# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1344 #Belonging to Paper 'Tuning the solid state organisation of C60 ... #by E.M.Veen, P.M. Postma, H.T.Jonkman, A.L.Spek & B.L.Feringa # Compounds 1 & 2 # # CIF-file generated for s1269b - compound #1 #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'May 17 17:51:36 1999' _audit_creation_method 'PLATON option' _audit_update_record ; ? ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Dr. A.L. Spek ; _publ_contact_author_address # Address of author for correspondence ; Bijvoet Center for Biomolecular Research Department of Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'spea@chem.uu.nl' _publ_contact_author_fax '+31 30 2533940' _publ_contact_author_phone '+31 30 2532538' #=============================================================================== data_s1269b #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60, 2(C20 H14), 2(C8 H10)' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C116 H48' _chemical_formula_weight 1441.54 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 19.767(2) _cell_length_b 9.9958(10) _cell_length_c 17.661(2) _cell_angle_alpha 90 _cell_angle_beta 109.882(10) _cell_angle_gamma 90 _cell_volume 3281.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.08 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD4T' _diffrn_measurement_method 'omega scan' # number of measured reflections (redundant set) _diffrn_reflns_number 11766 _diffrn_reflns_av_R_equivalents 0.1500 _diffrn_reflns_av_sigmaI/netI 0.2289 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.33 # number of unique reflections _reflns_number_total 5988 # number of observed reflections (> n sig(I)) _reflns_number_gt 2080 _reflns_threshold_expression 'I>2sigma(I)' _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'CALC W=1/[^2^(FO^2^)+(0.0857P)^2^] WHERE P=(FO^2^+2FC^2^)/3' _refine_ls_hydrogen_treatment 'H-atom refinement: see text ' _refine_ls_extinction_method none _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 5988 _refine_ls_number_parameters 527 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.2605 _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.2611 _refine_ls_wR_factor_gt 0.1882 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.004 _refine_diff_density_max 0.642 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.074 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv C1 C Uani 0.4219(4) 0.1274(7) 0.1384(5) 1.000 0.034(3) C2 C Uani 0.4803(6) 0.2209(7) 0.1462(5) 1.000 0.050(4) C3 C Uani 0.5503(5) 0.1487(12) 0.1908(5) 1.000 0.079(5) C4 C Uani 0.5280(3) 0.0085(9) 0.2085(3) 1.000 0.034(2) C5 C Uani 0.4503(3) 0.0001(8) 0.1745(3) 1.000 0.026(2) C6 C Uani 0.4181(4) -0.1150(7) 0.1365(4) 1.000 0.031(3) C7 C Uani 0.4622(5) -0.2275(7) 0.1333(5) 1.000 0.043(3) C8 C Uani 0.5350(5) -0.2202(9) 0.1656(5) 1.000 0.047(3) C9 C Uani 0.5810(6) -0.2732(9) 0.1206(6) 1.000 0.070(4) C10 C Uani 0.5507(6) -0.3335(9) 0.0548(7) 1.000 0.065(4) C11 C Uani 0.4746(6) -0.3452(8) 0.0196(6) 1.000 0.053(4) C12 C Uani 0.4295(5) -0.2946(7) 0.0538(6) 1.000 0.045(3) C13 C Uani 0.3658(5) -0.2190(10) 0.0099(6) 1.000 0.063(4) C14 C Uani 0.3574(5) -0.1054(10) 0.0642(5) 1.000 0.046(3) C15 C Uani 0.3328(4) 0.0077(13) 0.0283(6) 1.000 0.072(4) C16 C Uani 0.3117(4) 0.0313(12) -0.0619(6) 1.000 0.067(4) C17 C Uani 0.3328(5) 0.1639(11) -0.0732(5) 1.000 0.057(4) C18 C Uani 0.3626(5) 0.2251(10) 0.0028(6) 1.000 0.061(4) C19 C Uani 0.3640(4) 0.1265(10) 0.0673(6) 1.000 0.051(4) C20 C Uani 0.4206(7) 0.3081(9) 0.0161(8) 1.000 0.068(5) C21 C Uani 0.4805(8) 0.3086(8) 0.0868(6) 1.000 0.079(5) C22 C Uani 0.5451(6) 0.3287(8) 0.0677(7) 1.000 0.066(5) C23 C Uani 0.6086(7) 0.2591(10) 0.1099(7) 1.000 0.080(5) C24 C Uani 0.6103(6) 0.1648(13) 0.1734(7) 1.000 0.103(6) C25 C Uani 0.6517(5) 0.0530(9) 0.1718(6) 1.000 0.060(4) C26 C Uani 0.6816(5) 0.0747(10) 0.1027(6) 1.000 0.065(4) C27 C Uani 0.6542(6) 0.2028(10) 0.0681(8) 1.000 0.091(6) C28 C Uani 0.6337(5) -0.0777(11) 0.1856(5) 1.000 0.057(4) C29 C Uani 0.5686(5) -0.1001(10) 0.2034(5) 1.000 0.049(3) C30 C Uani 0.6433(4) -0.1826(10) 0.1333(5) 1.000 0.055(4) C101 C Uani 0.1348(4) 0.3759(7) 0.3532(4) 1.000 0.024(3) C102 C Uani 0.1429(4) 0.4441(7) 0.4237(4) 1.000 0.023(2) C103 C Uani 0.1438(4) 0.5828(7) 0.4256(4) 1.000 0.026(2) C104 C Uani 0.1379(3) 0.6538(7) 0.3551(4) 1.000 0.019(2) C105 C Uani 0.1299(4) 0.5849(7) 0.2852(4) 1.000 0.020(2) C106 C Uani 0.1285(4) 0.4449(6) 0.2844(4) 1.000 0.018(2) C107 C Uani -0.0115(4) 0.3845(7) 0.0960(4) 1.000 0.023(2) C108 C Uani -0.0696(4) 0.4566(8) 0.0457(4) 1.000 0.028(3) C109 C Uani -0.0670(4) 0.5954(8) 0.0473(4) 1.000 0.032(3) C110 C Uani -0.0083(4) 0.6643(7) 0.0979(4) 1.000 0.025(2) C111 C Uani 0.0497(4) 0.5899(7) 0.1468(4) 1.000 0.022(2) C112 C Uani 0.0476(4) 0.4498(6) 0.1462(4) 1.000 0.021(2) C113 C Uani 0.2218(4) 0.3737(7) 0.1463(4) 1.000 0.026(2) C114 C Uani 0.2703(4) 0.4408(7) 0.1180(4) 1.000 0.031(3) C115 C Uani 0.2729(4) 0.5796(7) 0.1192(4) 1.000 0.026(2) C116 C Uani 0.2262(4) 0.6514(7) 0.1468(4) 1.000 0.022(2) C117 C Uani 0.1788(4) 0.5836(7) 0.1750(4) 1.000 0.019(2) C118 C Uani 0.1754(4) 0.4449(6) 0.1735(4) 1.000 0.016(2) C119 C Uani 0.1175(4) 0.3865(7) 0.2012(4) 1.000 0.024(3) C120 C Uani 0.1204(3) 0.6465(6) 0.2040(4) 1.000 0.018(2) C91 C Uani 0.2227(3) 0.0117(8) 0.3683(3) 1.000 0.031(2) C92 C Uani 0.1753(3) 0.0130(7) 0.2807(3) 1.000 0.0191(17) C93 C Uani 0.1020(3) 0.0175(7) 0.2606(4) 1.000 0.027(2) C94 C Uani 0.0561(3) 0.0197(7) 0.1804(4) 1.000 0.030(2) C95 C Uani 0.0856(4) 0.0174(8) 0.1201(4) 1.000 0.034(2) C96 C Uani 0.1596(4) 0.0129(7) 0.1400(4) 1.000 0.027(2) C97 C Uani 0.2053(3) 0.0116(7) 0.2190(3) 1.000 0.0215(17) C98 C Uani 0.2854(3) 0.0080(8) 0.2375(4) 1.000 0.032(2) H101 H Uiso 0.13370 0.28090 0.35260 1.000 0.0290 H102 H Uiso 0.14780 0.39550 0.47150 1.000 0.0280 H103 H Uiso 0.14830 0.62920 0.47400 1.000 0.0310 H104 H Uiso 0.13940 0.74880 0.35560 1.000 0.0230 H107 H Uiso -0.01280 0.28950 0.09550 1.000 0.0280 H108 H Uiso -0.11050 0.41140 0.01060 1.000 0.0340 H109 H Uiso -0.10660 0.64450 0.01270 1.000 0.0390 H110 H Uiso -0.00760 0.75930 0.09930 1.000 0.0300 H113 H Uiso 0.22090 0.27870 0.14680 1.000 0.0320 H114 H Uiso 0.30150 0.39150 0.09770 1.000 0.0370 H115 H Uiso 0.30680 0.62520 0.10120 1.000 0.0310 H116 H Uiso 0.22680 0.74650 0.14630 1.000 0.0270 H119 H Uiso 0.11650 0.28650 0.20020 1.000 0.0280 H120 H Uiso 0.12170 0.74650 0.20510 1.000 0.0220 H91A H Uiso 0.19300 0.02450 0.40220 1.000 0.0460 H91B H Uiso 0.25810 0.08410 0.37820 1.000 0.0460 H91C H Uiso 0.24780 -0.07440 0.38120 1.000 0.0460 H93 H Uiso 0.08170 0.01920 0.30230 1.000 0.0330 H94 H Uiso 0.00550 0.02280 0.16770 1.000 0.0360 H95 H Uiso 0.05530 0.01880 0.06520 1.000 0.0410 H96 H Uiso 0.17950 0.01060 0.09800 1.000 0.0330 H98A H Uiso 0.29620 0.02700 0.18830 1.000 0.0480 H98B H Uiso 0.30380 -0.08090 0.25770 1.000 0.0480 H98C H Uiso 0.30840 0.07540 0.27840 1.000 0.0480 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 C1 0.048(6) 0.037(5) 0.028(5) -0.003(4) 0.026(4) 0.014(4) C2 0.112(9) 0.021(5) 0.032(5) -0.009(4) 0.045(6) -0.002(5) C3 0.045(6) 0.178(13) 0.031(6) -0.082(7) 0.036(5) -0.075(8) C4 0.032(4) 0.062(5) 0.010(3) 0.003(4) 0.011(3) 0.003(5) C5 0.031(4) 0.039(4) 0.019(3) -0.001(4) 0.022(3) -0.002(4) C6 0.039(5) 0.038(5) 0.021(4) 0.004(3) 0.016(4) -0.005(4) C7 0.072(7) 0.025(4) 0.048(6) 0.016(4) 0.041(5) 0.001(4) C8 0.052(6) 0.054(6) 0.043(6) 0.044(5) 0.028(5) 0.032(5) C9 0.099(9) 0.034(6) 0.053(7) 0.015(5) -0.006(7) 0.034(6) C10 0.064(7) 0.022(5) 0.104(10) 0.024(5) 0.021(7) 0.008(5) C11 0.091(8) 0.017(4) 0.068(7) 0.003(4) 0.051(6) 0.004(5) C12 0.047(6) 0.022(4) 0.067(7) 0.015(4) 0.022(5) -0.005(4) C13 0.052(7) 0.090(8) 0.037(6) 0.007(6) 0.004(5) -0.054(6) C14 0.040(6) 0.082(7) 0.030(5) 0.006(5) 0.030(5) -0.015(5) C15 0.024(4) 0.126(10) 0.078(7) 0.002(9) 0.031(5) -0.013(7) C16 0.016(4) 0.116(10) 0.059(6) -0.025(7) -0.002(4) 0.010(6) C17 0.031(5) 0.098(8) 0.045(6) 0.022(6) 0.015(5) 0.040(6) C18 0.055(7) 0.085(8) 0.037(6) 0.001(6) 0.008(5) 0.061(6) C19 0.008(4) 0.089(8) 0.053(7) -0.010(6) 0.007(4) 0.015(5) C20 0.091(9) 0.032(6) 0.104(10) 0.004(6) 0.062(8) 0.025(6) C21 0.162(13) 0.024(5) 0.058(7) -0.022(5) 0.048(8) 0.018(7) C22 0.101(10) 0.016(5) 0.111(10) -0.031(5) 0.076(9) -0.027(5) C23 0.114(11) 0.029(5) 0.053(7) -0.002(5) -0.027(7) -0.045(6) C24 0.088(10) 0.111(11) 0.062(8) -0.053(8) -0.038(8) -0.022(9) C25 0.057(7) 0.051(6) 0.040(6) -0.005(5) -0.027(5) -0.004(5) C26 0.024(5) 0.063(7) 0.079(8) 0.027(6) -0.020(5) -0.025(5) C27 0.056(8) 0.054(7) 0.148(14) -0.040(9) 0.014(9) -0.047(6) C28 0.037(5) 0.122(9) 0.007(4) 0.018(5) 0.000(4) 0.048(6) C29 0.041(5) 0.083(7) 0.023(5) 0.013(5) 0.010(4) 0.018(5) C30 0.031(5) 0.104(8) 0.038(5) 0.042(6) 0.022(4) 0.047(5) C101 0.023(4) 0.019(4) 0.032(5) 0.001(3) 0.011(4) -0.004(3) C102 0.021(4) 0.033(4) 0.017(4) 0.005(3) 0.008(3) -0.004(3) C103 0.022(4) 0.033(4) 0.022(4) -0.011(3) 0.006(4) -0.001(3) C104 0.015(4) 0.027(4) 0.014(4) -0.005(3) 0.005(3) -0.001(3) C105 0.012(4) 0.024(4) 0.023(4) 0.001(3) 0.004(3) 0.000(3) C106 0.019(4) 0.022(4) 0.014(4) -0.004(3) 0.007(3) -0.005(3) C107 0.022(4) 0.031(4) 0.020(4) -0.004(3) 0.011(3) -0.009(3) C108 0.011(4) 0.059(5) 0.012(4) -0.013(3) 0.000(3) -0.011(3) C109 0.031(5) 0.050(5) 0.018(4) 0.008(4) 0.011(4) 0.008(4) C110 0.032(4) 0.031(4) 0.015(4) -0.002(3) 0.011(3) 0.007(4) C111 0.024(4) 0.030(4) 0.014(4) 0.004(3) 0.011(3) -0.004(3) C112 0.019(4) 0.029(4) 0.018(4) 0.002(3) 0.009(3) 0.001(3) C113 0.019(4) 0.034(4) 0.018(4) -0.001(3) -0.003(3) 0.005(3) C114 0.032(5) 0.041(5) 0.030(5) -0.003(3) 0.025(4) 0.002(4) C115 0.018(4) 0.038(4) 0.022(4) 0.005(3) 0.008(4) -0.003(3) C116 0.024(4) 0.025(4) 0.025(4) 0.002(3) 0.017(4) -0.002(3) C117 0.019(4) 0.028(4) 0.009(4) 0.000(3) 0.003(3) -0.002(3) C118 0.014(4) 0.020(4) 0.013(4) 0.002(3) 0.003(3) -0.004(3) C119 0.032(5) 0.021(4) 0.019(4) 0.000(3) 0.009(3) -0.002(3) C120 0.015(4) 0.018(3) 0.021(4) 0.003(3) 0.005(3) 0.001(3) C91 0.038(4) 0.037(4) 0.017(3) -0.005(4) 0.010(3) -0.001(4) C92 0.023(3) 0.016(3) 0.017(3) -0.004(3) 0.005(3) -0.002(3) C93 0.032(4) 0.025(4) 0.028(4) -0.002(3) 0.014(3) -0.001(4) C94 0.018(3) 0.031(4) 0.038(4) -0.004(4) 0.006(3) -0.006(3) C95 0.040(4) 0.034(4) 0.022(3) -0.004(4) 0.002(3) -0.005(4) C96 0.035(4) 0.021(4) 0.029(3) 0.004(4) 0.015(3) -0.001(4) C97 0.027(3) 0.022(3) 0.014(3) -0.005(3) 0.005(3) 0.002(3) C98 0.032(4) 0.032(4) 0.035(4) 0.000(4) 0.015(3) 0.001(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.455(13) . . no C1 C5 1.448(10) . . no C1 C19 1.382(13) . . no C2 C3 1.521(15) . . no C2 C21 1.368(13) . . no C3 C4 1.533(14) . . no C3 C24 1.332(16) . . no C4 C5 1.449(9) . . no C4 C29 1.371(13) . . no C5 C6 1.374(10) . . no C6 C7 1.436(11) . . no C6 C14 1.427(11) . . no C7 C8 1.358(14) . . no C7 C12 1.491(12) . . no C8 C9 1.494(15) . . no C8 C29 1.424(13) . . no C9 C10 1.265(15) . . no C9 C30 1.483(14) . . no C10 C11 1.424(17) . . no C10 C20 1.561(18) . 3_655 no C11 C12 1.335(15) . . no C11 C22 1.465(15) . 3_655 no C12 C13 1.447(14) . . no C13 C14 1.531(14) . . no C13 C27 1.308(17) . 3_655 no C14 C15 1.306(16) . . no C15 C16 1.522(14) . . no C15 C19 1.406(16) . . no C16 C17 1.424(16) . . no C16 C26 1.313(15) . 3_655 no C17 C18 1.409(13) . . no C17 C30 1.314(12) . 3_655 no C18 C19 1.499(14) . . no C18 C20 1.369(16) . . no C20 C21 1.398(18) . . no C21 C22 1.44(2) . . no C22 C23 1.407(17) . . no C23 C24 1.457(17) . . no C23 C27 1.458(18) . . no C24 C25 1.391(16) . . no C25 C26 1.542(14) . . no C25 C28 1.397(14) . . no C26 C27 1.443(15) . . no C28 C29 1.442(15) . . no C28 C30 1.452(14) . . no C101 C102 1.380(10) . . no C101 C106 1.366(9) . . no C102 C103 1.387(10) . . no C103 C104 1.403(10) . . no C104 C105 1.375(10) . . no C105 C106 1.400(9) . . no C105 C120 1.513(9) . . no C106 C119 1.526(9) . . no C107 C108 1.391(11) . . no C107 C112 1.368(10) . . no C108 C109 1.388(11) . . no C109 C110 1.383(11) . . no C110 C111 1.393(10) . . no C111 C112 1.401(9) . . no C111 C120 1.528(10) . . no C112 C119 1.530(11) . . no C113 C114 1.395(11) . . no C113 C118 1.370(11) . . no C114 C115 1.388(10) . . no C115 C116 1.382(11) . . no C116 C117 1.379(11) . . no C117 C118 1.388(9) . . no C117 C120 1.547(10) . . no C118 C119 1.507(11) . . no C101 H101 0.9498 . . no C102 H102 0.9500 . . no C103 H103 0.9497 . . no C104 H104 0.9500 . . no C107 H107 0.9499 . . no C108 H108 0.9493 . . no C109 H109 0.9496 . . no C110 H110 0.9499 . . no C113 H113 0.9499 . . no C114 H114 0.9498 . . no C115 H115 0.9501 . . no C116 H116 0.9508 . . no C119 H119 0.9998 . . no C120 H120 0.9999 . . no C91 C92 1.512(7) . . no C92 C93 1.370(9) . . no C92 C97 1.407(8) . . no C93 C94 1.399(9) . . no C94 C95 1.377(10) . . no C95 C96 1.384(12) . . no C96 C97 1.380(9) . . no C97 C98 1.504(9) . . no C91 H91A 0.9791 . . no C91 H91B 0.9802 . . no C91 H91C 0.9808 . . no C93 H93 0.9512 . . no C94 H94 0.9482 . . no C95 H95 0.9508 . . no C96 H96 0.9508 . . no C98 H98A 0.9812 . . no C98 H98B 0.9803 . . no C98 H98C 0.9793 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 110.3(7) . . . no C2 C1 C19 118.4(7) . . . no C5 C1 C19 118.1(7) . . . no C1 C2 C3 107.3(7) . . . no C1 C2 C21 123.2(9) . . . no C3 C2 C21 117.5(11) . . . no C2 C3 C4 105.4(7) . . . no C2 C3 C24 123.2(10) . . . no C4 C3 C24 119.9(10) . . . no C3 C4 C5 107.8(7) . . . no C3 C4 C29 119.7(7) . . . no C5 C4 C29 119.2(8) . . . no C1 C5 C4 109.2(7) . . . no C1 C5 C6 118.3(6) . . . no C4 C5 C6 120.0(7) . . . no C5 C6 C7 119.2(7) . . . no C5 C6 C14 119.3(7) . . . no C7 C6 C14 110.8(7) . . . no C6 C7 C8 120.8(7) . . . no C6 C7 C12 108.4(7) . . . no C8 C7 C12 118.6(8) . . . no C7 C8 C9 120.5(8) . . . no C7 C8 C29 120.1(9) . . . no C9 C8 C29 106.1(9) . . . no C8 C9 C10 118.3(11) . . . no C8 C9 C30 109.1(8) . . . no C10 C9 C30 122.7(10) . . . no C9 C10 C11 122.7(11) . . . no C9 C10 C20 118.2(11) . . 3_655 no C11 C10 C20 106.3(10) . . 3_655 no C10 C11 C12 122.7(9) . . . no C10 C11 C22 108.3(10) . . 3_655 no C12 C11 C22 117.0(10) . . 3_655 no C7 C12 C11 117.0(9) . . . no C7 C12 C13 106.8(7) . . . no C11 C12 C13 123.3(9) . . . no C12 C13 C14 108.2(8) . . . no C12 C13 C27 121.7(10) . . 3_655 no C14 C13 C27 120.6(9) . . 3_655 no C6 C14 C13 105.9(8) . . . no C6 C14 C15 123.6(9) . . . no C13 C14 C15 116.1(8) . . . no C14 C15 C16 124.5(10) . . . no C14 C15 C19 117.7(9) . . . no C16 C15 C19 107.5(10) . . . no C15 C16 C17 107.6(9) . . . no C15 C16 C26 114.0(10) . . 3_655 no C17 C16 C26 125.8(9) . . 3_655 no C16 C17 C18 108.6(8) . . . no C16 C17 C30 116.7(9) . . 3_655 no C18 C17 C30 124.0(10) . . 3_655 no C17 C18 C19 109.4(9) . . . no C17 C18 C20 118.7(10) . . . no C19 C18 C20 118.0(9) . . . no C1 C19 C15 122.7(9) . . . no C1 C19 C18 118.8(8) . . . no C15 C19 C18 106.9(9) . . . no C18 C20 C21 124.1(11) . . . no C10 C20 C18 118.2(10) 3_655 . . no C10 C20 C21 106.7(12) 3_655 . . no C2 C21 C20 117.4(12) . . . no C2 C21 C22 120.2(11) . . . no C20 C21 C22 109.9(10) . . . no C21 C22 C23 120.6(10) . . . no C11 C22 C21 108.8(10) 3_655 . . no C11 C22 C23 118.9(11) 3_655 . . no C22 C23 C24 120.7(12) . . . no C22 C23 C27 121.1(11) . . . no C24 C23 C27 106.5(10) . . . no C3 C24 C23 117.8(11) . . . no C3 C24 C25 118.9(11) . . . no C23 C24 C25 111.3(10) . . . no C24 C25 C26 106.8(9) . . . no C24 C25 C28 124.1(10) . . . no C26 C25 C28 117.3(8) . . . no C25 C26 C27 105.7(9) . . . no C16 C26 C25 117.3(9) 3_655 . . no C16 C26 C27 125.2(10) 3_655 . . no C23 C27 C26 109.6(10) . . . no C13 C27 C23 117.9(11) 3_655 . . no C13 C27 C26 119.4(10) 3_655 . . no C25 C28 C29 118.8(9) . . . no C25 C28 C30 117.9(8) . . . no C29 C28 C30 110.2(9) . . . no C4 C29 C8 120.6(9) . . . no C4 C29 C28 118.5(9) . . . no C8 C29 C28 109.7(9) . . . no C9 C30 C28 104.8(8) . . . no C9 C30 C17 118.2(9) . . 3_655 no C17 C30 C28 124.9(10) 3_655 . . no C102 C101 C106 120.0(6) . . . no C101 C102 C103 120.8(6) . . . no C102 C103 C104 119.2(6) . . . no C103 C104 C105 119.5(6) . . . no C104 C105 C106 120.4(6) . . . no C104 C105 C120 125.9(6) . . . no C106 C105 C120 113.7(6) . . . no C101 C106 C105 120.0(6) . . . no C101 C106 C119 127.1(6) . . . no C105 C106 C119 112.8(6) . . . no C108 C107 C112 120.3(7) . . . no C107 C108 C109 119.2(7) . . . no C108 C109 C110 121.9(7) . . . no C109 C110 C111 117.9(7) . . . no C110 C111 C112 120.9(7) . . . no C110 C111 C120 126.0(6) . . . no C112 C111 C120 113.2(6) . . . no C107 C112 C111 119.9(7) . . . no C107 C112 C119 127.0(6) . . . no C111 C112 C119 113.0(6) . . . no C114 C113 C118 120.0(6) . . . no C113 C114 C115 120.1(7) . . . no C114 C115 C116 119.9(7) . . . no C115 C116 C117 119.3(7) . . . no C116 C117 C118 121.2(7) . . . no C116 C117 C120 126.5(6) . . . no C118 C117 C120 112.1(7) . . . no C113 C118 C117 119.4(7) . . . no C113 C118 C119 125.8(6) . . . no C117 C118 C119 114.7(7) . . . no C106 C119 C112 104.8(6) . . . no C106 C119 C118 106.8(6) . . . no C112 C119 C118 104.8(6) . . . no C105 C120 C111 105.5(5) . . . no C105 C120 C117 106.4(5) . . . no C111 C120 C117 104.4(5) . . . no C102 C101 H101 119.94 . . . no C106 C101 H101 120.01 . . . no C101 C102 H102 119.64 . . . no C103 C102 H102 119.55 . . . no C102 C103 H103 120.43 . . . no C104 C103 H103 120.38 . . . no C103 C104 H104 120.29 . . . no C105 C104 H104 120.18 . . . no C108 C107 H107 119.89 . . . no C112 C107 H107 119.82 . . . no C107 C108 H108 120.36 . . . no C109 C108 H108 120.42 . . . no C108 C109 H109 119.13 . . . no C110 C109 H109 119.02 . . . no C109 C110 H110 121.07 . . . no C111 C110 H110 121.07 . . . no C114 C113 H113 120.10 . . . no C118 C113 H113 119.94 . . . no C113 C114 H114 119.97 . . . no C115 C114 H114 119.92 . . . no C114 C115 H115 120.07 . . . no C116 C115 H115 120.03 . . . no C115 C116 H116 120.26 . . . no C117 C116 H116 120.45 . . . no C106 C119 H119 113.26 . . . no C112 C119 H119 113.21 . . . no C118 C119 H119 113.22 . . . no C105 C120 H120 113.23 . . . no C111 C120 H120 113.25 . . . no C117 C120 H120 113.31 . . . no C91 C92 C93 119.9(5) . . . no C91 C92 C97 121.0(5) . . . no C93 C92 C97 119.1(5) . . . no C92 C93 C94 121.8(6) . . . no C93 C94 C95 118.9(6) . . . no C94 C95 C96 119.5(6) . . . no C95 C96 C97 121.9(7) . . . no C92 C97 C96 118.7(6) . . . no C92 C97 C98 121.5(5) . . . no C96 C97 C98 119.9(6) . . . no C92 C91 H91A 109.44 . . . no C92 C91 H91B 109.43 . . . no C92 C91 H91C 109.50 . . . no H91A C91 H91B 109.55 . . . no H91A C91 H91C 109.50 . . . no H91B C91 H91C 109.41 . . . no C92 C93 H93 119.17 . . . no C94 C93 H93 118.99 . . . no C93 C94 H94 120.59 . . . no C95 C94 H94 120.50 . . . no C94 C95 H95 120.18 . . . no C96 C95 H95 120.28 . . . no C95 C96 H96 118.99 . . . no C97 C96 H96 119.09 . . . no C97 C98 H98A 109.45 . . . no C97 C98 H98B 109.48 . . . no C97 C98 H98C 109.52 . . . no H98A C98 H98B 109.40 . . . no H98A C98 H98C 109.50 . . . no H98B C98 H98C 109.48 . . . no 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 C5 C1 C2 C3 -0.5(9) . . . . no C5 C1 C2 C21 140.9(10) . . . . no C19 C1 C2 C3 -141.0(8) . . . . no C19 C1 C2 C21 0.4(14) . . . . no C2 C1 C5 C4 1.4(8) . . . . no C2 C1 C5 C6 -140.9(7) . . . . no C19 C1 C5 C4 141.9(7) . . . . no C19 C1 C5 C6 -0.3(11) . . . . no C2 C1 C19 C15 136.2(9) . . . . no C2 C1 C19 C18 -2.3(13) . . . . no C5 C1 C19 C15 -1.2(13) . . . . no C5 C1 C19 C18 -139.7(8) . . . . no C1 C2 C3 C4 -0.4(9) . . . . no C1 C2 C3 C24 142.4(11) . . . . no C21 C2 C3 C4 -144.4(7) . . . . no C21 C2 C3 C24 -1.6(14) . . . . no C1 C2 C21 C20 1.0(16) . . . . no C1 C2 C21 C22 -137.1(10) . . . . no C3 C2 C21 C20 138.8(11) . . . . no C3 C2 C21 C22 0.8(12) . . . . no C2 C3 C4 C5 1.3(8) . . . . no C2 C3 C4 C29 142.0(7) . . . . no C24 C3 C4 C5 -143.1(9) . . . . no C24 C3 C4 C29 -2.4(12) . . . . no C2 C3 C24 C23 1.7(16) . . . . no C2 C3 C24 C25 -137.9(11) . . . . no C4 C3 C24 C23 139.5(10) . . . . no C4 C3 C24 C25 -0.1(15) . . . . no C3 C4 C5 C1 -1.6(7) . . . . no C3 C4 C5 C6 139.9(7) . . . . no C29 C4 C5 C1 -142.5(7) . . . . no C29 C4 C5 C6 -1.1(9) . . . . no C3 C4 C29 C8 -136.7(8) . . . . no C3 C4 C29 C28 3.3(10) . . . . no C5 C4 C29 C8 -0.4(11) . . . . no C5 C4 C29 C28 139.6(7) . . . . no C1 C5 C6 C7 140.0(7) . . . . no C1 C5 C6 C14 -1.2(11) . . . . no C4 C5 C6 C7 2.0(10) . . . . no C4 C5 C6 C14 -139.3(7) . . . . no C5 C6 C7 C8 -1.5(12) . . . . no C5 C6 C7 C12 -143.2(7) . . . . no C14 C6 C7 C8 142.7(9) . . . . no C14 C6 C7 C12 1.1(10) . . . . no C5 C6 C14 C13 142.1(8) . . . . no C5 C6 C14 C15 4.6(14) . . . . no C7 C6 C14 C13 -2.1(10) . . . . no C7 C6 C14 C15 -139.6(10) . . . . no C6 C7 C8 C9 -135.4(9) . . . . no C6 C7 C8 C29 0.1(12) . . . . no C12 C7 C8 C9 2.6(12) . . . . no C12 C7 C8 C29 138.1(8) . . . . no C6 C7 C12 C11 143.5(8) . . . . no C6 C7 C12 C13 0.6(11) . . . . no C8 C7 C12 C11 0.8(11) . . . . no C8 C7 C12 C13 -142.1(8) . . . . no C7 C8 C9 C10 -5.1(13) . . . . no C7 C8 C9 C30 141.5(9) . . . . no C29 C8 C9 C10 -146.0(9) . . . . no C29 C8 C9 C30 0.7(10) . . . . no C7 C8 C29 C4 0.8(13) . . . . no C7 C8 C29 C28 -142.3(9) . . . . no C9 C8 C29 C4 141.9(8) . . . . no C9 C8 C29 C28 -1.3(10) . . . . no C8 C9 C10 C11 4.1(15) . . . . no C8 C9 C10 C20 140.4(10) . . . 3_655 no C30 C9 C10 C11 -137.8(11) . . . . no C30 C9 C10 C20 -1.5(16) . . . 3_655 no C8 C9 C30 C28 0.2(12) . . . . no C8 C9 C30 C17 -144.3(9) . . . 3_655 no C10 C9 C30 C28 145.1(10) . . . . no C10 C9 C30 C17 0.6(15) . . . 3_655 no C9 C10 C11 C12 -0.7(15) . . . . no C9 C10 C11 C22 140.6(10) . . . 3_655 no C20 C10 C11 C12 -141.3(9) 3_655 . . . no C20 C10 C11 C22 0.0(9) 3_655 . . 3_655 no C9 C10 C20 C18 2.0(16) . . 3_655 3_655 no C9 C10 C20 C21 -143.5(10) . . 3_655 3_655 no C11 C10 C20 C18 144.7(10) . . 3_655 3_655 no C11 C10 C20 C21 -0.8(10) . . 3_655 3_655 no C10 C11 C12 C7 -1.9(12) . . . . no C10 C11 C12 C13 134.4(10) . . . . no C22 C11 C12 C7 -140.1(8) 3_655 . . . no C22 C11 C12 C13 -3.8(13) 3_655 . . . no C10 C11 C22 C21 0.9(10) . . 3_655 3_655 no C10 C11 C22 C23 -142.5(9) . . 3_655 3_655 no C12 C11 C22 C21 144.6(8) . . 3_655 3_655 no C12 C11 C22 C23 1.3(13) . . 3_655 3_655 no C7 C12 C13 C14 -1.8(10) . . . . no C7 C12 C13 C27 144.6(10) . . . 3_655 no C11 C12 C13 C14 -141.9(9) . . . . no C11 C12 C13 C27 4.5(15) . . . 3_655 no C12 C13 C14 C6 2.5(11) . . . . no C12 C13 C14 C15 143.7(9) . . . . no C27 C13 C14 C6 -144.4(10) 3_655 . . . no C27 C13 C14 C15 -3.2(15) 3_655 . . . no C12 C13 C27 C23 -2.4(16) . . 3_655 3_655 no C12 C13 C27 C26 -139.7(11) . . 3_655 3_655 no C14 C13 C27 C23 139.9(10) . . 3_655 3_655 no C14 C13 C27 C26 2.6(17) . . 3_655 3_655 no C6 C14 C15 C16 134.5(10) . . . . no C6 C14 C15 C19 -6.0(14) . . . . no C13 C14 C15 C16 0.9(15) . . . . no C13 C14 C15 C19 -139.6(9) . . . . no C14 C15 C16 C17 -142.6(10) . . . . no C14 C15 C16 C26 1.8(14) . . . 3_655 no C19 C15 C16 C17 1.2(11) . . . . no C19 C15 C16 C26 145.6(9) . . . 3_655 no C14 C15 C19 C1 4.3(14) . . . . no C14 C15 C19 C18 146.9(9) . . . . no C16 C15 C19 C1 -142.4(9) . . . . no C16 C15 C19 C18 0.2(11) . . . . no C15 C16 C17 C18 -2.3(11) . . . . no C15 C16 C17 C30 143.7(9) . . . 3_655 no C26 C16 C17 C18 -141.2(11) 3_655 . . . no C26 C16 C17 C30 4.7(15) 3_655 . . 3_655 no C15 C16 C26 C25 -140.0(9) . . 3_655 3_655 no C15 C16 C26 C27 -2.5(15) . . 3_655 3_655 no C17 C16 C26 C25 -3.2(15) . . 3_655 3_655 no C17 C16 C26 C27 134.3(12) . . 3_655 3_655 no C16 C17 C18 C19 2.4(12) . . . . no C16 C17 C18 C20 142.0(10) . . . . no C30 C17 C18 C19 -140.4(10) 3_655 . . . no C30 C17 C18 C20 -0.9(16) 3_655 . . . no C16 C17 C30 C9 -140.0(9) . . 3_655 3_655 no C16 C17 C30 C28 -3.2(14) . . 3_655 3_655 no C18 C17 C30 C9 0.2(15) . . 3_655 3_655 no C18 C17 C30 C28 137.0(11) . . 3_655 3_655 no C17 C18 C19 C1 142.7(9) . . . . no C17 C18 C19 C15 -1.6(11) . . . . no C20 C18 C19 C1 2.8(14) . . . . no C20 C18 C19 C15 -141.5(10) . . . . no C17 C18 C20 C21 -137.5(12) . . . . no C17 C18 C20 C10 1.7(15) . . . 3_655 no C19 C18 C20 C21 -1.4(17) . . . . no C19 C18 C20 C10 137.8(10) . . . 3_655 no C18 C20 C21 C2 -0.5(18) . . . . no C18 C20 C21 C22 141.6(11) . . . . no C10 C20 C21 C2 -143.5(10) 3_655 . . . no C10 C20 C21 C22 -1.4(10) 3_655 . . . no C2 C21 C22 C23 -0.2(14) . . . . no C2 C21 C22 C11 142.3(8) . . . 3_655 no C20 C21 C22 C23 -141.1(10) . . . . no C20 C21 C22 C11 1.4(10) . . . 3_655 no C21 C22 C23 C24 0.4(15) . . . . no C21 C22 C23 C27 138.4(11) . . . . no C11 C22 C23 C24 -138.6(11) 3_655 . . . no C11 C22 C23 C27 -0.5(15) 3_655 . . . no C22 C23 C24 C3 -1.1(17) . . . . no C22 C23 C24 C25 141.4(11) . . . . no C27 C23 C24 C3 -144.4(12) . . . . no C27 C23 C24 C25 -1.9(14) . . . . no C22 C23 C27 C26 -141.2(11) . . . . no C22 C23 C27 C13 0.0(16) . . . 3_655 no C24 C23 C27 C26 1.9(14) . . . . no C24 C23 C27 C13 143.1(11) . . . 3_655 no C3 C24 C25 C26 143.2(10) . . . . no C3 C24 C25 C28 1.5(16) . . . . no C23 C24 C25 C26 1.2(13) . . . . no C23 C24 C25 C28 -140.5(11) . . . . no C24 C25 C26 C27 0.1(12) . . . . no C24 C25 C26 C16 -145.0(10) . . . 3_655 no C28 C25 C26 C27 144.8(10) . . . . no C28 C25 C26 C16 -0.3(14) . . . 3_655 no C24 C25 C28 C29 -0.5(15) . . . . no C24 C25 C28 C30 137.1(11) . . . . no C26 C25 C28 C29 -138.6(9) . . . . no C26 C25 C28 C30 -1.0(13) . . . . no C25 C26 C27 C23 -1.3(12) . . . . no C25 C26 C27 C13 -141.8(11) . . . 3_655 no C16 C26 C27 C23 140.1(11) 3_655 . . . no C16 C26 C27 C13 -0.4(18) 3_655 . . 3_655 no C25 C28 C29 C4 -2.0(12) . . . . no C25 C28 C29 C8 142.0(9) . . . . no C30 C28 C29 C4 -142.6(8) . . . . no C30 C28 C29 C8 1.4(11) . . . . no C25 C28 C30 C9 -141.9(9) . . . . no C25 C28 C30 C17 -0.6(14) . . . 3_655 no C29 C28 C30 C9 -0.9(10) . . . . no C29 C28 C30 C17 140.4(9) . . . 3_655 no C106 C101 C102 H102 -179.29 . . . . no H101 C101 C102 C103 -179.25 . . . . no H101 C101 C102 H102 0.59 . . . . no H101 C101 C106 C105 179.81 . . . . no H101 C101 C106 C119 1.66 . . . . no C101 C102 C103 H103 178.57 . . . . no H102 C102 C103 C104 178.80 . . . . no H102 C102 C103 H103 -1.27 . . . . no C102 C103 C104 H104 -178.72 . . . . no H103 C103 C104 C105 -178.63 . . . . no H103 C103 C104 H104 1.35 . . . . no H104 C104 C105 C106 179.26 . . . . no H104 C104 C105 C120 -2.13 . . . . no C104 C105 C120 H120 1.59 . . . . no C106 C105 C120 H120 -179.72 . . . . no C101 C106 C119 H119 -1.80 . . . . no C105 C106 C119 H119 179.94 . . . . no C112 C107 C108 H108 179.60 . . . . no H107 C107 C108 C109 179.79 . . . . no H107 C107 C108 H108 -0.35 . . . . no H107 C107 C112 C111 179.78 . . . . no H107 C107 C112 C119 3.99 . . . . no C107 C108 C109 H109 179.65 . . . . no H108 C108 C109 C110 179.81 . . . . no H108 C108 C109 H109 -0.20 . . . . no C108 C109 C110 H110 -178.60 . . . . no H109 C109 C110 C111 -178.67 . . . . no H109 C109 C110 H110 1.42 . . . . no H110 C110 C111 C112 178.18 . . . . no H110 C110 C111 C120 -2.73 . . . . no C110 C111 C120 H120 1.69 . . . . no C112 C111 C120 H120 -179.15 . . . . no C107 C112 C119 H119 -2.98 . . . . no C111 C112 C119 H119 -179.01 . . . . no C118 C113 C114 H114 -178.18 . . . . no H113 C113 C114 C115 -178.33 . . . . no H113 C113 C114 H114 1.88 . . . . no H113 C113 C118 C117 177.87 . . . . no H113 C113 C118 C119 -3.78 . . . . no C113 C114 C115 H115 178.38 . . . . no H114 C114 C115 C116 178.32 . . . . no H114 C114 C115 H115 -1.83 . . . . no C114 C115 C116 H116 -178.18 . . . . no H115 C115 C116 C117 -178.04 . . . . no H115 C115 C116 H116 1.97 . . . . no H116 C116 C117 C118 177.67 . . . . no H116 C116 C117 C120 3.30 . . . . no C116 C117 C120 H120 -4.75 . . . . no C118 C117 C120 H120 -179.55 . . . . no C113 C118 C119 H119 2.27 . . . . no C117 C118 C119 H119 -179.32 . . . . no C91 C92 C93 C94 179.6(7) . . . . no C97 C92 C93 C94 0.5(11) . . . . no C91 C92 C97 C96 -180.0(7) . . . . no C91 C92 C97 C98 0.3(11) . . . . no C93 C92 C97 C96 -0.9(10) . . . . no C93 C92 C97 C98 179.4(7) . . . . no C92 C93 C94 C95 -0.1(11) . . . . no C93 C94 C95 C96 0.0(11) . . . . no C94 C95 C96 C97 -0.5(11) . . . . no C95 C96 C97 C92 0.9(11) . . . . no C95 C96 C97 C98 -179.4(7) . . . . no #---END # CIF-file generated for s1561a - Complex # 2 data_s1561a #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60, C19 H13 N' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C79 H13 N' _chemical_formula_weight 975.90 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Hexagonal _symmetry_space_group_name_Hall 'P 6c -2c' _symmetry_space_group_name_H-M 'P 63 m c' loop_ _symmetry_equiv_pos_as_xyz x,y,z x-y,x,1/2+z -y,x-y,z -x,-y,1/2+z -x+y,-x,z y,-x+y,1/2+z y,x,1/2+z -x+y,y,z -x,-x+y,1/2+z -y,-x,z x-y,-y,1/2+z x,x-y,z _cell_length_a 13.4643(11) _cell_length_b 13.4643(11) _cell_length_c 12.6983(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1993.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 0.09 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating-Anode' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Nonius CAD4-T' _diffrn_measurement_method 'Omega-scan' # number of measured reflections (redundant set) _diffrn_reflns_number 6587 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.52 # number of unique reflections _reflns_number_total 909 # number of observed reflections (> n sig(I)) _reflns_number_gt 711 _reflns_threshold_expression 'I>2sigma(I)' _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs 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/[^2^(FO^2^)+(0.1351P)^2^+4.0391P] WHERE P=(FO^2^+2FC^2^)/3' _refine_ls_hydrogen_treatment 'H-atom refinement: see text ' _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 8(10) _refine_ls_number_reflns 909 _refine_ls_number_parameters 143 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2717 _refine_ls_wR_factor_gt 0.2438 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.113 _refine_ls_shift/su_mean 0.037 _refine_diff_density_max 0.651 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.078 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv C1 C Uani 0.1327(11) 0.4851(13) 0.4348(8) 1.000 0.144(6) C2 C Uani 0.2322(7) 0.5612(6) 0.5026(7) 1.000 0.189(14) C5 C Uani 0.0683(15) 0.5342(7) 0.380(2) 1.000 0.170(11) C6 C Uani 0.1189(14) 0.3842(11) 0.2699(17) 1.000 0.251(15) C7 C Uani 0.1916(6) 0.3831(12) 0.183(3) 1.000 0.28(3) C9 C Uani 0.1537(7) 0.4167(13) 0.3803(16) 1.000 0.246(11) C11 C Uani 0.0607(8) 0.4304(12) 0.2395(14) 1.000 0.212(9) C12 C Uani 0.0736(12) 0.4819(7) 0.1344(15) 1.000 0.241(16) C14 C Uani 0.0363(14) 0.5181(7) 0.284(3) 1.000 0.36(4) C16 C Uani 0.2279(6) 0.5659(7) -0.0027(7) 1.000 0.129(7) C17 C Uani 0.1392(12) 0.4752(12) 0.0630(8) 1.000 0.155(9) C19 C Uani 0.2155(11) 0.431(2) 0.092(2) 1.000 0.35(4) N1 N Uani 0.00000 0.00000 0.3505(10) 1.000 0.032(3) C101 C Uani 0.00000 0.00000 0.1465(12) 1.000 0.021(3) C102 C Uani 0.1176(6) 0.0588(3) 0.3056(8) 1.000 0.023(2) C103 C Uani 0.2199(8) 0.1100(4) 0.3603(9) 1.000 0.029(3) C104 C Uani 0.3220(7) 0.1610(4) 0.3049(9) 1.000 0.029(2) C105 C Uani 0.3209(7) 0.1605(4) 0.1960(10) 1.000 0.033(2) C106 C Uani 0.2181(8) 0.1091(4) 0.1388(8) 1.000 0.027(2) C107 C Uani 0.1176(6) 0.0588(3) 0.1949(9) 1.000 0.025(2) H101 H Uiso 0.00000 0.00000 0.06770 1.000 0.0250 H103 H Uiso 0.22020 0.11010 0.43510 1.000 0.0350 H104 H Uiso 0.39300 0.19650 0.34160 1.000 0.0340 H105 H Uiso 0.39170 0.19585 0.15900 1.000 0.0390 H106 H Uiso 0.21800 0.10900 0.06400 1.000 0.0330 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 C1 0.122(13) 0.110(10) 0.071(7) 0.025(8) 0.050(8) -0.039(10) C2 0.29(3) 0.31(3) 0.061(9) 0.108(12) 0.102(12) 0.22(2) C5 0.023(7) 0.29(3) 0.107(15) 0.017(4) 0.033(9) 0.011(4) C6 0.142(16) 0.049(8) 0.39(4) -0.024(17) 0.10(2) -0.081(10) C7 0.30(5) 0.004(6) 0.45(8) -0.08(2) -0.038(10) 0.002(3) C9 0.28(3) 0.074(9) 0.156(14) 0.060(11) 0.077(19) -0.082(15) C11 0.021(4) 0.23(2) 0.211(17) -0.147(17) 0.028(9) -0.068(8) C12 0.117(15) 0.25(4) 0.187(19) -0.076(19) -0.114(16) -0.036(17) C14 0.011(7) 0.54(10) 0.34(7) 0.044(11) 0.09(2) 0.006(3) C16 0.164(13) 0.154(14) 0.039(6) -0.046(7) -0.054(7) 0.058(11) C17 0.143(17) 0.190(18) 0.105(12) -0.118(13) -0.093(12) 0.063(14) C19 0.40(7) 0.25(5) 0.33(7) -0.29(6) -0.14(3) 0.12(3) N1 0.038(5) 0.038(5) 0.019(6) 0.0000 0.0000 0.019(2) C101 0.014(3) 0.014(3) 0.034(8) 0.0000 0.0000 0.0071(17) C102 0.026(4) 0.018(2) 0.027(4) 0.0003(15) 0.001(3) 0.0132(19) C103 0.034(5) 0.023(3) 0.034(5) -0.0019(18) -0.004(4) 0.017(2) C104 0.029(4) 0.018(3) 0.043(5) -0.003(2) -0.006(4) 0.014(2) C105 0.023(4) 0.026(3) 0.048(5) 0.005(2) 0.010(4) 0.0117(18) C106 0.035(5) 0.029(3) 0.021(4) 0.0046(17) 0.009(3) 0.018(2) C107 0.025(4) 0.021(3) 0.032(4) -0.0017(16) -0.003(3) 0.013(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C102 1.485(9) . 5_555 yes N1 C102 1.485(9) . . yes N1 C102 1.485(9) . 3_555 yes C1 C2 1.488(17) . . no C1 C5 1.50(3) . . no C1 C9 1.29(2) . . no C2 C2 1.303(16) . 8_555 no C2 C2 1.478(13) . 12_565 no C5 C14 1.27(4) . . no C6 C11 1.28(2) . . no C6 C9 1.47(3) . . no C6 C7 1.48(4) . . no C7 C19 1.28(4) . . no C9 C9 1.47(3) . 8_555 no C11 C12 1.47(2) . . no C11 C14 1.49(2) . . no C12 C12 1.48(2) . 12_565 no C12 C17 1.30(2) . . no C16 C17 1.468(16) . . no C16 C16 1.482(16) . 8_555 no C16 C16 1.294(13) . 12_565 no C17 C19 1.47(3) . . no C101 C107 1.503(10) . . no C101 C107 1.503(10) . 3_555 no C101 C107 1.503(10) . 5_555 no C102 C103 1.380(13) . . no C102 C107 1.406(15) . . no C103 C104 1.383(14) . . no C104 C105 1.383(17) . . no C105 C106 1.402(14) . . no C106 C107 1.371(13) . . no C101 H101 1.001(15) . . no C103 H103 0.950(11) . . no C104 H104 0.950(9) . . no C105 H105 0.950(10) . . no C106 H106 0.950(10) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C102 N1 C102 106.2(7) 3_555 . 5_555 yes C102 N1 C102 106.2(7) . . 3_555 yes C102 N1 C102 106.2(7) . . 5_555 yes C2 C1 C9 111.0(14) . . . no C2 C1 C5 119.0(12) . . . no C5 C1 C9 116.6(14) . . . no C1 C2 C2 123.8(9) . . 8_555 no C1 C2 C2 103.8(9) . . 12_565 no C2 C2 C2 120.0(8) 8_555 . 12_565 no C1 C5 C1 93.8(15) . . 12_565 no C1 C5 C14 126.3(13) 12_565 . . no C1 C5 C14 126.1(17) . . . no C7 C6 C11 110.4(19) . . . no C7 C6 C9 126.8(18) . . . no C9 C6 C11 108.9(16) . . . no C6 C7 C19 131.8(16) . . . no C6 C7 C6 84(2) . . 8_555 no C6 C7 C19 131.9(16) 8_555 . . no C6 C9 C9 99.8(15) . . 8_555 no C1 C9 C6 124.8(15) . . . no C1 C9 C9 125.1(16) . . 8_555 no C6 C11 C12 123.0(16) . . . no C6 C11 C14 135(2) . . . no C12 C11 C14 89.5(16) . . . no C12 C12 C17 114.1(13) 12_565 . . no C11 C12 C17 121.6(14) . . . no C11 C12 C12 114.3(15) . . 12_565 no C5 C14 C11 107.8(15) . . 12_565 no C5 C14 C11 108.0(18) . . . no C11 C14 C11 130(3) . . 12_565 no C16 C16 C17 113.4(9) 8_555 . . no C16 C16 C17 115.2(10) 12_565 . . no C16 C16 C16 120.0(8) 8_555 . 12_565 no C16 C17 C19 92.1(14) . . . no C12 C17 C16 129.6(12) . . . no C12 C17 C19 119.4(15) . . . no C7 C19 C17 112.3(17) . . . no C7 C19 C17 112.2(17) . . 8_555 no C17 C19 C17 128.9(19) . . 8_555 no C107 C101 C107 104.4(8) . . 3_555 no C107 C101 C107 104.4(8) . . 5_555 no C107 C101 C107 104.4(8) 3_555 . 5_555 no N1 C102 C103 127.2(10) . . . yes N1 C102 C107 112.6(8) . . . yes C103 C102 C107 120.2(8) . . . no C102 C103 C104 119.2(10) . . . no C103 C104 C105 120.0(9) . . . no C104 C105 C106 121.7(9) . . . no C105 C106 C107 117.5(10) . . . no C101 C107 C102 114.1(8) . . . no C101 C107 C106 124.6(11) . . . no C102 C107 C106 121.3(8) . . . no C107 C101 H101 114.1(7) . . . no C107 C101 H101 114.1(7) 3_555 . . no C107 C101 H101 114.1(7) 5_555 . . no C102 C103 H103 120.4(10) . . . no C104 C103 H103 120.4(10) . . . no C103 C104 H104 120.0(11) . . . no C105 C104 H104 119.9(9) . . . no C104 C105 H105 119.1(10) . . . no C106 C105 H105 119.1(12) . . . no C105 C106 H106 121.3(10) . . . no C107 C106 H106 121.2(10) . . . no 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 C5 C1 C2 C2 -136.7(14) . . . 8_555 no C5 C1 C2 C2 4.9(16) . . . 12_565 no C9 C1 C2 C2 2.8(17) . . . 8_555 no C9 C1 C2 C2 144.4(12) . . . 12_565 no C2 C1 C5 C14 134.6(14) . . . . no C2 C1 C5 C1 -6.9(18) . . . 12_565 no C9 C1 C5 C14 -3(2) . . . . no C9 C1 C5 C1 -144.3(16) . . . 12_565 no C2 C1 C9 C6 -140.8(14) . . . . no C2 C1 C9 C9 -3(2) . . . 8_555 no C5 C1 C9 C6 0(2) . . . . no C5 C1 C9 C9 137.8(18) . . . 8_555 no C1 C2 C2 C2 135.9(10) . . 8_555 3_665 no C1 C2 C2 C1 0.0(15) . . 8_555 8_555 no C1 C2 C2 C2 -143.4(10) . . 12_565 5_565 no C1 C2 C2 C1 0.0(11) . . 12_565 12_565 no C1 C5 C14 C11 7(2) . . . . no C1 C5 C14 C11 -136.9(15) . . . 12_565 no C1 C5 C14 C11 136.8(19) 12_565 . . . no C9 C6 C7 C19 -125(3) . . . . no C9 C6 C7 C6 17.9(16) . . . 8_555 no C11 C6 C7 C19 10(3) . . . . no C11 C6 C7 C6 153.1(13) . . . 8_555 no C7 C6 C9 C1 132.8(18) . . . . no C7 C6 C9 C9 -13.4(19) . . . 8_555 no C11 C6 C9 C1 -3(2) . . . . no C11 C6 C9 C9 -149.2(14) . . . 8_555 no C7 C6 C11 C12 -4(2) . . . . no C7 C6 C11 C14 -133(2) . . . . no C9 C6 C11 C12 139.2(15) . . . . no C9 C6 C11 C14 10(3) . . . . no C6 C7 C19 C17 -14(3) . . . . no C6 C7 C19 C17 141(2) . . . 8_555 no C6 C7 C19 C17 -141(2) 8_555 . . . no C1 C9 C9 C1 0(3) . . 8_555 8_555 no C1 C9 C9 C6 -146.1(17) . . 8_555 8_555 no C6 C9 C9 C1 146.1(17) . . 8_555 8_555 no C6 C9 C9 C6 0.0(14) . . 8_555 8_555 no C6 C11 C12 C17 6(2) . . . . no C6 C11 C12 C12 -138.0(17) . . . 12_565 no C14 C11 C12 C17 152.0(14) . . . . no C14 C11 C12 C12 8.5(16) . . . 12_565 no C6 C11 C14 C5 -12(3) . . . . no C6 C11 C14 C11 121(3) . . . 12_565 no C12 C11 C14 C5 -151.8(15) . . . . no C12 C11 C14 C11 -18(2) . . . 12_565 no C11 C12 C17 C16 -130.7(14) . . . . no C11 C12 C17 C19 -9(2) . . . . no C12 C12 C17 C16 13(2) 12_565 . . . no C12 C12 C17 C19 134.2(18) 12_565 . . . no C11 C12 C12 C11 0(2) . . 12_565 12_565 no C11 C12 C12 C17 146.3(16) . . 12_565 12_565 no C17 C12 C12 C11 -146.3(16) . . 12_565 12_565 no C17 C12 C12 C17 0(2) . . 12_565 12_565 no C16 C16 C17 C12 130.7(17) 8_555 . . . no C16 C16 C17 C19 -1.2(13) 8_555 . . . no C16 C16 C17 C12 -13(2) 12_565 . . . no C16 C16 C17 C19 -144.8(13) 12_565 . . . no C17 C16 C16 C16 -141.7(9) . . 8_555 3_665 no C17 C16 C16 C17 0.0(12) . . 8_555 8_555 no C17 C16 C16 C16 141.1(10) . . 12_565 5_565 no C17 C16 C16 C17 0.0(14) . . 12_565 12_565 no C12 C17 C19 C7 13(3) . . . . no C12 C17 C19 C17 -136(2) . . . 8_555 no C16 C17 C19 C7 151.3(18) . . . . no C16 C17 C19 C17 2(2) . . . 8_555 no H101 C101 C107 C102 -180.0(3) . . . . no H101 C101 C107 C106 0.0(6) . . . . no N1 C102 C103 H103 0.1(10) . . . . no C107 C102 C103 H103 -180.0(6) . . . . no C102 C103 C104 H104 -180.0(6) . . . . no H103 C103 C104 C105 180(4) . . . . no H103 C103 C104 H104 -0.1(11) . . . . no C103 C104 C105 H105 -180.0(6) . . . . no H104 C104 C105 C106 180(3) . . . . no H104 C104 C105 H105 0.1(11) . . . . no C104 C105 C106 H106 -179.9(7) . . . . no H105 C105 C106 C107 179.9(15) . . . . no H105 C105 C106 H106 0.0(11) . . . . no H106 C106 C107 C101 -0.1(10) . . . . no H106 C106 C107 C102 180.0(5) . . . . no # End of Crystallographic Information File