# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Carreon, Olinda Y.' 'Coulon, Claude' 'Penicaud, Alain' 'Perrier, Aurelie' 'Watkin, D.' _publ_contact_author_name 'Dr Alain Penicaud' _publ_contact_author_address ; Centre de Recherche Paul Pascal UPR 8641 CNRS, Universite de Bordeaux-I Av Schweitzer 33600 Pessac FRANCE ; _publ_contact_author_email 'PENICAUD@CRPP.U-BORDEAUX.FR' _publ_contact_author_phone ' 33 5 56 84 56 71 ' _publ_contact_author_fax ' 33 5 56 84 56 00 ' _publ_requested_journal 'test' _publ_requested_category ? _publ_requested_coeditor_name ' Prof Stephen Mann ' _publ_section_title ; Supramolecular Fullerene Chemistry: Synthesis, Crystal Structure and Potassium Intercalation of [(C60)][(C6H5)2] ; data_CRYSTALS_cif_1 _database_code_CSD 170506 _audit_creation_date 98-12-31 _audit_creation_method CRYSTALS_ver_07-07-97 #========================================================================== # Structural resolution at 293 K #========================================================================== # #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-nonius CAD4 ' _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment noref #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 10.424(5) _cell_angle_alpha 90 _cell_length_b 16.932(9) _cell_angle_beta 100.8(1) _cell_length_c 10.320(5) _cell_angle_gamma 90 _cell_volume 1789.3 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/m 1 ' 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' '-x,y,-z' 'x,-y,z' '-x+1/2,y+1/2,-z' 'x+1/2,-y+1/2,z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C72 H10 ' _chemical_formula_moiety ' C60, C12 H10 ' _chemical_compound_source ; ? ; _chemical_formula_weight 874.88 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3 _cell_measurement_theta_max 13 _cell_measurement_temperature 293 _cell_formula_units_Z 2 _exptl_crystal_description ' block ' _exptl_crystal_colour ' black ' _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 846.165 _exptl_absorpt_coefficient_mu 0.092 # Sheldrick geometric definitions 0.98 0.99 _diffrn_measurement_device_type ; Enraf-Nonius CAD4 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_data_reduction ; RC93 (Watkin, Prout & Lilley, 1994) ; _computing_cell_refinement ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_structure_solution ; STRUCTURE SOLUTION ; _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; Azimutal absorption correction (North et al, 1968) ; _exptl_absorpt_correction_T_min 0.99 _exptl_absorpt_correction_T_max 0.99 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 3 _diffrn_standards_decay_% 1.87 _diffrn_ambient_temperature 293 _diffrn_reflns_number 2228 _reflns_number_total 2228 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 2228 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 2126 _diffrn_measured_fraction_theta_max 1.000 _reflns_number_gt 883 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.84 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _refine_diff_density_min -0.10 _refine_diff_density_max 0.13 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 883 _refine_ls_number_parameters 297 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0463 _refine_ls_goodness_of_fit_ref 1.0899 _refine_ls_shift/su_max 0.038629 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, Carruthers & Watkin , 1979, 0.808 0.270 0.576 -.322E-010.172 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; User-defined structure solution reference Enraf-Nonius, (1989) Cad4 Express. North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 Watkin, D.J., Prout, C.K., Carruthers, J.R., Betteridge, P.W. & Cooper R.I. (2001) CRYSTALS Issue 11. Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type C1 C 0.2798(6) 1.0172(5) 0.6996(4) 0.1081 0.5000 Uani C2 C 0.3968(6) 0.9987(5) 0.6555(3) 0.1055 0.5000 Uani C3 C 0.5028(9) 1.0568(6) 0.6763(6) 0.1349 0.5000 Uani C4 C 0.489(1) 1.1289(5) 0.7342(6) 0.1229 0.5000 Uani C5 C 0.369(1) 1.1448(4) 0.7752(8) 0.1329 0.5000 Uani C6 C 0.2679(8) 1.0899(5) 0.7581(8) 0.1184 0.5000 Uani C7 C 0.1943(5) 1.0801(5) 0.8676(8) 0.1217 0.5000 Uani C8 C 0.1635(3) 0.9966(9) 0.8735(7) 0.1362 0.5000 Uani C9 C 0.2203(5) 0.9582(4) 0.7632(6) 0.0931 0.5000 Uani C10 C 0.2753(7) 0.8871(4) 0.7774(6) 0.0888 0.5000 Uani C11 C 0.3949(8) 0.8713(4) 0.7332(6) 0.1053 0.5000 Uani C12 C 0.4561(7) 0.9228(5) 0.6764(5) 0.1055 0.5000 Uani C13 C 0.5996(6) 0.9285(5) 0.7149(6) 0.1047 0.5000 Uani C14 C 0.6294(7) 1.0144(7) 0.7129(6) 0.1410 0.5000 Uani C15 C 0.7253(9) 1.0468(6) 0.8010(9) 0.1549 0.5000 Uani C16 C 0.711(1) 1.1243(5) 0.8672(9) 0.1405 0.5000 Uani C17 C 0.5938(12) 1.1628(5) 0.8300(9) 0.1496 0.5000 Uani C18 C 0.5411(8) 1.1998(2) 0.9324(8) 0.1077 0.5000 Uani C19 C 0.4014(11) 1.1906(4) 0.898(1) 0.1414 0.5000 Uani C20 C 0.668(1) 0.8207(4) 1.008(1) 0.1506 0.5000 Uani C21 C 0.7733(8) 0.8775(6) 1.0258(11) 0.1468 0.5000 Uani C22 C 0.7715(6) 0.9177(6) 0.9006(8) 0.1197 0.5000 Uani C23 C 0.7983(4) 0.997(1) 0.8921(7) 0.1344 0.5000 Uani C24 C 0.8318(4) 1.0411(5) 1.0179(9) 0.1284 0.5000 Uani C25 C 0.7765(8) 1.1174(6) 0.9997(11) 0.1352 0.5000 Uani C26 C 0.2749(6) 0.8480(4) 0.8979(7) 0.0947 0.5000 Uani C27 C 0.3950(9) 0.8054(3) 0.9421(8) 0.1073 0.5000 Uani C28 C 0.4711(9) 0.8185(3) 0.8381(8) 0.1093 0.5000 Uani C29 C 0.6047(11) 0.8253(4) 0.8745(9) 0.1424 0.5000 Uani C30 C 0.6616(8) 0.8849(5) 0.7994(9) 0.1232 0.5000 Uani C41 C 1.0000 0.95632(19) 0.5000 0.0445 1.0000 Uani C42 C 0.9240(3) 0.91330(18) 0.5697(3) 0.0774 1.0000 Uani C43 C 0.9247(4) 0.8324(2) 0.5697(3) 0.0963 1.0000 Uani C44 C 1.0000 0.7914(3) 0.5000 0.0881 1.0000 Uani H421 H 0.8657 0.9423 0.6218 0.0778 1.0000 Uiso H431 H 0.8671 0.8031 0.6224 0.0938 1.0000 Uiso H441 H 1.0000 0.7319 0.5000 0.0945 1.0000 Uiso 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 0.114(1) 0.138(1) 0.0515(9) 0.005(1) -0.0385(9) 0.018(1) C2 0.146(1) 0.133(1) 0.0281(9) -0.0129 -0.0098(9) 0.0107 C3 0.183(1) 0.183(1) 0.0496(9) 0.038(1) 0.050(1) -0.001(1) C4 0.203(1) 0.100(1) 0.0615(9) 0.0538(9) 0.016(1) -0.034(1) C5 0.177(1) 0.078(1) 0.117(1) 0.0654(9) -0.042(1) 0.010(1) C6 0.122(1) 0.101(1) 0.101(1) 0.030(1) -0.0615(9) 0.029(1) C7 0.0601(9) 0.161(1) 0.124(1) -0.026(1) -0.0335(9) 0.0709(9) C8 0.0298(9) 0.202(1) 0.162(1) -0.017(1) -0.0210(9) -0.003(1) C9 0.0707(9) 0.109(1) 0.078(1) 0.006(1) -0.0403(9) -0.0169(9) C10 0.084(1) 0.080(1) 0.092(1) -0.0172(9) -0.0125(9) -0.0475(9) C11 0.140(1) 0.108(1) 0.064(1) -0.0526(9) 0.010(1) -0.031(1) C12 0.141(1) 0.132(1) 0.0354(9) -0.0374(9) -0.0042(9) -0.005(1) C13 0.0776(9) 0.178(1) 0.0638(9) -0.0652(9) 0.0272(9) 0.024(1) C14 0.163(1) 0.210(1) 0.0769(9) 0.007(1) 0.0910(9) -0.015(1) C15 0.156(1) 0.204(1) 0.144(1) 0.001(1) 0.1279(9) -0.055(1) C16 0.156(1) 0.131(1) 0.149(1) 0.031(1) 0.067(1) -0.0933(9) C17 0.208(1) 0.109(1) 0.136(1) 0.067(1) 0.042(1) -0.064(1) C18 0.156(1) 0.0235(9) 0.129(1) 0.0268(9) -0.011(1) -0.023(1) C19 0.198(1) 0.0498(9) 0.159(1) 0.035(1) -0.014(1) 0.052(1) C20 0.176(1) 0.089(1) 0.183(1) 0.002(1) 0.023(1) 0.1081(9) C21 0.109(1) 0.162(1) 0.162(1) -0.008(1) 0.008(1) 0.103(1) C22 0.0729(9) 0.190(1) 0.106(1) -0.027(1) 0.0418(9) 0.052(1) C23 0.0614(9) 0.219(1) 0.142(1) -0.041(1) 0.0696(9) -0.011(1) C24 0.0335(9) 0.176(1) 0.181(1) -0.036(1) 0.0334(9) -0.0365(9) C25 0.095(1) 0.144(1) 0.178(1) -0.010(1) 0.056(1) -0.0865(9) C26 0.101(1) 0.0795(9) 0.097(1) -0.0151(9) 0.0004(9) -0.0730(9) C27 0.160(1) 0.0296(9) 0.128(1) 0.001(1) 0.015(1) -0.0364(9) C28 0.157(1) 0.0455(9) 0.117(1) -0.0527(9) 0.004(1) 0.015(1) C29 0.185(1) 0.075(1) 0.162(1) -0.051(1) 0.020(1) 0.077(1) C30 0.107(1) 0.140(1) 0.139(1) -0.0799(9) 0.0658(9) 0.019(1) C41 0.0344(8) 0.0669(9) 0.0310(8) 0.0000 0.0030(7) 0.0000 C42 0.0888(9) 0.0751(9) 0.0808(8) 0.0289(8) 0.0483(8) 0.0235(8) C43 0.1220(9) 0.0837(9) 0.0962(9) 0.0350(8) 0.0540(8) 0.0132(9) C44 0.121(1) 0.0684(9) 0.0749(9) 0.0000 0.0175(9) 0.0000 _refine_ls_extinction_coef 264.0(207) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.414(7) yes C1 . C6 . 1.39(1) yes C1 . C9 . 1.403(8) yes C2 . C3 . 1.46(1) yes C2 . C12 . 1.425(9) yes C3 . C4 . 1.379(12) yes C3 . C14 . 1.488(11) yes C4 . C5 . 1.427(12) yes C4 . C17 . 1.445(11) yes C5 . C6 . 1.388(12) yes C5 . C19 . 1.474(11) yes C6 . C7 . 1.489(12) yes C7 . C8 . 1.453(17) yes C8 . C9 . 1.52(1) yes C9 . C10 . 1.329(9) yes C10 . C11 . 1.431(11) yes C10 . C26 . 1.410(9) yes C11 . C12 . 1.284(9) yes C11 . C28 . 1.509(11) yes C12 . C13 . 1.48(1) yes C13 . C14 . 1.487(13) yes C13 . C30 . 1.230(11) yes C14 . C15 . 1.336(11) yes C15 . C16 . 1.501(12) yes C15 . C23 . 1.385(13) yes C16 . C17 . 1.372(14) yes C16 . C25 . 1.415(13) yes C17 . C18 . 1.424(12) yes C18 . C19 . 1.441(12) yes C20 . C21 . 1.447(14) yes C20 . C29 . 1.416(11) yes C21 . C22 . 1.457(13) yes C22 . C23 . 1.372(16) yes C22 . C30 . 1.505(11) yes C23 . C24 . 1.484(11) yes C24 . C25 . 1.414(12) yes C26 . C27 . 1.443(11) yes C27 . C28 . 1.466(11) yes C28 . C29 . 1.378(12) yes C29 . C30 . 1.463(13) yes C41 . C42 . 1.375(3) yes C42 . C43 . 1.370(5) yes C42 . H421 . 1.010 no C43 . C44 . 1.350(4) yes C43 . H431 . 1.013 no C44 . H441 . 1.008 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . C6 . 119.3(7) yes C2 . C1 . C9 . 118.5(6) yes C6 . C1 . C9 . 110.2(7) yes C1 . C2 . C3 . 118.4(5) yes C1 . C2 . C12 . 121.8(5) yes C3 . C2 . C12 . 106.8(6) yes C2 . C3 . C4 . 121.6(7) yes C2 . C3 . C14 . 108.8(8) yes C4 . C3 . C14 . 118.3(9) yes C3 . C4 . C5 . 117.5(8) yes C3 . C4 . C17 . 121.7(9) yes C5 . C4 . C17 . 108.4(8) yes C4 . C5 . C6 . 121.6(8) yes C4 . C5 . C19 . 106.3(8) yes C6 . C5 . C19 . 120.6(10) yes C1 . C6 . C5 . 121.5(9) yes C1 . C6 . C7 . 109.4(8) yes C5 . C6 . C7 . 117.6(8) yes C6 . C7 . C8 . 106.9(7) yes C7 . C8 . C9 . 105.3(8) yes C1 . C9 . C8 . 108.3(8) yes C1 . C9 . C10 . 118.5(6) yes C8 . C9 . C10 . 121.6(8) yes C9 . C10 . C11 . 121.2(7) yes C9 . C10 . C26 . 116.7(7) yes C11 . C10 . C26 . 109.9(7) yes C10 . C11 . C12 . 123.7(8) yes C10 . C11 . C28 . 104.7(7) yes C12 . C11 . C28 . 119.3(8) yes C2 . C12 . C11 . 116.3(7) yes C2 . C12 . C13 . 111.7(7) yes C11 . C12 . C13 . 119.1(8) yes C12 . C13 . C14 . 105.3(8) yes C12 . C13 . C30 . 121.4(8) yes C14 . C13 . C30 . 120.9(7) yes C3 . C14 . C13 . 107.3(8) yes C3 . C14 . C15 . 119.3(10) yes C13 . C14 . C15 . 121.6(9) yes C14 . C15 . C16 . 122.9(10) yes C14 . C15 . C23 . 117.1(10) yes C16 . C15 . C23 . 108.5(10) yes C15 . C16 . C17 . 116.7(9) yes C15 . C16 . C25 . 107.2(10) yes C17 . C16 . C25 . 123.6(9) yes C4 . C17 . C16 . 121.2(10) yes C4 . C17 . C18 . 109.7(9) yes C16 . C17 . C18 . 116.6(8) yes C17 . C18 . C19 . 106.5(7) yes C5 . C19 . C18 . 109.1(9) yes C21 . C20 . C29 . 106.8(10) yes C20 . C21 . C22 . 108.4(9) yes C21 . C22 . C23 . 122.9(8) yes C21 . C22 . C30 . 109.0(9) yes C23 . C22 . C30 . 116.9(8) yes C15 . C23 . C22 . 123.3(8) yes C15 . C23 . C24 . 107.0(11) yes C22 . C23 . C24 . 117.1(9) yes C23 . C24 . C25 . 108.9(9) yes C16 . C25 . C24 . 108.4(9) yes C10 . C26 . C27 . 111.6(7) yes C26 . C27 . C28 . 104.4(6) yes C11 . C28 . C27 . 109.3(7) yes C11 . C28 . C29 . 121.0(8) yes C27 . C28 . C29 . 118.1(8) yes C20 . C29 . C28 . 121.4(9) yes C20 . C29 . C30 . 113.2(9) yes C28 . C29 . C30 . 113.7(8) yes C13 . C30 . C22 . 120.1(9) yes C13 . C30 . C29 . 125.4(8) yes C22 . C30 . C29 . 102.6(8) yes C41 . C42 . C43 . 121.7(3) yes C41 . C42 . H421 . 118.959 no C43 . C42 . H421 . 119.333 no C42 . C43 . C44 . 121.2(3) yes C42 . C43 . H431 . 119.027 no C44 . C43 . H431 . 119.808 no C43 . C44 . H441 . 120.878 no data_2 _database_code_CSD 170507 _audit_creation_date 98-12-31 _audit_creation_method CRYSTALS_ver_07-07-97 # C60/biphenyl at 293 and 155 K #========================================================================== # Structural resolution at 155 K #========================================================================== # #========================================================================== # Diffractometer details #========================================================================== _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS ' _computing_data_collection 'STOE software' _computing_data_reduction 'STOE software ' _computing_cell_refinement 'STOE software ' # end_choice #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment constr #**************************************************************************** _cell_length_a 10.3990(11) _cell_angle_alpha 90. _cell_length_b 16.9100(12) _cell_angle_beta 100.870(13) _cell_length_c 20.464(2) _cell_angle_gamma 90. _cell_volume 3534.0 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'I 1 2/a 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z+1/2' '-x+1/2,-y+1/2,-z+1/2' '-x+1/2,y,-z' 'x+1/2,-y,z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0..5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C72 H10 ' _chemical_formula_moiety ' C60, C12H10 ' _chemical_compound_source ; ? ; _chemical_formula_weight 874.88 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 155 _cell_formula_units_Z 4 _exptl_crystal_description ' prism ' _exptl_crystal_colour ' black ' _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1768.34 _exptl_absorpt_coefficient_mu 0.09 _exptl_absorpt_correction_type none # Sheldrick geometric definitions 1.00 1.00 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 0 _diffrn_reflns_number 4153 _reflns_number_total 4153 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 4153 # Number of reflections without Friedels Law is 0 _reflns_number_observed 1923 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 28.15 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.38 _refine_diff_density_max 1.10 _refine_ls_number_reflns 1923 _refine_ls_number_parameters 332 _refine_ls_R_factor_obs 0.081775 _refine_ls_wR_factor_obs 0.0711 _refine_ls_goodness_of_fit_obs 1.1612 _refine_ls_shift/su_max 0.241488 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters (Carruthers & Watkin, 1979) 0.321 -3.69 -1.00 -1.76 -0.437 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type C1 0.5224(5) 0.2741(3) 0.0999(2) 0.0295 1.0000 Uani C2 0.6375(6) 0.2545(4) 0.0761(2) 0.0449 1.0000 Uani C3 0.7442(6) 0.3169(6) 0.0859(3) 0.0620 1.0000 Uani C4 0.7314(8) 0.3851(5) 0.1163(3) 0.0597 1.0000 Uani C5 0.6198(7) 0.4012(4) 0.1376(3) 0.0550 1.0000 Uani C6 0.5162(5) 0.3499(3) 0.1303(3) 0.0315 1.0000 Uani C7 0.4455(6) 0.3385(5) 0.1872(4) 0.0749 1.0000 Uani C8 0.4098(4) 0.2485(4) 0.1874(3) 0.0448 1.0000 Uani C9 0.4610(5) 0.2146(3) 0.1324(3) 0.0350 1.0000 Uani C10 0.5159(5) 0.1392(3) 0.1386(3) 0.0371 1.0000 Uani C11 0.6363(7) 0.1247(4) 0.1133(3) 0.0551 1.0000 Uani C12 0.6971(7) 0.1809(4) 0.0833(3) 0.0569 1.0000 Uani C13 0.8387(6) 0.1882(6) 0.1001(3) 0.0585 1.0000 Uani C14 0.8696(7) 0.2690(6) 0.1010(3) 0.0683 1.0000 Uani C15 0.9672(7) 0.2971(5) 0.1434(3) 0.0656 1.0000 Uani C16 0.9544(7) 0.3774(5) 0.1799(3) 0.0633 1.0000 Uani C17 0.8481(9) 0.4158(5) 0.1673(4) 0.0758 1.0000 Uani C18 0.7978(7) 0.4515(3) 0.2173(3) 0.0476 1.0000 Uani C19 0.6558(9) 0.4445(3) 0.2002(4) 0.0774 1.0000 Uani C20 0.5857(8) 0.4317(4) 0.2523(6) 0.0760 1.0000 Uani C21 0.4766(8) 0.3739(6) 0.2443(4) 0.0834 1.0000 Uani C22 0.4768(6) 0.3331(5) 0.3046(3) 0.0575 1.0000 Uani C23 0.4520(5) 0.2510(5) 0.3089(3) 0.0495 1.0000 Uani C24 0.4161(5) 0.2071(5) 0.2466(4) 0.0568 1.0000 Uani C25 0.4726(5) 0.1303(4) 0.2525(3) 0.0458 1.0000 Uani C26 0.5220(5) 0.0966(3) 0.1997(3) 0.0364 1.0000 Uani C27 0.6425(6) 0.0537(3) 0.2170(3) 0.0380 1.0000 Uani C28 0.7196(8) 0.0675(4) 0.1664(4) 0.0623 1.0000 Uani C29 0.6521(9) 0.4240(5) 0.3213(5) 0.0789 1.0000 Uani C30 0.9102(7) 0.1359(5) 0.1450(4) 0.0651 1.0000 Uani C41 0.2500 0.1996(4) 0.0000 0.0149 1.0000 Uani C42 0.3410(4) 0.1569(3) -0.0278(2) 0.0235 1.0000 Uani C43 0.3399(5) 0.0741(3) -0.0281(2) 0.0342 1.0000 Uani C44 0.2500 0.0339(5) 0.0000 0.0391 1.0000 Uani C45 0.2500 0.2876(4) 0.0000 0.0185 1.0000 Uani C46 0.3051(4) 0.3298(3) -0.0465(2) 0.0250 1.0000 Uani C47 0.3060(5) 0.4121(3) -0.0461(3) 0.0357 1.0000 Uani C48 0.2500 0.4531(5) 0.0000 0.0392 1.0000 Uani H2 0.4158(4) 0.1882(3) -0.0437(2) 0.038(7) 1.0000 Uiso H3 0.4077(5) 0.0505(3) -0.0514(2) 0.038(7) 1.0000 Uiso H4 0.2500 -0.0237(5) 0.0000 0.038(7) 1.0000 Uiso H6 0.3250(4) 0.2946(3) -0.0873(2) 0.038(7) 1.0000 Uiso H7 0.3465(5) 0.4457(3) -0.0802(3) 0.038(7) 1.0000 Uiso H8 0.2500 0.5074(5) 0.0000 0.038(7) 1.0000 Uiso 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 0.027(2) 0.030(3) 0.023(2) 0.0026(19) -0.0148(19) -0.001(2) C2 0.059(4) 0.062(4) 0.009(2) 0.001(2) -0.005(2) 0.017(3) C3 0.037(3) 0.134(8) 0.015(2) 0.039(4) 0.004(2) 0.001(4) C4 0.084(5) 0.059(5) 0.031(3) 0.025(3) -0.003(3) -0.021(4) C5 0.063(4) 0.028(3) 0.061(4) 0.031(3) -0.021(3) -0.009(3) C6 0.030(2) 0.031(3) 0.028(2) 0.009(2) -0.009(2) 0.010(2) C7 0.041(3) 0.105(7) 0.065(5) -0.024(4) -0.024(3) 0.062(4) C8 0.0079(19) 0.058(4) 0.063(4) 0.015(3) -0.007(2) -0.002(2) C9 0.026(2) 0.038(3) 0.032(3) 0.007(2) -0.018(2) -0.010(2) C10 0.043(3) 0.030(3) 0.030(3) -0.009(2) -0.014(2) -0.018(2) C11 0.086(5) 0.051(4) 0.028(3) -0.028(3) 0.010(3) -0.036(4) C12 0.075(5) 0.067(5) 0.025(3) -0.020(3) -0.001(3) 0.013(4) C13 0.040(3) 0.114(7) 0.026(3) -0.031(4) 0.017(2) 0.010(4) C14 0.056(4) 0.127(8) 0.030(3) 0.010(4) 0.029(3) -0.005(5) C15 0.051(4) 0.108(7) 0.048(4) 0.026(4) 0.036(3) 0.002(4) C16 0.058(4) 0.082(6) 0.052(4) 0.018(4) 0.013(3) -0.043(4) C17 0.090(6) 0.063(6) 0.072(5) 0.036(5) 0.009(5) -0.047(5) C18 0.073(4) 0.016(3) 0.046(3) 0.008(2) -0.011(3) -0.015(3) C19 0.093(6) 0.007(3) 0.100(6) 0.017(3) -0.063(5) -0.001(3) C20 0.056(4) 0.015(3) 0.154(9) -0.000(4) 0.013(5) 0.023(3) C21 0.075(5) 0.109(7) 0.066(5) -0.000(5) 0.011(4) 0.071(6) C22 0.039(3) 0.093(6) 0.049(3) 0.002(3) 0.029(3) 0.044(3) C23 0.020(2) 0.084(5) 0.049(3) -0.005(4) 0.020(2) -0.010(3) C24 0.016(2) 0.083(5) 0.074(4) -0.005(4) 0.015(3) -0.017(3) C25 0.022(3) 0.050(4) 0.066(4) 0.013(3) 0.008(3) -0.024(3) C26 0.036(3) 0.029(3) 0.039(3) 0.001(2) -0.006(2) -0.025(2) C27 0.052(3) 0.008(3) 0.049(3) -0.003(2) -0.005(3) -0.013(2) C28 0.071(5) 0.026(4) 0.089(5) -0.042(3) 0.012(4) -0.007(3) C29 0.099(7) 0.040(5) 0.097(6) -0.039(4) 0.015(5) 0.028(5) C30 0.069(5) 0.053(5) 0.090(6) -0.043(4) 0.057(5) -0.004(4) C41 0.016(3) 0.021(3) 0.007(2) 0.0000 0.001(2) 0.0000 C42 0.023(2) 0.025(3) 0.020(2) -0.0055(18) -0.0025(17) -0.0005(19) C43 0.049(3) 0.031(3) 0.024(2) -0.009(2) 0.010(2) 0.008(2) C44 0.064(5) 0.020(4) 0.033(4) 0.0000 0.007(4) 0.0000 C45 0.008(2) 0.027(4) 0.018(3) 0.0000 -0.004(2) 0.0000 C46 0.022(2) 0.031(3) 0.022(2) 0.0037(19) 0.0057(17) 0.0022(19) C47 0.045(3) 0.030(3) 0.034(3) 0.008(2) 0.015(2) -0.004(2) C48 0.062(5) 0.020(4) 0.034(4) 0.0000 0.005(4) 0.0000 _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . C2 . 1.415(8) yes C1 . C6 . 1.431(7) yes C1 . C9 . 1.422(7) yes C2 . C3 . 1.52(1) yes C2 . C12 . 1.386(9) yes C3 . C4 . 1.328(11) yes C3 . C14 . 1.52(1) yes C4 . C5 . 1.341(11) yes C4 . C17 . 1.53(1) yes C5 . C6 . 1.369(8) yes C5 . C19 . 1.463(11) yes C6 . C7 . 1.50(1) yes C7 . C8 . 1.567(11) yes C7 . C21 . 1.299(11) yes C8 . C9 . 1.449(9) yes C8 . C24 . 1.390(9) yes C9 . C10 . 1.393(8) yes C10 . C11 . 1.462(9) yes C10 . C26 . 1.434(8) yes C11 . C12 . 1.35(1) yes C11 . C28 . 1.585(11) yes C12 . C13 . 1.453(9) yes C13 . C14 . 1.403(12) yes C13 . C30 . 1.387(11) yes C14 . C15 . 1.29(1) yes C15 . C16 . 1.568(11) yes C15 . C23 4_655 1.419(9) yes C16 . C17 . 1.266(12) yes C16 . C25 4_655 1.453(9) yes C17 . C18 . 1.374(12) yes C18 . C19 . 1.457(11) yes C18 . C27 4_655 1.373(8) yes C19 . C20 . 1.416(13) yes C20 . C21 . 1.484(13) yes C20 . C29 . 1.457(13) yes C21 . C22 . 1.413(11) yes C22 . C23 . 1.418(11) yes C22 . C30 4_655 1.50(1) yes C23 . C24 . 1.462(9) yes C24 . C25 . 1.42(1) yes C25 . C26 . 1.403(9) yes C26 . C27 . 1.434(8) yes C27 . C28 . 1.44(1) yes C28 . C29 4_655 1.318(11) yes C29 . C30 4_655 1.446(12) yes C41 . C42 . 1.393(5) yes C41 . C42 5_555 1.393(5) yes C41 . C45 . 1.488(8) yes C42 . C43 . 1.401(7) yes C42 . H2 . 1.041 no C43 . C44 . 1.367(7) yes C43 . H3 . 1.005 no C44 . H4 . 0.973 no C45 . C46 . 1.396(6) yes C45 . C46 5_555 1.396(6) yes C46 . C47 . 1.391(7) yes C46 . H6 . 1.076 no C47 . C48 . 1.384(7) yes C47 . H7 . 1.048 no C48 . H8 . 0.919 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . C1 . C6 . 118.0(5) yes C2 . C1 . C9 . 118.7(5) yes C6 . C1 . C9 . 111.7(5) yes C1 . C2 . C3 . 115.9(6) yes C1 . C2 . C12 . 124.3(6) yes C3 . C2 . C12 . 108.0(6) yes C2 . C3 . C4 . 122.1(6) yes C2 . C3 . C14 . 103.6(7) yes C4 . C3 . C14 . 121.8(7) yes C3 . C4 . C5 . 119.8(7) yes C3 . C4 . C17 . 118.4(8) yes C5 . C4 . C17 . 109.4(7) yes C4 . C5 . C6 . 123.2(7) yes C4 . C5 . C19 . 107.0(7) yes C6 . C5 . C19 . 118.6(7) yes C1 . C6 . C5 . 121.1(6) yes C1 . C6 . C7 . 106.9(5) yes C5 . C6 . C7 . 119..1(6) yes C6 . C7 . C8 . 106.1(5) yes C6 . C7 . C21 . 124.3(9) yes C8 . C7 . C21 . 117.7(8) yes C7 . C8 . C9 . 105.1(5) yes C7 . C8 . C24 . 121.3(6) yes C9 . C8 . C24 . 120.9(6) yes C1 . C9 . C8 . 110.2(5) yes C1 . C9 . C10 . 118.5(5) yes C8 . C9 . C10 . 119.7(5) yes C9 . C10 . C11 . 119.0(5) yes C9 . C10 . C26 . 119.3(5) yes C11 . C10 . C26 . 108.9(5) yes C10 . C11 . C12 . 123.3(7) yes C10 . C11 . C28 . 104.7(5) yes C12 . C11 . C28 . 119.9(7) yes C2 . C12 . C11 . 116.2(7) yes C2 . C12 . C13 . 111.2(7) yes C11 . C12 . C13 . 119.5(7) yes C12 . C13 . C14 . 107.8(7) yes C12 . C13 . C30 . 119.7(8) yes C14 . C13 . C30 . 121.3(6) yes C3 . C14 . C13 . 109.3(7) yes C3 . C14 . C15 . 118.4(9) yes C13 . C14 . C15 . 121.0(8) yes C14 . C15 . C16 . 120.7(7) yes C14 . C15 . C23 4_655 122.6(8) yes C16 . C15 . C23 4_655 105.1(7) yes C15 . C16 . C17 . 119.8(7) yes C15 . C16 . C25 4_655 107.4(7) yes C17 . C16 .. C25 4_655 121.3(8) yes C4 . C17 . C16 . 120.9(9) yes C4 . C17 . C18 . 107.0(8) yes C16 . C17 . C18 . 120.9(8) yes C17 . C18 . C19 . 107.2(7) yes C17 . C18 . C27 4_655 122.4(7) yes C19 . C18 . C27 4_655 118.7(7) yes C5 . C19 . C18 . 109.3(8) yes C5 . C19 . C20 . 120.0(7) yes C18 . C19 . C20 . 118.3(7) yes C19 . C20 . C21 . 120.6(8) yes C19 . C20 . C29 . 121.8(7) yes C21 . C20 . C29 . 105.1(8) yes C7 . C21 . C20 . 117.2(10) yes C7 . C21 . C22 . 121.3(10) yes C20 . C21 . C22 . 110.5(8) yes C21 . C22 . C23 . 124.2(7) yes C21 . C22 . C30 4_655 107.5(8) yes C23 . C22 . C30 4_655 115.3(6) yes C15 4_655 C23 . C22 . 120.8(6) yes C15 4_655 C23 . C24 . 109.3(7) yes C22 . C23 . C24 . 117.6(6) yes C8 . C24 . C23 . 117.8(6) yes C8 . C24 . C25 . 119.0(6) yes C23 . C24 . C25 . 110.9(6) yes C16 4_655 C25 . C24 . 107.3(7) yes C16 4_655 C25 . C26 . 119.7(6) yes C24 . C25 . C26 . 120.7(6) yes C10 . C26 . C25 . 120.4(6) yes C10 . C26 . C27 . 111.3(5) yes C25 . C26 . C27 . 116.4(5) yes C18 4_655 C27 . C26 . 119.1(6) yes C18 4_655 C27 . C28 . 120.2(6) yes C26 . C27 . C28 . 108.6(5) yes C11 . C28 . C27 . 106.5(6) yes C11 . C28 . C29 4_655 117.8(8) yes C27 . C28 . C29 4_655 124.1(8) yes C20 . C29 . C28 4_655 116.9(9) yes C20 . C29 . C30 4_655 110.6(8) yes C28 4_655 C29 . C30 4_655 120.9(9) yes C13 . C30 . C22 4_655 118.9(7) yes C13 . C30 . C29 4_655 122.1(7) yes C22 4_655 C30 . C29 4_655 106.3(8) yes C42 . C41 . C42 5_555 117.7(6) yes C42 . C41 . C45 . 121.2(3) yes C42 5_555 C41 . C45 . 121.2(3) yes C41 . C42 . C43 . 120.9(5) yes C41 . C42 . H2 . 118.0(3) no C43 . C42 . H2 . 120.8(3) no C42 . C43 . C44 . 120.0(5) yes C42 . C43 . H3 . 113.2(3) no C44 . C43 . H3 . 126.8(4) no C43 . C44 . C43 5_555 120.4(7) yes C43 . C44 . H4 . 119.8(4) no C43 5_555 C44 . H4 . 119.8(4) no C41 . C45 . C46 . 120.8(3) yes C41 . C45 . C46 5_555 120.8(3) yes C46 . C45 . C46 5_555 118.4(6) yes C45 . C46 . C47 . 120.7(5) yes C45 . C46 . H6 . 114.1(3) no C47 . C46 . H6 . 123.8(3) no C46 . C47 . C48 . 120.1(5) yes C46 . C47 . H7 . 122.8(3) no C48 . C47 . H7 . 117.1(4) no C47 . C48 . C47 5_555 119.9(7) yes C47 . C48 . H8 . 120.1(4) no C47 5_555 C48 . H8 . 120.1(4) no