# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Stuart James' 'Conor Dawson' 'Peter N Horton' 'Michael B. Hursthouse' _publ_contact_author_name 'Stuart James' _publ_contact_author_email S.JAMES@QUEENS-BELFAST.AC.UK _publ_section_title ; Channeled crystals formed by columnar stacking of a 4+4 phenylene-piperazine macrocycle ; # Attachment '2008src1295.cif' data_2008src1295 _database_code_depnum_ccdc_archive 'CCDC 746235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 N8' _chemical_formula_weight 753.07 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 31.7084(16) _cell_length_b 5.6724(2) _cell_length_c 22.6344(11) _cell_angle_alpha 90.00 _cell_angle_beta 134.288(5) _cell_angle_gamma 90.00 _cell_volume 2914.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6502 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9591 _exptl_absorpt_correction_T_max 0.9985 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; SADABS was used to perform the Absorption correction Estimated minimum and maximum transmission: 0.6137 0.7456 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30406 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3676 _reflns_number_gt 2894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1164P)^2^+1.1607P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3676 _refine_ls_number_parameters 253 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1998 _refine_ls_wR_factor_gt 0.1895 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.26543(12) 0.3664(5) 0.10601(17) 0.0299(6) Uani 1 1 d . . . N4 N 0.34244(12) 0.5001(5) 0.58057(16) 0.0308(7) Uani 1 1 d . . . N3 N 0.55134(12) 0.2966(6) 0.26716(17) 0.0318(7) Uani 1 1 d . . . N2 N 0.22424(13) 0.5725(6) 0.17420(18) 0.0336(7) Uani 1 1 d . . . C16 C 0.51463(15) 0.0967(7) 0.2143(2) 0.0367(9) Uani 1 1 d . . . H16A H 0.5337 -0.0512 0.2461 0.044 Uiso 1 1 calc R . . H16B H 0.5112 0.0914 0.1674 0.044 Uiso 1 1 calc R . . C9 C 0.27748(15) 0.1629(7) 0.0804(2) 0.0338(8) Uani 1 1 d . . . H9A H 0.2503 0.1667 0.0196 0.041 Uiso 1 1 calc R . . H9B H 0.2690 0.0178 0.0948 0.041 Uiso 1 1 calc R . . C24 C 0.30578(16) 0.7068(7) 0.5304(2) 0.0344(8) Uani 1 1 d . . . H24A H 0.3284 0.8515 0.5616 0.041 Uiso 1 1 calc R . . H24B H 0.2705 0.7056 0.5216 0.041 Uiso 1 1 calc R . . C17 C 0.21097(17) 0.7734(7) 0.1992(2) 0.0353(8) Uani 1 1 d . . . H17A H 0.1677 0.7860 0.1617 0.042 Uiso 1 1 calc R . . H17B H 0.2249 0.9194 0.1935 0.042 Uiso 1 1 calc R . . C5 C 0.56302(14) 0.2978(7) 0.3421(2) 0.0319(8) Uani 1 1 d . . . H5A H 0.5828 0.1490 0.3728 0.038 Uiso 1 1 calc R . . H5B H 0.5253 0.3070 0.3269 0.038 Uiso 1 1 calc R . . C13 C 0.45344(15) 0.1122(6) 0.1813(2) 0.0324(8) Uani 1 1 d . . . C20 C 0.25297(15) 0.5356(7) 0.3909(2) 0.0325(8) Uani 1 1 d . . . H20 H 0.2460 0.3970 0.4065 0.039 Uiso 1 1 calc R . . C6 C 0.39817(14) 0.5061(7) 0.6029(2) 0.0300(7) Uani 1 1 d . . . H6A H 0.4191 0.6551 0.6322 0.036 Uiso 1 1 calc R . . H6B H 0.3903 0.5014 0.5521 0.036 Uiso 1 1 calc R . . C2 C 0.28677(15) 0.5692(7) 0.2197(2) 0.0334(8) Uani 1 1 d . . . H2A H 0.3108 0.5607 0.2797 0.040 Uiso 1 1 calc R . . H2B H 0.2970 0.7170 0.2089 0.040 Uiso 1 1 calc R . . C15 C 0.36339(14) 0.3308(7) 0.1069(2) 0.0298(7) Uani 1 1 d . . . H15 H 0.3406 0.4681 0.0771 0.036 Uiso 1 1 calc R . . C14 C 0.41887(14) 0.3129(6) 0.1377(2) 0.0308(7) Uani 1 1 d . . . H14 H 0.4341 0.4384 0.1294 0.037 Uiso 1 1 calc R . . C7 C 0.35438(15) 0.4998(7) 0.6558(2) 0.0317(8) Uani 1 1 d . . . H7A H 0.3167 0.4917 0.6410 0.038 Uiso 1 1 calc R . . H7B H 0.3746 0.6478 0.6868 0.038 Uiso 1 1 calc R . . C19 C 0.22987(16) 0.5517(6) 0.3122(2) 0.0326(8) Uani 1 1 d . . . H19 H 0.2076 0.4246 0.2747 0.039 Uiso 1 1 calc R . . C4 C 0.20320(15) 0.3694(7) 0.0607(2) 0.0310(8) Uani 1 1 d . . . H4A H 0.1929 0.2220 0.0716 0.037 Uiso 1 1 calc R . . H4B H 0.1792 0.3776 0.0007 0.037 Uiso 1 1 calc R . . C8 C 0.60690(15) 0.2882(7) 0.2897(2) 0.0342(8) Uani 1 1 d . . . H8A H 0.5992 0.2898 0.2392 0.041 Uiso 1 1 calc R . . H8B H 0.6278 0.1401 0.3199 0.041 Uiso 1 1 calc R . . C18 C 0.23911(16) 0.7546(6) 0.2872(2) 0.0326(8) Uani 1 1 d . . . C1 C 0.30100(15) 0.3609(7) 0.1946(2) 0.0317(8) Uani 1 1 d . . . H1A H 0.3433 0.3643 0.2254 0.038 Uiso 1 1 calc R . . H1B H 0.2932 0.2128 0.2087 0.038 Uiso 1 1 calc R . . C21 C 0.28620(14) 0.7161(6) 0.4481(2) 0.0287(8) Uani 1 1 d . . . C23 C 0.27434(16) 0.9323(7) 0.3446(2) 0.0355(8) Uani 1 1 d . . . H23 H 0.2829 1.0677 0.3298 0.043 Uiso 1 1 calc R . . C10 C 0.33996(15) 0.1495(7) 0.1186(2) 0.0310(8) Uani 1 1 d . . . C12 C 0.43080(16) -0.0654(7) 0.1933(2) 0.0357(8) Uani 1 1 d . . . H12 H 0.4537 -0.2027 0.2227 0.043 Uiso 1 1 calc R . . C3 C 0.18921(15) 0.5795(7) 0.0861(2) 0.0333(8) Uani 1 1 d . . . H3A H 0.1976 0.7272 0.0725 0.040 Uiso 1 1 calc R . . H3B H 0.1468 0.5782 0.0549 0.040 Uiso 1 1 calc R . . C22 C 0.29693(16) 0.9130(7) 0.4229(2) 0.0370(9) Uani 1 1 d . . . H22 H 0.3206 1.0373 0.4612 0.044 Uiso 1 1 calc R . . C11 C 0.37463(17) -0.0481(7) 0.1629(2) 0.0357(8) Uani 1 1 d . . . H11 H 0.3600 -0.1723 0.1725 0.043 Uiso 1 1 calc R . . 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 0.0306(15) 0.0313(16) 0.0309(14) -0.0050(12) 0.0226(13) -0.0071(13) N4 0.0280(14) 0.0314(16) 0.0312(14) -0.0050(13) 0.0199(12) -0.0029(13) N3 0.0245(14) 0.0321(16) 0.0324(14) -0.0023(13) 0.0174(12) 0.0015(13) N2 0.0431(17) 0.0295(16) 0.0368(15) 0.0040(13) 0.0310(14) 0.0033(13) C16 0.0312(19) 0.032(2) 0.0393(19) -0.0002(16) 0.0218(16) 0.0055(16) C9 0.0301(18) 0.033(2) 0.0343(18) -0.0049(15) 0.0210(16) -0.0097(16) C24 0.0338(19) 0.0278(18) 0.042(2) -0.0023(15) 0.0268(17) 0.0023(15) C17 0.045(2) 0.0285(19) 0.042(2) 0.0086(17) 0.0340(18) 0.0083(17) C5 0.0253(16) 0.0299(19) 0.0378(18) -0.0027(16) 0.0211(15) -0.0014(15) C13 0.0331(19) 0.0289(19) 0.0276(17) -0.0044(15) 0.0184(16) -0.0013(15) C20 0.044(2) 0.0232(18) 0.0412(19) -0.0025(15) 0.0339(17) -0.0019(16) C6 0.0281(17) 0.0299(18) 0.0313(17) -0.0002(15) 0.0205(15) -0.0006(15) C2 0.0345(19) 0.032(2) 0.0318(17) 0.0022(15) 0.0223(16) 0.0009(16) C15 0.0302(18) 0.0263(18) 0.0283(16) -0.0003(14) 0.0187(15) -0.0012(15) C14 0.0260(17) 0.0229(17) 0.0344(17) 0.0005(15) 0.0178(15) -0.0022(14) C7 0.0293(18) 0.037(2) 0.0295(16) -0.0066(16) 0.0208(15) -0.0055(16) C19 0.046(2) 0.0247(18) 0.0366(18) -0.0059(15) 0.0320(17) -0.0020(16) C4 0.0330(18) 0.0338(19) 0.0305(16) 0.0027(15) 0.0238(15) -0.0013(15) C8 0.0289(18) 0.040(2) 0.0351(18) 0.0030(17) 0.0227(16) 0.0069(17) C18 0.040(2) 0.028(2) 0.043(2) 0.0016(16) 0.0333(18) 0.0055(15) C1 0.0336(18) 0.0325(19) 0.0338(17) 0.0027(16) 0.0252(16) 0.0020(16) C21 0.0269(17) 0.0239(17) 0.0353(18) 0.0021(14) 0.0217(15) 0.0065(14) C23 0.039(2) 0.0196(16) 0.053(2) 0.0030(16) 0.0338(18) -0.0013(15) C10 0.0317(18) 0.0285(19) 0.0263(17) -0.0052(14) 0.0179(15) -0.0039(15) C12 0.0346(19) 0.0233(17) 0.0332(18) 0.0025(15) 0.0177(16) 0.0056(15) C3 0.0308(18) 0.034(2) 0.0346(18) 0.0097(16) 0.0227(16) 0.0057(16) C22 0.0313(19) 0.0264(19) 0.044(2) -0.0050(16) 0.0230(17) -0.0031(15) C11 0.046(2) 0.0230(18) 0.0375(19) -0.0036(15) 0.0287(17) -0.0034(16) _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 C4 1.456(4) . ? N1 C9 1.457(5) . ? N1 C1 1.461(4) . ? N4 C6 1.461(4) . ? N4 C7 1.464(4) . ? N4 C24 1.474(5) . ? N3 C8 1.452(4) . ? N3 C16 1.458(5) . ? N3 C5 1.462(4) . ? N2 C3 1.456(4) . ? N2 C17 1.459(5) . ? N2 C2 1.463(4) . ? C16 C13 1.519(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C9 C10 1.512(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C24 C21 1.497(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C17 C18 1.514(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C5 C6 1.524(5) 2_656 ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C13 C12 1.369(5) . ? C13 C14 1.400(5) . ? C20 C19 1.376(5) . ? C20 C21 1.389(5) . ? C20 H20 0.9500 . ? C6 C5 1.524(5) 2_656 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C2 C1 1.511(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C15 C14 1.370(5) . ? C15 C10 1.399(5) . ? C15 H15 0.9500 . ? C14 H14 0.9500 . ? C7 C8 1.534(5) 2_656 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C19 C18 1.401(5) . ? C19 H19 0.9500 . ? C4 C3 1.518(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C8 C7 1.534(6) 2_656 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C18 C23 1.387(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C21 C22 1.399(5) . ? C23 C22 1.377(5) . ? C23 H23 0.9500 . ? C10 C11 1.389(5) . ? C12 C11 1.394(5) . ? C12 H12 0.9500 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C22 H22 0.9500 . ? C11 H11 0.9500 . ? 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 C4 N1 C9 109.4(3) . . ? C4 N1 C1 109.6(2) . . ? C9 N1 C1 111.3(3) . . ? C6 N4 C7 109.3(2) . . ? C6 N4 C24 111.1(3) . . ? C7 N4 C24 108.8(3) . . ? C8 N3 C16 109.9(3) . . ? C8 N3 C5 109.2(2) . . ? C16 N3 C5 111.4(3) . . ? C3 N2 C17 111.1(3) . . ? C3 N2 C2 109.1(2) . . ? C17 N2 C2 110.7(3) . . ? N3 C16 C13 111.9(3) . . ? N3 C16 H16A 109.2 . . ? C13 C16 H16A 109.2 . . ? N3 C16 H16B 109.2 . . ? C13 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N1 C9 C10 114.5(3) . . ? N1 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? N1 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N4 C24 C21 113.9(3) . . ? N4 C24 H24A 108.8 . . ? C21 C24 H24A 108.8 . . ? N4 C24 H24B 108.8 . . ? C21 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? N2 C17 C18 113.0(3) . . ? N2 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? N2 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N3 C5 C6 111.0(3) . 2_656 ? N3 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 2_656 . ? N3 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 2_656 . ? H5A C5 H5B 108.0 . . ? C12 C13 C14 118.5(3) . . ? C12 C13 C16 121.8(3) . . ? C14 C13 C16 119.7(3) . . ? C19 C20 C21 122.0(3) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? N4 C6 C5 110.8(3) . 2_656 ? N4 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 2_656 . ? N4 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 2_656 . ? H6A C6 H6B 108.1 . . ? N2 C2 C1 111.0(3) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C14 C15 C10 120.8(3) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C15 C14 C13 120.9(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? N4 C7 C8 110.3(3) . 2_656 ? N4 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 2_656 . ? N4 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 2_656 . ? H7A C7 H7B 108.1 . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? N1 C4 C3 110.7(3) . . ? N1 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N3 C8 C7 110.6(3) . 2_656 ? N3 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 2_656 . ? N3 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 2_656 . ? H8A C8 H8B 108.1 . . ? C23 C18 C19 118.6(3) . . ? C23 C18 C17 122.0(3) . . ? C19 C18 C17 119.5(3) . . ? N1 C1 C2 110.7(3) . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C20 C21 C22 116.7(3) . . ? C20 C21 C24 121.3(3) . . ? C22 C21 C24 121.8(3) . . ? C22 C23 C18 120.1(3) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? C11 C10 C15 118.2(3) . . ? C11 C10 C9 121.0(3) . . ? C15 C10 C9 120.8(3) . . ? C13 C12 C11 121.1(3) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? N2 C3 C4 110.6(3) . . ? N2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C23 C22 C21 122.2(3) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.315 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.066 # SQUEEZE RESULTS (APPEND TO CIF) # 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 0.000 0.041 0.000 240 22 ' ' 2 0.000 -0.045 0.500 280 18 ' ' 3 0.500 -0.058 0.500 280 18 ' ' 4 0.500 -0.151 1.000 240 22 ' ' _platon_squeeze_details ; ;