# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Myoung Soo Lah' _publ_contact_author_email mslah@unist.ac.kr _publ_section_title ; An Unprecedented Twofold Interpenetrated Layered Metal-Organic Framework with a MoS2-H Topology ; loop_ _publ_author_name L.Rajput 'Seunghee Hong' 'Xinfang Liu' 'Minhak Oh' 'Dongwook Kim' 'Myoung Soo Lah' # Attachment '- mslah_rev3.cif' data_l8_37rh _database_code_depnum_ccdc_archive 'CCDC 826842' #TrackingRef '- mslah_rev3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H126 N18 O44 Zn8' _chemical_formula_weight 3335.59 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.837(5) _cell_length_b 17.837(5) _cell_length_c 81.03(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 22327(15) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34661 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 25.15 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10248 _exptl_absorpt_coefficient_mu 1.354 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7926 _exptl_absorpt_correction_T_max 0.8125 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; Even though Laue group -3m for the reflection data has large R(int) value, it is chosen as a Laue group of the data because the other possible lower symmetry Laue groups also have comparably large R(int) vlaues. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34661 _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -94 _diffrn_reflns_limit_l_max 96 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.15 _reflns_number_total 4408 _reflns_number_gt 3312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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. To reduce large anisotropic dispalcement coefficients of O6 atom compared to the adjacent atoms, ISOR command was employed for O6 during the least-squares refinement of the structural model using XL program of SHELXTL program package. Even though some residual electron densities were observed in the vicinity of the metal centers, they were not included in the structural model because of the difficulties in the explanation of the chemical sense. Some of them still appear in the difference Fourier map as residual electron densities even after the modification of the relection data for the residual electron densities as the electron densities of disordered solvent region using SQUEEZE option of the PLATON program. ; _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^)+(0.0974P)^2^+632.4644P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4408 _refine_ls_number_parameters 325 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1608 _refine_ls_R_factor_gt 0.1257 _refine_ls_wR_factor_ref 0.2772 _refine_ls_wR_factor_gt 0.2593 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.192 _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 Zn1 Zn 0.34116(7) 0.56540(8) 0.097460(15) 0.0347(4) Uani 1 1 d . . . Zn2 Zn 0.3333 0.6667 0.12809(3) 0.0497(7) Uani 1 3 d S . . O1M O 0.3333 0.6667 0.10440(12) 0.030(3) Uani 1 3 d S . . O1 O 0.3529(5) 0.5085(5) 0.11734(10) 0.052(2) Uani 1 1 d . . . O2 O 0.2883(5) 0.5492(5) 0.13619(11) 0.055(2) Uani 1 1 d . . . O3 O 0.5692(4) 0.4640(4) 0.13671(9) 0.0388(18) Uani 1 1 d . . . O4 O 0.4472(4) 0.6076(5) 0.08501(10) 0.0459(19) Uani 1 1 d . . . O5 O 0.5064(5) 0.7511(5) 0.08307(9) 0.0463(19) Uani 1 1 d . . . O6 O 0.5338(6) 0.4316(6) 0.06900(15) 0.087(3) Uani 1 1 d U . . N1 N 0.4757(5) 0.3594(6) 0.15419(11) 0.038(2) Uani 1 1 d . . . H1 H 0.4670 0.3140 0.1600 0.046 Uiso 1 1 calc R . . N2 N 0.6596(6) 0.5376(5) 0.05875(11) 0.040(2) Uani 1 1 d . . . H2 H 0.7086 0.5473 0.0543 0.049 Uiso 1 1 calc R . . C1 C 0.3243(6) 0.5066(6) 0.13165(15) 0.038(3) Uani 1 1 d . . . C2 C 0.3342(7) 0.4520(6) 0.14443(14) 0.040(3) Uani 1 1 d . . . C3 C 0.3962(6) 0.4278(6) 0.14224(13) 0.035(2) Uani 1 1 d . . . H3 H 0.4287 0.4414 0.1323 0.043 Uiso 1 1 calc R . . C4 C 0.4100(6) 0.3833(7) 0.15478(14) 0.040(3) Uani 1 1 d . . . C5 C 0.3588(8) 0.3585(8) 0.16866(16) 0.057(3) Uani 1 1 d . . . H5 H 0.3678 0.3271 0.1772 0.068 Uiso 1 1 calc R . . C6 C 0.2937(8) 0.3793(9) 0.17018(18) 0.067(4) Uani 1 1 d . . . H6 H 0.2563 0.3596 0.1795 0.080 Uiso 1 1 calc R . . C7 C 0.2830(8) 0.4280(9) 0.15842(16) 0.057(3) Uani 1 1 d . . . H7 H 0.2409 0.4452 0.1598 0.068 Uiso 1 1 calc R . . C8 C 0.5504(6) 0.4017(6) 0.14539(11) 0.030(2) Uani 1 1 d . . . C9 C 0.6083(6) 0.3636(6) 0.14679(12) 0.027(2) Uani 1 1 d . . . C10 C 0.5781(6) 0.2763(7) 0.14671(12) 0.034(2) Uani 1 1 d . . . H10 H 0.5176 0.2368 0.1466 0.041 Uiso 1 1 calc R . . C11 C 0.5046(6) 0.6814(7) 0.07999(12) 0.036(2) Uani 1 1 d . . . C12 C 0.5757(7) 0.6828(7) 0.06992(12) 0.035(2) Uani 1 1 d . . . C13 C 0.5816(6) 0.6094(7) 0.06878(13) 0.035(2) Uani 1 1 d . . . H13 H 0.5400 0.5580 0.0742 0.042 Uiso 1 1 calc R . . C14 C 0.6475(6) 0.6093(6) 0.05987(12) 0.034(2) Uani 1 1 d . . . C15 C 0.7091(7) 0.6859(7) 0.05197(13) 0.038(2) Uani 1 1 d . . . H15 H 0.7550 0.6868 0.0458 0.045 Uiso 1 1 calc R . . C16 C 0.7026(7) 0.7590(7) 0.05317(14) 0.042(3) Uani 1 1 d . . . H16 H 0.7439 0.8107 0.0478 0.051 Uiso 1 1 calc R . . C17 C 0.6364(7) 0.7582(7) 0.06220(13) 0.041(3) Uani 1 1 d . . . H17 H 0.6325 0.8092 0.0631 0.049 Uiso 1 1 calc R . . C18 C 0.6058(7) 0.4562(7) 0.06365(14) 0.043(3) Uani 1 1 d . . . C19 C 0.6393(6) 0.3946(7) 0.06246(12) 0.033(2) Uani 1 1 d . . . C20 C 0.7270(7) 0.4205(7) 0.06261(12) 0.040(3) Uani 1 1 d . . . H20 H 0.7685 0.4806 0.0628 0.048 Uiso 1 1 calc R . . O1S O 0.4629(7) 0.2346(8) 0.17627(13) 0.089(4) Uani 1 1 d . . . N1S N 0.4720(11) 0.1685(10) 0.19865(17) 0.091(4) Uani 1 1 d . . . C1S C 0.4331(10) 0.1962(10) 0.18889(19) 0.067(4) Uani 1 1 d . . . C2S C 0.3431(10) 0.1744(10) 0.19442(19) 0.078(4) Uani 1 1 d . . . H2S1 H 0.3478 0.2145 0.2032 0.117 Uiso 1 1 calc R . . H2S2 H 0.3121 0.1150 0.1987 0.117 Uiso 1 1 calc R . . H2S3 H 0.3114 0.1796 0.1850 0.117 Uiso 1 1 calc R . . C3S C 0.4354(13) 0.1202(13) 0.21410(18) 0.103(6) Uani 1 1 d . . . H3S1 H 0.3921 0.1336 0.2184 0.155 Uiso 1 1 calc R . . H3S2 H 0.4818 0.1369 0.2222 0.155 Uiso 1 1 calc R . . H3S3 H 0.4080 0.0579 0.2119 0.155 Uiso 1 1 calc R . . C4S C 0.5572(14) 0.1836(17) 0.1932(3) 0.145(10) Uani 1 1 d . . . H4S1 H 0.5675 0.2042 0.1818 0.217 Uiso 1 1 calc R . . H4S2 H 0.5585 0.1294 0.1939 0.217 Uiso 1 1 calc R . . H4S3 H 0.6024 0.2273 0.2003 0.217 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 Zn1 0.0216(6) 0.0387(7) 0.0387(7) 0.0049(5) -0.0007(5) 0.0112(5) Zn2 0.0483(9) 0.0483(9) 0.0526(15) 0.000 0.000 0.0241(5) O1M 0.040(4) 0.040(4) 0.009(5) 0.000 0.000 0.020(2) O1 0.060(5) 0.060(5) 0.055(5) 0.023(4) 0.009(4) 0.045(5) O2 0.041(5) 0.042(5) 0.089(6) 0.026(4) 0.020(4) 0.026(4) O3 0.035(4) 0.034(4) 0.055(4) 0.016(3) 0.020(3) 0.022(3) O4 0.028(4) 0.048(5) 0.063(5) -0.003(4) 0.010(4) 0.019(4) O5 0.048(5) 0.049(5) 0.058(5) 0.013(4) 0.020(4) 0.036(4) O6 0.056(6) 0.051(5) 0.164(9) 0.044(6) 0.045(6) 0.035(5) N1 0.035(5) 0.036(5) 0.051(5) 0.016(4) 0.011(4) 0.023(4) N2 0.038(5) 0.025(4) 0.063(6) 0.004(4) 0.016(4) 0.019(4) C1 0.022(5) 0.023(5) 0.066(8) 0.021(5) 0.007(5) 0.009(4) C2 0.030(6) 0.024(5) 0.063(7) 0.008(5) 0.007(5) 0.011(5) C3 0.026(5) 0.037(6) 0.045(6) 0.003(5) 0.002(4) 0.018(5) C4 0.030(6) 0.034(6) 0.060(7) 0.015(5) 0.006(5) 0.019(5) C5 0.050(7) 0.068(9) 0.056(8) 0.031(7) 0.021(6) 0.032(7) C6 0.053(8) 0.084(10) 0.082(10) 0.044(8) 0.038(7) 0.048(8) C7 0.039(7) 0.074(9) 0.069(9) 0.019(7) 0.015(6) 0.037(7) C8 0.031(5) 0.030(5) 0.030(5) 0.009(4) 0.004(4) 0.017(4) C9 0.027(5) 0.025(5) 0.035(5) 0.004(4) 0.007(4) 0.016(4) C10 0.030(5) 0.037(6) 0.034(6) 0.007(4) -0.002(4) 0.015(5) C11 0.030(6) 0.055(7) 0.025(5) 0.007(5) -0.007(4) 0.023(5) C12 0.037(6) 0.037(6) 0.035(6) -0.002(5) 0.001(5) 0.022(5) C13 0.027(5) 0.037(6) 0.040(6) 0.006(5) 0.010(4) 0.014(5) C14 0.027(5) 0.034(6) 0.031(5) -0.004(4) 0.002(4) 0.008(5) C15 0.030(6) 0.042(6) 0.041(6) 0.005(5) 0.009(5) 0.017(5) C16 0.041(6) 0.037(6) 0.054(7) 0.011(5) 0.017(5) 0.023(5) C17 0.047(7) 0.032(6) 0.054(7) 0.010(5) 0.007(5) 0.027(5) C18 0.035(6) 0.040(6) 0.059(7) 0.005(5) 0.013(5) 0.022(5) C19 0.032(6) 0.035(5) 0.037(6) 0.007(4) 0.010(4) 0.020(5) C20 0.043(6) 0.034(6) 0.035(6) 0.003(5) 0.008(5) 0.014(5) O1S 0.087(7) 0.126(9) 0.084(7) 0.073(7) 0.043(6) 0.076(7) N1S 0.119(12) 0.105(11) 0.076(9) 0.025(8) 0.009(9) 0.076(10) C1S 0.068(10) 0.069(10) 0.071(10) -0.006(8) -0.002(8) 0.040(8) C2S 0.077(11) 0.076(10) 0.071(10) 0.004(8) -0.005(8) 0.031(9) C3S 0.153(18) 0.138(17) 0.055(9) 0.043(10) 0.019(10) 0.100(15) C4S 0.132(19) 0.21(3) 0.16(2) 0.088(19) 0.060(16) 0.13(2) _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 Zn1 O4 1.934(7) . ? Zn1 O5 1.938(7) 3_565 ? Zn1 O1M 1.962(3) . ? Zn1 O1 1.971(7) . ? Zn1 Zn2 3.114(3) . ? Zn2 O1M 1.920(10) . ? Zn2 O2 1.944(7) 3_565 ? Zn2 O2 1.944(7) . ? Zn2 O2 1.944(7) 2_665 ? Zn2 Zn1 3.114(3) 3_565 ? Zn2 Zn1 3.114(3) 2_665 ? O1M Zn1 1.962(3) 3_565 ? O1M Zn1 1.962(3) 2_665 ? O1 C1 1.260(13) . ? O2 C1 1.272(13) . ? O3 C8 1.212(11) . ? O4 C11 1.264(12) . ? O5 C11 1.253(13) . ? O5 Zn1 1.938(7) 2_665 ? O6 C18 1.212(13) . ? N1 C8 1.359(12) . ? N1 C4 1.434(12) . ? N2 C18 1.339(13) . ? N2 C14 1.402(13) . ? C1 C2 1.491(14) . ? C2 C7 1.382(16) . ? C2 C3 1.384(14) . ? C3 C4 1.385(14) . ? C4 C5 1.375(16) . ? C5 C6 1.391(17) . ? C6 C7 1.365(17) . ? C8 C9 1.497(13) . ? C9 C10 1.370(13) . ? C9 C10 1.409(13) 3_665 ? C10 C9 1.409(13) 2_655 ? C11 C12 1.498(14) . ? C12 C13 1.368(14) . ? C12 C17 1.384(14) . ? C13 C14 1.379(14) . ? C14 C15 1.408(14) . ? C15 C16 1.370(15) . ? C16 C17 1.384(14) . ? C18 C19 1.493(14) . ? C19 C20 1.391(14) 2_655 ? C19 C20 1.392(14) . ? C20 C19 1.391(14) 3_665 ? O1S C1S 1.197(16) . ? N1S C1S 1.300(18) . ? N1S C4S 1.47(2) . ? N1S C3S 1.475(19) . ? C1S C2S 1.52(2) . ? 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 O4 Zn1 O5 108.4(3) . 3_565 ? O4 Zn1 O1M 107.3(3) . . ? O5 Zn1 O1M 109.4(3) 3_565 . ? O4 Zn1 O1 106.9(3) . . ? O5 Zn1 O1 116.1(4) 3_565 . ? O1M Zn1 O1 108.4(4) . . ? O4 Zn1 Zn2 120.6(2) . . ? O5 Zn1 Zn2 125.5(2) 3_565 . ? O1M Zn1 Zn2 36.2(3) . . ? O1 Zn1 Zn2 72.2(3) . . ? O1M Zn2 O2 109.7(3) . 3_565 ? O1M Zn2 O2 109.7(3) . . ? O2 Zn2 O2 109.2(3) 3_565 . ? O1M Zn2 O2 109.7(3) . 2_665 ? O2 Zn2 O2 109.2(3) 3_565 2_665 ? O2 Zn2 O2 109.2(3) . 2_665 ? O1M Zn2 Zn1 37.14(4) . 3_565 ? O2 Zn2 Zn1 76.0(3) 3_565 3_565 ? O2 Zn2 Zn1 108.0(3) . 3_565 ? O2 Zn2 Zn1 137.8(3) 2_665 3_565 ? O1M Zn2 Zn1 37.14(4) . 2_665 ? O2 Zn2 Zn1 108.0(3) 3_565 2_665 ? O2 Zn2 Zn1 137.8(3) . 2_665 ? O2 Zn2 Zn1 76.0(3) 2_665 2_665 ? Zn1 Zn2 Zn1 63.05(6) 3_565 2_665 ? O1M Zn2 Zn1 37.14(4) . . ? O2 Zn2 Zn1 137.8(3) 3_565 . ? O2 Zn2 Zn1 76.0(3) . . ? O2 Zn2 Zn1 107.9(3) 2_665 . ? Zn1 Zn2 Zn1 63.05(6) 3_565 . ? Zn1 Zn2 Zn1 63.05(6) 2_665 . ? Zn2 O1M Zn1 106.7(3) . 3_565 ? Zn2 O1M Zn1 106.7(3) . 2_665 ? Zn1 O1M Zn1 112.1(2) 3_565 2_665 ? Zn2 O1M Zn1 106.7(3) . . ? Zn1 O1M Zn1 112.1(2) 3_565 . ? Zn1 O1M Zn1 112.1(2) 2_665 . ? C1 O1 Zn1 128.3(7) . . ? C1 O2 Zn2 119.1(6) . . ? C11 O4 Zn1 134.3(7) . . ? C11 O5 Zn1 130.8(7) . 2_665 ? C8 N1 C4 124.9(8) . . ? C18 N2 C14 128.1(9) . . ? O1 C1 O2 124.7(9) . . ? O1 C1 C2 118.6(9) . . ? O2 C1 C2 116.8(10) . . ? C7 C2 C3 121.0(10) . . ? C7 C2 C1 119.7(10) . . ? C3 C2 C1 119.2(10) . . ? C2 C3 C4 118.9(10) . . ? C5 C4 C3 120.3(10) . . ? C5 C4 N1 116.2(10) . . ? C3 C4 N1 123.5(10) . . ? C4 C5 C6 119.7(11) . . ? C7 C6 C5 120.5(12) . . ? C6 C7 C2 119.3(11) . . ? O3 C8 N1 124.0(9) . . ? O3 C8 C9 121.5(8) . . ? N1 C8 C9 114.6(8) . . ? C10 C9 C10 119.5(10) . 3_665 ? C10 C9 C8 123.2(9) . . ? C10 C9 C8 117.0(8) 3_665 . ? C9 C10 C9 120.5(10) . 2_655 ? O5 C11 O4 125.1(10) . . ? O5 C11 C12 119.4(9) . . ? O4 C11 C12 115.5(10) . . ? C13 C12 C17 120.2(9) . . ? C13 C12 C11 119.4(9) . . ? C17 C12 C11 120.4(9) . . ? C12 C13 C14 120.6(10) . . ? C13 C14 N2 123.6(9) . . ? C13 C14 C15 119.3(10) . . ? N2 C14 C15 117.0(9) . . ? C16 C15 C14 119.7(10) . . ? C15 C16 C17 120.3(10) . . ? C16 C17 C12 119.9(9) . . ? O6 C18 N2 123.6(10) . . ? O6 C18 C19 119.9(10) . . ? N2 C18 C19 116.5(9) . . ? C20 C19 C20 118.4(10) 2_655 . ? C20 C19 C18 117.9(9) 2_655 . ? C20 C19 C18 123.5(10) . . ? C19 C20 C19 121.6(10) 3_665 . ? C1S N1S C4S 116.6(14) . . ? C1S N1S C3S 125.0(16) . . ? C4S N1S C3S 118.3(14) . . ? O1S C1S N1S 124.6(15) . . ? O1S C1S C2S 120.6(14) . . ? N1S C1S C2S 114.8(14) . . ? 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 H2 O3 0.88 2.16 2.882(11) 138.7 18_654 N1 H1 O1S 0.88 1.91 2.776(12) 166.9 . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.512 _refine_diff_density_min -1.966 _refine_diff_density_rms 0.138 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 -0.026 0.641 0.083 72.5 19.3 2 0.000 0.000 0.108 15.5 0.3 3 0.000 0.308 0.250 73.7 20.1 4 0.000 0.000 0.392 15.5 0.6 5 0.026 0.667 0.417 72.5 19.3 6 -0.026 0.333 0.583 72.4 20.0 7 0.000 0.000 0.608 15.5 -0.3 8 0.000 0.692 0.750 73.8 19.3 9 0.000 0.000 0.892 15.5 0.2 10 0.026 0.359 0.917 72.5 20.0 11 0.307 1.000 0.250 73.8 20.0 12 0.308 0.308 0.750 73.8 19.3 13 0.333 0.359 0.417 72.7 19.3 14 0.333 0.974 0.917 72.4 20.0 15 0.359 0.333 0.083 72.8 19.3 16 0.359 1.026 0.583 72.5 20.0 17 0.333 0.667 0.059 15.4 0.6 18 0.333 0.667 0.559 15.4 0.1 19 0.333 0.667 0.275 15.9 -0.2 20 0.333 0.667 0.775 15.9 0.3 21 0.641 0.974 0.417 72.5 19.3 22 0.641 0.667 0.917 72.7 19.9 23 0.667 0.026 0.083 72.4 19.3 24 0.667 0.641 0.583 72.8 20.0 25 0.692 0.692 0.250 73.8 20.0 26 0.692 1.000 0.750 73.8 19.3 27 0.666 0.333 0.225 15.8 0.3 28 0.666 0.333 0.725 15.8 0.7 29 0.667 0.333 0.441 15.4 0.3 30 0.666 0.333 0.941 15.4 -0.4 _platon_squeeze_details ; ? ;