# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jerry Atwood' _publ_contact_author_address ; Department of Chemistry University of Missouri-Columbia 601 South College Avenue Columbia Missouri MO 65211 UNITED STATES OF AMERICA ; _publ_contact_author_email ATWOODJ@MISSOURI.EDU _publ_section_title ; Calix[5]arene: A versatile sublimate that displays gas sorption properties ; loop_ _publ_author_name 'J. L. Atwood' 'Thomas E. Clark' 'Scott Dalgarno' 'Mohamed Makha' 'Colin Raston' 'Jian Tian.' ; J.E.Warren ; data_Alpha _database_code_depnum_ccdc_archive 'CCDC 637165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H30 O5' _chemical_formula_weight 530.59 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.7324(14) _cell_length_b 11.924(4) _cell_length_c 22.876(7) _cell_angle_alpha 90.517(4) _cell_angle_beta 92.792(4) _cell_angle_gamma 94.965(4) _cell_volume 1284.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69070 _diffrn_radiation_type Synchrotron _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Bruker APEX II diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13714 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 30.72 _reflns_number_total 7670 _reflns_number_gt 6198 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.0746P)^2^+7.8179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7670 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.1257 _refine_ls_wR_factor_ref 0.3297 _refine_ls_wR_factor_gt 0.3232 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 O1 O 0.8511(7) 0.3971(3) 0.26174(14) 0.0247(6) Uani 1 1 d . . . H1 H 0.8992 0.3836 0.2286 0.030 Uiso 1 1 calc R . . O2 O 0.7569(7) 0.2390(3) 0.34560(14) 0.0239(6) Uani 1 1 d . . . H2 H 0.8184 0.2955 0.3285 0.029 Uiso 1 1 calc R . . O3 O 0.3122(7) 0.1043(3) 0.29520(13) 0.0231(6) Uani 1 1 d . . . H3 H 0.4426 0.1362 0.3156 0.028 Uiso 1 1 calc R . . O4 O 0.2561(7) 0.1378(2) 0.18253(13) 0.0224(6) Uani 1 1 d . . . H4 H 0.3220 0.1356 0.2163 0.027 Uiso 1 1 calc R . . O5 O 0.8411(7) 0.2845(3) 0.15946(14) 0.0268(7) Uani 1 1 d . . . H5 H 0.9246 0.2294 0.1513 0.032 Uiso 1 1 calc R . . C6 C 0.5376(9) 0.0597(3) 0.41201(18) 0.0200(7) Uani 1 1 d . . . H6A H 0.7049 0.0609 0.3891 0.024 Uiso 1 1 calc R . . H6B H 0.5833 0.0261 0.4494 0.024 Uiso 1 1 calc R . . C7 C 0.6372(8) 0.3007(4) 0.11580(18) 0.0207(7) Uani 1 1 d . . . C8 C -0.1522(9) -0.0203(4) 0.23567(18) 0.0220(8) Uani 1 1 d . . . H8A H -0.3413 -0.0583 0.2298 0.026 Uiso 1 1 calc R . . H8B H -0.1712 0.0600 0.2359 0.026 Uiso 1 1 calc R . . C9 C -0.0303(8) -0.0521(3) 0.29548(18) 0.0198(7) Uani 1 1 d . . . C10 C 0.1965(8) 0.0119(3) 0.32413(18) 0.0189(7) Uani 1 1 d . . . C11 C 0.6670(8) 0.4799(3) 0.25946(19) 0.0212(8) Uani 1 1 d . . . C12 C 0.3592(8) 0.0076(3) 0.10982(17) 0.0201(7) Uani 1 1 d . . . C13 C 0.5433(9) 0.3822(3) 0.40125(18) 0.0227(8) Uani 1 1 d . . . C14 C 0.2992(8) -0.0133(3) 0.38065(18) 0.0193(7) Uani 1 1 d . . . C15 C 0.2920(9) 0.2374(4) 0.03989(18) 0.0225(8) Uani 1 1 d . . . H15 H 0.2014 0.1803 0.0160 0.027 Uiso 1 1 calc R . . C16 C 0.4689(8) 0.1807(3) 0.42272(17) 0.0186(7) Uani 1 1 d . . . C17 C 0.5843(9) 0.5295(3) 0.20631(19) 0.0225(8) Uani 1 1 d . . . C18 C 0.2149(9) 0.0304(3) 0.15952(17) 0.0193(7) Uani 1 1 d . . . C19 C 0.5767(9) 0.5175(3) 0.31346(19) 0.0224(8) Uani 1 1 d . . . C20 C 0.5027(8) 0.2118(3) 0.08097(17) 0.0188(7) Uani 1 1 d . . . C21 C 0.1730(9) -0.1093(3) 0.40696(19) 0.0227(8) Uani 1 1 d . . . H21 H 0.2397 -0.1293 0.4440 0.027 Uiso 1 1 calc R . . C22 C 0.7141(10) 0.5043(4) 0.1484(2) 0.0251(8) Uani 1 1 d . . . H22A H 0.7249 0.5727 0.1257 0.030 Uiso 1 1 calc R . . H22B H 0.9071 0.4855 0.1568 0.030 Uiso 1 1 calc R . . C23 C 0.3548(10) 0.4028(4) 0.44394(19) 0.0249(8) Uani 1 1 d . . . H23 H 0.3177 0.4766 0.4518 0.030 Uiso 1 1 calc R . . C24 C 0.5616(9) 0.4112(3) 0.11085(18) 0.0213(7) Uani 1 1 d . . . C25 C 0.3501(10) 0.4323(4) 0.0688(2) 0.0261(9) Uani 1 1 d . . . H25 H 0.2990 0.5054 0.0641 0.031 Uiso 1 1 calc R . . C26 C 0.5899(8) 0.2694(3) 0.38961(18) 0.0195(7) Uani 1 1 d . . . C27 C 0.3827(9) 0.5993(3) 0.3128(2) 0.0237(8) Uani 1 1 d . . . H27 H 0.3175 0.6234 0.3480 0.028 Uiso 1 1 calc R . . C28 C 0.5836(9) 0.0917(4) 0.08704(18) 0.0220(8) Uani 1 1 d . . . H28A H 0.6341 0.0654 0.0490 0.026 Uiso 1 1 calc R . . H28B H 0.7519 0.0925 0.1131 0.026 Uiso 1 1 calc R . . C29 C -0.0486(10) -0.1751(4) 0.3790(2) 0.0253(8) Uani 1 1 d . . . H29 H -0.1288 -0.2389 0.3971 0.030 Uiso 1 1 calc R . . C30 C 0.2851(10) 0.6452(4) 0.2616(2) 0.0279(9) Uani 1 1 d . . . H30 H 0.1513 0.6979 0.2621 0.034 Uiso 1 1 calc R . . C31 C 0.3056(10) -0.1002(4) 0.08392(18) 0.0254(8) Uani 1 1 d . . . H31 H 0.4000 -0.1181 0.0508 0.030 Uiso 1 1 calc R . . C32 C -0.0282(10) -0.1560(3) 0.15698(19) 0.0240(8) Uani 1 1 d . . . H32 H -0.1548 -0.2106 0.1725 0.029 Uiso 1 1 calc R . . C33 C -0.1520(9) -0.1462(3) 0.32374(19) 0.0226(8) Uani 1 1 d . . . H33 H -0.3036 -0.1900 0.3054 0.027 Uiso 1 1 calc R . . C34 C 0.0205(8) -0.0485(3) 0.18391(17) 0.0187(7) Uani 1 1 d . . . C35 C 0.2809(9) 0.2060(4) 0.46479(18) 0.0223(8) Uani 1 1 d . . . H35 H 0.1944 0.1481 0.4863 0.027 Uiso 1 1 calc R . . C36 C 0.7075(10) 0.4787(3) 0.37090(19) 0.0245(8) Uani 1 1 d . . . H36A H 0.7325 0.5427 0.3977 0.029 Uiso 1 1 calc R . . H36B H 0.8950 0.4561 0.3637 0.029 Uiso 1 1 calc R . . C37 C 0.2200(10) 0.3158(4) 0.47525(19) 0.0269(9) Uani 1 1 d . . . H37 H 0.0904 0.3312 0.5029 0.032 Uiso 1 1 calc R . . C38 C 0.3901(9) 0.6114(4) 0.2086(2) 0.0258(9) Uani 1 1 d . . . H38 H 0.3293 0.6443 0.1740 0.031 Uiso 1 1 calc R . . C39 C 0.2147(10) 0.3460(4) 0.0339(2) 0.0268(9) Uani 1 1 d . . . H39 H 0.0720 0.3613 0.0065 0.032 Uiso 1 1 calc R . . C40 C 0.1141(11) -0.1798(4) 0.1072(2) 0.0282(9) Uani 1 1 d . . . H40 H 0.0800 -0.2503 0.0893 0.034 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 O1 0.0258(15) 0.0204(14) 0.0285(15) 0.0014(11) 0.0007(12) 0.0064(11) O2 0.0232(14) 0.0207(14) 0.0285(15) -0.0004(11) 0.0072(12) 0.0020(11) O3 0.0250(15) 0.0199(14) 0.0230(14) 0.0032(11) -0.0001(11) -0.0051(11) O4 0.0270(15) 0.0162(13) 0.0241(14) -0.0015(10) 0.0018(11) 0.0024(11) O5 0.0258(15) 0.0262(15) 0.0294(15) -0.0035(12) -0.0053(12) 0.0115(12) C6 0.0189(17) 0.0180(17) 0.0231(18) 0.0021(14) -0.0007(14) 0.0030(13) C7 0.0170(17) 0.0250(19) 0.0209(17) 0.0018(14) 0.0017(13) 0.0050(14) C8 0.0190(18) 0.0238(19) 0.0236(18) -0.0003(15) 0.0006(14) 0.0044(14) C9 0.0184(17) 0.0187(17) 0.0229(17) -0.0001(14) 0.0027(14) 0.0033(14) C10 0.0197(17) 0.0131(16) 0.0244(18) -0.0004(13) 0.0039(14) 0.0023(13) C11 0.0160(17) 0.0166(17) 0.031(2) -0.0020(14) -0.0003(14) 0.0016(13) C12 0.0191(17) 0.0205(18) 0.0212(17) 0.0003(14) -0.0031(14) 0.0073(14) C13 0.0251(19) 0.0182(18) 0.0241(18) -0.0024(14) -0.0046(15) 0.0016(14) C14 0.0164(16) 0.0181(17) 0.0237(18) -0.0015(14) 0.0032(13) 0.0019(13) C15 0.0206(18) 0.0239(19) 0.0233(18) -0.0004(15) -0.0001(14) 0.0050(15) C16 0.0164(16) 0.0188(17) 0.0205(17) -0.0027(13) -0.0017(13) 0.0019(13) C17 0.0222(18) 0.0149(16) 0.030(2) 0.0009(14) -0.0008(15) -0.0015(14) C18 0.0209(18) 0.0159(16) 0.0212(17) -0.0004(13) -0.0030(14) 0.0046(13) C19 0.0224(19) 0.0124(16) 0.032(2) 0.0007(14) -0.0007(15) -0.0016(13) C20 0.0196(17) 0.0186(17) 0.0191(16) 0.0030(13) 0.0031(13) 0.0048(13) C21 0.028(2) 0.0165(17) 0.0242(18) 0.0019(14) 0.0022(15) 0.0038(15) C22 0.024(2) 0.0197(18) 0.032(2) 0.0043(16) 0.0020(16) -0.0001(15) C23 0.031(2) 0.0186(18) 0.0250(19) -0.0050(15) -0.0022(16) 0.0057(16) C24 0.0211(18) 0.0198(18) 0.0232(18) 0.0035(14) 0.0031(14) 0.0022(14) C25 0.025(2) 0.023(2) 0.031(2) 0.0069(16) 0.0005(16) 0.0052(16) C26 0.0159(16) 0.0186(17) 0.0238(18) -0.0039(14) -0.0015(13) 0.0023(13) C27 0.0216(18) 0.0137(16) 0.035(2) -0.0026(15) 0.0023(16) -0.0012(14) C28 0.0204(18) 0.0226(19) 0.0240(18) 0.0015(14) 0.0017(14) 0.0077(14) C29 0.028(2) 0.0156(17) 0.031(2) 0.0024(15) 0.0042(17) -0.0039(15) C30 0.024(2) 0.0203(19) 0.039(2) -0.0011(17) -0.0047(18) 0.0055(16) C31 0.034(2) 0.0228(19) 0.0205(18) -0.0023(15) 0.0003(16) 0.0094(17) C32 0.027(2) 0.0154(17) 0.029(2) 0.0010(15) -0.0031(16) -0.0002(15) C33 0.0213(18) 0.0146(17) 0.031(2) -0.0010(14) 0.0043(15) -0.0038(14) C34 0.0171(16) 0.0172(17) 0.0220(17) 0.0004(13) -0.0018(13) 0.0033(13) C35 0.0222(19) 0.0221(19) 0.0224(18) -0.0014(14) 0.0024(14) 0.0017(15) C36 0.027(2) 0.0158(17) 0.029(2) -0.0022(15) -0.0033(16) -0.0033(15) C37 0.029(2) 0.029(2) 0.0244(19) -0.0047(16) 0.0038(16) 0.0070(17) C38 0.0225(19) 0.0167(18) 0.038(2) 0.0019(16) -0.0055(17) 0.0020(14) C39 0.027(2) 0.026(2) 0.027(2) 0.0039(16) -0.0039(16) 0.0079(16) C40 0.041(3) 0.0179(18) 0.025(2) -0.0051(15) -0.0054(18) 0.0030(17) _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 O1 C11 1.372(5) . ? O2 C26 1.375(5) . ? O3 C10 1.377(5) . ? O4 C18 1.374(5) . ? O5 C7 1.381(5) . ? C6 C14 1.512(6) . ? C6 C16 1.526(5) . ? C7 C24 1.399(6) . ? C7 C20 1.407(6) . ? C8 C34 1.522(6) . ? C8 C9 1.523(6) . ? C9 C10 1.395(6) . ? C9 C33 1.395(6) . ? C10 C14 1.403(6) . ? C11 C19 1.408(6) . ? C11 C17 1.410(6) . ? C12 C18 1.391(6) . ? C12 C31 1.408(6) . ? C12 C28 1.511(6) . ? C13 C23 1.388(6) . ? C13 C26 1.406(5) . ? C13 C36 1.524(6) . ? C14 C21 1.400(6) . ? C15 C39 1.383(6) . ? C15 C20 1.392(6) . ? C16 C35 1.390(6) . ? C16 C26 1.405(6) . ? C17 C38 1.401(6) . ? C17 C22 1.525(6) . ? C18 C34 1.398(6) . ? C19 C27 1.396(6) . ? C19 C36 1.518(6) . ? C20 C28 1.521(6) . ? C21 C29 1.381(6) . ? C22 C24 1.509(6) . ? C23 C37 1.392(7) . ? C24 C25 1.395(6) . ? C25 C39 1.388(7) . ? C27 C30 1.373(6) . ? C29 C33 1.390(6) . ? C30 C38 1.401(7) . ? C31 C40 1.383(7) . ? C32 C40 1.390(6) . ? C32 C34 1.413(6) . ? C35 C37 1.386(6) . ? 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 C14 C6 C16 113.9(3) . . ? O5 C7 C24 115.0(4) . . ? O5 C7 C20 122.7(4) . . ? C24 C7 C20 122.1(4) . . ? C34 C8 C9 115.5(3) . . ? C10 C9 C33 118.3(4) . . ? C10 C9 C8 122.0(4) . . ? C33 C9 C8 119.7(4) . . ? O3 C10 C9 117.0(4) . . ? O3 C10 C14 120.7(4) . . ? C9 C10 C14 122.3(4) . . ? O1 C11 C19 116.4(4) . . ? O1 C11 C17 122.0(4) . . ? C19 C11 C17 121.5(4) . . ? C18 C12 C31 117.7(4) . . ? C18 C12 C28 121.4(4) . . ? C31 C12 C28 120.7(4) . . ? C23 C13 C26 117.6(4) . . ? C23 C13 C36 121.1(4) . . ? C26 C13 C36 121.2(4) . . ? C21 C14 C10 117.4(4) . . ? C21 C14 C6 121.1(4) . . ? C10 C14 C6 121.6(3) . . ? C39 C15 C20 121.2(4) . . ? C35 C16 C26 118.1(4) . . ? C35 C16 C6 121.0(4) . . ? C26 C16 C6 120.9(3) . . ? C38 C17 C11 117.5(4) . . ? C38 C17 C22 119.5(4) . . ? C11 C17 C22 122.9(4) . . ? O4 C18 C12 117.3(4) . . ? O4 C18 C34 119.9(4) . . ? C12 C18 C34 122.7(4) . . ? C27 C19 C11 118.1(4) . . ? C27 C19 C36 120.7(4) . . ? C11 C19 C36 121.0(4) . . ? C15 C20 C7 117.7(4) . . ? C15 C20 C28 120.4(4) . . ? C7 C20 C28 121.9(4) . . ? C29 C21 C14 121.3(4) . . ? C24 C22 C17 116.6(4) . . ? C13 C23 C37 121.7(4) . . ? C25 C24 C7 117.8(4) . . ? C25 C24 C22 121.7(4) . . ? C7 C24 C22 120.5(4) . . ? C39 C25 C24 121.0(4) . . ? O2 C26 C16 115.8(3) . . ? O2 C26 C13 122.4(4) . . ? C16 C26 C13 121.7(4) . . ? C30 C27 C19 122.0(4) . . ? C12 C28 C20 116.0(3) . . ? C21 C29 C33 120.1(4) . . ? C27 C30 C38 119.0(4) . . ? C40 C31 C12 120.7(4) . . ? C40 C32 C34 119.6(4) . . ? C29 C33 C9 120.6(4) . . ? C18 C34 C32 118.2(4) . . ? C18 C34 C8 122.4(4) . . ? C32 C34 C8 119.3(4) . . ? C37 C35 C16 121.4(4) . . ? C19 C36 C13 116.7(4) . . ? C35 C37 C23 119.3(4) . . ? C17 C38 C30 121.7(4) . . ? C15 C39 C25 120.0(4) . . ? C31 C40 C32 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 30.72 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 0.674 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.112 # Attachment 'Beta.cif' data_Beta _database_code_depnum_ccdc_archive 'CCDC 637166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C105 H90 O15' _chemical_formula_weight 1591.77 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 Rhombohedral _symmetry_space_group_name_H-M P31 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 24.2871(9) _cell_length_b 24.2871(9) _cell_length_c 12.1358(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6199.4(4) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9933 _exptl_absorpt_correction_T_max 0.9966 _exptl_absorpt_process_details ? _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69070 _diffrn_radiation_type Synchrotron _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Bruker APEX II diffractometer' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60966 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.1186 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.41 _reflns_number_total 20352 _reflns_number_gt 16947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.1345P)^2^+24.8727P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.2(15) _refine_ls_number_reflns 20352 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.1225 _refine_ls_wR_factor_ref 0.3309 _refine_ls_wR_factor_gt 0.3215 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 O1 O 0.1008(2) 0.2398(2) -0.1123(4) 0.0302(9) Uani 1 1 d . . . H1 H 0.0904 0.2197 -0.0525 0.036 Uiso 1 1 calc R . . O2 O 0.3148(2) 0.5191(2) 0.1776(4) 0.0361(10) Uani 1 1 d . . . H2 H 0.3385 0.5353 0.1224 0.043 Uiso 1 1 calc R . . O15 O 0.0783(2) 0.1483(2) 0.0471(4) 0.0332(10) Uani 1 1 d . . . H15 H 0.1055 0.1400 0.0729 0.040 Uiso 1 1 calc R . . O3 O 0.5148(2) 0.2502(2) 0.6075(4) 0.0344(10) Uani 1 1 d . . . H3 H 0.5193 0.2844 0.6331 0.041 Uiso 1 1 calc R . . O4 O 0.4123(2) 0.5868(2) 0.0208(4) 0.0381(11) Uani 1 1 d . . . H4 H 0.4460 0.6217 0.0291 0.046 Uiso 1 1 calc R . . O5 O 0.4284(2) 0.1759(2) 0.4464(4) 0.0298(9) Uani 1 1 d . . . H5 H 0.4493 0.1890 0.5052 0.036 Uiso 1 1 calc R . . O6 O 0.3799(2) 0.2487(2) 0.3551(4) 0.0305(9) Uani 1 1 d . . . H6 H 0.3815 0.2158 0.3704 0.037 Uiso 1 1 calc R . . O7 O 0.5132(2) 0.3650(2) 0.6446(4) 0.0338(10) Uani 1 1 d . . . H7 H 0.4867 0.3753 0.6230 0.041 Uiso 1 1 calc R . . O8 O 0.1843(2) 0.1303(2) 0.0746(4) 0.0336(10) Uani 1 1 d . . . H8 H 0.2218 0.1543 0.0531 0.040 Uiso 1 1 calc R . . O9 O 0.3527(2) 0.5768(2) 0.3825(4) 0.0352(10) Uani 1 1 d . . . H9 H 0.3249 0.5598 0.3332 0.042 Uiso 1 1 calc R . . O10 O 0.4801(2) 0.6730(2) 0.3594(4) 0.0334(10) Uani 1 1 d . . . H10 H 0.4430 0.6541 0.3848 0.040 Uiso 1 1 calc R . . O11 O 0.2217(2) 0.2824(2) -0.1985(4) 0.0336(10) Uani 1 1 d . . . H11 H 0.1899 0.2852 -0.1799 0.040 Uiso 1 1 calc R . . O12 O 0.4361(2) 0.3659(2) 0.4661(4) 0.0337(10) Uani 1 1 d . . . H12 H 0.4114 0.3338 0.4286 0.040 Uiso 1 1 calc R . . O13 O 0.5168(2) 0.6834(2) 0.1337(4) 0.0327(9) Uani 1 1 d . . . H13 H 0.5116 0.6918 0.1986 0.039 Uiso 1 1 calc R . . O14 O 0.2641(2) 0.2028(2) -0.0959(4) 0.0360(10) Uani 1 1 d . . . H14 H 0.2642 0.2344 -0.1246 0.043 Uiso 1 1 calc R . . C1 C 0.6121(3) 0.7421(3) 0.3039(5) 0.0327(13) Uani 1 1 d . . . H1A H 0.5840 0.7584 0.2795 0.039 Uiso 1 1 calc R . . H1B H 0.6548 0.7792 0.3167 0.039 Uiso 1 1 calc R . . C3 C 0.1236(3) 0.2878(3) -0.3298(6) 0.0299(12) Uani 1 1 d . . . H3A H 0.1435 0.3156 -0.2651 0.036 Uiso 1 1 calc R . . H3B H 0.1169 0.3133 -0.3863 0.036 Uiso 1 1 calc R . . C4 C 0.5140(3) 0.1379(3) 0.5353(5) 0.0272(11) Uani 1 1 d . . . H4A H 0.5171 0.0992 0.5475 0.033 Uiso 1 1 calc R . . H4B H 0.4754 0.1318 0.5737 0.033 Uiso 1 1 calc R . . C5 C 0.0483(3) 0.2145(3) -0.1835(5) 0.0286(12) Uani 1 1 d . . . C6 C 0.5756(3) 0.4131(3) 0.6138(5) 0.0280(12) Uani 1 1 d . . . C7 C 0.4614(3) 0.1589(3) 0.3724(5) 0.0237(10) Uani 1 1 d . . . C8 C 0.3877(3) 0.3118(3) 0.1976(5) 0.0298(12) Uani 1 1 d . . . C9 C 0.5718(3) 0.1943(3) 0.5867(5) 0.0296(12) Uani 1 1 d . . . C10 C 0.2990(3) 0.1284(3) -0.1296(5) 0.0303(12) Uani 1 1 d . . . C11 C 0.2038(3) 0.0520(3) -0.0092(5) 0.0328(13) Uani 1 1 d . . . C12 C 0.6226(3) 0.2983(3) 0.6742(5) 0.0299(12) Uani 1 1 d . . . C13 C 0.1652(3) 0.0680(3) 0.0456(5) 0.0311(13) Uani 1 1 d . . . C14 C 0.3246(3) 0.2144(3) -0.2590(5) 0.0314(13) Uani 1 1 d . . . C15 C 0.2956(3) 0.1819(3) -0.1645(5) 0.0278(12) Uani 1 1 d . . . C17 C 0.3885(3) 0.2601(3) 0.2431(5) 0.0256(11) Uani 1 1 d . . . C18 C 0.0650(3) 0.0364(3) 0.1614(5) 0.0315(13) Uani 1 1 d . . . H18A H 0.0482 0.0031 0.2190 0.038 Uiso 1 1 calc R . . H18B H 0.0939 0.0774 0.1980 0.038 Uiso 1 1 calc R . . C19 C 0.2147(3) 0.3516(3) 0.2457(5) 0.0345(14) Uani 1 1 d . . . H19 H 0.1911 0.3260 0.3065 0.041 Uiso 1 1 calc R . . C20 C 0.0102(3) 0.0405(3) 0.1119(5) 0.0297(12) Uani 1 1 d . . . C21 C -0.0346(3) 0.0984(3) 0.0211(5) 0.0295(12) Uani 1 1 d . . . C22 C -0.0124(3) 0.1724(3) -0.1474(5) 0.0298(13) Uani 1 1 d . . . C23 C 0.4995(3) 0.6489(3) 0.5410(6) 0.0318(13) Uani 1 1 d . . . C24 C 0.5223(3) 0.6753(3) 0.4396(5) 0.0282(12) Uani 1 1 d . . . C25 C 0.5703(3) 0.2483(3) 0.6231(5) 0.0261(11) Uani 1 1 d . . . C26 C 0.3888(3) 0.1561(3) 0.2202(5) 0.0276(12) Uani 1 1 d . . . H26A H 0.3685 0.1239 0.1613 0.033 Uiso 1 1 calc R . . H26B H 0.3583 0.1428 0.2823 0.033 Uiso 1 1 calc R . . C27 C 0.5063(3) 0.1445(3) 0.4135(5) 0.0246(11) Uani 1 1 d . . . C28 C 0.5436(3) 0.1341(3) 0.3386(6) 0.0326(13) Uani 1 1 d . . . H28 H 0.5756 0.1259 0.3649 0.039 Uiso 1 1 calc R . . C29 C -0.0255(3) 0.1618(3) -0.0243(6) 0.0332(13) Uani 1 1 d . . . H29A H -0.0643 0.1640 -0.0076 0.040 Uiso 1 1 calc R . . H29B H 0.0103 0.1971 0.0157 0.040 Uiso 1 1 calc R . . C30 C 0.4231(3) 0.4153(3) 0.3027(6) 0.0328(13) Uani 1 1 d . . . C31 C 0.3982(3) 0.2181(3) 0.1772(5) 0.0279(12) Uani 1 1 d . . . C32 C 0.6165(3) 0.7029(3) 0.2134(5) 0.0275(12) Uani 1 1 d . . . C33 C -0.0510(3) -0.0124(3) 0.1171(5) 0.0335(13) Uani 1 1 d . . . H33 H -0.0575 -0.0503 0.1516 0.040 Uiso 1 1 calc R . . C34 C 0.2819(3) 0.4534(3) 0.1674(6) 0.0316(13) Uani 1 1 d . . . C35 C 0.0180(3) 0.0954(3) 0.0583(5) 0.0264(11) Uani 1 1 d . . . C36 C 0.4996(3) 0.5238(3) -0.1294(5) 0.0338(13) Uani 1 1 d . . . H36 H 0.5416 0.5372 -0.1539 0.041 Uiso 1 1 calc R . . C37 C 0.0597(3) 0.2343(3) -0.2956(5) 0.0318(13) Uani 1 1 d . . . C38 C 0.4470(3) 0.1541(3) 0.2596(5) 0.0244(11) Uani 1 1 d . . . C39 C 0.5868(3) 0.7069(3) 0.4129(5) 0.0320(13) Uani 1 1 d . . . C40 C 0.3250(3) 0.2749(3) -0.2931(6) 0.0332(13) Uani 1 1 d . . . H40A H 0.3274 0.2991 -0.2259 0.040 Uiso 1 1 calc R . . H40B H 0.3638 0.3014 -0.3370 0.040 Uiso 1 1 calc R . . C41 C 0.3461(3) 0.5313(3) 0.4573(5) 0.0296(12) Uani 1 1 d . . . C42 C 0.2626(3) 0.2474(3) -0.4683(6) 0.0338(13) Uani 1 1 d . . . H42 H 0.2942 0.2402 -0.5002 0.041 Uiso 1 1 calc R . . C43 C 0.6280(3) 0.1926(4) 0.5995(6) 0.0359(14) Uani 1 1 d . . . H43 H 0.6301 0.1564 0.5753 0.043 Uiso 1 1 calc R . . C44 C 0.5720(3) 0.6791(3) 0.1278(5) 0.0283(12) Uani 1 1 d . . . C45 C 0.2679(3) 0.2642(3) -0.3595(5) 0.0294(12) Uani 1 1 d . . . C46 C 0.5305(4) 0.4837(3) 0.5559(6) 0.0367(14) Uani 1 1 d . . . H46A H 0.4960 0.4551 0.6066 0.044 Uiso 1 1 calc R . . H46B H 0.5471 0.5277 0.5826 0.044 Uiso 1 1 calc R . . C47 C 0.6756(3) 0.6615(3) 0.1194(6) 0.0326(13) Uani 1 1 d . . . H47 H 0.7106 0.6543 0.1183 0.039 Uiso 1 1 calc R . . C48 C 0.5020(3) 0.4782(3) 0.4426(5) 0.0319(13) Uani 1 1 d . . . C49 C 0.4251(3) 0.5453(3) -0.0382(5) 0.0322(13) Uani 1 1 d . . . C50 C 0.6856(3) 0.4477(3) 0.6025(5) 0.0318(13) Uani 1 1 d . . . H50 H 0.7205 0.4414 0.6167 0.038 Uiso 1 1 calc R . . C51 C 0.3757(3) 0.4843(3) -0.0616(5) 0.0324(13) Uani 1 1 d . . . C52 C 0.2193(3) 0.2709(3) -0.3092(5) 0.0293(12) Uani 1 1 d . . . C53 C 0.5346(3) 0.1357(3) 0.2258(5) 0.0328(13) Uani 1 1 d . . . H53 H 0.5622 0.1317 0.1751 0.039 Uiso 1 1 calc R . . C54 C 0.1699(3) 0.2691(3) -0.3754(5) 0.0262(11) Uani 1 1 d . . . C55 C 0.6661(3) 0.6902(3) 0.2069(6) 0.0343(13) Uani 1 1 d . . . H55 H 0.6948 0.7023 0.2671 0.041 Uiso 1 1 calc R . . C56 C 0.6185(3) 0.3537(3) 0.7231(5) 0.0282(11) Uani 1 1 d . . . H56A H 0.5770 0.3366 0.7608 0.034 Uiso 1 1 calc R . . H56B H 0.6520 0.3741 0.7799 0.034 Uiso 1 1 calc R . . C57 C 0.5836(3) 0.4681(3) 0.5638(5) 0.0304(13) Uani 1 1 d . . . C58 C 0.4547(3) 0.4208(3) 0.4041(5) 0.0307(12) Uani 1 1 d . . . C59 C 0.3545(3) 0.1895(4) -0.3279(5) 0.0317(13) Uani 1 1 d . . . H59 H 0.3733 0.2106 -0.3952 0.038 Uiso 1 1 calc R . . C60 C 0.6253(3) 0.4039(3) 0.6430(5) 0.0342(13) Uani 1 1 d . . . C61 C 0.3867(3) 0.5512(3) 0.5488(5) 0.0330(13) Uani 1 1 d . . . C62 C 0.2749(3) 0.0978(3) -0.0198(5) 0.0319(13) Uani 1 1 d . . . H62A H 0.2871 0.1319 0.0355 0.038 Uiso 1 1 calc R . . H62B H 0.2972 0.0744 -0.0003 0.038 Uiso 1 1 calc R . . C63 C 0.4877(3) 0.5668(3) -0.0772(5) 0.0315(13) Uani 1 1 d . . . C64 C 0.2455(3) 0.4477(4) 0.3660(5) 0.0363(15) Uani 1 1 d . . . H64A H 0.2412 0.4851 0.3481 0.044 Uiso 1 1 calc R . . H64B H 0.2061 0.4168 0.4047 0.044 Uiso 1 1 calc R . . C65 C 0.4129(3) 0.2345(3) 0.0647(5) 0.0334(13) Uani 1 1 d . . . H65 H 0.4211 0.2080 0.0182 0.040 Uiso 1 1 calc R . . C66 C 0.6452(3) 0.5112(3) 0.5228(5) 0.0338(14) Uani 1 1 d . . . H66 H 0.6521 0.5476 0.4823 0.041 Uiso 1 1 calc R . . C67 C 0.4846(3) 0.1433(3) 0.1882(5) 0.0325(13) Uani 1 1 d . . . H67 H 0.4763 0.1409 0.1113 0.039 Uiso 1 1 calc R . . C68 C 0.2483(3) 0.4178(3) 0.2590(6) 0.0353(14) Uani 1 1 d . . . C69 C 0.5395(3) 0.6357(3) -0.0681(5) 0.0337(13) Uani 1 1 d . . . H69A H 0.5192 0.6624 -0.0688 0.040 Uiso 1 1 calc R . . H69B H 0.5667 0.6468 -0.1345 0.040 Uiso 1 1 calc R . . C70 C 0.1793(3) -0.0105(3) -0.0458(5) 0.0323(13) Uani 1 1 d . . . H70 H 0.2058 -0.0219 -0.0854 0.039 Uiso 1 1 calc R . . C71 C 0.4154(4) 0.2874(4) 0.0222(6) 0.0405(16) Uani 1 1 d . . . H71 H 0.4278 0.2991 -0.0523 0.049 Uiso 1 1 calc R . . C72 C 0.3687(3) 0.3533(3) 0.2661(6) 0.0324(13) Uani 1 1 d . . . H72A H 0.3395 0.3617 0.2216 0.039 Uiso 1 1 calc R . . H72B H 0.3450 0.3289 0.3320 0.039 Uiso 1 1 calc R . . C73 C 0.2788(3) 0.4253(4) 0.0676(6) 0.0360(14) Uani 1 1 d . . . C74 C -0.0941(3) 0.0454(3) 0.0283(6) 0.0323(13) Uani 1 1 d . . . H74 H -0.1297 0.0478 0.0024 0.039 Uiso 1 1 calc R . . C75 C 0.3901(3) 0.4426(3) -0.1147(5) 0.0325(13) Uani 1 1 d . . . H75 H 0.3571 0.4004 -0.1293 0.039 Uiso 1 1 calc R . . C76 C 0.2474(3) 0.3599(3) 0.0596(6) 0.0382(15) Uani 1 1 d . . . H76 H 0.2484 0.3407 -0.0080 0.046 Uiso 1 1 calc R . . C77 C 0.3999(4) 0.3242(3) 0.0874(6) 0.0371(14) Uani 1 1 d . . . H77 H 0.3977 0.3587 0.0554 0.044 Uiso 1 1 calc R . . C78 C -0.1035(3) -0.0098(4) 0.0709(6) 0.0388(15) Uani 1 1 d . . . H78 H -0.1446 -0.0465 0.0701 0.047 Uiso 1 1 calc R . . C79 C 0.5818(3) 0.6532(3) 0.0327(5) 0.0335(13) Uani 1 1 d . . . C80 C 0.5212(4) 0.5322(3) 0.3763(6) 0.0381(15) Uani 1 1 d . . . H80 H 0.5547 0.5725 0.3996 0.046 Uiso 1 1 calc R . . C81 C 0.1038(3) 0.0217(3) 0.0802(5) 0.0291(12) Uani 1 1 d . . . C82 C 0.3299(3) 0.1069(3) -0.1967(6) 0.0324(13) Uani 1 1 d . . . H82 H 0.3336 0.0715 -0.1738 0.039 Uiso 1 1 calc R . . C83 C 0.6778(4) 0.2955(4) 0.6856(6) 0.0423(16) Uani 1 1 d . . . H83 H 0.7140 0.3297 0.7198 0.051 Uiso 1 1 calc R . . C84 C 0.2991(3) 0.4686(3) 0.4446(5) 0.0325(13) Uani 1 1 d . . . C85 C 0.0093(3) 0.2051(3) -0.3683(5) 0.0320(13) Uani 1 1 d . . . H85 H 0.0161 0.2170 -0.4438 0.038 Uiso 1 1 calc R . . C86 C 0.1666(3) 0.2513(3) -0.4833(5) 0.0317(13) Uani 1 1 d . . . H86 H 0.1314 0.2459 -0.5260 0.038 Uiso 1 1 calc R . . C87 C 0.3075(3) 0.4647(3) -0.0388(5) 0.0321(13) Uani 1 1 d . . . H87A H 0.2814 0.4395 -0.1023 0.039 Uiso 1 1 calc R . . H87B H 0.3040 0.5035 -0.0342 0.039 Uiso 1 1 calc R . . C88 C 0.2988(4) 0.4234(3) 0.5201(6) 0.047(2) Uani 1 1 d . . . H88 H 0.2676 0.3797 0.5125 0.056 Uiso 1 1 calc R . . C89 C -0.0515(3) 0.1584(4) -0.3344(6) 0.0384(15) Uani 1 1 d . . . H89 H -0.0847 0.1368 -0.3865 0.046 Uiso 1 1 calc R . . C90 C 0.4526(3) 0.4615(3) -0.1476(6) 0.0354(14) Uani 1 1 d . . . H90 H 0.4623 0.4321 -0.1814 0.042 Uiso 1 1 calc R . . C91 C 0.2142(4) 0.3217(4) 0.1490(6) 0.0398(15) Uani 1 1 d . . . H91 H 0.1921 0.2766 0.1435 0.048 Uiso 1 1 calc R . . C92 C 0.2122(3) 0.2407(3) -0.5341(6) 0.0361(14) Uani 1 1 d . . . H92 H 0.2092 0.2295 -0.6098 0.043 Uiso 1 1 calc R . . C93 C 0.6336(3) 0.6426(3) 0.0309(6) 0.0338(13) Uani 1 1 d . . . H93 H 0.6399 0.6225 -0.0309 0.041 Uiso 1 1 calc R . . C94 C 0.4913(4) 0.5261(4) 0.2778(7) 0.0403(15) Uani 1 1 d . . . H94 H 0.5045 0.5625 0.2326 0.048 Uiso 1 1 calc R . . C95 C 0.6950(3) 0.5004(4) 0.5417(6) 0.0398(16) Uani 1 1 d . . . H95 H 0.7360 0.5290 0.5130 0.048 Uiso 1 1 calc R . . C96 C 0.0802(3) -0.0408(3) 0.0429(6) 0.0330(13) Uani 1 1 d . . . H96 H 0.0389 -0.0730 0.0642 0.040 Uiso 1 1 calc R . . C97 C 0.3568(3) 0.1365(4) -0.3001(6) 0.0383(15) Uani 1 1 d . . . H97 H 0.3757 0.1197 -0.3479 0.046 Uiso 1 1 calc R . . C98 C 0.1169(4) -0.0558(3) -0.0251(6) 0.0359(14) Uani 1 1 d . . . H98 H 0.0992 -0.0969 -0.0569 0.043 Uiso 1 1 calc R . . C99 C 0.4425(4) 0.4684(4) 0.2429(6) 0.0379(15) Uani 1 1 d . . . H99 H 0.4221 0.4659 0.1748 0.046 Uiso 1 1 calc R . . C100 C 0.6292(4) 0.7075(4) 0.4930(6) 0.0412(16) Uani 1 1 d . . . H100 H 0.6734 0.7283 0.4777 0.049 Uiso 1 1 calc R . . C101 C 0.4307(3) 0.6212(3) 0.5746(5) 0.0349(14) Uani 1 1 d . . . H10A H 0.4137 0.6459 0.5378 0.042 Uiso 1 1 calc R . . H10B H 0.4293 0.6272 0.6550 0.042 Uiso 1 1 calc R . . C102 C 0.5436(4) 0.6492(3) 0.6193(6) 0.0385(15) Uani 1 1 d . . . H102 H 0.5290 0.6294 0.6890 0.046 Uiso 1 1 calc R . . C103 C 0.6810(3) 0.2432(4) 0.6474(7) 0.0430(17) Uani 1 1 d . . . H103 H 0.7194 0.2422 0.6541 0.052 Uiso 1 1 calc R . . C104 C -0.0622(3) 0.1442(3) -0.2221(6) 0.0373(14) Uani 1 1 d . . . H104 H -0.1039 0.1151 -0.1968 0.045 Uiso 1 1 calc R . . C105 C 0.3859(4) 0.5046(4) 0.6216(6) 0.0441(17) Uani 1 1 d . . . H105 H 0.4148 0.5172 0.6816 0.053 Uiso 1 1 calc R . . C106 C 0.3432(5) 0.4420(4) 0.6042(8) 0.055(2) Uani 1 1 d . . . H106 H 0.3438 0.4107 0.6503 0.066 Uiso 1 1 calc R . . C107 C 0.6069(4) 0.6781(4) 0.5935(7) 0.0483(18) Uani 1 1 d . . . H107 H 0.6360 0.6779 0.6456 0.058 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 O1 0.033(2) 0.033(2) 0.024(2) -0.0007(17) -0.0018(17) 0.0160(19) O2 0.041(3) 0.035(2) 0.028(2) -0.0033(18) -0.0043(19) 0.016(2) O15 0.023(2) 0.029(2) 0.042(3) 0.0022(18) 0.0056(18) 0.0084(18) O3 0.032(2) 0.037(2) 0.041(3) 0.001(2) 0.0021(19) 0.022(2) O4 0.037(2) 0.042(3) 0.041(3) -0.003(2) 0.001(2) 0.024(2) O5 0.030(2) 0.036(2) 0.026(2) -0.0034(17) -0.0023(16) 0.0191(19) O6 0.033(2) 0.034(2) 0.029(2) 0.0037(17) 0.0026(17) 0.0197(19) O7 0.040(2) 0.031(2) 0.032(2) 0.0026(18) -0.0020(19) 0.019(2) O8 0.035(2) 0.032(2) 0.034(2) -0.0026(18) 0.0031(18) 0.0165(19) O9 0.045(3) 0.029(2) 0.034(2) 0.0011(18) -0.005(2) 0.020(2) O10 0.038(2) 0.038(2) 0.029(2) -0.0027(18) -0.0059(18) 0.023(2) O11 0.034(2) 0.041(2) 0.028(2) -0.0059(18) 0.0037(18) 0.020(2) O12 0.036(2) 0.029(2) 0.035(2) 0.0040(18) 0.0015(19) 0.0161(19) O13 0.028(2) 0.041(2) 0.031(2) -0.0019(19) 0.0023(17) 0.020(2) O14 0.039(2) 0.042(3) 0.032(2) -0.008(2) 0.0060(19) 0.024(2) C1 0.040(3) 0.022(3) 0.032(3) -0.001(2) 0.007(3) 0.013(3) C3 0.030(3) 0.027(3) 0.034(3) -0.001(2) -0.001(2) 0.015(2) C4 0.029(3) 0.024(3) 0.029(3) 0.009(2) 0.006(2) 0.013(2) C5 0.029(3) 0.029(3) 0.029(3) 0.000(2) 0.006(2) 0.016(2) C6 0.032(3) 0.028(3) 0.021(3) -0.005(2) -0.005(2) 0.013(2) C7 0.021(2) 0.026(3) 0.023(3) 0.005(2) 0.002(2) 0.010(2) C8 0.017(2) 0.031(3) 0.038(3) 0.005(2) 0.000(2) 0.009(2) C9 0.028(3) 0.028(3) 0.037(3) 0.000(2) 0.001(2) 0.017(2) C10 0.027(3) 0.032(3) 0.026(3) 0.000(2) -0.003(2) 0.010(2) C11 0.041(3) 0.041(3) 0.023(3) 0.004(2) -0.004(2) 0.025(3) C12 0.034(3) 0.028(3) 0.024(3) -0.004(2) -0.003(2) 0.013(3) C13 0.032(3) 0.027(3) 0.033(3) 0.006(2) -0.003(2) 0.014(2) C14 0.026(3) 0.034(3) 0.030(3) -0.004(2) 0.006(2) 0.012(2) C15 0.026(3) 0.029(3) 0.030(3) -0.004(2) -0.004(2) 0.015(2) C17 0.022(3) 0.026(3) 0.024(3) -0.001(2) -0.002(2) 0.008(2) C18 0.037(3) 0.035(3) 0.023(3) 0.003(2) 0.007(2) 0.019(3) C19 0.033(3) 0.036(3) 0.023(3) 0.005(2) -0.002(2) 0.009(3) C20 0.040(3) 0.029(3) 0.025(3) 0.003(2) 0.003(2) 0.020(3) C21 0.032(3) 0.037(3) 0.028(3) -0.003(2) 0.004(2) 0.024(3) C22 0.036(3) 0.029(3) 0.030(3) 0.006(2) 0.014(2) 0.020(3) C23 0.029(3) 0.026(3) 0.035(3) -0.009(2) -0.005(2) 0.011(2) C24 0.037(3) 0.027(3) 0.028(3) -0.001(2) 0.001(2) 0.021(3) C25 0.021(2) 0.031(3) 0.025(3) 0.005(2) -0.001(2) 0.011(2) C26 0.029(3) 0.024(3) 0.026(3) -0.002(2) -0.008(2) 0.010(2) C27 0.021(2) 0.027(3) 0.022(3) 0.004(2) 0.002(2) 0.010(2) C28 0.030(3) 0.030(3) 0.042(4) 0.003(3) 0.009(3) 0.018(3) C29 0.030(3) 0.040(3) 0.039(3) 0.002(3) 0.007(3) 0.024(3) C30 0.031(3) 0.028(3) 0.042(4) 0.000(3) 0.001(3) 0.017(3) C31 0.026(3) 0.027(3) 0.032(3) 0.005(2) -0.002(2) 0.014(2) C32 0.037(3) 0.022(3) 0.024(3) 0.004(2) 0.002(2) 0.016(2) C33 0.030(3) 0.038(3) 0.030(3) 0.000(3) 0.002(2) 0.015(3) C34 0.023(3) 0.034(3) 0.039(3) 0.002(3) -0.006(2) 0.015(2) C35 0.022(3) 0.024(3) 0.030(3) 0.005(2) 0.007(2) 0.009(2) C36 0.036(3) 0.043(4) 0.028(3) -0.003(3) 0.002(2) 0.024(3) C37 0.042(3) 0.032(3) 0.032(3) 0.005(2) 0.007(3) 0.026(3) C38 0.027(3) 0.017(2) 0.029(3) 0.000(2) 0.000(2) 0.011(2) C39 0.040(3) 0.032(3) 0.029(3) -0.006(2) 0.002(3) 0.021(3) C40 0.021(3) 0.036(3) 0.035(3) 0.004(3) 0.001(2) 0.008(2) C41 0.031(3) 0.035(3) 0.026(3) 0.002(2) 0.006(2) 0.019(3) C42 0.037(3) 0.037(3) 0.031(3) 0.005(3) 0.015(3) 0.022(3) C43 0.037(3) 0.042(4) 0.039(4) 0.001(3) -0.004(3) 0.028(3) C44 0.025(3) 0.024(3) 0.039(3) 0.001(2) -0.007(2) 0.014(2) C45 0.029(3) 0.021(3) 0.033(3) 0.001(2) 0.007(2) 0.008(2) C46 0.051(4) 0.033(3) 0.032(3) -0.006(3) -0.002(3) 0.025(3) C47 0.027(3) 0.037(3) 0.038(3) -0.009(3) -0.004(2) 0.019(3) C48 0.042(3) 0.029(3) 0.031(3) -0.004(2) 0.002(3) 0.023(3) C49 0.036(3) 0.036(3) 0.027(3) 0.006(2) 0.000(2) 0.020(3) C50 0.036(3) 0.038(3) 0.020(3) -0.004(2) -0.001(2) 0.017(3) C51 0.029(3) 0.043(3) 0.020(3) 0.000(2) -0.002(2) 0.014(3) C52 0.038(3) 0.025(3) 0.026(3) -0.003(2) -0.001(2) 0.016(2) C53 0.034(3) 0.036(3) 0.027(3) -0.002(2) 0.010(2) 0.017(3) C54 0.027(3) 0.023(3) 0.026(3) 0.003(2) 0.005(2) 0.011(2) C55 0.035(3) 0.029(3) 0.039(3) 0.003(3) -0.002(3) 0.016(3) C56 0.029(3) 0.027(3) 0.026(3) -0.003(2) -0.004(2) 0.013(2) C57 0.048(4) 0.027(3) 0.018(3) -0.001(2) -0.002(2) 0.021(3) C58 0.039(3) 0.035(3) 0.028(3) 0.005(2) 0.004(2) 0.026(3) C59 0.024(3) 0.052(4) 0.018(3) 0.000(2) 0.003(2) 0.018(3) C60 0.040(3) 0.039(3) 0.021(3) -0.007(2) -0.004(2) 0.018(3) C61 0.031(3) 0.029(3) 0.030(3) -0.001(2) -0.006(2) 0.009(3) C62 0.037(3) 0.038(3) 0.024(3) 0.006(2) 0.006(2) 0.021(3) C63 0.034(3) 0.041(3) 0.020(3) -0.001(2) -0.001(2) 0.019(3) C64 0.024(3) 0.041(4) 0.028(3) -0.002(3) 0.002(2) 0.004(3) C65 0.035(3) 0.042(4) 0.021(3) -0.005(2) -0.001(2) 0.017(3) C66 0.046(4) 0.034(3) 0.017(3) 0.003(2) -0.002(2) 0.016(3) C67 0.046(4) 0.030(3) 0.018(3) 0.006(2) 0.008(2) 0.016(3) C68 0.031(3) 0.036(3) 0.032(3) 0.005(3) -0.012(3) 0.012(3) C69 0.034(3) 0.041(4) 0.023(3) 0.007(2) 0.001(2) 0.017(3) C70 0.047(4) 0.034(3) 0.020(3) 0.002(2) 0.000(2) 0.023(3) C71 0.042(4) 0.050(4) 0.024(3) 0.005(3) -0.004(3) 0.019(3) C72 0.035(3) 0.034(3) 0.032(3) 0.001(2) -0.006(3) 0.021(3) C73 0.027(3) 0.046(4) 0.032(3) 0.003(3) -0.007(2) 0.015(3) C74 0.022(3) 0.033(3) 0.041(3) -0.003(3) 0.005(2) 0.013(2) C75 0.037(3) 0.032(3) 0.029(3) 0.000(2) -0.002(2) 0.017(3) C76 0.029(3) 0.038(3) 0.037(4) -0.010(3) -0.015(3) 0.009(3) C77 0.043(4) 0.036(3) 0.035(3) 0.012(3) -0.002(3) 0.022(3) C78 0.029(3) 0.043(4) 0.043(4) 0.004(3) 0.004(3) 0.017(3) C79 0.024(3) 0.040(3) 0.030(3) 0.004(3) 0.001(2) 0.012(3) C80 0.043(4) 0.029(3) 0.044(4) 0.008(3) 0.005(3) 0.019(3) C81 0.029(3) 0.035(3) 0.027(3) 0.004(2) 0.000(2) 0.018(3) C82 0.022(3) 0.033(3) 0.039(3) 0.002(3) 0.005(2) 0.012(2) C83 0.041(4) 0.054(4) 0.030(3) 0.000(3) -0.010(3) 0.022(3) C84 0.034(3) 0.036(3) 0.027(3) 0.000(2) -0.002(2) 0.017(3) C85 0.041(3) 0.038(3) 0.024(3) 0.007(2) 0.007(2) 0.025(3) C86 0.035(3) 0.027(3) 0.026(3) 0.001(2) 0.004(2) 0.011(3) C87 0.033(3) 0.038(3) 0.026(3) -0.003(2) 0.000(2) 0.018(3) C88 0.047(4) 0.032(3) 0.034(4) 0.007(3) -0.019(3) -0.001(3) C89 0.031(3) 0.043(4) 0.042(4) -0.010(3) -0.010(3) 0.019(3) C90 0.036(3) 0.041(4) 0.031(3) -0.003(3) 0.004(3) 0.021(3) C91 0.042(4) 0.034(3) 0.038(4) -0.003(3) -0.003(3) 0.015(3) C92 0.041(4) 0.037(3) 0.026(3) -0.007(3) 0.006(3) 0.017(3) C93 0.030(3) 0.034(3) 0.038(3) -0.003(3) 0.000(3) 0.017(3) C94 0.047(4) 0.035(3) 0.044(4) 0.007(3) 0.006(3) 0.025(3) C95 0.032(3) 0.041(4) 0.029(3) -0.008(3) 0.004(3) 0.005(3) C96 0.034(3) 0.028(3) 0.038(3) 0.001(3) 0.001(3) 0.016(3) C97 0.034(3) 0.042(4) 0.038(4) -0.010(3) 0.003(3) 0.017(3) C98 0.047(4) 0.034(3) 0.032(3) -0.002(3) -0.005(3) 0.023(3) C99 0.048(4) 0.043(4) 0.032(3) 0.003(3) -0.007(3) 0.030(3) C100 0.038(4) 0.055(4) 0.035(4) -0.019(3) -0.008(3) 0.026(3) C101 0.034(3) 0.033(3) 0.027(3) -0.011(2) 0.002(2) 0.008(3) C102 0.043(4) 0.035(3) 0.030(3) -0.007(3) -0.010(3) 0.015(3) C103 0.025(3) 0.046(4) 0.056(5) -0.001(3) -0.012(3) 0.016(3) C104 0.038(3) 0.034(3) 0.043(4) -0.002(3) 0.001(3) 0.020(3) C105 0.036(4) 0.046(4) 0.030(3) 0.008(3) 0.000(3) 0.006(3) C106 0.068(5) 0.031(4) 0.057(5) 0.001(3) -0.030(4) 0.018(4) C107 0.050(4) 0.064(5) 0.045(4) -0.006(4) -0.010(3) 0.039(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 O1 C5 1.402(8) . ? O2 C34 1.388(8) . ? O15 C35 1.390(7) . ? O3 C25 1.384(7) . ? O4 C49 1.394(8) . ? O5 C7 1.396(7) . ? O6 C17 1.382(7) . ? O7 C6 1.425(8) . ? O8 C13 1.387(8) . ? O9 C41 1.376(8) . ? O10 C24 1.393(8) . ? O11 C52 1.367(7) . ? O12 C58 1.395(8) . ? O13 C44 1.399(7) . ? O14 C15 1.388(7) . ? C1 C32 1.493(8) . ? C1 C39 1.527(9) . ? C3 C37 1.499(9) . ? C3 C54 1.513(8) . ? C4 C27 1.509(8) . ? C4 C9 1.522(9) . ? C5 C22 1.380(9) . ? C5 C37 1.423(9) . ? C6 C60 1.379(9) . ? C6 C57 1.388(8) . ? C7 C27 1.394(8) . ? C7 C38 1.403(8) . ? C8 C77 1.369(10) . ? C8 C17 1.381(9) . ? C8 C72 1.545(9) . ? C9 C43 1.395(9) . ? C9 C25 1.403(9) . ? C10 C82 1.376(9) . ? C10 C15 1.406(9) . ? C10 C62 1.495(9) . ? C11 C13 1.355(10) . ? C11 C70 1.399(9) . ? C11 C62 1.521(10) . ? C12 C83 1.383(10) . ? C12 C25 1.390(8) . ? C12 C56 1.518(9) . ? C13 C81 1.410(9) . ? C14 C15 1.371(9) . ? C14 C59 1.425(9) . ? C14 C40 1.521(10) . ? C17 C31 1.407(9) . ? C18 C20 1.510(9) . ? C18 C81 1.524(9) . ? C19 C91 1.377(10) . ? C19 C68 1.403(10) . ? C20 C33 1.397(9) . ? C20 C35 1.408(8) . ? C21 C74 1.376(9) . ? C21 C35 1.390(8) . ? C21 C29 1.544(9) . ? C22 C104 1.388(10) . ? C22 C29 1.523(9) . ? C23 C24 1.370(9) . ? C23 C102 1.429(10) . ? C23 C101 1.511(9) . ? C24 C39 1.395(9) . ? C26 C31 1.498(8) . ? C26 C38 1.517(8) . ? C27 C28 1.391(8) . ? C28 C53 1.390(10) . ? C30 C99 1.342(10) . ? C30 C58 1.421(9) . ? C30 C72 1.492(9) . ? C31 C65 1.417(9) . ? C32 C55 1.384(9) . ? C32 C44 1.399(8) . ? C33 C78 1.423(10) . ? C34 C73 1.373(10) . ? C34 C68 1.394(10) . ? C36 C63 1.370(9) . ? C36 C90 1.384(10) . ? C37 C85 1.384(10) . ? C38 C67 1.376(9) . ? C39 C100 1.411(10) . ? C40 C45 1.510(9) . ? C41 C84 1.382(9) . ? C41 C61 1.401(9) . ? C42 C45 1.368(9) . ? C42 C92 1.401(10) . ? C43 C103 1.386(10) . ? C44 C79 1.390(10) . ? C45 C52 1.409(9) . ? C46 C48 1.515(10) . ? C46 C57 1.519(10) . ? C47 C55 1.353(10) . ? C47 C93 1.392(9) . ? C48 C58 1.371(10) . ? C48 C80 1.404(9) . ? C49 C51 1.391(10) . ? C49 C63 1.420(9) . ? C50 C95 1.392(11) . ? C50 C60 1.399(10) . ? C51 C75 1.384(10) . ? C51 C87 1.505(9) . ? C52 C54 1.427(9) . ? C53 C67 1.392(10) . ? C54 C86 1.368(9) . ? C56 C60 1.503(9) . ? C57 C66 1.419(10) . ? C59 C97 1.359(11) . ? C61 C105 1.427(10) . ? C61 C101 1.520(9) . ? C63 C69 1.513(10) . ? C64 C84 1.483(9) . ? C64 C68 1.505(10) . ? C65 C71 1.357(11) . ? C66 C95 1.381(11) . ? C69 C79 1.516(9) . ? C70 C98 1.378(10) . ? C71 C77 1.379(11) . ? C73 C76 1.379(10) . ? C73 C87 1.550(10) . ? C74 C78 1.345(10) . ? C75 C90 1.406(10) . ? C76 C91 1.394(11) . ? C79 C93 1.403(9) . ? C80 C94 1.369(11) . ? C81 C96 1.402(9) . ? C82 C97 1.432(10) . ? C83 C103 1.389(12) . ? C84 C88 1.427(10) . ? C85 C89 1.400(10) . ? C86 C92 1.401(9) . ? C88 C106 1.386(10) . ? C89 C104 1.398(11) . ? C94 C99 1.374(11) . ? C96 C98 1.390(10) . ? C100 C107 1.378(12) . ? C102 C107 1.370(12) . ? C105 C106 1.362(11) . ? 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 C32 C1 C39 114.7(5) . . ? C37 C3 C54 116.3(5) . . ? C27 C4 C9 114.5(5) . . ? C22 C5 O1 122.0(6) . . ? C22 C5 C37 120.6(6) . . ? O1 C5 C37 117.4(5) . . ? C60 C6 C57 123.7(6) . . ? C60 C6 O7 117.3(6) . . ? C57 C6 O7 118.8(6) . . ? C27 C7 O5 118.8(5) . . ? C27 C7 C38 121.4(5) . . ? O5 C7 C38 119.8(5) . . ? C77 C8 C17 119.4(6) . . ? C77 C8 C72 119.0(6) . . ? C17 C8 C72 121.5(6) . . ? C43 C9 C25 118.5(6) . . ? C43 C9 C4 119.6(6) . . ? C25 C9 C4 121.8(5) . . ? C82 C10 C15 117.9(6) . . ? C82 C10 C62 119.3(6) . . ? C15 C10 C62 122.6(6) . . ? C13 C11 C70 119.2(7) . . ? C13 C11 C62 121.9(6) . . ? C70 C11 C62 118.5(6) . . ? C83 C12 C25 119.2(6) . . ? C83 C12 C56 120.0(6) . . ? C25 C12 C56 120.8(6) . . ? C11 C13 O8 122.3(6) . . ? C11 C13 C81 121.6(6) . . ? O8 C13 C81 116.0(6) . . ? C15 C14 C59 118.1(6) . . ? C15 C14 C40 122.5(6) . . ? C59 C14 C40 119.4(6) . . ? C14 C15 O14 120.6(6) . . ? C14 C15 C10 122.2(6) . . ? O14 C15 C10 117.1(6) . . ? C8 C17 O6 120.5(5) . . ? C8 C17 C31 121.0(6) . . ? O6 C17 C31 118.5(5) . . ? C20 C18 C81 115.3(5) . . ? C91 C19 C68 123.3(6) . . ? C33 C20 C35 118.0(6) . . ? C33 C20 C18 119.2(6) . . ? C35 C20 C18 122.7(6) . . ? C74 C21 C35 119.5(6) . . ? C74 C21 C29 121.0(6) . . ? C35 C21 C29 119.4(6) . . ? C5 C22 C104 120.2(6) . . ? C5 C22 C29 119.5(6) . . ? C104 C22 C29 120.0(6) . . ? C24 C23 C102 117.9(6) . . ? C24 C23 C101 123.3(6) . . ? C102 C23 C101 118.8(6) . . ? C23 C24 O10 119.4(6) . . ? C23 C24 C39 123.1(6) . . ? O10 C24 C39 117.4(6) . . ? O3 C25 C12 120.9(6) . . ? O3 C25 C9 118.0(5) . . ? C12 C25 C9 121.1(6) . . ? C31 C26 C38 117.8(5) . . ? C28 C27 C7 118.3(5) . . ? C28 C27 C4 119.6(5) . . ? C7 C27 C4 122.1(5) . . ? C53 C28 C27 120.8(6) . . ? C22 C29 C21 115.6(5) . . ? C99 C30 C58 117.7(6) . . ? C99 C30 C72 121.1(6) . . ? C58 C30 C72 121.2(6) . . ? C17 C31 C65 117.0(5) . . ? C17 C31 C26 122.3(6) . . ? C65 C31 C26 120.6(6) . . ? C55 C32 C44 116.4(6) . . ? C55 C32 C1 122.1(6) . . ? C44 C32 C1 121.5(6) . . ? C20 C33 C78 120.3(6) . . ? C73 C34 O2 120.5(6) . . ? C73 C34 C68 121.7(6) . . ? O2 C34 C68 117.6(6) . . ? O15 C35 C21 119.4(5) . . ? O15 C35 C20 120.0(6) . . ? C21 C35 C20 120.5(6) . . ? C63 C36 C90 122.4(6) . . ? C85 C37 C5 117.6(6) . . ? C85 C37 C3 122.3(6) . . ? C5 C37 C3 120.0(6) . . ? C67 C38 C7 118.0(6) . . ? C67 C38 C26 121.7(6) . . ? C7 C38 C26 120.1(5) . . ? C24 C39 C100 117.3(6) . . ? C24 C39 C1 122.4(6) . . ? C100 C39 C1 120.3(6) . . ? C45 C40 C14 114.7(5) . . ? O9 C41 C84 120.8(6) . . ? O9 C41 C61 117.8(6) . . ? C84 C41 C61 121.3(6) . . ? C45 C42 C92 122.0(6) . . ? C103 C43 C9 120.4(7) . . ? C79 C44 O13 117.6(5) . . ? C79 C44 C32 122.1(6) . . ? O13 C44 C32 120.2(6) . . ? C42 C45 C52 119.6(6) . . ? C42 C45 C40 120.5(6) . . ? C52 C45 C40 119.9(6) . . ? C48 C46 C57 116.3(5) . . ? C55 C47 C93 119.3(6) . . ? C58 C48 C80 118.2(6) . . ? C58 C48 C46 120.8(6) . . ? C80 C48 C46 120.9(6) . . ? C51 C49 O4 119.4(6) . . ? C51 C49 C63 121.2(6) . . ? O4 C49 C63 119.4(6) . . ? C95 C50 C60 121.0(7) . . ? C75 C51 C49 118.4(6) . . ? C75 C51 C87 119.7(6) . . ? C49 C51 C87 121.7(6) . . ? O11 C52 C45 119.8(6) . . ? O11 C52 C54 120.6(6) . . ? C45 C52 C54 119.5(6) . . ? C28 C53 C67 119.2(6) . . ? C86 C54 C52 117.7(6) . . ? C86 C54 C3 120.6(6) . . ? C52 C54 C3 121.7(5) . . ? C47 C55 C32 123.4(6) . . ? C60 C56 C12 115.9(5) . . ? C6 C57 C66 116.9(6) . . ? C6 C57 C46 122.6(6) . . ? C66 C57 C46 120.4(6) . . ? C48 C58 O12 119.7(6) . . ? C48 C58 C30 121.9(6) . . ? O12 C58 C30 118.4(6) . . ? C97 C59 C14 121.8(6) . . ? C6 C60 C50 117.0(6) . . ? C6 C60 C56 123.2(6) . . ? C50 C60 C56 119.6(6) . . ? C41 C61 C105 119.3(6) . . ? C41 C61 C101 121.9(6) . . ? C105 C61 C101 118.8(6) . . ? C10 C62 C11 117.3(5) . . ? C36 C63 C49 117.9(6) . . ? C36 C63 C69 120.2(6) . . ? C49 C63 C69 121.8(6) . . ? C84 C64 C68 118.4(6) . . ? C71 C65 C31 121.3(6) . . ? C95 C66 C57 120.1(6) . . ? C38 C67 C53 121.6(6) . . ? C34 C68 C19 116.3(6) . . ? C34 C68 C64 122.9(6) . . ? C19 C68 C64 120.7(6) . . ? C63 C69 C79 116.1(5) . . ? C98 C70 C11 120.6(6) . . ? C65 C71 C77 119.8(6) . . ? C30 C72 C8 114.5(5) . . ? C34 C73 C76 119.7(7) . . ? C34 C73 C87 122.1(6) . . ? C76 C73 C87 118.1(6) . . ? C78 C74 C21 122.1(6) . . ? C51 C75 C90 121.3(6) . . ? C73 C76 C91 121.0(7) . . ? C8 C77 C71 121.1(6) . . ? C74 C78 C33 119.1(7) . . ? C44 C79 C93 117.8(6) . . ? C44 C79 C69 123.4(6) . . ? C93 C79 C69 118.8(6) . . ? C94 C80 C48 119.3(7) . . ? C96 C81 C13 117.7(6) . . ? C96 C81 C18 119.8(6) . . ? C13 C81 C18 122.4(6) . . ? C10 C82 C97 121.8(6) . . ? C12 C83 C103 120.6(7) . . ? C41 C84 C88 117.3(6) . . ? C41 C84 C64 123.4(6) . . ? C88 C84 C64 118.9(6) . . ? C37 C85 C89 122.2(6) . . ? C54 C86 C92 123.5(7) . . ? C51 C87 C73 115.6(5) . . ? C106 C88 C84 121.2(7) . . ? C104 C89 C85 118.5(6) . . ? C36 C90 C75 118.4(6) . . ? C19 C91 C76 117.5(7) . . ? C42 C92 C86 116.9(6) . . ? C47 C93 C79 120.3(6) . . ? C80 C94 C99 121.3(7) . . ? C66 C95 C50 120.3(6) . . ? C98 C96 C81 120.5(6) . . ? C59 C97 C82 117.9(6) . . ? C70 C98 C96 119.5(6) . . ? C30 C99 C94 121.5(7) . . ? C107 C100 C39 120.6(7) . . ? C23 C101 C61 116.5(6) . . ? C107 C102 C23 119.8(7) . . ? C43 C103 C83 120.1(6) . . ? C22 C104 C89 120.4(7) . . ? C106 C105 C61 119.3(7) . . ? C105 C106 C88 120.8(7) . . ? C102 C107 C100 121.1(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.532 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.122