####################################################################### # # 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_RS010 _database_code_depnum_ccdc_archive 'CCDC 2127619' loop_ _audit_author_name _audit_author_address 'Rui Sun' ;Harvard University United States of America ; _audit_update_record ; 2021-12-09 deposited with the CCDC. 2021-12-30 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 F4 N4' _chemical_formula_weight 798.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 9.2143(2) _cell_length_b 12.7406(3) _cell_length_c 12.6200(3) _cell_angle_alpha 85.1670(10) _cell_angle_beta 73.2420(10) _cell_angle_gamma 71.7860(10) _cell_volume 1347.51(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5704 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.5 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.984 _exptl_crystal_F_000 418 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.548 _shelx_estimated_absorpt_T_min 0.957 _shelx_estimated_absorpt_T_max 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7526 _exptl_absorpt_correction_T_max 0.8014 _exptl_absorpt_process_details TWINABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'I\mS microfocus tube' _diffrn_radiation_monochromator 'multilayer mirror' _diffrn_measurement_device_type ; Bruker D8 goniometer with CCD area detector ; _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4572 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.652 _diffrn_reflns_theta_max 66.642 _diffrn_reflns_theta_full 66.642 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measured_fraction_theta_full 0.947 _diffrn_reflns_Laue_measured_fraction_max 0.947 _diffrn_reflns_Laue_measured_fraction_full 0.947 _diffrn_reflns_point_group_measured_fraction_max 0.947 _diffrn_reflns_point_group_measured_fraction_full 0.947 _reflns_number_total 4572 _reflns_number_gt 3450 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT 8.37A (Bruker-AXS, 2015)' _computing_data_reduction 'SAINT 8.37A (Bruker-AXS, 2015)' _computing_structure_solution 'SHELXT-2014 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2015)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2015)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2015)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. All non-H atoms were located in difference-Fourier maps, and then refined anisotropically. The crystal is 4-component non-merohedrol twin, but we have well refined the structure by using reflections in hkl5 format that is created by Cell_Now/Twinabs.Refined. The severe disorder solvent could not be located in the Fourier map and have been squeezed out by using PLATON/SQUEEZE. ; # start Validation Reply Form _vrf_PLAT029_RS010 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.947 Why? RESPONSE: This is the twinning crystal collected on a fixed Chi diffractometer with Cu radiation ; _vrf_PLAT911_RS010 ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.595 332 Report RESPONSE: This is the twinning crystal collected on a fixed Chi diffractometer with Cu radiation ; # end Validation Reply Form _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^)+(0.0984P)^2^+0.0259P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4572 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1666 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 F1 F 0.2802(2) 0.70712(13) 0.26184(17) 0.0812(6) Uani 1 1 d . . . . . F2 F 0.0068(2) 0.23564(16) 1.20633(13) 0.0779(5) Uani 1 1 d . . . . . N1 N 0.5423(2) 0.07459(14) 0.34828(15) 0.0407(4) Uani 1 1 d . . . . . H1 H 0.5264 0.0430 0.4136 0.049 Uiso 0.5 1 calc R U P A 2 N2 N 0.3769(2) 0.15189(15) 0.57337(14) 0.0402(4) Uani 1 1 d . . . . . H2 H 0.4281 0.0868 0.5415 0.048 Uiso 0.5 1 calc R U P B 1 C1 C 0.6210(3) 0.02172(18) 0.24886(17) 0.0403(5) Uani 1 1 d . . . . . C2 C 0.6208(3) 0.10218(19) 0.16273(18) 0.0439(5) Uani 1 1 d . . . . . H2A H 0.6673 0.0876 0.0857 0.053 Uiso 1 1 calc R U . . . C3 C 0.5428(3) 0.20243(18) 0.21057(18) 0.0424(5) Uani 1 1 d . . . . . H3 H 0.5244 0.2714 0.1736 0.051 Uiso 1 1 calc R U . . . C4 C 0.4924(3) 0.18537(18) 0.32821(18) 0.0414(5) Uani 1 1 d . . . . . C5 C 0.4060(3) 0.26918(18) 0.40734(18) 0.0400(5) Uani 1 1 d . . . . . C6 C 0.3519(3) 0.25206(17) 0.52113(19) 0.0418(5) Uani 1 1 d . . . . . C7 C 0.2630(3) 0.33731(18) 0.60243(19) 0.0433(5) Uani 1 1 d . . . . . H7 H 0.2295 0.4143 0.5884 0.052 Uiso 1 1 calc R U . . . C8 C 0.2351(3) 0.28917(18) 0.70204(18) 0.0427(5) Uani 1 1 d . . . . . H8 H 0.1784 0.3257 0.7711 0.051 Uiso 1 1 calc R U . . . C9 C 0.3072(3) 0.17179(18) 0.68453(18) 0.0410(5) Uani 1 1 d . . . . . C10 C 0.3085(3) 0.09200(18) 0.76804(17) 0.0396(5) Uani 1 1 d . . . . . C11 C 0.3704(3) 0.38682(19) 0.36770(17) 0.0418(5) Uani 1 1 d . . . . . C12 C 0.2235(3) 0.44155(19) 0.34866(19) 0.0447(5) Uani 1 1 d . . . . . C13 C 0.1940(3) 0.5510(2) 0.3130(2) 0.0518(6) Uani 1 1 d . . . . . H13 H 0.0947 0.5903 0.2999 0.062 Uiso 1 1 calc R U . . . C14 C 0.3103(3) 0.6007(2) 0.2973(2) 0.0557(7) Uani 1 1 d . . . . . C15 C 0.4548(3) 0.5496(2) 0.3153(2) 0.0552(6) Uani 1 1 d . . . . . H15 H 0.5315 0.5878 0.3038 0.066 Uiso 1 1 calc R U . . . C16 C 0.4885(3) 0.4393(2) 0.3512(2) 0.0472(6) Uani 1 1 d . . . . . C17 C 0.0971(3) 0.3853(2) 0.3668(2) 0.0554(6) Uani 1 1 d . . . . . H17A H 0.1469 0.3077 0.3436 0.083 Uiso 1 1 calc R U . . . H17B H 0.0232 0.4223 0.3233 0.083 Uiso 1 1 calc R U . . . H17C H 0.0390 0.3891 0.4455 0.083 Uiso 1 1 calc R U . . . C18 C 0.6472(3) 0.3814(2) 0.3722(2) 0.0569(6) Uani 1 1 d . . . . . H18A H 0.6325 0.3687 0.4518 0.085 Uiso 1 1 calc R U . . . H18B H 0.7179 0.4275 0.3458 0.085 Uiso 1 1 calc R U . . . H18C H 0.6945 0.3104 0.3328 0.085 Uiso 1 1 calc R U . . . C19 C 0.2262(3) 0.13180(17) 0.88540(18) 0.0415(5) Uani 1 1 d . . . . . C20 C 0.0647(3) 0.1429(2) 0.9297(2) 0.0465(6) Uani 1 1 d . . . . . C21 C -0.0085(3) 0.1783(2) 1.0401(2) 0.0543(6) Uani 1 1 d . . . . . H21 H -0.1181 0.1863 1.0725 0.065 Uiso 1 1 calc R U . . . C22 C 0.0798(3) 0.2009(2) 1.1000(2) 0.0573(7) Uani 1 1 d . . . . . C23 C 0.2379(3) 0.1908(2) 1.0583(2) 0.0550(6) Uani 1 1 d . . . . . H23 H 0.2953 0.2069 1.1031 0.066 Uiso 1 1 calc R U . . . C24 C 0.3138(3) 0.1562(2) 0.94840(19) 0.0475(6) Uani 1 1 d . . . . . C25 C -0.0298(3) 0.1161(2) 0.8625(2) 0.0565(6) Uani 1 1 d . . . . . H25A H -0.0269 0.1631 0.7968 0.085 Uiso 1 1 calc R U . . . H25B H -0.1403 0.1293 0.9073 0.085 Uiso 1 1 calc R U . . . H25C H 0.0159 0.0383 0.8395 0.085 Uiso 1 1 calc R U . . . C26 C 0.4877(3) 0.1455(3) 0.9006(2) 0.0563(7) Uani 1 1 d . . . . . H26A H 0.5504 0.0674 0.8987 0.084 Uiso 1 1 calc R U . . . H26B H 0.5202 0.1871 0.9466 0.084 Uiso 1 1 calc R U . . . H26C H 0.5057 0.1750 0.8252 0.084 Uiso 1 1 calc R U . . . 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 F1 0.0830(12) 0.0427(9) 0.1097(15) 0.0310(10) -0.0270(10) -0.0154(8) F2 0.0767(11) 0.1045(14) 0.0404(8) -0.0253(9) 0.0066(7) -0.0250(10) N1 0.0476(10) 0.0336(9) 0.0349(9) -0.0004(8) -0.0090(8) -0.0061(8) N2 0.0482(10) 0.0351(9) 0.0316(9) 0.0025(8) -0.0087(7) -0.0073(8) C1 0.0436(12) 0.0404(12) 0.0321(10) -0.0002(10) -0.0083(9) -0.0079(9) C2 0.0515(13) 0.0415(12) 0.0321(11) 0.0014(10) -0.0069(9) -0.0097(10) C3 0.0495(12) 0.0350(11) 0.0375(11) 0.0049(10) -0.0102(9) -0.0084(9) C4 0.0442(12) 0.0387(12) 0.0385(11) 0.0007(10) -0.0114(9) -0.0089(9) C5 0.0450(12) 0.0322(11) 0.0378(11) 0.0014(10) -0.0095(9) -0.0069(9) C6 0.0473(12) 0.0307(10) 0.0417(12) -0.0009(10) -0.0110(9) -0.0048(9) C7 0.0468(12) 0.0334(11) 0.0429(12) -0.0027(10) -0.0092(10) -0.0049(9) C8 0.0457(12) 0.0382(12) 0.0370(11) -0.0041(10) -0.0080(9) -0.0047(9) C9 0.0434(11) 0.0399(12) 0.0353(11) -0.0024(10) -0.0084(9) -0.0082(9) C10 0.0441(12) 0.0375(11) 0.0335(11) 0.0008(10) -0.0086(9) -0.0091(9) C11 0.0475(12) 0.0372(12) 0.0327(11) -0.0016(10) -0.0067(9) -0.0053(10) C12 0.0472(12) 0.0370(12) 0.0410(12) -0.0019(10) -0.0073(9) -0.0043(10) C13 0.0501(13) 0.0452(13) 0.0518(14) 0.0072(12) -0.0159(11) -0.0033(11) C14 0.0631(16) 0.0335(12) 0.0604(15) 0.0122(12) -0.0105(12) -0.0100(11) C15 0.0604(15) 0.0404(13) 0.0592(16) 0.0051(12) -0.0078(12) -0.0168(11) C16 0.0532(14) 0.0386(12) 0.0428(12) -0.0002(11) -0.0069(10) -0.0102(10) C17 0.0552(14) 0.0497(14) 0.0573(15) 0.0020(13) -0.0156(12) -0.0108(12) C18 0.0521(14) 0.0491(14) 0.0681(17) 0.0022(13) -0.0176(12) -0.0131(12) C19 0.0514(13) 0.0324(11) 0.0334(11) 0.0020(10) -0.0068(9) -0.0076(9) C20 0.0496(13) 0.0404(12) 0.0410(12) 0.0006(11) -0.0070(10) -0.0071(10) C21 0.0527(14) 0.0590(16) 0.0416(13) -0.0033(12) -0.0010(11) -0.0134(12) C22 0.0644(16) 0.0602(16) 0.0359(12) -0.0100(12) -0.0003(11) -0.0129(13) C23 0.0675(17) 0.0579(15) 0.0373(12) -0.0072(12) -0.0102(11) -0.0177(13) C24 0.0534(14) 0.0459(13) 0.0379(12) -0.0002(11) -0.0085(10) -0.0113(11) C25 0.0497(14) 0.0625(16) 0.0529(14) -0.0010(13) -0.0111(11) -0.0135(12) C26 0.0525(14) 0.0744(18) 0.0415(13) -0.0038(13) -0.0091(11) -0.0209(13) _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 F1 C14 1.361(3) . ? F2 C22 1.358(3) . ? N1 C1 1.366(3) . ? N1 C4 1.367(3) . ? N1 H1 0.8800 . ? N2 C6 1.371(3) . ? N2 C9 1.372(3) . ? N2 H2 0.8800 . ? C1 C10 1.397(3) 2_656 ? C1 C2 1.430(3) . ? C2 C3 1.349(3) . ? C2 H2A 0.9500 . ? C3 C4 1.442(3) . ? C3 H3 0.9500 . ? C4 C5 1.400(3) . ? C5 C6 1.400(3) . ? C5 C11 1.505(3) . ? C6 C7 1.432(3) . ? C7 C8 1.343(3) . ? C7 H7 0.9500 . ? C8 C9 1.441(3) . ? C8 H8 0.9500 . ? C9 C10 1.401(3) . ? C10 C1 1.397(3) 2_656 ? C10 C19 1.505(3) . ? C11 C12 1.395(3) . ? C11 C16 1.405(3) . ? C12 C13 1.396(3) . ? C12 C17 1.505(4) . ? C13 C14 1.367(4) . ? C13 H13 0.9500 . ? C14 C15 1.362(4) . ? C15 C16 1.406(3) . ? C15 H15 0.9500 . ? C16 C18 1.506(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.396(3) . ? C19 C20 1.396(3) . ? C20 C21 1.405(3) . ? C20 C25 1.501(4) . ? C21 C22 1.362(4) . ? C21 H21 0.9500 . ? C22 C23 1.367(4) . ? C23 C24 1.399(3) . ? C23 H23 0.9500 . ? C24 C26 1.507(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 C4 107.81(18) . . ? C1 N1 H1 126.1 . . ? C4 N1 H1 126.1 . . ? C6 N2 C9 107.39(18) . . ? C6 N2 H2 126.3 . . ? C9 N2 H2 126.3 . . ? N1 C1 C10 126.5(2) . 2_656 ? N1 C1 C2 108.86(19) . . ? C10 C1 C2 124.6(2) 2_656 . ? C3 C2 C1 107.6(2) . . ? C3 C2 H2A 126.2 . . ? C1 C2 H2A 126.2 . . ? C2 C3 C4 107.2(2) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 126.4(2) . . ? N1 C4 C3 108.49(19) . . ? C5 C4 C3 125.1(2) . . ? C6 C5 C4 125.0(2) . . ? C6 C5 C11 117.29(19) . . ? C4 C5 C11 117.75(19) . . ? N2 C6 C5 126.0(2) . . ? N2 C6 C7 108.75(19) . . ? C5 C6 C7 125.3(2) . . ? C8 C7 C6 108.0(2) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? C7 C8 C9 107.2(2) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N2 C9 C10 126.0(2) . . ? N2 C9 C8 108.72(19) . . ? C10 C9 C8 125.3(2) . . ? C1 C10 C9 125.3(2) 2_656 . ? C1 C10 C19 117.27(19) 2_656 . ? C9 C10 C19 117.45(19) . . ? C12 C11 C16 121.4(2) . . ? C12 C11 C5 120.4(2) . . ? C16 C11 C5 118.2(2) . . ? C11 C12 C13 118.8(2) . . ? C11 C12 C17 121.3(2) . . ? C13 C12 C17 119.9(2) . . ? C14 C13 C12 118.9(2) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? F1 C14 C15 118.1(2) . . ? F1 C14 C13 118.2(2) . . ? C15 C14 C13 123.7(2) . . ? C14 C15 C16 118.9(2) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C11 C16 C15 118.2(2) . . ? C11 C16 C18 122.0(2) . . ? C15 C16 C18 119.8(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 121.2(2) . . ? C24 C19 C10 119.1(2) . . ? C20 C19 C10 119.7(2) . . ? C19 C20 C21 118.5(2) . . ? C19 C20 C25 121.4(2) . . ? C21 C20 C25 120.1(2) . . ? C22 C21 C20 119.1(2) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? F2 C22 C21 118.3(2) . . ? F2 C22 C23 118.4(3) . . ? C21 C22 C23 123.3(3) . . ? C22 C23 C24 118.8(3) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C19 C24 C23 119.0(2) . . ? C19 C24 C26 121.3(2) . . ? C23 C24 C26 119.6(2) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 C1 C10 179.8(2) . . . 2_656 ? C4 N1 C1 C2 -0.1(2) . . . . ? N1 C1 C2 C3 0.2(3) . . . . ? C10 C1 C2 C3 -179.7(2) 2_656 . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? C1 N1 C4 C5 179.5(2) . . . . ? C1 N1 C4 C3 -0.1(2) . . . . ? C2 C3 C4 N1 0.2(3) . . . . ? C2 C3 C4 C5 -179.4(2) . . . . ? N1 C4 C5 C6 -2.1(4) . . . . ? C3 C4 C5 C6 177.4(2) . . . . ? N1 C4 C5 C11 176.9(2) . . . . ? C3 C4 C5 C11 -3.6(3) . . . . ? C9 N2 C6 C5 178.8(2) . . . . ? C9 N2 C6 C7 -0.3(2) . . . . ? C4 C5 C6 N2 1.3(4) . . . . ? C11 C5 C6 N2 -177.7(2) . . . . ? C4 C5 C6 C7 -179.7(2) . . . . ? C11 C5 C6 C7 1.2(3) . . . . ? N2 C6 C7 C8 0.1(3) . . . . ? C5 C6 C7 C8 -179.0(2) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C6 N2 C9 C10 -178.2(2) . . . . ? C6 N2 C9 C8 0.4(2) . . . . ? C7 C8 C9 N2 -0.3(3) . . . . ? C7 C8 C9 C10 178.3(2) . . . . ? N2 C9 C10 C1 -1.3(4) . . . 2_656 ? C8 C9 C10 C1 -179.7(2) . . . 2_656 ? N2 C9 C10 C19 179.3(2) . . . . ? C8 C9 C10 C19 0.9(3) . . . . ? C6 C5 C11 C12 -83.2(3) . . . . ? C4 C5 C11 C12 97.7(3) . . . . ? C6 C5 C11 C16 96.5(3) . . . . ? C4 C5 C11 C16 -82.6(3) . . . . ? C16 C11 C12 C13 -0.4(3) . . . . ? C5 C11 C12 C13 179.3(2) . . . . ? C16 C11 C12 C17 -179.8(2) . . . . ? C5 C11 C12 C17 -0.1(3) . . . . ? C11 C12 C13 C14 0.4(4) . . . . ? C17 C12 C13 C14 179.8(2) . . . . ? C12 C13 C14 F1 179.5(2) . . . . ? C12 C13 C14 C15 -0.5(4) . . . . ? F1 C14 C15 C16 -179.5(2) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C12 C11 C16 C15 0.4(3) . . . . ? C5 C11 C16 C15 -179.3(2) . . . . ? C12 C11 C16 C18 179.6(2) . . . . ? C5 C11 C16 C18 -0.2(3) . . . . ? C14 C15 C16 C11 -0.5(4) . . . . ? C14 C15 C16 C18 -179.7(2) . . . . ? C1 C10 C19 C24 88.8(3) 2_656 . . . ? C9 C10 C19 C24 -91.7(3) . . . . ? C1 C10 C19 C20 -90.7(3) 2_656 . . . ? C9 C10 C19 C20 88.8(3) . . . . ? C24 C19 C20 C21 -0.6(3) . . . . ? C10 C19 C20 C21 178.9(2) . . . . ? C24 C19 C20 C25 -179.6(2) . . . . ? C10 C19 C20 C25 -0.1(3) . . . . ? C19 C20 C21 C22 0.2(4) . . . . ? C25 C20 C21 C22 179.2(2) . . . . ? C20 C21 C22 F2 179.6(2) . . . . ? C20 C21 C22 C23 -0.1(4) . . . . ? F2 C22 C23 C24 -179.3(2) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C20 C19 C24 C23 1.0(4) . . . . ? C10 C19 C24 C23 -178.5(2) . . . . ? C20 C19 C24 C26 -179.4(2) . . . . ? C10 C19 C24 C26 1.1(3) . . . . ? C22 C23 C24 C19 -0.9(4) . . . . ? C22 C23 C24 C26 179.5(2) . . . . ? _refine_diff_density_max 0.227 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.040 _shelx_res_file ; twin5_sq.res created by SHELXL-2014/7 TITL twin5.res in P-1 CELL 1.54178 9.2143 12.7406 12.62 85.167 73.242 71.786 ZERR 1 0.0002 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H F N UNIT 52 42 4 4 L.S. 10 0 55 PLAN -1 SIZE 0.02 0.06 0.08 TEMP -173.15 BOND $H CONF ABIN fmap 2 acta OMIT 0 6 3 OMIT 0 -3 6 REM REM REM WGHT 0.098400 0.025900 BASF 0.25772 0.25204 0.22548 FVAR 0.96302 F1 3 0.280187 0.707122 0.261839 11.00000 0.08300 0.04271 = 0.10973 0.03103 -0.02697 -0.01540 F2 3 0.006780 0.235637 1.206329 11.00000 0.07667 0.10452 = 0.04042 -0.02532 0.00658 -0.02501 N1 4 0.542257 0.074589 0.348279 11.00000 0.04756 0.03358 = 0.03491 -0.00036 -0.00902 -0.00608 PART 2 AFIX 43 H1 2 0.526405 0.042970 0.413591 10.50000 -1.20000 AFIX 0 PART 0 N2 4 0.376855 0.151887 0.573372 11.00000 0.04817 0.03508 = 0.03159 0.00253 -0.00869 -0.00734 PART 1 AFIX 43 H2 2 0.428128 0.086796 0.541502 10.50000 -1.20000 AFIX 0 PART 0 C1 1 0.621043 0.021716 0.248859 11.00000 0.04364 0.04036 = 0.03210 -0.00023 -0.00826 -0.00788 C2 1 0.620827 0.102182 0.162726 11.00000 0.05147 0.04155 = 0.03211 0.00137 -0.00693 -0.00966 AFIX 43 H2A 2 0.667263 0.087647 0.085734 11.00000 -1.20000 AFIX 0 C3 1 0.542776 0.202434 0.210571 11.00000 0.04948 0.03498 = 0.03748 0.00492 -0.01018 -0.00837 AFIX 43 H3 2 0.524388 0.271449 0.173633 11.00000 -1.20000 AFIX 0 C4 1 0.492441 0.185365 0.328212 11.00000 0.04417 0.03868 = 0.03854 0.00070 -0.01143 -0.00889 C5 1 0.406042 0.269180 0.407338 11.00000 0.04500 0.03218 = 0.03777 0.00144 -0.00948 -0.00691 C6 1 0.351901 0.252057 0.521131 11.00000 0.04731 0.03069 = 0.04166 -0.00087 -0.01103 -0.00483 C7 1 0.262950 0.337306 0.602428 11.00000 0.04678 0.03339 = 0.04295 -0.00271 -0.00922 -0.00489 AFIX 43 H7 2 0.229545 0.414332 0.588395 11.00000 -1.20000 AFIX 0 C8 1 0.235061 0.289174 0.702037 11.00000 0.04572 0.03822 = 0.03702 -0.00414 -0.00801 -0.00472 AFIX 43 H8 2 0.178415 0.325683 0.771093 11.00000 -1.20000 AFIX 0 C9 1 0.307160 0.171788 0.684526 11.00000 0.04341 0.03989 = 0.03533 -0.00238 -0.00841 -0.00816 C10 1 0.308522 0.092000 0.768045 11.00000 0.04406 0.03746 = 0.03354 0.00085 -0.00862 -0.00909 C11 1 0.370415 0.386820 0.367702 11.00000 0.04752 0.03715 = 0.03275 -0.00161 -0.00665 -0.00528 C12 1 0.223517 0.441549 0.348655 11.00000 0.04715 0.03698 = 0.04098 -0.00185 -0.00729 -0.00428 C13 1 0.194042 0.550984 0.313041 11.00000 0.05010 0.04524 = 0.05181 0.00717 -0.01589 -0.00329 AFIX 43 H13 2 0.094737 0.590321 0.299928 11.00000 -1.20000 AFIX 0 C14 1 0.310312 0.600654 0.297329 11.00000 0.06311 0.03352 = 0.06044 0.01217 -0.01047 -0.00997 C15 1 0.454807 0.549574 0.315330 11.00000 0.06041 0.04045 = 0.05921 0.00512 -0.00779 -0.01676 AFIX 43 H15 2 0.531510 0.587833 0.303846 11.00000 -1.20000 AFIX 0 C16 1 0.488526 0.439291 0.351188 11.00000 0.05319 0.03862 = 0.04284 -0.00017 -0.00687 -0.01016 C17 1 0.097112 0.385271 0.366842 11.00000 0.05523 0.04968 = 0.05729 0.00197 -0.01555 -0.01076 AFIX 137 H17A 2 0.146861 0.307736 0.343571 11.00000 -1.50000 H17B 2 0.023176 0.422328 0.323282 11.00000 -1.50000 H17C 2 0.038962 0.389092 0.445521 11.00000 -1.50000 AFIX 0 C18 1 0.647221 0.381435 0.372212 11.00000 0.05213 0.04906 = 0.06808 0.00220 -0.01758 -0.01307 AFIX 137 H18A 2 0.632545 0.368742 0.451766 11.00000 -1.50000 H18B 2 0.717885 0.427502 0.345761 11.00000 -1.50000 H18C 2 0.694482 0.310420 0.332789 11.00000 -1.50000 AFIX 0 C19 1 0.226192 0.131805 0.885403 11.00000 0.05143 0.03238 = 0.03336 0.00198 -0.00684 -0.00759 C20 1 0.064664 0.142869 0.929664 11.00000 0.04962 0.04040 = 0.04098 0.00062 -0.00697 -0.00708 C21 1 -0.008492 0.178264 1.040051 11.00000 0.05272 0.05898 = 0.04158 -0.00325 -0.00104 -0.01342 AFIX 43 H21 2 -0.118136 0.186335 1.072487 11.00000 -1.20000 AFIX 0 C22 1 0.079803 0.200867 1.099982 11.00000 0.06444 0.06019 = 0.03589 -0.01003 -0.00032 -0.01293 C23 1 0.237917 0.190773 1.058290 11.00000 0.06747 0.05789 = 0.03731 -0.00718 -0.01024 -0.01774 AFIX 43 H23 2 0.295292 0.206922 1.103147 11.00000 -1.20000 AFIX 0 C24 1 0.313762 0.156243 0.948400 11.00000 0.05342 0.04594 = 0.03793 -0.00021 -0.00845 -0.01134 C25 1 -0.029834 0.116076 0.862473 11.00000 0.04975 0.06250 = 0.05288 -0.00097 -0.01106 -0.01354 AFIX 137 H25A 2 -0.026851 0.163128 0.796804 11.00000 -1.50000 H25B 2 -0.140262 0.129307 0.907259 11.00000 -1.50000 H25C 2 0.015929 0.038304 0.839498 11.00000 -1.50000 AFIX 0 C26 1 0.487746 0.145512 0.900567 11.00000 0.05245 0.07442 = 0.04153 -0.00385 -0.00908 -0.02093 AFIX 137 H26A 2 0.550423 0.067445 0.898725 11.00000 -1.50000 H26B 2 0.520245 0.187116 0.946646 11.00000 -1.50000 H26C 2 0.505689 0.174997 0.825229 11.00000 -1.50000 AFIX 0 HKLF 5 REM twin5.res in P-1 REM R1 = 0.0528 for 3450 Fo > 4sig(Fo) and 0.0675 for all 4572 data REM 278 parameters refined using 0 restraints END WGHT 0.0984 0.0259 REM Highest difference peak 0.227, deepest hole -0.207, 1-sigma level 0.040 Q1 1 0.5083 0.1381 0.5613 11.00000 0.05 0.23 ; _shelx_res_checksum 57376 _shelx_hkl_file ; 1 0 0 281.174 5.23249 4 2 0 0 24.4516 1.03372 4 3 0 0 267.053 5.00040 4 4 0 0 225.466 4.31965 4 5 0 0 91.7782 3.03694 -2 5 4 0 91.7782 3.03694 4 5 0 0 6.43765 1.49293 -3 5 0 4 6.43765 1.49293 4 6 0 0 21.7855 2.06222 -3 6 0 5 21.7855 2.06222 4 6 0 0 9.03212 3.37371 -2 6 5 0 9.03212 3.37371 4 7 0 0 25.1174 1.30758 4 9 0 0 0.15314 0.29203 4 10 0 0 1.37312 0.27728 4 -9 1 0 2.36941 0.37690 4 -7 1 0 12.5709 1.05835 4 -6 1 0 33.5779 4.42618 -2 -6 -5 1 33.5779 4.42618 4 -6 1 0 30.3074 2.27040 -3 6 0 6 30.3074 2.27040 4 -5 1 0 35.2806 1.72045 -2 -5 -4 1 35.2806 1.72045 4 -5 1 0 34.4937 3.47987 -3 5 0 5 34.4937 3.47987 4 -5 1 0 4.36632 0.64444 4 -4 1 0 11.4175 1.32122 4 -3 1 0 26.9482 0.80375 4 -2 1 0 211.532 3.97724 4 -1 1 0 863.351 14.8049 4 0 0 1 207.266 7.45839 -3 0 0 1 207.266 7.45839 -2 0 1 0 207.266 7.45839 -1 0 1 0 207.266 7.45839 4 1 1 0 292.702 6.49275 4 2 1 0 267.317 4.91308 4 3 1 0 74.2188 1.63394 4 4 1 0 24.8370 1.03396 4 5 1 0 52.6418 3.54188 -3 5 0 3 52.6418 3.54188 4 5 1 0 14.4093 2.83583 -2 5 4 1 14.4093 2.83583 4 6 1 0 15.8182 3.38047 -2 6 5 1 15.8182 3.38047 4 7 1 0 24.0068 1.04002 4 9 1 0 0.25353 0.28702 4 10 1 0 0.06100 0.30217 4 -9 2 0 7.79290 0.60473 4 -7 2 0 1.84168 0.33229 4 -7 2 0 1.44669 1.30803 -2 -7 -6 2 1.44669 1.30803 4 -6 2 0 26.5085 2.29758 -3 6 0 7 26.5085 2.29758 4 -6 2 0 15.9522 4.02596 -2 -6 -5 2 15.9522 4.02596 4 -5 2 0 2.71676 0.54561 4 -5 2 0 28.7921 3.48596 -2 -5 -4 2 28.7921 3.48596 4 -4 2 0 10.1170 0.98727 4 -3 2 0 550.943 10.4702 4 -2 2 0 84.4854 1.93529 4 -1 2 0 175.102 3.24836 4 0 0 2 4.84980 0.98368 -3 0 0 2 4.84980 0.98368 -2 0 2 0 4.84980 0.98368 -1 0 2 0 4.84980 0.98368 4 1 2 0 248.676 5.61848 4 2 2 0 99.3057 2.93241 4 3 2 0 4.17834 0.58508 4 4 2 0 428.599 7.60398 4 6 2 0 53.9699 4.76859 -2 6 5 2 53.9699 4.76859 4 6 2 0 12.7666 4.49932 -3 6 0 3 12.7666 4.49932 4 7 2 0 36.8822 1.24210 4 9 2 0 10.3857 0.51913 4 10 2 0 0.39146 0.24996 4 -9 3 0 1.69788 0.38259 4 -8 3 0 1.33684 0.47995 4 -7 3 0 0.77706 0.49728 4 -7 3 0 4.57035 2.96898 -2 -7 -6 3 4.57035 2.96898 4 -6 3 0 57.6490 3.27044 -3 6 0 8 57.6490 3.27044 4 -5 3 0 4.78141 0.77731 4 -4 3 0 35.4535 1.24143 4 -3 3 0 24.3046 1.21938 4 -2 3 0 75.7402 1.48723 4 -1 3 0 128.650 3.98662 -2 -1 -1 3 128.650 3.98662 4 0 0 3 5700.27 123.940 -3 0 0 3 5700.27 123.940 -2 0 3 0 5700.27 123.940 -1 0 3 0 5700.27 123.940 4 1 3 0 108.870 2.08139 4 2 3 0 813.043 11.6621 4 3 3 0 167.046 2.79646 4 4 3 0 242.213 4.55947 4 6 3 0 3.00670 4.42365 -3 6 0 2 3.00670 4.42365 4 9 3 0 0.36139 0.30300 4 10 3 0 1.24872 0.27575 4 -8 4 0 2.58247 0.78178 4 -7 4 0 7.19875 1.03895 4 -6 4 0 3.86071 0.94638 4 -6 4 0 17.7773 2.70581 -3 6 0 9 17.7773 2.70581 4 -5 4 0 9.18257 0.98171 4 -4 4 0 4.72580 0.62365 4 -3 4 0 69.5453 1.80870 4 -2 4 0 51.3216 1.20097 4 -1 4 0 26.3638 1.70739 -2 -1 -1 4 26.3638 1.70739 4 0 0 4 728.325 11.4928 -3 0 0 4 728.325 11.4928 -2 0 4 0 728.325 11.4928 -1 0 4 0 728.325 11.4928 4 1 4 0 223.783 3.80792 4 2 4 0 11.7493 0.50531 4 3 4 0 37.4414 0.93794 4 4 4 0 69.7132 1.72577 4 6 4 0 -4.1282 4.43345 -3 6 0 1 -4.1282 4.43345 4 9 4 0 2.71699 0.31071 4 10 4 0 2.23544 0.32199 4 -8 5 0 1.75420 0.66909 4 -7 5 0 7.02528 0.95874 4 -6 5 0 21.1959 1.48074 4 -6 5 0 34.1993 3.30391 -3 6 0 10 34.1993 3.30391 4 -4 5 0 5.04139 0.77739 4 -3 5 0 1.70161 0.36463 4 -2 5 0 103.417 2.05750 4 -1 5 0 336.223 7.63157 -2 -1 -1 5 336.223 7.63157 4 0 0 5 81.7050 1.95512 -3 0 0 5 81.7050 1.95512 -2 0 5 0 81.7050 1.95512 -1 0 5 0 81.7050 1.95512 4 2 5 0 49.3963 1.02347 4 3 5 0 0.91094 0.32778 4 4 5 0 17.0955 0.84153 4 6 5 0 11.1027 4.95187 -3 6 0 0 11.1027 4.95187 4 7 5 0 4.25409 0.54929 4 9 5 0 -0.1973 0.27917 4 10 5 0 1.71874 0.28129 4 -7 6 0 0.91872 0.73557 4 -6 6 0 8.80236 1.19879 -3 6 0 11 8.80236 1.19879 4 -6 6 0 3.05555 0.78913 4 -5 6 0 8.57444 2.79070 -3 5 0 10 8.57444 2.79070 4 -4 6 0 23.2519 1.39698 4 -3 6 0 0.69450 0.40810 4 -2 6 0 9.30410 0.50461 4 -1 6 0 66.9818 2.78258 -2 -1 -1 6 66.9818 2.78258 4 0 0 6 16.4049 1.00118 -3 0 0 6 16.4049 1.00118 -2 0 6 0 16.4049 1.00118 -1 0 6 0 16.4049 1.00118 4 -1 0 5 172.626 9.60633 -3 1 6 0 172.626 9.60633 -1 1 -5 1 172.626 9.60633 4 1 6 0 22.8420 0.89396 4 2 6 0 134.131 2.38083 4 3 6 0 5.52344 0.47516 4 4 6 0 13.2635 0.61697 4 5 6 0 22.9711 4.47924 -3 -5 0 2 22.9711 4.47924 4 5 6 0 16.4275 0.81602 4 6 6 0 -1.2869 4.51137 -3 -6 0 1 -1.2869 4.51137 4 7 6 0 0.45269 0.44991 4 9 6 0 2.48284 0.33952 4 10 6 0 1.94358 0.30252 4 -7 7 0 3.07493 0.70138 4 -6 7 0 3.13823 0.74183 4 -6 7 0 3.99847 1.15431 -3 6 0 12 3.99847 1.15431 4 -5 7 0 27.8791 3.14815 -3 5 0 11 27.8791 3.14815 4 -4 7 0 14.5440 1.25726 4 -3 7 0 9.08212 0.69498 4 -2 7 0 34.9645 0.95045 4 -1 7 0 13.8603 1.12275 -2 -1 -1 7 13.8603 1.12275 4 0 0 7 524.984 8.69603 -3 0 0 7 524.984 8.69603 -2 0 7 0 524.984 8.69603 -1 0 7 0 524.984 8.69603 4 1 7 0 26.7557 0.84705 4 -1 0 6 91.6931 5.07604 -3 1 7 0 91.6931 5.07604 -1 1 -6 1 91.6931 5.07604 4 2 7 0 69.5369 1.37955 4 3 7 0 38.1107 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-0.63 0.00 3 -6 13 -0.17 0.00 8 2 13 0.03 0.00 6 3 13 0.07 0.00 8 3 13 0.16 0.00 -1 4 13 -0.29 0.00 4 4 13 0.01 0.00 5 4 13 -0.25 0.00 6 4 13 0.39 0.00 8 4 13 0.18 0.00 5 5 13 -0.54 0.00 6 5 13 -0.63 0.00 8 5 13 -0.05 0.00 6 6 13 0.41 0.00 2 8 13 -0.03 0.00 -1 -1 14 -0.02 0.00 6 -1 14 0.63 0.00 -1 0 14 -0.19 0.00 5 2 14 -0.36 0.00 6 2 14 -0.21 0.00 4 3 14 -0.05 0.00 5 3 14 -0.43 0.00 6 3 14 -0.20 0.00 7 3 14 0.05 0.00 4 4 14 -0.11 0.00 5 4 14 0.16 0.00 6 4 14 0.10 0.00 1 5 14 0.30 0.00 4 5 14 -0.35 0.00 5 5 14 -0.28 0.00 6 5 14 -0.04 0.00 2 6 14 0.05 0.00 5 6 14 0.32 0.00 6 6 14 0.47 0.00 4 7 14 -0.25 0.00 2 0 15 -0.29 0.00 3 0 15 -0.42 0.00 4 0 15 -0.26 0.00 2 1 15 0.39 0.00 4 1 15 -0.25 0.00 2 2 15 -0.19 0.00 4 2 15 -0.41 0.00 3 3 15 0.05 0.00 4 3 15 0.07 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 171020) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.040 0.500 0.000 219 49 ' ' 2 0.000 0.000 0.500 236 50 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL twin5 P -1 R = 0.16 CELL 9.2143 12.7406 12.6200 85.17 73.24 71.79 SPGR P-1 # Solvent Accessible Volume = 451 # Electrons Found in S.A.V. = 98 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.069 0.507 0.029 ! 2.32 eA-3 C102 0.171 1.002 0.373 ! 2.25 eA-3 C103 0.687 0.450 0.018 ! 2.15 eA-3 C104 0.800 0.502 0.048 ! 1.98 eA-3 C105 0.414 0.491 0.003 ! 1.96 eA-3 C106 0.947 0.090 0.488 ! 1.82 eA-3 C107 0.210 0.925 0.442 ! 1.82 eA-3 C108 0.067 0.011 0.481 ! 1.55 eA-3 ) ; _shelx_fab_checksum 12843