# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(C60H28){Rb(C2H4O)6}2(THF)3.5_(2) _vrf_CHEMW03_C60H28{RbC2H4O6}2THF3.5_2 ; PROBLEM: WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: SQUEEZE was applied during refinement and calculated formula differs from the given by the amount of squeezed solvent ; _vrf_PLAT019_C60H28{RbC2H4O6}2THF3.5_2 ; PROBLEM: Check _diffrn_measured_fraction_theta_full/_max 0.973 RESPONSE: This might be because the structure was initially solved with the older version of software. ; _vrf_PLAT411_C60H28{RbC2H4O6}2THF3.5_2 ; PROBLEM: Short Inter H...H Contact H14 .. H84A .. 1.94 Ang. RESPONSE: The disorder of crown ether ligand was modeled over two orientations. Two disordered orientations of the crown ether ligand have hydrogens which were fixed at geometrically idealized positions. Just because we average two disordered forms into one, some H-H contacts appear very short. In reality, when each unit cell has only one orientation of crown ether ligand, intermolecular H-H contacts will be well within the accepted range. ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; bisdibenzo[1,10-6,7]fluorantheno[2,3-b:2'3'-n] tetraphenylene-bis-((18-crown-6)-rubidium) tetrahydrofuran solvate ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; C60 H28 {Rb C2 H4 O6}2 (C4 H8 O)3.5 ; _chemical_formula_sum 'C98 H104 O15.50 Rb2' _chemical_formula_weight 1700.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3921(2) _cell_length_b 16.1731(3) _cell_length_c 28.6015(5) _cell_angle_alpha 80.358(1) _cell_angle_beta 89.767(1) _cell_angle_gamma 80.008(1) _cell_volume 4216.81(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 65.84 _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_density_diffrn 1.339 _exptl_crystal_F_000 1780 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 2.048 _shelx_estimated_absorpt_T_min 0.709 _shelx_estimated_absorpt_T_max 0.960 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ; ImuS micro-focus source with Quazar optics ; _diffrn_measurement_device_type 'Quazar optics' _diffrn_measurement_method 'Bruker SMART APEX2 area detector' _diffrn_detector_area_resol_mean '0.5 deg wide \w exposures' _diffrn_reflns_number 56730 _diffrn_reflns_av_unetI/netI 0.0546 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.815 _diffrn_reflns_theta_max 66.490 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measured_fraction_theta_full 0.937 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_Laue_measured_fraction_full 0.937 _diffrn_reflns_point_group_measured_fraction_max 0.963 _diffrn_reflns_point_group_measured_fraction_full 0.937 _reflns_number_total 14310 _reflns_number_gt 10031 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. SQUEEZE instruction was employed to account for the solvent electron density (132 electrons/cell), which is in a good agreement with 1.5 THF molecules occupying solvent accessible voids in the crystal lattice.Two additional THF molecules are coordinated to Rb3 above and below the plane of 18-crown-6 ether, and those were refined. ; _computing_data_collection 'Apex2 (Bruker AXS Inc., 2013)' _computing_cell_refinement 'Apex2 (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXT (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXP (Sheldrick, 2008)' _computing_publication_material 'SHELXCIF-2013/2 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1179P)^2^] 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 14310 _refine_ls_number_parameters 1150 _refine_ls_number_restraints 2254 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1739 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.009 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1862(5) 0.1617(3) 0.04981(14) 0.0352(9) Uani 1 1 d . U . . . C2 C 0.2631(5) 0.2110(3) 0.01609(14) 0.0353(9) Uani 1 1 d . U . . . C3 C 0.1628(5) 0.2765(3) -0.01012(15) 0.0396(9) Uani 1 1 d . U . . . C4 C 0.0245(5) 0.2696(3) 0.00817(14) 0.0389(9) Uani 1 1 d . U . . . C5 C 0.0391(5) 0.1980(3) 0.04471(14) 0.0346(9) Uani 1 1 d . U . . . C6 C 0.2509(5) 0.1124(3) 0.09090(14) 0.0335(9) Uani 1 1 d . U . . . C7 C 0.4028(5) 0.1080(3) 0.09539(15) 0.0377(9) Uani 1 1 d . U . . . H7 H 0.4505 0.0833 0.1270 0.045 Uiso 1 1 calc R U . . . C8 C 0.4808(5) 0.1574(3) 0.06146(15) 0.0398(10) Uani 1 1 d . U . . . H8 H 0.5743 0.1699 0.0726 0.048 Uiso 1 1 calc R U . . . C9 C 0.4073(5) 0.2154(3) 0.02208(15) 0.0383(9) Uani 1 1 d . U . . . C10 C 0.4514(5) 0.2881(3) -0.00832(16) 0.0454(11) Uani 1 1 d . U . . . H10 H 0.5516 0.2905 -0.0110 0.055 Uiso 1 1 calc R U . . . C11 C 0.3530(6) 0.3529(3) -0.03316(16) 0.0476(11) Uani 1 1 d . U . . . H11 H 0.3876 0.3998 -0.0513 0.057 Uiso 1 1 calc R U . . . C12 C 0.1987(6) 0.3533(3) -0.03300(15) 0.0457(10) Uani 1 1 d . U . . . C13 C 0.0802(6) 0.4215(3) -0.04211(18) 0.0542(12) Uani 1 1 d . U . . . H13 H 0.0947 0.4738 -0.0606 0.065 Uiso 1 1 calc R U . . . C14 C -0.0596(6) 0.4145(3) -0.02456(18) 0.0541(12) Uani 1 1 d . U . . . H14 H -0.1369 0.4612 -0.0327 0.065 Uiso 1 1 calc R U . . . C15 C -0.0868(5) 0.3382(3) 0.00519(16) 0.0445(10) Uani 1 1 d . U . . . C16 C -0.2004(5) 0.3263(3) 0.03855(17) 0.0475(11) Uani 1 1 d . U . . . H16 H -0.2876 0.3668 0.0357 0.057 Uiso 1 1 calc R U . . . C17 C -0.1831(5) 0.2550(3) 0.07541(16) 0.0431(10) Uani 1 1 d . U . . . H17 H -0.2579 0.2507 0.0977 0.052 Uiso 1 1 calc R U . . . C18 C -0.0606(5) 0.1904(3) 0.08075(14) 0.0355(9) Uani 1 1 d . U . . . C19 C -0.0057(5) 0.1223(3) 0.12127(14) 0.0350(9) Uani 1 1 d . U . . . C20 C 0.1464(4) 0.0851(3) 0.12652(14) 0.0329(9) Uani 1 1 d . U . . . C21 C 0.1751(6) 0.1634(3) 0.41809(15) 0.0446(10) Uani 1 1 d . U . . . C22 C 0.2499(6) 0.2131(3) 0.44295(15) 0.0508(11) Uani 1 1 d . U . . . C23 C 0.1485(7) 0.2785(4) 0.45650(16) 0.0563(13) Uani 1 1 d . U . . . C24 C 0.0120(6) 0.2722(4) 0.43898(17) 0.0555(12) Uani 1 1 d . U . . . C25 C 0.0283(6) 0.1996(3) 0.41554(15) 0.0479(11) Uani 1 1 d . U . . . C26 C 0.2423(5) 0.1142(3) 0.38672(14) 0.0424(10) Uani 1 1 d . U . . . C27 C 0.3946(6) 0.1091(3) 0.38462(16) 0.0473(11) Uani 1 1 d . U . . . H27 H 0.4440 0.0855 0.3575 0.057 Uiso 1 1 calc R U . . . C28 C 0.4704(6) 0.1591(4) 0.40911(17) 0.0537(12) Uani 1 1 d . U . . . H28 H 0.5626 0.1733 0.3950 0.064 Uiso 1 1 calc R U . . . C29 C 0.3943(6) 0.2170(3) 0.43699(17) 0.0532(11) Uani 1 1 d . U . . . C30 C 0.4368(7) 0.2898(4) 0.45387(18) 0.0603(14) Uani 1 1 d . U . . . H30 H 0.5366 0.2926 0.4563 0.072 Uiso 1 1 calc R U . . . C31 C 0.3361(7) 0.3543(4) 0.46637(18) 0.0634(14) Uani 1 1 d . U . . . H31 H 0.3700 0.4010 0.4761 0.076 Uiso 1 1 calc R U . . . C32 C 0.1850(7) 0.3554(4) 0.46562(18) 0.0620(14) Uani 1 1 d . U . . . C33 C 0.0651(7) 0.4224(4) 0.4615(2) 0.0694(16) Uani 1 1 d . U . . . H33 H 0.0779 0.4746 0.4704 0.083 Uiso 1 1 calc R U . . . C34 C -0.0728(8) 0.4157(4) 0.4447(2) 0.0721(16) Uani 1 1 d . U . . . H34 H -0.1498 0.4627 0.4436 0.086 Uiso 1 1 calc R U . . . C35 C -0.1000(7) 0.3393(4) 0.42913(19) 0.0618(14) Uani 1 1 d . U . . . C36 C -0.2116(6) 0.3268(4) 0.3978(2) 0.0614(14) Uani 1 1 d . U . . . H36 H -0.2993 0.3667 0.3933 0.074 Uiso 1 1 calc R U . . . C37 C -0.1927(6) 0.2555(3) 0.37358(18) 0.0539(12) Uani 1 1 d . U . . . H37 H -0.2664 0.2510 0.3520 0.065 Uiso 1 1 calc R U . . . C38 C -0.0688(5) 0.1918(3) 0.38063(16) 0.0465(11) Uani 1 1 d . U . . . C39 C -0.0120(5) 0.1235(3) 0.35325(14) 0.0401(10) Uani 1 1 d . U . . . C40 C 0.1386(5) 0.0854(3) 0.35656(14) 0.0401(10) Uani 1 1 d . U . . . C41 C 0.1891(4) 0.0204(3) 0.16484(14) 0.0336(9) Uani 1 1 d . U . . . H41 H 0.2890 -0.0036 0.1687 0.040 Uiso 1 1 calc R U . . . C42 C 0.0939(5) -0.0116(3) 0.19801(14) 0.0343(9) Uani 1 1 d . U . . . C43 C -0.0538(5) 0.0254(3) 0.19336(14) 0.0353(9) Uani 1 1 d . U . . . C44 C -0.0985(5) 0.0913(3) 0.15580(14) 0.0370(9) Uani 1 1 d . U . . . H44 H -0.1978 0.1169 0.1534 0.044 Uiso 1 1 calc R U . . . C45 C -0.1025(5) 0.0919(3) 0.32416(15) 0.0411(10) Uani 1 1 d . U . . . H45 H -0.2019 0.1171 0.3214 0.049 Uiso 1 1 calc R U . . . C46 C -0.0549(5) 0.0256(3) 0.29907(14) 0.0382(10) Uani 1 1 d . U . . . C47 C 0.0922(5) -0.0108(3) 0.30271(14) 0.0381(9) Uani 1 1 d . U . . . C48 C 0.1852(5) 0.0206(3) 0.33025(14) 0.0379(9) Uani 1 1 d . U . . . H48 H 0.2853 -0.0032 0.3313 0.045 Uiso 1 1 calc R U . . . C49 C 0.1514(5) -0.0889(3) 0.23310(14) 0.0364(9) Uani 1 1 d . U . . . C50 C 0.2170(5) -0.1619(3) 0.21648(16) 0.0445(10) Uani 1 1 d . U . . . H50 H 0.2172 -0.1621 0.1833 0.053 Uiso 1 1 calc R U . . . C51 C 0.2816(6) -0.2339(3) 0.24672(19) 0.0552(13) Uani 1 1 d . U . . . H51 H 0.3239 -0.2835 0.2346 0.066 Uiso 1 1 calc R U . . . C52 C 0.2842(6) -0.2331(3) 0.29564(18) 0.0557(13) Uani 1 1 d . U . . . H52 H 0.3300 -0.2818 0.3170 0.067 Uiso 1 1 calc R U . . . C53 C 0.2206(5) -0.1620(3) 0.31226(16) 0.0455(11) Uani 1 1 d . U . . . H53 H 0.2230 -0.1621 0.3455 0.055 Uiso 1 1 calc R U . . . C54 C 0.1511(5) -0.0883(3) 0.28203(15) 0.0388(9) Uani 1 1 d . U . . . C55 C -0.1643(5) -0.0091(3) 0.22515(15) 0.0377(9) Uani 1 1 d . U . . . C56 C -0.2754(5) -0.0386(3) 0.20422(16) 0.0412(10) Uani 1 1 d . U . . . H56 H -0.2763 -0.0378 0.1709 0.049 Uiso 1 1 calc R U . . . C57 C -0.3846(5) -0.0691(3) 0.23098(16) 0.0461(11) Uani 1 1 d . U . . . H57 H -0.4574 -0.0909 0.2163 0.055 Uiso 1 1 calc R U . . . C58 C -0.3866(5) -0.0675(3) 0.27942(16) 0.0485(12) Uani 1 1 d . U . . . H58 H -0.4623 -0.0869 0.2980 0.058 Uiso 1 1 calc R U . . . C59 C -0.2784(5) -0.0378(3) 0.30038(15) 0.0425(10) Uani 1 1 d . U . . . H59 H -0.2799 -0.0374 0.3336 0.051 Uiso 1 1 calc R U . . . C60 C -0.1660(5) -0.0081(3) 0.27386(15) 0.0391(10) Uani 1 1 d . U . . . C61 C 0.1490(4) -0.0093(3) -0.04863(15) 0.0358(9) Uani 1 1 d . U . . . H61A H 0.0445 -0.0121 -0.0475 0.043 Uiso 1 1 calc R U . . . H61B H 0.1962 -0.0520 -0.0674 0.043 Uiso 1 1 calc R U . . . C62 C 0.2006(4) -0.1127(3) 0.02068(14) 0.0347(9) Uani 1 1 d . U . . . H62A H 0.2526 -0.1543 0.0020 0.042 Uiso 1 1 calc R U . . . H62B H 0.0980 -0.1198 0.0223 0.042 Uiso 1 1 calc R U . . . C63 C 0.2666(4) -0.1283(3) 0.06988(14) 0.0366(9) Uani 1 1 d . U . . . H63A H 0.2242 -0.0818 0.0869 0.044 Uiso 1 1 calc R U . . . H63B H 0.2457 -0.1826 0.0877 0.044 Uiso 1 1 calc R U . . . C64 C 0.4912(5) -0.1505(3) 0.11147(14) 0.0365(9) Uani 1 1 d . U . . . H64A H 0.4702 -0.2047 0.1294 0.044 Uiso 1 1 calc R U . . . H64B H 0.4579 -0.1047 0.1301 0.044 Uiso 1 1 calc R U . . . C65 C 0.6511(5) -0.1576(3) 0.10371(15) 0.0361(9) Uani 1 1 d . U . . . H65A H 0.7049 -0.1778 0.1343 0.043 Uiso 1 1 calc R U . . . H65B H 0.6825 -0.1993 0.0824 0.043 Uiso 1 1 calc R U . . . C66 C 0.8306(4) -0.0780(3) 0.07180(15) 0.0350(9) Uani 1 1 d . U . . . H66A H 0.8600 -0.1193 0.0501 0.042 Uiso 1 1 calc R U . . . H66B H 0.8914 -0.0965 0.1011 0.042 Uiso 1 1 calc R U . . . C67 C 0.2624(5) -0.1237(3) 0.45368(16) 0.0459(11) Uani 1 1 d . U . . . H67A H 0.2376 -0.1762 0.4448 0.055 Uiso 1 1 calc R U . . . H67B H 0.2234 -0.0750 0.4287 0.055 Uiso 1 1 calc R U . . . C68 C 0.4886(5) -0.1478(3) 0.41606(15) 0.0467(11) Uani 1 1 d . U . . . H68A H 0.4563 -0.1004 0.3896 0.056 Uiso 1 1 calc R U . . . H68B H 0.4668 -0.2010 0.4072 0.056 Uiso 1 1 calc R U . . . C69 C 0.6490(6) -0.1563(3) 0.42553(16) 0.0483(11) Uani 1 1 d . U . . . H69A H 0.6784 -0.1977 0.4549 0.058 Uiso 1 1 calc R U . . . H69B H 0.7036 -0.1773 0.3989 0.058 Uiso 1 1 calc R U . . . C70 C 0.8289(5) -0.0779(3) 0.44115(17) 0.0489(11) Uani 1 1 d . U . . . H70A H 0.8886 -0.0962 0.4149 0.059 Uiso 1 1 calc R U . . . H70B H 0.8590 -0.1195 0.4704 0.059 Uiso 1 1 calc R U . . . C71 C 0.8517(5) 0.0089(3) 0.44789(16) 0.0471(11) Uani 1 1 d . U . . . H71A H 0.9564 0.0109 0.4484 0.056 Uiso 1 1 calc R U . . . H71B H 0.8050 0.0522 0.4213 0.056 Uiso 1 1 calc R U . . . C72 C 0.8019(5) 0.1100(3) 0.49912(16) 0.0471(11) Uani 1 1 d . U . . . H72A H 0.7495 0.1528 0.4733 0.057 Uiso 1 1 calc R U . . . H72B H 0.9047 0.1166 0.4990 0.057 Uiso 1 1 calc R U . . . Rb1 Rb 0.5000 0.0000 0.0000 0.03851(16) Uani 1 2 d S U P . . Rb2 Rb 0.5000 0.0000 0.5000 0.0516(2) Uani 1 2 d S U P . . O1 O 0.2102(3) -0.02811(18) -0.00174(9) 0.0337(6) Uani 1 1 d . U . . . O2 O 0.4182(3) -0.13194(19) 0.06692(9) 0.0357(6) Uani 1 1 d . U . . . O3 O 0.6810(3) -0.07569(18) 0.08300(9) 0.0345(6) Uani 1 1 d . U . . . O4 O 0.4153(3) -0.1313(2) 0.45833(10) 0.0462(8) Uani 1 1 d . U . . . O5 O 0.6800(3) -0.0755(2) 0.43047(10) 0.0462(7) Uani 1 1 d . U . . . O6 O 0.7903(4) 0.0269(2) 0.49173(10) 0.0457(7) Uani 1 1 d . U . . . Rb3 Rb 0.31914(6) 0.41065(3) 0.21343(2) 0.05196(16) Uani 1 1 d . U . . . O7 O 0.5929(9) 0.2391(5) 0.2084(3) 0.121(2) Uani 0.42(3) 1 d . U P A 1 C73 C 0.5686(8) 0.2677(5) 0.2485(2) 0.1025(17) Uani 0.42(3) 1 d . U P A 1 H73A H 0.5082 0.3251 0.2428 0.123 Uiso 0.42(3) 1 calc R U P A 1 H73B H 0.6610 0.2712 0.2640 0.123 Uiso 0.42(3) 1 calc R U P A 1 O7A O 0.5686(8) 0.2677(5) 0.2485(2) 0.1025(17) Uani 0.58(3) 1 d . U P A 2 C73A C 0.5929(9) 0.2391(5) 0.2084(3) 0.121(2) Uani 0.58(3) 1 d . U P A 2 H73C H 0.6937 0.2081 0.2090 0.145 Uiso 0.58(3) 1 calc R U P A 2 H73D H 0.5830 0.2881 0.1821 0.145 Uiso 0.58(3) 1 calc R U P A 2 C74 C 0.4950(9) 0.1823(5) 0.1990(3) 0.096(2) Uani 1 1 d . U . . . H74A H 0.5494 0.1268 0.1935 0.115 Uiso 1 1 calc R U . A 1 H74B H 0.4306 0.2083 0.1712 0.115 Uiso 1 1 calc R U . A 1 C75 C 0.4101(8) 0.1722(5) 0.2440(3) 0.087(2) Uani 1 1 d . U . . . H75A H 0.4067 0.1115 0.2559 0.105 Uiso 1 1 calc R U . . . H75B H 0.3101 0.2043 0.2388 0.105 Uiso 1 1 calc R U . . . C76 C 0.4953(9) 0.2090(6) 0.2779(3) 0.0992(19) Uani 1 1 d . U . . . H76A H 0.4297 0.2385 0.2995 0.119 Uiso 1 1 calc R U . A 1 H76B H 0.5654 0.1634 0.2972 0.119 Uiso 1 1 calc R U . A 1 O8 O 0.1854(7) 0.5865(3) 0.1878(2) 0.1089(16) Uani 1 1 d . U . . . C77 C 0.1850(9) 0.6386(5) 0.1423(3) 0.089(2) Uani 1 1 d . U . . . H77A H 0.2008 0.6029 0.1172 0.107 Uiso 1 1 calc R U . . . H77B H 0.2623 0.6734 0.1409 0.107 Uiso 1 1 calc R U . . . C78 C 0.0380(7) 0.6950(4) 0.1358(2) 0.0779(18) Uani 1 1 d . U . . . H78A H 0.0411 0.7511 0.1449 0.093 Uiso 1 1 calc R U . . . H78B H 0.0023 0.7037 0.1025 0.093 Uiso 1 1 calc R U . . . C79 C -0.0540(10) 0.6471(7) 0.1680(4) 0.128(3) Uani 1 1 d . U . . . H79A H -0.0878 0.6027 0.1531 0.153 Uiso 1 1 calc R U . B 1 H79B H -0.1387 0.6855 0.1778 0.153 Uiso 1 1 calc R U . B 1 C80 C 0.0529(16) 0.6069(12) 0.2109(7) 0.092(3) Uani 0.62(3) 1 d . U P C 1 H80A H 0.0595 0.6482 0.2324 0.110 Uiso 0.62(3) 1 calc R U P C 1 H80B H 0.0234 0.5552 0.2292 0.110 Uiso 0.62(3) 1 calc R U P C 1 C80A C 0.024(3) 0.576(2) 0.1912(14) 0.107(5) Uani 0.38(3) 1 d . U P C 2 H80C H 0.0090 0.5263 0.1766 0.128 Uiso 0.38(3) 1 calc R U P C 2 H80D H -0.0040 0.5657 0.2248 0.128 Uiso 0.38(3) 1 calc R U P C 2 O9 O 0.5955(9) 0.4674(6) 0.2109(2) 0.0821(19) Uani 0.613(4) 1 d D U P D 1 C81 C 0.6218(14) 0.5049(7) 0.1634(4) 0.083(3) Uani 0.613(4) 1 d D U P D 1 H81A H 0.5533 0.5591 0.1545 0.099 Uiso 0.613(4) 1 calc R U P D 1 H81B H 0.7211 0.5179 0.1619 0.099 Uiso 0.613(4) 1 calc R U P D 1 C82 C 0.6059(11) 0.4496(7) 0.1304(3) 0.076(3) Uani 0.613(4) 1 d D U P D 1 H82A H 0.6350 0.4756 0.0987 0.091 Uiso 0.613(4) 1 calc R U P D 1 H82B H 0.6728 0.3949 0.1401 0.091 Uiso 0.613(4) 1 calc R U P D 1 O10 O 0.4678(9) 0.4330(6) 0.1265(2) 0.089(2) Uani 0.613(4) 1 d D U P D 1 C83 C 0.4252(15) 0.3924(11) 0.0934(4) 0.078(4) Uani 0.613(4) 1 d D U P D 1 H83A H 0.4850 0.3348 0.0978 0.094 Uiso 0.613(4) 1 calc R U P D 1 H83B H 0.4481 0.4228 0.0621 0.094 Uiso 0.613(4) 1 calc R U P D 1 C84 C 0.2804(12) 0.3830(7) 0.0916(3) 0.075(3) Uani 0.613(4) 1 d D U P D 1 H84A H 0.2223 0.4387 0.0777 0.090 Uiso 0.613(4) 1 calc R U P D 1 H84B H 0.2712 0.3428 0.0697 0.090 Uiso 0.613(4) 1 calc R U P D 1 O11 O 0.2213(8) 0.3546(7) 0.1338(2) 0.094(2) Uani 0.613(4) 1 d D U P D 1 C85 C 0.0842(19) 0.3411(16) 0.1354(4) 0.087(4) Uani 0.613(4) 1 d D U P D 1 H85A H 0.0711 0.3057 0.1112 0.105 Uiso 0.613(4) 1 calc R U P D 1 H85B H 0.0199 0.3968 0.1259 0.105 Uiso 0.613(4) 1 calc R U P D 1 C86 C 0.0335(13) 0.2999(10) 0.1809(4) 0.094(3) Uani 0.613(4) 1 d D U P D 1 H86A H -0.0725 0.3027 0.1787 0.113 Uiso 0.613(4) 1 calc R U P D 1 H86B H 0.0795 0.2390 0.1872 0.113 Uiso 0.613(4) 1 calc R U P D 1 O12 O 0.0663(7) 0.3387(4) 0.2180(2) 0.0674(16) Uani 0.613(4) 1 d D U P D 1 C87 C 0.0290(12) 0.2992(7) 0.2637(4) 0.065(3) Uani 0.613(4) 1 d D U P D 1 H87A H 0.0846 0.2406 0.2712 0.077 Uiso 0.613(4) 1 calc R U P D 1 H87B H -0.0752 0.2958 0.2638 0.077 Uiso 0.613(4) 1 calc R U P D 1 C88 C 0.0616(11) 0.3493(8) 0.3006(4) 0.067(3) Uani 0.613(4) 1 d D U P D 1 H88A H -0.0099 0.4029 0.2965 0.080 Uiso 0.613(4) 1 calc R U P D 1 H88B H 0.0467 0.3165 0.3321 0.080 Uiso 0.613(4) 1 calc R U P D 1 O13 O 0.1947(9) 0.3695(6) 0.3008(2) 0.092(2) Uani 0.613(4) 1 d D U P D 1 C89 C 0.2425(15) 0.4008(13) 0.3388(4) 0.082(4) Uani 0.613(4) 1 d D U P D 1 H89A H 0.2243 0.3634 0.3686 0.098 Uiso 0.613(4) 1 calc R U P D 1 H89B H 0.1856 0.4582 0.3395 0.098 Uiso 0.613(4) 1 calc R U P D 1 C90 C 0.3948(15) 0.4065(11) 0.3375(3) 0.110(4) Uani 0.613(4) 1 d D U P D 1 H90A H 0.4185 0.4339 0.3642 0.132 Uiso 0.613(4) 1 calc R U P D 1 H90B H 0.4517 0.3480 0.3425 0.132 Uiso 0.613(4) 1 calc R U P D 1 O14 O 0.4366(7) 0.4496(5) 0.2974(2) 0.0682(16) Uani 0.613(4) 1 d D U P D 1 C91 C 0.5758(14) 0.4666(11) 0.2930(4) 0.096(4) Uani 0.613(4) 1 d D U P D 1 H91A H 0.5891 0.5040 0.3161 0.116 Uiso 0.613(4) 1 calc R U P D 1 H91B H 0.6430 0.4121 0.3029 0.116 Uiso 0.613(4) 1 calc R U P D 1 C92 C 0.6195(16) 0.5037(11) 0.2496(4) 0.116(4) Uani 0.613(4) 1 d D U P D 1 H92A H 0.5703 0.5639 0.2433 0.139 Uiso 0.613(4) 1 calc R U P D 1 H92B H 0.7246 0.5038 0.2521 0.139 Uiso 0.613(4) 1 calc R U P D 1 O9A O 0.5231(14) 0.4911(10) 0.2470(4) 0.107(3) Uani 0.387(4) 1 d D U P D 2 C81A C 0.643(2) 0.4901(18) 0.2189(6) 0.110(5) Uani 0.387(4) 1 d D U P D 2 H81C H 0.6657 0.5482 0.2147 0.132 Uiso 0.387(4) 1 calc R U P D 2 H81D H 0.7233 0.4523 0.2381 0.132 Uiso 0.387(4) 1 calc R U P D 2 C82A C 0.6493(19) 0.4673(17) 0.1754(6) 0.110(6) Uani 0.387(4) 1 d D U P D 2 H82C H 0.7232 0.4150 0.1778 0.132 Uiso 0.387(4) 1 calc R U P D 2 H82D H 0.6878 0.5125 0.1540 0.132 Uiso 0.387(4) 1 calc R U P D 2 O10A O 0.5289(12) 0.4521(10) 0.1523(4) 0.097(3) Uani 0.387(4) 1 d D U P D 2 C83A C 0.4940(19) 0.4644(13) 0.1063(4) 0.091(4) Uani 0.387(4) 1 d D U P D 2 H83C H 0.5853 0.4541 0.0891 0.109 Uiso 0.387(4) 1 calc R U P D 2 H83D H 0.4519 0.5254 0.0968 0.109 Uiso 0.387(4) 1 calc R U P D 2 C84A C 0.401(2) 0.4181(19) 0.0899(5) 0.089(6) Uani 0.387(4) 1 d D U P D 2 H84C H 0.4570 0.3617 0.0865 0.107 Uiso 0.387(4) 1 calc R U P D 2 H84D H 0.3660 0.4473 0.0577 0.107 Uiso 0.387(4) 1 calc R U P D 2 O11A O 0.2813(13) 0.4045(8) 0.1165(3) 0.080(2) Uani 0.387(4) 1 d D U P D 2 C85A C 0.1977(18) 0.3500(13) 0.1043(5) 0.090(4) Uani 0.387(4) 1 d D U P D 2 H85C H 0.2584 0.2928 0.1073 0.107 Uiso 0.387(4) 1 calc R U P D 2 H85D H 0.1685 0.3686 0.0704 0.107 Uiso 0.387(4) 1 calc R U P D 2 C86A C 0.067(3) 0.342(3) 0.1314(6) 0.093(5) Uani 0.387(4) 1 d D U P D 2 H86C H -0.0059 0.3941 0.1221 0.112 Uiso 0.387(4) 1 calc R U P D 2 H86D H 0.0266 0.2932 0.1235 0.112 Uiso 0.387(4) 1 calc R U P D 2 O12A O 0.0947(13) 0.3293(8) 0.1808(3) 0.082(3) Uani 0.387(4) 1 d D U P D 2 C87A C -0.0286(17) 0.3217(15) 0.2078(5) 0.098(5) Uani 0.387(4) 1 d D U P D 2 H87C H -0.0558 0.2658 0.2059 0.117 Uiso 0.387(4) 1 calc R U P D 2 H87D H -0.1091 0.3663 0.1931 0.117 Uiso 0.387(4) 1 calc R U P D 2 C88A C -0.015(2) 0.3284(18) 0.2566(6) 0.098(6) Uani 0.387(4) 1 d D U P D 2 H88C H -0.1093 0.3591 0.2653 0.118 Uiso 0.387(4) 1 calc R U P D 2 H88D H -0.0041 0.2697 0.2746 0.118 Uiso 0.387(4) 1 calc R U P D 2 O13A O 0.0851(12) 0.3640(9) 0.2740(3) 0.088(3) Uani 0.387(4) 1 d D U P D 2 C89A C 0.115(2) 0.3538(13) 0.3225(4) 0.086(5) Uani 0.387(4) 1 d D U P D 2 H89C H 0.1666 0.2949 0.3335 0.103 Uiso 0.387(4) 1 calc R U P D 2 H89D H 0.0230 0.3612 0.3393 0.103 Uiso 0.387(4) 1 calc R U P D 2 C90A C 0.200(3) 0.411(2) 0.3348(6) 0.092(5) Uani 0.387(4) 1 d D U P D 2 H90C H 0.1379 0.4679 0.3313 0.110 Uiso 0.387(4) 1 calc R U P D 2 H90D H 0.2274 0.3933 0.3689 0.110 Uiso 0.387(4) 1 calc R U P D 2 O14A O 0.3207(14) 0.4194(9) 0.3108(3) 0.090(3) Uani 0.387(4) 1 d D U P D 2 C91A C 0.404(2) 0.4770(16) 0.3216(5) 0.112(5) Uani 0.387(4) 1 d D U P D 2 H91C H 0.3378 0.5314 0.3224 0.134 Uiso 0.387(4) 1 calc R U P D 2 H91D H 0.4436 0.4558 0.3543 0.134 Uiso 0.387(4) 1 calc R U P D 2 C92A C 0.517(2) 0.496(2) 0.2942(6) 0.110(6) Uani 0.387(4) 1 d D U P D 2 H92C H 0.6049 0.4583 0.3094 0.132 Uiso 0.387(4) 1 calc R U P D 2 H92D H 0.5267 0.5547 0.2970 0.132 Uiso 0.387(4) 1 calc R U P D 2 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 0.043(2) 0.039(2) 0.029(2) -0.0136(16) 0.0060(17) -0.0143(18) C2 0.049(2) 0.037(2) 0.0225(19) -0.0090(16) 0.0049(18) -0.0112(18) C3 0.052(2) 0.046(2) 0.026(2) -0.0133(17) 0.0073(19) -0.0157(19) C4 0.048(2) 0.048(2) 0.026(2) -0.0128(17) -0.0028(18) -0.0162(19) C5 0.042(2) 0.042(2) 0.026(2) -0.0130(16) -0.0012(17) -0.0146(18) C6 0.039(2) 0.041(2) 0.025(2) -0.0121(16) 0.0018(17) -0.0122(18) C7 0.038(2) 0.046(2) 0.031(2) -0.0101(18) 0.0042(18) -0.0098(18) C8 0.036(2) 0.051(2) 0.035(2) -0.0102(18) 0.0091(18) -0.0139(19) C9 0.048(2) 0.043(2) 0.030(2) -0.0122(17) 0.0120(18) -0.0160(19) C10 0.051(3) 0.052(3) 0.038(2) -0.012(2) 0.012(2) -0.018(2) C11 0.068(3) 0.048(3) 0.033(2) -0.0079(19) 0.010(2) -0.025(2) C12 0.068(3) 0.045(2) 0.027(2) -0.0095(18) 0.002(2) -0.015(2) C13 0.075(3) 0.046(3) 0.042(3) -0.007(2) 0.004(2) -0.013(2) C14 0.071(3) 0.047(3) 0.043(3) -0.006(2) -0.004(2) -0.008(2) C15 0.048(3) 0.054(3) 0.034(2) -0.0147(19) -0.009(2) -0.009(2) C16 0.042(2) 0.057(3) 0.044(3) -0.012(2) -0.009(2) -0.005(2) C17 0.040(2) 0.059(3) 0.036(2) -0.019(2) 0.0000(19) -0.015(2) C18 0.039(2) 0.043(2) 0.029(2) -0.0111(17) -0.0009(17) -0.0141(18) C19 0.037(2) 0.051(2) 0.0219(19) -0.0126(17) -0.0014(16) -0.0146(18) C20 0.035(2) 0.046(2) 0.0225(19) -0.0136(16) 0.0016(16) -0.0119(18) C21 0.062(3) 0.055(3) 0.024(2) -0.0058(18) 0.008(2) -0.030(2) C22 0.079(3) 0.057(3) 0.024(2) -0.0071(19) 0.008(2) -0.033(2) C23 0.086(3) 0.069(3) 0.028(2) -0.019(2) 0.019(2) -0.045(3) C24 0.075(3) 0.067(3) 0.038(3) -0.023(2) 0.028(2) -0.035(3) C25 0.073(3) 0.057(3) 0.027(2) -0.0147(19) 0.021(2) -0.041(2) C26 0.063(3) 0.050(3) 0.020(2) -0.0046(17) 0.0009(19) -0.029(2) C27 0.059(3) 0.058(3) 0.031(2) -0.0090(19) 0.000(2) -0.025(2) C28 0.063(3) 0.067(3) 0.039(3) -0.011(2) -0.003(2) -0.031(2) C29 0.070(3) 0.064(3) 0.031(2) -0.004(2) -0.004(2) -0.034(2) C30 0.080(4) 0.071(3) 0.042(3) -0.016(2) 0.001(3) -0.042(3) C31 0.090(4) 0.074(4) 0.041(3) -0.017(3) 0.008(3) -0.046(3) C32 0.092(4) 0.070(3) 0.039(3) -0.025(2) 0.022(3) -0.039(3) C33 0.095(4) 0.077(4) 0.056(3) -0.037(3) 0.032(3) -0.045(3) C34 0.087(4) 0.073(4) 0.069(4) -0.036(3) 0.033(3) -0.027(3) C35 0.077(3) 0.073(3) 0.051(3) -0.032(3) 0.036(3) -0.037(3) C36 0.064(3) 0.064(3) 0.063(3) -0.022(3) 0.029(3) -0.020(3) C37 0.058(3) 0.066(3) 0.048(3) -0.021(2) 0.023(2) -0.027(2) C38 0.056(3) 0.059(3) 0.033(2) -0.015(2) 0.018(2) -0.028(2) C39 0.052(2) 0.051(3) 0.024(2) -0.0085(18) 0.0117(19) -0.025(2) C40 0.054(2) 0.050(3) 0.020(2) -0.0033(17) 0.0044(18) -0.024(2) C41 0.032(2) 0.049(2) 0.025(2) -0.0143(17) 0.0004(16) -0.0106(18) C42 0.040(2) 0.049(2) 0.0201(19) -0.0130(16) 0.0036(16) -0.0158(18) C43 0.039(2) 0.050(2) 0.024(2) -0.0131(17) 0.0055(17) -0.0206(19) C44 0.035(2) 0.052(3) 0.029(2) -0.0150(18) 0.0042(17) -0.0149(19) C45 0.044(2) 0.055(3) 0.031(2) -0.0110(19) 0.0136(19) -0.024(2) C46 0.043(2) 0.056(3) 0.0207(19) -0.0080(17) 0.0109(17) -0.021(2) C47 0.049(2) 0.050(2) 0.022(2) -0.0070(17) 0.0085(18) -0.0241(19) C48 0.043(2) 0.053(3) 0.0207(19) -0.0041(17) 0.0047(17) -0.020(2) C49 0.040(2) 0.045(2) 0.029(2) -0.0088(17) 0.0038(17) -0.0194(18) C50 0.055(3) 0.050(3) 0.033(2) -0.0100(19) 0.005(2) -0.015(2) C51 0.069(3) 0.048(3) 0.050(3) -0.014(2) 0.011(3) -0.010(2) C52 0.075(4) 0.049(3) 0.040(3) 0.001(2) -0.001(3) -0.010(2) C53 0.058(3) 0.050(3) 0.030(2) -0.0024(18) -0.001(2) -0.019(2) C54 0.044(2) 0.048(2) 0.027(2) -0.0066(17) 0.0012(18) -0.0179(19) C55 0.037(2) 0.051(3) 0.028(2) -0.0107(18) 0.0063(18) -0.0142(19) C56 0.044(2) 0.055(3) 0.031(2) -0.0155(19) 0.0047(19) -0.018(2) C57 0.042(2) 0.067(3) 0.037(2) -0.014(2) 0.001(2) -0.023(2) C58 0.047(3) 0.070(3) 0.036(2) -0.011(2) 0.012(2) -0.029(2) C59 0.046(2) 0.058(3) 0.029(2) -0.012(2) 0.0101(19) -0.021(2) C60 0.042(2) 0.050(3) 0.030(2) -0.0118(18) 0.0051(18) -0.017(2) C61 0.028(2) 0.050(3) 0.033(2) -0.0128(18) 0.0001(16) -0.0123(18) C62 0.030(2) 0.046(2) 0.033(2) -0.0083(17) 0.0034(17) -0.0157(18) C63 0.032(2) 0.052(3) 0.030(2) -0.0105(18) 0.0084(17) -0.0154(19) C64 0.040(2) 0.051(3) 0.0219(19) -0.0091(17) 0.0028(17) -0.0153(19) C65 0.040(2) 0.044(2) 0.026(2) -0.0058(17) -0.0014(17) -0.0109(18) C66 0.0297(19) 0.043(2) 0.035(2) -0.0098(18) 0.0019(17) -0.0094(17) C67 0.051(3) 0.063(3) 0.029(2) -0.005(2) -0.004(2) -0.027(2) C68 0.061(3) 0.060(3) 0.026(2) -0.0100(19) 0.002(2) -0.026(2) C69 0.060(3) 0.063(3) 0.029(2) -0.014(2) 0.009(2) -0.026(2) C70 0.050(3) 0.068(3) 0.035(2) -0.011(2) 0.010(2) -0.024(2) C71 0.045(2) 0.072(3) 0.029(2) -0.010(2) 0.011(2) -0.024(2) C72 0.051(3) 0.063(3) 0.033(2) -0.002(2) -0.001(2) -0.031(2) Rb1 0.0337(3) 0.0541(4) 0.0300(3) 0.0005(2) -0.0023(2) -0.0216(3) Rb2 0.0521(4) 0.0748(5) 0.0422(4) -0.0244(3) 0.0143(3) -0.0368(3) O1 0.0322(14) 0.0452(16) 0.0280(14) -0.0095(12) 0.0038(11) -0.0157(12) O2 0.0350(14) 0.0543(17) 0.0220(13) -0.0068(12) 0.0049(11) -0.0187(13) O3 0.0332(14) 0.0458(16) 0.0271(14) -0.0070(12) 0.0039(11) -0.0130(12) O4 0.0512(18) 0.068(2) 0.0266(15) -0.0082(14) 0.0011(14) -0.0291(16) O5 0.0492(18) 0.064(2) 0.0307(16) -0.0085(14) 0.0051(14) -0.0247(15) O6 0.0538(18) 0.061(2) 0.0283(15) -0.0064(13) 0.0061(14) -0.0288(16) Rb3 0.0590(3) 0.0666(3) 0.0333(3) -0.0061(2) 0.0007(2) -0.0216(2) O7 0.123(4) 0.108(4) 0.146(5) -0.050(4) 0.064(4) -0.034(3) C73 0.116(4) 0.121(4) 0.076(4) -0.007(3) -0.005(3) -0.046(3) O7A 0.116(4) 0.121(4) 0.076(4) -0.007(3) -0.005(3) -0.046(3) C73A 0.123(4) 0.108(4) 0.146(5) -0.050(4) 0.064(4) -0.034(3) C74 0.107(6) 0.085(5) 0.098(5) -0.040(4) 0.012(4) -0.004(4) C75 0.067(4) 0.085(5) 0.104(5) 0.001(4) -0.005(4) -0.015(3) C76 0.102(5) 0.124(4) 0.072(4) 0.006(3) -0.011(3) -0.040(4) O8 0.138(4) 0.085(3) 0.093(4) 0.002(2) 0.000(3) -0.008(3) C77 0.109(5) 0.067(4) 0.082(5) 0.008(3) -0.007(4) -0.006(4) C78 0.089(4) 0.073(4) 0.074(4) -0.002(3) -0.024(3) -0.028(3) C79 0.100(5) 0.129(7) 0.137(8) 0.042(6) -0.012(5) -0.038(5) C80 0.101(6) 0.081(6) 0.090(8) 0.001(5) 0.002(5) -0.026(5) C80A 0.126(7) 0.077(8) 0.102(13) 0.010(7) 0.024(8) 0.000(7) O9 0.080(4) 0.122(5) 0.054(3) 0.001(4) 0.005(3) -0.058(4) C81 0.112(8) 0.061(6) 0.082(5) 0.005(5) 0.026(6) -0.054(6) C82 0.076(5) 0.097(7) 0.045(5) 0.013(4) 0.010(4) -0.010(5) O10 0.127(6) 0.106(5) 0.057(4) -0.035(3) 0.036(4) -0.068(4) C83 0.078(6) 0.110(10) 0.045(5) -0.029(6) 0.012(5) 0.004(7) C84 0.112(7) 0.072(6) 0.042(4) -0.007(5) -0.004(5) -0.025(6) O11 0.078(4) 0.168(7) 0.049(3) -0.050(4) 0.010(3) -0.030(4) C85 0.118(8) 0.099(9) 0.065(5) -0.020(7) -0.024(6) -0.069(8) C86 0.085(8) 0.137(10) 0.078(6) -0.045(6) 0.003(6) -0.043(7) O12 0.079(3) 0.079(4) 0.054(3) -0.011(3) 0.000(3) -0.040(3) C87 0.054(6) 0.066(6) 0.076(5) -0.004(5) 0.010(5) -0.023(5) C88 0.062(5) 0.085(7) 0.052(6) -0.002(5) 0.020(5) -0.021(5) O13 0.103(5) 0.154(6) 0.042(3) -0.025(3) 0.020(3) -0.078(4) C89 0.094(8) 0.132(10) 0.028(5) -0.012(6) 0.013(5) -0.045(8) C90 0.129(8) 0.172(11) 0.050(5) -0.021(7) 0.004(6) -0.080(9) O14 0.071(4) 0.097(4) 0.048(3) -0.022(3) 0.004(3) -0.035(3) C91 0.098(8) 0.142(11) 0.063(6) -0.015(7) -0.020(6) -0.060(8) C92 0.122(9) 0.165(11) 0.099(7) -0.057(8) 0.032(7) -0.099(8) O9A 0.117(7) 0.139(6) 0.092(7) -0.050(7) 0.007(5) -0.069(6) C81A 0.118(11) 0.132(14) 0.095(10) -0.002(11) 0.000(7) -0.080(10) C82A 0.113(10) 0.133(15) 0.112(10) -0.031(11) 0.045(7) -0.087(11) O10A 0.095(6) 0.134(8) 0.070(5) -0.011(5) 0.027(5) -0.049(6) C83A 0.109(10) 0.091(11) 0.068(6) 0.002(8) 0.042(7) -0.023(8) C84A 0.080(10) 0.133(16) 0.041(6) -0.007(9) 0.011(6) 0.009(10) O11A 0.141(7) 0.081(6) 0.034(4) -0.017(4) 0.022(4) -0.054(5) C85A 0.129(11) 0.104(11) 0.046(7) -0.035(8) -0.008(7) -0.028(9) C86A 0.104(11) 0.114(14) 0.072(8) -0.022(11) -0.025(8) -0.040(10) O12A 0.104(6) 0.097(7) 0.061(5) -0.017(5) -0.001(4) -0.060(5) C87A 0.079(9) 0.121(12) 0.101(8) -0.016(10) 0.003(8) -0.043(9) C88A 0.055(10) 0.147(16) 0.099(9) -0.025(12) 0.025(8) -0.033(10) O13A 0.072(7) 0.132(9) 0.054(6) 0.021(6) 0.005(5) -0.039(6) C89A 0.114(12) 0.098(11) 0.045(7) 0.011(8) 0.032(8) -0.041(9) C90A 0.127(12) 0.106(12) 0.050(8) -0.025(10) 0.027(8) -0.028(10) O14A 0.126(8) 0.122(7) 0.035(4) -0.020(4) 0.001(4) -0.054(5) C91A 0.171(13) 0.129(13) 0.053(8) -0.020(10) -0.019(8) -0.071(11) C92A 0.120(13) 0.146(15) 0.084(9) -0.035(11) -0.024(8) -0.058(12) _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 C6 1.382(6) . ? C1 C5 1.402(6) . ? C1 C2 1.423(6) . ? C2 C9 1.382(6) . ? C2 C3 1.402(6) . ? C3 C12 1.399(6) . ? C3 C4 1.414(6) . ? C4 C15 1.377(7) . ? C4 C5 1.411(6) . ? C5 C18 1.395(6) . ? C6 C7 1.422(6) . ? C6 C20 1.479(5) . ? C7 C8 1.433(6) . ? C7 Rb1 3.514(4) . ? C7 H7 1.0000 . ? C8 C9 1.433(6) . ? C8 Rb1 3.307(4) . ? C8 H8 1.0000 . ? C9 C10 1.460(6) . ? C9 Rb1 3.602(4) . ? C10 C11 1.371(7) . ? C10 H10 0.9500 . ? C11 C12 1.447(7) . ? C11 H11 0.9500 . ? C12 C13 1.416(7) . ? C13 C14 1.420(8) . ? C13 H13 0.9500 . ? C14 C15 1.438(7) . ? C14 H14 0.9500 . ? C15 C16 1.445(7) . ? C16 C17 1.412(7) . ? C16 H16 0.9500 . ? C17 C18 1.404(6) . ? C17 H17 0.9500 . ? C18 C19 1.484(6) . ? C19 C44 1.402(6) . ? C19 C20 1.448(6) . ? C20 C41 1.390(6) . ? C21 C26 1.378(7) . ? C21 C25 1.398(8) . ? C21 C22 1.427(7) . ? C22 C29 1.376(8) . ? C22 C23 1.400(8) . ? C23 C24 1.404(8) . ? C23 C32 1.410(7) . ? C24 C35 1.367(9) . ? C24 C25 1.432(7) . ? C25 C38 1.391(7) . ? C26 C27 1.419(7) . ? C26 C40 1.486(6) . ? C27 C28 1.430(7) . ? C27 Rb2 3.529(5) . ? C27 H27 1.0000 . ? C28 C29 1.427(8) . ? C28 Rb2 3.313(5) . ? C28 H28 1.0000 . ? C29 C30 1.461(7) . ? C29 Rb2 3.638(5) . ? C30 C31 1.375(9) . ? C30 H30 0.9500 . ? C31 C32 1.417(9) . ? C31 H31 0.9500 . ? C32 C33 1.411(9) . ? C33 C34 1.411(9) . ? C33 H33 0.9500 . ? C34 C35 1.445(8) . ? C34 H34 0.9500 . ? C35 C36 1.443(8) . ? C36 C37 1.427(7) . ? C36 H36 0.9500 . ? C37 C38 1.405(8) . ? C37 H37 0.9500 . ? C38 C39 1.484(6) . ? C39 C45 1.405(6) . ? C39 C40 1.438(7) . ? C40 C48 1.400(6) . ? C41 C42 1.399(6) . ? C41 H41 0.9500 . ? C42 C43 1.409(6) . ? C42 C49 1.487(6) . ? C43 C44 1.390(6) . ? C43 C55 1.496(6) . ? C44 H44 0.9500 . ? C45 C46 1.397(6) . ? C45 H45 0.9500 . ? C46 C47 1.401(7) . ? C46 C60 1.498(6) . ? C47 C48 1.391(6) . ? C47 C54 1.494(6) . ? C48 H48 0.9500 . ? C49 C50 1.390(6) . ? C49 C54 1.401(6) . ? C50 C51 1.377(7) . ? C50 H50 0.9500 . ? C51 C52 1.402(7) . ? C51 H51 0.9500 . ? C52 C53 1.359(7) . ? C52 H52 0.9500 . ? C53 C54 1.409(7) . ? C53 H53 0.9500 . ? C55 C56 1.396(6) . ? C55 C60 1.396(6) . ? C56 C57 1.387(6) . ? C56 H56 0.9500 . ? C57 C58 1.390(6) . ? C57 H57 0.9500 . ? C58 C59 1.377(6) . ? C58 H58 0.9500 . ? C59 C60 1.403(6) . ? C59 H59 0.9500 . ? C61 O1 1.425(5) . ? C61 C66 1.501(6) 2_655 ? C61 Rb1 3.621(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O1 1.428(5) . ? C62 C63 1.504(6) . ? C62 Rb1 3.603(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 O2 1.417(5) . ? C63 Rb1 3.641(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 O2 1.411(5) . ? C64 C65 1.505(6) . ? C64 Rb1 3.683(4) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 O3 1.432(5) . ? C65 Rb1 3.682(4) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 O3 1.435(5) . ? C66 C61 1.501(6) 2_655 ? C66 Rb1 3.643(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 O4 1.425(6) . ? C67 C72 1.511(6) 2_656 ? C67 Rb2 3.633(4) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 O4 1.430(5) . ? C68 C69 1.510(7) . ? C68 Rb2 3.675(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 O5 1.416(6) . ? C69 Rb2 3.666(5) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 O5 1.425(6) . ? C70 C71 1.500(7) . ? C70 Rb2 3.644(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 O6 1.431(5) . ? C71 Rb2 3.634(4) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 O6 1.417(6) . ? C72 C67 1.511(6) 2_656 ? C72 Rb2 3.597(4) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? Rb1 O2 2.828(3) . ? Rb1 O2 2.828(3) 2_655 ? Rb1 O1 2.839(3) . ? Rb1 O1 2.839(3) 2_655 ? Rb1 O3 2.892(3) 2_655 ? Rb1 O3 2.892(3) . ? Rb1 C8 3.307(4) 2_655 ? Rb1 C7 3.515(4) 2_655 ? Rb1 C9 3.602(4) 2_655 ? Rb2 O4 2.829(3) 2_656 ? Rb2 O4 2.829(3) . ? Rb2 O6 2.838(3) 2_656 ? Rb2 O6 2.838(3) . ? Rb2 O5 2.894(3) 2_656 ? Rb2 O5 2.894(3) . ? Rb2 C28 3.313(5) 2_656 ? Rb2 C27 3.529(5) 2_656 ? Rb2 C72 3.597(5) 2_656 ? Rb3 O10A 2.725(9) . ? Rb3 O9A 2.754(10) . ? Rb3 O13 2.782(6) . ? Rb3 O11 2.803(6) . ? Rb3 O12 2.813(6) . ? Rb3 O14A 2.813(9) . ? Rb3 O11A 2.817(9) . ? Rb3 O10 2.848(6) . ? Rb3 O14 2.855(6) . ? Rb3 O8 2.877(5) . ? Rb3 O9 2.896(7) . ? Rb3 O12A 2.904(9) . ? O7 C73 1.313(9) . ? O7 C74 1.462(11) . ? C73 C76 1.427(9) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.511(10) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.518(10) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? O8 C80 1.421(16) . ? O8 C77 1.427(8) . ? O8 C80A 1.55(3) . ? C77 C78 1.511(10) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.476(10) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80A 1.33(2) . ? C79 C80 1.567(18) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C80A H80C 0.9900 . ? C80A H80D 0.9900 . ? O9 C92 1.371(10) . ? O9 C81 1.431(11) . ? C81 C82 1.431(15) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 O10 1.378(11) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? O10 C83 1.336(12) . ? C83 C84 1.397(16) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 O11 1.367(11) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? O11 C85 1.342(13) . ? C85 C86 1.476(17) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 O12 1.383(10) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? O12 C87 1.426(11) . ? C87 C88 1.495(16) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 O13 1.346(11) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? O13 C89 1.382(12) . ? C89 C90 1.450(16) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 O14 1.334(12) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? O14 C91 1.383(12) . ? C91 C92 1.378(15) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? O9A C92A 1.365(13) . ? O9A C81A 1.376(13) . ? C81A C82A 1.354(17) . ? C81A H81C 0.9900 . ? C81A H81D 0.9900 . ? C82A O10A 1.390(14) . ? C82A H82C 0.9900 . ? C82A H82D 0.9900 . ? O10A C83A 1.331(14) . ? C83A C84A 1.378(19) . ? C83A H83C 0.9900 . ? C83A H83D 0.9900 . ? C84A O11A 1.382(14) . ? C84A H84C 0.9900 . ? C84A H84D 0.9900 . ? O11A C85A 1.364(14) . ? C85A C86A 1.461(19) . ? C85A H85C 0.9900 . ? C85A H85D 0.9900 . ? C86A O12A 1.412(15) . ? C86A H86C 0.9900 . ? C86A H86D 0.9900 . ? O12A C87A 1.401(12) . ? C87A C88A 1.427(18) . ? C87A H87C 0.9900 . ? C87A H87D 0.9900 . ? C88A O13A 1.323(14) . ? C88A H88C 0.9900 . ? C88A H88D 0.9900 . ? O13A C89A 1.393(13) . ? C89A C90A 1.406(19) . ? C89A H89C 0.9900 . ? C89A H89D 0.9900 . ? C90A O14A 1.339(15) . ? C90A H90C 0.9900 . ? C90A H90D 0.9900 . ? O14A C91A 1.390(14) . ? C91A C92A 1.360(17) . ? C91A H91C 0.9900 . ? C91A H91D 0.9900 . ? C92A H92C 0.9900 . ? C92A H92D 0.9900 . ? 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 C6 C1 C5 124.5(4) . . ? C6 C1 C2 122.6(4) . . ? C5 C1 C2 108.0(4) . . ? C9 C2 C3 123.7(4) . . ? C9 C2 C1 123.1(4) . . ? C3 C2 C1 108.1(4) . . ? C12 C3 C2 123.3(4) . . ? C12 C3 C4 123.1(4) . . ? C2 C3 C4 107.7(4) . . ? C15 C4 C5 123.6(4) . . ? C15 C4 C3 122.9(4) . . ? C5 C4 C3 108.4(4) . . ? C18 C5 C1 124.4(4) . . ? C18 C5 C4 122.3(4) . . ? C1 C5 C4 107.8(4) . . ? C1 C6 C7 115.5(4) . . ? C1 C6 C20 113.6(4) . . ? C7 C6 C20 130.0(4) . . ? C6 C7 C8 121.9(4) . . ? C6 C7 Rb1 97.0(2) . . ? C8 C7 Rb1 69.9(2) . . ? C6 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? Rb1 C7 H7 117.9 . . ? C9 C8 C7 121.0(4) . . ? C9 C8 Rb1 89.9(3) . . ? C7 C8 Rb1 86.1(3) . . ? C9 C8 H8 117.0 . . ? C7 C8 H8 117.0 . . ? Rb1 C8 H8 117.0 . . ? C2 C9 C8 115.2(4) . . ? C2 C9 C10 113.3(4) . . ? C8 C9 C10 130.7(4) . . ? C2 C9 Rb1 88.9(3) . . ? C8 C9 Rb1 66.6(2) . . ? C10 C9 Rb1 123.2(3) . . ? C11 C10 C9 122.1(4) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C10 C11 C12 123.1(4) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C3 C12 C13 114.4(5) . . ? C3 C12 C11 113.0(4) . . ? C13 C12 C11 131.0(5) . . ? C12 C13 C14 122.3(5) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C15 121.4(5) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C4 C15 C14 114.7(4) . . ? C4 C15 C16 114.5(4) . . ? C14 C15 C16 129.8(5) . . ? C17 C16 C15 120.6(4) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 123.1(4) . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C5 C18 C17 114.9(4) . . ? C5 C18 C19 112.7(4) . . ? C17 C18 C19 131.6(4) . . ? C44 C19 C20 117.4(4) . . ? C44 C19 C18 121.5(4) . . ? C20 C19 C18 121.1(4) . . ? C41 C20 C19 117.7(4) . . ? C41 C20 C6 121.4(4) . . ? C19 C20 C6 120.8(4) . . ? C26 C21 C25 124.5(4) . . ? C26 C21 C22 122.6(5) . . ? C25 C21 C22 108.0(4) . . ? C29 C22 C23 124.0(5) . . ? C29 C22 C21 122.9(5) . . ? C23 C22 C21 108.3(5) . . ? C22 C23 C24 107.9(4) . . ? C22 C23 C32 122.9(5) . . ? C24 C23 C32 123.4(6) . . ? C35 C24 C23 124.0(5) . . ? C35 C24 C25 123.0(5) . . ? C23 C24 C25 108.3(5) . . ? C38 C25 C21 124.6(4) . . ? C38 C25 C24 122.6(5) . . ? C21 C25 C24 107.5(5) . . ? C21 C26 C27 115.1(4) . . ? C21 C26 C40 113.0(4) . . ? C27 C26 C40 131.3(4) . . ? C26 C27 C28 122.4(5) . . ? C26 C27 Rb2 100.4(3) . . ? C28 C27 Rb2 69.6(3) . . ? C26 C27 H27 117.3 . . ? C28 C27 H27 117.3 . . ? Rb2 C27 H27 117.3 . . ? C29 C28 C27 120.6(5) . . ? C29 C28 Rb2 91.4(3) . . ? C27 C28 Rb2 86.6(3) . . ? C29 C28 H28 116.7 . . ? C27 C28 H28 116.7 . . ? Rb2 C28 H28 116.7 . . ? C22 C29 C28 115.6(4) . . ? C22 C29 C30 113.0(5) . . ? C28 C29 C30 130.5(5) . . ? C22 C29 Rb2 91.5(3) . . ? C28 C29 Rb2 65.6(3) . . ? C30 C29 Rb2 122.2(4) . . ? C31 C30 C29 121.8(5) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 123.9(5) . . ? C30 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C23 C32 C33 112.8(6) . . ? C23 C32 C31 113.0(6) . . ? C33 C32 C31 132.3(5) . . ? C34 C33 C32 123.3(5) . . ? C34 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C33 C34 C35 121.7(6) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C24 C35 C36 114.8(5) . . ? C24 C35 C34 113.6(6) . . ? C36 C35 C34 130.5(6) . . ? C37 C36 C35 121.3(6) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C38 C37 C36 122.1(5) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C25 C38 C37 115.2(5) . . ? C25 C38 C39 112.8(5) . . ? C37 C38 C39 131.4(5) . . ? C45 C39 C40 117.3(4) . . ? C45 C39 C38 121.9(4) . . ? C40 C39 C38 120.8(4) . . ? C48 C40 C39 118.0(4) . . ? C48 C40 C26 120.8(4) . . ? C39 C40 C26 121.2(4) . . ? C20 C41 C42 123.9(4) . . ? C20 C41 H41 118.0 . . ? C42 C41 H41 118.0 . . ? C41 C42 C43 118.4(4) . . ? C41 C42 C49 117.9(4) . . ? C43 C42 C49 123.3(4) . . ? C44 C43 C42 118.6(4) . . ? C44 C43 C55 119.4(4) . . ? C42 C43 C55 121.8(4) . . ? C43 C44 C19 123.8(4) . . ? C43 C44 H44 118.1 . . ? C19 C44 H44 118.1 . . ? C46 C45 C39 123.9(4) . . ? C46 C45 H45 118.0 . . ? C39 C45 H45 118.0 . . ? C45 C46 C47 118.0(4) . . ? C45 C46 C60 118.1(4) . . ? C47 C46 C60 123.6(4) . . ? C48 C47 C46 119.5(4) . . ? C48 C47 C54 118.0(4) . . ? C46 C47 C54 122.3(4) . . ? C47 C48 C40 123.2(4) . . ? C47 C48 H48 118.4 . . ? C40 C48 H48 118.4 . . ? C50 C49 C54 119.3(4) . . ? C50 C49 C42 118.6(4) . . ? C54 C49 C42 122.0(4) . . ? C51 C50 C49 121.9(4) . . ? C51 C50 H50 119.0 . . ? C49 C50 H50 119.0 . . ? C50 C51 C52 119.1(5) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? C53 C52 C51 119.4(5) . . ? C53 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? C52 C53 C54 122.4(4) . . ? C52 C53 H53 118.8 . . ? C54 C53 H53 118.8 . . ? C49 C54 C53 117.9(4) . . ? C49 C54 C47 122.7(4) . . ? C53 C54 C47 119.2(4) . . ? C56 C55 C60 119.0(4) . . ? C56 C55 C43 117.8(4) . . ? C60 C55 C43 123.1(4) . . ? C57 C56 C55 121.4(4) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C56 C57 C58 119.5(4) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C59 C58 C57 119.6(4) . . ? C59 C58 H58 120.2 . . ? C57 C58 H58 120.2 . . ? C58 C59 C60 121.5(4) . . ? C58 C59 H59 119.3 . . ? C60 C59 H59 119.3 . . ? C55 C60 C59 119.0(4) . . ? C55 C60 C46 122.8(4) . . ? C59 C60 C46 118.2(4) . . ? O1 C61 C66 109.8(3) . 2_655 ? O1 C61 Rb1 46.66(16) . . ? C66 C61 Rb1 78.9(2) 2_655 . ? O1 C61 H61A 109.7 . . ? C66 C61 H61A 109.7 2_655 . ? Rb1 C61 H61A 155.5 . . ? O1 C61 H61B 109.7 . . ? C66 C61 H61B 109.7 2_655 . ? Rb1 C61 H61B 89.2 . . ? H61A C61 H61B 108.2 . . ? O1 C62 C63 109.0(3) . . ? O1 C62 Rb1 47.40(17) . . ? C63 C62 Rb1 79.4(2) . . ? O1 C62 H62A 109.9 . . ? C63 C62 H62A 109.9 . . ? Rb1 C62 H62A 87.0 . . ? O1 C62 H62B 109.9 . . ? C63 C62 H62B 109.9 . . ? Rb1 C62 H62B 156.9 . . ? H62A C62 H62B 108.3 . . ? O2 C63 C62 109.4(3) . . ? O2 C63 Rb1 45.23(18) . . ? C62 C63 Rb1 76.6(2) . . ? O2 C63 H63A 109.8 . . ? C62 C63 H63A 109.8 . . ? Rb1 C63 H63A 93.5 . . ? O2 C63 H63B 109.8 . . ? C62 C63 H63B 109.8 . . ? Rb1 C63 H63B 152.6 . . ? H63A C63 H63B 108.2 . . ? O2 C64 C65 108.8(3) . . ? O2 C64 Rb1 43.34(17) . . ? C65 C64 Rb1 78.2(2) . . ? O2 C64 H64A 109.9 . . ? C65 C64 H64A 109.9 . . ? Rb1 C64 H64A 151.5 . . ? O2 C64 H64B 109.9 . . ? C65 C64 H64B 109.9 . . ? Rb1 C64 H64B 93.4 . . ? H64A C64 H64B 108.3 . . ? O3 C65 C64 108.9(4) . . ? O3 C65 Rb1 46.59(17) . . ? C64 C65 Rb1 78.3(2) . . ? O3 C65 H65A 109.9 . . ? C64 C65 H65A 109.9 . . ? Rb1 C65 H65A 155.6 . . ? O3 C65 H65B 109.9 . . ? C64 C65 H65B 109.9 . . ? Rb1 C65 H65B 89.3 . . ? H65A C65 H65B 108.3 . . ? O3 C66 C61 108.9(3) . 2_655 ? O3 C66 Rb1 48.18(18) . . ? C61 C66 Rb1 77.2(2) 2_655 . ? O3 C66 H66A 109.9 . . ? C61 C66 H66A 109.9 2_655 . ? Rb1 C66 H66A 88.4 . . ? O3 C66 H66B 109.9 . . ? C61 C66 H66B 109.9 2_655 . ? Rb1 C66 H66B 157.1 . . ? H66A C66 H66B 108.3 . . ? O4 C67 C72 107.9(4) . 2_656 ? O4 C67 Rb2 45.7(2) . . ? C72 C67 Rb2 76.6(2) 2_656 . ? O4 C67 H67A 110.1 . . ? C72 C67 H67A 110.1 2_656 . ? Rb2 C67 H67A 154.3 . . ? O4 C67 H67B 110.1 . . ? C72 C67 H67B 110.1 2_656 . ? Rb2 C67 H67B 91.3 . . ? H67A C67 H67B 108.4 . . ? O4 C68 C69 108.1(4) . . ? O4 C68 Rb2 44.12(19) . . ? C69 C68 Rb2 77.8(2) . . ? O4 C68 H68A 110.1 . . ? C69 C68 H68A 110.1 . . ? Rb2 C68 H68A 92.1 . . ? O4 C68 H68B 110.1 . . ? C69 C68 H68B 110.1 . . ? Rb2 C68 H68B 152.7 . . ? H68A C68 H68B 108.4 . . ? O5 C69 C68 108.8(4) . . ? O5 C69 Rb2 47.10(19) . . ? C68 C69 Rb2 78.5(3) . . ? O5 C69 H69A 109.9 . . ? C68 C69 H69A 109.9 . . ? Rb2 C69 H69A 88.3 . . ? O5 C69 H69B 109.9 . . ? C68 C69 H69B 109.9 . . ? Rb2 C69 H69B 156.3 . . ? H69A C69 H69B 108.3 . . ? O5 C70 C71 109.5(4) . . ? O5 C70 Rb2 48.1(2) . . ? C71 C70 Rb2 77.7(3) . . ? O5 C70 H70A 109.8 . . ? C71 C70 H70A 109.8 . . ? Rb2 C70 H70A 156.9 . . ? O5 C70 H70B 109.8 . . ? C71 C70 H70B 109.8 . . ? Rb2 C70 H70B 88.6 . . ? H70A C70 H70B 108.2 . . ? O6 C71 C70 109.1(4) . . ? O6 C71 Rb2 46.19(19) . . ? C70 C71 Rb2 78.5(2) . . ? O6 C71 H71A 109.9 . . ? C70 C71 H71A 109.9 . . ? Rb2 C71 H71A 155.1 . . ? O6 C71 H71B 109.9 . . ? C70 C71 H71B 109.9 . . ? Rb2 C71 H71B 89.6 . . ? H71A C71 H71B 108.3 . . ? O6 C72 C67 108.9(4) . 2_656 ? O6 C72 Rb2 47.5(2) . . ? C67 C72 Rb2 79.3(2) 2_656 . ? O6 C72 H72A 109.9 . . ? C67 C72 H72A 109.9 2_656 . ? Rb2 C72 H72A 87.0 . . ? O6 C72 H72B 109.9 . . ? C67 C72 H72B 109.9 2_656 . ? Rb2 C72 H72B 157.0 . . ? H72A C72 H72B 108.3 . . ? O2 Rb1 O2 180.0 . 2_655 ? O2 Rb1 O1 61.04(8) . . ? O2 Rb1 O1 118.96(8) 2_655 . ? O2 Rb1 O1 118.96(8) . 2_655 ? O2 Rb1 O1 61.04(8) 2_655 2_655 ? O1 Rb1 O1 180.0 . 2_655 ? O2 Rb1 O3 120.48(8) . 2_655 ? O2 Rb1 O3 59.52(8) 2_655 2_655 ? O1 Rb1 O3 61.28(8) . 2_655 ? O1 Rb1 O3 118.72(8) 2_655 2_655 ? O2 Rb1 O3 59.52(8) . . ? O2 Rb1 O3 120.48(8) 2_655 . ? O1 Rb1 O3 118.71(8) . . ? O1 Rb1 O3 61.28(8) 2_655 . ? O3 Rb1 O3 180.0 2_655 . ? O2 Rb1 C8 77.53(9) . 2_655 ? O2 Rb1 C8 102.47(9) 2_655 2_655 ? O1 Rb1 C8 76.97(9) . 2_655 ? O1 Rb1 C8 103.03(9) 2_655 2_655 ? O3 Rb1 C8 76.69(10) 2_655 2_655 ? O3 Rb1 C8 103.31(10) . 2_655 ? O2 Rb1 C8 102.47(9) . . ? O2 Rb1 C8 77.53(9) 2_655 . ? O1 Rb1 C8 103.03(9) . . ? O1 Rb1 C8 76.97(9) 2_655 . ? O3 Rb1 C8 103.31(10) 2_655 . ? O3 Rb1 C8 76.69(10) . . ? C8 Rb1 C8 180.0 2_655 . ? O2 Rb1 C7 79.15(9) . . ? O2 Rb1 C7 100.85(9) 2_655 . ? O1 Rb1 C7 86.84(9) . . ? O1 Rb1 C7 93.16(9) 2_655 . ? O3 Rb1 C7 110.99(9) 2_655 . ? O3 Rb1 C7 69.01(9) . . ? C8 Rb1 C7 155.99(10) 2_655 . ? C8 Rb1 C7 24.01(10) . . ? O2 Rb1 C7 100.85(9) . 2_655 ? O2 Rb1 C7 79.15(9) 2_655 2_655 ? O1 Rb1 C7 93.16(9) . 2_655 ? O1 Rb1 C7 86.84(9) 2_655 2_655 ? O3 Rb1 C7 69.01(9) 2_655 2_655 ? O3 Rb1 C7 110.99(9) . 2_655 ? C8 Rb1 C7 24.01(10) 2_655 2_655 ? C8 Rb1 C7 155.99(10) . 2_655 ? C7 Rb1 C7 180.0 . 2_655 ? O2 Rb1 C9 118.22(9) . . ? O2 Rb1 C9 61.78(9) 2_655 . ? O1 Rb1 C9 95.09(9) . . ? O1 Rb1 C9 84.91(9) 2_655 . ? O3 Rb1 C9 80.15(9) 2_655 . ? O3 Rb1 C9 99.85(9) . . ? C8 Rb1 C9 156.56(11) 2_655 . ? C8 Rb1 C9 23.44(11) . . ? C7 Rb1 C9 41.01(10) . . ? C7 Rb1 C9 138.99(10) 2_655 . ? O2 Rb1 C9 61.78(9) . 2_655 ? O2 Rb1 C9 118.22(9) 2_655 2_655 ? O1 Rb1 C9 84.91(9) . 2_655 ? O1 Rb1 C9 95.09(9) 2_655 2_655 ? O3 Rb1 C9 99.85(9) 2_655 2_655 ? O3 Rb1 C9 80.15(9) . 2_655 ? C8 Rb1 C9 23.44(11) 2_655 2_655 ? C8 Rb1 C9 156.56(11) . 2_655 ? C7 Rb1 C9 138.99(10) . 2_655 ? C7 Rb1 C9 41.02(10) 2_655 2_655 ? C9 Rb1 C9 180.0 . 2_655 ? O4 Rb2 O4 180.0 2_656 . ? O4 Rb2 O6 119.00(9) 2_656 2_656 ? O4 Rb2 O6 61.00(9) . 2_656 ? O4 Rb2 O6 61.00(9) 2_656 . ? O4 Rb2 O6 119.00(9) . . ? O6 Rb2 O6 180.0 2_656 . ? O4 Rb2 O5 59.84(9) 2_656 2_656 ? O4 Rb2 O5 120.16(9) . 2_656 ? O6 Rb2 O5 61.02(9) 2_656 2_656 ? O6 Rb2 O5 118.98(9) . 2_656 ? O4 Rb2 O5 120.16(9) 2_656 . ? O4 Rb2 O5 59.84(9) . . ? O6 Rb2 O5 118.98(9) 2_656 . ? O6 Rb2 O5 61.02(9) . . ? O5 Rb2 O5 180.0 2_656 . ? O4 Rb2 C28 77.83(10) 2_656 . ? O4 Rb2 C28 102.17(10) . . ? O6 Rb2 C28 101.36(11) 2_656 . ? O6 Rb2 C28 78.64(11) . . ? O5 Rb2 C28 102.22(12) 2_656 . ? O5 Rb2 C28 77.78(12) . . ? O4 Rb2 C28 102.17(10) 2_656 2_656 ? O4 Rb2 C28 77.83(10) . 2_656 ? O6 Rb2 C28 78.64(11) 2_656 2_656 ? O6 Rb2 C28 101.36(11) . 2_656 ? O5 Rb2 C28 77.78(12) 2_656 2_656 ? O5 Rb2 C28 102.22(12) . 2_656 ? C28 Rb2 C28 180.0 . 2_656 ? O4 Rb2 C27 78.85(10) 2_656 2_656 ? O4 Rb2 C27 101.15(10) . 2_656 ? O6 Rb2 C27 94.22(10) 2_656 2_656 ? O6 Rb2 C27 85.78(10) . 2_656 ? O5 Rb2 C27 69.76(11) 2_656 2_656 ? O5 Rb2 C27 110.24(11) . 2_656 ? C28 Rb2 C27 156.15(11) . 2_656 ? C28 Rb2 C27 23.85(11) 2_656 2_656 ? O4 Rb2 C27 101.15(10) 2_656 . ? O4 Rb2 C27 78.84(10) . . ? O6 Rb2 C27 85.78(10) 2_656 . ? O6 Rb2 C27 94.22(10) . . ? O5 Rb2 C27 110.24(11) 2_656 . ? O5 Rb2 C27 69.76(11) . . ? C28 Rb2 C27 23.85(11) . . ? C28 Rb2 C27 156.15(11) 2_656 . ? C27 Rb2 C27 180.0 2_656 . ? O4 Rb2 C72 138.77(10) 2_656 2_656 ? O4 Rb2 C72 41.23(10) . 2_656 ? O6 Rb2 C72 21.59(11) 2_656 2_656 ? O6 Rb2 C72 158.41(11) . 2_656 ? O5 Rb2 C72 79.03(10) 2_656 2_656 ? O5 Rb2 C72 100.97(10) . 2_656 ? C28 Rb2 C72 110.74(12) . 2_656 ? C28 Rb2 C72 69.26(12) 2_656 2_656 ? C27 Rb2 C72 90.22(11) 2_656 2_656 ? C27 Rb2 C72 89.77(11) . 2_656 ? O4 Rb2 C72 41.22(10) 2_656 . ? O4 Rb2 C72 138.78(10) . . ? O6 Rb2 C72 158.41(11) 2_656 . ? O6 Rb2 C72 21.59(11) . . ? O5 Rb2 C72 100.97(10) 2_656 . ? O5 Rb2 C72 79.03(10) . . ? C28 Rb2 C72 69.26(12) . . ? C28 Rb2 C72 110.74(12) 2_656 . ? C27 Rb2 C72 89.77(11) 2_656 . ? C27 Rb2 C72 90.23(11) . . ? C72 Rb2 C72 180.0 2_656 . ? C61 O1 C62 111.7(3) . . ? C61 O1 Rb1 111.9(2) . . ? C62 O1 Rb1 110.9(2) . . ? C64 O2 C63 113.7(3) . . ? C64 O2 Rb1 116.6(2) . . ? C63 O2 Rb1 113.9(2) . . ? C65 O3 C66 112.4(3) . . ? C65 O3 Rb1 112.3(2) . . ? C66 O3 Rb1 110.1(2) . . ? C67 O4 C68 112.9(3) . . ? C67 O4 Rb2 113.1(3) . . ? C68 O4 Rb2 115.3(2) . . ? C69 O5 C70 112.8(4) . . ? C69 O5 Rb2 111.9(2) . . ? C70 O5 Rb2 110.4(2) . . ? C72 O6 C71 112.0(3) . . ? C72 O6 Rb2 110.9(3) . . ? C71 O6 Rb2 112.5(3) . . ? O10A Rb3 O9A 63.4(3) . . ? O13 Rb3 O11 119.6(2) . . ? O13 Rb3 O12 60.44(17) . . ? O11 Rb3 O12 60.02(18) . . ? O10A Rb3 O14A 125.0(3) . . ? O9A Rb3 O14A 62.4(3) . . ? O10A Rb3 O11A 61.2(3) . . ? O9A Rb3 O11A 123.1(3) . . ? O14A Rb3 O11A 173.1(3) . . ? O13 Rb3 O10 173.1(3) . . ? O11 Rb3 O10 59.8(2) . . ? O12 Rb3 O10 119.76(18) . . ? O13 Rb3 O14 59.50(18) . . ? O11 Rb3 O14 173.8(3) . . ? O12 Rb3 O14 119.84(16) . . ? O10 Rb3 O14 120.2(2) . . ? O10A Rb3 O8 85.4(4) . . ? O9A Rb3 O8 78.8(4) . . ? O13 Rb3 O8 100.2(2) . . ? O11 Rb3 O8 96.9(2) . . ? O12 Rb3 O8 98.0(2) . . ? O14A Rb3 O8 92.7(3) . . ? O11A Rb3 O8 84.7(3) . . ? O10 Rb3 O8 86.6(2) . . ? O14 Rb3 O8 89.2(2) . . ? O13 Rb3 O9 118.85(18) . . ? O11 Rb3 O9 119.30(19) . . ? O12 Rb3 O9 174.3(3) . . ? O10 Rb3 O9 60.16(18) . . ? O14 Rb3 O9 60.12(17) . . ? O8 Rb3 O9 87.7(2) . . ? O10A Rb3 O12A 118.8(3) . . ? O9A Rb3 O12A 177.4(3) . . ? O14A Rb3 O12A 115.6(3) . . ? O11A Rb3 O12A 58.8(2) . . ? O8 Rb3 O12A 99.9(3) . . ? C73 O7 C74 113.4(7) . . ? C73 O7 Rb3 60.3(5) . . ? C74 O7 Rb3 94.5(5) . . ? O7 C73 C76 106.9(7) . . ? O7 C73 Rb3 97.6(5) . . ? C76 C73 Rb3 101.1(5) . . ? O7 C73 H73A 110.3 . . ? C76 C73 H73A 110.3 . . ? Rb3 C73 H73A 20.0 . . ? O7 C73 H73B 110.3 . . ? C76 C73 H73B 110.3 . . ? Rb3 C73 H73B 128.4 . . ? H73A C73 H73B 108.6 . . ? O7 C74 C75 103.0(6) . . ? O7 C74 H74A 111.2 . . ? C75 C74 H74A 111.2 . . ? O7 C74 H74B 111.2 . . ? C75 C74 H74B 111.2 . . ? H74A C74 H74B 109.1 . . ? C74 C75 C76 102.9(6) . . ? C74 C75 H75A 111.2 . . ? C76 C75 H75A 111.2 . . ? C74 C75 H75B 111.2 . . ? C76 C75 H75B 111.2 . . ? H75A C75 H75B 109.1 . . ? C73 C76 C75 105.4(6) . . ? C73 C76 Rb3 55.9(4) . . ? C75 C76 Rb3 84.1(4) . . ? C73 C76 H76A 110.7 . . ? C75 C76 H76A 110.7 . . ? Rb3 C76 H76A 71.2 . . ? C73 C76 H76B 110.7 . . ? C75 C76 H76B 110.7 . . ? Rb3 C76 H76B 163.3 . . ? H76A C76 H76B 108.8 . . ? C80 O8 C77 111.2(8) . . ? C77 O8 C80A 101.1(12) . . ? C80 O8 Rb3 113.1(7) . . ? C77 O8 Rb3 126.7(5) . . ? C80A O8 Rb3 98.9(11) . . ? O8 C77 C78 106.0(6) . . ? O8 C77 H77A 110.5 . . ? C78 C77 H77A 110.5 . . ? O8 C77 H77B 110.5 . . ? C78 C77 H77B 110.5 . . ? H77A C77 H77B 108.7 . . ? C79 C78 C77 103.6(6) . . ? C79 C78 H78A 111.0 . . ? C77 C78 H78A 111.0 . . ? C79 C78 H78B 111.0 . . ? C77 C78 H78B 111.0 . . ? H78A C78 H78B 109.0 . . ? C80A C79 C78 110.3(14) . . ? C78 C79 C80 101.7(8) . . ? C78 C79 H79A 111.4 . . ? C80 C79 H79A 111.4 . . ? C78 C79 H79B 111.4 . . ? C80 C79 H79B 111.4 . . ? H79A C79 H79B 109.3 . . ? O8 C80 C79 102.0(12) . . ? O8 C80 Rb3 46.1(6) . . ? C79 C80 Rb3 123.5(12) . . ? O8 C80 H80A 111.4 . . ? C79 C80 H80A 111.4 . . ? Rb3 C80 H80A 122.9 . . ? O8 C80 H80B 111.4 . . ? C79 C80 H80B 111.4 . . ? Rb3 C80 H80B 65.6 . . ? H80A C80 H80B 109.2 . . ? C79 C80A O8 107(2) . . ? C79 C80A Rb3 156.5(16) . . ? O8 C80A Rb3 54.9(8) . . ? C79 C80A H80C 110.3 . . ? O8 C80A H80C 110.3 . . ? Rb3 C80A H80C 68.9 . . ? C79 C80A H80D 110.3 . . ? O8 C80A H80D 110.3 . . ? Rb3 C80A H80D 91.5 . . ? H80C C80A H80D 108.6 . . ? C92 O9 C81 122.8(9) . . ? C92 O9 Rb3 112.5(6) . . ? C81 O9 Rb3 109.4(6) . . ? C82 C81 O9 111.8(8) . . ? C82 C81 Rb3 79.4(6) . . ? O9 C81 Rb3 48.8(4) . . ? C82 C81 H81A 109.3 . . ? O9 C81 H81A 109.3 . . ? Rb3 C81 H81A 87.8 . . ? C82 C81 H81B 109.3 . . ? O9 C81 H81B 109.3 . . ? Rb3 C81 H81B 157.3 . . ? H81A C81 H81B 107.9 . . ? O10 C82 C81 114.3(9) . . ? O10 C82 Rb3 45.0(4) . . ? C81 C82 Rb3 77.9(6) . . ? O10 C82 H82A 108.7 . . ? C81 C82 H82A 108.7 . . ? Rb3 C82 H82A 149.1 . . ? O10 C82 H82B 108.7 . . ? C81 C82 H82B 108.7 . . ? Rb3 C82 H82B 98.1 . . ? H82A C82 H82B 107.6 . . ? C83 O10 C82 123.9(8) . . ? C83 O10 Rb3 114.6(6) . . ? C82 O10 Rb3 115.1(5) . . ? O10 C83 C84 118.7(10) . . ? O10 C83 Rb3 45.7(4) . . ? C84 C83 Rb3 78.8(6) . . ? O10 C83 H83A 107.7 . . ? C84 C83 H83A 107.7 . . ? Rb3 C83 H83A 101.9 . . ? O10 C83 H83B 107.7 . . ? C84 C83 H83B 107.7 . . ? Rb3 C83 H83B 146.3 . . ? H83A C83 H83B 107.1 . . ? O11 C84 C83 116.5(10) . . ? O11 C84 Rb3 44.3(4) . . ? C83 C84 Rb3 78.9(6) . . ? O11 C84 H84A 108.2 . . ? C83 C84 H84A 108.2 . . ? Rb3 C84 H84A 100.9 . . ? O11 C84 H84B 108.2 . . ? C83 C84 H84B 108.2 . . ? Rb3 C84 H84B 146.5 . . ? H84A C84 H84B 107.3 . . ? C85 O11 C84 120.9(8) . . ? C85 O11 Rb3 115.1(7) . . ? C84 O11 Rb3 115.8(6) . . ? O11 C85 C86 117.9(12) . . ? O11 C85 Rb3 45.0(5) . . ? C86 C85 Rb3 81.8(6) . . ? O11 C85 H85A 107.8 . . ? C86 C85 H85A 107.8 . . ? Rb3 C85 H85A 149.4 . . ? O11 C85 H85B 107.8 . . ? C86 C85 H85B 107.8 . . ? Rb3 C85 H85B 96.8 . . ? H85A C85 H85B 107.2 . . ? O12 C86 C85 111.4(10) . . ? O12 C86 Rb3 42.3(4) . . ? C85 C86 Rb3 74.8(6) . . ? O12 C86 H86A 109.3 . . ? C85 C86 H86A 109.3 . . ? Rb3 C86 H86A 144.1 . . ? O12 C86 H86B 109.3 . . ? C85 C86 H86B 109.3 . . ? Rb3 C86 H86B 103.6 . . ? H86A C86 H86B 108.0 . . ? C86 O12 C87 114.9(8) . . ? C86 O12 Rb3 118.4(5) . . ? C87 O12 Rb3 116.7(5) . . ? O12 C87 C88 110.2(8) . . ? O12 C87 Rb3 43.1(4) . . ? C88 C87 Rb3 75.4(5) . . ? O12 C87 H87A 109.6 . . ? C88 C87 H87A 109.6 . . ? Rb3 C87 H87A 99.3 . . ? O12 C87 H87B 109.6 . . ? C88 C87 H87B 109.6 . . ? Rb3 C87 H87B 147.7 . . ? H87A C87 H87B 108.1 . . ? O13 C88 C87 116.9(9) . . ? O13 C88 Rb3 43.2(4) . . ? C87 C88 Rb3 81.0(5) . . ? O13 C88 H88A 108.1 . . ? C87 C88 H88A 108.1 . . ? Rb3 C88 H88A 99.7 . . ? O13 C88 H88B 108.1 . . ? C87 C88 H88B 108.1 . . ? Rb3 C88 H88B 146.6 . . ? H88A C88 H88B 107.3 . . ? C88 O13 C89 120.1(7) . . ? C88 O13 Rb3 117.4(6) . . ? C89 O13 Rb3 117.8(6) . . ? O13 C89 C90 113.5(10) . . ? O13 C89 Rb3 42.6(4) . . ? C90 C89 Rb3 77.3(6) . . ? O13 C89 H89A 108.9 . . ? C90 C89 H89A 108.9 . . ? Rb3 C89 H89A 145.2 . . ? O13 C89 H89B 108.9 . . ? C90 C89 H89B 108.9 . . ? Rb3 C89 H89B 102.0 . . ? H89A C89 H89B 107.7 . . ? O14 C90 C89 115.1(11) . . ? O14 C90 Rb3 46.3(4) . . ? C89 C90 Rb3 79.6(6) . . ? O14 C90 H90A 108.5 . . ? C89 C90 H90A 108.5 . . ? Rb3 C90 H90A 152.0 . . ? O14 C90 H90B 108.5 . . ? C89 C90 H90B 108.5 . . ? Rb3 C90 H90B 94.4 . . ? H90A C90 H90B 107.5 . . ? C90 O14 C91 121.1(9) . . ? C90 O14 Rb3 113.9(6) . . ? C91 O14 Rb3 114.2(5) . . ? C92 C91 O14 119.5(10) . . ? C92 C91 Rb3 79.2(6) . . ? O14 C91 Rb3 45.6(4) . . ? C92 C91 H91A 107.5 . . ? O14 C91 H91A 107.5 . . ? Rb3 C91 H91A 145.2 . . ? C92 C91 H91B 107.5 . . ? O14 C91 H91B 107.5 . . ? Rb3 C91 H91B 103.1 . . ? H91A C91 H91B 107.0 . . ? O9 C92 C91 117.5(10) . . ? O9 C92 Rb3 47.2(4) . . ? C91 C92 Rb3 79.0(6) . . ? O9 C92 H92A 107.9 . . ? C91 C92 H92A 107.9 . . ? Rb3 C92 H92A 97.1 . . ? O9 C92 H92B 107.9 . . ? C91 C92 H92B 107.9 . . ? Rb3 C92 H92B 150.6 . . ? H92A C92 H92B 107.2 . . ? C92A O9A C81A 127.5(13) . . ? C92A O9A Rb3 115.4(7) . . ? C81A O9A Rb3 112.0(7) . . ? C82A C81A O9A 124.4(11) . . ? C82A C81A Rb3 78.5(7) . . ? O9A C81A Rb3 46.7(5) . . ? C82A C81A H81C 106.2 . . ? O9A C81A H81C 106.2 . . ? Rb3 C81A H81C 133.5 . . ? C82A C81A H81D 106.2 . . ? O9A C81A H81D 106.2 . . ? Rb3 C81A H81D 116.7 . . ? H81C C81A H81D 106.4 . . ? C81A C82A O10A 122.3(13) . . ? C81A C82A Rb3 79.2(8) . . ? O10A C82A Rb3 45.9(5) . . ? C81A C82A H82C 106.7 . . ? O10A C82A H82C 106.7 . . ? Rb3 C82A H82C 108.9 . . ? C81A C82A H82D 106.7 . . ? O10A C82A H82D 106.7 . . ? Rb3 C82A H82D 140.4 . . ? H82C C82A H82D 106.6 . . ? C83A O10A C82A 130.6(10) . . ? C83A O10A Rb3 116.2(8) . . ? C82A O10A Rb3 112.6(7) . . ? O10A C83A C84A 120.3(14) . . ? O10A C83A Rb3 43.9(6) . . ? C84A C83A Rb3 82.1(8) . . ? O10A C83A H83C 107.3 . . ? C84A C83A H83C 107.3 . . ? Rb3 C83A H83C 145.0 . . ? O10A C83A H83D 107.3 . . ? C84A C83A H83D 107.3 . . ? Rb3 C83A H83D 102.0 . . ? H83C C83A H83D 106.9 . . ? C83A C84A O11A 117.8(13) . . ? C83A C84A Rb3 75.7(8) . . ? O11A C84A Rb3 45.8(6) . . ? C83A C84A H84C 107.8 . . ? O11A C84A H84C 107.8 . . ? Rb3 C84A H84C 107.2 . . ? C83A C84A H84D 107.8 . . ? O11A C84A H84D 107.8 . . ? Rb3 C84A H84D 142.2 . . ? H84C C84A H84D 107.2 . . ? C85A O11A C84A 118.9(11) . . ? C85A O11A Rb3 118.4(7) . . ? C84A O11A Rb3 113.6(8) . . ? O11A C85A C86A 117.0(13) . . ? O11A C85A Rb3 42.5(5) . . ? C86A C85A Rb3 82.5(7) . . ? O11A C85A H85C 108.0 . . ? C86A C85A H85C 108.0 . . ? Rb3 C85A H85C 98.6 . . ? O11A C85A H85D 108.0 . . ? C86A C85A H85D 108.0 . . ? Rb3 C85A H85D 146.8 . . ? H85C C85A H85D 107.3 . . ? O12A C86A C85A 112.2(14) . . ? O12A C86A H86C 109.2 . . ? C85A C86A H86C 109.2 . . ? O12A C86A H86D 109.2 . . ? C85A C86A H86D 109.2 . . ? H86C C86A H86D 107.9 . . ? C87A O12A C86A 113.5(12) . . ? C87A O12A Rb3 120.1(7) . . ? C86A O12A Rb3 117.2(8) . . ? O12A C87A C88A 115.8(11) . . ? O12A C87A H87C 108.3 . . ? C88A C87A H87C 108.3 . . ? O12A C87A H87D 108.3 . . ? C88A C87A H87D 108.3 . . ? H87C C87A H87D 107.4 . . ? O13A C88A C87A 124.1(11) . . ? O13A C88A Rb3 42.9(5) . . ? C87A C88A Rb3 81.6(7) . . ? O13A C88A H88C 106.3 . . ? C87A C88A H88C 106.3 . . ? Rb3 C88A H88C 130.4 . . ? O13A C88A H88D 106.3 . . ? C87A C88A H88D 106.3 . . ? Rb3 C88A H88D 118.3 . . ? H88C C88A H88D 106.4 . . ? C88A O13A C89A 122.4(10) . . ? C88A O13A Rb3 119.1(7) . . ? C89A O13A Rb3 114.6(7) . . ? O13A C89A C90A 113.9(13) . . ? O13A C89A Rb3 45.5(5) . . ? C90A C89A Rb3 76.0(8) . . ? O13A C89A H89C 108.8 . . ? C90A C89A H89C 108.8 . . ? Rb3 C89A H89C 99.9 . . ? O13A C89A H89D 108.8 . . ? C90A C89A H89D 108.8 . . ? Rb3 C89A H89D 148.1 . . ? H89C C89A H89D 107.7 . . ? O14A C90A C89A 118.1(15) . . ? O14A C90A Rb3 42.8(6) . . ? C89A C90A Rb3 82.0(8) . . ? O14A C90A H90C 107.8 . . ? C89A C90A H90C 107.8 . . ? Rb3 C90A H90C 100.5 . . ? O14A C90A H90D 107.8 . . ? C89A C90A H90D 107.8 . . ? Rb3 C90A H90D 145.7 . . ? H90C C90A H90D 107.1 . . ? C90A O14A C91A 119.2(12) . . ? C90A O14A Rb3 118.3(8) . . ? C91A O14A Rb3 112.2(7) . . ? C92A C91A O14A 121.1(14) . . ? C92A C91A Rb3 78.3(8) . . ? O14A C91A Rb3 46.7(5) . . ? C92A C91A H91C 107.0 . . ? O14A C91A H91C 107.0 . . ? Rb3 C91A H91C 106.0 . . ? C92A C91A H91D 107.0 . . ? O14A C91A H91D 107.0 . . ? Rb3 C91A H91D 143.3 . . ? H91C C91A H91D 106.8 . . ? C91A C92A O9A 123.3(11) . . ? C91A C92A Rb3 79.7(8) . . ? O9A C92A Rb3 44.3(6) . . ? C91A C92A H92C 106.5 . . ? O9A C92A H92C 106.5 . . ? Rb3 C92A H92C 116.7 . . ? C91A C92A H92D 106.5 . . ? O9A C92A H92D 106.5 . . ? Rb3 C92A H92D 132.6 . . ? H92C C92A H92D 106.5 . . ? _refine_diff_density_max 1.531 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.084 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.015 0.500 0.500 575 132 ' ' _platon_squeeze_details ? _shelxl_version_number 2013-4 _shelx_res_file ; TITL sad in P-1 CELL 1.54178 9.3921 16.1731 28.6015 80.358 89.767 80.008 ZERR 2.00 0.0002 0.0003 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H Rb O UNIT 196 208 4 31 L.S. 20 BOND $H FMAP 2 PLAN -20 OMIT 2 2 0 OMIT 1 0 0 OMIT 2 2 2 OMIT 0 3 10 EXYZ O7 C73A EXYZ C73 O7A EADP O7 C73A EADP C73 O7A BOND Rb3 O7 BOND Rb3 O7A simu delu ACTA TEMP -173.000 SIZE 0.18 0.04 0.02 WGHT 0.117900 FVAR 0.97001 0.61758 0.61251 0.42485 C1 1 0.186235 0.161693 0.049808 11.00000 0.04281 0.03949 = 0.02856 -0.01362 0.00603 -0.01430 C2 1 0.263104 0.211013 0.016095 11.00000 0.04906 0.03709 = 0.02254 -0.00905 0.00489 -0.01122 C3 1 0.162813 0.276527 -0.010124 11.00000 0.05217 0.04568 = 0.02605 -0.01334 0.00734 -0.01567 C4 1 0.024470 0.269602 0.008171 11.00000 0.04792 0.04836 = 0.02556 -0.01284 -0.00281 -0.01624 C5 1 0.039143 0.198027 0.044712 11.00000 0.04181 0.04171 = 0.02552 -0.01299 -0.00119 -0.01455 C6 1 0.250866 0.112378 0.090903 11.00000 0.03867 0.04095 = 0.02504 -0.01206 0.00176 -0.01215 C7 1 0.402787 0.107996 0.095394 11.00000 0.03780 0.04609 = 0.03132 -0.01011 0.00421 -0.00977 AFIX 13 H7 2 0.450499 0.083287 0.127045 11.00000 -1.20000 AFIX 0 C8 1 0.480801 0.157375 0.061458 11.00000 0.03580 0.05146 = 0.03547 -0.01016 0.00906 -0.01389 AFIX 13 H8 2 0.574345 0.169864 0.072616 11.00000 -1.20000 AFIX 0 C9 1 0.407337 0.215428 0.022081 11.00000 0.04761 0.04279 = 0.02955 -0.01222 0.01196 -0.01601 C10 1 0.451449 0.288058 -0.008316 11.00000 0.05062 0.05196 = 0.03828 -0.01180 0.01188 -0.01769 AFIX 43 H10 2 0.551564 0.290456 -0.010968 11.00000 -1.20000 AFIX 0 C11 1 0.352957 0.352922 -0.033158 11.00000 0.06757 0.04824 = 0.03265 -0.00786 0.01021 -0.02477 AFIX 43 H11 2 0.387575 0.399786 -0.051330 11.00000 -1.20000 AFIX 0 C12 1 0.198735 0.353349 -0.032998 11.00000 0.06774 0.04518 = 0.02731 -0.00953 0.00245 -0.01538 C13 1 0.080183 0.421540 -0.042109 11.00000 0.07491 0.04625 = 0.04213 -0.00650 0.00394 -0.01348 AFIX 43 H13 2 0.094660 0.473817 -0.060598 11.00000 -1.20000 AFIX 0 C14 1 -0.059642 0.414498 -0.024565 11.00000 0.07080 0.04742 = 0.04270 -0.00649 -0.00407 -0.00756 AFIX 43 H14 2 -0.136859 0.461189 -0.032653 11.00000 -1.20000 AFIX 0 C15 1 -0.086836 0.338181 0.005189 11.00000 0.04825 0.05379 = 0.03410 -0.01468 -0.00893 -0.00897 C16 1 -0.200413 0.326285 0.038555 11.00000 0.04199 0.05685 = 0.04360 -0.01247 -0.00869 -0.00466 AFIX 43 H16 2 -0.287594 0.366777 0.035677 11.00000 -1.20000 AFIX 0 C17 1 -0.183096 0.255039 0.075412 11.00000 0.04018 0.05938 = 0.03580 -0.01878 0.00004 -0.01472 AFIX 43 H17 2 -0.257940 0.250654 0.097657 11.00000 -1.20000 AFIX 0 C18 1 -0.060594 0.190397 0.080749 11.00000 0.03865 0.04305 = 0.02921 -0.01110 -0.00094 -0.01413 C19 1 -0.005664 0.122306 0.121268 11.00000 0.03740 0.05063 = 0.02187 -0.01264 -0.00143 -0.01459 C20 1 0.146387 0.085083 0.126522 11.00000 0.03478 0.04571 = 0.02254 -0.01355 0.00157 -0.01191 C21 1 0.175085 0.163446 0.418091 11.00000 0.06183 0.05521 = 0.02359 -0.00579 0.00797 -0.03002 C22 1 0.249927 0.213145 0.442954 11.00000 0.07926 0.05693 = 0.02381 -0.00708 0.00760 -0.03309 C23 1 0.148459 0.278492 0.456504 11.00000 0.08630 0.06913 = 0.02850 -0.01875 0.01912 -0.04490 C24 1 0.011989 0.272158 0.438981 11.00000 0.07504 0.06657 = 0.03801 -0.02286 0.02845 -0.03533 C25 1 0.028338 0.199616 0.415540 11.00000 0.07332 0.05703 = 0.02651 -0.01473 0.02064 -0.04110 C26 1 0.242342 0.114214 0.386718 11.00000 0.06348 0.05017 = 0.02008 -0.00463 0.00092 -0.02885 C27 1 0.394567 0.109129 0.384625 11.00000 0.05895 0.05815 = 0.03067 -0.00900 -0.00002 -0.02518 AFIX 13 H27 2 0.444001 0.085534 0.357455 11.00000 -1.20000 AFIX 0 C28 1 0.470358 0.159107 0.409107 11.00000 0.06301 0.06677 = 0.03933 -0.01082 -0.00278 -0.03119 AFIX 13 H28 2 0.562554 0.173296 0.395017 11.00000 -1.20000 AFIX 0 C29 1 0.394254 0.216976 0.436995 11.00000 0.07047 0.06430 = 0.03142 -0.00393 -0.00414 -0.03358 C30 1 0.436772 0.289768 0.453873 11.00000 0.07962 0.07117 = 0.04249 -0.01577 0.00088 -0.04158 AFIX 43 H30 2 0.536610 0.292588 0.456281 11.00000 -1.20000 AFIX 0 C31 1 0.336143 0.354324 0.466370 11.00000 0.08960 0.07386 = 0.04062 -0.01667 0.00767 -0.04623 AFIX 43 H31 2 0.369977 0.401005 0.476088 11.00000 -1.20000 AFIX 0 C32 1 0.185011 0.355369 0.465617 11.00000 0.09204 0.06981 = 0.03866 -0.02485 0.02213 -0.03930 C33 1 0.065082 0.422373 0.461473 11.00000 0.09464 0.07691 = 0.05631 -0.03704 0.03211 -0.04511 AFIX 43 H33 2 0.077855 0.474623 0.470449 11.00000 -1.20000 AFIX 0 C34 1 -0.072811 0.415715 0.444681 11.00000 0.08714 0.07292 = 0.06912 -0.03614 0.03278 -0.02717 AFIX 43 H34 2 -0.149754 0.462713 0.443576 11.00000 -1.20000 AFIX 0 C35 1 -0.099998 0.339266 0.429127 11.00000 0.07706 0.07273 = 0.05120 -0.03160 0.03589 -0.03652 C36 1 -0.211566 0.326755 0.397840 11.00000 0.06410 0.06402 = 0.06299 -0.02169 0.02884 -0.02029 AFIX 43 H36 2 -0.299336 0.366750 0.393299 11.00000 -1.20000 AFIX 0 C37 1 -0.192735 0.255518 0.373577 11.00000 0.05762 0.06625 = 0.04758 -0.02121 0.02268 -0.02732 AFIX 43 H37 2 -0.266415 0.251019 0.351959 11.00000 -1.20000 AFIX 0 C38 1 -0.068774 0.191827 0.380625 11.00000 0.05612 0.05857 = 0.03337 -0.01451 0.01798 -0.02778 C39 1 -0.011967 0.123474 0.353252 11.00000 0.05185 0.05078 = 0.02421 -0.00854 0.01170 -0.02545 C40 1 0.138610 0.085429 0.356555 11.00000 0.05405 0.05025 = 0.02042 -0.00329 0.00439 -0.02404 C41 1 0.189149 0.020363 0.164841 11.00000 0.03162 0.04851 = 0.02495 -0.01431 0.00039 -0.01065 AFIX 43 H41 2 0.289017 -0.003573 0.168747 11.00000 -1.20000 AFIX 0 C42 1 0.093895 -0.011645 0.198008 11.00000 0.03952 0.04867 = 0.02013 -0.01297 0.00355 -0.01577 C43 1 -0.053760 0.025356 0.193356 11.00000 0.03857 0.04989 = 0.02435 -0.01314 0.00552 -0.02060 C44 1 -0.098545 0.091331 0.155802 11.00000 0.03541 0.05191 = 0.02905 -0.01503 0.00418 -0.01487 AFIX 43 H44 2 -0.197828 0.116910 0.153399 11.00000 -1.20000 AFIX 0 C45 1 -0.102452 0.091866 0.324155 11.00000 0.04401 0.05541 = 0.03078 -0.01100 0.01355 -0.02417 AFIX 43 H45 2 -0.201905 0.117058 0.321381 11.00000 -1.20000 AFIX 0 C46 1 -0.054875 0.025628 0.299075 11.00000 0.04310 0.05569 = 0.02070 -0.00796 0.01089 -0.02076 C47 1 0.092174 -0.010781 0.302710 11.00000 0.04851 0.04980 = 0.02192 -0.00701 0.00850 -0.02412 C48 1 0.185216 0.020572 0.330253 11.00000 0.04339 0.05304 = 0.02066 -0.00412 0.00472 -0.01988 AFIX 43 H48 2 0.285259 -0.003178 0.331267 11.00000 -1.20000 AFIX 0 C49 1 0.151420 -0.088903 0.233097 11.00000 0.04033 0.04542 = 0.02863 -0.00883 0.00376 -0.01938 C50 1 0.216977 -0.161876 0.216475 11.00000 0.05461 0.04952 = 0.03254 -0.00995 0.00459 -0.01532 AFIX 43 H50 2 0.217199 -0.162057 0.183277 11.00000 -1.20000 AFIX 0 C51 1 0.281597 -0.233898 0.246718 11.00000 0.06908 0.04778 = 0.05049 -0.01397 0.01103 -0.00975 AFIX 43 H51 2 0.323880 -0.283481 0.234594 11.00000 -1.20000 AFIX 0 C52 1 0.284190 -0.233113 0.295639 11.00000 0.07505 0.04888 = 0.04012 0.00119 -0.00133 -0.01046 AFIX 43 H52 2 0.330010 -0.281844 0.316992 11.00000 -1.20000 AFIX 0 C53 1 0.220571 -0.162018 0.312256 11.00000 0.05802 0.05038 = 0.02995 -0.00244 -0.00074 -0.01902 AFIX 43 H53 2 0.223042 -0.162059 0.345462 11.00000 -1.20000 AFIX 0 C54 1 0.151092 -0.088265 0.282032 11.00000 0.04437 0.04824 = 0.02735 -0.00659 0.00123 -0.01790 C55 1 -0.164285 -0.009124 0.225146 11.00000 0.03740 0.05114 = 0.02813 -0.01074 0.00633 -0.01423 C56 1 -0.275432 -0.038617 0.204215 11.00000 0.04408 0.05477 = 0.03096 -0.01551 0.00466 -0.01758 AFIX 43 H56 2 -0.276292 -0.037788 0.170926 11.00000 -1.20000 AFIX 0 C57 1 -0.384593 -0.069094 0.230981 11.00000 0.04176 0.06681 = 0.03651 -0.01434 0.00131 -0.02259 AFIX 43 H57 2 -0.457393 -0.090867 0.216327 11.00000 -1.20000 AFIX 0 C58 1 -0.386646 -0.067531 0.279417 11.00000 0.04669 0.07020 = 0.03585 -0.01070 0.01162 -0.02897 AFIX 43 H58 2 -0.462324 -0.086859 0.297952 11.00000 -1.20000 AFIX 0 C59 1 -0.278412 -0.037820 0.300384 11.00000 0.04610 0.05843 = 0.02895 -0.01240 0.01010 -0.02069 AFIX 43 H59 2 -0.279867 -0.037422 0.333559 11.00000 -1.20000 AFIX 0 C60 1 -0.166002 -0.008113 0.273863 11.00000 0.04200 0.05036 = 0.02961 -0.01184 0.00508 -0.01652 C61 1 0.148957 -0.009326 -0.048633 11.00000 0.02823 0.04997 = 0.03327 -0.01281 0.00009 -0.01225 AFIX 23 H61A 2 0.044505 -0.012109 -0.047470 11.00000 -1.20000 H61B 2 0.196237 -0.052042 -0.067446 11.00000 -1.20000 AFIX 0 C62 1 0.200563 -0.112655 0.020680 11.00000 0.02958 0.04594 = 0.03252 -0.00833 0.00345 -0.01568 AFIX 23 H62A 2 0.252554 -0.154280 0.002034 11.00000 -1.20000 H62B 2 0.098006 -0.119833 0.022339 11.00000 -1.20000 AFIX 0 C63 1 0.266572 -0.128263 0.069875 11.00000 0.03198 0.05226 = 0.02966 -0.01046 0.00837 -0.01538 AFIX 23 H63A 2 0.224194 -0.081756 0.086946 11.00000 -1.20000 H63B 2 0.245651 -0.182583 0.087734 11.00000 -1.20000 AFIX 0 C64 1 0.491182 -0.150520 0.111475 11.00000 0.04003 0.05132 = 0.02195 -0.00913 0.00282 -0.01529 AFIX 23 H64A 2 0.470182 -0.204738 0.129440 11.00000 -1.20000 H64B 2 0.457900 -0.104694 0.130068 11.00000 -1.20000 AFIX 0 C65 1 0.651113 -0.157644 0.103708 11.00000 0.03969 0.04358 = 0.02642 -0.00585 -0.00139 -0.01086 AFIX 23 H65A 2 0.704925 -0.177828 0.134339 11.00000 -1.20000 H65B 2 0.682467 -0.199252 0.082352 11.00000 -1.20000 AFIX 0 C66 1 0.830564 -0.078048 0.071803 11.00000 0.02972 0.04289 = 0.03464 -0.00976 0.00194 -0.00938 AFIX 23 H66A 2 0.859980 -0.119275 0.050087 11.00000 -1.20000 H66B 2 0.891418 -0.096470 0.101130 11.00000 -1.20000 AFIX 0 C67 1 0.262354 -0.123708 0.453681 11.00000 0.05105 0.06283 = 0.02922 -0.00517 -0.00388 -0.02720 AFIX 23 H67A 2 0.237634 -0.176159 0.444754 11.00000 -1.20000 H67B 2 0.223351 -0.074958 0.428683 11.00000 -1.20000 AFIX 0 C68 1 0.488605 -0.147796 0.416060 11.00000 0.06108 0.05959 = 0.02599 -0.01000 0.00187 -0.02613 AFIX 23 H68A 2 0.456270 -0.100438 0.389558 11.00000 -1.20000 H68B 2 0.466799 -0.200997 0.407244 11.00000 -1.20000 AFIX 0 C69 1 0.648995 -0.156299 0.425535 11.00000 0.05989 0.06339 = 0.02938 -0.01445 0.00885 -0.02596 AFIX 23 H69A 2 0.678374 -0.197697 0.454921 11.00000 -1.20000 H69B 2 0.703567 -0.177296 0.398929 11.00000 -1.20000 AFIX 0 C70 1 0.828913 -0.077912 0.441145 11.00000 0.04976 0.06768 = 0.03494 -0.01101 0.00991 -0.02431 AFIX 23 H70A 2 0.888649 -0.096247 0.414889 11.00000 -1.20000 H70B 2 0.859006 -0.119490 0.470410 11.00000 -1.20000 AFIX 0 C71 1 0.851666 0.008882 0.447894 11.00000 0.04509 0.07219 = 0.02915 -0.00994 0.01122 -0.02372 AFIX 23 H71A 2 0.956396 0.010887 0.448371 11.00000 -1.20000 H71B 2 0.804993 0.052184 0.421268 11.00000 -1.20000 AFIX 0 C72 1 0.801858 0.110011 0.499119 11.00000 0.05135 0.06301 = 0.03252 -0.00240 -0.00113 -0.03070 AFIX 23 H72A 2 0.749474 0.152841 0.473312 11.00000 -1.20000 H72B 2 0.904712 0.116600 0.498974 11.00000 -1.20000 AFIX 0 RB1 3 0.500000 0.000000 0.000000 10.50000 0.03371 0.05414 = 0.03004 0.00055 -0.00235 -0.02155 RB2 3 0.500000 0.000000 0.500000 10.50000 0.05209 0.07479 = 0.04216 -0.02443 0.01429 -0.03681 O1 4 0.210161 -0.028105 -0.001744 11.00000 0.03221 0.04523 = 0.02796 -0.00949 0.00377 -0.01571 O2 4 0.418167 -0.131940 0.066921 11.00000 0.03496 0.05426 = 0.02200 -0.00680 0.00491 -0.01869 O3 4 0.681035 -0.075691 0.082996 11.00000 0.03316 0.04577 = 0.02708 -0.00702 0.00386 -0.01297 O4 4 0.415268 -0.131264 0.458333 11.00000 0.05120 0.06754 = 0.02661 -0.00824 0.00109 -0.02908 O5 4 0.679989 -0.075518 0.430465 11.00000 0.04923 0.06424 = 0.03067 -0.00847 0.00506 -0.02465 O6 4 0.790344 0.026895 0.491731 11.00000 0.05380 0.06140 = 0.02829 -0.00644 0.00613 -0.02883 RB3 3 0.319142 0.410650 0.213435 11.00000 0.05902 0.06658 = 0.03331 -0.00614 0.00074 -0.02159 PART 1 O7 4 0.592936 0.239063 0.208394 41.00000 0.12342 0.10817 = 0.14616 -0.05033 0.06445 -0.03410 C73 1 0.568644 0.267652 0.248544 41.00000 0.11604 0.12097 = 0.07634 -0.00725 -0.00469 -0.04562 AFIX 23 H73A 2 0.508159 0.325126 0.242799 41.00000 -1.20000 H73B 2 0.661030 0.271201 0.263984 41.00000 -1.20000 AFIX 0 PART 2 O7A 4 0.568644 0.267652 0.248544 -41.00000 0.11604 0.12097 = 0.07634 -0.00725 -0.00469 -0.04562 C73A 1 0.592936 0.239063 0.208394 -41.00000 0.12342 0.10817 = 0.14616 -0.05033 0.06445 -0.03410 AFIX 23 H73C 2 0.693746 0.208097 0.209044 -41.00000 -1.20000 H73D 2 0.583013 0.288123 0.182066 -41.00000 -1.20000 AFIX 0 PART 0 C74 1 0.494998 0.182343 0.199001 11.00000 0.10659 0.08548 = 0.09844 -0.04038 0.01231 -0.00388 AFIX 23 H74A 2 0.549438 0.126840 0.193457 11.00000 -1.20000 H74B 2 0.430580 0.208267 0.171157 11.00000 -1.20000 AFIX 0 C75 1 0.410118 0.172159 0.243962 11.00000 0.06711 0.08548 = 0.10367 0.00066 -0.00543 -0.01521 AFIX 23 H75A 2 0.406686 0.111452 0.255890 11.00000 -1.20000 H75B 2 0.310135 0.204333 0.238831 11.00000 -1.20000 AFIX 0 C76 1 0.495310 0.208959 0.277923 11.00000 0.10167 0.12357 = 0.07189 0.00571 -0.01106 -0.03953 AFIX 23 H76A 2 0.429697 0.238470 0.299454 11.00000 -1.20000 H76B 2 0.565437 0.163401 0.297238 11.00000 -1.20000 AFIX 0 O8 4 0.185426 0.586545 0.187829 11.00000 0.13783 0.08524 = 0.09332 0.00229 0.00003 -0.00788 C77 1 0.184994 0.638588 0.142306 11.00000 0.10912 0.06664 = 0.08159 0.00845 -0.00702 -0.00563 AFIX 23 H77A 2 0.200787 0.602905 0.117175 11.00000 -1.20000 H77B 2 0.262254 0.673438 0.140949 11.00000 -1.20000 AFIX 0 C78 1 0.037965 0.695006 0.135828 11.00000 0.08873 0.07281 = 0.07357 -0.00167 -0.02413 -0.02817 AFIX 23 H78A 2 0.041098 0.751140 0.144877 11.00000 -1.20000 H78B 2 0.002282 0.703732 0.102536 11.00000 -1.20000 AFIX 0 C79 1 -0.054022 0.647145 0.167994 11.00000 0.10011 0.12915 = 0.13733 0.04249 -0.01208 -0.03794 AFIX 23 H79A 2 -0.087786 0.602721 0.153126 11.00000 -1.20000 H79B 2 -0.138714 0.685463 0.177768 11.00000 -1.20000 AFIX 0 PART 1 C80 1 0.052866 0.606879 0.210934 21.00000 0.10123 0.08105 = 0.09036 0.00118 0.00172 -0.02589 AFIX 23 H80A 2 0.059492 0.648160 0.232436 21.00000 -1.20000 H80B 2 0.023396 0.555230 0.229196 21.00000 -1.20000 AFIX 0 PART 2 C80A 1 0.024281 0.575574 0.191172 -21.00000 0.12616 0.07701 = 0.10158 0.01029 0.02355 0.00027 AFIX 23 H80C 2 0.008983 0.526339 0.176590 -21.00000 -1.20000 H80D 2 -0.003961 0.565710 0.224763 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 SAME O9A > C92A SAME O9 C92 < C81 O9 4 0.595486 0.467432 0.210938 31.00000 0.07972 0.12156 = 0.05403 0.00140 0.00531 -0.05837 C81 1 0.621835 0.504856 0.163410 31.00000 0.11215 0.06088 = 0.08241 0.00520 0.02635 -0.05382 AFIX 23 H81A 2 0.553269 0.559107 0.154458 31.00000 -1.20000 H81B 2 0.721072 0.517914 0.161876 31.00000 -1.20000 AFIX 0 C82 1 0.605929 0.449566 0.130353 31.00000 0.07579 0.09678 = 0.04452 0.01264 0.00972 -0.00989 AFIX 23 H82A 2 0.635024 0.475552 0.098725 31.00000 -1.20000 H82B 2 0.672846 0.394915 0.140105 31.00000 -1.20000 AFIX 0 O10 4 0.467792 0.432967 0.126489 31.00000 0.12669 0.10597 = 0.05742 -0.03548 0.03635 -0.06794 C83 1 0.425170 0.392410 0.093441 31.00000 0.07768 0.10952 = 0.04533 -0.02876 0.01235 0.00393 AFIX 23 H83A 2 0.485020 0.334780 0.097788 31.00000 -1.20000 H83B 2 0.448100 0.422840 0.062088 31.00000 -1.20000 AFIX 0 C84 1 0.280393 0.382961 0.091605 31.00000 0.11223 0.07206 = 0.04174 -0.00651 -0.00426 -0.02472 AFIX 23 H84A 2 0.222297 0.438733 0.077714 31.00000 -1.20000 H84B 2 0.271162 0.342756 0.069682 31.00000 -1.20000 AFIX 0 O11 4 0.221256 0.354606 0.133756 31.00000 0.07841 0.16790 = 0.04949 -0.05017 0.01049 -0.02984 C85 1 0.084158 0.341082 0.135423 31.00000 0.11804 0.09890 = 0.06549 -0.01957 -0.02365 -0.06893 AFIX 23 H85A 2 0.071092 0.305736 0.111187 31.00000 -1.20000 H85B 2 0.019927 0.396789 0.125938 31.00000 -1.20000 AFIX 0 C86 1 0.033497 0.299855 0.180905 31.00000 0.08483 0.13696 = 0.07803 -0.04460 0.00291 -0.04326 AFIX 23 H86A 2 -0.072469 0.302735 0.178700 31.00000 -1.20000 H86B 2 0.079457 0.239042 0.187211 31.00000 -1.20000 AFIX 0 O12 4 0.066322 0.338749 0.218045 31.00000 0.07901 0.07904 = 0.05378 -0.01131 0.00002 -0.04020 C87 1 0.029011 0.299246 0.263749 31.00000 0.05359 0.06602 = 0.07588 -0.00427 0.00970 -0.02311 AFIX 23 H87A 2 0.084581 0.240555 0.271212 31.00000 -1.20000 H87B 2 -0.075224 0.295845 0.263790 31.00000 -1.20000 AFIX 0 C88 1 0.061589 0.349308 0.300600 31.00000 0.06195 0.08537 = 0.05221 -0.00154 0.01981 -0.02078 AFIX 23 H88A 2 -0.009937 0.402867 0.296537 31.00000 -1.20000 H88B 2 0.046665 0.316460 0.332143 31.00000 -1.20000 AFIX 0 O13 4 0.194709 0.369542 0.300805 31.00000 0.10323 0.15440 = 0.04210 -0.02454 0.02021 -0.07806 C89 1 0.242461 0.400843 0.338847 31.00000 0.09419 0.13217 = 0.02814 -0.01241 0.01303 -0.04528 AFIX 23 H89A 2 0.224271 0.363436 0.368566 31.00000 -1.20000 H89B 2 0.185566 0.458216 0.339454 31.00000 -1.20000 AFIX 0 C90 1 0.394811 0.406496 0.337467 31.00000 0.12852 0.17225 = 0.05004 -0.02119 0.00375 -0.07956 AFIX 23 H90A 2 0.418456 0.433928 0.364202 31.00000 -1.20000 H90B 2 0.451679 0.348022 0.342503 31.00000 -1.20000 AFIX 0 O14 4 0.436634 0.449636 0.297368 31.00000 0.07055 0.09686 = 0.04790 -0.02205 0.00406 -0.03476 C91 1 0.575801 0.466618 0.292957 31.00000 0.09798 0.14173 = 0.06327 -0.01540 -0.02004 -0.05971 AFIX 23 H91A 2 0.589118 0.504039 0.316074 31.00000 -1.20000 H91B 2 0.643024 0.412145 0.302894 31.00000 -1.20000 AFIX 0 C92 1 0.619541 0.503656 0.249574 31.00000 0.12189 0.16516 = 0.09938 -0.05726 0.03186 -0.09874 AFIX 23 H92A 2 0.570290 0.563860 0.243265 31.00000 -1.20000 H92B 2 0.724582 0.503788 0.252146 31.00000 -1.20000 AFIX 0 PART 2 O9A 4 0.523130 0.491091 0.247038 -31.00000 0.11662 0.13856 = 0.09243 -0.05011 0.00668 -0.06948 C81A 1 0.642511 0.490056 0.218933 -31.00000 0.11806 0.13164 = 0.09465 -0.00212 -0.00004 -0.08037 AFIX 23 H81C 2 0.665694 0.548233 0.214701 -31.00000 -1.20000 H81D 2 0.723329 0.452271 0.238091 -31.00000 -1.20000 AFIX 0 C82A 1 0.649325 0.467342 0.175398 -31.00000 0.11287 0.13316 = 0.11207 -0.03148 0.04495 -0.08651 AFIX 23 H82C 2 0.723233 0.415010 0.177762 -31.00000 -1.20000 H82D 2 0.687822 0.512518 0.153968 -31.00000 -1.20000 AFIX 0 O10A 4 0.528871 0.452136 0.152320 -31.00000 0.09519 0.13369 = 0.06964 -0.01103 0.02652 -0.04930 C83A 1 0.494020 0.464378 0.106327 -31.00000 0.10910 0.09143 = 0.06790 0.00208 0.04200 -0.02258 AFIX 23 H83C 2 0.585267 0.454078 0.089079 -31.00000 -1.20000 H83D 2 0.451908 0.525396 0.096770 -31.00000 -1.20000 AFIX 0 C84A 1 0.400779 0.418057 0.089881 -31.00000 0.08032 0.13284 = 0.04097 -0.00749 0.01092 0.00880 AFIX 23 H84C 2 0.457006 0.361716 0.086540 -31.00000 -1.20000 H84D 2 0.365963 0.447273 0.057709 -31.00000 -1.20000 AFIX 0 O11A 4 0.281257 0.404525 0.116499 -31.00000 0.14076 0.08087 = 0.03412 -0.01746 0.02184 -0.05404 C85A 1 0.197689 0.350038 0.104307 -31.00000 0.12912 0.10359 = 0.04641 -0.03451 -0.00820 -0.02831 AFIX 23 H85C 2 0.258387 0.292798 0.107285 -31.00000 -1.20000 H85D 2 0.168531 0.368613 0.070432 -31.00000 -1.20000 AFIX 0 C86A 1 0.067188 0.341906 0.131390 -31.00000 0.10388 0.11418 = 0.07229 -0.02203 -0.02461 -0.04026 AFIX 23 H86C 2 -0.005915 0.394107 0.122083 -31.00000 -1.20000 H86D 2 0.026625 0.293217 0.123517 -31.00000 -1.20000 AFIX 0 O12A 4 0.094737 0.329291 0.180805 -31.00000 0.10387 0.09700 = 0.06142 -0.01749 -0.00069 -0.06035 C87A 1 -0.028647 0.321666 0.207760 -31.00000 0.07902 0.12077 = 0.10107 -0.01614 0.00258 -0.04296 AFIX 23 H87C 2 -0.055768 0.265803 0.205895 -31.00000 -1.20000 H87D 2 -0.109127 0.366319 0.193119 -31.00000 -1.20000 AFIX 0 C88A 1 -0.014964 0.328416 0.256605 -31.00000 0.05507 0.14736 = 0.09881 -0.02485 0.02465 -0.03274 AFIX 23 H88C 2 -0.109342 0.359079 0.265280 -31.00000 -1.20000 H88D 2 -0.004149 0.269697 0.274590 -31.00000 -1.20000 AFIX 0 O13A 4 0.085135 0.364022 0.273983 -31.00000 0.07237 0.13226 = 0.05371 0.02112 0.00534 -0.03874 C89A 1 0.115393 0.353763 0.322454 -31.00000 0.11390 0.09844 = 0.04496 0.01072 0.03230 -0.04090 AFIX 23 H89C 2 0.166627 0.294852 0.333462 -31.00000 -1.20000 H89D 2 0.023005 0.361178 0.339328 -31.00000 -1.20000 AFIX 0 C90A 1 0.199889 0.410929 0.334817 -31.00000 0.12736 0.10574 = 0.04985 -0.02508 0.02703 -0.02804 AFIX 23 H90C 2 0.137919 0.467858 0.331303 -31.00000 -1.20000 H90D 2 0.227433 0.393263 0.368865 -31.00000 -1.20000 AFIX 0 O14A 4 0.320705 0.419397 0.310829 -31.00000 0.12639 0.12181 = 0.03477 -0.01952 0.00125 -0.05387 C91A 1 0.404313 0.476982 0.321611 -31.00000 0.17056 0.12908 = 0.05343 -0.01996 -0.01913 -0.07086 AFIX 23 H91C 2 0.337841 0.531370 0.322414 -31.00000 -1.20000 H91D 2 0.443581 0.455784 0.354317 -31.00000 -1.20000 AFIX 0 C92A 1 0.516951 0.495770 0.294225 -31.00000 0.11971 0.14606 = 0.08371 -0.03484 -0.02426 -0.05816 AFIX 23 H92C 2 0.604931 0.458316 0.309444 -31.00000 -1.20000 H92D 2 0.526661 0.554738 0.297026 -31.00000 -1.20000 PART 0 AFIX 0 HKLF 4 REM sad in P-1 REM R1 = 0.0655 for 10031 Fo > 4sig(Fo) and 0.0916 for all 14310 data REM 1150 parameters refined using 2254 restraints END WGHT 0.1182 0.0000 REM Highest difference peak 1.531, deepest hole -0.670, 1-sigma level 0.084 Q1 1 0.2412 0.4720 0.2057 11.00000 0.05 1.53 Q2 1 0.6376 0.2196 0.2415 11.00000 0.05 0.95 Q3 1 0.4408 0.0521 -0.0027 11.00000 0.05 0.86 Q4 1 0.5252 0.2650 0.1978 11.00000 0.05 0.71 Q5 1 0.4468 0.0598 0.4854 11.00000 0.05 0.71 Q6 1 0.3097 0.4793 0.3339 11.00000 0.05 0.70 Q7 1 0.1375 0.4197 0.2943 11.00000 0.05 0.59 Q8 1 0.4063 0.3715 0.1998 11.00000 0.05 0.59 Q9 1 -0.0063 0.3666 0.1678 11.00000 0.05 0.43 Q10 1 -0.0019 0.4243 0.1414 11.00000 0.05 0.38 Q11 1 0.4238 0.5728 0.2226 11.00000 0.05 0.38 Q12 1 0.1391 0.2243 0.2347 11.00000 0.05 0.37 Q13 1 0.4840 0.0624 0.1137 11.00000 0.05 0.37 Q14 1 0.7237 0.1876 0.2296 11.00000 0.05 0.36 Q15 1 0.5129 -0.0151 0.4790 11.00000 0.05 0.36 Q16 1 0.5889 0.1378 0.4121 11.00000 0.05 0.36 Q17 1 0.2332 0.3977 0.1274 11.00000 0.05 0.36 Q18 1 -0.0590 0.6913 0.1966 11.00000 0.05 0.35 Q19 1 -0.1591 0.4586 0.4222 11.00000 0.05 0.34 Q20 1 0.2672 -0.0225 -0.0167 11.00000 0.05 0.34 ; _database_code_depnum_ccdc_archive 'CCDC 973695' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(C60H28)_(1) _audit_creation_method SHELXL-2013 _chemical_name_systematic ; Bisdibenzo[1,10-6,7]fluorantheno[2,3-b:2',3'-n]tetraphenylene ; _chemical_melting_point 'not measured' _chemical_formula_moiety 'C60 H28' _chemical_formula_sum 'C60 H28' _chemical_formula_weight 748.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8507(3) _cell_length_b 14.1479(4) _cell_length_c 15.1646(4) _cell_angle_alpha 105.607(1) _cell_angle_beta 102.809(1) _cell_angle_gamma 110.367(1) _cell_volume 1788.10(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 69.94 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_density_diffrn 1.391 _exptl_crystal_F_000 776 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.605 _shelx_estimated_absorpt_T_min 0.920 _shelx_estimated_absorpt_T_max 0.982 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'ImuS micro-focus source with Quazar optics' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '0.5 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26110 _diffrn_reflns_av_unetI/netI 0.0203 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.229 _diffrn_reflns_theta_max 69.932 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_point_group_measured_fraction_full 0.973 _reflns_number_total 6486 _reflns_number_gt 5763 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex2 (Bruker AXS Inc., 2013)' _computing_cell_refinement 'Apex2 (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXT (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXP (Sheldrick, 2008)' _computing_publication_material 'SHELXCIF-2013/2 (Sheldrick, 2013)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.7590P] 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 6486 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0930 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.40219(15) 0.27871(10) 0.35860(9) 0.0167(3) Uani 1 1 d . . . . . C2 C 0.32037(15) 0.33448(11) 0.32547(9) 0.0171(3) Uani 1 1 d . . . . . C3 C 0.41663(15) 0.41138(11) 0.29653(9) 0.0167(3) Uani 1 1 d . . . . . C4 C 0.55809(15) 0.40266(11) 0.31007(9) 0.0164(3) Uani 1 1 d . . . . . C5 C 0.55035(15) 0.32124(10) 0.34903(9) 0.0160(3) Uani 1 1 d . . . . . C6 C 0.37533(15) 0.23468(10) 0.42697(10) 0.0178(3) Uani 1 1 d . . . . . C7 C 0.23980(16) 0.23255(11) 0.44942(10) 0.0211(3) Uani 1 1 d . . . . . H7A H 0.2050 0.1931 0.4880 0.025 Uiso 1 1 calc R U . . . C8 C 0.15897(16) 0.28628(12) 0.41647(11) 0.0222(3) Uani 1 1 d . . . . . H8A H 0.0695 0.2820 0.4324 0.027 Uiso 1 1 calc R U . . . C9 C 0.20656(15) 0.34866(11) 0.35869(10) 0.0199(3) Uani 1 1 d . . . . . C10 C 0.17984(16) 0.44002(12) 0.34889(10) 0.0218(3) Uani 1 1 d . . . . . H10A H 0.0936 0.4483 0.3616 0.026 Uiso 1 1 calc R U . . . C11 C 0.27474(16) 0.51564(11) 0.32179(10) 0.0204(3) Uani 1 1 d . . . . . H11A H 0.2526 0.5746 0.3170 0.024 Uiso 1 1 calc R U . . . C12 C 0.40695(16) 0.50755(11) 0.30052(9) 0.0181(3) Uani 1 1 d . . . . . C13 C 0.54292(16) 0.59116(11) 0.30105(10) 0.0199(3) Uani 1 1 d . . . . . H13A H 0.5376 0.6542 0.2929 0.024 Uiso 1 1 calc R U . . . C14 C 0.68029(16) 0.58240(11) 0.31303(10) 0.0193(3) Uani 1 1 d . . . . . H14A H 0.7670 0.6392 0.3126 0.023 Uiso 1 1 calc R U . . . C15 C 0.69495(16) 0.48839(11) 0.32619(9) 0.0176(3) Uani 1 1 d . . . . . C16 C 0.83096(15) 0.47902(11) 0.37245(10) 0.0187(3) Uani 1 1 d . . . . . H16A H 0.9289 0.5288 0.3770 0.022 Uiso 1 1 calc R U . . . C17 C 0.82354(15) 0.39947(11) 0.41057(10) 0.0179(3) Uani 1 1 d . . . . . H17A H 0.9167 0.3966 0.4407 0.021 Uiso 1 1 calc R U . . . C18 C 0.67935(15) 0.32099(10) 0.40602(9) 0.0162(3) Uani 1 1 d . . . . . C19 C 0.65205(15) 0.25922(10) 0.46936(9) 0.0164(3) Uani 1 1 d . . . . . C20 C 0.50369(15) 0.21837(10) 0.48073(10) 0.0170(3) Uani 1 1 d . . . . . C21 C 0.87638(15) 0.67979(10) 0.95831(9) 0.0159(3) Uani 1 1 d . . . . . C22 C 0.82322(16) 0.76125(10) 0.96127(9) 0.0173(3) Uani 1 1 d . . . . . C23 C 0.92493(16) 0.84118(10) 0.93774(10) 0.0182(3) Uani 1 1 d . . . . . C24 C 1.04338(15) 0.81146(10) 0.92296(10) 0.0179(3) Uani 1 1 d . . . . . C25 C 1.01404(15) 0.71158(10) 0.93537(9) 0.0164(3) Uani 1 1 d . . . . . C26 C 0.77982(15) 0.57382(11) 0.93831(9) 0.0164(3) Uani 1 1 d . . . . . C27 C 0.62624(16) 0.55610(11) 0.93755(10) 0.0185(3) Uani 1 1 d . . . . . H27A H 0.5580 0.4872 0.9337 0.022 Uiso 1 1 calc R U . . . C28 C 0.57483(16) 0.63643(11) 0.94226(10) 0.0202(3) Uani 1 1 d . . . . . H28A H 0.4733 0.6214 0.9428 0.024 Uiso 1 1 calc R U . . . C29 C 0.67134(16) 0.74207(11) 0.94633(10) 0.0196(3) Uani 1 1 d . . . . . C30 C 0.63036(17) 0.82100(11) 0.91774(10) 0.0229(3) Uani 1 1 d . . . . . H30A H 0.5331 0.8202 0.9163 0.027 Uiso 1 1 calc R U . . . C31 C 0.72844(17) 0.89739(11) 0.89251(10) 0.0235(3) Uani 1 1 d . . . . . H31A H 0.6958 0.9467 0.8730 0.028 Uiso 1 1 calc R U . . . C32 C 0.87914(17) 0.90458(11) 0.89483(10) 0.0210(3) Uani 1 1 d . . . . . C33 C 0.97793(17) 0.95295(11) 0.84594(11) 0.0242(3) Uani 1 1 d . . . . . H33A H 0.9617 1.0054 0.8225 0.029 Uiso 1 1 calc R U . . . C34 C 1.09470(17) 0.92530(11) 0.83237(11) 0.0241(3) Uani 1 1 d . . . . . H34A H 1.1571 0.9597 0.8003 0.029 Uiso 1 1 calc R U . . . C35 C 1.12568(16) 0.84521(11) 0.86551(10) 0.0206(3) Uani 1 1 d . . . . . C36 C 1.20179(16) 0.77935(11) 0.83346(10) 0.0211(3) Uani 1 1 d . . . . . H36A H 1.2736 0.8035 0.8025 0.025 Uiso 1 1 calc R U . . . C37 C 1.17376(15) 0.68179(11) 0.84631(10) 0.0188(3) Uani 1 1 d . . . . . H37A H 1.2272 0.6414 0.8240 0.023 Uiso 1 1 calc R U . . . C38 C 1.06630(15) 0.63975(10) 0.89231(9) 0.0165(3) Uani 1 1 d . . . . . C39 C 0.97895(15) 0.52612(10) 0.88029(9) 0.0156(3) Uani 1 1 d . . . . . C40 C 0.83784(15) 0.49387(10) 0.90164(9) 0.0155(3) Uani 1 1 d . . . . . C41 C 0.49121(15) 0.17296(10) 0.55176(10) 0.0179(3) Uani 1 1 d . . . . . H41A H 0.3936 0.1452 0.5594 0.021 Uiso 1 1 calc R U . . . C42 C 0.61393(16) 0.16635(10) 0.61160(10) 0.0171(3) Uani 1 1 d . . . . . C43 C 0.75683(15) 0.20115(10) 0.59688(9) 0.0166(3) Uani 1 1 d . . . . . C44 C 0.77199(15) 0.24575(10) 0.52642(10) 0.0165(3) Uani 1 1 d . . . . . H44A H 0.8681 0.2682 0.5163 0.020 Uiso 1 1 calc R U . . . C45 C 0.74672(15) 0.38216(11) 0.87355(9) 0.0165(3) Uani 1 1 d . . . . . H45A H 0.6560 0.3603 0.8898 0.020 Uiso 1 1 calc R U . . . C46 C 0.78251(15) 0.30202(10) 0.82316(9) 0.0160(3) Uani 1 1 d . . . . . C47 C 0.92337(15) 0.33369(10) 0.80516(9) 0.0159(3) Uani 1 1 d . . . . . C48 C 1.01849(15) 0.44397(11) 0.83569(9) 0.0163(3) Uani 1 1 d . . . . . H48A H 1.1149 0.4648 0.8259 0.020 Uiso 1 1 calc R U . . . C49 C 0.89059(15) 0.18851(10) 0.65259(10) 0.0175(3) Uani 1 1 d . . . . . C50 C 0.94219(17) 0.11730(11) 0.60355(11) 0.0224(3) Uani 1 1 d . . . . . H50A H 0.8883 0.0745 0.5359 0.027 Uiso 1 1 calc R U . . . C51 C 1.07128(18) 0.10815(12) 0.65232(11) 0.0248(3) Uani 1 1 d . . . . . H51A H 1.1037 0.0581 0.6184 0.030 Uiso 1 1 calc R U . . . C52 C 1.15253(17) 0.17221(12) 0.75048(11) 0.0223(3) Uani 1 1 d . . . . . H52A H 1.2416 0.1668 0.7839 0.027 Uiso 1 1 calc R U . . . C53 C 1.10349(16) 0.24435(11) 0.79994(10) 0.0189(3) Uani 1 1 d . . . . . H53A H 1.1605 0.2889 0.8670 0.023 Uiso 1 1 calc R U . . . C54 C 0.97118(15) 0.25233(10) 0.75228(10) 0.0163(3) Uani 1 1 d . . . . . C55 C 0.58800(15) 0.12210(10) 0.68873(10) 0.0173(3) Uani 1 1 d . . . . . C56 C 0.46998(16) 0.01809(11) 0.66000(10) 0.0204(3) Uani 1 1 d . . . . . H56A H 0.4173 -0.0257 0.5924 0.025 Uiso 1 1 calc R U . . . C57 C 0.42825(16) -0.02238(11) 0.72882(11) 0.0222(3) Uani 1 1 d . . . . . H57A H 0.3481 -0.0935 0.7083 0.027 Uiso 1 1 calc R U . . . C58 C 0.50419(16) 0.04154(11) 0.82768(10) 0.0214(3) Uani 1 1 d . . . . . H58A H 0.4750 0.0148 0.8750 0.026 Uiso 1 1 calc R U . . . C59 C 0.62293(16) 0.14472(11) 0.85712(10) 0.0183(3) Uani 1 1 d . . . . . H59A H 0.6752 0.1879 0.9249 0.022 Uiso 1 1 calc R U . . . C60 C 0.66697(15) 0.18615(10) 0.78863(10) 0.0169(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 0.0156(6) 0.0156(6) 0.0146(7) 0.0031(5) 0.0034(5) 0.0054(5) C2 0.0145(6) 0.0190(6) 0.0125(6) 0.0037(5) 0.0010(5) 0.0053(5) C3 0.0172(6) 0.0205(6) 0.0096(6) 0.0043(5) 0.0023(5) 0.0074(5) C4 0.0198(7) 0.0204(6) 0.0110(6) 0.0057(5) 0.0064(5) 0.0104(5) C5 0.0174(6) 0.0158(6) 0.0130(6) 0.0027(5) 0.0054(5) 0.0073(5) C6 0.0165(6) 0.0157(6) 0.0163(7) 0.0043(5) 0.0035(5) 0.0042(5) C7 0.0176(7) 0.0243(7) 0.0204(7) 0.0105(6) 0.0070(6) 0.0062(6) C8 0.0151(6) 0.0287(7) 0.0239(8) 0.0112(6) 0.0079(6) 0.0090(6) C9 0.0151(6) 0.0252(7) 0.0162(7) 0.0068(6) 0.0030(5) 0.0075(6) C10 0.0178(7) 0.0304(7) 0.0190(7) 0.0089(6) 0.0049(6) 0.0138(6) C11 0.0218(7) 0.0256(7) 0.0157(7) 0.0077(6) 0.0039(6) 0.0140(6) C12 0.0203(7) 0.0230(7) 0.0111(6) 0.0063(5) 0.0030(5) 0.0111(6) C13 0.0249(7) 0.0207(7) 0.0165(7) 0.0088(5) 0.0064(6) 0.0117(6) C14 0.0208(7) 0.0205(7) 0.0168(7) 0.0087(5) 0.0067(6) 0.0078(6) C15 0.0201(7) 0.0220(7) 0.0138(7) 0.0075(5) 0.0084(6) 0.0105(6) C16 0.0170(6) 0.0222(7) 0.0179(7) 0.0082(5) 0.0086(6) 0.0075(5) C17 0.0167(6) 0.0227(7) 0.0163(7) 0.0072(5) 0.0069(5) 0.0101(5) C18 0.0183(6) 0.0165(6) 0.0144(6) 0.0042(5) 0.0066(5) 0.0092(5) C19 0.0187(6) 0.0141(6) 0.0139(6) 0.0025(5) 0.0050(5) 0.0068(5) C20 0.0174(6) 0.0143(6) 0.0159(7) 0.0032(5) 0.0048(5) 0.0058(5) C21 0.0195(6) 0.0173(6) 0.0104(6) 0.0043(5) 0.0041(5) 0.0089(5) C22 0.0218(7) 0.0159(6) 0.0116(6) 0.0022(5) 0.0045(5) 0.0083(5) C23 0.0206(7) 0.0135(6) 0.0146(7) 0.0010(5) 0.0028(6) 0.0061(5) C24 0.0175(6) 0.0136(6) 0.0155(7) 0.0024(5) 0.0011(5) 0.0042(5) C25 0.0157(6) 0.0160(6) 0.0120(6) 0.0033(5) 0.0003(5) 0.0051(5) C26 0.0194(7) 0.0188(6) 0.0116(6) 0.0058(5) 0.0053(5) 0.0089(5) C27 0.0215(7) 0.0185(6) 0.0153(7) 0.0059(5) 0.0084(6) 0.0077(5) C28 0.0197(7) 0.0230(7) 0.0183(7) 0.0057(6) 0.0086(6) 0.0102(6) C29 0.0225(7) 0.0202(7) 0.0155(7) 0.0032(5) 0.0069(6) 0.0113(6) C30 0.0233(7) 0.0224(7) 0.0224(7) 0.0045(6) 0.0058(6) 0.0136(6) C31 0.0285(8) 0.0181(7) 0.0229(8) 0.0055(6) 0.0045(6) 0.0134(6) C32 0.0252(7) 0.0143(6) 0.0188(7) 0.0030(5) 0.0036(6) 0.0083(6) C33 0.0300(8) 0.0160(6) 0.0247(8) 0.0086(6) 0.0064(6) 0.0093(6) C34 0.0264(7) 0.0177(6) 0.0248(8) 0.0090(6) 0.0084(6) 0.0055(6) C35 0.0193(7) 0.0156(6) 0.0219(7) 0.0057(5) 0.0051(6) 0.0043(5) C36 0.0185(7) 0.0193(7) 0.0224(7) 0.0079(6) 0.0081(6) 0.0042(5) C37 0.0160(6) 0.0177(6) 0.0191(7) 0.0046(5) 0.0045(6) 0.0061(5) C38 0.0148(6) 0.0174(6) 0.0142(6) 0.0057(5) 0.0017(5) 0.0060(5) C39 0.0164(6) 0.0166(6) 0.0118(6) 0.0054(5) 0.0021(5) 0.0066(5) C40 0.0179(6) 0.0174(6) 0.0111(6) 0.0058(5) 0.0037(5) 0.0080(5) C41 0.0175(6) 0.0146(6) 0.0183(7) 0.0043(5) 0.0064(6) 0.0049(5) C42 0.0208(7) 0.0124(6) 0.0153(7) 0.0031(5) 0.0058(6) 0.0061(5) C43 0.0195(6) 0.0125(6) 0.0153(7) 0.0027(5) 0.0046(5) 0.0073(5) C44 0.0170(6) 0.0146(6) 0.0167(7) 0.0039(5) 0.0065(5) 0.0065(5) C45 0.0177(6) 0.0181(6) 0.0143(6) 0.0072(5) 0.0060(5) 0.0075(5) C46 0.0189(6) 0.0168(6) 0.0121(6) 0.0067(5) 0.0035(5) 0.0078(5) C47 0.0189(6) 0.0179(6) 0.0121(6) 0.0068(5) 0.0036(5) 0.0096(5) C48 0.0148(6) 0.0190(6) 0.0153(7) 0.0074(5) 0.0041(5) 0.0076(5) C49 0.0196(7) 0.0156(6) 0.0189(7) 0.0081(5) 0.0078(6) 0.0077(5) C50 0.0275(7) 0.0222(7) 0.0181(7) 0.0055(6) 0.0079(6) 0.0130(6) C51 0.0311(8) 0.0248(7) 0.0263(8) 0.0095(6) 0.0135(7) 0.0186(6) C52 0.0239(7) 0.0263(7) 0.0255(8) 0.0146(6) 0.0103(6) 0.0158(6) C53 0.0210(7) 0.0198(6) 0.0178(7) 0.0089(5) 0.0070(6) 0.0095(6) C54 0.0186(6) 0.0148(6) 0.0175(7) 0.0084(5) 0.0076(5) 0.0069(5) C55 0.0188(6) 0.0165(6) 0.0184(7) 0.0069(5) 0.0070(6) 0.0090(5) C56 0.0229(7) 0.0167(6) 0.0191(7) 0.0054(5) 0.0062(6) 0.0074(6) C57 0.0228(7) 0.0155(6) 0.0248(8) 0.0079(6) 0.0077(6) 0.0048(5) C58 0.0255(7) 0.0213(7) 0.0229(7) 0.0128(6) 0.0121(6) 0.0106(6) C59 0.0204(7) 0.0187(6) 0.0171(7) 0.0067(5) 0.0067(6) 0.0096(5) C60 0.0175(6) 0.0166(6) 0.0193(7) 0.0074(5) 0.0069(6) 0.0097(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 C6 1.3737(19) . ? C1 C2 1.4146(18) . ? C1 C5 1.4293(18) . ? C2 C9 1.3797(19) . ? C2 C3 1.4136(19) . ? C3 C12 1.3829(19) . ? C3 C4 1.4161(18) . ? C4 C15 1.3801(19) . ? C4 C5 1.4167(18) . ? C5 C18 1.3709(18) . ? C6 C7 1.4416(19) . ? C6 C20 1.4710(18) . ? C7 C8 1.382(2) . ? C7 H7A 0.9500 . ? C8 C9 1.4411(19) . ? C8 H8A 0.9500 . ? C9 C10 1.4440(19) . ? C10 C11 1.378(2) . ? C10 H10A 0.9500 . ? C11 C12 1.4433(19) . ? C11 H11A 0.9500 . ? C12 C13 1.4425(19) . ? C13 C14 1.3782(19) . ? C13 H13A 0.9500 . ? C14 C15 1.4469(18) . ? C14 H14A 0.9500 . ? C15 C16 1.4358(19) . ? C16 C17 1.3848(19) . ? C16 H16A 0.9500 . ? C17 C18 1.4396(18) . ? C17 H17A 0.9500 . ? C18 C19 1.4701(18) . ? C19 C44 1.4047(18) . ? C19 C20 1.4412(18) . ? C20 C41 1.4015(18) . ? C21 C26 1.3708(19) . ? C21 C22 1.4167(18) . ? C21 C25 1.4251(18) . ? C22 C29 1.3774(19) . ? C22 C23 1.4131(19) . ? C23 C32 1.3774(19) . ? C23 C24 1.4125(19) . ? C24 C35 1.3826(19) . ? C24 C25 1.4138(18) . ? C25 C38 1.3713(19) . ? C26 C27 1.4417(19) . ? C26 C40 1.4725(18) . ? C27 C28 1.3877(19) . ? C27 H27A 0.9500 . ? C28 C29 1.441(2) . ? C28 H28A 0.9500 . ? C29 C30 1.4472(19) . ? C30 C31 1.381(2) . ? C30 H30A 0.9500 . ? C31 C32 1.444(2) . ? C31 H31A 0.9500 . ? C32 C33 1.447(2) . ? C33 C34 1.376(2) . ? C33 H33A 0.9500 . ? C34 C35 1.4521(19) . ? C34 H34A 0.9500 . ? C35 C36 1.4390(19) . ? C36 C37 1.3866(19) . ? C36 H36A 0.9500 . ? C37 C38 1.4399(18) . ? C37 H37A 0.9500 . ? C38 C39 1.4724(18) . ? C39 C48 1.4032(18) . ? C39 C40 1.4432(18) . ? C40 C45 1.4020(18) . ? C41 C42 1.3898(19) . ? C41 H41A 0.9500 . ? C42 C43 1.4106(19) . ? C42 C55 1.4968(18) . ? C43 C44 1.3893(18) . ? C43 C49 1.4944(18) . ? C44 H44A 0.9500 . ? C45 C46 1.3876(18) . ? C45 H45A 0.9500 . ? C46 C47 1.4148(18) . ? C46 C60 1.4939(18) . ? C47 C48 1.3886(18) . ? C47 C54 1.4960(18) . ? C48 H48A 0.9500 . ? C49 C50 1.3955(19) . ? C49 C54 1.4019(19) . ? C50 C51 1.389(2) . ? C50 H50A 0.9500 . ? C51 C52 1.385(2) . ? C51 H51A 0.9500 . ? C52 C53 1.3891(19) . ? C52 H52A 0.9500 . ? C53 C54 1.4009(19) . ? C53 H53A 0.9500 . ? C55 C56 1.3951(19) . ? C55 C60 1.403(2) . ? C56 C57 1.3907(19) . ? C56 H56A 0.9500 . ? C57 C58 1.388(2) . ? C57 H57A 0.9500 . ? C58 C59 1.3885(19) . ? C58 H58A 0.9500 . ? C59 C60 1.4003(18) . ? C59 H59A 0.9500 . ? 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 C6 C1 C2 122.70(12) . . ? C6 C1 C5 123.22(12) . . ? C2 C1 C5 107.61(11) . . ? C9 C2 C3 122.45(12) . . ? C9 C2 C1 122.83(12) . . ? C3 C2 C1 108.27(11) . . ? C12 C3 C2 123.22(12) . . ? C12 C3 C4 122.06(12) . . ? C2 C3 C4 108.28(11) . . ? C15 C4 C3 122.61(12) . . ? C15 C4 C5 123.26(12) . . ? C3 C4 C5 107.90(11) . . ? C18 C5 C4 122.50(12) . . ? C18 C5 C1 123.59(12) . . ? C4 C5 C1 107.93(11) . . ? C1 C6 C7 114.62(12) . . ? C1 C6 C20 115.36(12) . . ? C7 C6 C20 128.63(12) . . ? C8 C7 C6 121.91(12) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C7 C8 C9 121.85(12) . . ? C7 C8 H8A 119.1 . . ? C9 C8 H8A 119.1 . . ? C2 C9 C8 114.38(12) . . ? C2 C9 C10 114.54(12) . . ? C8 C9 C10 129.44(12) . . ? C11 C10 C9 122.46(12) . . ? C11 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? C10 C11 C12 121.72(12) . . ? C10 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C3 C12 C13 115.14(12) . . ? C3 C12 C11 114.39(12) . . ? C13 C12 C11 129.34(12) . . ? C14 C13 C12 122.02(12) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C15 121.27(12) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C4 C15 C16 114.16(12) . . ? C4 C15 C14 115.25(12) . . ? C16 C15 C14 129.20(12) . . ? C17 C16 C15 121.91(12) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C16 C17 C18 122.17(12) . . ? C16 C17 H17A 118.9 . . ? C18 C17 H17A 118.9 . . ? C5 C18 C17 114.60(12) . . ? C5 C18 C19 115.34(12) . . ? C17 C18 C19 128.55(12) . . ? C44 C19 C20 117.92(12) . . ? C44 C19 C18 121.34(12) . . ? C20 C19 C18 120.54(12) . . ? C41 C20 C19 117.61(12) . . ? C41 C20 C6 121.33(12) . . ? C19 C20 C6 120.74(12) . . ? C26 C21 C22 122.68(12) . . ? C26 C21 C25 123.85(12) . . ? C22 C21 C25 107.91(11) . . ? C29 C22 C23 123.23(12) . . ? C29 C22 C21 123.37(12) . . ? C23 C22 C21 107.81(12) . . ? C32 C23 C24 123.06(13) . . ? C32 C23 C22 122.73(13) . . ? C24 C23 C22 108.42(11) . . ? C35 C24 C23 122.91(12) . . ? C35 C24 C25 123.23(12) . . ? C23 C24 C25 108.07(12) . . ? C38 C25 C24 122.98(12) . . ? C38 C25 C21 123.80(12) . . ? C24 C25 C21 107.76(11) . . ? C21 C26 C27 114.41(12) . . ? C21 C26 C40 114.88(12) . . ? C27 C26 C40 129.37(12) . . ? C28 C27 C26 122.18(12) . . ? C28 C27 H27A 118.9 . . ? C26 C27 H27A 118.9 . . ? C27 C28 C29 121.78(13) . . ? C27 C28 H28A 119.1 . . ? C29 C28 H28A 119.1 . . ? C22 C29 C28 114.08(12) . . ? C22 C29 C30 114.13(12) . . ? C28 C29 C30 130.40(13) . . ? C31 C30 C29 121.98(13) . . ? C31 C30 H30A 119.0 . . ? C29 C30 H30A 119.0 . . ? C30 C31 C32 122.00(13) . . ? C30 C31 H31A 119.0 . . ? C32 C31 H31A 119.0 . . ? C23 C32 C31 114.40(13) . . ? C23 C32 C33 114.48(13) . . ? C31 C32 C33 130.26(13) . . ? C34 C33 C32 122.03(13) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C33 C34 C35 122.11(13) . . ? C33 C34 H34A 118.9 . . ? C35 C34 H34A 118.9 . . ? C24 C35 C36 113.73(12) . . ? C24 C35 C34 114.23(12) . . ? C36 C35 C34 130.68(13) . . ? C37 C36 C35 122.14(12) . . ? C37 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C36 C37 C38 122.14(12) . . ? C36 C37 H37A 118.9 . . ? C38 C37 H37A 118.9 . . ? C25 C38 C37 114.24(12) . . ? C25 C38 C39 115.13(12) . . ? C37 C38 C39 128.93(12) . . ? C48 C39 C40 117.93(12) . . ? C48 C39 C38 120.99(12) . . ? C40 C39 C38 120.53(11) . . ? C45 C40 C39 117.76(11) . . ? C45 C40 C26 120.56(12) . . ? C39 C40 C26 121.08(11) . . ? C42 C41 C20 123.50(12) . . ? C42 C41 H41A 118.2 . . ? C20 C41 H41A 118.2 . . ? C41 C42 C43 118.74(12) . . ? C41 C42 C55 118.31(12) . . ? C43 C42 C55 122.95(12) . . ? C44 C43 C42 118.82(12) . . ? C44 C43 C49 119.09(12) . . ? C42 C43 C49 122.06(12) . . ? C43 C44 C19 123.20(12) . . ? C43 C44 H44A 118.4 . . ? C19 C44 H44A 118.4 . . ? C46 C45 C40 123.27(12) . . ? C46 C45 H45A 118.4 . . ? C40 C45 H45A 118.4 . . ? C45 C46 C47 118.86(12) . . ? C45 C46 C60 117.63(12) . . ? C47 C46 C60 123.50(11) . . ? C48 C47 C46 118.80(12) . . ? C48 C47 C54 119.03(11) . . ? C46 C47 C54 122.16(12) . . ? C47 C48 C39 123.13(12) . . ? C47 C48 H48A 118.4 . . ? C39 C48 H48A 118.4 . . ? C50 C49 C54 119.41(12) . . ? C50 C49 C43 119.62(12) . . ? C54 C49 C43 120.84(11) . . ? C51 C50 C49 120.93(13) . . ? C51 C50 H50A 119.5 . . ? C49 C50 H50A 119.5 . . ? C52 C51 C50 119.82(13) . . ? C52 C51 H51A 120.1 . . ? C50 C51 H51A 120.1 . . ? C51 C52 C53 119.85(13) . . ? C51 C52 H52A 120.1 . . ? C53 C52 H52A 120.1 . . ? C52 C53 C54 120.91(13) . . ? C52 C53 H53A 119.5 . . ? C54 C53 H53A 119.5 . . ? C53 C54 C49 119.04(12) . . ? C53 C54 C47 120.40(12) . . ? C49 C54 C47 120.41(12) . . ? C56 C55 C60 119.40(12) . . ? C56 C55 C42 118.33(12) . . ? C60 C55 C42 121.90(12) . . ? C57 C56 C55 120.99(13) . . ? C57 C56 H56A 119.5 . . ? C55 C56 H56A 119.5 . . ? C58 C57 C56 119.76(13) . . ? C58 C57 H57A 120.1 . . ? C56 C57 H57A 120.1 . . ? C57 C58 C59 119.74(12) . . ? C57 C58 H58A 120.1 . . ? C59 C58 H58A 120.1 . . ? C58 C59 C60 121.10(13) . . ? C58 C59 H59A 119.5 . . ? C60 C59 H59A 119.5 . . ? C59 C60 C55 119.00(12) . . ? C59 C60 C46 119.12(12) . . ? C55 C60 C46 121.43(12) . . ? _refine_diff_density_max 0.215 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.046 _shelxl_version_number 2013-4 _shelx_res_file ; TITL sad1 in P-1 CELL 1.54178 9.8507 14.1479 15.1646 105.607 102.809 110.367 ZERR 2.00 0.0003 0.0004 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H UNIT 120 56 L.S. 8 ACTA BOND $H FMAP 2 PLAN -10 OMIT 3 2 2 SIZE 0.030 0.070 0.140 TEMP -173.100 WGHT 0.051600 0.759000 FVAR 0.15328 C1 1 0.402187 0.278712 0.358604 11.00000 0.01557 0.01564 = 0.01460 0.00307 0.00339 0.00537 C2 1 0.320372 0.334485 0.325466 11.00000 0.01455 0.01898 = 0.01246 0.00371 0.00097 0.00533 C3 1 0.416627 0.411375 0.296529 11.00000 0.01720 0.02047 = 0.00957 0.00426 0.00230 0.00741 C4 1 0.558087 0.402662 0.310071 11.00000 0.01980 0.02036 = 0.01099 0.00568 0.00643 0.01038 C5 1 0.550346 0.321236 0.349027 11.00000 0.01742 0.01580 = 0.01304 0.00275 0.00536 0.00732 C6 1 0.375326 0.234683 0.426966 11.00000 0.01648 0.01572 = 0.01629 0.00430 0.00350 0.00419 C7 1 0.239804 0.232552 0.449420 11.00000 0.01758 0.02433 = 0.02044 0.01048 0.00699 0.00617 AFIX 43 H7A 2 0.205042 0.193080 0.487983 11.00000 -1.20000 AFIX 0 C8 1 0.158968 0.286277 0.416467 11.00000 0.01508 0.02867 = 0.02386 0.01124 0.00792 0.00898 AFIX 43 H8A 2 0.069532 0.281954 0.432355 11.00000 -1.20000 AFIX 0 C9 1 0.206561 0.348661 0.358686 11.00000 0.01509 0.02522 = 0.01619 0.00681 0.00300 0.00751 C10 1 0.179838 0.440024 0.348887 11.00000 0.01781 0.03044 = 0.01904 0.00894 0.00492 0.01376 AFIX 43 H10A 2 0.093589 0.448302 0.361603 11.00000 -1.20000 AFIX 0 C11 1 0.274743 0.515639 0.321787 11.00000 0.02177 0.02561 = 0.01568 0.00772 0.00394 0.01400 AFIX 43 H11A 2 0.252588 0.574647 0.316970 11.00000 -1.20000 AFIX 0 C12 1 0.406949 0.507547 0.300524 11.00000 0.02034 0.02295 = 0.01109 0.00634 0.00300 0.01106 C13 1 0.542917 0.591160 0.301048 11.00000 0.02491 0.02071 = 0.01654 0.00878 0.00644 0.01171 AFIX 43 H13A 2 0.537608 0.654199 0.292883 11.00000 -1.20000 AFIX 0 C14 1 0.680290 0.582402 0.313029 11.00000 0.02079 0.02053 = 0.01677 0.00870 0.00668 0.00782 AFIX 43 H14A 2 0.767029 0.639188 0.312642 11.00000 -1.20000 AFIX 0 C15 1 0.694955 0.488391 0.326187 11.00000 0.02015 0.02201 = 0.01377 0.00755 0.00837 0.01048 C16 1 0.830956 0.479022 0.372453 11.00000 0.01705 0.02217 = 0.01790 0.00825 0.00859 0.00754 AFIX 43 H16A 2 0.928870 0.528840 0.377049 11.00000 -1.20000 AFIX 0 C17 1 0.823537 0.399471 0.410571 11.00000 0.01671 0.02267 = 0.01626 0.00722 0.00688 0.01008 AFIX 43 H17A 2 0.916674 0.396589 0.440719 11.00000 -1.20000 AFIX 0 C18 1 0.679348 0.320994 0.406020 11.00000 0.01833 0.01653 = 0.01442 0.00417 0.00658 0.00916 C19 1 0.652049 0.259225 0.469358 11.00000 0.01865 0.01405 = 0.01390 0.00249 0.00505 0.00682 C20 1 0.503687 0.218375 0.480730 11.00000 0.01738 0.01434 = 0.01594 0.00317 0.00483 0.00579 C21 1 0.876379 0.679789 0.958306 11.00000 0.01955 0.01730 = 0.01043 0.00432 0.00410 0.00891 C22 1 0.823217 0.761247 0.961267 11.00000 0.02183 0.01586 = 0.01162 0.00220 0.00452 0.00833 C23 1 0.924926 0.841179 0.937742 11.00000 0.02061 0.01345 = 0.01460 0.00102 0.00284 0.00606 C24 1 1.043375 0.811460 0.922957 11.00000 0.01750 0.01364 = 0.01545 0.00242 0.00112 0.00422 C25 1 1.014041 0.711580 0.935374 11.00000 0.01568 0.01599 = 0.01195 0.00326 0.00027 0.00513 C26 1 0.779816 0.573825 0.938307 11.00000 0.01936 0.01885 = 0.01158 0.00581 0.00526 0.00888 C27 1 0.626236 0.556102 0.937549 11.00000 0.02154 0.01853 = 0.01530 0.00594 0.00837 0.00766 AFIX 43 H27A 2 0.557964 0.487156 0.933698 11.00000 -1.20000 AFIX 0 C28 1 0.574835 0.636426 0.942261 11.00000 0.01970 0.02303 = 0.01831 0.00570 0.00860 0.01016 AFIX 43 H28A 2 0.473284 0.621364 0.942817 11.00000 -1.20000 AFIX 0 C29 1 0.671344 0.742073 0.946332 11.00000 0.02254 0.02023 = 0.01546 0.00317 0.00694 0.01133 C30 1 0.630361 0.820997 0.917739 11.00000 0.02330 0.02241 = 0.02238 0.00448 0.00579 0.01359 AFIX 43 H30A 2 0.533064 0.820236 0.916279 11.00000 -1.20000 AFIX 0 C31 1 0.728445 0.897389 0.892512 11.00000 0.02848 0.01812 = 0.02291 0.00546 0.00447 0.01336 AFIX 43 H31A 2 0.695773 0.946702 0.873041 11.00000 -1.20000 AFIX 0 C32 1 0.879136 0.904581 0.894830 11.00000 0.02521 0.01434 = 0.01876 0.00300 0.00358 0.00831 C33 1 0.977927 0.952945 0.845935 11.00000 0.02999 0.01605 = 0.02472 0.00860 0.00639 0.00933 AFIX 43 H33A 2 0.961651 1.005398 0.822479 11.00000 -1.20000 AFIX 0 C34 1 1.094700 0.925300 0.832373 11.00000 0.02642 0.01765 = 0.02478 0.00900 0.00844 0.00553 AFIX 43 H34A 2 1.157052 0.959709 0.800302 11.00000 -1.20000 AFIX 0 C35 1 1.125681 0.845211 0.865513 11.00000 0.01927 0.01561 = 0.02189 0.00571 0.00514 0.00425 C36 1 1.201787 0.779351 0.833465 11.00000 0.01845 0.01928 = 0.02236 0.00785 0.00810 0.00420 AFIX 43 H36A 2 1.273564 0.803497 0.802501 11.00000 -1.20000 AFIX 0 C37 1 1.173761 0.681787 0.846308 11.00000 0.01600 0.01769 = 0.01913 0.00455 0.00448 0.00613 AFIX 43 H37A 2 1.227190 0.641368 0.824034 11.00000 -1.20000 AFIX 0 C38 1 1.066303 0.639749 0.892312 11.00000 0.01479 0.01744 = 0.01419 0.00568 0.00170 0.00596 C39 1 0.978955 0.526123 0.880294 11.00000 0.01637 0.01663 = 0.01179 0.00537 0.00210 0.00658 C40 1 0.837843 0.493865 0.901638 11.00000 0.01795 0.01744 = 0.01108 0.00584 0.00369 0.00798 C41 1 0.491206 0.172959 0.551760 11.00000 0.01751 0.01464 = 0.01834 0.00430 0.00640 0.00489 AFIX 43 H41A 2 0.393649 0.145214 0.559414 11.00000 -1.20000 AFIX 0 C42 1 0.613926 0.166346 0.611595 11.00000 0.02078 0.01236 = 0.01529 0.00309 0.00577 0.00609 C43 1 0.756832 0.201146 0.596881 11.00000 0.01954 0.01253 = 0.01530 0.00266 0.00460 0.00729 C44 1 0.771989 0.245746 0.526415 11.00000 0.01704 0.01456 = 0.01671 0.00394 0.00648 0.00655 AFIX 43 H44A 2 0.868147 0.268220 0.516329 11.00000 -1.20000 AFIX 0 C45 1 0.746722 0.382165 0.873553 11.00000 0.01774 0.01815 = 0.01430 0.00724 0.00598 0.00749 AFIX 43 H45A 2 0.655959 0.360257 0.889830 11.00000 -1.20000 AFIX 0 C46 1 0.782505 0.302015 0.823165 11.00000 0.01886 0.01679 = 0.01211 0.00665 0.00349 0.00782 C47 1 0.923368 0.333686 0.805163 11.00000 0.01894 0.01787 = 0.01211 0.00685 0.00364 0.00959 C48 1 1.018492 0.443970 0.835689 11.00000 0.01483 0.01899 = 0.01527 0.00742 0.00411 0.00757 AFIX 43 H48A 2 1.114934 0.464794 0.825909 11.00000 -1.20000 AFIX 0 C49 1 0.890590 0.188510 0.652587 11.00000 0.01961 0.01562 = 0.01886 0.00806 0.00781 0.00771 C50 1 0.942195 0.117298 0.603553 11.00000 0.02746 0.02223 = 0.01814 0.00546 0.00791 0.01302 AFIX 43 H50A 2 0.888282 0.074468 0.535863 11.00000 -1.20000 AFIX 0 C51 1 1.071277 0.108153 0.652320 11.00000 0.03114 0.02476 = 0.02631 0.00949 0.01353 0.01858 AFIX 43 H51A 2 1.103746 0.058098 0.618441 11.00000 -1.20000 AFIX 0 C52 1 1.152529 0.172214 0.750480 11.00000 0.02395 0.02627 = 0.02549 0.01455 0.01033 0.01581 AFIX 43 H52A 2 1.241591 0.166828 0.783897 11.00000 -1.20000 AFIX 0 C53 1 1.103488 0.244350 0.799944 11.00000 0.02099 0.01985 = 0.01781 0.00889 0.00704 0.00955 AFIX 43 H53A 2 1.160454 0.288884 0.867021 11.00000 -1.20000 AFIX 0 C54 1 0.971178 0.252332 0.752276 11.00000 0.01860 0.01481 = 0.01754 0.00842 0.00760 0.00686 C55 1 0.588003 0.122097 0.688729 11.00000 0.01878 0.01652 = 0.01838 0.00693 0.00700 0.00902 C56 1 0.469980 0.018094 0.659999 11.00000 0.02289 0.01667 = 0.01906 0.00539 0.00623 0.00736 AFIX 43 H56A 2 0.417330 -0.025735 0.592410 11.00000 -1.20000 AFIX 0 C57 1 0.428246 -0.022382 0.728818 11.00000 0.02282 0.01552 = 0.02481 0.00793 0.00769 0.00481 AFIX 43 H57A 2 0.348065 -0.093513 0.708255 11.00000 -1.20000 AFIX 0 C58 1 0.504187 0.041541 0.827679 11.00000 0.02549 0.02127 = 0.02295 0.01281 0.01214 0.01062 AFIX 43 H58A 2 0.475021 0.014789 0.874996 11.00000 -1.20000 AFIX 0 C59 1 0.622931 0.144724 0.857124 11.00000 0.02038 0.01865 = 0.01709 0.00674 0.00668 0.00961 AFIX 43 H59A 2 0.675167 0.187940 0.924863 11.00000 -1.20000 AFIX 0 C60 1 0.666974 0.186148 0.788629 11.00000 0.01750 0.01665 = 0.01934 0.00743 0.00687 0.00974 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM sad1 in P-1 REM R1 = 0.0374 for 5763 Fo > 4sig(Fo) and 0.0424 for all 6486 data REM 541 parameters refined using 0 restraints END WGHT 0.0516 0.7591 REM Highest difference peak 0.215, deepest hole -0.203, 1-sigma level 0.046 Q1 1 0.6083 0.1358 0.6487 11.00000 0.05 0.20 Q2 1 1.1827 0.6181 0.7854 11.00000 0.05 0.19 Q3 1 0.9354 0.5637 0.4088 11.00000 0.05 0.18 Q4 1 0.3659 0.2233 0.3641 11.00000 0.05 0.18 Q5 1 0.6582 0.2639 0.4138 11.00000 0.05 0.16 Q6 1 0.5589 0.3590 0.3214 11.00000 0.05 0.16 Q7 1 0.2369 0.3176 0.3114 11.00000 0.05 0.16 Q8 1 1.0394 0.5836 0.8966 11.00000 0.05 0.16 Q9 1 0.9005 0.9803 0.7935 11.00000 0.05 0.16 Q10 1 0.3409 0.3518 0.2851 11.00000 0.05 0.16 ; _database_code_depnum_ccdc_archive 'CCDC 973696'