# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Prof Luigi Nassimbeni' _publ_contact_author_address ; Department of Chemistry University of Cape Town Rondebosch 7701 Cape Town SOUTH AFRICA ; _publ_contact_author_email XRAYLUIG@SCIENCE.UCT.AC.ZA _publ_section_title ; Inclusion by a Fluorenyl Host with Volatile Guests: Structures, Thermal Stability and Kinetics ; loop_ _publ_author_name 'Luigi Nassimbeni' 'Mino R. Caira' 'T.le Roex' 'Luigi Nassimbeni' 'John A. Ripmeester' ; E.Weber ; data_c:_H _database_code_depnum_ccdc_archive 'CCDC 229154' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 9,9'(Biphenyl-4,4'-diyl)difluoren-9-ol ; _chemical_name_common 9,9'(Biphenyl-4,4'-diyl)difluoren-9-ol _chemical_melting_point '306.4 (host)' _chemical_formula_moiety 'C38 H26 O2' _chemical_formula_sum 'C38 H26 O2' _chemical_formula_weight 514.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.80020(10) _cell_length_b 14.4736(3) _cell_length_c 15.7510(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.1410(10) _cell_angle_gamma 90.00 _cell_volume 1322.03(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9678 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'clear plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type none _exptl_special_details ; Crystal coated with paratone oil. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'combination of phi and omega' _diffrn_reflns_number 5370 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3027 _reflns_number_gt 2479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0598P)^2^+0.3003P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3027 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.1123 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.003 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 0.5135(3) 0.40486(10) 0.13710(11) 0.0555(4) Uani 1 1 d . . . H1 H 0.4330 0.3985 0.0858 0.067 Uiso 1 1 calc R . . C2 C 0.6729(3) 0.47617(11) 0.14927(15) 0.0742(6) Uani 1 1 d . . . H2 H 0.7002 0.5174 0.1053 0.089 Uiso 1 1 calc R . . C3 C 0.7904(3) 0.48624(13) 0.22564(17) 0.0824(7) Uani 1 1 d . . . H3 H 0.8954 0.5343 0.2327 0.099 Uiso 1 1 calc R . . C4 C 0.7541(3) 0.42611(14) 0.29133(13) 0.0707(6) Uani 1 1 d . . . H4 H 0.8333 0.4335 0.3428 0.085 Uiso 1 1 calc R . . C5 C 0.5919(3) 0.26097(15) 0.42191(11) 0.0689(5) Uani 1 1 d . . . H5 H 0.7085 0.2946 0.4490 0.083 Uiso 1 1 calc R . . C6 C 0.4839(4) 0.19018(16) 0.46345(11) 0.0774(6) Uani 1 1 d . . . H6 H 0.5266 0.1765 0.5193 0.093 Uiso 1 1 calc R . . C7 C 0.3139(4) 0.13940(15) 0.42361(10) 0.0770(6) Uani 1 1 d . . . H7 H 0.2424 0.0919 0.4528 0.092 Uiso 1 1 calc R . . C8 C 0.2469(3) 0.15813(12) 0.34000(9) 0.0593(4) Uani 1 1 d . . . H8 H 0.1317 0.1235 0.3132 0.071 Uiso 1 1 calc R . . O9 O 0.08249(14) 0.28485(7) 0.18647(6) 0.0466(3) Uani 1 1 d . . . H9 H 0.0374 0.3231 0.2207 0.056 Uiso 1 1 calc R . . C9 C 0.31625(19) 0.26116(8) 0.20617(7) 0.0341(3) Uani 1 1 d . . . C10 C 0.37542(18) 0.18441(8) 0.14353(7) 0.0296(2) Uani 1 1 d . . . C11 C 0.5806(2) 0.18186(8) 0.10030(8) 0.0374(3) Uani 1 1 d . . . H11 H 0.6888 0.2285 0.1090 0.045 Uiso 1 1 calc R . . C12 C 0.62724(19) 0.11085(8) 0.04414(8) 0.0368(3) Uani 1 1 d . . . H12 H 0.7653 0.1116 0.0151 0.044 Uiso 1 1 calc R . . C13 C 0.47359(18) 0.03841(7) 0.02987(6) 0.0265(2) Uani 1 1 d . . . C14 C 0.26895(19) 0.04091(8) 0.07485(8) 0.0346(3) Uani 1 1 d . . . H14 H 0.1629 -0.0068 0.0677 0.042 Uiso 1 1 calc R . . C15 C 0.2198(2) 0.11251(9) 0.12977(8) 0.0365(3) Uani 1 1 d . . . H15 H 0.0804 0.1126 0.1580 0.044 Uiso 1 1 calc R . . C1A C 0.4781(2) 0.34411(9) 0.20293(9) 0.0403(3) Uani 1 1 d . . . C4A C 0.5979(2) 0.35398(10) 0.28029(9) 0.0483(4) Uani 1 1 d . . . C5A C 0.5245(2) 0.28180(10) 0.33844(9) 0.0478(4) Uani 1 1 d . . . C8A C 0.3540(2) 0.22871(9) 0.29768(8) 0.0409(3) Uani 1 1 d . . . 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 0.0610(9) 0.0378(7) 0.0679(10) -0.0093(7) 0.0102(7) -0.0005(6) C2 0.0790(12) 0.0367(8) 0.1083(16) -0.0140(9) 0.0320(11) -0.0096(8) C3 0.0660(11) 0.0551(10) 0.1272(19) -0.0492(12) 0.0262(11) -0.0235(9) C4 0.0503(9) 0.0728(12) 0.0893(13) -0.0520(11) 0.0051(8) -0.0135(8) C5 0.0609(10) 0.0992(14) 0.0459(9) -0.0330(9) -0.0149(7) 0.0171(10) C6 0.0950(14) 0.1025(15) 0.0343(8) -0.0101(9) -0.0062(8) 0.0284(12) C7 0.1092(15) 0.0834(13) 0.0388(8) 0.0004(8) 0.0114(9) 0.0071(11) C8 0.0732(10) 0.0669(10) 0.0380(7) -0.0071(7) 0.0061(7) -0.0080(8) O9 0.0334(5) 0.0517(6) 0.0545(6) -0.0203(4) -0.0036(4) 0.0088(4) C9 0.0302(6) 0.0366(6) 0.0354(6) -0.0116(5) -0.0019(4) 0.0007(5) C10 0.0294(5) 0.0309(5) 0.0284(5) -0.0056(4) -0.0038(4) 0.0020(4) C11 0.0320(6) 0.0334(6) 0.0470(7) -0.0134(5) 0.0027(5) -0.0069(5) C12 0.0289(5) 0.0356(6) 0.0461(7) -0.0119(5) 0.0073(5) -0.0045(5) C13 0.0273(5) 0.0268(5) 0.0251(5) -0.0016(4) -0.0053(4) 0.0017(4) C14 0.0312(6) 0.0346(6) 0.0381(6) -0.0093(5) 0.0019(5) -0.0080(5) C15 0.0303(6) 0.0419(7) 0.0374(6) -0.0105(5) 0.0050(4) -0.0053(5) C1A 0.0359(6) 0.0344(6) 0.0508(7) -0.0182(5) 0.0040(5) 0.0008(5) C4A 0.0354(6) 0.0527(8) 0.0568(8) -0.0336(7) 0.0019(6) 0.0002(6) C5A 0.0403(7) 0.0618(9) 0.0412(7) -0.0252(6) -0.0040(5) 0.0085(6) C8A 0.0416(7) 0.0483(7) 0.0327(6) -0.0143(5) 0.0014(5) 0.0039(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 C1 C1A 1.378(2) . ? C1 C2 1.397(2) . ? C2 C3 1.379(3) . ? C3 C4 1.372(3) . ? C4 C4A 1.391(2) . ? C5 C6 1.373(3) . ? C5 C5A 1.397(2) . ? C6 C7 1.372(3) . ? C7 C8 1.392(2) . ? C8 C8A 1.375(2) . ? O9 C9 1.4268(14) . ? C9 C1A 1.5255(17) . ? C9 C8A 1.5275(17) . ? C9 C10 1.5292(15) . ? C10 C11 1.3833(16) . ? C10 C15 1.3919(16) . ? C11 C12 1.3862(16) . ? C12 C13 1.3914(15) . ? C13 C14 1.3948(15) . ? C13 C13 1.492(2) 3_655 ? C14 C15 1.3833(16) . ? C1A C4A 1.3979(19) . ? C4A C5A 1.459(2) . ? C5A C8A 1.3985(18) . ? 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 C1A C1 C2 118.45(17) . . ? C3 C2 C1 120.83(19) . . ? C4 C3 C2 120.70(16) . . ? C3 C4 C4A 119.42(18) . . ? C6 C5 C5A 119.18(16) . . ? C7 C6 C5 120.81(16) . . ? C6 C7 C8 120.86(19) . . ? C8A C8 C7 118.89(17) . . ? O9 C9 C1A 112.72(10) . . ? O9 C9 C8A 113.38(10) . . ? C1A C9 C8A 101.35(10) . . ? O9 C9 C10 105.00(9) . . ? C1A C9 C10 113.83(9) . . ? C8A C9 C10 110.84(10) . . ? C11 C10 C15 117.72(10) . . ? C11 C10 C9 122.91(10) . . ? C15 C10 C9 119.36(10) . . ? C10 C11 C12 120.97(10) . . ? C11 C12 C13 121.96(10) . . ? C12 C13 C14 116.57(10) . . ? C12 C13 C13 121.63(12) . 3_655 ? C14 C13 C13 121.80(12) . 3_655 ? C15 C14 C13 121.68(10) . . ? C14 C15 C10 121.08(10) . . ? C1 C1A C4A 120.79(13) . . ? C1 C1A C9 128.92(12) . . ? C4A C1A C9 110.29(12) . . ? C4 C4A C1A 119.80(17) . . ? C4 C4A C5A 131.04(15) . . ? C1A C4A C5A 109.14(11) . . ? C5 C5A C8A 119.71(16) . . ? C5 C5A C4A 131.75(15) . . ? C8A C5A C4A 108.53(12) . . ? C8 C8A C5A 120.52(13) . . ? C8 C8A C9 128.93(12) . . ? C5A C8A C9 110.55(12) . . ? 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 C1A C1 C2 C3 -0.7(2) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C2 C3 C4 C4A 0.4(3) . . . . ? C5A C5 C6 C7 0.8(3) . . . . ? C5 C6 C7 C8 0.2(3) . . . . ? C6 C7 C8 C8A -0.1(3) . . . . ? O9 C9 C10 C11 135.85(12) . . . . ? C1A C9 C10 C11 12.11(16) . . . . ? C8A C9 C10 C11 -101.36(13) . . . . ? O9 C9 C10 C15 -45.34(14) . . . . ? C1A C9 C10 C15 -169.08(11) . . . . ? C8A C9 C10 C15 77.45(13) . . . . ? C15 C10 C11 C12 1.08(19) . . . . ? C9 C10 C11 C12 179.91(12) . . . . ? C10 C11 C12 C13 -1.3(2) . . . . ? C11 C12 C13 C14 0.20(18) . . . . ? C11 C12 C13 C13 -179.20(13) . . . 3_655 ? C12 C13 C14 C15 1.02(17) . . . . ? C13 C13 C14 C15 -179.58(12) 3_655 . . . ? C13 C14 C15 C10 -1.20(19) . . . . ? C11 C10 C15 C14 0.12(18) . . . . ? C9 C10 C15 C14 -178.75(11) . . . . ? C2 C1 C1A C4A 0.4(2) . . . . ? C2 C1 C1A C9 -179.85(13) . . . . ? O9 C9 C1A C1 -55.68(16) . . . . ? C8A C9 C1A C1 -177.20(13) . . . . ? C10 C9 C1A C1 63.77(17) . . . . ? O9 C9 C1A C4A 124.09(11) . . . . ? C8A C9 C1A C4A 2.56(12) . . . . ? C10 C9 C1A C4A -116.47(11) . . . . ? C3 C4 C4A C1A -0.7(2) . . . . ? C3 C4 C4A C5A -179.13(15) . . . . ? C1 C1A C4A C4 0.27(19) . . . . ? C9 C1A C4A C4 -179.52(11) . . . . ? C1 C1A C4A C5A 179.05(12) . . . . ? C9 C1A C4A C5A -0.74(14) . . . . ? C6 C5 C5A C8A -2.0(2) . . . . ? C6 C5 C5A C4A 176.91(15) . . . . ? C4 C4A C5A C5 -2.1(3) . . . . ? C1A C4A C5A C5 179.35(14) . . . . ? C4 C4A C5A C8A 176.94(14) . . . . ? C1A C4A C5A C8A -1.65(14) . . . . ? C7 C8 C8A C5A -1.1(2) . . . . ? C7 C8 C8A C9 178.44(14) . . . . ? C5 C5A C8A C8 2.1(2) . . . . ? C4A C5A C8A C8 -177.00(13) . . . . ? C5 C5A C8A C9 -177.48(12) . . . . ? C4A C5A C8A C9 3.39(14) . . . . ? O9 C9 C8A C8 55.76(18) . . . . ? C1A C9 C8A C8 176.82(14) . . . . ? C10 C9 C8A C8 -62.02(17) . . . . ? O9 C9 C8A C5A -124.67(11) . . . . ? C1A C9 C8A C5A -3.61(13) . . . . ? C10 C9 C8A C5A 117.55(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.230 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.032 #========================================================END data_c:_H.4DMA _database_code_depnum_ccdc_archive 'CCDC 229155' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 9,9'-(Biphenyl-4,4'-diyl)bis(fluoren-9-ol). 4(N,N-dimethylacetamide) clathrate ; _chemical_name_common ;9,9'-(Biphenyl-4,4'-diyl)bis(fluoren-9-ol). 4(N,N- dimethylacetamide) clathrate ; _chemical_melting_point '315.3 (host)' _chemical_formula_moiety 'C38 H26 O2. 4(C4 H9 N O)' _chemical_formula_sum 'C54 H62 N4 O6' _chemical_formula_weight 863.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.29610(10) _cell_length_b 14.9893(2) _cell_length_c 17.8825(3) _cell_angle_alpha 108.2550(10) _cell_angle_beta 91.5240(10) _cell_angle_gamma 109.2840(10) _cell_volume 2447.71(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 39845 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'clear plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_special_details ; Crystal coated with Paratone oil. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'combination of phi and omega' _diffrn_reflns_number 18802 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11071 _reflns_number_gt 5786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1359P)^2^+0.9795P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 11071 _refine_ls_number_parameters 577 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1611 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.2990 _refine_ls_wR_factor_gt 0.2508 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.172 _refine_ls_shift/su_mean 0.009 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 C2 C 1.4115(4) 0.7355(4) -0.0867(3) 0.0913(12) Uani 1 1 d . . . H2 H 1.4649 0.7492 -0.0389 0.110 Uiso 1 1 calc R . . C3 C 1.4241(4) 0.6671(4) -0.1537(3) 0.0931(13) Uani 1 1 d . . . H3 H 1.4862 0.6346 -0.1514 0.112 Uiso 1 1 calc R . . C4 C 1.3457(4) 0.6448(3) -0.2259(2) 0.0769(10) Uani 1 1 d . . . H4 H 1.3543 0.5976 -0.2719 0.092 Uiso 1 1 calc R . . C5 C 1.1322(4) 0.6271(3) -0.3730(2) 0.0799(10) Uani 1 1 d . . . H5 H 1.1802 0.5837 -0.3920 0.096 Uiso 1 1 calc R . . C6 C 1.0352(5) 0.6330(4) -0.4234(2) 0.0998(14) Uani 1 1 d . . . H6 H 1.0175 0.5938 -0.4770 0.120 Uiso 1 1 calc R . . C7 C 0.9646(4) 0.6964(4) -0.3951(3) 0.0984(14) Uani 1 1 d . . . H7 H 0.8985 0.6993 -0.4299 0.118 Uiso 1 1 calc R . . C8 C 0.9895(4) 0.7569(3) -0.3153(2) 0.0775(10) Uani 1 1 d . . . H8 H 0.9409 0.8000 -0.2967 0.093 Uiso 1 1 calc R . . O9 O 1.1984(2) 0.91598(14) -0.16070(14) 0.0718(7) Uani 1 1 d . . . H9 H 1.2660 0.9275 -0.1842 0.086 Uiso 1 1 calc R . . C9 C 1.1368(3) 0.8104(2) -0.17657(17) 0.0512(7) Uani 1 1 d . . . C10 C 1.0224(3) 0.79531(19) -0.12435(16) 0.0475(6) Uani 1 1 d . . . C11 C 0.9162(3) 0.7026(2) -0.14165(18) 0.0556(7) Uani 1 1 d . . . H11 H 0.9106 0.6505 -0.1881 0.067 Uiso 1 1 calc R . . C12 C 0.8193(3) 0.6868(2) -0.09119(17) 0.0528(7) Uani 1 1 d . . . H12 H 0.7500 0.6237 -0.1040 0.063 Uiso 1 1 calc R . . C13 C 0.8221(3) 0.76309(19) -0.02101(16) 0.0442(6) Uani 1 1 d . . . C14 C 0.9274(3) 0.85582(19) -0.00506(17) 0.0499(7) Uani 1 1 d . . . H14 H 0.9321 0.9086 0.0407 0.060 Uiso 1 1 calc R . . C15 C 1.0261(3) 0.87166(19) -0.05575(17) 0.0522(7) Uani 1 1 d . . . H15 H 1.0955 0.9346 -0.0432 0.063 Uiso 1 1 calc R . . C16 C 0.7201(2) 0.74428(18) 0.03424(16) 0.0438(6) Uani 1 1 d . . . C17 C 0.6539(3) 0.6488(2) 0.03656(19) 0.0589(8) Uani 1 1 d . . . H17 H 0.6772 0.5958 0.0045 0.071 Uiso 1 1 calc R . . C18 C 0.5531(3) 0.6301(2) 0.08572(19) 0.0590(8) Uani 1 1 d . . . H18 H 0.5101 0.5649 0.0858 0.071 Uiso 1 1 calc R . . C19 C 0.5161(3) 0.70671(19) 0.13420(16) 0.0459(6) Uani 1 1 d . . . C20 C 0.5863(3) 0.8033(2) 0.13472(17) 0.0513(7) Uani 1 1 d . . . H20 H 0.5662 0.8566 0.1689 0.062 Uiso 1 1 calc R . . C21 C 0.6851(3) 0.8221(2) 0.08585(16) 0.0494(6) Uani 1 1 d . . . H21 H 0.7296 0.8877 0.0871 0.059 Uiso 1 1 calc R . . O22 O 0.3455(2) 0.58131(14) 0.16977(12) 0.0599(5) Uani 1 1 d . . . H22 H 0.2822 0.5683 0.1960 0.072 Uiso 1 1 calc R . . C22 C 0.3984(3) 0.6865(2) 0.18396(17) 0.0482(6) Uani 1 1 d . . . C23 C 0.2087(3) 0.6960(2) 0.08978(19) 0.0610(8) Uani 1 1 d . . . H23 H 0.2237 0.6502 0.0452 0.073 Uiso 1 1 calc R . . C24 C 0.1087(4) 0.7373(3) 0.0839(2) 0.0743(10) Uani 1 1 d . . . H24 H 0.0557 0.7190 0.0349 0.089 Uiso 1 1 calc R . . C25 C 0.0870(4) 0.8054(3) 0.1500(2) 0.0773(10) Uani 1 1 d . . . H25 H 0.0185 0.8318 0.1452 0.093 Uiso 1 1 calc R . . C26 C 0.1652(3) 0.8350(3) 0.2230(2) 0.0687(9) Uani 1 1 d . . . H26 H 0.1509 0.8816 0.2673 0.082 Uiso 1 1 calc R . . C27 C 0.3803(4) 0.8684(3) 0.37676(19) 0.0725(9) Uani 1 1 d . . . H27 H 0.3269 0.9084 0.3936 0.087 Uiso 1 1 calc R . . C28 C 0.4795(5) 0.8674(3) 0.4301(2) 0.0838(11) Uani 1 1 d . . . H28 H 0.4921 0.9065 0.4835 0.101 Uiso 1 1 calc R . . C29 C 0.5590(4) 0.8096(3) 0.4050(2) 0.0824(11) Uani 1 1 d . . . H29 H 0.6263 0.8111 0.4415 0.099 Uiso 1 1 calc R . . C30 C 0.5411(3) 0.7487(3) 0.3259(2) 0.0672(9) Uani 1 1 d . . . H30 H 0.5949 0.7090 0.3094 0.081 Uiso 1 1 calc R . . C1A C 1.2429(3) 0.7655(2) -0.15920(17) 0.0504(7) Uani 1 1 d . . . C4A C 1.2544(3) 0.6945(2) -0.22784(17) 0.0542(7) Uani 1 1 d . . . C5A C 1.1575(3) 0.6859(2) -0.29413(17) 0.0553(7) Uani 1 1 d . . . C8A C 1.0872(3) 0.7515(2) -0.26490(18) 0.0544(7) Uani 1 1 d . . . C23A C 0.2857(3) 0.7238(2) 0.16286(16) 0.0477(6) Uani 1 1 d . . . C26A C 0.2656(3) 0.7938(2) 0.22915(17) 0.0515(7) Uani 1 1 d . . . C27A C 0.3628(3) 0.8086(2) 0.29792(17) 0.0536(7) Uani 1 1 d . . . C30A C 0.4420(3) 0.7486(2) 0.27262(16) 0.0499(7) Uani 1 1 d . . . O1G O 1.4341(3) 0.9590(2) -0.2290(2) 0.1003(9) Uani 1 1 d . . . N1G N 1.6199(5) 0.9283(4) -0.1919(4) 0.149(2) Uani 1 1 d D . . C1G C 1.5272(6) 0.9270(4) -0.2363(5) 0.149(3) Uani 1 1 d D . . C2G C 1.5399(7) 0.8610(5) -0.3265(3) 0.167(3) Uani 1 1 d D . . C3G C 1.6018(7) 1.0013(5) -0.1039(3) 0.165(3) Uani 1 1 d D . . C4G C 1.7340(6) 0.8928(6) -0.1969(5) 0.177(3) Uani 1 1 d D . . O11G O 0.1098(2) 0.54116(18) 0.24152(16) 0.0791(7) Uani 1 1 d . . . N11G N -0.0682(5) 0.5906(4) 0.2461(5) 0.177(3) Uani 1 1 d D . . C11G C 0.0058(5) 0.5513(4) 0.2178(5) 0.141(3) Uani 1 1 d D . . C12G C -0.0589(5) 0.4923(4) 0.1213(3) 0.1121(16) Uani 1 1 d D . . C13G C -0.0024(7) 0.6456(5) 0.3427(3) 0.144(2) Uani 1 1 d D . . C14G C -0.1886(5) 0.6099(5) 0.2206(5) 0.144(2) Uani 1 1 d D . . O21G O 0.1188(4) 1.0380(4) 0.3871(3) 0.1618(17) Uani 1 1 d . . . N21G N -0.0855(6) 1.0402(5) 0.3865(5) 0.189(3) Uani 1 1 d D . . C21G C 0.0198(10) 1.0628(7) 0.4162(7) 0.220(6) Uani 1 1 d D . . C22G C 0.0424(8) 1.1360(5) 0.5086(3) 0.150(3) Uani 1 1 d D . . C23G C -0.1136(7) 0.9612(4) 0.2922(3) 0.132(2) Uani 1 1 d D . . C24G C -0.2081(6) 1.0687(5) 0.4108(5) 0.163(3) Uani 1 1 d D . . O31G O 0.6349(4) 0.5471(3) 0.3993(3) 0.1433(15) Uani 1 1 d . . . N31G N 0.4257(5) 0.5483(4) 0.4016(4) 0.141(2) Uani 1 1 d D . . C31G C 0.5439(7) 0.5764(5) 0.4349(5) 0.157(3) Uani 1 1 d D . . C33G C 0.3884(5) 0.4710(4) 0.3124(3) 0.1050(15) Uani 1 1 d D . . C34G C 0.3104(5) 0.5806(5) 0.4345(4) 0.132(2) Uani 1 1 d D . . C1 C 1.3201(3) 0.7855(3) -0.0882(2) 0.0712(9) Uani 1 1 d . . . H1 H 1.3112 0.8319 -0.0418 0.085 Uiso 1 1 calc R . . C32G C 0.5727(7) 0.6484(4) 0.5229(3) 0.1258(19) Uani 1 1 d D . . 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 C2 0.061(2) 0.129(4) 0.086(3) 0.039(3) -0.005(2) 0.035(2) C3 0.070(2) 0.130(4) 0.106(3) 0.047(3) 0.017(2) 0.061(2) C4 0.077(2) 0.081(2) 0.085(3) 0.024(2) 0.029(2) 0.0472(19) C5 0.095(3) 0.080(2) 0.054(2) 0.0158(17) 0.0185(19) 0.024(2) C6 0.110(3) 0.108(3) 0.058(2) 0.025(2) 0.004(2) 0.012(3) C7 0.080(3) 0.129(4) 0.087(3) 0.068(3) -0.004(2) 0.010(3) C8 0.062(2) 0.095(3) 0.091(3) 0.056(2) 0.0142(19) 0.0252(18) O9 0.0692(13) 0.0447(11) 0.1020(18) 0.0258(11) 0.0410(12) 0.0180(10) C9 0.0494(15) 0.0422(14) 0.0627(18) 0.0170(13) 0.0185(13) 0.0171(12) C10 0.0465(14) 0.0423(14) 0.0576(16) 0.0161(12) 0.0152(12) 0.0209(12) C11 0.0513(15) 0.0457(15) 0.0622(18) 0.0084(13) 0.0175(14) 0.0164(12) C12 0.0449(14) 0.0440(15) 0.0610(18) 0.0095(13) 0.0113(13) 0.0129(12) C13 0.0405(13) 0.0427(14) 0.0529(15) 0.0148(12) 0.0088(12) 0.0208(11) C14 0.0547(15) 0.0393(14) 0.0538(16) 0.0097(12) 0.0099(13) 0.0202(12) C15 0.0503(15) 0.0375(14) 0.0669(18) 0.0158(13) 0.0154(14) 0.0145(11) C16 0.0399(13) 0.0430(14) 0.0507(15) 0.0147(11) 0.0076(11) 0.0188(11) C17 0.0614(17) 0.0451(16) 0.075(2) 0.0171(14) 0.0270(15) 0.0268(13) C18 0.0600(17) 0.0444(15) 0.079(2) 0.0245(14) 0.0251(16) 0.0218(13) C19 0.0444(14) 0.0476(15) 0.0485(15) 0.0157(12) 0.0096(12) 0.0203(11) C20 0.0528(15) 0.0439(15) 0.0549(16) 0.0100(12) 0.0162(13) 0.0203(12) C21 0.0498(15) 0.0415(14) 0.0533(16) 0.0111(12) 0.0112(13) 0.0163(12) O22 0.0594(12) 0.0496(11) 0.0755(14) 0.0255(10) 0.0248(10) 0.0205(9) C22 0.0456(14) 0.0463(15) 0.0561(16) 0.0200(12) 0.0123(12) 0.0178(12) C23 0.0568(17) 0.0684(19) 0.0570(18) 0.0202(15) 0.0073(15) 0.0223(15) C24 0.063(2) 0.093(3) 0.075(2) 0.034(2) 0.0013(17) 0.0326(18) C25 0.067(2) 0.100(3) 0.089(3) 0.044(2) 0.0168(19) 0.049(2) C26 0.071(2) 0.077(2) 0.072(2) 0.0244(17) 0.0246(18) 0.0453(18) C27 0.086(2) 0.070(2) 0.056(2) 0.0159(16) 0.0168(18) 0.0251(18) C28 0.104(3) 0.077(2) 0.052(2) 0.0122(17) 0.006(2) 0.017(2) C29 0.082(2) 0.092(3) 0.064(2) 0.037(2) -0.0102(19) 0.012(2) C30 0.0623(19) 0.076(2) 0.068(2) 0.0341(18) 0.0054(16) 0.0221(16) C1A 0.0413(14) 0.0518(15) 0.0554(17) 0.0175(13) 0.0125(13) 0.0136(12) C4A 0.0522(16) 0.0550(16) 0.0593(18) 0.0199(14) 0.0189(14) 0.0230(13) C5A 0.0590(17) 0.0530(17) 0.0499(17) 0.0160(13) 0.0152(14) 0.0160(13) C8A 0.0495(15) 0.0585(17) 0.0609(18) 0.0305(14) 0.0153(14) 0.0165(13) C23A 0.0449(14) 0.0483(15) 0.0523(16) 0.0191(12) 0.0113(12) 0.0173(12) C26A 0.0522(15) 0.0518(16) 0.0537(17) 0.0185(13) 0.0147(13) 0.0217(13) C27A 0.0593(17) 0.0519(16) 0.0483(16) 0.0165(13) 0.0133(13) 0.0182(13) C30A 0.0478(15) 0.0539(16) 0.0515(16) 0.0238(13) 0.0107(13) 0.0170(12) O1G 0.0776(17) 0.0874(19) 0.139(3) 0.0368(17) 0.0491(17) 0.0323(15) N1G 0.088(3) 0.127(4) 0.229(6) 0.084(4) 0.008(3) 0.012(3) C1G 0.083(4) 0.106(4) 0.282(10) 0.109(5) 0.055(5) 0.020(3) C2G 0.177(6) 0.161(5) 0.096(4) -0.022(4) 0.059(4) 0.035(5) C3G 0.174(6) 0.142(5) 0.084(3) -0.011(3) 0.030(4) -0.016(4) C4G 0.110(4) 0.188(7) 0.267(9) 0.083(6) 0.038(5) 0.090(5) O11G 0.0616(14) 0.0772(16) 0.1052(19) 0.0331(14) 0.0288(13) 0.0302(12) N11G 0.085(3) 0.133(4) 0.370(10) 0.141(5) 0.083(4) 0.054(3) C11G 0.079(3) 0.101(4) 0.296(9) 0.123(5) 0.086(4) 0.039(3) C12G 0.124(4) 0.106(3) 0.067(3) 0.016(2) -0.008(3) 0.005(3) C13G 0.152(5) 0.143(5) 0.084(3) -0.020(3) 0.027(3) 0.041(4) C14G 0.089(3) 0.144(5) 0.236(7) 0.082(5) 0.033(4) 0.071(3) O21G 0.115(3) 0.219(5) 0.209(5) 0.101(4) 0.065(3) 0.103(3) N21G 0.112(4) 0.190(6) 0.361(11) 0.213(7) 0.069(6) 0.061(4) C21G 0.133(6) 0.226(10) 0.430(18) 0.264(12) 0.087(10) 0.079(7) C22G 0.223(7) 0.127(5) 0.072(3) 0.017(3) 0.017(4) 0.043(5) C23G 0.167(5) 0.114(4) 0.092(3) 0.005(3) -0.010(3) 0.051(4) C24G 0.105(4) 0.157(5) 0.275(9) 0.112(6) 0.091(5) 0.066(4) O31G 0.099(2) 0.184(4) 0.188(4) 0.076(3) 0.052(2) 0.087(3) N31G 0.111(3) 0.159(4) 0.231(6) 0.143(5) 0.068(4) 0.072(3) C31G 0.119(5) 0.162(6) 0.270(10) 0.161(7) 0.065(6) 0.065(5) C33G 0.132(4) 0.110(3) 0.065(3) 0.010(2) -0.001(2) 0.053(3) C34G 0.090(3) 0.147(5) 0.184(6) 0.063(4) 0.062(3) 0.064(3) C1 0.0548(18) 0.085(2) 0.061(2) 0.0129(17) 0.0058(15) 0.0204(17) C32G 0.171(5) 0.104(4) 0.078(3) 0.017(3) 0.005(3) 0.033(3) _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 C2 C3 1.353(6) . ? C2 C1 1.388(5) . ? C3 C4 1.387(5) . ? C4 C4A 1.384(4) . ? C5 C6 1.370(6) . ? C5 C5A 1.373(4) . ? C6 C7 1.364(6) . ? C7 C8 1.393(6) . ? C8 C8A 1.373(4) . ? O9 C9 1.426(3) . ? C9 C10 1.524(4) . ? C9 C8A 1.523(4) . ? C9 C1A 1.531(4) . ? C10 C15 1.380(4) . ? C10 C11 1.390(4) . ? C11 C12 1.376(4) . ? C12 C13 1.400(4) . ? C13 C14 1.389(4) . ? C13 C16 1.481(4) . ? C14 C15 1.391(4) . ? C16 C17 1.381(4) . ? C16 C21 1.401(4) . ? C17 C18 1.393(4) . ? C18 C19 1.378(4) . ? C19 C20 1.385(4) . ? C19 C22 1.528(4) . ? C20 C21 1.375(4) . ? O22 C22 1.422(3) . ? C22 C23A 1.529(4) . ? C22 C30A 1.531(4) . ? C23 C23A 1.377(4) . ? C23 C24 1.383(4) . ? C24 C25 1.378(5) . ? C25 C26 1.377(5) . ? C26 C26A 1.384(4) . ? C27 C28 1.386(5) . ? C27 C27A 1.383(4) . ? C28 C29 1.366(6) . ? C29 C30 1.390(5) . ? C30 C30A 1.377(4) . ? C1A C1 1.373(4) . ? C1A C4A 1.388(4) . ? C4A C5A 1.475(4) . ? C5A C8A 1.390(4) . ? C23A C26A 1.389(4) . ? C26A C27A 1.477(4) . ? C27A C30A 1.388(4) . ? O1G C1G 1.198(6) . ? N1G C1G 1.218(7) . ? N1G C4G 1.435(7) . ? N1G C3G 1.666(7) . ? C1G C2G 1.641(8) . ? O11G C11G 1.213(6) . ? N11G C11G 1.147(6) . ? N11G C14G 1.456(6) . ? N11G C13G 1.673(8) . ? C11G C12G 1.674(8) . ? O21G C21G 1.267(10) . ? N21G C21G 1.089(9) . ? N21G C24G 1.495(7) . ? N21G C23G 1.681(9) . ? C21G C22G 1.631(12) . ? O31G C31G 1.266(7) . ? N31G C31G 1.216(7) . ? N31G C34G 1.493(6) . ? N31G C33G 1.597(7) . ? C31G C32G 1.559(9) . ? 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 C3 C2 C1 120.9(3) . . ? C2 C3 C4 120.9(3) . . ? C3 C4 C4A 118.4(3) . . ? C6 C5 C5A 119.1(4) . . ? C7 C6 C5 120.2(4) . . ? C6 C7 C8 121.4(4) . . ? C8A C8 C7 118.5(4) . . ? O9 C9 C10 106.8(2) . . ? O9 C9 C8A 112.3(2) . . ? C10 C9 C8A 114.1(2) . . ? O9 C9 C1A 112.1(2) . . ? C10 C9 C1A 110.7(2) . . ? C8A C9 C1A 101.0(2) . . ? C15 C10 C11 118.0(3) . . ? C15 C10 C9 120.9(2) . . ? C11 C10 C9 121.1(2) . . ? C12 C11 C10 121.1(3) . . ? C11 C12 C13 121.7(3) . . ? C14 C13 C12 116.6(2) . . ? C14 C13 C16 122.1(2) . . ? C12 C13 C16 121.3(2) . . ? C15 C14 C13 121.6(2) . . ? C10 C15 C14 121.0(2) . . ? C17 C16 C21 117.0(2) . . ? C17 C16 C13 121.4(2) . . ? C21 C16 C13 121.6(2) . . ? C16 C17 C18 121.6(2) . . ? C19 C18 C17 120.9(3) . . ? C18 C19 C20 117.8(2) . . ? C18 C19 C22 121.7(2) . . ? C20 C19 C22 120.5(2) . . ? C21 C20 C19 121.5(2) . . ? C20 C21 C16 121.2(2) . . ? O22 C22 C19 107.3(2) . . ? O22 C22 C23A 111.9(2) . . ? C19 C22 C23A 110.8(2) . . ? O22 C22 C30A 112.4(2) . . ? C19 C22 C30A 113.5(2) . . ? C23A C22 C30A 100.8(2) . . ? C23A C23 C24 118.9(3) . . ? C25 C24 C23 120.5(3) . . ? C24 C25 C26 121.1(3) . . ? C25 C26 C26A 118.6(3) . . ? C28 C27 C27A 118.4(3) . . ? C29 C28 C27 120.6(3) . . ? C28 C29 C30 121.3(3) . . ? C30A C30 C29 118.5(3) . . ? C1 C1A C4A 120.1(3) . . ? C1 C1A C9 129.1(3) . . ? C4A C1A C9 110.8(2) . . ? C1A C4A C4 120.5(3) . . ? C1A C4A C5A 108.7(2) . . ? C4 C4A C5A 130.8(3) . . ? C5 C5A C8A 121.1(3) . . ? C5 C5A C4A 130.5(3) . . ? C8A C5A C4A 108.4(2) . . ? C8 C8A C5A 119.6(3) . . ? C8 C8A C9 129.3(3) . . ? C5A C8A C9 111.1(2) . . ? C23 C23A C26A 120.6(3) . . ? C23 C23A C22 128.1(3) . . ? C26A C23A C22 111.3(2) . . ? C26 C26A C23A 120.4(3) . . ? C26 C26A C27A 131.5(3) . . ? C23A C26A C27A 108.1(2) . . ? C27 C27A C30A 121.0(3) . . ? C27 C27A C26A 130.1(3) . . ? C30A C27A C26A 108.8(2) . . ? C30 C30A C27A 120.2(3) . . ? C30 C30A C22 128.9(3) . . ? C27A C30A C22 110.8(2) . . ? C1G N1G C4G 138.6(7) . . ? C1G N1G C3G 102.3(6) . . ? C4G N1G C3G 118.9(6) . . ? N1G C1G O1G 136.0(8) . . ? N1G C1G C2G 106.6(6) . . ? O1G C1G C2G 117.4(7) . . ? C11G N11G C14G 138.2(8) . . ? C11G N11G C13G 105.0(6) . . ? C14G N11G C13G 116.6(6) . . ? N11G C11G O11G 135.8(8) . . ? N11G C11G C12G 106.6(6) . . ? O11G C11G C12G 117.5(5) . . ? C21G N21G C24G 133.3(11) . . ? C21G N21G C23G 113.3(9) . . ? C24G N21G C23G 113.2(6) . . ? N21G C21G O21G 127.5(12) . . ? N21G C21G C22G 112.3(10) . . ? O21G C21G C22G 120.3(8) . . ? C31G N31G C34G 126.9(7) . . ? C31G N31G C33G 117.7(6) . . ? C34G N31G C33G 115.4(5) . . ? N31G C31G O31G 121.1(8) . . ? N31G C31G C32G 115.4(7) . . ? O31G C31G C32G 123.5(7) . . ? C1A C1 C2 119.0(3) . . ? 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 C1 C2 C3 C4 -0.2(7) . . . . ? C2 C3 C4 C4A 0.3(6) . . . . ? C5A C5 C6 C7 -0.3(6) . . . . ? C5 C6 C7 C8 0.6(7) . . . . ? C6 C7 C8 C8A -0.1(6) . . . . ? O9 C9 C10 C15 -23.5(4) . . . . ? C8A C9 C10 C15 -148.1(3) . . . . ? C1A C9 C10 C15 98.8(3) . . . . ? O9 C9 C10 C11 160.5(3) . . . . ? C8A C9 C10 C11 35.9(4) . . . . ? C1A C9 C10 C11 -77.2(3) . . . . ? C15 C10 C11 C12 -1.3(4) . . . . ? C9 C10 C11 C12 174.9(3) . . . . ? C10 C11 C12 C13 0.7(4) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C11 C12 C13 C16 -177.9(3) . . . . ? C12 C13 C14 C15 -0.8(4) . . . . ? C16 C13 C14 C15 177.4(2) . . . . ? C11 C10 C15 C14 0.8(4) . . . . ? C9 C10 C15 C14 -175.3(2) . . . . ? C13 C14 C15 C10 0.2(4) . . . . ? C14 C13 C16 C17 -153.9(3) . . . . ? C12 C13 C16 C17 24.2(4) . . . . ? C14 C13 C16 C21 26.8(4) . . . . ? C12 C13 C16 C21 -155.1(3) . . . . ? C21 C16 C17 C18 2.4(4) . . . . ? C13 C16 C17 C18 -176.9(3) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C17 C18 C19 C20 -2.6(4) . . . . ? C17 C18 C19 C22 175.5(3) . . . . ? C18 C19 C20 C21 3.1(4) . . . . ? C22 C19 C20 C21 -174.9(2) . . . . ? C19 C20 C21 C16 -0.9(4) . . . . ? C17 C16 C21 C20 -1.9(4) . . . . ? C13 C16 C21 C20 177.5(2) . . . . ? C18 C19 C22 O22 0.8(3) . . . . ? C20 C19 C22 O22 178.8(2) . . . . ? C18 C19 C22 C23A -121.7(3) . . . . ? C20 C19 C22 C23A 56.3(3) . . . . ? C18 C19 C22 C30A 125.7(3) . . . . ? C20 C19 C22 C30A -56.4(3) . . . . ? C23A C23 C24 C25 0.2(5) . . . . ? C23 C24 C25 C26 0.9(6) . . . . ? C24 C25 C26 C26A -0.8(5) . . . . ? C27A C27 C28 C29 0.8(6) . . . . ? C27 C28 C29 C30 -1.4(6) . . . . ? C28 C29 C30 C30A 0.8(5) . . . . ? O9 C9 C1A C1 62.9(4) . . . . ? C10 C9 C1A C1 -56.2(4) . . . . ? C8A C9 C1A C1 -177.3(3) . . . . ? O9 C9 C1A C4A -118.2(3) . . . . ? C10 C9 C1A C4A 122.8(3) . . . . ? C8A C9 C1A C4A 1.6(3) . . . . ? C1 C1A C4A C4 -1.4(4) . . . . ? C9 C1A C4A C4 179.5(3) . . . . ? C1 C1A C4A C5A 178.2(3) . . . . ? C9 C1A C4A C5A -0.9(3) . . . . ? C3 C4 C4A C1A 0.6(5) . . . . ? C3 C4 C4A C5A -179.0(3) . . . . ? C6 C5 C5A C8A -0.4(5) . . . . ? C6 C5 C5A C4A 180.0(3) . . . . ? C1A C4A C5A C5 179.3(3) . . . . ? C4 C4A C5A C5 -1.1(6) . . . . ? C1A C4A C5A C8A -0.4(3) . . . . ? C4 C4A C5A C8A 179.2(3) . . . . ? C7 C8 C8A C5A -0.5(5) . . . . ? C7 C8 C8A C9 178.3(3) . . . . ? C5 C5A C8A C8 0.8(5) . . . . ? C4A C5A C8A C8 -179.5(3) . . . . ? C5 C5A C8A C9 -178.3(3) . . . . ? C4A C5A C8A C9 1.5(3) . . . . ? O9 C9 C8A C8 -61.2(4) . . . . ? C10 C9 C8A C8 60.5(4) . . . . ? C1A C9 C8A C8 179.2(3) . . . . ? O9 C9 C8A C5A 117.8(3) . . . . ? C10 C9 C8A C5A -120.6(3) . . . . ? C1A C9 C8A C5A -1.9(3) . . . . ? C24 C23 C23A C26A -1.5(4) . . . . ? C24 C23 C23A C22 178.4(3) . . . . ? O22 C22 C23A C23 -61.6(4) . . . . ? C19 C22 C23A C23 58.2(4) . . . . ? C30A C22 C23A C23 178.7(3) . . . . ? O22 C22 C23A C26A 118.3(3) . . . . ? C19 C22 C23A C26A -121.9(2) . . . . ? C30A C22 C23A C26A -1.4(3) . . . . ? C25 C26 C26A C23A -0.4(5) . . . . ? C25 C26 C26A C27A -178.9(3) . . . . ? C23 C23A C26A C26 1.6(4) . . . . ? C22 C23A C26A C26 -178.3(3) . . . . ? C23 C23A C26A C27A -179.6(3) . . . . ? C22 C23A C26A C27A 0.5(3) . . . . ? C28 C27 C27A C30A 0.2(5) . . . . ? C28 C27 C27A C26A 179.2(3) . . . . ? C26 C26A C27A C27 0.3(6) . . . . ? C23A C26A C27A C27 -178.3(3) . . . . ? C26 C26A C27A C30A 179.4(3) . . . . ? C23A C26A C27A C30A 0.8(3) . . . . ? C29 C30 C30A C27A 0.3(5) . . . . ? C29 C30 C30A C22 -177.7(3) . . . . ? C27 C27A C30A C30 -0.8(4) . . . . ? C26A C27A C30A C30 180.0(3) . . . . ? C27 C27A C30A C22 177.5(3) . . . . ? C26A C27A C30A C22 -1.7(3) . . . . ? O22 C22 C30A C30 60.6(4) . . . . ? C19 C22 C30A C30 -61.5(4) . . . . ? C23A C22 C30A C30 180.0(3) . . . . ? O22 C22 C30A C27A -117.5(2) . . . . ? C19 C22 C30A C27A 120.4(3) . . . . ? C23A C22 C30A C27A 1.8(3) . . . . ? C4G N1G C1G O1G -179.2(6) . . . . ? C3G N1G C1G O1G -4.8(8) . . . . ? C4G N1G C1G C2G 2.9(10) . . . . ? C3G N1G C1G C2G 177.2(4) . . . . ? C14G N11G C11G O11G 175.6(5) . . . . ? C13G N11G C11G O11G 1.4(8) . . . . ? C14G N11G C11G C12G -7.4(8) . . . . ? C13G N11G C11G C12G 178.4(4) . . . . ? C24G N21G C21G O21G -174.8(6) . . . . ? C23G N21G C21G O21G 1.6(10) . . . . ? C24G N21G C21G C22G 5.8(11) . . . . ? C23G N21G C21G C22G -177.9(4) . . . . ? C34G N31G C31G O31G -176.6(5) . . . . ? C33G N31G C31G O31G 1.5(8) . . . . ? C34G N31G C31G C32G 4.2(8) . . . . ? C33G N31G C31G C32G -177.7(4) . . . . ? C4A C1A C1 C2 1.5(5) . . . . ? C9 C1A C1 C2 -179.7(3) . . . . ? C3 C2 C1 C1A -0.7(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9 O1G 0.82 1.91 2.723(3) 174.4 . O22 H22 O11G 0.82 1.95 2.754(3) 168.1 . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.652 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.047 #========================================================END data_c:_H.2DMA _database_code_depnum_ccdc_archive 'CCDC 229156' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 9,9'-(Biphenyl-4,4'-diyl)bis(fluoren-9-ol). 2(N,N-dimethylacetamide) clathrate ; _chemical_name_common ;9,9'-(Biphenyl-4,4'-diyl)bis(fluoren-9-ol). 2(N,N- dimethylacetamide) clathrate ; _chemical_melting_point '315.3 (host)' _chemical_formula_moiety 'C38 H26 O2. 2(C4 H9 N O)' _chemical_formula_sum 'C46 H44 N2 O4' _chemical_formula_weight 688.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9629(3) _cell_length_b 9.0266(4) _cell_length_c 13.5092(7) _cell_angle_alpha 77.015(2) _cell_angle_beta 83.033(2) _cell_angle_gamma 84.212(2) _cell_volume 936.47(7) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6852 _cell_measurement_theta_min 1.20 _cell_measurement_theta_max 25.35 _exptl_crystal_description 'clear elongated plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 366 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none _exptl_special_details ; Crystal coated with Paratone oil. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'combination of phi and omega' _diffrn_reflns_number 4708 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3328 _reflns_number_gt 2008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical inerface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0788P)^2^+0.5827P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3328 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 0.1534(5) 0.5309(4) 0.8650(3) 0.0772(11) Uani 1 1 d . . . H1 H 0.0991 0.5553 0.9248 0.093 Uiso 1 1 calc R . . C2 C 0.2003(7) 0.3834(5) 0.8611(5) 0.1127(18) Uani 1 1 d . . . H2 H 0.1760 0.3064 0.9182 0.135 Uiso 1 1 calc R . . C3 C 0.2827(7) 0.3475(5) 0.7743(6) 0.121(2) Uani 1 1 d . . . H3 H 0.3163 0.2460 0.7736 0.145 Uiso 1 1 calc R . . C4 C 0.3182(6) 0.4596(6) 0.6860(5) 0.1048(16) Uani 1 1 d . . . H4 H 0.3739 0.4340 0.6269 0.126 Uiso 1 1 calc R . . C5 C 0.3372(6) 0.7822(8) 0.5101(4) 0.1123(17) Uani 1 1 d . . . H5 H 0.3899 0.7034 0.4808 0.135 Uiso 1 1 calc R . . C6 C 0.3203(9) 0.9263(11) 0.4536(4) 0.142(3) Uani 1 1 d . . . H6 H 0.3632 0.9456 0.3852 0.170 Uiso 1 1 calc R . . C7 C 0.2418(8) 1.0444(7) 0.4945(4) 0.125(2) Uani 1 1 d . . . H7 H 0.2294 1.1415 0.4532 0.150 Uiso 1 1 calc R . . C8 C 0.1797(5) 1.0196(5) 0.5984(3) 0.0851(12) Uani 1 1 d . . . H8 H 0.1288 1.0994 0.6273 0.102 Uiso 1 1 calc R . . O9 O -0.0302(2) 0.8534(3) 0.79739(18) 0.0647(7) Uani 1 1 d . . . H9 H -0.0894 0.8052 0.7723 0.078 Uiso 1 1 calc R . . C9 C 0.1439(3) 0.8152(3) 0.7688(2) 0.0452(7) Uani 1 1 d . . . C10 C 0.2491(3) 0.8760(3) 0.8359(2) 0.0426(7) Uani 1 1 d . . . C11 C 0.4239(4) 0.8716(4) 0.8179(2) 0.0604(9) Uani 1 1 d . . . H11 H 0.4774 0.8356 0.7619 0.072 Uiso 1 1 calc R . . C12 C 0.5206(4) 0.9194(4) 0.8809(2) 0.0582(9) Uani 1 1 d . . . H12 H 0.6379 0.9149 0.8662 0.070 Uiso 1 1 calc R . . C13 C 0.4481(3) 0.9744(3) 0.9658(2) 0.0384(6) Uani 1 1 d . . . C14 C 0.2737(3) 0.9791(4) 0.9822(2) 0.0544(8) Uani 1 1 d . . . H14 H 0.2194 1.0160 1.0377 0.065 Uiso 1 1 calc R . . C15 C 0.1765(4) 0.9308(4) 0.9190(2) 0.0561(8) Uani 1 1 d . . . H15 H 0.0591 0.9356 0.9334 0.067 Uiso 1 1 calc R . . C1A C 0.1868(4) 0.6441(3) 0.7796(2) 0.0517(8) Uani 1 1 d . . . C4A C 0.2669(4) 0.6119(4) 0.6895(3) 0.0653(9) Uani 1 1 d . . . C5A C 0.2744(4) 0.7546(5) 0.6123(3) 0.0682(10) Uani 1 1 d . . . C8A C 0.1970(4) 0.8732(4) 0.6557(2) 0.0559(8) Uani 1 1 d . . . O1G O -0.2295(3) 0.6762(3) 0.7270(2) 0.0750(7) Uani 1 1 d . . . N1G N -0.2080(5) 0.4279(5) 0.7263(4) 0.1216(16) Uani 1 1 d . . . C1G C -0.2427(5) 0.5376(7) 0.7625(5) 0.1090(18) Uani 1 1 d . . . C2G C -0.3288(6) 0.4884(6) 0.8799(3) 0.1062(15) Uani 1 1 d . . . H18A H -0.4422 0.4611 0.8798 0.159 Uiso 1 1 calc R . . H18B H -0.3319 0.5723 0.9130 0.159 Uiso 1 1 calc R . . H18C H -0.2628 0.4027 0.9159 0.159 Uiso 1 1 calc R . . C3G C -0.1227(7) 0.4805(7) 0.6135(3) 0.1190(18) Uani 1 1 d . . . H20A H -0.1971 0.5565 0.5752 0.178 Uiso 1 1 calc R . . H20B H -0.1020 0.3944 0.5817 0.178 Uiso 1 1 calc R . . H20C H -0.0172 0.5225 0.6149 0.178 Uiso 1 1 calc R . . C4G C -0.2211(7) 0.2676(5) 0.7664(4) 0.1152(17) Uani 1 1 d . . . H21A H -0.1217 0.2249 0.7995 0.173 Uiso 1 1 calc R . . H21B H -0.2306 0.2181 0.7116 0.173 Uiso 1 1 calc R . . H21C H -0.3198 0.2526 0.8149 0.173 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 0.080(3) 0.061(2) 0.094(3) -0.004(2) -0.030(2) -0.0210(19) C2 0.120(4) 0.058(3) 0.163(5) -0.004(3) -0.057(4) -0.015(3) C3 0.115(4) 0.053(3) 0.211(7) -0.043(4) -0.068(4) 0.014(3) C4 0.088(3) 0.100(4) 0.154(5) -0.084(4) -0.030(3) 0.015(3) C5 0.107(4) 0.181(6) 0.067(3) -0.060(3) 0.014(3) -0.051(4) C6 0.160(6) 0.218(8) 0.062(3) -0.024(4) -0.004(3) -0.106(6) C7 0.156(5) 0.135(5) 0.082(4) 0.035(3) -0.058(4) -0.075(4) C8 0.097(3) 0.075(3) 0.085(3) 0.003(2) -0.037(2) -0.024(2) O9 0.0387(12) 0.0814(16) 0.0876(17) -0.0460(13) -0.0098(11) -0.0023(10) C9 0.0355(15) 0.0493(17) 0.0553(18) -0.0201(14) -0.0045(13) -0.0041(12) C10 0.0387(15) 0.0418(15) 0.0499(17) -0.0148(13) -0.0055(12) -0.0027(12) C11 0.0416(17) 0.088(2) 0.064(2) -0.0477(18) 0.0023(15) -0.0045(15) C12 0.0341(15) 0.082(2) 0.070(2) -0.0422(18) 0.0024(14) -0.0091(14) C13 0.0342(14) 0.0347(14) 0.0463(16) -0.0092(11) -0.0034(11) -0.0030(11) C14 0.0387(16) 0.077(2) 0.0551(18) -0.0328(16) -0.0014(13) -0.0014(14) C15 0.0320(15) 0.080(2) 0.065(2) -0.0373(17) -0.0019(14) -0.0015(14) C1A 0.0462(17) 0.0462(17) 0.068(2) -0.0160(16) -0.0163(15) -0.0069(13) C4A 0.055(2) 0.067(2) 0.086(3) -0.042(2) -0.0153(18) 0.0044(16) C5A 0.060(2) 0.101(3) 0.056(2) -0.039(2) -0.0025(16) -0.0181(19) C8A 0.0535(18) 0.064(2) 0.0544(19) -0.0115(16) -0.0173(15) -0.0135(15) O1G 0.0701(16) 0.0665(17) 0.0948(19) -0.0227(14) -0.0166(13) -0.0138(12) N1G 0.109(3) 0.077(3) 0.189(5) -0.024(3) -0.055(3) -0.015(2) C1G 0.068(3) 0.103(4) 0.182(6) -0.065(4) -0.066(3) 0.008(3) C2G 0.116(4) 0.144(4) 0.058(3) -0.024(3) 0.004(2) -0.015(3) C3G 0.126(4) 0.163(5) 0.068(3) -0.031(3) 0.023(3) -0.035(3) C4G 0.161(5) 0.063(3) 0.119(4) -0.009(3) -0.012(3) -0.023(3) _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 C2 1.356(6) . ? C1 C1A 1.377(5) . ? C2 C3 1.362(8) . ? C3 C4 1.400(8) . ? C4 C4A 1.403(5) . ? C5 C6 1.354(8) . ? C5 C5A 1.386(6) . ? C6 C7 1.371(8) . ? C7 C8 1.406(7) . ? C8 C8A 1.377(5) . ? O9 C9 1.423(3) . ? C9 C8A 1.521(4) . ? C9 C10 1.524(4) . ? C9 C1A 1.526(4) . ? C10 C15 1.369(4) . ? C10 C11 1.381(4) . ? C11 C12 1.376(4) . ? C12 C13 1.390(4) . ? C13 C14 1.378(4) . ? C13 C13 1.484(5) 2_677 ? C14 C15 1.383(4) . ? C1A C4A 1.381(4) . ? C4A C5A 1.466(5) . ? C5A C8A 1.390(5) . ? O1G C1G 1.245(6) . ? N1G C1G 1.194(6) . ? N1G C4G 1.436(5) . ? N1G C3G 1.580(6) . ? C1G C2G 1.632(7) . ? 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 C2 C1 C1A 119.5(5) . . ? C1 C2 C3 120.4(5) . . ? C2 C3 C4 121.6(4) . . ? C3 C4 C4A 117.9(4) . . ? C6 C5 C5A 118.8(5) . . ? C5 C6 C7 121.9(5) . . ? C6 C7 C8 120.4(5) . . ? C8A C8 C7 117.7(4) . . ? O9 C9 C8A 113.1(2) . . ? O9 C9 C10 107.9(2) . . ? C8A C9 C10 111.9(2) . . ? O9 C9 C1A 113.1(2) . . ? C8A C9 C1A 101.0(2) . . ? C10 C9 C1A 109.7(2) . . ? C15 C10 C11 116.9(2) . . ? C15 C10 C9 121.9(2) . . ? C11 C10 C9 121.1(2) . . ? C12 C11 C10 121.5(3) . . ? C11 C12 C13 122.0(3) . . ? C14 C13 C12 115.7(2) . . ? C14 C13 C13 122.1(3) . 2_677 ? C12 C13 C13 122.2(3) . 2_677 ? C13 C14 C15 122.3(3) . . ? C10 C15 C14 121.6(3) . . ? C1 C1A C4A 121.8(3) . . ? C1 C1A C9 127.3(3) . . ? C4A C1A C9 111.0(3) . . ? C1A C4A C4 118.8(4) . . ? C1A C4A C5A 108.5(3) . . ? C4 C4A C5A 132.7(4) . . ? C5 C5A C8A 120.3(4) . . ? C5 C5A C4A 130.8(4) . . ? C8A C5A C4A 108.8(3) . . ? C8 C8A C5A 121.0(3) . . ? C8 C8A C9 128.6(3) . . ? C5A C8A C9 110.4(3) . . ? C1G N1G C4G 133.1(6) . . ? C1G N1G C3G 108.7(5) . . ? C4G N1G C3G 118.1(5) . . ? N1G C1G O1G 132.5(6) . . ? N1G C1G C2G 110.4(6) . . ? O1G C1G C2G 117.1(4) . . ? 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 C1A C1 C2 C3 1.3(6) . . . . ? C1 C2 C3 C4 -1.5(8) . . . . ? C2 C3 C4 C4A 0.4(7) . . . . ? C5A C5 C6 C7 -0.6(8) . . . . ? C5 C6 C7 C8 1.7(9) . . . . ? C6 C7 C8 C8A -1.6(7) . . . . ? O9 C9 C10 C15 10.5(4) . . . . ? C8A C9 C10 C15 135.7(3) . . . . ? C1A C9 C10 C15 -113.1(3) . . . . ? O9 C9 C10 C11 -172.5(3) . . . . ? C8A C9 C10 C11 -47.3(4) . . . . ? C1A C9 C10 C11 63.9(3) . . . . ? C15 C10 C11 C12 0.3(5) . . . . ? C9 C10 C11 C12 -176.8(3) . . . . ? C10 C11 C12 C13 0.1(5) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C11 C12 C13 C13 179.8(3) . . . 2_677 ? C12 C13 C14 C15 0.7(4) . . . . ? C13 C13 C14 C15 -179.7(3) 2_677 . . . ? C11 C10 C15 C14 -0.2(5) . . . . ? C9 C10 C15 C14 176.9(3) . . . . ? C13 C14 C15 C10 -0.3(5) . . . . ? C2 C1 C1A C4A 0.1(5) . . . . ? C2 C1 C1A C9 179.8(3) . . . . ? O9 C9 C1A C1 -53.3(4) . . . . ? C8A C9 C1A C1 -174.6(3) . . . . ? C10 C9 C1A C1 67.1(4) . . . . ? O9 C9 C1A C4A 126.4(3) . . . . ? C8A C9 C1A C4A 5.2(3) . . . . ? C10 C9 C1A C4A -113.1(3) . . . . ? C1 C1A C4A C4 -1.2(5) . . . . ? C9 C1A C4A C4 179.0(3) . . . . ? C1 C1A C4A C5A 176.6(3) . . . . ? C9 C1A C4A C5A -3.1(3) . . . . ? C3 C4 C4A C1A 0.9(5) . . . . ? C3 C4 C4A C5A -176.3(4) . . . . ? C6 C5 C5A C8A -0.6(6) . . . . ? C6 C5 C5A C4A 176.6(4) . . . . ? C1A C4A C5A C5 -178.0(4) . . . . ? C4 C4A C5A C5 -0.5(7) . . . . ? C1A C4A C5A C8A -0.5(4) . . . . ? C4 C4A C5A C8A 176.9(4) . . . . ? C7 C8 C8A C5A 0.5(5) . . . . ? C7 C8 C8A C9 179.1(3) . . . . ? C5 C5A C8A C8 0.6(5) . . . . ? C4A C5A C8A C8 -177.1(3) . . . . ? C5 C5A C8A C9 -178.3(3) . . . . ? C4A C5A C8A C9 4.0(3) . . . . ? O9 C9 C8A C8 54.6(4) . . . . ? C10 C9 C8A C8 -67.6(4) . . . . ? C1A C9 C8A C8 175.8(3) . . . . ? O9 C9 C8A C5A -126.7(3) . . . . ? C10 C9 C8A C5A 111.2(3) . . . . ? C1A C9 C8A C5A -5.5(3) . . . . ? C4G N1G C1G O1G 179.4(4) . . . . ? C3G N1G C1G O1G 3.0(7) . . . . ? C4G N1G C1G C2G -2.8(7) . . . . ? C3G N1G C1G C2G -179.2(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9 O1G 0.82 1.93 2.747(3) 173.9 . _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.565 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.040 #========================================================END data_c:_H.3DIOX _database_code_depnum_ccdc_archive 'CCDC 229157' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 9,9'-(Biphenyl-4,4'-diyl)bis(fluoren-9-ol). 3(1,4-dioxane) clathrate ; _chemical_name_common ;9,9'-(Biphenyl-4,4'-diyl)bis(fluoren-9-ol). 3(1,4-dioxane) clathrate ; _chemical_melting_point '317.8 (host)' _chemical_formula_moiety 'C38 H26 O2. 3(C4 H8 O2)' _chemical_formula_sum 'C50 H50 O8' _chemical_formula_weight 778.90 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 13.1096(3) _cell_length_b 12.8883(2) _cell_length_c 12.0038(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.2470(10) _cell_angle_gamma 90.00 _cell_volume 2026.61(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4851 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'clear plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type none _exptl_special_details ; Crystal coated with Paratone oil. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'combination of phi and omega' _diffrn_reflns_number 7890 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4628 _reflns_number_gt 3355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0546P)^2^+0.4259P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4628 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.18616(11) 0.22488(11) 0.80966(11) 0.0286(3) Uani 1 1 d . . . H1 H 0.2335 0.2551 0.7612 0.034 Uiso 1 1 calc R . . C2 C 0.08179(11) 0.23409(11) 0.78734(12) 0.0328(3) Uani 1 1 d . . . H2 H 0.0576 0.2696 0.7222 0.039 Uiso 1 1 calc R . . C3 C 0.01257(11) 0.19204(11) 0.85922(13) 0.0341(4) Uani 1 1 d . . . H3 H -0.0586 0.1986 0.8425 0.041 Uiso 1 1 calc R . . C4 C 0.04622(11) 0.14038(11) 0.95542(12) 0.0297(3) Uani 1 1 d . . . H4 H -0.0012 0.1129 1.0054 0.036 Uiso 1 1 calc R . . C5 C 0.17446(11) 0.02040(11) 1.15838(12) 0.0302(3) Uani 1 1 d . . . H5 H 0.1038 0.0166 1.1729 0.036 Uiso 1 1 calc R . . C6 C 0.24630(13) -0.02930(12) 1.22752(13) 0.0382(4) Uani 1 1 d . . . H6 H 0.2246 -0.0674 1.2901 0.046 Uiso 1 1 calc R . . C7 C 0.34947(13) -0.02392(13) 1.20625(14) 0.0423(4) Uani 1 1 d . . . H7 H 0.3976 -0.0596 1.2535 0.051 Uiso 1 1 calc R . . C8 C 0.38320(12) 0.03309(12) 1.11650(13) 0.0357(4) Uani 1 1 d . . . H8 H 0.4539 0.0372 1.1025 0.043 Uiso 1 1 calc R . . O9 O 0.38478(7) 0.09107(8) 0.86233(8) 0.0315(3) Uani 1 1 d . . . H9 H 0.3618 0.0304 0.8571 0.038 Uiso 1 1 calc R . . C9 C 0.32997(10) 0.14716(10) 0.94355(11) 0.0240(3) Uani 1 1 d . . . C10 C 0.38772(10) 0.24840(10) 0.96484(11) 0.0236(3) Uani 1 1 d . . . C11 C 0.37418(13) 0.30623(12) 1.05984(13) 0.0399(4) Uani 1 1 d . . . H11 H 0.3335 0.2789 1.1166 0.048 Uiso 1 1 calc R . . C12 C 0.41846(13) 0.40310(12) 1.07448(13) 0.0386(4) Uani 1 1 d . . . H12 H 0.4080 0.4404 1.1413 0.046 Uiso 1 1 calc R . . C13 C 0.47791(10) 0.44695(10) 0.99338(11) 0.0232(3) Uani 1 1 d . . . C14 C 0.49458(12) 0.38617(12) 0.90076(12) 0.0344(4) Uani 1 1 d . . . H14 H 0.5376 0.4120 0.8452 0.041 Uiso 1 1 calc R . . C15 C 0.45085(11) 0.28910(12) 0.88615(12) 0.0333(4) Uani 1 1 d . . . H15 H 0.4644 0.2500 0.8213 0.040 Uiso 1 1 calc R . . C1A C 0.21989(10) 0.17099(10) 0.90359(11) 0.0228(3) Uani 1 1 d . . . C4A C 0.15020(10) 0.12972(10) 0.97700(11) 0.0228(3) Uani 1 1 d . . . C5A C 0.20784(10) 0.07578(10) 1.06752(11) 0.0234(3) Uani 1 1 d . . . C8A C 0.31229(10) 0.08346(10) 1.04822(11) 0.0252(3) Uani 1 1 d . . . O1G O 0.33336(8) -0.11056(8) 0.81227(9) 0.0399(3) Uani 1 1 d . . . C1G C 0.32813(14) -0.20020(13) 0.88245(16) 0.0472(4) Uani 1 1 d . . . H1GA H 0.3836 -0.1973 0.9408 0.057 Uiso 1 1 calc R . . H1GB H 0.3377 -0.2636 0.8375 0.057 Uiso 1 1 calc R . . O2G O 0.14475(9) -0.20379(9) 0.85499(9) 0.0447(3) Uani 1 1 d . . . C2G C 0.22680(14) -0.20493(14) 0.93634(14) 0.0478(4) Uani 1 1 d . . . H2GA H 0.2231 -0.2690 0.9814 0.057 Uiso 1 1 calc R . . H2GB H 0.2203 -0.1449 0.9870 0.057 Uiso 1 1 calc R . . C3G C 0.15100(13) -0.11415(13) 0.78673(14) 0.0420(4) Uani 1 1 d . . . H3GA H 0.1440 -0.0511 0.8329 0.050 Uiso 1 1 calc R . . H3GB H 0.0945 -0.1147 0.7295 0.050 Uiso 1 1 calc R . . C4G C 0.25078(14) -0.11170(14) 0.73120(14) 0.0466(4) Uani 1 1 d . . . H4GA H 0.2566 -0.1734 0.6828 0.056 Uiso 1 1 calc R . . H4GB H 0.2542 -0.0491 0.6837 0.056 Uiso 1 1 calc R . . O11G O -0.09632(9) 0.04916(9) 0.48636(10) 0.0457(3) Uani 1 1 d . . . C11G C -0.01925(15) 0.08647(14) 0.56285(15) 0.0490(5) Uani 1 1 d . . . H1G2 H -0.0292 0.0557 0.6372 0.059 Uiso 1 1 calc R . . H1G1 H -0.0255 0.1627 0.5697 0.059 Uiso 1 1 calc R . . C14G C -0.08458(14) -0.06008(13) 0.47404(17) 0.0502(5) Uani 1 1 d . . . H4G1 H -0.1363 -0.0862 0.4186 0.060 Uiso 1 1 calc R . . H4G2 H -0.0963 -0.0946 0.5461 0.060 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 0.0312(8) 0.0285(7) 0.0262(7) -0.0009(6) 0.0028(6) -0.0003(6) C2 0.0356(8) 0.0312(8) 0.0311(8) 0.0013(7) -0.0066(6) 0.0010(6) C3 0.0243(8) 0.0314(8) 0.0461(9) 0.0004(7) -0.0057(7) 0.0005(6) C4 0.0235(7) 0.0274(7) 0.0385(8) 0.0003(6) 0.0052(6) -0.0029(6) C5 0.0312(8) 0.0265(7) 0.0333(8) 0.0023(6) 0.0066(6) -0.0044(6) C6 0.0461(10) 0.0333(8) 0.0352(8) 0.0121(7) 0.0006(7) -0.0063(7) C7 0.0408(9) 0.0380(9) 0.0470(10) 0.0154(8) -0.0112(8) -0.0041(7) C8 0.0262(8) 0.0338(8) 0.0467(9) 0.0083(7) -0.0038(7) -0.0029(6) O9 0.0298(6) 0.0267(5) 0.0389(6) -0.0063(5) 0.0123(5) -0.0010(4) C9 0.0210(7) 0.0247(7) 0.0265(7) -0.0011(6) 0.0045(5) -0.0002(5) C10 0.0201(7) 0.0255(7) 0.0252(7) 0.0025(6) 0.0013(5) -0.0010(5) C11 0.0490(10) 0.0365(8) 0.0357(8) -0.0056(7) 0.0224(7) -0.0161(7) C12 0.0500(10) 0.0342(8) 0.0330(8) -0.0080(7) 0.0192(7) -0.0127(7) C13 0.0194(7) 0.0268(7) 0.0235(7) 0.0022(6) 0.0022(5) -0.0028(5) C14 0.0377(9) 0.0359(8) 0.0309(8) -0.0044(7) 0.0171(7) -0.0125(6) C15 0.0363(8) 0.0348(8) 0.0298(8) -0.0083(7) 0.0122(6) -0.0086(6) C1A 0.0239(7) 0.0213(6) 0.0235(7) -0.0046(6) 0.0026(5) -0.0017(5) C4A 0.0232(7) 0.0195(6) 0.0258(7) -0.0035(5) 0.0020(5) -0.0019(5) C5A 0.0248(7) 0.0192(6) 0.0264(7) -0.0033(6) 0.0025(5) -0.0024(5) C8A 0.0251(7) 0.0210(6) 0.0295(7) -0.0002(6) 0.0013(6) -0.0035(5) O1G 0.0365(6) 0.0401(6) 0.0434(6) -0.0056(5) 0.0055(5) -0.0116(5) C1G 0.0461(10) 0.0338(9) 0.0609(11) -0.0031(8) -0.0058(8) -0.0018(7) O2G 0.0422(7) 0.0478(7) 0.0441(7) 0.0047(6) 0.0030(5) -0.0183(5) C2G 0.0575(12) 0.0474(10) 0.0383(9) 0.0065(8) -0.0011(8) -0.0135(8) C3G 0.0402(10) 0.0393(9) 0.0462(10) 0.0014(8) -0.0035(8) -0.0097(7) C4G 0.0510(11) 0.0541(11) 0.0347(9) 0.0008(8) 0.0014(8) -0.0209(8) O11G 0.0465(7) 0.0398(6) 0.0501(7) -0.0007(5) -0.0057(5) 0.0120(5) C11G 0.0606(12) 0.0400(9) 0.0458(10) -0.0093(8) -0.0064(9) 0.0129(8) C14G 0.0490(11) 0.0357(9) 0.0652(12) 0.0010(9) -0.0084(9) 0.0012(8) _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 C1A 1.3820(19) . ? C1 C2 1.389(2) . ? C2 C3 1.387(2) . ? C3 C4 1.390(2) . ? C4 C4A 1.3843(19) . ? C5 C6 1.387(2) . ? C5 C5A 1.3885(19) . ? C6 C7 1.388(2) . ? C7 C8 1.390(2) . ? C8 C8A 1.377(2) . ? O9 C9 1.4297(15) . ? C9 C10 1.5251(18) . ? C9 C8A 1.5262(19) . ? C9 C1A 1.5338(19) . ? C10 C11 1.380(2) . ? C10 C15 1.3833(19) . ? C11 C12 1.385(2) . ? C12 C13 1.3907(19) . ? C13 C14 1.384(2) . ? C13 C13 1.491(3) 3_667 ? C14 C15 1.384(2) . ? C1A C4A 1.3991(18) . ? C4A C5A 1.4734(19) . ? C5A C8A 1.4011(19) . ? O1G C4G 1.427(2) . ? O1G C1G 1.433(2) . ? C1G C2G 1.501(2) . ? O2G C3G 1.421(2) . ? O2G C2G 1.424(2) . ? C3G C4G 1.491(2) . ? O11G C11G 1.422(2) . ? O11G C14G 1.425(2) . ? C11G C14G 1.487(3) 3_556 ? C14G C11G 1.487(3) 3_556 ? 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 C1A C1 C2 118.79(13) . . ? C3 C2 C1 120.68(13) . . ? C2 C3 C4 120.67(13) . . ? C4A C4 C3 118.76(13) . . ? C6 C5 C5A 118.67(14) . . ? C7 C6 C5 120.69(14) . . ? C6 C7 C8 120.71(15) . . ? C8A C8 C7 118.84(14) . . ? O9 C9 C10 106.70(10) . . ? O9 C9 C8A 112.71(11) . . ? C10 C9 C8A 114.38(11) . . ? O9 C9 C1A 112.32(11) . . ? C10 C9 C1A 109.62(11) . . ? C8A C9 C1A 101.18(10) . . ? C11 C10 C15 117.35(13) . . ? C11 C10 C9 121.44(12) . . ? C15 C10 C9 121.08(12) . . ? C10 C11 C12 121.67(13) . . ? C11 C12 C13 121.40(14) . . ? C14 C13 C12 116.27(13) . . ? C14 C13 C13 122.11(14) . 3_667 ? C12 C13 C13 121.61(15) . 3_667 ? C13 C14 C15 122.37(13) . . ? C10 C15 C14 120.80(13) . . ? C1 C1A C4A 120.59(13) . . ? C1 C1A C9 128.52(12) . . ? C4A C1A C9 110.89(11) . . ? C4 C4A C1A 120.47(13) . . ? C4 C4A C5A 131.12(12) . . ? C1A C4A C5A 108.37(11) . . ? C5 C5A C8A 120.42(13) . . ? C5 C5A C4A 130.81(13) . . ? C8A C5A C4A 108.73(11) . . ? C8 C8A C5A 120.63(13) . . ? C8 C8A C9 128.50(13) . . ? C5A C8A C9 110.80(12) . . ? C4G O1G C1G 109.88(12) . . ? O1G C1G C2G 110.46(14) . . ? C3G O2G C2G 110.17(12) . . ? O2G C2G C1G 111.19(14) . . ? O2G C3G C4G 110.27(15) . . ? O1G C4G C3G 110.52(13) . . ? C11G O11G C14G 108.92(12) . . ? O11G C11G C14G 111.46(14) . 3_556 ? O11G C14G C11G 111.15(15) . 3_556 ? 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 C1A C1 C2 C3 1.4(2) . . . . ? C1 C2 C3 C4 0.4(2) . . . . ? C2 C3 C4 C4A -1.4(2) . . . . ? C5A C5 C6 C7 -0.1(2) . . . . ? C5 C6 C7 C8 1.3(2) . . . . ? C6 C7 C8 C8A -0.6(2) . . . . ? O9 C9 C10 C11 -160.70(13) . . . . ? C8A C9 C10 C11 -35.36(18) . . . . ? C1A C9 C10 C11 77.43(16) . . . . ? O9 C9 C10 C15 23.47(17) . . . . ? C8A C9 C10 C15 148.81(13) . . . . ? C1A C9 C10 C15 -98.40(15) . . . . ? C15 C10 C11 C12 2.5(2) . . . . ? C9 C10 C11 C12 -173.46(15) . . . . ? C10 C11 C12 C13 0.6(3) . . . . ? C11 C12 C13 C14 -3.4(2) . . . . ? C11 C12 C13 C13 177.36(17) . . . 3_667 ? C12 C13 C14 C15 3.1(2) . . . . ? C13 C13 C14 C15 -177.67(16) 3_667 . . . ? C11 C10 C15 C14 -2.8(2) . . . . ? C9 C10 C15 C14 173.16(14) . . . . ? C13 C14 C15 C10 0.0(3) . . . . ? C2 C1 C1A C4A -2.3(2) . . . . ? C2 C1 C1A C9 177.67(13) . . . . ? O9 C9 C1A C1 -57.81(18) . . . . ? C10 C9 C1A C1 60.62(17) . . . . ? C8A C9 C1A C1 -178.24(13) . . . . ? O9 C9 C1A C4A 122.15(12) . . . . ? C10 C9 C1A C4A -119.41(12) . . . . ? C8A C9 C1A C4A 1.72(13) . . . . ? C3 C4 C4A C1A 0.5(2) . . . . ? C3 C4 C4A C5A -176.79(13) . . . . ? C1 C1A C4A C4 1.35(19) . . . . ? C9 C1A C4A C4 -178.61(12) . . . . ? C1 C1A C4A C5A 179.20(12) . . . . ? C9 C1A C4A C5A -0.77(14) . . . . ? C6 C5 C5A C8A -1.7(2) . . . . ? C6 C5 C5A C4A 175.47(14) . . . . ? C4 C4A C5A C5 -0.6(2) . . . . ? C1A C4A C5A C5 -178.11(13) . . . . ? C4 C4A C5A C8A 176.89(14) . . . . ? C1A C4A C5A C8A -0.64(15) . . . . ? C7 C8 C8A C5A -1.2(2) . . . . ? C7 C8 C8A C9 -177.81(14) . . . . ? C5 C5A C8A C8 2.4(2) . . . . ? C4A C5A C8A C8 -175.34(13) . . . . ? C5 C5A C8A C9 179.58(12) . . . . ? C4A C5A C8A C9 1.80(15) . . . . ? O9 C9 C8A C8 54.59(19) . . . . ? C10 C9 C8A C8 -67.53(18) . . . . ? C1A C9 C8A C8 174.74(14) . . . . ? O9 C9 C8A C5A -122.27(12) . . . . ? C10 C9 C8A C5A 115.61(13) . . . . ? C1A C9 C8A C5A -2.12(14) . . . . ? C4G O1G C1G C2G -56.54(17) . . . . ? C3G O2G C2G C1G -56.89(18) . . . . ? O1G C1G C2G O2G 56.24(19) . . . . ? C2G O2G C3G C4G 58.14(17) . . . . ? C1G O1G C4G C3G 58.36(18) . . . . ? O2G C3G C4G O1G -59.42(18) . . . . ? C14G O11G C11G C14G 57.0(2) . . . 3_556 ? C11G O11G C14G C11G -56.8(2) . . . 3_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.287 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.040 #========================================================END data_c:_H.2MEK _database_code_depnum_ccdc_archive 'CCDC 229158' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 9,9'-(Biphenyl-4,4'-diyl)bis(flouren-9-ol). 2(methyl ethyl ketone) clathrate ; _chemical_name_common ;9,9'-(Biphenyl-4,4'-diyl)bis(flouren-9-ol). 2(methyl ethyl ketone) clathrate ; _chemical_melting_point '318.0 (host)' _chemical_formula_moiety 'C38 H26 O2. 2(C4 H8 O)' _chemical_formula_sum 'C46 H42 O4' _chemical_formula_weight 658.80 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.79930(10) _cell_length_b 21.9845(4) _cell_length_c 21.0296(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.5520(10) _cell_angle_gamma 90.00 _cell_volume 3594.44(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14205 _cell_measurement_theta_min 0.21 _cell_measurement_theta_max 26.37 _exptl_crystal_description 'clear plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_special_details ; Crystal coated with paratone oil. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'combination of phi and omega' _diffrn_reflns_number 17163 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.39 _reflns_number_total 7322 _reflns_number_gt 5891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0432P)^2^+1.1046P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7322 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.003 _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 1.21468(19) 0.09460(7) 0.24449(7) 0.0372(3) Uani 1 1 d . . . H1 H 1.2255 0.1216 0.2098 0.045 Uiso 1 1 calc R . . C2 C 1.2662(2) 0.11233(8) 0.30682(7) 0.0455(4) Uani 1 1 d . . . H2 H 1.3119 0.1519 0.3147 0.055 Uiso 1 1 calc R . . C3 C 1.2511(2) 0.07253(8) 0.35731(7) 0.0469(4) Uani 1 1 d . . . H3 H 1.2865 0.0853 0.3995 0.056 Uiso 1 1 calc R . . C4 C 1.18559(19) 0.01478(8) 0.34716(7) 0.0406(4) Uani 1 1 d . . . H4 H 1.1766 -0.0124 0.3819 0.049 Uiso 1 1 calc R . . C5 C 1.0003(2) -0.11137(8) 0.29138(7) 0.0438(4) Uani 1 1 d . . . H5 H 1.0234 -0.1157 0.3362 0.053 Uiso 1 1 calc R . . C6 C 0.9151(2) -0.15665(8) 0.25581(9) 0.0536(4) Uani 1 1 d . . . H6 H 0.8770 -0.1920 0.2766 0.064 Uiso 1 1 calc R . . C7 C 0.8847(2) -0.15115(8) 0.19021(9) 0.0528(4) Uani 1 1 d . . . H7 H 0.8273 -0.1829 0.1665 0.063 Uiso 1 1 calc R . . C8 C 0.9373(2) -0.09966(7) 0.15893(7) 0.0414(4) Uani 1 1 d . . . H8 H 0.9174 -0.0961 0.1139 0.050 Uiso 1 1 calc R . . O9 O 0.92682(12) 0.04249(5) 0.14485(4) 0.0344(2) Uani 1 1 d . . . H9 H 0.8660 0.0533 0.1741 0.041 Uiso 1 1 calc R . . C9 C 1.07285(16) 0.00918(6) 0.17172(6) 0.0285(3) Uani 1 1 d . . . C10 C 1.20122(16) 0.00651(6) 0.12052(6) 0.0270(3) Uani 1 1 d . . . C11 C 1.3674(2) -0.01274(10) 0.13441(7) 0.0597(6) Uani 1 1 d . . . H11 H 1.4032 -0.0248 0.1768 0.072 Uiso 1 1 calc R . . C12 C 1.4843(2) -0.01500(11) 0.08814(7) 0.0612(6) Uani 1 1 d . . . H12 H 1.5989 -0.0279 0.0997 0.073 Uiso 1 1 calc R . . C13 C 1.43782(16) 0.00115(6) 0.02533(6) 0.0261(3) Uani 1 1 d . . . C14 C 1.27019(17) 0.01936(7) 0.01177(6) 0.0325(3) Uani 1 1 d . . . H14 H 1.2326 0.0300 -0.0309 0.039 Uiso 1 1 calc R . . C15 C 1.15387(17) 0.02273(7) 0.05849(6) 0.0325(3) Uani 1 1 d . . . H15 H 1.0399 0.0365 0.0473 0.039 Uiso 1 1 calc R . . C16 C 1.93459(16) -0.02400(6) 0.49142(6) 0.0250(3) Uani 1 1 d . . . C17 C 1.76019(16) -0.01016(6) 0.48090(6) 0.0272(3) Uani 1 1 d . . . H17 H 1.7244 0.0311 0.4828 0.033 Uiso 1 1 calc R . . C18 C 1.63770(17) -0.05508(6) 0.46772(6) 0.0288(3) Uani 1 1 d . . . H18 H 1.5201 -0.0440 0.4604 0.035 Uiso 1 1 calc R . . C19 C 1.68363(16) -0.11595(6) 0.46497(6) 0.0275(3) Uani 1 1 d . . . C20 C 1.85744(17) -0.12985(6) 0.47250(7) 0.0360(3) Uani 1 1 d . . . H20 H 1.8931 -0.1709 0.4688 0.043 Uiso 1 1 calc R . . C21 C 1.98002(17) -0.08508(6) 0.48528(7) 0.0340(3) Uani 1 1 d . . . H21 H 2.0981 -0.0961 0.4900 0.041 Uiso 1 1 calc R . . O22 O 1.39524(12) -0.14263(4) 0.48035(5) 0.0406(3) Uani 1 1 d . . . H22 H 1.3146 -0.1677 0.4734 0.049 Uiso 1 1 calc R . . C22 C 1.54672(17) -0.16533(6) 0.45412(7) 0.0315(3) Uani 1 1 d . . . C23 C 1.45114(19) -0.14539(7) 0.33359(8) 0.0413(4) Uani 1 1 d . . . H23 H 1.4253 -0.1038 0.3405 0.050 Uiso 1 1 calc R . . C24 C 1.4268(2) -0.17060(8) 0.27308(8) 0.0504(4) Uani 1 1 d . . . H24 H 1.3825 -0.1462 0.2383 0.060 Uiso 1 1 calc R . . C25 C 1.4662(2) -0.23100(9) 0.26284(8) 0.0516(4) Uani 1 1 d . . . H25 H 1.4497 -0.2474 0.2210 0.062 Uiso 1 1 calc R . . C26 C 1.5294(2) -0.26787(8) 0.31261(8) 0.0450(4) Uani 1 1 d . . . H26 H 1.5576 -0.3092 0.3052 0.054 Uiso 1 1 calc R . . C27 C 1.6489(2) -0.33072(7) 0.45207(9) 0.0461(4) Uani 1 1 d . . . H27 H 1.6494 -0.3614 0.4203 0.055 Uiso 1 1 calc R . . C28 C 1.6921(2) -0.34446(8) 0.51576(9) 0.0539(4) Uani 1 1 d . . . H28 H 1.7226 -0.3850 0.5275 0.065 Uiso 1 1 calc R . . C29 C 1.6915(2) -0.30002(8) 0.56239(9) 0.0525(4) Uani 1 1 d . . . H29 H 1.7220 -0.3102 0.6057 0.063 Uiso 1 1 calc R . . C30 C 1.6463(2) -0.24035(7) 0.54606(8) 0.0442(4) Uani 1 1 d . . . H30 H 1.6453 -0.2098 0.5780 0.053 Uiso 1 1 calc R . . C1A C 1.14807(16) 0.03734(6) 0.23436(6) 0.0300(3) Uani 1 1 d . . . C4A C 1.13281(17) -0.00302(7) 0.28519(6) 0.0319(3) Uani 1 1 d . . . C5A C 1.05150(17) -0.05937(7) 0.26034(6) 0.0323(3) Uani 1 1 d . . . C8A C 1.01894(16) -0.05360(7) 0.19427(6) 0.0309(3) Uani 1 1 d . . . C23A C 1.51353(16) -0.18184(6) 0.38344(7) 0.0326(3) Uani 1 1 d . . . C26A C 1.55072(17) -0.24331(6) 0.37358(7) 0.0339(3) Uani 1 1 d . . . C27A C 1.60506(17) -0.27123(6) 0.43572(7) 0.0352(3) Uani 1 1 d . . . C30A C 1.60319(17) -0.22633(6) 0.48292(7) 0.0337(3) Uani 1 1 d . . . O1G O 0.75719(16) 0.09151(6) 0.24402(5) 0.0535(3) Uani 1 1 d . . . C1G C 0.72189(19) 0.06806(8) 0.29370(7) 0.0404(4) Uani 1 1 d . . . C2G C 0.6594(2) 0.00422(8) 0.29628(9) 0.0525(4) Uani 1 1 d . . . H2GA H 0.5356 0.0042 0.3015 0.079 Uiso 1 1 calc R . . H2GB H 0.7202 -0.0168 0.3325 0.079 Uiso 1 1 calc R . . H2GC H 0.6812 -0.0168 0.2566 0.079 Uiso 1 1 calc R . . C3G C 0.7404(2) 0.10235(8) 0.35527(8) 0.0498(4) Uani 1 1 d . . . H3GA H 0.8335 0.0834 0.3832 0.060 Uiso 1 1 calc R . . H3GB H 0.6324 0.0980 0.3766 0.060 Uiso 1 1 calc R . . C4G C 0.7792(4) 0.16880(11) 0.34918(11) 0.0905(8) Uani 1 1 d . . . H4GA H 0.8883 0.1738 0.3296 0.136 Uiso 1 1 calc R . . H4GB H 0.7882 0.1876 0.3916 0.136 Uiso 1 1 calc R . . H4GC H 0.6866 0.1884 0.3224 0.136 Uiso 1 1 calc R . . O11G O 1.14973(15) -0.23212(5) 0.44837(8) 0.0664(4) Uani 1 1 d . . . C11G C 1.14749(19) -0.28684(7) 0.45823(9) 0.0459(4) Uani 1 1 d . . . C12G C 1.2001(3) -0.31292(10) 0.52210(9) 0.0690(6) Uani 1 1 d . . . H2G1 H 1.2904 -0.3434 0.5180 0.103 Uiso 1 1 calc R . . H2G2 H 1.1006 -0.3322 0.5395 0.103 Uiso 1 1 calc R . . H2G3 H 1.2441 -0.2804 0.5508 0.103 Uiso 1 1 calc R . . C13G C 1.0920(2) -0.32998(8) 0.40630(8) 0.0494(4) Uani 1 1 d . . . H3G1 H 1.0028 -0.3572 0.4216 0.059 Uiso 1 1 calc R . . H3G2 H 1.1915 -0.3556 0.3972 0.059 Uiso 1 1 calc R . . C14G C 1.0211(3) -0.30042(10) 0.34483(9) 0.0640(5) Uani 1 1 d . . . H4G1 H 0.9212 -0.2754 0.3530 0.096 Uiso 1 1 calc R . . H4G2 H 0.9864 -0.3320 0.3135 0.096 Uiso 1 1 calc R . . H4G3 H 1.1099 -0.2747 0.3282 0.096 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 0.0441(8) 0.0383(8) 0.0300(7) -0.0009(6) 0.0074(6) 0.0035(7) C2 0.0527(9) 0.0444(9) 0.0394(8) -0.0108(7) 0.0044(7) 0.0005(7) C3 0.0523(9) 0.0624(11) 0.0259(7) -0.0098(7) 0.0032(6) 0.0041(8) C4 0.0428(8) 0.0566(10) 0.0230(7) 0.0021(6) 0.0058(6) 0.0063(7) C5 0.0450(9) 0.0495(10) 0.0373(8) 0.0174(7) 0.0061(6) 0.0038(7) C6 0.0536(10) 0.0440(10) 0.0631(11) 0.0186(8) 0.0048(8) -0.0056(8) C7 0.0583(10) 0.0407(10) 0.0582(11) 0.0050(8) -0.0030(8) -0.0072(8) C8 0.0458(9) 0.0409(9) 0.0368(8) 0.0010(7) -0.0014(6) 0.0003(7) O9 0.0333(5) 0.0453(6) 0.0253(5) 0.0048(4) 0.0065(4) 0.0135(4) C9 0.0288(7) 0.0340(7) 0.0230(6) 0.0023(5) 0.0042(5) 0.0075(5) C10 0.0301(7) 0.0292(7) 0.0219(6) -0.0003(5) 0.0034(5) 0.0024(5) C11 0.0442(9) 0.1145(17) 0.0208(7) 0.0111(8) 0.0055(6) 0.0329(10) C12 0.0345(8) 0.1240(18) 0.0255(8) 0.0065(9) 0.0038(6) 0.0333(10) C13 0.0284(6) 0.0278(7) 0.0225(6) -0.0027(5) 0.0030(5) -0.0001(5) C14 0.0313(7) 0.0445(8) 0.0218(6) 0.0072(6) 0.0028(5) 0.0039(6) C15 0.0264(7) 0.0436(8) 0.0274(7) 0.0052(6) 0.0025(5) 0.0044(6) C16 0.0292(6) 0.0241(7) 0.0225(6) -0.0027(5) 0.0068(5) -0.0020(5) C17 0.0315(7) 0.0211(6) 0.0289(7) 0.0004(5) 0.0031(5) 0.0005(5) C18 0.0273(6) 0.0255(7) 0.0336(7) -0.0017(5) 0.0017(5) 0.0002(5) C19 0.0300(7) 0.0240(7) 0.0292(7) -0.0054(5) 0.0062(5) -0.0023(5) C20 0.0330(7) 0.0222(7) 0.0537(9) -0.0101(6) 0.0092(6) 0.0012(6) C21 0.0257(6) 0.0264(7) 0.0506(9) -0.0082(6) 0.0069(6) 0.0010(5) O22 0.0310(5) 0.0275(5) 0.0653(7) -0.0137(5) 0.0176(5) -0.0044(4) C22 0.0281(7) 0.0243(7) 0.0430(8) -0.0073(6) 0.0088(6) -0.0006(5) C23 0.0359(8) 0.0347(8) 0.0526(9) -0.0060(7) -0.0020(6) 0.0014(6) C24 0.0460(9) 0.0548(11) 0.0488(9) -0.0034(8) -0.0065(7) 0.0022(8) C25 0.0460(9) 0.0608(12) 0.0470(10) -0.0199(8) -0.0025(7) -0.0001(8) C26 0.0379(8) 0.0397(9) 0.0574(10) -0.0212(8) 0.0037(7) 0.0006(7) C27 0.0457(9) 0.0262(8) 0.0673(11) -0.0076(7) 0.0090(8) 0.0012(7) C28 0.0549(10) 0.0284(8) 0.0786(13) 0.0088(8) 0.0076(9) 0.0018(7) C29 0.0579(10) 0.0422(10) 0.0573(10) 0.0107(8) 0.0036(8) -0.0049(8) C30 0.0514(9) 0.0345(9) 0.0475(9) -0.0027(7) 0.0085(7) -0.0068(7) C1A 0.0293(7) 0.0381(8) 0.0234(6) 0.0001(6) 0.0069(5) 0.0075(6) C4A 0.0298(7) 0.0432(8) 0.0236(6) 0.0037(6) 0.0069(5) 0.0079(6) C5A 0.0290(7) 0.0392(8) 0.0293(7) 0.0054(6) 0.0065(5) 0.0069(6) C8A 0.0280(7) 0.0363(8) 0.0289(7) 0.0041(6) 0.0055(5) 0.0062(6) C23A 0.0237(6) 0.0275(7) 0.0467(8) -0.0087(6) 0.0032(6) -0.0029(5) C26A 0.0256(7) 0.0285(7) 0.0481(8) -0.0112(6) 0.0049(6) -0.0024(5) C27A 0.0284(7) 0.0254(7) 0.0526(9) -0.0079(6) 0.0082(6) -0.0033(5) C30A 0.0301(7) 0.0247(7) 0.0472(8) -0.0042(6) 0.0086(6) -0.0049(5) O1G 0.0646(7) 0.0604(8) 0.0379(6) 0.0081(5) 0.0199(5) 0.0204(6) C1G 0.0363(8) 0.0496(9) 0.0366(8) 0.0048(7) 0.0108(6) 0.0128(7) C2G 0.0494(10) 0.0547(11) 0.0545(10) -0.0046(8) 0.0118(8) 0.0057(8) C3G 0.0584(10) 0.0546(11) 0.0379(9) 0.0016(7) 0.0135(7) -0.0006(8) C4G 0.150(2) 0.0573(13) 0.0687(14) -0.0106(11) 0.0374(15) -0.0214(15) O11G 0.0405(6) 0.0302(7) 0.1282(12) -0.0105(7) 0.0058(7) 0.0001(5) C11G 0.0320(8) 0.0362(9) 0.0702(11) -0.0087(8) 0.0081(7) 0.0023(6) C12G 0.0766(14) 0.0741(15) 0.0548(11) -0.0139(10) -0.0035(10) -0.0001(11) C13G 0.0529(10) 0.0376(9) 0.0571(10) -0.0022(8) 0.0008(8) 0.0052(7) C14G 0.0558(11) 0.0722(14) 0.0632(12) 0.0092(10) -0.0006(9) 0.0142(10) _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 C1A 1.372(2) . ? C1 C2 1.396(2) . ? C2 C3 1.388(2) . ? C3 C4 1.379(2) . ? C4 C4A 1.3914(19) . ? C5 C6 1.383(2) . ? C5 C5A 1.390(2) . ? C6 C7 1.386(2) . ? C7 C8 1.387(2) . ? C8 C8A 1.381(2) . ? O9 C9 1.4319(15) . ? C9 C10 1.5285(17) . ? C9 C8A 1.5291(19) . ? C9 C1A 1.5298(18) . ? C10 C11 1.373(2) . ? C10 C15 1.3742(18) . ? C11 C12 1.386(2) . ? C12 C13 1.388(2) . ? C13 C14 1.3754(18) . ? C13 C13 1.497(2) 3_855 ? C14 C15 1.3912(18) . ? C16 C17 1.3942(18) . ? C16 C21 1.3975(18) . ? C16 C16 1.492(2) 3_956 ? C17 C18 1.3868(18) . ? C18 C19 1.3877(18) . ? C19 C20 1.3864(19) . ? C19 C22 1.5271(18) . ? C20 C21 1.3835(19) . ? O22 C22 1.4327(15) . ? C22 C30A 1.522(2) . ? C22 C23A 1.5319(19) . ? C23 C23A 1.377(2) . ? C23 C24 1.387(2) . ? C24 C25 1.384(3) . ? C25 C26 1.383(2) . ? C26 C26A 1.389(2) . ? C27 C28 1.388(3) . ? C27 C27A 1.388(2) . ? C28 C29 1.384(3) . ? C29 C30 1.394(2) . ? C30 C30A 1.379(2) . ? C1A C4A 1.4013(19) . ? C4A C5A 1.469(2) . ? C5A C8A 1.3983(18) . ? C23A C26A 1.4011(19) . ? C26A C27A 1.475(2) . ? C27A C30A 1.4008(19) . ? O1G C1G 1.2160(18) . ? C1G C2G 1.488(2) . ? C1G C3G 1.495(2) . ? C3G C4G 1.499(3) . ? O11G C11G 1.221(2) . ? C11G C13G 1.485(2) . ? C11G C12G 1.488(3) . ? C13G C14G 1.512(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A C1 C2 118.64(14) . . ? C3 C2 C1 120.45(15) . . ? C4 C3 C2 120.99(14) . . ? C3 C4 C4A 118.84(14) . . ? C6 C5 C5A 118.77(14) . . ? C5 C6 C7 120.82(15) . . ? C6 C7 C8 120.60(16) . . ? C8A C8 C7 118.96(14) . . ? O9 C9 C10 106.66(10) . . ? O9 C9 C8A 110.75(11) . . ? C10 C9 C8A 113.29(11) . . ? O9 C9 C1A 111.81(10) . . ? C10 C9 C1A 113.22(11) . . ? C8A C9 C1A 101.20(10) . . ? C11 C10 C15 117.40(12) . . ? C11 C10 C9 121.48(11) . . ? C15 C10 C9 121.13(11) . . ? C10 C11 C12 121.61(14) . . ? C11 C12 C13 121.48(14) . . ? C14 C13 C12 116.36(12) . . ? C14 C13 C13 121.41(14) . 3_855 ? C12 C13 C13 122.23(15) . 3_855 ? C13 C14 C15 122.11(12) . . ? C10 C15 C14 121.02(12) . . ? C17 C16 C21 116.51(12) . . ? C17 C16 C16 121.59(14) . 3_956 ? C21 C16 C16 121.89(14) . 3_956 ? C18 C17 C16 121.61(12) . . ? C17 C18 C19 121.27(12) . . ? C20 C19 C18 117.46(12) . . ? C20 C19 C22 121.75(12) . . ? C18 C19 C22 120.79(11) . . ? C21 C20 C19 121.32(13) . . ? C20 C21 C16 121.68(12) . . ? O22 C22 C30A 112.03(11) . . ? O22 C22 C19 106.44(10) . . ? C30A C22 C19 112.95(11) . . ? O22 C22 C23A 112.03(11) . . ? C30A C22 C23A 101.46(11) . . ? C19 C22 C23A 112.06(11) . . ? C23A C23 C24 118.70(15) . . ? C25 C24 C23 120.68(16) . . ? C26 C25 C24 120.98(15) . . ? C25 C26 C26A 118.69(15) . . ? C28 C27 C27A 118.70(15) . . ? C29 C28 C27 121.04(16) . . ? C28 C29 C30 120.30(17) . . ? C30A C30 C29 119.03(15) . . ? C1 C1A C4A 121.10(13) . . ? C1 C1A C9 128.28(12) . . ? C4A C1A C9 110.53(12) . . ? C4 C4A C1A 119.97(14) . . ? C4 C4A C5A 131.12(13) . . ? C1A C4A C5A 108.85(11) . . ? C5 C5A C8A 120.32(14) . . ? C5 C5A C4A 131.18(13) . . ? C8A C5A C4A 108.43(12) . . ? C8 C8A C5A 120.50(13) . . ? C8 C8A C9 128.41(12) . . ? C5A C8A C9 110.94(12) . . ? C23 C23A C26A 120.89(13) . . ? C23 C23A C22 128.54(13) . . ? C26A C23A C22 110.55(12) . . ? C26 C26A C23A 120.03(14) . . ? C26 C26A C27A 131.37(14) . . ? C23A C26A C27A 108.58(12) . . ? C27 C27A C30A 120.30(15) . . ? C27 C27A C26A 131.25(14) . . ? C30A C27A C26A 108.43(12) . . ? C30 C30A C27A 120.63(14) . . ? C30 C30A C22 128.40(13) . . ? C27A C30A C22 110.96(13) . . ? O1G C1G C2G 121.89(15) . . ? O1G C1G C3G 121.16(16) . . ? C2G C1G C3G 116.95(14) . . ? C1G C3G C4G 115.05(15) . . ? O11G C11G C13G 120.76(17) . . ? O11G C11G C12G 121.76(17) . . ? C13G C11G C12G 117.48(15) . . ? C11G C13G C14G 114.83(16) . . ? 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 C1A C1 C2 C3 0.4(2) . . . . ? C1 C2 C3 C4 0.1(2) . . . . ? C2 C3 C4 C4A -0.6(2) . . . . ? C5A C5 C6 C7 1.5(3) . . . . ? C5 C6 C7 C8 -0.8(3) . . . . ? C6 C7 C8 C8A -0.7(3) . . . . ? O9 C9 C10 C11 168.25(15) . . . . ? C8A C9 C10 C11 -69.65(19) . . . . ? C1A C9 C10 C11 44.9(2) . . . . ? O9 C9 C10 C15 -12.45(18) . . . . ? C8A C9 C10 C15 109.65(15) . . . . ? C1A C9 C10 C15 -135.84(13) . . . . ? C15 C10 C11 C12 0.9(3) . . . . ? C9 C10 C11 C12 -179.75(18) . . . . ? C10 C11 C12 C13 -1.1(3) . . . . ? C11 C12 C13 C14 0.0(3) . . . . ? C11 C12 C13 C13 -179.8(2) . . . 3_855 ? C12 C13 C14 C15 1.3(2) . . . . ? C13 C13 C14 C15 -178.90(15) 3_855 . . . ? C11 C10 C15 C14 0.3(2) . . . . ? C9 C10 C15 C14 -178.99(13) . . . . ? C13 C14 C15 C10 -1.5(2) . . . . ? C21 C16 C17 C18 2.65(18) . . . . ? C16 C16 C17 C18 -177.11(14) 3_956 . . . ? C16 C17 C18 C19 0.6(2) . . . . ? C17 C18 C19 C20 -3.38(19) . . . . ? C17 C18 C19 C22 176.54(12) . . . . ? C18 C19 C20 C21 3.0(2) . . . . ? C22 C19 C20 C21 -176.93(13) . . . . ? C19 C20 C21 C16 0.3(2) . . . . ? C17 C16 C21 C20 -3.1(2) . . . . ? C16 C16 C21 C20 176.71(15) 3_956 . . . ? C20 C19 C22 O22 150.89(13) . . . . ? C18 C19 C22 O22 -29.03(17) . . . . ? C20 C19 C22 C30A 27.54(18) . . . . ? C18 C19 C22 C30A -152.38(12) . . . . ? C20 C19 C22 C23A -86.32(16) . . . . ? C18 C19 C22 C23A 93.77(14) . . . . ? C23A C23 C24 C25 -0.7(2) . . . . ? C23 C24 C25 C26 0.6(3) . . . . ? C24 C25 C26 C26A 0.8(2) . . . . ? C27A C27 C28 C29 0.1(2) . . . . ? C27 C28 C29 C30 0.3(3) . . . . ? C28 C29 C30 C30A -0.3(2) . . . . ? C2 C1 C1A C4A -0.5(2) . . . . ? C2 C1 C1A C9 175.72(13) . . . . ? O9 C9 C1A C1 -60.52(17) . . . . ? C10 C9 C1A C1 59.99(18) . . . . ? C8A C9 C1A C1 -178.44(13) . . . . ? O9 C9 C1A C4A 116.02(12) . . . . ? C10 C9 C1A C4A -123.47(12) . . . . ? C8A C9 C1A C4A -1.90(13) . . . . ? C3 C4 C4A C1A 0.5(2) . . . . ? C3 C4 C4A C5A -176.58(14) . . . . ? C1 C1A C4A C4 0.0(2) . . . . ? C9 C1A C4A C4 -176.80(12) . . . . ? C1 C1A C4A C5A 177.72(12) . . . . ? C9 C1A C4A C5A 0.89(14) . . . . ? C6 C5 C5A C8A -0.8(2) . . . . ? C6 C5 C5A C4A 175.65(15) . . . . ? C4 C4A C5A C5 1.2(3) . . . . ? C1A C4A C5A C5 -176.10(14) . . . . ? C4 C4A C5A C8A 177.99(14) . . . . ? C1A C4A C5A C8A 0.64(15) . . . . ? C7 C8 C8A C5A 1.4(2) . . . . ? C7 C8 C8A C9 -173.73(14) . . . . ? C5 C5A C8A C8 -0.7(2) . . . . ? C4A C5A C8A C8 -177.86(12) . . . . ? C5 C5A C8A C9 175.23(12) . . . . ? C4A C5A C8A C9 -1.93(14) . . . . ? O9 C9 C8A C8 59.15(17) . . . . ? C10 C9 C8A C8 -60.64(18) . . . . ? C1A C9 C8A C8 177.84(14) . . . . ? O9 C9 C8A C5A -116.37(12) . . . . ? C10 C9 C8A C5A 123.84(12) . . . . ? C1A C9 C8A C5A 2.32(13) . . . . ? C24 C23 C23A C26A -0.4(2) . . . . ? C24 C23 C23A C22 -178.27(14) . . . . ? O22 C22 C23A C23 56.94(18) . . . . ? C30A C22 C23A C23 176.60(14) . . . . ? C19 C22 C23A C23 -62.63(18) . . . . ? O22 C22 C23A C26A -121.08(12) . . . . ? C30A C22 C23A C26A -1.41(13) . . . . ? C19 C22 C23A C26A 119.35(12) . . . . ? C25 C26 C26A C23A -1.9(2) . . . . ? C25 C26 C26A C27A 176.18(15) . . . . ? C23 C23A C26A C26 1.8(2) . . . . ? C22 C23A C26A C26 179.99(12) . . . . ? C23 C23A C26A C27A -176.71(12) . . . . ? C22 C23A C26A C27A 1.48(15) . . . . ? C28 C27 C27A C30A -0.6(2) . . . . ? C28 C27 C27A C26A -178.56(15) . . . . ? C26 C26A C27A C27 -1.0(3) . . . . ? C23A C26A C27A C27 177.25(15) . . . . ? C26 C26A C27A C30A -179.19(14) . . . . ? C23A C26A C27A C30A -0.91(15) . . . . ? C29 C30 C30A C27A -0.2(2) . . . . ? C29 C30 C30A C22 178.66(14) . . . . ? C27 C27A C30A C30 0.6(2) . . . . ? C26A C27A C30A C30 179.02(13) . . . . ? C27 C27A C30A C22 -178.42(12) . . . . ? C26A C27A C30A C22 -0.02(15) . . . . ? O22 C22 C30A C30 -58.44(18) . . . . ? C19 C22 C30A C30 61.76(18) . . . . ? C23A C22 C30A C30 -178.10(14) . . . . ? O22 C22 C30A C27A 120.50(12) . . . . ? C19 C22 C30A C27A -119.30(12) . . . . ? C23A C22 C30A C27A 0.84(14) . . . . ? O1G C1G C3G C4G 8.6(3) . . . . ? C2G C1G C3G C4G -171.68(19) . . . . ? O11G C11G C13G C14G -6.8(2) . . . . ? C12G C11G C13G C14G 173.36(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9 O1G 0.84 1.95 2.7746(14) 168.7 . O22 H22 O11G 0.84 1.96 2.7902(15) 171.2 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.218 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.033 #========================================================END