Supplementary Material for Organic & Biomolecular Chemistry This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 loop_ _publ_author_name _publ_author_address 'Tony Farrell' ; Bergische Universit\"at Wuppertal Makromolekulare Chemie Gaussstrasse 20 D-42097 Wuppertal Germany ; 'Askin Bilge' ; Max-Planck-Institut f\"ur Kohlenforschung Kaiser-Wilhelm-Platz 1 D-45470 M\"ulheim an der Ruhr Germany ; 'David J. Brauer' '' 'Frank Galbrecht' '' 'Christian W. Lehmann' '' ; B.S.Nehls ; '' 'Ulrich Scherf' '' _publ_contact_author_name 'Tony Farrell' _publ_contact_author_address ; Makromolekulare Chemie Institut f\"ur Polymertechnologie Gauss-Str. 20 Wuppertal 42097 GERMANY ; _publ_contact_author_email FARRELL@UNI-WUPPERTAL.DE _publ_section_title ; Synthesis and Spectroscopy of an Oligophenyl Based Cruciform with Remarkable p-p Assisted Folding ; data_4901 _database_code_depnum_ccdc_archive 'CCDC 274216' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source solvent _chemical_formula_moiety 'C32 H34' _chemical_formula_sum 'C32 H34' _chemical_formula_weight 418.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.68070(10) _cell_length_b 13.23650(10) _cell_length_c 24.2500(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.2000(10) _cell_angle_gamma 90.00 _cell_volume 2461.55(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 69.19 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method none _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.471 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'XPREP, Siemens (1995)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.95 _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART' _diffrn_measurement_method 'CCD \w-scan' _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 15596 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 69.16 _reflns_number_total 4157 _reflns_number_gt 4081 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART software (Siemens, 1995)' _computing_cell_refinement 'SMART software (Siemens, 1995)' _computing_data_reduction 'SAINT software (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.8977P] 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 SHELXL _refine_ls_extinction_coef 0.0070(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4157 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0431 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 C10 C -0.07930(17) 0.27410(8) -0.03854(5) 0.0251(3) Uani 1 1 d . . . C11 C 0.24615(16) 0.08426(8) 0.07298(4) 0.0215(3) Uani 1 1 d . . . C12 C 0.06680(17) 0.07135(8) 0.06810(5) 0.0236(3) Uani 1 1 d . . . H12 H 0.0146 0.0203 0.0892 0.028 Uiso 1 1 calc R . . C13 C -0.03818(17) 0.13140(9) 0.03298(5) 0.0241(3) Uani 1 1 d . . . H13 H -0.1607 0.1207 0.0306 0.029 Uiso 1 1 calc R . . C14 C 0.03299(17) 0.20712(8) 0.00119(4) 0.0222(3) Uani 1 1 d . . . C15 C 0.21292(17) 0.22020(9) 0.00652(5) 0.0240(3) Uani 1 1 d . . . H15 H 0.2652 0.2715 -0.0144 0.029 Uiso 1 1 calc R . . C16 C 0.31768(17) 0.16047(9) 0.04144(4) 0.0237(3) Uani 1 1 d . . . H16 H 0.4401 0.1714 0.0440 0.028 Uiso 1 1 calc R . . C17 C -0.0258(2) 0.25632(11) -0.09800(5) 0.0407(4) Uani 1 1 d . . . H17A H 0.0977 0.2734 -0.1005 0.061 Uiso 1 1 calc R . . H17B H -0.0968 0.2990 -0.1235 0.061 Uiso 1 1 calc R . . H17C H -0.0441 0.1852 -0.1079 0.061 Uiso 1 1 calc R . . C18 C -0.27309(19) 0.25237(10) -0.03617(6) 0.0368(3) Uani 1 1 d . . . H18A H -0.2962 0.1820 -0.0468 0.055 Uiso 1 1 calc R . . H18B H -0.3390 0.2975 -0.0617 0.055 Uiso 1 1 calc R . . H18C H -0.3090 0.2636 0.0015 0.055 Uiso 1 1 calc R . . C19 C -0.04713(18) 0.38526(9) -0.02340(5) 0.0279(3) Uani 1 1 d . . . H19A H -0.0818 0.3975 0.0143 0.042 Uiso 1 1 calc R . . H19B H -0.1160 0.4285 -0.0492 0.042 Uiso 1 1 calc R . . H19C H 0.0770 0.4009 -0.0257 0.042 Uiso 1 1 calc R . . C21 C 0.36140(17) 0.01651(8) 0.10781(5) 0.0232(3) Uani 1 1 d . . . C22 C 0.32102(17) -0.01440(8) 0.16135(5) 0.0244(3) Uani 1 1 d . . . C23 C 0.42748(19) -0.08682(9) 0.18845(5) 0.0305(3) Uani 1 1 d . . . H23 H 0.3986 -0.1099 0.2239 0.037 Uiso 1 1 calc R . . C24 C 0.57322(19) -0.12569(9) 0.16517(6) 0.0344(3) Uani 1 1 d . . . H24 H 0.6420 -0.1757 0.1841 0.041 Uiso 1 1 calc R . . C25 C 0.61831(19) -0.09112(10) 0.11394(6) 0.0329(3) Uani 1 1 d . . . H25 H 0.7213 -0.1149 0.0983 0.040 Uiso 1 1 calc R . . C26 C 0.51178(18) -0.02164(9) 0.08578(5) 0.0275(3) Uani 1 1 d . . . H26 H 0.5422 0.0007 0.0504 0.033 Uiso 1 1 calc R . . C31 C 0.17342(17) 0.02768(9) 0.19141(4) 0.0248(3) Uani 1 1 d . . . C32 C 0.15404(17) 0.13168(9) 0.20203(4) 0.0242(3) Uani 1 1 d . . . C33 C 0.01357(18) 0.16296(10) 0.23213(5) 0.0301(3) Uani 1 1 d . . . H33 H 0.0001 0.2329 0.2397 0.036 Uiso 1 1 calc R . . C34 C -0.10632(19) 0.09535(11) 0.25121(5) 0.0351(3) Uani 1 1 d . . . H34 H -0.2006 0.1187 0.2715 0.042 Uiso 1 1 calc R . . C35 C -0.08784(19) -0.00661(11) 0.24054(5) 0.0361(3) Uani 1 1 d . . . H35 H -0.1699 -0.0538 0.2532 0.043 Uiso 1 1 calc R . . C36 C 0.05077(19) -0.03932(10) 0.21138(5) 0.0314(3) Uani 1 1 d . . . H36 H 0.0633 -0.1096 0.2046 0.038 Uiso 1 1 calc R . . C40 C 0.59409(17) 0.46113(9) 0.12848(5) 0.0239(3) Uani 1 1 d . . . C41 C 0.27313(17) 0.21090(8) 0.18251(4) 0.0224(3) Uani 1 1 d . . . C42 C 0.45376(16) 0.20605(8) 0.18902(4) 0.0225(3) Uani 1 1 d . . . H42 H 0.5073 0.1481 0.2057 0.027 Uiso 1 1 calc R . . C43 C 0.55749(17) 0.28455(8) 0.17155(4) 0.0225(3) Uani 1 1 d . . . H43 H 0.6807 0.2788 0.1763 0.027 Uiso 1 1 calc R . . C44 C 0.48486(16) 0.37172(8) 0.14721(4) 0.0212(3) Uani 1 1 d . . . C45 C 0.30393(17) 0.37542(9) 0.14050(5) 0.0245(3) Uani 1 1 d . . . H45 H 0.2501 0.4333 0.1238 0.029 Uiso 1 1 calc R . . C46 C 0.20041(17) 0.29729(9) 0.15739(5) 0.0253(3) Uani 1 1 d . . . H46 H 0.0773 0.3024 0.1518 0.030 Uiso 1 1 calc R . . C47 C 0.5510(2) 0.55538(9) 0.16248(5) 0.0338(3) Uani 1 1 d . . . H47A H 0.5788 0.5421 0.2018 0.051 Uiso 1 1 calc R . . H47B H 0.4266 0.5711 0.1568 0.051 Uiso 1 1 calc R . . H47C H 0.6202 0.6128 0.1506 0.051 Uiso 1 1 calc R . . C48 C 0.54856(18) 0.48249(10) 0.06716(5) 0.0282(3) Uani 1 1 d . . . H48A H 0.6181 0.5396 0.0551 0.042 Uiso 1 1 calc R . . H48B H 0.4243 0.4989 0.0619 0.042 Uiso 1 1 calc R . . H48C H 0.5742 0.4226 0.0453 0.042 Uiso 1 1 calc R . . C49 C 0.78923(18) 0.44055(10) 0.13567(5) 0.0312(3) Uani 1 1 d . . . H49A H 0.8183 0.3813 0.1138 0.047 Uiso 1 1 calc R . . H49B H 0.8212 0.4278 0.1747 0.047 Uiso 1 1 calc R . . H49C H 0.8537 0.4994 0.1231 0.047 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 C10 0.0310(8) 0.0205(6) 0.0235(6) -0.0004(4) -0.0011(5) 0.0027(5) C11 0.0268(7) 0.0213(5) 0.0163(5) -0.0038(4) 0.0011(4) -0.0002(5) C12 0.0294(8) 0.0212(5) 0.0201(5) 0.0007(4) 0.0011(5) -0.0045(5) C13 0.0247(7) 0.0235(6) 0.0238(6) -0.0020(4) -0.0008(5) -0.0023(5) C14 0.0288(8) 0.0194(5) 0.0182(5) -0.0044(4) 0.0001(4) 0.0009(5) C15 0.0292(8) 0.0227(6) 0.0204(6) 0.0012(4) 0.0048(5) -0.0024(5) C16 0.0232(7) 0.0272(6) 0.0209(6) -0.0022(4) 0.0035(4) -0.0011(5) C17 0.0624(11) 0.0369(7) 0.0219(6) -0.0001(5) -0.0050(6) 0.0200(7) C18 0.0339(9) 0.0239(6) 0.0509(8) 0.0056(6) -0.0127(6) -0.0014(5) C19 0.0299(8) 0.0219(6) 0.0323(6) 0.0013(5) 0.0039(5) 0.0011(5) C21 0.0282(8) 0.0193(5) 0.0216(6) -0.0039(4) -0.0028(5) -0.0022(5) C22 0.0313(8) 0.0195(5) 0.0217(6) -0.0018(4) -0.0040(5) -0.0040(5) C23 0.0429(9) 0.0226(6) 0.0249(6) 0.0005(5) -0.0079(5) -0.0026(5) C24 0.0424(9) 0.0229(6) 0.0359(7) -0.0045(5) -0.0147(6) 0.0067(5) C25 0.0313(9) 0.0301(6) 0.0364(7) -0.0112(5) -0.0068(5) 0.0052(5) C26 0.0313(8) 0.0262(6) 0.0245(6) -0.0063(5) -0.0019(5) 0.0003(5) C31 0.0308(8) 0.0283(6) 0.0147(5) 0.0024(4) -0.0045(5) -0.0039(5) C32 0.0246(7) 0.0304(6) 0.0172(5) 0.0004(4) -0.0023(4) -0.0005(5) C33 0.0280(8) 0.0383(7) 0.0239(6) -0.0012(5) 0.0014(5) -0.0001(5) C34 0.0273(8) 0.0553(9) 0.0229(6) 0.0021(6) 0.0024(5) -0.0044(6) C35 0.0365(9) 0.0520(8) 0.0193(6) 0.0073(5) -0.0022(5) -0.0171(6) C36 0.0409(9) 0.0339(7) 0.0187(6) 0.0044(5) -0.0046(5) -0.0104(6) C40 0.0272(7) 0.0246(6) 0.0198(6) 0.0011(4) 0.0006(5) 0.0011(5) C41 0.0265(7) 0.0237(6) 0.0170(5) -0.0043(4) 0.0011(4) 0.0007(5) C42 0.0267(7) 0.0216(6) 0.0189(5) -0.0010(4) -0.0021(4) 0.0032(5) C43 0.0216(7) 0.0259(6) 0.0197(5) -0.0028(4) -0.0016(4) 0.0018(5) C44 0.0254(7) 0.0233(6) 0.0149(5) -0.0034(4) 0.0005(4) 0.0017(5) C45 0.0273(8) 0.0226(6) 0.0236(6) 0.0004(4) 0.0014(5) 0.0063(5) C46 0.0223(7) 0.0279(6) 0.0256(6) -0.0027(5) 0.0007(5) 0.0047(5) C47 0.0476(10) 0.0249(6) 0.0292(6) -0.0012(5) 0.0057(6) -0.0043(6) C48 0.0279(8) 0.0339(7) 0.0230(6) 0.0045(5) 0.0021(5) 0.0044(5) C49 0.0287(8) 0.0355(7) 0.0289(6) 0.0086(5) -0.0024(5) -0.0040(5) _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 C10 C18 1.520(2) . ? C10 C19 1.5332(16) . ? C10 C14 1.5380(16) . ? C10 C17 1.5395(17) . ? C11 C12 1.3865(18) . ? C11 C16 1.3969(16) . ? C11 C21 1.4892(16) . ? C12 C13 1.3894(17) . ? C12 H12 0.9500 . N C13 C14 1.3945(17) . ? C13 H13 0.9500 . N C14 C15 1.3916(18) . ? C15 C16 1.3833(17) . ? C15 H15 0.9500 . N C16 H16 0.9500 . N C17 H17A 0.9800 . N C17 H17B 0.9800 . N C17 H17C 0.9800 . N C18 H18A 0.9800 . N C18 H18B 0.9800 . N C18 H18C 0.9800 . N C19 H19A 0.9800 . N C19 H19B 0.9800 . N C19 H19C 0.9800 . N C21 C26 1.3940(18) . ? C21 C22 1.4122(16) . ? C22 C23 1.3999(18) . ? C22 C31 1.4896(18) . ? C23 C24 1.381(2) . ? C23 H23 0.9500 . N C24 C25 1.386(2) . ? C24 H24 0.9500 . N C25 C26 1.3854(18) . ? C25 H25 0.9500 . N C26 H26 0.9500 . N C31 C36 1.3997(18) . ? C31 C32 1.4099(17) . ? C32 C33 1.3987(18) . ? C32 C41 1.4862(17) . ? C33 C34 1.3822(19) . ? C33 H33 0.9500 . N C34 C35 1.383(2) . ? C34 H34 0.9500 . N C35 C36 1.380(2) . ? C35 H35 0.9500 . N C36 H36 0.9500 . N C40 C49 1.5238(19) . ? C40 C44 1.5341(16) . ? C40 C48 1.5348(15) . ? C40 C47 1.5414(17) . ? C41 C42 1.3890(18) . ? C41 C46 1.3974(16) . ? C42 C43 1.3897(17) . ? C42 H42 0.9500 . N C43 C44 1.3979(16) . ? C43 H43 0.9500 . N C44 C45 1.3910(18) . ? C45 C46 1.3806(18) . ? C45 H45 0.9500 . N C46 H46 0.9500 . N C47 H47A 0.9800 . N C47 H47B 0.9800 . N C47 H47C 0.9800 . N C48 H48A 0.9800 . N C48 H48B 0.9800 . N C48 H48C 0.9800 . N C49 H49A 0.9800 . N C49 H49B 0.9800 . N C49 H49C 0.9800 . N 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 C18 C10 C19 108.52(10) . . ? C18 C10 C14 112.54(10) . . ? C19 C10 C14 109.02(10) . . ? C18 C10 C17 108.65(11) . . ? C19 C10 C17 108.85(10) . . ? C14 C10 C17 109.20(10) . . ? C12 C11 C16 117.48(11) . . ? C12 C11 C21 122.04(10) . . ? C16 C11 C21 120.39(11) . . ? C11 C12 C13 121.44(11) . . ? C11 C12 H12 119.3 . . N C13 C12 H12 119.3 . . N C12 C13 C14 121.20(12) . . ? C12 C13 H13 119.4 . . N C14 C13 H13 119.4 . . N C15 C14 C13 117.13(11) . . ? C15 C14 C10 120.38(11) . . ? C13 C14 C10 122.49(12) . . ? C16 C15 C14 121.76(11) . . ? C16 C15 H15 119.1 . . N C14 C15 H15 119.1 . . N C15 C16 C11 120.99(12) . . ? C15 C16 H16 119.5 . . N C11 C16 H16 119.5 . . N C10 C17 H17A 109.5 . . N C10 C17 H17B 109.5 . . N H17A C17 H17B 109.5 . . N C10 C17 H17C 109.5 . . N H17A C17 H17C 109.5 . . N H17B C17 H17C 109.5 . . N C10 C18 H18A 109.5 . . N C10 C18 H18B 109.5 . . N H18A C18 H18B 109.5 . . N C10 C18 H18C 109.5 . . N H18A C18 H18C 109.5 . . N H18B C18 H18C 109.5 . . N C10 C19 H19A 109.5 . . N C10 C19 H19B 109.5 . . N H19A C19 H19B 109.5 . . N C10 C19 H19C 109.5 . . N H19A C19 H19C 109.5 . . N H19B C19 H19C 109.5 . . N C26 C21 C22 118.46(11) . . ? C26 C21 C11 118.67(10) . . ? C22 C21 C11 122.80(12) . . ? C23 C22 C21 118.52(12) . . ? C23 C22 C31 117.82(11) . . ? C21 C22 C31 123.63(11) . . ? C24 C23 C22 121.92(12) . . ? C24 C23 H23 119.0 . . N C22 C23 H23 119.0 . . N C23 C24 C25 119.49(12) . . ? C23 C24 H24 120.3 . . N C25 C24 H24 120.3 . . N C26 C25 C24 119.39(13) . . ? C26 C25 H25 120.3 . . N C24 C25 H25 120.3 . . N C25 C26 C21 122.05(12) . . ? C25 C26 H26 119.0 . . N C21 C26 H26 119.0 . . N C36 C31 C32 118.39(12) . . ? C36 C31 C22 118.54(11) . . ? C32 C31 C22 123.05(11) . . ? C33 C32 C31 118.47(12) . . ? C33 C32 C41 117.63(11) . . ? C31 C32 C41 123.89(11) . . ? C34 C33 C32 122.05(13) . . ? C34 C33 H33 119.0 . . N C32 C33 H33 119.0 . . N C33 C34 C35 119.47(13) . . ? C33 C34 H34 120.3 . . N C35 C34 H34 120.3 . . N C36 C35 C34 119.48(13) . . ? C36 C35 H35 120.3 . . N C34 C35 H35 120.3 . . N C35 C36 C31 122.13(13) . . ? C35 C36 H36 118.9 . . N C31 C36 H36 118.9 . . N C49 C40 C44 112.26(10) . . ? C49 C40 C48 108.25(10) . . ? C44 C40 C48 109.28(10) . . ? C49 C40 C47 108.83(11) . . ? C44 C40 C47 109.19(10) . . ? C48 C40 C47 108.97(10) . . ? C42 C41 C46 117.37(11) . . ? C42 C41 C32 124.04(10) . . ? C46 C41 C32 118.56(11) . . ? C41 C42 C43 121.12(11) . . ? C41 C42 H42 119.4 . . N C43 C42 H42 119.4 . . N C42 C43 C44 121.58(12) . . ? C42 C43 H43 119.2 . . N C44 C43 H43 119.2 . . N C45 C44 C43 116.81(11) . . ? C45 C44 C40 119.83(10) . . ? C43 C44 C40 123.36(11) . . ? C46 C45 C44 121.81(11) . . ? C46 C45 H45 119.1 . . N C44 C45 H45 119.1 . . N C45 C46 C41 121.30(12) . . ? C45 C46 H46 119.3 . . N C41 C46 H46 119.3 . . N C40 C47 H47A 109.5 . . N C40 C47 H47B 109.5 . . N H47A C47 H47B 109.5 . . N C40 C47 H47C 109.5 . . N H47A C47 H47C 109.5 . . N H47B C47 H47C 109.5 . . N C40 C48 H48A 109.5 . . N C40 C48 H48B 109.5 . . N H48A C48 H48B 109.5 . . N C40 C48 H48C 109.5 . . N H48A C48 H48C 109.5 . . N H48B C48 H48C 109.5 . . N C40 C49 H49A 109.5 . . N C40 C49 H49B 109.5 . . N H49A C49 H49B 109.5 . . N C40 C49 H49C 109.5 . . N H49A C49 H49C 109.5 . . N H49B C49 H49C 109.5 . . N _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 69.16 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.222 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.043 ############################################################################ # # # # # ### # # ### ### # ### # # ### # # ### # ### # # # # # # # # # # # # # ## ## # ## # # # # # # # # # # ### # # ### ### # ### # # # ### # ## # ### ### # # # # # # # # # # # # # # # # # # ## # # # ### ### # # ### ### # # ### # # # # # # # # # # # # # # # # # ### ### ### # # # # # ## ## # # # # # # # # # # # # # # # ### # ### ### # ### # # # # # # # # # ## # # # # # # # # # # # ### # # # # # ### # # # # # ############################################################################ ############################################################################ # # # This Supplementary Material is written in the Crystallographic # # Information File (CIF) format. For further details see: S.R. Hall, # # F.H. Allen and I.D. Brown, Acta Cryst. (1991) A47, 655-685. # # # ############################################################################ data_4945 _database_code_depnum_ccdc_archive 'CCDC 274217' # # ############################################################################ _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'deuterated THF' _chemical_formula_moiety 'C52 H58' _chemical_formula_sum 'C52 H58' _chemical_formula_weight 682.98 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.1849(6) _cell_length_b 15.8390(4) _cell_length_c 10.0760(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.7280(10) _cell_angle_gamma 90.00 _cell_volume 4059.57(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 22661 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 31.51 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method none _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min 1 _exptl_absorpt_correction_T_max 1 _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '0.3 mm rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD \w-scan' _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 57798 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 31.66 _reflns_number_total 6800 _reflns_number_gt 4994 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect software (Nonius, 1998)' _computing_cell_refinement 'Denzo / Scalepack (Otwinowski 1997)' _computing_data_reduction 'Denzo / Scalepack (Otwinowski 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+3.7659P] 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_number_reflns 6800 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1529 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 C1 C -0.21059(8) 0.88208(12) 0.94437(18) 0.0369(4) Uani 1 1 d . . . H1A H -0.2177 0.8336 0.9978 0.055 Uiso 1 1 calc R . . H1B H -0.2294 0.9317 0.9662 0.055 Uiso 1 1 calc R . . H1C H -0.1727 0.8936 0.9668 0.055 Uiso 1 1 calc R . . C2 C -0.28894(6) 0.84869(11) 0.7564(2) 0.0322(4) Uani 1 1 d . . . H2A H -0.3012 0.8347 0.6593 0.048 Uiso 1 1 calc R . . H2B H -0.3063 0.9005 0.7761 0.048 Uiso 1 1 calc R . . H2C H -0.2975 0.8023 0.8117 0.048 Uiso 1 1 calc R . . C3 C -0.21766(6) 0.93774(9) 0.70726(18) 0.0272(3) Uani 1 1 d . . . H3A H -0.1799 0.9498 0.7316 0.041 Uiso 1 1 calc R . . H3B H -0.2370 0.9873 0.7270 0.041 Uiso 1 1 calc R . . H3C H -0.2287 0.9244 0.6097 0.041 Uiso 1 1 calc R . . C4 C -0.22925(6) 0.86210(9) 0.79120(15) 0.0210(3) Uani 1 1 d . . . C5 C 0.05347(6) 0.08518(10) 0.42190(16) 0.0259(3) Uani 1 1 d . . . H5A H 0.0164 0.0705 0.4124 0.039 Uiso 1 1 calc R . . H5B H 0.0739 0.0336 0.4191 0.039 Uiso 1 1 calc R . . H5C H 0.0567 0.1226 0.3469 0.039 Uiso 1 1 calc R . . C6 C 0.07001(6) 0.07107(9) 0.67662(16) 0.0224(3) Uani 1 1 d . . . H6A H 0.0844 0.0992 0.7642 0.034 Uiso 1 1 calc R . . H6B H 0.0899 0.0192 0.6715 0.034 Uiso 1 1 calc R . . H6C H 0.0330 0.0570 0.6691 0.034 Uiso 1 1 calc R . . C7 C 0.13301(5) 0.14942(9) 0.57531(15) 0.0197(3) Uani 1 1 d . . . H7A H 0.1375 0.1857 0.5001 0.029 Uiso 1 1 calc R . . H7B H 0.1522 0.0964 0.5738 0.029 Uiso 1 1 calc R . . H7C H 0.1467 0.1783 0.6625 0.029 Uiso 1 1 calc R . . C8 C 0.07445(5) 0.13038(8) 0.55892(14) 0.0154(2) Uani 1 1 d . . . C11 C -0.01901(5) 0.35555(8) 0.58875(12) 0.0114(2) Uani 1 1 d . . . C12 C -0.04084(5) 0.27437(8) 0.58174(13) 0.0135(2) Uani 1 1 d . . . H12 H -0.0765 0.2677 0.5861 0.016 Uiso 1 1 calc R . . C13 C -0.01117(5) 0.20360(8) 0.56858(13) 0.0141(2) Uani 1 1 d . . . H13 H -0.0271 0.1494 0.5626 0.017 Uiso 1 1 calc R . . C14 C 0.04186(5) 0.21021(8) 0.56384(12) 0.0125(2) Uani 1 1 d . . . C15 C 0.06264(5) 0.29147(8) 0.56415(13) 0.0132(2) Uani 1 1 d . . . H15 H 0.0979 0.2982 0.5565 0.016 Uiso 1 1 calc R . . C16 C 0.03277(5) 0.36292(8) 0.57549(12) 0.0127(2) Uani 1 1 d . . . H16 H 0.0478 0.4174 0.5742 0.015 Uiso 1 1 calc R . . C21 C -0.11125(5) 0.57061(8) 0.66077(12) 0.0121(2) Uani 1 1 d . . . C22 C -0.05870(5) 0.56116(8) 0.73102(12) 0.0118(2) Uani 1 1 d . . . H22 H -0.0434 0.6027 0.7963 0.014 Uiso 1 1 calc R . . C23 C -0.02789(5) 0.49305(8) 0.70896(12) 0.0112(2) Uani 1 1 d . . . C24 C -0.04980(5) 0.43043(8) 0.61301(12) 0.0114(2) Uani 1 1 d . . . C25 C -0.10267(5) 0.43961(8) 0.54261(12) 0.0129(2) Uani 1 1 d . . . H25 H -0.1184 0.3978 0.4782 0.016 Uiso 1 1 calc R . . C26 C -0.13261(5) 0.50836(8) 0.56478(13) 0.0132(2) Uani 1 1 d . . . H26 H -0.1680 0.5132 0.5141 0.016 Uiso 1 1 calc R . . C31 C -0.14189(5) 0.64420(8) 0.69086(12) 0.0125(2) Uani 1 1 d . . . C32 C -0.19656(5) 0.64172(8) 0.66958(15) 0.0182(3) Uani 1 1 d . . . H32 H -0.2149 0.5921 0.6329 0.022 Uiso 1 1 calc R . . C33 C -0.22476(5) 0.71054(9) 0.70099(16) 0.0209(3) Uani 1 1 d . . . H33 H -0.2620 0.7069 0.6841 0.025 Uiso 1 1 calc R . . C34 C -0.19969(5) 0.78461(8) 0.75665(13) 0.0162(2) Uani 1 1 d . . . C35 C -0.14487(5) 0.78651(8) 0.77903(14) 0.0164(2) Uani 1 1 d . . . H35 H -0.1264 0.8356 0.8180 0.020 Uiso 1 1 calc R . . C36 C -0.11672(5) 0.71872(8) 0.74588(13) 0.0151(2) Uani 1 1 d . . . H36 H -0.0796 0.7229 0.7608 0.018 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 C1 0.0464(10) 0.0362(9) 0.0292(9) -0.0111(7) 0.0110(7) 0.0132(8) C2 0.0219(7) 0.0231(8) 0.0554(11) -0.0062(7) 0.0167(7) 0.0057(6) C3 0.0242(7) 0.0163(7) 0.0399(9) -0.0004(6) 0.0052(6) 0.0049(6) C4 0.0211(7) 0.0159(6) 0.0269(7) -0.0051(5) 0.0078(5) 0.0047(5) C5 0.0279(8) 0.0218(7) 0.0283(8) -0.0110(6) 0.0073(6) 0.0014(6) C6 0.0224(7) 0.0161(6) 0.0312(8) 0.0065(5) 0.0113(6) 0.0053(5) C7 0.0164(6) 0.0171(6) 0.0274(7) 0.0018(5) 0.0090(5) 0.0037(5) C8 0.0167(6) 0.0110(5) 0.0198(6) -0.0008(4) 0.0067(5) 0.0009(4) C11 0.0132(5) 0.0107(5) 0.0099(5) -0.0008(4) 0.0019(4) 0.0000(4) C12 0.0110(5) 0.0137(6) 0.0156(6) -0.0017(4) 0.0031(4) -0.0017(4) C13 0.0143(5) 0.0105(5) 0.0174(6) -0.0010(4) 0.0034(4) -0.0023(4) C14 0.0141(5) 0.0114(5) 0.0121(5) -0.0010(4) 0.0034(4) 0.0007(4) C15 0.0129(5) 0.0122(5) 0.0155(5) -0.0003(4) 0.0054(4) -0.0001(4) C16 0.0147(5) 0.0100(5) 0.0138(5) -0.0002(4) 0.0042(4) -0.0013(4) C21 0.0121(5) 0.0119(5) 0.0126(5) 0.0012(4) 0.0035(4) 0.0000(4) C22 0.0119(5) 0.0109(5) 0.0129(5) -0.0003(4) 0.0033(4) -0.0002(4) C23 0.0105(5) 0.0108(5) 0.0123(5) 0.0017(4) 0.0029(4) -0.0006(4) C24 0.0125(5) 0.0102(5) 0.0121(5) 0.0011(4) 0.0040(4) -0.0002(4) C25 0.0128(5) 0.0122(5) 0.0133(5) -0.0016(4) 0.0021(4) -0.0009(4) C26 0.0104(5) 0.0142(6) 0.0145(5) 0.0002(4) 0.0022(4) 0.0008(4) C31 0.0139(5) 0.0112(5) 0.0124(5) 0.0007(4) 0.0029(4) 0.0013(4) C32 0.0139(6) 0.0149(6) 0.0257(7) -0.0052(5) 0.0046(5) -0.0015(5) C33 0.0124(6) 0.0188(6) 0.0320(8) -0.0058(6) 0.0062(5) 0.0013(5) C34 0.0164(6) 0.0144(6) 0.0185(6) -0.0006(5) 0.0053(5) 0.0035(5) C35 0.0165(6) 0.0128(6) 0.0190(6) -0.0016(5) 0.0021(5) -0.0002(5) C36 0.0122(5) 0.0130(6) 0.0193(6) -0.0001(5) 0.0020(4) 0.0006(4) _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 C1 C4 1.537(2) . ? C1 H1A 0.9800 . N C1 H1B 0.9800 . N C1 H1C 0.9800 . N C2 C4 1.533(2) . ? C2 H2A 0.9800 . N C2 H2B 0.9800 . N C2 H2C 0.9800 . N C3 C4 1.538(2) . ? C3 H3A 0.9800 . N C3 H3B 0.9800 . N C3 H3C 0.9800 . N C4 C34 1.5344(18) . ? C5 C8 1.5364(19) . ? C5 H5A 0.9800 . N C5 H5B 0.9800 . N C5 H5C 0.9800 . N C6 C8 1.5388(19) . ? C6 H6A 0.9800 . N C6 H6B 0.9800 . N C6 H6C 0.9800 . N C7 C8 1.5327(18) . ? C7 H7A 0.9800 . N C7 H7B 0.9800 . N C7 H7C 0.9800 . N C8 C14 1.5329(17) . ? C11 C16 1.3987(17) . ? C11 C12 1.4020(17) . ? C11 C24 1.4864(17) . ? C12 C13 1.3881(17) . ? C12 H12 0.9500 . N C13 C14 1.4047(17) . ? C13 H13 0.9500 . N C14 C15 1.3970(17) . ? C15 C16 1.3957(17) . ? C15 H15 0.9500 . N C16 H16 0.9500 . N C21 C22 1.3981(16) . ? C21 C26 1.4012(17) . ? C21 C31 1.4866(17) . ? C22 C23 1.3961(17) . ? C22 H22 0.9500 . N C23 C24 1.4088(16) . ? C23 C23 1.498(2) 2_556 ? C24 C25 1.4052(16) . ? C25 C26 1.3905(17) . ? C25 H25 0.9500 . N C26 H26 0.9500 . N C31 C32 1.3967(17) . ? C31 C36 1.4005(17) . ? C32 C33 1.3944(18) . ? C32 H32 0.9500 . N C33 C34 1.3954(19) . ? C33 H33 0.9500 . N C34 C35 1.3995(18) . ? C35 C36 1.3874(18) . ? C35 H35 0.9500 . N C36 H36 0.9500 . N loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C1 H1A 109.5 . . N C4 C1 H1B 109.5 . . N H1A C1 H1B 109.5 . . N C4 C1 H1C 109.5 . . N H1A C1 H1C 109.5 . . N H1B C1 H1C 109.5 . . N C4 C2 H2A 109.5 . . N C4 C2 H2B 109.5 . . N H2A C2 H2B 109.5 . . N C4 C2 H2C 109.5 . . N H2A C2 H2C 109.5 . . N H2B C2 H2C 109.5 . . N C4 C3 H3A 109.5 . . N C4 C3 H3B 109.5 . . N H3A C3 H3B 109.5 . . N C4 C3 H3C 109.5 . . N H3A C3 H3C 109.5 . . N H3B C3 H3C 109.5 . . N C2 C4 C34 112.27(12) . . ? C2 C4 C1 108.78(14) . . ? C34 C4 C1 109.59(12) . . ? C2 C4 C3 107.80(13) . . ? C34 C4 C3 108.81(12) . . ? C1 C4 C3 109.55(13) . . ? C8 C5 H5A 109.5 . . N C8 C5 H5B 109.5 . . N H5A C5 H5B 109.5 . . N C8 C5 H5C 109.5 . . N H5A C5 H5C 109.5 . . N H5B C5 H5C 109.5 . . N C8 C6 H6A 109.5 . . N C8 C6 H6B 109.5 . . N H6A C6 H6B 109.5 . . N C8 C6 H6C 109.5 . . N H6A C6 H6C 109.5 . . N H6B C6 H6C 109.5 . . N C8 C7 H7A 109.5 . . N C8 C7 H7B 109.5 . . N H7A C7 H7B 109.5 . . N C8 C7 H7C 109.5 . . N H7A C7 H7C 109.5 . . N H7B C7 H7C 109.5 . . N C7 C8 C14 112.62(11) . . ? C7 C8 C5 108.89(11) . . ? C14 C8 C5 109.29(11) . . ? C7 C8 C6 107.08(11) . . ? C14 C8 C6 109.53(11) . . ? C5 C8 C6 109.38(12) . . ? C16 C11 C12 117.68(11) . . ? C16 C11 C24 121.67(11) . . ? C12 C11 C24 120.63(11) . . ? C13 C12 C11 120.99(11) . . ? C13 C12 H12 119.5 . . N C11 C12 H12 119.5 . . N C12 C13 C14 121.55(11) . . ? C12 C13 H13 119.2 . . N C14 C13 H13 119.2 . . N C15 C14 C13 117.15(11) . . ? C15 C14 C8 122.72(11) . . ? C13 C14 C8 120.13(11) . . ? C16 C15 C14 121.45(11) . . ? C16 C15 H15 119.3 . . N C14 C15 H15 119.3 . . N C15 C16 C11 120.99(11) . . ? C15 C16 H16 119.5 . . N C11 C16 H16 119.5 . . N C22 C21 C26 117.24(11) . . ? C22 C21 C31 119.65(11) . . ? C26 C21 C31 123.11(11) . . ? C23 C22 C21 122.59(11) . . ? C23 C22 H22 118.7 . . N C21 C22 H22 118.7 . . N C22 C23 C24 119.78(11) . . ? C22 C23 C23 115.89(9) . 2_556 ? C24 C23 C23 124.33(9) . 2_556 ? C25 C24 C23 117.75(11) . . ? C25 C24 C11 120.48(11) . . ? C23 C24 C11 121.74(10) . . ? C26 C25 C24 121.70(11) . . ? C26 C25 H25 119.2 . . N C24 C25 H25 119.2 . . N C25 C26 C21 120.93(11) . . ? C25 C26 H26 119.5 . . N C21 C26 H26 119.5 . . N C32 C31 C36 116.97(11) . . ? C32 C31 C21 121.99(11) . . ? C36 C31 C21 121.02(11) . . ? C33 C32 C31 121.45(12) . . ? C33 C32 H32 119.3 . . N C31 C32 H32 119.3 . . N C32 C33 C34 121.63(12) . . ? C32 C33 H33 119.2 . . N C34 C33 H33 119.2 . . N C33 C34 C35 116.71(12) . . ? C33 C34 C4 123.31(12) . . ? C35 C34 C4 119.97(12) . . ? C36 C35 C34 121.86(12) . . ? C36 C35 H35 119.1 . . N C34 C35 H35 119.1 . . N C35 C36 C31 121.36(12) . . ? C35 C36 H36 119.3 . . N C31 C36 H36 119.3 . . N 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 C12 C11 C24 C23 133.87(12) . . . . ? C22 C21 C31 C32 -153.97(12) . . . . ? C22 C23 C23 C22 -61.6(2) . . 2_556 2_556 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.75 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.455 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.058