 5 -2 0 90.79 9.40 -5 -2 0 86.69 9.30 -5 2 0 76.49 12.50 5 2 0 78.79 8.70 5 2 0 101.29 8.40 -6 -2 0 183.78 18.80 6 -2 0 227.68 16.30 6 2 0 188.08 20.70 6 2 0 214.28 15.80 -6 2 0 198.78 18.20 -7 -2 0 3.10 4.30 7 -2 0 6.70 4.60 -7 2 0 1.10 4.90 7 2 0 10.10 3.90 8 -2 0 43.00 10.40 -8 2 0 38.80 11.40 8 2 0 76.69 9.60 9 -2 0 17.00 7.50 9 2 0 15.40 6.10 0 -3 0 -0.20 1.00 0 -3 0 0.20 0.70 0 3 0 0.10 0.70 1 -3 0 80.29 5.40 -1 -3 0 86.59 3.10 1 -3 0 86.09 6.70 -1 3 0 70.89 6.30 1 3 0 85.29 2.80 2 -3 0 32.10 6.00 -2 -3 0 36.40 2.70 2 -3 0 32.10 4.20 -2 3 0 39.80 6.60 2 3 0 38.40 2.50 -3 -3 0 17.00 3.00 3 -3 0 14.80 4.90 3 -3 0 12.00 3.70 -3 3 0 21.00 5.80 3 3 0 12.40 2.60 4 -3 0 870.51 35.20 -4 -3 0 877.31 26.60 4 3 0 924.71 24.00 4 3 0 923.51 26.50 5 -3 0 64.69 8.30 -5 -3 0 37.30 6.80 -5 3 0 41.30 9.60 5 3 0 61.89 6.20 5 3 0 51.89 6.70 -6 -3 0 263.27 17.60 6 -3 0 242.28 17.30 -6 3 0 293.37 23.00 6 3 0 235.28 19.40 6 3 0 239.88 13.80 7 -3 0 1.20 4.30 -7 3 0 11.00 6.10 7 3 0 7.90 3.40 8 -3 0 50.79 11.30 8 3 0 77.39 9.60 -8 3 0 61.49 14.30 9 -3 0 -6.50 5.20 9 3 0 3.40 4.40 0 -4 0 318.57 12.20 0 -4 0 292.27 9.80 1 -4 0 45.80 5.40 -1 -4 0 51.79 3.40 -1 -4 0 48.60 2.60 1 -4 0 54.29 4.70 1 4 0 51.09 2.70 -1 4 0 53.09 5.80 -2 -4 0 5.30 1.00 2 -4 0 3.90 2.30 2 -4 0 9.10 3.40 2 4 0 5.20 0.80 -3 -4 0 32.60 3.20 3 -4 0 36.70 6.20 3 -4 0 31.20 11.50 3 4 0 35.10 3.00 -3 4 0 43.10 8.10 -4 -4 0 256.27 11.70 4 -4 0 260.47 15.50 -4 4 0 258.27 18.60 4 4 0 268.57 11.30 4 4 0 250.97 10.10 -5 -4 0 5.60 2.60 5 -4 0 -2.40 2.50 5 4 0 4.60 2.20 -5 4 0 1.60 2.60 5 4 0 -2.10 2.30 -6 -4 0 197.88 13.50 6 -4 0 198.68 16.30 6 4 0 181.88 11.30 6 4 0 186.08 12.70 -6 4 0 174.68 18.90 7 -4 0 -2.80 4.00 7 4 0 2.40 3.50 -7 4 0 -3.00 6.00 7 4 0 1.10 2.60 8 -4 0 135.49 15.50 8 4 0 149.88 12.10 -8 4 0 111.69 19.30 9 -4 0 5.00 5.30 9 4 0 5.50 4.60 0 -5 0 0.30 0.90 0 -5 0 -1.20 1.20 -1 -5 0 783.72 19.40 1 -5 0 805.32 22.80 1 -5 0 782.22 26.50 -1 -5 0 794.32 17.00 -1 5 0 794.22 26.50 2 -5 0 58.69 6.20 2 -5 0 56.59 7.30 -2 5 0 65.59 8.20 -3 -5 0 46.30 2.60 3 -5 0 44.20 7.10 3 -5 0 47.60 8.60 3 5 0 48.40 2.30 -3 5 0 44.20 8.90 3 5 0 46.90 2.20 4 -5 0 18.20 5.40 -4 5 0 31.10 8.00 4 5 0 25.20 3.10 4 5 0 18.20 3.00 5 -5 0 24.40 6.40 -5 -5 0 31.90 5.00 -5 5 0 41.80 10.80 5 5 0 22.70 3.70 5 5 0 29.80 4.60 6 -5 0 259.97 18.90 6 5 0 246.18 13.20 6 5 0 227.18 11.60 -6 5 0 229.28 21.70 7 -5 0 -3.00 3.20 7 5 0 -0.80 1.90 -7 5 0 -1.10 3.10 7 5 0 0.00 3.60 8 -5 0 47.50 10.80 8 5 0 42.80 7.30 9 -5 0 -4.60 5.30 9 5 0 1.90 5.60 0 -6 0 488.05 18.60 0 -6 0 502.75 15.60 -1 -6 0 -0.90 1.20 1 -6 0 -3.10 1.90 1 -6 0 1.30 1.30 -1 -6 0 1.90 0.90 -2 -6 0 1.60 0.70 2 -6 0 0.00 1.80 -2 -6 0 1.10 0.70 2 -6 0 4.20 4.90 3 -6 0 25.40 5.70 3 -6 0 22.50 6.50 -3 6 0 17.10 5.60 4 -6 0 23.90 6.10 -4 6 0 40.90 9.60 5 -6 0 35.10 8.40 5 6 0 44.60 3.60 -5 6 0 37.50 9.70 5 6 0 36.30 4.00 6 -6 0 52.09 15.30 6 6 0 56.29 4.80 6 6 0 48.30 5.60 -6 6 0 58.89 19.90 7 -6 0 1.10 4.20 7 6 0 6.70 3.40 7 6 0 8.10 2.90 -7 6 0 2.10 7.20 8 -6 0 60.29 12.30 8 6 0 59.29 6.70 0 -7 0 5.30 2.80 0 -7 0 3.60 1.80 -1 -7 0 64.59 5.70 -1 -7 0 65.59 4.40 1 -7 0 79.49 8.60 1 -7 0 74.69 6.90 -2 -7 0 89.59 4.40 -2 -7 0 92.29 3.90 2 -7 0 93.99 8.60 2 -7 0 83.29 10.00 -2 7 0 97.39 10.60 3 -7 0 30.00 6.50 -3 7 0 24.00 7.20 4 -7 0 7.80 4.00 -4 7 0 13.60 5.60 5 -7 0 25.50 7.60 -5 7 0 12.70 6.40 6 -7 0 117.39 13.80 -6 7 0 100.59 17.60 7 -7 0 10.40 5.80 7 7 0 10.60 2.00 8 -7 0 10.50 6.20 0 -8 0 115.19 9.90 0 -8 0 143.39 8.60 1 -8 0 50.79 14.60 -1 -8 0 44.40 4.20 1 -8 0 55.39 6.30 -1 -8 0 50.89 5.90 -2 -8 0 103.69 5.30 -2 -8 0 100.79 4.80 2 -8 0 99.39 11.30 2 -8 0 113.19 9.80 3 -8 0 256.87 16.50 4 -8 0 1373.86 45.60 -4 8 0 1428.26 54.59 5 -8 0 4.20 4.90 6 -8 0 62.69 11.50 7 -8 0 1.20 3.70 8 -8 0 28.30 7.10 0 -9 0 -3.50 2.90 0 -9 0 1.60 1.80 1 -9 0 14.00 5.90 -1 -9 0 22.90 3.80 1 -9 0 17.30 4.70 -1 -9 0 9.70 4.00 -2 -9 0 1870.31 37.40 2 -9 0 1874.41 50.19 -2 -9 0 1863.41 35.80 3 -9 0 -4.60 2.90 4 -9 0 23.60 6.50 5 -9 0 25.30 7.60 6 -9 0 29.20 8.60 7 -9 0 4.00 4.80 0 -10 0 5779.92 108.29 0 -10 0 5780.72 119.19 -1 -10 0 2.60 3.40 1 -10 0 -0.20 2.80 1 -10 0 5.00 5.30 -1 -10 0 2.00 1.90 -2 -10 0 321.87 11.30 2 -10 0 330.87 18.60 3 -10 0 183.48 14.90 4 -10 0 227.98 21.50 5 -10 0 21.00 6.90 6 -10 0 44.40 10.40 7 -10 0 -1.70 3.90 0 -11 0 -1.20 2.20 0 -11 0 -0.70 4.10 -1 -11 0 143.09 8.60 1 -11 0 123.29 10.80 -1 -11 0 128.99 10.80 2 -11 0 166.28 13.90 3 -11 0 43.60 9.10 4 -11 0 -2.90 3.00 5 -11 0 1.00 3.90 6 -11 0 6.10 4.90 0 -12 0 -1.60 5.20 0 -12 0 9.10 3.30 1 -12 0 14.40 4.90 -1 -12 0 26.70 6.20 -1 -12 0 19.10 4.40 2 -12 0 419.86 22.50 3 -12 0 -1.50 4.00 4 -12 0 125.19 14.20 5 -12 0 -1.60 4.60 0 -13 0 3.90 3.20 -1 -13 0 24.10 4.70 -1 -13 0 19.70 6.60 1 -13 0 17.50 5.30 2 -13 0 11.20 4.50 3 -13 0 18.00 6.10 4 -13 0 66.49 12.50 5 -13 0 0.00 5.50 0 -14 0 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