# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_d1203 #TrackingRef '19658_web_deposit_cif_file_0_MarkS.Taylor_1366401291.2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 B2 O3' _chemical_formula_sum 'C24 H16 B2 O3' _chemical_formula_weight 373.99 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' B B 0.0090 0.0039 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4797(6) _cell_length_b 45.490(3) _cell_length_c 21.7415(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.764(3) _cell_angle_gamma 90.00 _cell_volume 9364.8(10) _cell_formula_units_Z 20 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 9859 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 65.43 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3880 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6604 _exptl_absorpt_correction_T_max 0.7527 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Cu microsource' _diffrn_radiation_monochromator 'multi layer optics' _diffrn_measurement_device_type 'Bruker APEX DUO ' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60123 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 66.02 _reflns_number_total 15900 _reflns_number_gt 12861 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+6.7596P] 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 15900 _refine_ls_number_parameters 1306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O -0.05443(18) 0.24323(4) 0.40388(8) 0.0553(5) Uani 1 1 d . . . O2A O -0.23603(15) 0.29470(4) 0.25865(6) 0.0397(4) Uani 1 1 d . . . O3A O 0.26629(14) 0.18459(3) 0.46871(6) 0.0303(3) Uani 1 1 d . . . C1A C -0.0290(2) 0.26816(4) 0.29935(9) 0.0287(4) Uani 1 1 d . . . C2A C 0.1131(2) 0.26121(5) 0.28941(10) 0.0365(5) Uani 1 1 d . . . H2AA H 0.1643 0.2494 0.3188 0.044 Uiso 1 1 calc R . . C3A C 0.1798(2) 0.27097(6) 0.23851(11) 0.0479(6) Uani 1 1 d . . . H3AA H 0.2751 0.2657 0.2327 0.057 Uiso 1 1 calc R . . C4A C 0.1074(3) 0.28859(7) 0.19569(12) 0.0574(7) Uani 1 1 d . . . H4AA H 0.1538 0.2955 0.1607 0.069 Uiso 1 1 calc R . . C5A C -0.0313(3) 0.29616(7) 0.20351(11) 0.0526(7) Uani 1 1 d . . . H5AA H -0.0809 0.3083 0.1742 0.063 Uiso 1 1 calc R . . C6A C -0.0978(2) 0.28580(5) 0.25502(9) 0.0330(5) Uani 1 1 d . . . C7A C -0.3165(2) 0.28649(5) 0.30703(9) 0.0286(4) Uani 1 1 d . . . C8A C -0.4546(2) 0.29699(5) 0.30338(10) 0.0395(5) Uani 1 1 d . . . H8AA H -0.4871 0.3088 0.2696 0.047 Uiso 1 1 calc R . . C9A C -0.5431(2) 0.28999(5) 0.34927(10) 0.0379(5) Uani 1 1 d . . . H9AA H -0.6372 0.2972 0.3472 0.045 Uiso 1 1 calc R . . C10A C -0.4972(2) 0.27259(5) 0.39856(10) 0.0354(5) Uani 1 1 d . . . H10A H -0.5596 0.2676 0.4298 0.042 Uiso 1 1 calc R . . C11A C -0.3599(2) 0.26258(4) 0.40160(9) 0.0322(5) Uani 1 1 d . . . H11A H -0.3281 0.2509 0.4357 0.039 Uiso 1 1 calc R . . C12A C -0.2657(2) 0.26921(4) 0.35575(9) 0.0257(4) Uani 1 1 d . . . C13A C 0.0579(2) 0.19240(5) 0.40095(9) 0.0331(5) Uani 1 1 d . . . C14A C -0.0369(2) 0.17933(6) 0.35754(10) 0.0423(6) Uani 1 1 d . . . H14A H -0.1118 0.1908 0.3397 0.051 Uiso 1 1 calc R . . C15A C -0.0246(2) 0.15065(6) 0.34020(10) 0.0481(6) Uani 1 1 d . . . H15A H -0.0903 0.1424 0.3106 0.058 Uiso 1 1 calc R . . C16A C 0.0849(2) 0.13336(5) 0.36618(10) 0.0428(5) Uani 1 1 d . . . H16A H 0.0935 0.1134 0.3542 0.051 Uiso 1 1 calc R . . C17A C 0.1810(2) 0.14528(5) 0.40944(10) 0.0341(5) Uani 1 1 d . . . H17A H 0.2554 0.1337 0.4274 0.041 Uiso 1 1 calc R . . C18A C 0.1660(2) 0.17452(4) 0.42593(9) 0.0287(4) Uani 1 1 d . . . C19A C 0.2640(2) 0.21284(4) 0.49151(9) 0.0304(4) Uani 1 1 d . . . C20A C 0.3712(2) 0.21907(5) 0.53556(10) 0.0378(5) Uani 1 1 d . . . H20A H 0.4384 0.2044 0.5476 0.045 Uiso 1 1 calc R . . C21A C 0.3790(3) 0.24659(5) 0.56141(12) 0.0477(6) Uani 1 1 d . . . H21A H 0.4523 0.2510 0.5913 0.057 Uiso 1 1 calc R . . C22A C 0.2809(3) 0.26784(6) 0.54413(12) 0.0515(6) Uani 1 1 d . . . H22A H 0.2865 0.2868 0.5622 0.062 Uiso 1 1 calc R . . C23A C 0.1751(3) 0.26148(5) 0.50074(12) 0.0470(6) Uani 1 1 d . . . H23A H 0.1082 0.2763 0.4894 0.056 Uiso 1 1 calc R . . C24A C 0.1625(2) 0.23349(5) 0.47235(10) 0.0338(5) Uani 1 1 d . . . B1A B -0.1114(2) 0.25868(5) 0.35536(11) 0.0298(5) Uani 1 1 d . . . B2A B 0.0501(3) 0.22431(6) 0.42375(12) 0.0371(6) Uani 1 1 d . . . O1B O 0.58647(16) 0.13160(4) 0.11890(8) 0.0508(4) Uani 1 1 d . . . O2B O 0.73237(14) 0.19996(3) 0.23774(6) 0.0290(3) Uani 1 1 d . . . O3B O 0.24213(14) 0.08528(3) 0.03299(6) 0.0328(3) Uani 1 1 d . . . C1B C 0.5376(2) 0.16762(4) 0.20560(9) 0.0297(4) Uani 1 1 d . . . C2B C 0.3967(2) 0.15972(5) 0.21655(11) 0.0382(5) Uani 1 1 d . . . H2BA H 0.3519 0.1449 0.1919 0.046 Uiso 1 1 calc R . . C3B C 0.3227(2) 0.17296(6) 0.26195(11) 0.0445(6) Uani 1 1 d . . . H3BA H 0.2282 0.1672 0.2684 0.053 Uiso 1 1 calc R . . C4B C 0.3866(2) 0.19465(6) 0.29816(11) 0.0445(6) Uani 1 1 d . . . H4BA H 0.3354 0.2037 0.3296 0.053 Uiso 1 1 calc R . . C5B C 0.5232(2) 0.20327(5) 0.28928(10) 0.0367(5) Uani 1 1 d . . . H5BA H 0.5667 0.2182 0.3142 0.044 Uiso 1 1 calc R . . C6B C 0.5969(2) 0.18968(4) 0.24304(9) 0.0279(4) Uani 1 1 d . . . C7B C 0.8196(2) 0.18895(4) 0.19431(8) 0.0258(4) Uani 1 1 d . . . C8B C 0.9532(2) 0.20180(5) 0.19471(9) 0.0310(4) Uani 1 1 d . . . H8BA H 0.9784 0.2170 0.2232 0.037 Uiso 1 1 calc R . . C9B C 1.0479(2) 0.19221(5) 0.15324(10) 0.0355(5) Uani 1 1 d . . . H9BA H 1.1393 0.2008 0.1533 0.043 Uiso 1 1 calc R . . C10B C 1.0119(2) 0.17015(5) 0.11138(10) 0.0390(5) Uani 1 1 d . . . H10B H 1.0782 0.1636 0.0830 0.047 Uiso 1 1 calc R . . C11B C 0.8795(2) 0.15782(5) 0.11126(10) 0.0363(5) Uani 1 1 d . . . H11B H 0.8549 0.1429 0.0821 0.044 Uiso 1 1 calc R . . C12B C 0.7791(2) 0.16675(4) 0.15336(9) 0.0278(4) Uani 1 1 d . . . C13B C 0.3682(2) 0.13177(5) 0.04561(10) 0.0333(5) Uani 1 1 d . . . C14B C 0.3744(3) 0.16122(5) 0.02676(12) 0.0478(6) Uani 1 1 d . . . H14B H 0.4472 0.1735 0.0439 0.057 Uiso 1 1 calc R . . C15B C 0.2795(3) 0.17266(6) -0.01518(13) 0.0600(8) Uani 1 1 d . . . H15B H 0.2864 0.1927 -0.0271 0.072 Uiso 1 1 calc R . . C16B C 0.1714(3) 0.15502(7) -0.04089(12) 0.0629(9) Uani 1 1 d . . . H16B H 0.1055 0.1631 -0.0705 0.076 Uiso 1 1 calc R . . C17B C 0.1591(3) 0.12569(6) -0.02369(10) 0.0463(6) Uani 1 1 d . . . H17B H 0.0850 0.1137 -0.0406 0.056 Uiso 1 1 calc R . . C18B C 0.2592(2) 0.11453(5) 0.01920(9) 0.0312(4) Uani 1 1 d . . . C19B C 0.3363(2) 0.07066(4) 0.07219(9) 0.0290(4) Uani 1 1 d . . . C20B C 0.3078(2) 0.04087(5) 0.07978(12) 0.0432(6) Uani 1 1 d . . . H20B H 0.2293 0.0319 0.0584 0.052 Uiso 1 1 calc R . . C21B C 0.3954(3) 0.02473(6) 0.11883(13) 0.0534(7) Uani 1 1 d . . . H21B H 0.3771 0.0044 0.1243 0.064 Uiso 1 1 calc R . . C22B C 0.5093(3) 0.03741(6) 0.15031(12) 0.0527(7) Uani 1 1 d . . . H22B H 0.5686 0.0259 0.1773 0.063 Uiso 1 1 calc R . . C23B C 0.5366(2) 0.06683(6) 0.14238(10) 0.0412(5) Uani 1 1 d . . . H23B H 0.6158 0.0754 0.1640 0.049 Uiso 1 1 calc R . . C24B C 0.4506(2) 0.08449(5) 0.10315(9) 0.0293(4) Uani 1 1 d . . . B1B B 0.6294(2) 0.15404(5) 0.15635(11) 0.0322(5) Uani 1 1 d . . . B2B B 0.4743(2) 0.11723(5) 0.09153(11) 0.0319(5) Uani 1 1 d . . . O1C O 1.04514(15) 0.15428(3) 0.58613(6) 0.0349(3) Uani 1 1 d . . . O2C O 1.24692(16) 0.11553(4) 0.74442(7) 0.0444(4) Uani 1 1 d . . . O3C O 0.73218(14) 0.21435(3) 0.51919(6) 0.0295(3) Uani 1 1 d . . . C1C C 1.2664(2) 0.13499(4) 0.64058(9) 0.0279(4) Uani 1 1 d . . . C2C C 1.3582(2) 0.13982(5) 0.59245(9) 0.0318(4) Uani 1 1 d . . . H2CA H 1.3233 0.1494 0.5559 0.038 Uiso 1 1 calc R . . C3C C 1.4974(2) 0.13103(5) 0.59715(10) 0.0396(5) Uani 1 1 d . . . H3CA H 1.5578 0.1346 0.5643 0.048 Uiso 1 1 calc R . . C4C C 1.5488(2) 0.11691(6) 0.65051(11) 0.0441(6) Uani 1 1 d . . . H4CA H 1.6443 0.1105 0.6536 0.053 Uiso 1 1 calc R . . C5C C 1.4637(2) 0.11209(6) 0.69866(11) 0.0436(6) Uani 1 1 d . . . H5CA H 1.4998 0.1026 0.7350 0.052 Uiso 1 1 calc R . . C6C C 1.3237(2) 0.12127(5) 0.69372(9) 0.0332(5) Uani 1 1 d . . . C7C C 1.1071(2) 0.12356(5) 0.74681(10) 0.0380(5) Uani 1 1 d . . . C8C C 1.0453(3) 0.11606(7) 0.80150(11) 0.0555(7) Uani 1 1 d . . . H8CA H 1.0987 0.1064 0.8336 0.067 Uiso 1 1 calc R . . C9C C 0.9050(3) 0.12297(7) 0.80828(12) 0.0627(8) Uani 1 1 d . . . H9CA H 0.8614 0.1179 0.8452 0.075 Uiso 1 1 calc R . . C10C C 0.8271(3) 0.13732(7) 0.76145(13) 0.0554(7) Uani 1 1 d . . . H10C H 0.7312 0.1423 0.7667 0.066 Uiso 1 1 calc R . . C11C C 0.8894(2) 0.14425(5) 0.70751(11) 0.0410(5) Uani 1 1 d . . . H11C H 0.8348 0.1538 0.6756 0.049 Uiso 1 1 calc R . . C12C C 1.0325(2) 0.13760(5) 0.69825(10) 0.0327(5) Uani 1 1 d . . . C13C C 0.8319(2) 0.16500(4) 0.51471(8) 0.0254(4) Uani 1 1 d . . . C14C C 0.8194(2) 0.13727(4) 0.48719(9) 0.0295(4) Uani 1 1 d . . . H14C H 0.8856 0.1224 0.4989 0.035 Uiso 1 1 calc R . . C15C C 0.7134(2) 0.13106(5) 0.44349(10) 0.0352(5) Uani 1 1 d . . . H15C H 0.7064 0.1120 0.4257 0.042 Uiso 1 1 calc R . . C16C C 0.6167(2) 0.15282(5) 0.42563(10) 0.0364(5) Uani 1 1 d . . . H16C H 0.5435 0.1485 0.3956 0.044 Uiso 1 1 calc R . . C17C C 0.6259(2) 0.18046(5) 0.45099(9) 0.0329(5) Uani 1 1 d . . . H17C H 0.5607 0.1954 0.4383 0.039 Uiso 1 1 calc R . . C18C C 0.7329(2) 0.18619(4) 0.49559(9) 0.0265(4) Uani 1 1 d . . . C19C C 0.8327(2) 0.22377(4) 0.56259(9) 0.0271(4) Uani 1 1 d . . . C20C C 0.8199(2) 0.25300(5) 0.58005(10) 0.0362(5) Uani 1 1 d . . . H20C H 0.7470 0.2650 0.5622 0.043 Uiso 1 1 calc R . . C21C C 0.9153(2) 0.26415(5) 0.62385(11) 0.0423(6) Uani 1 1 d . . . H21C H 0.9073 0.2840 0.6366 0.051 Uiso 1 1 calc R . . C22C C 1.0230(2) 0.24678(5) 0.64962(11) 0.0411(5) Uani 1 1 d . . . H22C H 1.0887 0.2548 0.6794 0.049 Uiso 1 1 calc R . . C23C C 1.0340(2) 0.21807(5) 0.63192(10) 0.0346(5) Uani 1 1 d . . . H23C H 1.1076 0.2063 0.6500 0.042 Uiso 1 1 calc R . . C24C C 0.93879(19) 0.20553(4) 0.58756(9) 0.0269(4) Uani 1 1 d . . . B1C B 1.1094(2) 0.14372(5) 0.63846(10) 0.0279(5) Uani 1 1 d . . . B2C B 0.9446(2) 0.17361(5) 0.56482(10) 0.0263(5) Uani 1 1 d . . . O1D O 1.08197(16) -0.02823(3) 0.61256(8) 0.0468(4) Uani 1 1 d . . . O2D O 1.22712(16) -0.09304(4) 0.74024(7) 0.0426(4) Uani 1 1 d . . . O3D O 0.72968(15) 0.01315(3) 0.52072(7) 0.0386(4) Uani 1 1 d . . . C1D C 1.0339(2) -0.06089(5) 0.70497(10) 0.0351(5) Uani 1 1 d . . . C2D C 0.8933(2) -0.05240(6) 0.71516(11) 0.0452(6) Uani 1 1 d . . . H2DA H 0.8493 -0.0379 0.6893 0.054 Uiso 1 1 calc R . . C3D C 0.8184(3) -0.06457(7) 0.76171(13) 0.0603(8) Uani 1 1 d . . . H3DA H 0.7248 -0.0582 0.7682 0.072 Uiso 1 1 calc R . . C4D C 0.8808(3) -0.08623(8) 0.79912(13) 0.0686(9) Uani 1 1 d . . . H4DA H 0.8286 -0.0949 0.8306 0.082 Uiso 1 1 calc R . . C5D C 1.0171(3) -0.09513(7) 0.79105(11) 0.0608(8) Uani 1 1 d . . . H5DA H 1.0597 -0.1098 0.8168 0.073 Uiso 1 1 calc R . . C6D C 1.0919(2) -0.08221(6) 0.74438(10) 0.0392(5) Uani 1 1 d . . . C7D C 1.3162(2) -0.08259(5) 0.69696(9) 0.0311(4) Uani 1 1 d . . . C8D C 1.4495(2) -0.09553(5) 0.69909(10) 0.0392(5) Uani 1 1 d . . . H8DA H 1.4733 -0.1102 0.7288 0.047 Uiso 1 1 calc R . . C9D C 1.5462(2) -0.08678(5) 0.65782(10) 0.0390(5) Uani 1 1 d . . . H9DA H 1.6374 -0.0955 0.6592 0.047 Uiso 1 1 calc R . . C10D C 1.5125(2) -0.06536(5) 0.61408(10) 0.0390(5) Uani 1 1 d . . . H10D H 1.5799 -0.0594 0.5856 0.047 Uiso 1 1 calc R . . C11D C 1.3796(2) -0.05281(5) 0.61243(10) 0.0341(5) Uani 1 1 d . . . H11D H 1.3567 -0.0382 0.5824 0.041 Uiso 1 1 calc R . . C12D C 1.2771(2) -0.06100(4) 0.65393(9) 0.0286(4) Uani 1 1 d . . . C13D C 0.9363(2) 0.01726(4) 0.59092(10) 0.0318(5) Uani 1 1 d . . . C14D C 1.0189(2) 0.03613(5) 0.62880(11) 0.0397(5) Uani 1 1 d . . . H14D H 1.0984 0.0284 0.6518 0.048 Uiso 1 1 calc R . . C15D C 0.9875(3) 0.06549(5) 0.63341(11) 0.0455(6) Uani 1 1 d . . . H15D H 1.0440 0.0779 0.6597 0.055 Uiso 1 1 calc R . . C16D C 0.8728(3) 0.07691(5) 0.59941(12) 0.0446(6) Uani 1 1 d . . . H16D H 0.8519 0.0973 0.6024 0.053 Uiso 1 1 calc R . . C17D C 0.7885(2) 0.05930(5) 0.56142(11) 0.0415(5) Uani 1 1 d . . . H17D H 0.7104 0.0673 0.5380 0.050 Uiso 1 1 calc R . . C18D C 0.8210(2) 0.02947(4) 0.55823(10) 0.0327(5) Uani 1 1 d . . . C19D C 0.7511(2) -0.01655(5) 0.51156(10) 0.0358(5) Uani 1 1 d . . . C20D C 0.6528(3) -0.02971(6) 0.47061(11) 0.0480(6) Uani 1 1 d . . . H20D H 0.5771 -0.0186 0.4521 0.058 Uiso 1 1 calc R . . C21D C 0.6680(3) -0.05928(6) 0.45761(12) 0.0556(7) Uani 1 1 d . . . H21D H 0.6030 -0.0685 0.4292 0.067 Uiso 1 1 calc R . . C22D C 0.7771(3) -0.07561(6) 0.48567(12) 0.0523(6) Uani 1 1 d . . . H22D H 0.7859 -0.0960 0.4768 0.063 Uiso 1 1 calc R . . C23D C 0.8720(3) -0.06226(5) 0.52615(11) 0.0440(6) Uani 1 1 d . . . H23D H 0.9462 -0.0736 0.5451 0.053 Uiso 1 1 calc R . . C24D C 0.8624(2) -0.03224(5) 0.54024(10) 0.0343(5) Uani 1 1 d . . . B1D B 1.1262(2) -0.04865(5) 0.65424(11) 0.0313(5) Uani 1 1 d . . . B2D B 0.9660(3) -0.01555(5) 0.58359(12) 0.0343(5) Uani 1 1 d . . . O1E O 0.44356(19) 0.06304(5) 0.90811(8) 0.0657(6) Uani 1 1 d . . . O2E O 0.78084(14) 0.11376(3) 0.98638(6) 0.0324(3) Uani 1 1 d . . . O3E O 0.26008(17) 0.01771(4) 0.75482(7) 0.0462(4) Uani 1 1 d . . . C1E C 0.5732(2) 0.11173(5) 0.91671(9) 0.0348(5) Uani 1 1 d . . . C2E C 0.4837(3) 0.12767(7) 0.87537(11) 0.0536(7) Uani 1 1 d . . . H2EA H 0.4065 0.1179 0.8547 0.064 Uiso 1 1 calc R . . C3E C 0.5051(3) 0.15667(8) 0.86444(13) 0.0679(9) Uani 1 1 d . . . H3EA H 0.4440 0.1670 0.8360 0.081 Uiso 1 1 calc R . . C4E C 0.6161(3) 0.17117(6) 0.89480(14) 0.0643(9) Uani 1 1 d . . . H4EA H 0.6300 0.1915 0.8872 0.077 Uiso 1 1 calc R . . C5E C 0.7070(3) 0.15669(5) 0.93599(12) 0.0464(6) Uani 1 1 d . . . H5EA H 0.7828 0.1668 0.9569 0.056 Uiso 1 1 calc R . . C6E C 0.6848(2) 0.12690(4) 0.94613(9) 0.0300(4) Uani 1 1 d . . . C7E C 0.7698(2) 0.08468(4) 1.00239(9) 0.0309(4) Uani 1 1 d . . . C8E C 0.8749(3) 0.07524(6) 1.04494(11) 0.0480(6) Uani 1 1 d . . . H8EA H 0.9462 0.0885 1.0598 0.058 Uiso 1 1 calc R . . C9E C 0.8746(3) 0.04703(7) 1.06488(14) 0.0649(8) Uani 1 1 d . . . H9EA H 0.9453 0.0405 1.0942 0.078 Uiso 1 1 calc R . . C10E C 0.7715(4) 0.02770(6) 1.04265(16) 0.0717(10) Uani 1 1 d . . . H10E H 0.7723 0.0079 1.0565 0.086 Uiso 1 1 calc R . . C11E C 0.6670(3) 0.03707(5) 1.00033(14) 0.0572(8) Uani 1 1 d . . . H11E H 0.5966 0.0236 0.9857 0.069 Uiso 1 1 calc R . . C12E C 0.6635(2) 0.06632(4) 0.97854(10) 0.0345(5) Uani 1 1 d . . . C13E C 0.4679(2) 0.04287(5) 0.79947(10) 0.0322(5) Uani 1 1 d . . . C14E C 0.6101(2) 0.05031(6) 0.79062(12) 0.0454(6) Uani 1 1 d . . . H14E H 0.6615 0.0611 0.8218 0.055 Uiso 1 1 calc R . . C15E C 0.6761(3) 0.04247(7) 0.73836(14) 0.0622(8) Uani 1 1 d . . . H15E H 0.7715 0.0480 0.7333 0.075 Uiso 1 1 calc R . . C16E C 0.6031(3) 0.02652(8) 0.69318(14) 0.0750(10) Uani 1 1 d . . . H16E H 0.6495 0.0209 0.6572 0.090 Uiso 1 1 calc R . . C17E C 0.4640(3) 0.01856(8) 0.69935(12) 0.0665(8) Uani 1 1 d . . . H17E H 0.4142 0.0076 0.6681 0.080 Uiso 1 1 calc R . . C18E C 0.3982(2) 0.02705(5) 0.75252(10) 0.0393(5) Uani 1 1 d . . . C19E C 0.1792(2) 0.02451(5) 0.80379(9) 0.0328(5) Uani 1 1 d . . . C20E C 0.0416(2) 0.01372(6) 0.79913(11) 0.0469(6) Uani 1 1 d . . . H20E H 0.0100 0.0026 0.7642 0.056 Uiso 1 1 calc R . . C21E C -0.0474(2) 0.01930(6) 0.84534(12) 0.0481(6) Uani 1 1 d . . . H21E H -0.1413 0.0120 0.8423 0.058 Uiso 1 1 calc R . . C22E C -0.0025(2) 0.03551(5) 0.89644(11) 0.0429(5) Uani 1 1 d . . . H22E H -0.0652 0.0395 0.9282 0.051 Uiso 1 1 calc R . . C23E C 0.1340(2) 0.04584(5) 0.90080(10) 0.0375(5) Uani 1 1 d . . . H23E H 0.1645 0.0569 0.9361 0.045 Uiso 1 1 calc R . . C24E C 0.2300(2) 0.04052(4) 0.85456(9) 0.0281(4) Uani 1 1 d . . . B1E B 0.5545(3) 0.07924(6) 0.93191(11) 0.0381(6) Uani 1 1 d . . . B2E B 0.3849(3) 0.05026(5) 0.85685(11) 0.0334(5) 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 O1A 0.0432(9) 0.0678(12) 0.0555(11) 0.0275(9) 0.0079(8) 0.0288(9) O2A 0.0269(7) 0.0637(10) 0.0287(8) 0.0119(7) 0.0040(6) 0.0099(7) O3A 0.0265(7) 0.0276(7) 0.0362(8) 0.0003(6) -0.0036(6) 0.0049(6) C1A 0.0232(9) 0.0294(10) 0.0331(11) -0.0122(8) -0.0018(8) -0.0003(8) C2A 0.0235(10) 0.0423(12) 0.0436(12) -0.0153(10) 0.0000(9) 0.0016(9) C3A 0.0256(11) 0.0680(17) 0.0509(14) -0.0230(13) 0.0088(10) -0.0049(11) C4A 0.0390(14) 0.093(2) 0.0414(14) -0.0029(14) 0.0158(11) -0.0057(14) C5A 0.0404(13) 0.0823(19) 0.0358(13) 0.0100(12) 0.0086(10) 0.0025(13) C6A 0.0228(10) 0.0482(13) 0.0282(10) -0.0033(9) 0.0025(8) 0.0010(9) C7A 0.0228(9) 0.0400(11) 0.0232(10) -0.0017(8) 0.0013(8) 0.0009(8) C8A 0.0286(11) 0.0587(15) 0.0308(11) 0.0057(10) -0.0017(9) 0.0099(10) C9A 0.0216(10) 0.0531(14) 0.0391(12) -0.0061(10) 0.0015(9) 0.0055(9) C10A 0.0311(11) 0.0415(12) 0.0343(11) -0.0042(9) 0.0097(9) -0.0066(9) C11A 0.0357(11) 0.0296(11) 0.0316(11) 0.0030(8) 0.0037(9) 0.0007(9) C12A 0.0262(10) 0.0230(9) 0.0278(10) -0.0025(8) -0.0006(8) -0.0011(8) C13A 0.0236(10) 0.0474(13) 0.0286(10) 0.0106(9) 0.0045(8) 0.0031(9) C14A 0.0262(11) 0.0676(17) 0.0331(12) 0.0087(11) -0.0004(9) 0.0005(10) C15A 0.0315(12) 0.0822(19) 0.0306(12) -0.0040(12) -0.0004(9) -0.0146(12) C16A 0.0441(13) 0.0475(14) 0.0373(12) -0.0065(10) 0.0069(10) -0.0127(11) C17A 0.0311(11) 0.0369(12) 0.0343(11) 0.0019(9) 0.0038(9) -0.0003(9) C18A 0.0243(10) 0.0364(11) 0.0254(10) 0.0062(8) 0.0026(8) -0.0020(8) C19A 0.0287(10) 0.0280(10) 0.0352(11) 0.0022(8) 0.0086(8) 0.0009(8) C20A 0.0322(11) 0.0432(13) 0.0384(12) -0.0053(10) 0.0049(9) -0.0010(9) C21A 0.0436(13) 0.0471(14) 0.0531(15) -0.0140(11) 0.0109(11) -0.0072(11) C22A 0.0574(16) 0.0394(13) 0.0597(16) -0.0156(12) 0.0242(13) -0.0109(12) C23A 0.0491(14) 0.0295(12) 0.0650(16) 0.0082(11) 0.0299(12) 0.0094(10) C24A 0.0308(11) 0.0305(11) 0.0414(12) 0.0086(9) 0.0147(9) 0.0042(9) B1A 0.0301(12) 0.0252(11) 0.0337(12) -0.0012(9) -0.0021(9) 0.0042(9) B2A 0.0287(12) 0.0455(15) 0.0381(13) 0.0196(11) 0.0112(10) 0.0101(11) O1B 0.0349(9) 0.0523(10) 0.0651(11) -0.0271(9) 0.0015(8) -0.0144(7) O2B 0.0267(7) 0.0343(8) 0.0261(7) -0.0044(6) 0.0038(5) -0.0030(6) O3B 0.0292(7) 0.0321(8) 0.0365(8) -0.0052(6) -0.0039(6) -0.0039(6) C1B 0.0230(10) 0.0321(11) 0.0336(11) 0.0086(8) -0.0018(8) -0.0006(8) C2B 0.0254(11) 0.0415(12) 0.0473(13) 0.0102(10) -0.0028(9) -0.0030(9) C3B 0.0225(10) 0.0611(16) 0.0505(14) 0.0225(12) 0.0065(10) 0.0018(10) C4B 0.0389(13) 0.0571(15) 0.0387(12) 0.0119(11) 0.0136(10) 0.0129(11) C5B 0.0365(12) 0.0441(13) 0.0301(11) 0.0018(9) 0.0079(9) 0.0045(10) C6B 0.0269(10) 0.0302(10) 0.0267(10) 0.0068(8) 0.0023(8) 0.0015(8) C7B 0.0258(10) 0.0280(10) 0.0234(9) 0.0000(8) 0.0013(7) -0.0004(8) C8B 0.0286(10) 0.0334(11) 0.0307(10) 0.0004(8) -0.0024(8) -0.0083(8) C9B 0.0245(10) 0.0443(12) 0.0377(12) 0.0055(10) 0.0029(9) -0.0061(9) C10B 0.0317(11) 0.0464(13) 0.0397(12) -0.0016(10) 0.0111(9) 0.0017(10) C11B 0.0354(12) 0.0381(12) 0.0356(11) -0.0102(9) 0.0044(9) -0.0025(9) C12B 0.0281(10) 0.0268(10) 0.0283(10) -0.0010(8) -0.0007(8) -0.0018(8) C13B 0.0360(11) 0.0289(11) 0.0361(11) -0.0041(9) 0.0144(9) -0.0025(9) C14B 0.0554(15) 0.0324(12) 0.0579(15) 0.0040(11) 0.0263(12) 0.0013(11) C15B 0.079(2) 0.0445(15) 0.0588(17) 0.0166(13) 0.0312(15) 0.0120(14) C16B 0.078(2) 0.079(2) 0.0339(13) 0.0213(13) 0.0160(13) 0.0434(17) C17B 0.0454(14) 0.0632(16) 0.0304(11) -0.0007(11) 0.0022(10) 0.0145(12) C18B 0.0327(11) 0.0354(11) 0.0260(10) -0.0013(8) 0.0068(8) 0.0047(9) C19B 0.0262(10) 0.0292(11) 0.0320(10) -0.0030(8) 0.0060(8) -0.0019(8) C20B 0.0352(12) 0.0318(12) 0.0637(16) -0.0043(11) 0.0145(11) -0.0062(9) C21B 0.0473(15) 0.0369(13) 0.0783(19) 0.0175(13) 0.0268(13) 0.0058(11) C22B 0.0464(15) 0.0590(17) 0.0541(15) 0.0235(13) 0.0166(12) 0.0166(12) C23B 0.0312(11) 0.0610(15) 0.0317(11) 0.0027(10) 0.0031(9) 0.0054(10) C24B 0.0245(10) 0.0383(11) 0.0256(10) -0.0038(8) 0.0061(8) -0.0023(8) B1B 0.0305(12) 0.0280(12) 0.0377(13) -0.0011(10) -0.0028(10) -0.0036(10) B2B 0.0262(11) 0.0372(13) 0.0327(12) -0.0128(10) 0.0066(9) -0.0083(10) O1C 0.0361(8) 0.0383(8) 0.0297(7) -0.0031(6) -0.0064(6) 0.0127(6) O2C 0.0309(8) 0.0748(12) 0.0279(8) 0.0127(7) 0.0041(6) 0.0122(8) O3C 0.0287(7) 0.0244(7) 0.0349(8) -0.0011(6) -0.0044(6) 0.0045(5) C1C 0.0277(10) 0.0293(10) 0.0265(10) -0.0014(8) -0.0001(8) 0.0014(8) C2C 0.0344(11) 0.0344(11) 0.0266(10) -0.0015(8) 0.0015(8) -0.0024(9) C3C 0.0313(11) 0.0492(14) 0.0392(12) -0.0080(10) 0.0105(9) -0.0053(10) C4C 0.0232(11) 0.0606(15) 0.0481(14) -0.0075(11) -0.0008(10) 0.0065(10) C5C 0.0315(12) 0.0625(16) 0.0363(12) 0.0030(11) -0.0049(9) 0.0111(11) C6C 0.0275(10) 0.0457(12) 0.0264(10) 0.0005(9) 0.0015(8) 0.0051(9) C7C 0.0278(11) 0.0567(14) 0.0299(11) -0.0011(10) 0.0057(9) 0.0022(10) C8C 0.0462(15) 0.088(2) 0.0335(13) 0.0043(13) 0.0103(11) 0.0004(14) C9C 0.0472(15) 0.101(2) 0.0419(14) -0.0048(15) 0.0216(12) -0.0099(15) C10C 0.0288(12) 0.0795(19) 0.0588(16) -0.0219(14) 0.0117(11) -0.0045(12) C11C 0.0273(11) 0.0499(14) 0.0458(13) -0.0139(11) 0.0010(9) -0.0007(10) C12C 0.0255(10) 0.0372(11) 0.0351(11) -0.0083(9) 0.0001(8) 0.0014(8) C13C 0.0257(10) 0.0284(10) 0.0225(9) 0.0023(8) 0.0048(7) 0.0020(8) C14C 0.0324(11) 0.0300(10) 0.0263(10) -0.0008(8) 0.0028(8) 0.0048(8) C15C 0.0386(12) 0.0345(11) 0.0327(11) -0.0067(9) 0.0026(9) -0.0034(9) C16C 0.0323(11) 0.0447(13) 0.0315(11) -0.0023(9) -0.0049(9) -0.0026(9) C17C 0.0280(10) 0.0393(12) 0.0309(11) 0.0020(9) -0.0028(8) 0.0049(9) C18C 0.0257(10) 0.0275(10) 0.0265(10) 0.0016(8) 0.0038(8) -0.0002(8) C19C 0.0242(9) 0.0290(10) 0.0284(10) -0.0006(8) 0.0037(8) -0.0019(8) C20C 0.0351(11) 0.0294(11) 0.0447(12) -0.0030(9) 0.0092(9) 0.0018(9) C21C 0.0436(13) 0.0327(12) 0.0518(14) -0.0150(10) 0.0145(11) -0.0096(10) C22C 0.0351(12) 0.0457(13) 0.0427(13) -0.0138(10) 0.0036(10) -0.0108(10) C23C 0.0272(10) 0.0428(12) 0.0339(11) -0.0056(9) 0.0020(8) -0.0029(9) C24C 0.0230(9) 0.0318(11) 0.0262(10) 0.0000(8) 0.0048(8) -0.0005(8) B1C 0.0283(11) 0.0266(11) 0.0285(11) -0.0043(9) -0.0039(9) 0.0025(9) B2C 0.0235(11) 0.0316(12) 0.0242(11) 0.0024(9) 0.0049(8) 0.0039(9) O1D 0.0346(8) 0.0351(9) 0.0705(11) 0.0133(8) 0.0012(8) 0.0071(7) O2D 0.0334(8) 0.0653(11) 0.0291(8) 0.0109(7) 0.0031(6) 0.0066(7) O3D 0.0351(8) 0.0337(8) 0.0470(9) 0.0079(7) 0.0006(7) 0.0053(6) C1D 0.0276(11) 0.0428(12) 0.0347(11) -0.0145(9) -0.0013(9) -0.0008(9) C2D 0.0289(11) 0.0603(16) 0.0463(13) -0.0213(12) -0.0001(10) 0.0025(10) C3D 0.0304(13) 0.100(2) 0.0512(16) -0.0314(16) 0.0100(11) -0.0037(13) C4D 0.0455(16) 0.123(3) 0.0385(14) -0.0032(16) 0.0159(12) -0.0119(17) C5D 0.0495(15) 0.100(2) 0.0334(13) 0.0118(14) 0.0098(11) -0.0006(15) C6D 0.0290(11) 0.0614(15) 0.0272(11) -0.0028(10) 0.0014(9) 0.0001(10) C7D 0.0286(10) 0.0416(12) 0.0228(10) -0.0017(8) -0.0011(8) 0.0012(9) C8D 0.0350(12) 0.0497(14) 0.0322(11) 0.0023(10) -0.0050(9) 0.0092(10) C9D 0.0262(11) 0.0497(14) 0.0407(12) -0.0082(10) -0.0011(9) 0.0072(9) C10D 0.0319(11) 0.0458(13) 0.0399(12) -0.0061(10) 0.0065(9) -0.0025(10) C11D 0.0358(11) 0.0319(11) 0.0347(11) -0.0016(9) 0.0019(9) -0.0010(9) C12D 0.0291(10) 0.0293(10) 0.0270(10) -0.0073(8) -0.0018(8) -0.0004(8) C13D 0.0312(11) 0.0292(11) 0.0359(11) 0.0056(9) 0.0107(9) 0.0027(8) C14D 0.0402(12) 0.0363(12) 0.0431(13) 0.0048(10) 0.0086(10) -0.0010(10) C15D 0.0570(15) 0.0347(12) 0.0460(14) -0.0047(10) 0.0148(11) -0.0060(11) C16D 0.0548(15) 0.0251(11) 0.0560(15) 0.0002(10) 0.0253(12) 0.0031(10) C17D 0.0394(12) 0.0342(12) 0.0524(14) 0.0110(10) 0.0179(10) 0.0120(10) C18D 0.0311(11) 0.0287(11) 0.0393(12) 0.0062(9) 0.0111(9) 0.0024(9) C19D 0.0375(12) 0.0342(12) 0.0365(12) 0.0036(9) 0.0108(9) -0.0015(9) C20D 0.0476(14) 0.0557(16) 0.0407(13) 0.0046(11) 0.0032(11) -0.0108(12) C21D 0.0686(18) 0.0606(17) 0.0385(13) -0.0080(12) 0.0100(12) -0.0260(14) C22D 0.0693(18) 0.0386(13) 0.0506(15) -0.0079(11) 0.0201(13) -0.0091(13) C23D 0.0512(14) 0.0312(12) 0.0514(14) 0.0002(10) 0.0200(11) 0.0023(10) C24D 0.0339(11) 0.0295(11) 0.0406(12) 0.0033(9) 0.0144(9) 0.0022(9) B1D 0.0315(12) 0.0260(12) 0.0360(13) -0.0091(10) -0.0020(10) 0.0007(9) B2D 0.0287(12) 0.0326(13) 0.0426(14) 0.0096(10) 0.0102(10) 0.0051(10) O1E 0.0482(10) 0.0978(15) 0.0518(11) -0.0324(10) 0.0096(8) -0.0401(10) O2E 0.0294(7) 0.0301(7) 0.0372(8) -0.0023(6) -0.0034(6) -0.0030(6) O3E 0.0439(9) 0.0665(11) 0.0287(8) -0.0121(7) 0.0061(7) -0.0130(8) C1E 0.0266(10) 0.0528(13) 0.0255(10) -0.0007(9) 0.0062(8) 0.0034(9) C2E 0.0369(13) 0.092(2) 0.0322(12) 0.0118(13) 0.0039(10) 0.0160(13) C3E 0.0544(18) 0.096(2) 0.0549(17) 0.0387(17) 0.0201(14) 0.0352(17) C4E 0.0681(19) 0.0520(16) 0.077(2) 0.0355(15) 0.0439(16) 0.0278(15) C5E 0.0437(13) 0.0369(13) 0.0606(15) 0.0053(11) 0.0230(11) 0.0028(10) C6E 0.0282(10) 0.0336(11) 0.0289(10) 0.0027(8) 0.0079(8) 0.0034(8) C7E 0.0326(11) 0.0313(11) 0.0295(10) -0.0003(8) 0.0073(8) 0.0028(8) C8E 0.0415(13) 0.0608(16) 0.0418(13) 0.0093(12) 0.0024(10) 0.0120(12) C9E 0.0603(18) 0.070(2) 0.0658(18) 0.0301(16) 0.0214(14) 0.0247(16) C10E 0.083(2) 0.0458(16) 0.091(2) 0.0365(16) 0.0500(19) 0.0327(16) C11E 0.0651(17) 0.0305(13) 0.080(2) -0.0061(13) 0.0448(15) -0.0054(12) C12E 0.0366(11) 0.0289(11) 0.0395(12) -0.0050(9) 0.0176(9) -0.0025(9) C13E 0.0277(10) 0.0344(11) 0.0346(11) 0.0110(9) 0.0023(8) 0.0033(8) C14E 0.0292(11) 0.0545(15) 0.0529(14) 0.0200(12) 0.0063(10) 0.0020(10) C15E 0.0361(14) 0.087(2) 0.0653(18) 0.0342(16) 0.0175(13) 0.0103(14) C16E 0.068(2) 0.109(3) 0.0513(17) 0.0126(17) 0.0348(16) 0.0171(19) C17E 0.072(2) 0.091(2) 0.0380(14) -0.0071(14) 0.0217(13) 0.0015(17) C18E 0.0389(12) 0.0471(13) 0.0324(11) 0.0029(10) 0.0061(9) 0.0000(10) C19E 0.0323(11) 0.0379(12) 0.0280(10) 0.0010(9) -0.0003(8) -0.0030(9) C20E 0.0395(13) 0.0608(16) 0.0395(13) -0.0004(11) -0.0074(10) -0.0156(11) C21E 0.0284(12) 0.0614(16) 0.0542(15) 0.0140(12) -0.0024(11) -0.0082(11) C22E 0.0326(12) 0.0511(14) 0.0461(13) 0.0066(11) 0.0136(10) 0.0060(10) C23E 0.0381(12) 0.0385(12) 0.0363(12) -0.0049(9) 0.0060(9) -0.0010(9) C24E 0.0286(10) 0.0275(10) 0.0281(10) 0.0011(8) 0.0012(8) 0.0009(8) B1E 0.0296(12) 0.0538(16) 0.0318(12) -0.0156(11) 0.0101(10) -0.0126(11) B2E 0.0331(13) 0.0334(13) 0.0335(12) -0.0002(10) -0.0010(10) -0.0054(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A B1A 1.358(3) . ? O1A B2A 1.367(3) . ? O2A C6A 1.377(2) . ? O2A C7A 1.380(2) . ? O3A C18A 1.376(2) . ? O3A C19A 1.378(2) . ? C1A C6A 1.392(3) . ? C1A C2A 1.410(3) . ? C1A B1A 1.540(3) . ? C2A C3A 1.374(3) . ? C2A H2AA 0.9500 . ? C3A C4A 1.385(4) . ? C3A H3AA 0.9500 . ? C4A C5A 1.378(4) . ? C4A H4AA 0.9500 . ? C5A C6A 1.394(3) . ? C5A H5AA 0.9500 . ? C7A C12A 1.386(3) . ? C7A C8A 1.392(3) . ? C8A C9A 1.371(3) . ? C8A H8AA 0.9500 . ? C9A C10A 1.385(3) . ? C9A H9AA 0.9500 . ? C10A C11A 1.378(3) . ? C10A H10A 0.9500 . ? C11A C12A 1.403(3) . ? C11A H11A 0.9500 . ? C12A B1A 1.540(3) . ? C13A C18A 1.398(3) . ? C13A C14A 1.403(3) . ? C13A B2A 1.537(4) . ? C14A C15A 1.364(4) . ? C14A H14A 0.9500 . ? C15A C16A 1.400(4) . ? C15A H15A 0.9500 . ? C16A C17A 1.387(3) . ? C16A H16A 0.9500 . ? C17A C18A 1.387(3) . ? C17A H17A 0.9500 . ? C19A C20A 1.391(3) . ? C19A C24A 1.394(3) . ? C20A C21A 1.373(3) . ? C20A H20A 0.9500 . ? C21A C22A 1.381(4) . ? C21A H21A 0.9500 . ? C22A C23A 1.374(4) . ? C22A H22A 0.9500 . ? C23A C24A 1.417(3) . ? C23A H23A 0.9500 . ? C24A B2A 1.522(3) . ? O1B B1B 1.356(3) . ? O1B B2B 1.361(3) . ? O2B C6B 1.377(2) . ? O2B C7B 1.379(2) . ? O3B C19B 1.375(2) . ? O3B C18B 1.376(3) . ? C1B C6B 1.393(3) . ? C1B C2B 1.414(3) . ? C1B B1B 1.541(3) . ? C2B C3B 1.377(3) . ? C2B H2BA 0.9500 . ? C3B C4B 1.384(4) . ? C3B H3BA 0.9500 . ? C4B C5B 1.376(3) . ? C4B H4BA 0.9500 . ? C5B C6B 1.396(3) . ? C5B H5BA 0.9500 . ? C7B C12B 1.388(3) . ? C7B C8B 1.395(3) . ? C8B C9B 1.374(3) . ? C8B H8BA 0.9500 . ? C9B C10B 1.386(3) . ? C9B H9BA 0.9500 . ? C10B C11B 1.375(3) . ? C10B H10B 0.9500 . ? C11B C12B 1.412(3) . ? C11B H11B 0.9500 . ? C12B B1B 1.537(3) . ? C13B C18B 1.398(3) . ? C13B C14B 1.403(3) . ? C13B B2B 1.533(3) . ? C14B C15B 1.354(4) . ? C14B H14B 0.9500 . ? C15B C16B 1.397(4) . ? C15B H15B 0.9500 . ? C16B C17B 1.392(4) . ? C16B H16B 0.9500 . ? C17B C18B 1.394(3) . ? C17B H17B 0.9500 . ? C19B C20B 1.393(3) . ? C19B C24B 1.398(3) . ? C20B C21B 1.372(4) . ? C20B H20B 0.9500 . ? C21B C22B 1.377(4) . ? C21B H21B 0.9500 . ? C22B C23B 1.376(4) . ? C22B H22B 0.9500 . ? C23B C24B 1.404(3) . ? C23B H23B 0.9500 . ? C24B B2B 1.529(3) . ? O1C B1C 1.353(3) . ? O1C B2C 1.362(3) . ? O2C C6C 1.375(3) . ? O2C C7C 1.378(3) . ? O3C C19C 1.376(2) . ? O3C C18C 1.380(2) . ? C1C C6C 1.400(3) . ? C1C C2C 1.410(3) . ? C1C B1C 1.539(3) . ? C2C C3C 1.378(3) . ? C2C H2CA 0.9500 . ? C3C C4C 1.394(3) . ? C3C H3CA 0.9500 . ? C4C C5C 1.370(3) . ? C4C H4CA 0.9500 . ? C5C C6C 1.390(3) . ? C5C H5CA 0.9500 . ? C7C C8C 1.393(3) . ? C7C C12C 1.397(3) . ? C8C C9C 1.381(4) . ? C8C H8CA 0.9500 . ? C9C C10C 1.391(4) . ? C9C H9CA 0.9500 . ? C10C C11C 1.375(4) . ? C10C H10C 0.9500 . ? C11C C12C 1.414(3) . ? C11C H11C 0.9500 . ? C12C B1C 1.546(3) . ? C13C C18C 1.395(3) . ? C13C C14C 1.399(3) . ? C13C B2C 1.539(3) . ? C14C C15C 1.378(3) . ? C14C H14C 0.9500 . ? C15C C16C 1.392(3) . ? C15C H15C 0.9500 . ? C16C C17C 1.374(3) . ? C16C H16C 0.9500 . ? C17C C18C 1.393(3) . ? C17C H17C 0.9500 . ? C19C C20C 1.389(3) . ? C19C C24C 1.394(3) . ? C20C C21C 1.378(3) . ? C20C H20C 0.9500 . ? C21C C22C 1.387(3) . ? C21C H21C 0.9500 . ? C22C C23C 1.367(3) . ? C22C H22C 0.9500 . ? C23C C24C 1.409(3) . ? C23C H23C 0.9500 . ? C24C B2C 1.536(3) . ? O1D B1D 1.350(3) . ? O1D B2D 1.368(3) . ? O2D C7D 1.379(3) . ? O2D C6D 1.380(3) . ? O3D C18D 1.377(3) . ? O3D C19D 1.382(3) . ? C1D C6D 1.390(3) . ? C1D C2D 1.415(3) . ? C1D B1D 1.544(3) . ? C2D C3D 1.380(4) . ? C2D H2DA 0.9500 . ? C3D C4D 1.391(5) . ? C3D H3DA 0.9500 . ? C4D C5D 1.373(4) . ? C4D H4DA 0.9500 . ? C5D C6D 1.395(3) . ? C5D H5DA 0.9500 . ? C7D C8D 1.393(3) . ? C7D C12D 1.394(3) . ? C8D C9D 1.372(3) . ? C8D H8DA 0.9500 . ? C9D C10D 1.388(3) . ? C9D H9DA 0.9500 . ? C10D C11D 1.382(3) . ? C10D H10D 0.9500 . ? C11D C12D 1.408(3) . ? C11D H11D 0.9500 . ? C12D B1D 1.537(3) . ? C13D C18D 1.391(3) . ? C13D C14D 1.402(3) . ? C13D B2D 1.528(3) . ? C14D C15D 1.373(3) . ? C14D H14D 0.9500 . ? C15D C16D 1.386(4) . ? C15D H15D 0.9500 . ? C16D C17D 1.378(4) . ? C16D H16D 0.9500 . ? C17D C18D 1.394(3) . ? C17D H17D 0.9500 . ? C19D C20D 1.393(3) . ? C19D C24D 1.395(3) . ? C20D C21D 1.383(4) . ? C20D H20D 0.9500 . ? C21D C22D 1.391(4) . ? C21D H21D 0.9500 . ? C22D C23D 1.370(4) . ? C22D H22D 0.9500 . ? C23D C24D 1.403(3) . ? C23D H23D 0.9500 . ? C24D B2D 1.530(3) . ? O1E B2E 1.353(3) . ? O1E B1E 1.365(3) . ? O2E C6E 1.369(2) . ? O2E C7E 1.373(2) . ? O3E C19E 1.377(3) . ? O3E C18E 1.380(3) . ? C1E C6E 1.393(3) . ? C1E C2E 1.408(3) . ? C1E B1E 1.527(4) . ? C2E C3E 1.357(4) . ? C2E H2EA 0.9500 . ? C3E C4E 1.382(5) . ? C3E H3EA 0.9500 . ? C4E C5E 1.380(4) . ? C4E H4EA 0.9500 . ? C5E C6E 1.390(3) . ? C5E H5EA 0.9500 . ? C7E C12E 1.390(3) . ? C7E C8E 1.394(3) . ? C8E C9E 1.355(4) . ? C8E H8EA 0.9500 . ? C9E C10E 1.385(5) . ? C9E H9EA 0.9500 . ? C10E C11E 1.386(4) . ? C10E H10E 0.9500 . ? C11E C12E 1.413(3) . ? C11E H11E 0.9500 . ? C12E B1E 1.530(4) . ? C13E C18E 1.390(3) . ? C13E C14E 1.412(3) . ? C13E B2E 1.544(3) . ? C14E C15E 1.370(4) . ? C14E H14E 0.9500 . ? C15E C16E 1.380(5) . ? C15E H15E 0.9500 . ? C16E C17E 1.381(4) . ? C16E H16E 0.9500 . ? C17E C18E 1.394(3) . ? C17E H17E 0.9500 . ? C19E C24E 1.389(3) . ? C19E C20E 1.393(3) . ? C20E C21E 1.367(4) . ? C20E H20E 0.9500 . ? C21E C22E 1.383(4) . ? C21E H21E 0.9500 . ? C22E C23E 1.375(3) . ? C22E H22E 0.9500 . ? C23E C24E 1.409(3) . ? C23E H23E 0.9500 . ? C24E B2E 1.532(3) . ? 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 B1A O1A B2A 145.8(2) . . ? C6A O2A C7A 121.74(16) . . ? C18A O3A C19A 122.10(15) . . ? C6A C1A C2A 116.3(2) . . ? C6A C1A B1A 118.03(18) . . ? C2A C1A B1A 125.69(19) . . ? C3A C2A C1A 122.1(2) . . ? C3A C2A H2AA 119.0 . . ? C1A C2A H2AA 119.0 . . ? C2A C3A C4A 119.7(2) . . ? C2A C3A H3AA 120.1 . . ? C4A C3A H3AA 120.1 . . ? C5A C4A C3A 120.4(2) . . ? C5A C4A H4AA 119.8 . . ? C3A C4A H4AA 119.8 . . ? C4A C5A C6A 119.1(2) . . ? C4A C5A H5AA 120.5 . . ? C6A C5A H5AA 120.5 . . ? O2A C6A C1A 123.06(18) . . ? O2A C6A C5A 114.51(19) . . ? C1A C6A C5A 122.4(2) . . ? O2A C7A C12A 123.49(17) . . ? O2A C7A C8A 114.61(18) . . ? C12A C7A C8A 121.90(19) . . ? C9A C8A C7A 119.0(2) . . ? C9A C8A H8AA 120.5 . . ? C7A C8A H8AA 120.5 . . ? C8A C9A C10A 121.0(2) . . ? C8A C9A H9AA 119.5 . . ? C10A C9A H9AA 119.5 . . ? C11A C10A C9A 119.1(2) . . ? C11A C10A H10A 120.4 . . ? C9A C10A H10A 120.4 . . ? C10A C11A C12A 121.81(19) . . ? C10A C11A H11A 119.1 . . ? C12A C11A H11A 119.1 . . ? C7A C12A C11A 117.11(18) . . ? C7A C12A B1A 117.81(18) . . ? C11A C12A B1A 125.07(18) . . ? C18A C13A C14A 116.6(2) . . ? C18A C13A B2A 118.01(19) . . ? C14A C13A B2A 125.3(2) . . ? C15A C14A C13A 122.1(2) . . ? C15A C14A H14A 119.0 . . ? C13A C14A H14A 119.0 . . ? C14A C15A C16A 119.8(2) . . ? C14A C15A H15A 120.1 . . ? C16A C15A H15A 120.1 . . ? C17A C16A C15A 120.2(2) . . ? C17A C16A H16A 119.9 . . ? C15A C16A H16A 119.9 . . ? C18A C17A C16A 118.6(2) . . ? C18A C17A H17A 120.7 . . ? C16A C17A H17A 120.7 . . ? O3A C18A C17A 114.72(17) . . ? O3A C18A C13A 122.61(19) . . ? C17A C18A C13A 122.68(19) . . ? O3A C19A C20A 114.47(18) . . ? O3A C19A C24A 122.92(19) . . ? C20A C19A C24A 122.6(2) . . ? C21A C20A C19A 119.4(2) . . ? C21A C20A H20A 120.3 . . ? C19A C20A H20A 120.3 . . ? C20A C21A C22A 120.3(2) . . ? C20A C21A H21A 119.9 . . ? C22A C21A H21A 119.9 . . ? C23A C22A C21A 120.0(2) . . ? C23A C22A H22A 120.0 . . ? C21A C22A H22A 120.0 . . ? C22A C23A C24A 122.1(2) . . ? C22A C23A H23A 119.0 . . ? C24A C23A H23A 119.0 . . ? C19A C24A C23A 115.7(2) . . ? C19A C24A B2A 118.2(2) . . ? C23A C24A B2A 126.2(2) . . ? O1A B1A C1A 124.15(19) . . ? O1A B1A C12A 119.9(2) . . ? C1A B1A C12A 115.85(18) . . ? O1A B2A C24A 121.3(2) . . ? O1A B2A C13A 122.5(2) . . ? C24A B2A C13A 116.13(18) . . ? B1B O1B B2B 146.1(2) . . ? C6B O2B C7B 121.77(15) . . ? C19B O3B C18B 121.55(15) . . ? C6B C1B C2B 116.3(2) . . ? C6B C1B B1B 117.98(18) . . ? C2B C1B B1B 125.76(19) . . ? C3B C2B C1B 121.8(2) . . ? C3B C2B H2BA 119.1 . . ? C1B C2B H2BA 119.1 . . ? C2B C3B C4B 119.7(2) . . ? C2B C3B H3BA 120.1 . . ? C4B C3B H3BA 120.1 . . ? C5B C4B C3B 120.8(2) . . ? C5B C4B H4BA 119.6 . . ? C3B C4B H4BA 119.6 . . ? C4B C5B C6B 118.8(2) . . ? C4B C5B H5BA 120.6 . . ? C6B C5B H5BA 120.6 . . ? O2B C6B C1B 123.19(18) . . ? O2B C6B C5B 114.26(18) . . ? C1B C6B C5B 122.54(19) . . ? O2B C7B C12B 123.16(17) . . ? O2B C7B C8B 114.70(17) . . ? C12B C7B C8B 122.14(18) . . ? C9B C8B C7B 119.01(19) . . ? C9B C8B H8BA 120.5 . . ? C7B C8B H8BA 120.5 . . ? C8B C9B C10B 120.83(19) . . ? C8B C9B H9BA 119.6 . . ? C10B C9B H9BA 119.6 . . ? C11B C10B C9B 119.5(2) . . ? C11B C10B H10B 120.2 . . ? C9B C10B H10B 120.2 . . ? C10B C11B C12B 121.7(2) . . ? C10B C11B H11B 119.2 . . ? C12B C11B H11B 119.2 . . ? C7B C12B C11B 116.81(18) . . ? C7B C12B B1B 118.30(18) . . ? C11B C12B B1B 124.88(18) . . ? C18B C13B C14B 117.1(2) . . ? C18B C13B B2B 118.30(19) . . ? C14B C13B B2B 124.6(2) . . ? C15B C14B C13B 121.9(3) . . ? C15B C14B H14B 119.1 . . ? C13B C14B H14B 119.1 . . ? C14B C15B C16B 120.0(2) . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C17B C16B C15B 120.8(2) . . ? C17B C16B H16B 119.6 . . ? C15B C16B H16B 119.6 . . ? C16B C17B C18B 117.7(3) . . ? C16B C17B H17B 121.1 . . ? C18B C17B H17B 121.1 . . ? O3B C18B C17B 114.51(19) . . ? O3B C18B C13B 123.05(18) . . ? C17B C18B C13B 122.4(2) . . ? O3B C19B C20B 114.82(18) . . ? O3B C19B C24B 123.08(18) . . ? C20B C19B C24B 122.1(2) . . ? C21B C20B C19B 118.6(2) . . ? C21B C20B H20B 120.7 . . ? C19B C20B H20B 120.7 . . ? C20B C21B C22B 121.3(2) . . ? C20B C21B H21B 119.3 . . ? C22B C21B H21B 119.3 . . ? C23B C22B C21B 119.6(2) . . ? C23B C22B H22B 120.2 . . ? C21B C22B H22B 120.2 . . ? C22B C23B C24B 121.7(2) . . ? C22B C23B H23B 119.1 . . ? C24B C23B H23B 119.1 . . ? C19B C24B C23B 116.7(2) . . ? C19B C24B B2B 118.38(18) . . ? C23B C24B B2B 124.94(19) . . ? O1B B1B C12B 120.6(2) . . ? O1B B1B C1B 123.8(2) . . ? C12B B1B C1B 115.59(18) . . ? O1B B2B C24B 120.9(2) . . ? O1B B2B C13B 123.5(2) . . ? C24B B2B C13B 115.56(17) . . ? B1C O1C B2C 142.65(17) . . ? C6C O2C C7C 121.81(16) . . ? C19C O3C C18C 121.89(15) . . ? C6C C1C C2C 116.95(18) . . ? C6C C1C B1C 118.42(18) . . ? C2C C1C B1C 124.62(18) . . ? C3C C2C C1C 121.53(19) . . ? C3C C2C H2CA 119.2 . . ? C1C C2C H2CA 119.2 . . ? C2C C3C C4C 119.4(2) . . ? C2C C3C H3CA 120.3 . . ? C4C C3C H3CA 120.3 . . ? C5C C4C C3C 121.0(2) . . ? C5C C4C H4CA 119.5 . . ? C3C C4C H4CA 119.5 . . ? C4C C5C C6C 119.2(2) . . ? C4C C5C H5CA 120.4 . . ? C6C C5C H5CA 120.4 . . ? O2C C6C C5C 114.91(18) . . ? O2C C6C C1C 123.17(18) . . ? C5C C6C C1C 121.9(2) . . ? O2C C7C C8C 114.3(2) . . ? O2C C7C C12C 123.08(19) . . ? C8C C7C C12C 122.6(2) . . ? C9C C8C C7C 118.8(2) . . ? C9C C8C H8CA 120.6 . . ? C7C C8C H8CA 120.6 . . ? C8C C9C C10C 120.6(2) . . ? C8C C9C H9CA 119.7 . . ? C10C C9C H9CA 119.7 . . ? C11C C10C C9C 119.8(2) . . ? C11C C10C H10C 120.1 . . ? C9C C10C H10C 120.1 . . ? C10C C11C C12C 121.8(2) . . ? C10C C11C H11C 119.1 . . ? C12C C11C H11C 119.1 . . ? C7C C12C C11C 116.4(2) . . ? C7C C12C B1C 118.39(18) . . ? C11C C12C B1C 125.2(2) . . ? C18C C13C C14C 116.98(17) . . ? C18C C13C B2C 118.00(17) . . ? C14C C13C B2C 125.02(17) . . ? C15C C14C C13C 121.58(19) . . ? C15C C14C H14C 119.2 . . ? C13C C14C H14C 119.2 . . ? C14C C15C C16C 119.7(2) . . ? C14C C15C H15C 120.2 . . ? C16C C15C H15C 120.2 . . ? C17C C16C C15C 120.68(19) . . ? C17C C16C H16C 119.7 . . ? C15C C16C H16C 119.7 . . ? C16C C17C C18C 118.73(19) . . ? C16C C17C H17C 120.6 . . ? C18C C17C H17C 120.6 . . ? O3C C18C C17C 114.58(17) . . ? O3C C18C C13C 123.07(17) . . ? C17C C18C C13C 122.35(18) . . ? O3C C19C C20C 114.75(17) . . ? O3C C19C C24C 122.97(17) . . ? C20C C19C C24C 122.27(18) . . ? C21C C20C C19C 118.6(2) . . ? C21C C20C H20C 120.7 . . ? C19C C20C H20C 120.7 . . ? C20C C21C C22C 121.0(2) . . ? C20C C21C H21C 119.5 . . ? C22C C21C H21C 119.5 . . ? C23C C22C C21C 119.7(2) . . ? C23C C22C H22C 120.2 . . ? C21C C22C H22C 120.2 . . ? C22C C23C C24C 121.6(2) . . ? C22C C23C H23C 119.2 . . ? C24C C23C H23C 119.2 . . ? C19C C24C C23C 116.86(18) . . ? C19C C24C B2C 118.29(17) . . ? C23C C24C B2C 124.85(18) . . ? O1C B1C C1C 120.83(19) . . ? O1C B1C C12C 124.04(19) . . ? C1C B1C C12C 115.02(17) . . ? O1C B2C C24C 122.46(18) . . ? O1C B2C C13C 121.80(18) . . ? C24C B2C C13C 115.72(17) . . ? B1D O1D B2D 144.65(19) . . ? C7D O2D C6D 121.51(17) . . ? C18D O3D C19D 121.32(16) . . ? C6D C1D C2D 116.2(2) . . ? C6D C1D B1D 118.08(19) . . ? C2D C1D B1D 125.7(2) . . ? C3D C2D C1D 121.8(3) . . ? C3D C2D H2DA 119.1 . . ? C1D C2D H2DA 119.1 . . ? C2D C3D C4D 119.6(2) . . ? C2D C3D H3DA 120.2 . . ? C4D C3D H3DA 120.2 . . ? C5D C4D C3D 120.7(3) . . ? C5D C4D H4DA 119.7 . . ? C3D C4D H4DA 119.7 . . ? C4D C5D C6D 118.9(3) . . ? C4D C5D H5DA 120.6 . . ? C6D C5D H5DA 120.6 . . ? O2D C6D C1D 123.4(2) . . ? O2D C6D C5D 113.8(2) . . ? C1D C6D C5D 122.8(2) . . ? O2D C7D C8D 114.59(18) . . ? O2D C7D C12D 123.29(18) . . ? C8D C7D C12D 122.1(2) . . ? C9D C8D C7D 119.3(2) . . ? C9D C8D H8DA 120.4 . . ? C7D C8D H8DA 120.4 . . ? C8D C9D C10D 120.8(2) . . ? C8D C9D H9DA 119.6 . . ? C10D C9D H9DA 119.6 . . ? C11D C10D C9D 119.2(2) . . ? C11D C10D H10D 120.4 . . ? C9D C10D H10D 120.4 . . ? C10D C11D C12D 122.0(2) . . ? C10D C11D H11D 119.0 . . ? C12D C11D H11D 119.0 . . ? C7D C12D C11D 116.55(19) . . ? C7D C12D B1D 118.18(19) . . ? C11D C12D B1D 125.25(19) . . ? C18D C13D C14D 117.30(19) . . ? C18D C13D B2D 118.75(19) . . ? C14D C13D B2D 123.9(2) . . ? C15D C14D C13D 121.4(2) . . ? C15D C14D H14D 119.3 . . ? C13D C14D H14D 119.3 . . ? C14D C15D C16D 119.6(2) . . ? C14D C15D H15D 120.2 . . ? C16D C15D H15D 120.2 . . ? C17D C16D C15D 121.3(2) . . ? C17D C16D H16D 119.4 . . ? C15D C16D H16D 119.4 . . ? C16D C17D C18D 118.2(2) . . ? C16D C17D H17D 120.9 . . ? C18D C17D H17D 120.9 . . ? O3D C18D C13D 122.90(18) . . ? O3D C18D C17D 114.86(19) . . ? C13D C18D C17D 122.2(2) . . ? O3D C19D C20D 114.4(2) . . ? O3D C19D C24D 123.28(19) . . ? C20D C19D C24D 122.3(2) . . ? C21D C20D C19D 118.4(2) . . ? C21D C20D H20D 120.8 . . ? C19D C20D H20D 120.8 . . ? C20D C21D C22D 120.8(2) . . ? C20D C21D H21D 119.6 . . ? C22D C21D H21D 119.6 . . ? C23D C22D C21D 119.8(2) . . ? C23D C22D H22D 120.1 . . ? C21D C22D H22D 120.1 . . ? C22D C23D C24D 121.6(2) . . ? C22D C23D H23D 119.2 . . ? C24D C23D H23D 119.2 . . ? C19D C24D C23D 117.1(2) . . ? C19D C24D B2D 118.06(19) . . ? C23D C24D B2D 124.8(2) . . ? O1D B1D C12D 120.5(2) . . ? O1D B1D C1D 124.0(2) . . ? C12D B1D C1D 115.51(19) . . ? O1D B2D C13D 120.8(2) . . ? O1D B2D C24D 123.5(2) . . ? C13D B2D C24D 115.66(19) . . ? B2E O1E B1E 145.4(2) . . ? C6E O2E C7E 121.75(16) . . ? C19E O3E C18E 121.55(17) . . ? C6E C1E C2E 117.3(2) . . ? C6E C1E B1E 118.32(19) . . ? C2E C1E B1E 124.3(2) . . ? C3E C2E C1E 121.5(3) . . ? C3E C2E H2EA 119.3 . . ? C1E C2E H2EA 119.3 . . ? C2E C3E C4E 119.8(2) . . ? C2E C3E H3EA 120.1 . . ? C4E C3E H3EA 120.1 . . ? C5E C4E C3E 121.3(3) . . ? C5E C4E H4EA 119.3 . . ? C3E C4E H4EA 119.3 . . ? C4E C5E C6E 118.3(3) . . ? C4E C5E H5EA 120.9 . . ? C6E C5E H5EA 120.9 . . ? O2E C6E C5E 115.21(19) . . ? O2E C6E C1E 122.95(19) . . ? C5E C6E C1E 121.8(2) . . ? O2E C7E C12E 123.15(18) . . ? O2E C7E C8E 113.83(19) . . ? C12E C7E C8E 123.0(2) . . ? C9E C8E C7E 119.4(3) . . ? C9E C8E H8EA 120.3 . . ? C7E C8E H8EA 120.3 . . ? C8E C9E C10E 120.2(3) . . ? C8E C9E H9EA 119.9 . . ? C10E C9E H9EA 119.9 . . ? C9E C10E C11E 120.4(2) . . ? C9E C10E H10E 119.8 . . ? C11E C10E H10E 119.8 . . ? C10E C11E C12E 121.1(3) . . ? C10E C11E H11E 119.4 . . ? C12E C11E H11E 119.4 . . ? C7E C12E C11E 115.8(2) . . ? C7E C12E B1E 118.12(19) . . ? C11E C12E B1E 126.0(2) . . ? C18E C13E C14E 116.6(2) . . ? C18E C13E B2E 117.63(19) . . ? C14E C13E B2E 125.8(2) . . ? C15E C14E C13E 121.8(3) . . ? C15E C14E H14E 119.1 . . ? C13E C14E H14E 119.1 . . ? C14E C15E C16E 119.6(3) . . ? C14E C15E H15E 120.2 . . ? C16E C15E H15E 120.2 . . ? C15E C16E C17E 121.1(3) . . ? C15E C16E H16E 119.4 . . ? C17E C16E H16E 119.4 . . ? C16E C17E C18E 118.4(3) . . ? C16E C17E H17E 120.8 . . ? C18E C17E H17E 120.8 . . ? O3E C18E C13E 123.4(2) . . ? O3E C18E C17E 114.1(2) . . ? C13E C18E C17E 122.5(2) . . ? O3E C19E C24E 123.23(19) . . ? O3E C19E C20E 114.75(19) . . ? C24E C19E C20E 122.0(2) . . ? C21E C20E C19E 119.4(2) . . ? C21E C20E H20E 120.3 . . ? C19E C20E H20E 120.3 . . ? C20E C21E C22E 120.8(2) . . ? C20E C21E H21E 119.6 . . ? C22E C21E H21E 119.6 . . ? C23E C22E C21E 119.3(2) . . ? C23E C22E H22E 120.4 . . ? C21E C22E H22E 120.4 . . ? C22E C23E C24E 122.0(2) . . ? C22E C23E H23E 119.0 . . ? C24E C23E H23E 119.0 . . ? C19E C24E C23E 116.47(19) . . ? C19E C24E B2E 118.19(19) . . ? C23E C24E B2E 125.32(19) . . ? O1E B1E C1E 122.4(2) . . ? O1E B1E C12E 121.8(2) . . ? C1E B1E C12E 115.66(19) . . ? O1E B2E C24E 120.4(2) . . ? O1E B2E C13E 123.7(2) . . ? C24E B2E C13E 115.82(18) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 66.02 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.429 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.046 _iucr_refine_instructions_details ; TITL d1203 in P2(1)/n CELL 1.54178 9.4797 45.4904 21.7415 90.000 92.764 90.000 ZERR 20 0.0006 0.0026 0.0013 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H B O UNIT 480 320 40 60 ACTA TEMP -123.140 SIZE 0.150 0.210 0.310 L.S. 4 BOND $H FMAP 2 PLAN 20 WGHT 0.056400 6.759600 FVAR 0.02743 O1A 4 -0.054430 0.243229 0.403878 11.00000 0.04322 0.06780 = 0.05548 0.02754 0.00788 0.02876 O2A 4 -0.236032 0.294701 0.258647 11.00000 0.02688 0.06374 = 0.02867 0.01186 0.00402 0.00985 O3A 4 0.266294 0.184594 0.468706 11.00000 0.02651 0.02756 = 0.03623 0.00032 -0.00364 0.00486 C1A 1 -0.028971 0.268156 0.299353 11.00000 0.02316 0.02935 = 0.03314 -0.01220 -0.00184 -0.00025 C2A 1 0.113102 0.261209 0.289406 11.00000 0.02347 0.04226 = 0.04355 -0.01527 -0.00002 0.00159 AFIX 43 H2AA 2 0.164321 0.249411 0.318809 11.00000 -1.20000 AFIX 0 C3A 1 0.179786 0.270971 0.238513 11.00000 0.02556 0.06797 = 0.05086 -0.02303 0.00881 -0.00486 AFIX 43 H3AA 2 0.275148 0.265654 0.232730 11.00000 -1.20000 AFIX 0 C4A 1 0.107443 0.288588 0.195691 11.00000 0.03901 0.09325 = 0.04138 -0.00287 0.01582 -0.00568 AFIX 43 H4AA 2 0.153758 0.295495 0.160699 11.00000 -1.20000 AFIX 0 C5A 1 -0.031310 0.296165 0.203513 11.00000 0.04035 0.08234 = 0.03584 0.01004 0.00861 0.00251 AFIX 43 H5AA 2 -0.080926 0.308286 0.174200 11.00000 -1.20000 AFIX 0 C6A 1 -0.097818 0.285796 0.255024 11.00000 0.02277 0.04816 = 0.02823 -0.00332 0.00255 0.00102 C7A 1 -0.316457 0.286492 0.307028 11.00000 0.02275 0.03999 = 0.02316 -0.00173 0.00131 0.00085 C8A 1 -0.454579 0.296987 0.303384 11.00000 0.02860 0.05870 = 0.03082 0.00565 -0.00167 0.00991 AFIX 43 H8AA 2 -0.487060 0.308822 0.269596 11.00000 -1.20000 AFIX 0 C9A 1 -0.543058 0.289993 0.349266 11.00000 0.02161 0.05308 = 0.03905 -0.00609 0.00146 0.00551 AFIX 43 H9AA 2 -0.637238 0.297192 0.347215 11.00000 -1.20000 AFIX 0 C10A 1 -0.497225 0.272591 0.398562 11.00000 0.03113 0.04154 = 0.03425 -0.00422 0.00970 -0.00657 AFIX 43 H10A 2 -0.559639 0.267629 0.429847 11.00000 -1.20000 AFIX 0 C11A 1 -0.359916 0.262579 0.401600 11.00000 0.03567 0.02961 = 0.03155 0.00297 0.00365 0.00070 AFIX 43 H11A 2 -0.328133 0.250865 0.435689 11.00000 -1.20000 AFIX 0 C12A 1 -0.265747 0.269206 0.355747 11.00000 0.02618 0.02303 = 0.02784 -0.00249 -0.00064 -0.00111 C13A 1 0.057865 0.192398 0.400950 11.00000 0.02363 0.04740 = 0.02863 0.01058 0.00451 0.00306 C14A 1 -0.036850 0.179328 0.357538 11.00000 0.02617 0.06758 = 0.03306 0.00873 -0.00043 0.00054 AFIX 43 H14A 2 -0.111839 0.190807 0.339656 11.00000 -1.20000 AFIX 0 C15A 1 -0.024636 0.150652 0.340200 11.00000 0.03146 0.08216 = 0.03061 -0.00403 -0.00037 -0.01462 AFIX 43 H15A 2 -0.090272 0.142445 0.310584 11.00000 -1.20000 AFIX 0 C16A 1 0.084923 0.133356 0.366185 11.00000 0.04410 0.04751 = 0.03732 -0.00648 0.00692 -0.01269 AFIX 43 H16A 2 0.093524 0.113384 0.354157 11.00000 -1.20000 AFIX 0 C17A 1 0.180970 0.145280 0.409436 11.00000 0.03115 0.03690 = 0.03433 0.00187 0.00383 -0.00032 AFIX 43 H17A 2 0.255397 0.133662 0.427365 11.00000 -1.20000 AFIX 0 C18A 1 0.165992 0.174522 0.425933 11.00000 0.02428 0.03644 = 0.02536 0.00625 0.00256 -0.00199 C19A 1 0.264025 0.212839 0.491513 11.00000 0.02875 0.02804 = 0.03517 0.00216 0.00857 0.00092 C20A 1 0.371212 0.219074 0.535562 11.00000 0.03220 0.04319 = 0.03840 -0.00527 0.00490 -0.00099 AFIX 43 H20A 2 0.438365 0.204419 0.547636 11.00000 -1.20000 AFIX 0 C21A 1 0.379048 0.246589 0.561411 11.00000 0.04361 0.04715 = 0.05314 -0.01399 0.01087 -0.00722 AFIX 43 H21A 2 0.452310 0.251039 0.591317 11.00000 -1.20000 AFIX 0 C22A 1 0.280857 0.267836 0.544126 11.00000 0.05742 0.03936 = 0.05972 -0.01563 0.02422 -0.01085 AFIX 43 H22A 2 0.286473 0.286833 0.562226 11.00000 -1.20000 AFIX 0 C23A 1 0.175067 0.261482 0.500742 11.00000 0.04912 0.02946 = 0.06495 0.00816 0.02988 0.00938 AFIX 43 H23A 2 0.108220 0.276315 0.489413 11.00000 -1.20000 AFIX 0 C24A 1 0.162517 0.233495 0.472355 11.00000 0.03082 0.03052 = 0.04142 0.00863 0.01474 0.00423 B1A 3 -0.111385 0.258685 0.355356 11.00000 0.03012 0.02523 = 0.03370 -0.00119 -0.00210 0.00419 B2A 3 0.050135 0.224311 0.423753 11.00000 0.02872 0.04554 = 0.03808 0.01957 0.01119 0.01008 O1B 4 0.586470 0.131602 0.118899 11.00000 0.03491 0.05232 = 0.06506 -0.02714 0.00148 -0.01439 O2B 4 0.732371 0.199958 0.237739 11.00000 0.02665 0.03433 = 0.02612 -0.00444 0.00376 -0.00301 O3B 4 0.242126 0.085278 0.032995 11.00000 0.02919 0.03209 = 0.03655 -0.00523 -0.00387 -0.00393 C1B 1 0.537601 0.167619 0.205599 11.00000 0.02298 0.03210 = 0.03356 0.00859 -0.00180 -0.00063 C2B 1 0.396742 0.159716 0.216555 11.00000 0.02541 0.04146 = 0.04735 0.01023 -0.00275 -0.00300 AFIX 43 H2BA 2 0.351942 0.144855 0.191912 11.00000 -1.20000 AFIX 0 C3B 1 0.322688 0.172961 0.261950 11.00000 0.02246 0.06110 = 0.05047 0.02248 0.00654 0.00181 AFIX 43 H3BA 2 0.228164 0.167227 0.268372 11.00000 -1.20000 AFIX 0 C4B 1 0.386571 0.194655 0.298164 11.00000 0.03887 0.05710 = 0.03874 0.01193 0.01358 0.01287 AFIX 43 H4BA 2 0.335438 0.203714 0.329557 11.00000 -1.20000 AFIX 0 C5B 1 0.523238 0.203274 0.289279 11.00000 0.03654 0.04411 = 0.03008 0.00178 0.00787 0.00454 AFIX 43 H5BA 2 0.566670 0.218210 0.314168 11.00000 -1.20000 AFIX 0 C6B 1 0.596918 0.189678 0.243041 11.00000 0.02694 0.03021 = 0.02666 0.00682 0.00229 0.00151 C7B 1 0.819578 0.188949 0.194308 11.00000 0.02582 0.02804 = 0.02342 0.00005 0.00125 -0.00039 C8B 1 0.953232 0.201803 0.194705 11.00000 0.02860 0.03343 = 0.03071 0.00042 -0.00241 -0.00829 AFIX 43 H8BA 2 0.978373 0.216961 0.223224 11.00000 -1.20000 AFIX 0 C9B 1 1.047942 0.192213 0.153244 11.00000 0.02453 0.04432 = 0.03766 0.00548 0.00289 -0.00605 AFIX 43 H9BA 2 1.139280 0.200807 0.153252 11.00000 -1.20000 AFIX 0 C10B 1 1.011899 0.170151 0.111385 11.00000 0.03175 0.04640 = 0.03969 -0.00162 0.01106 0.00167 AFIX 43 H10B 2 1.078225 0.163603 0.082993 11.00000 -1.20000 AFIX 0 C11B 1 0.879491 0.157817 0.111260 11.00000 0.03544 0.03814 = 0.03565 -0.01024 0.00440 -0.00249 AFIX 43 H11B 2 0.854929 0.142899 0.082098 11.00000 -1.20000 AFIX 0 C12B 1 0.779079 0.166753 0.153363 11.00000 0.02806 0.02679 = 0.02832 -0.00099 -0.00070 -0.00177 C13B 1 0.368176 0.131773 0.045615 11.00000 0.03602 0.02893 = 0.03612 -0.00408 0.01442 -0.00252 C14B 1 0.374360 0.161218 0.026757 11.00000 0.05542 0.03240 = 0.05790 0.00402 0.02630 0.00132 AFIX 43 H14B 2 0.447232 0.173479 0.043907 11.00000 -1.20000 AFIX 0 C15B 1 0.279463 0.172657 -0.015175 11.00000 0.07948 0.04450 = 0.05880 0.01661 0.03122 0.01205 AFIX 43 H15B 2 0.286350 0.192676 -0.027106 11.00000 -1.20000 AFIX 0 C16B 1 0.171420 0.155016 -0.040893 11.00000 0.07760 0.07850 = 0.03394 0.02128 0.01596 0.04337 AFIX 43 H16B 2 0.105503 0.163134 -0.070504 11.00000 -1.20000 AFIX 0 C17B 1 0.159095 0.125690 -0.023689 11.00000 0.04543 0.06322 = 0.03041 -0.00066 0.00222 0.01447 AFIX 43 H17B 2 0.084957 0.113687 -0.040609 11.00000 -1.20000 AFIX 0 C18B 1 0.259194 0.114535 0.019196 11.00000 0.03265 0.03542 = 0.02598 -0.00127 0.00675 0.00472 C19B 1 0.336269 0.070663 0.072192 11.00000 0.02618 0.02915 = 0.03204 -0.00297 0.00598 -0.00190 C20B 1 0.307771 0.040872 0.079778 11.00000 0.03520 0.03176 = 0.06371 -0.00434 0.01450 -0.00618 AFIX 43 H20B 2 0.229303 0.031924 0.058356 11.00000 -1.20000 AFIX 0 C21B 1 0.395401 0.024728 0.118832 11.00000 0.04731 0.03687 = 0.07832 0.01750 0.02684 0.00584 AFIX 43 H21B 2 0.377120 0.004383 0.124264 11.00000 -1.20000 AFIX 0 C22B 1 0.509277 0.037408 0.150309 11.00000 0.04643 0.05899 = 0.05407 0.02349 0.01663 0.01665 AFIX 43 H22B 2 0.568578 0.025918 0.177329 11.00000 -1.20000 AFIX 0 C23B 1 0.536631 0.066828 0.142376 11.00000 0.03121 0.06096 = 0.03173 0.00271 0.00310 0.00543 AFIX 43 H23B 2 0.615768 0.075414 0.164009 11.00000 -1.20000 AFIX 0 C24B 1 0.450642 0.084493 0.103146 11.00000 0.02450 0.03828 = 0.02556 -0.00383 0.00614 -0.00228 B1B 3 0.629369 0.154038 0.156353 11.00000 0.03053 0.02797 = 0.03773 -0.00108 -0.00275 -0.00365 B2B 3 0.474256 0.117227 0.091526 11.00000 0.02615 0.03722 = 0.03269 -0.01282 0.00660 -0.00833 O1C 4 1.045139 0.154275 0.586128 11.00000 0.03609 0.03830 = 0.02966 -0.00312 -0.00639 0.01269 O2C 4 1.246918 0.115528 0.744422 11.00000 0.03085 0.07481 = 0.02786 0.01273 0.00405 0.01224 O3C 4 0.732183 0.214352 0.519192 11.00000 0.02867 0.02443 = 0.03491 -0.00115 -0.00441 0.00446 C1C 1 1.266423 0.134990 0.640584 11.00000 0.02773 0.02932 = 0.02647 -0.00140 -0.00010 0.00142 C2C 1 1.358232 0.139822 0.592454 11.00000 0.03439 0.03445 = 0.02659 -0.00148 0.00151 -0.00240 AFIX 43 H2CA 2 1.323303 0.149361 0.555949 11.00000 -1.20000 AFIX 0 C3C 1 1.497401 0.131031 0.597145 11.00000 0.03128 0.04919 = 0.03922 -0.00799 0.01050 -0.00529 AFIX 43 H3CA 2 1.557760 0.134564 0.564303 11.00000 -1.20000 AFIX 0 C4C 1 1.548824 0.116908 0.650512 11.00000 0.02320 0.06057 = 0.04815 -0.00754 -0.00077 0.00648 AFIX 43 H4CA 2 1.644324 0.110525 0.653551 11.00000 -1.20000 AFIX 0 C5C 1 1.463652 0.112095 0.698662 11.00000 0.03147 0.06251 = 0.03632 0.00305 -0.00487 0.01113 AFIX 43 H5CA 2 1.499829 0.102596 0.735005 11.00000 -1.20000 AFIX 0 C6C 1 1.323706 0.121269 0.693721 11.00000 0.02754 0.04567 = 0.02641 0.00045 0.00145 0.00507 C7C 1 1.107148 0.123562 0.746814 11.00000 0.02782 0.05672 = 0.02992 -0.00106 0.00566 0.00220 C8C 1 1.045316 0.116063 0.801497 11.00000 0.04619 0.08772 = 0.03345 0.00428 0.01027 0.00038 AFIX 43 H8CA 2 1.098700 0.106368 0.833559 11.00000 -1.20000 AFIX 0 C9C 1 0.905050 0.122968 0.808284 11.00000 0.04725 0.10078 = 0.04185 -0.00477 0.02158 -0.00991 AFIX 43 H9CA 2 0.861393 0.117877 0.845238 11.00000 -1.20000 AFIX 0 C10C 1 0.827141 0.137321 0.761446 11.00000 0.02878 0.07945 = 0.05885 -0.02190 0.01168 -0.00455 AFIX 43 H10C 2 0.731178 0.142317 0.766729 11.00000 -1.20000 AFIX 0 C11C 1 0.889404 0.144251 0.707506 11.00000 0.02734 0.04986 = 0.04578 -0.01389 0.00099 -0.00070 AFIX 43 H11C 2 0.834785 0.153766 0.675583 11.00000 -1.20000 AFIX 0 C12C 1 1.032491 0.137602 0.698251 11.00000 0.02550 0.03718 = 0.03514 -0.00829 0.00008 0.00143 C13C 1 0.831929 0.165004 0.514710 11.00000 0.02574 0.02837 = 0.02250 0.00230 0.00483 0.00205 C14C 1 0.819421 0.137269 0.487185 11.00000 0.03237 0.03001 = 0.02632 -0.00076 0.00277 0.00478 AFIX 43 H14C 2 0.885567 0.122361 0.498889 11.00000 -1.20000 AFIX 0 C15C 1 0.713431 0.131057 0.443494 11.00000 0.03855 0.03449 = 0.03266 -0.00672 0.00264 -0.00335 AFIX 43 H15C 2 0.706445 0.112016 0.425659 11.00000 -1.20000 AFIX 0 C16C 1 0.616658 0.152819 0.425626 11.00000 0.03228 0.04470 = 0.03149 -0.00229 -0.00486 -0.00264 AFIX 43 H16C 2 0.543456 0.148515 0.395594 11.00000 -1.20000 AFIX 0 C17C 1 0.625940 0.180462 0.450985 11.00000 0.02802 0.03927 = 0.03094 0.00203 -0.00281 0.00490 AFIX 43 H17C 2 0.560693 0.195384 0.438342 11.00000 -1.20000 AFIX 0 C18C 1 0.732872 0.186187 0.495594 11.00000 0.02569 0.02747 = 0.02652 0.00157 0.00385 -0.00021 C19C 1 0.832660 0.223772 0.562593 11.00000 0.02419 0.02899 = 0.02835 -0.00058 0.00373 -0.00186 C20C 1 0.819899 0.252997 0.580049 11.00000 0.03508 0.02941 = 0.04471 -0.00296 0.00924 0.00179 AFIX 43 H20C 2 0.746982 0.265031 0.562182 11.00000 -1.20000 AFIX 0 C21C 1 0.915336 0.264148 0.623854 11.00000 0.04363 0.03273 = 0.05179 -0.01501 0.01448 -0.00960 AFIX 43 H21C 2 0.907286 0.284029 0.636591 11.00000 -1.20000 AFIX 0 C22C 1 1.022956 0.246776 0.649617 11.00000 0.03508 0.04571 = 0.04266 -0.01378 0.00360 -0.01078 AFIX 43 H22C 2 1.088699 0.254793 0.679427 11.00000 -1.20000 AFIX 0 C23C 1 1.033972 0.218073 0.631915 11.00000 0.02720 0.04276 = 0.03394 -0.00560 0.00198 -0.00288 AFIX 43 H23C 2 1.107619 0.206284 0.649960 11.00000 -1.20000 AFIX 0 C24C 1 0.938793 0.205531 0.587560 11.00000 0.02296 0.03176 = 0.02619 0.00000 0.00483 -0.00054 B1C 3 1.109390 0.143718 0.638461 11.00000 0.02830 0.02656 = 0.02845 -0.00431 -0.00392 0.00254 B2C 3 0.944611 0.173612 0.564822 11.00000 0.02353 0.03158 = 0.02418 0.00240 0.00487 0.00388 O1D 4 1.081974 -0.028226 0.612555 11.00000 0.03456 0.03508 = 0.07048 0.01330 0.00119 0.00712 O2D 4 1.227115 -0.093043 0.740243 11.00000 0.03345 0.06531 = 0.02907 0.01095 0.00311 0.00656 O3D 4 0.729684 0.013148 0.520719 11.00000 0.03514 0.03369 = 0.04697 0.00786 0.00064 0.00535 C1D 1 1.033883 -0.060889 0.704966 11.00000 0.02758 0.04281 = 0.03469 -0.01453 -0.00126 -0.00082 C2D 1 0.893334 -0.052400 0.715162 11.00000 0.02891 0.06030 = 0.04627 -0.02133 -0.00009 0.00247 AFIX 43 H2DA 2 0.849323 -0.037922 0.689251 11.00000 -1.20000 AFIX 0 C3D 1 0.818425 -0.064573 0.761712 11.00000 0.03038 0.10004 = 0.05116 -0.03145 0.00997 -0.00374 AFIX 43 H3DA 2 0.724850 -0.058206 0.768170 11.00000 -1.20000 AFIX 0 C4D 1 0.880826 -0.086226 0.799118 11.00000 0.04551 0.12309 = 0.03847 -0.00321 0.01588 -0.01188 AFIX 43 H4DA 2 0.828618 -0.094945 0.830570 11.00000 -1.20000 AFIX 0 C5D 1 1.017105 -0.095129 0.791048 11.00000 0.04946 0.10036 = 0.03342 0.01184 0.00983 -0.00062 AFIX 43 H5DA 2 1.059726 -0.109835 0.816801 11.00000 -1.20000 AFIX 0 C6D 1 1.091938 -0.082210 0.744384 11.00000 0.02895 0.06144 = 0.02718 -0.00282 0.00141 0.00010 C7D 1 1.316219 -0.082590 0.696957 11.00000 0.02856 0.04164 = 0.02282 -0.00170 -0.00105 0.00116 C8D 1 1.449525 -0.095527 0.699090 11.00000 0.03497 0.04967 = 0.03224 0.00230 -0.00504 0.00915 AFIX 43 H8DA 2 1.473267 -0.110249 0.728804 11.00000 -1.20000 AFIX 0 C9D 1 1.546184 -0.086781 0.657822 11.00000 0.02623 0.04968 = 0.04071 -0.00821 -0.00112 0.00716 AFIX 43 H9DA 2 1.637351 -0.095497 0.659198 11.00000 -1.20000 AFIX 0 C10D 1 1.512465 -0.065360 0.614084 11.00000 0.03188 0.04579 = 0.03994 -0.00607 0.00655 -0.00245 AFIX 43 H10D 2 1.579892 -0.059401 0.585643 11.00000 -1.20000 AFIX 0 C11D 1 1.379591 -0.052811 0.612431 11.00000 0.03581 0.03187 = 0.03466 -0.00164 0.00189 -0.00101 AFIX 43 H11D 2 1.356701 -0.038204 0.582356 11.00000 -1.20000 AFIX 0 C12D 1 1.277091 -0.061002 0.653933 11.00000 0.02909 0.02929 = 0.02704 -0.00730 -0.00179 -0.00039 C13D 1 0.936291 0.017256 0.590923 11.00000 0.03120 0.02918 = 0.03587 0.00559 0.01066 0.00269 C14D 1 1.018939 0.036126 0.628802 11.00000 0.04023 0.03629 = 0.04313 0.00485 0.00860 -0.00099 AFIX 43 H14D 2 1.098367 0.028432 0.651767 11.00000 -1.20000 AFIX 0 C15D 1 0.987514 0.065490 0.633407 11.00000 0.05698 0.03470 = 0.04596 -0.00475 0.01481 -0.00598 AFIX 43 H15D 2 1.044004 0.077887 0.659718 11.00000 -1.20000 AFIX 0 C16D 1 0.872836 0.076915 0.599414 11.00000 0.05476 0.02511 = 0.05603 0.00016 0.02526 0.00310 AFIX 43 H16D 2 0.851944 0.097276 0.602357 11.00000 -1.20000 AFIX 0 C17D 1 0.788524 0.059301 0.561420 11.00000 0.03942 0.03418 = 0.05238 0.01104 0.01792 0.01198 AFIX 43 H17D 2 0.710387 0.067277 0.538034 11.00000 -1.20000 AFIX 0 C18D 1 0.820975 0.029471 0.558229 11.00000 0.03112 0.02870 = 0.03927 0.00620 0.01111 0.00242 C19D 1 0.751109 -0.016553 0.511564 11.00000 0.03754 0.03424 = 0.03647 0.00358 0.01075 -0.00152 C20D 1 0.652773 -0.029711 0.470608 11.00000 0.04763 0.05567 = 0.04067 0.00456 0.00324 -0.01077 AFIX 43 H20D 2 0.577114 -0.018649 0.452051 11.00000 -1.20000 AFIX 0 C21D 1 0.667961 -0.059277 0.457612 11.00000 0.06856 0.06057 = 0.03846 -0.00804 0.00999 -0.02600 AFIX 43 H21D 2 0.603012 -0.068542 0.429166 11.00000 -1.20000 AFIX 0 C22D 1 0.777147 -0.075610 0.485675 11.00000 0.06925 0.03861 = 0.05065 -0.00791 0.02010 -0.00911 AFIX 43 H22D 2 0.785881 -0.095959 0.476795 11.00000 -1.20000 AFIX 0 C23D 1 0.872018 -0.062261 0.526149 11.00000 0.05124 0.03117 = 0.05135 0.00018 0.02003 0.00227 AFIX 43 H23D 2 0.946157 -0.073597 0.545148 11.00000 -1.20000 AFIX 0 C24D 1 0.862379 -0.032242 0.540241 11.00000 0.03387 0.02953 = 0.04061 0.00329 0.01443 0.00218 B1D 3 1.126191 -0.048647 0.654237 11.00000 0.03148 0.02599 = 0.03604 -0.00908 -0.00202 0.00073 B2D 3 0.965989 -0.015546 0.583590 11.00000 0.02869 0.03257 = 0.04258 0.00958 0.01021 0.00511 O1E 4 0.443557 0.063041 0.908112 11.00000 0.04819 0.09782 = 0.05179 -0.03239 0.00958 -0.04011 O2E 4 0.780836 0.113763 0.986382 11.00000 0.02944 0.03006 = 0.03716 -0.00226 -0.00344 -0.00303 O3E 4 0.260079 0.017710 0.754816 11.00000 0.04388 0.06648 = 0.02870 -0.01208 0.00612 -0.01298 C1E 1 0.573248 0.111730 0.916715 11.00000 0.02661 0.05275 = 0.02545 -0.00072 0.00620 0.00337 C2E 1 0.483690 0.127674 0.875373 11.00000 0.03695 0.09176 = 0.03224 0.01176 0.00393 0.01600 AFIX 43 H2EA 2 0.406546 0.117924 0.854664 11.00000 -1.20000 AFIX 0 C3E 1 0.505106 0.156673 0.864438 11.00000 0.05441 0.09611 = 0.05489 0.03872 0.02006 0.03516 AFIX 43 H3EA 2 0.444014 0.166972 0.836005 11.00000 -1.20000 AFIX 0 C4E 1 0.616066 0.171166 0.894799 11.00000 0.06811 0.05202 = 0.07680 0.03546 0.04391 0.02783 AFIX 43 H4EA 2 0.630013 0.191496 0.887162 11.00000 -1.20000 AFIX 0 C5E 1 0.707008 0.156691 0.935990 11.00000 0.04370 0.03691 = 0.06060 0.00533 0.02300 0.00282 AFIX 43 H5EA 2 0.782768 0.166813 0.956873 11.00000 -1.20000 AFIX 0 C6E 1 0.684850 0.126904 0.946127 11.00000 0.02825 0.03362 = 0.02885 0.00270 0.00791 0.00336 C7E 1 0.769815 0.084676 1.002390 11.00000 0.03258 0.03128 = 0.02950 -0.00026 0.00732 0.00284 C8E 1 0.874931 0.075242 1.044939 11.00000 0.04147 0.06078 = 0.04181 0.00933 0.00244 0.01198 AFIX 43 H8EA 2 0.946172 0.088484 1.059814 11.00000 -1.20000 AFIX 0 C9E 1 0.874605 0.047034 1.064885 11.00000 0.06028 0.07037 = 0.06577 0.03007 0.02136 0.02469 AFIX 43 H9EA 2 0.945296 0.040499 1.094200 11.00000 -1.20000 AFIX 0 C10E 1 0.771488 0.027703 1.042647 11.00000 0.08267 0.04583 = 0.09094 0.03646 0.04996 0.03266 AFIX 43 H10E 2 0.772345 0.007893 1.056488 11.00000 -1.20000 AFIX 0 C11E 1 0.667040 0.037066 1.000331 11.00000 0.06511 0.03052 = 0.07994 -0.00609 0.04481 -0.00544 AFIX 43 H11E 2 0.596612 0.023579 0.985729 11.00000 -1.20000 AFIX 0 C12E 1 0.663511 0.066323 0.978539 11.00000 0.03656 0.02895 = 0.03954 -0.00497 0.01764 -0.00248 C13E 1 0.467879 0.042872 0.799473 11.00000 0.02767 0.03442 = 0.03457 0.01096 0.00235 0.00325 C14E 1 0.610106 0.050312 0.790618 11.00000 0.02922 0.05455 = 0.05293 0.02001 0.00632 0.00205 AFIX 43 H14E 2 0.661469 0.061056 0.821758 11.00000 -1.20000 AFIX 0 C15E 1 0.676094 0.042469 0.738364 11.00000 0.03607 0.08653 = 0.06530 0.03421 0.01748 0.01029 AFIX 43 H15E 2 0.771489 0.047979 0.733275 11.00000 -1.20000 AFIX 0 C16E 1 0.603133 0.026517 0.693177 11.00000 0.06771 0.10924 = 0.05128 0.01261 0.03477 0.01714 AFIX 43 H16E 2 0.649458 0.020911 0.657210 11.00000 -1.20000 AFIX 0 C17E 1 0.463959 0.018565 0.699348 11.00000 0.07213 0.09130 = 0.03804 -0.00712 0.02168 0.00149 AFIX 43 H17E 2 0.414212 0.007576 0.668115 11.00000 -1.20000 AFIX 0 C18E 1 0.398213 0.027052 0.752522 11.00000 0.03894 0.04710 = 0.03242 0.00294 0.00614 0.00004 C19E 1 0.179243 0.024515 0.803792 11.00000 0.03231 0.03789 = 0.02798 0.00098 -0.00031 -0.00302 C20E 1 0.041627 0.013719 0.799133 11.00000 0.03952 0.06079 = 0.03948 -0.00044 -0.00737 -0.01556 AFIX 43 H20E 2 0.009962 0.002585 0.764168 11.00000 -1.20000 AFIX 0 C21E 1 -0.047384 0.019297 0.845340 11.00000 0.02841 0.06139 = 0.05420 0.01401 -0.00241 -0.00822 AFIX 43 H21E 2 -0.141273 0.011951 0.842332 11.00000 -1.20000 AFIX 0 C22E 1 -0.002480 0.035507 0.896443 11.00000 0.03259 0.05106 = 0.04613 0.00662 0.01359 0.00603 AFIX 43 H22E 2 -0.065248 0.039463 0.928191 11.00000 -1.20000 AFIX 0 C23E 1 0.134005 0.045835 0.900800 11.00000 0.03808 0.03853 = 0.03626 -0.00487 0.00602 -0.00098 AFIX 43 H23E 2 0.164469 0.056890 0.936056 11.00000 -1.20000 AFIX 0 C24E 1 0.230033 0.040518 0.854560 11.00000 0.02857 0.02751 = 0.02811 0.00114 0.00121 0.00088 B1E 3 0.554475 0.079236 0.931915 11.00000 0.02959 0.05375 = 0.03183 -0.01561 0.01010 -0.01257 B2E 3 0.384914 0.050256 0.856854 11.00000 0.03310 0.03340 = 0.03346 -0.00016 -0.00096 -0.00538 HKLF 4 REM d1203 in P2(1)/n REM R1 = 0.0595 for 12861 Fo > 4sig(Fo) and 0.0721 for all 15900 data REM 1306 parameters refined using 0 restraints END WGHT 0.0558 6.8113 REM Highest difference peak 0.429, deepest hole -0.254, 1-sigma level 0.046 Q1 1 0.5606 0.1426 0.0887 11.00000 0.05 0.43 Q2 1 -0.0820 0.2322 0.3669 11.00000 0.05 0.33 Q3 1 1.0543 -0.0388 0.5831 11.00000 0.05 0.29 Q4 1 0.8801 0.1685 0.5418 11.00000 0.05 0.25 Q5 1 1.1992 0.1392 0.6430 11.00000 0.05 0.24 Q6 1 0.4441 0.1252 0.0588 11.00000 0.05 0.24 Q7 1 -0.2003 0.2644 0.3562 11.00000 0.05 0.22 Q8 1 0.3273 0.1591 -0.0033 11.00000 0.05 0.21 Q9 1 0.6070 0.0308 0.9770 11.00000 0.05 0.21 Q10 1 0.4136 0.0725 0.8806 11.00000 0.05 0.21 Q11 1 0.3037 0.0438 0.8573 11.00000 0.05 0.21 Q12 1 0.1005 0.1471 -0.0633 11.00000 0.05 0.21 Q13 1 0.2212 0.2744 0.5169 11.00000 0.05 0.20 Q14 1 0.7051 0.0234 1.0190 11.00000 0.05 0.20 Q15 1 0.7234 0.1605 0.1518 11.00000 0.05 0.19 Q16 1 0.9371 0.0022 0.5971 11.00000 0.05 0.19 Q17 1 0.1299 0.2290 0.4457 11.00000 0.05 0.19 Q18 1 -0.0028 0.1369 0.3726 11.00000 0.05 0.19 Q19 1 0.8164 0.0340 1.0396 11.00000 0.05 0.19 Q20 1 0.0947 0.1817 0.4214 11.00000 0.05 0.19 ; _database_code_depnum_ccdc_archive 'CCDC 935003' ####################################################################### # # 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_d1221 #TrackingRef '19659_web_deposit_cif_file_1_MarkS.Taylor_1366401291.2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 B2 N2 O' _chemical_formula_sum 'C26 H22 B2 N2 O' _chemical_formula_weight 400.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 10.6981(4) _cell_length_b 14.3379(7) _cell_length_c 26.3743(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4045.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 4684 _cell_measurement_theta_min 5.32 _cell_measurement_theta_max 65.23 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.610 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6416 _exptl_absorpt_correction_T_max 0.7527 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source "Bruker microsource'" _diffrn_radiation_monochromator 'muli-layer optics' _diffrn_measurement_device_type 'Bruker APEX DUOD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13911 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 66.11 _reflns_number_total 3362 _reflns_number_gt 2630 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.7160P] 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 3362 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.35736(10) 0.38015(9) 0.09677(4) 0.0371(3) Uani 1 1 d . . . N1 N 0.05418(12) 0.36258(10) -0.00804(5) 0.0315(3) Uani 1 1 d . . . N2 N 0.39161(13) 0.37434(11) 0.25747(5) 0.0375(4) Uani 1 1 d . . . C1 C 0.24979(14) 0.43751(12) 0.01752(6) 0.0281(4) Uani 1 1 d . . . C2 C 0.33976(15) 0.50641(12) 0.00834(6) 0.0326(4) Uani 1 1 d . . . H2A H 0.4074 0.5129 0.0314 0.039 Uiso 1 1 calc R . . C3 C 0.33365(17) 0.56467(14) -0.03271(7) 0.0403(5) Uani 1 1 d . . . H3A H 0.3959 0.6109 -0.0382 0.048 Uiso 1 1 calc R . . C4 C 0.23436(19) 0.55461(15) -0.06610(7) 0.0480(5) Uani 1 1 d . . . H4A H 0.2293 0.5944 -0.0948 0.058 Uiso 1 1 calc R . . C5 C 0.14326(17) 0.48864(14) -0.05863(7) 0.0411(5) Uani 1 1 d . . . H5A H 0.0763 0.4836 -0.0821 0.049 Uiso 1 1 calc R . . C6 C 0.14781(15) 0.42827(12) -0.01649(6) 0.0301(4) Uani 1 1 d . . . C7 C 0.05573(15) 0.30081(12) 0.03317(6) 0.0310(4) Uani 1 1 d . . . C8 C -0.04270(17) 0.23663(13) 0.03948(7) 0.0393(4) Uani 1 1 d . . . H8A H -0.1117 0.2378 0.0168 0.047 Uiso 1 1 calc R . . C9 C -0.04003(17) 0.17236(13) 0.07806(7) 0.0425(5) Uani 1 1 d . . . H9A H -0.1073 0.1296 0.0816 0.051 Uiso 1 1 calc R . . C10 C 0.05919(17) 0.16868(13) 0.11209(7) 0.0401(4) Uani 1 1 d . . . H10A H 0.0615 0.1228 0.1381 0.048 Uiso 1 1 calc R . . C11 C 0.15368(16) 0.23278(13) 0.10734(7) 0.0349(4) Uani 1 1 d . . . H11A H 0.2207 0.2314 0.1309 0.042 Uiso 1 1 calc R . . C12 C 0.15479(15) 0.30078(12) 0.06863(6) 0.0304(4) Uani 1 1 d . . . C13 C -0.05362(18) 0.36010(15) -0.04244(8) 0.0484(5) Uani 1 1 d . . . H13A H -0.0396 0.4034 -0.0706 0.073 Uiso 1 1 calc R . . H13B H -0.1291 0.3785 -0.0239 0.073 Uiso 1 1 calc R . . H13C H -0.0641 0.2967 -0.0557 0.073 Uiso 1 1 calc R . . C14 C 0.28826(15) 0.44109(12) 0.18307(6) 0.0324(4) Uani 1 1 d . . . C15 C 0.19897(16) 0.50430(13) 0.16440(7) 0.0419(5) Uani 1 1 d . . . H15A H 0.1930 0.5134 0.1288 0.050 Uiso 1 1 calc R . . C16 C 0.12022(19) 0.55327(15) 0.19557(9) 0.0499(5) Uani 1 1 d . . . H16A H 0.0626 0.5971 0.1820 0.060 Uiso 1 1 calc R . . C17 C 0.12666(19) 0.53722(14) 0.24739(9) 0.0497(5) Uani 1 1 d . . . H17A H 0.0689 0.5677 0.2692 0.060 Uiso 1 1 calc R . . C18 C 0.21392(18) 0.47873(14) 0.26790(7) 0.0430(5) Uani 1 1 d . . . H18A H 0.2170 0.4699 0.3036 0.052 Uiso 1 1 calc R . . C19 C 0.29947(15) 0.43132(12) 0.23633(6) 0.0334(4) Uani 1 1 d . . . C20 C 0.47484(15) 0.32218(12) 0.22857(6) 0.0327(4) Uani 1 1 d . . . C21 C 0.56311(18) 0.26400(14) 0.25272(8) 0.0450(5) Uani 1 1 d . . . H21A H 0.5637 0.2595 0.2887 0.054 Uiso 1 1 calc R . . C22 C 0.6476(2) 0.21418(15) 0.22501(9) 0.0537(6) Uani 1 1 d . . . H22A H 0.7061 0.1755 0.2421 0.064 Uiso 1 1 calc R . . C23 C 0.65022(18) 0.21875(14) 0.17251(9) 0.0498(5) Uani 1 1 d . . . H23A H 0.7104 0.1846 0.1536 0.060 Uiso 1 1 calc R . . C24 C 0.56357(16) 0.27392(13) 0.14843(7) 0.0380(4) Uani 1 1 d . . . H24A H 0.5645 0.2770 0.1125 0.046 Uiso 1 1 calc R . . C25 C 0.47376(15) 0.32580(12) 0.17503(6) 0.0308(4) Uani 1 1 d . . . C26 C 0.4075(2) 0.37486(19) 0.31271(8) 0.0656(7) Uani 1 1 d . . . H26A H 0.4962 0.3673 0.3210 0.098 Uiso 1 1 calc R . . H26B H 0.3597 0.3234 0.3276 0.098 Uiso 1 1 calc R . . H26C H 0.3773 0.4342 0.3264 0.098 Uiso 1 1 calc R . . B1 B 0.25843(17) 0.37336(14) 0.06365(7) 0.0292(4) Uani 1 1 d . . . B2 B 0.37221(17) 0.38282(14) 0.14866(7) 0.0316(4) 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 O1 0.0281(6) 0.0546(8) 0.0286(6) 0.0073(5) -0.0049(5) -0.0017(5) N1 0.0279(7) 0.0361(8) 0.0306(7) -0.0060(6) -0.0059(6) 0.0020(6) N2 0.0373(8) 0.0472(9) 0.0281(8) 0.0092(7) -0.0037(6) -0.0089(7) C1 0.0257(8) 0.0339(9) 0.0246(8) -0.0050(7) -0.0011(7) 0.0058(7) C2 0.0290(8) 0.0392(10) 0.0295(9) -0.0018(7) -0.0022(7) 0.0035(7) C3 0.0407(10) 0.0422(11) 0.0380(10) 0.0061(8) -0.0039(8) -0.0045(8) C4 0.0542(12) 0.0532(13) 0.0367(10) 0.0140(9) -0.0101(9) -0.0036(10) C5 0.0432(10) 0.0485(12) 0.0315(9) 0.0031(8) -0.0135(8) 0.0014(9) C6 0.0298(8) 0.0334(10) 0.0271(9) -0.0061(7) -0.0023(7) 0.0056(7) C7 0.0298(8) 0.0315(9) 0.0318(9) -0.0086(7) 0.0019(7) 0.0042(7) C8 0.0348(9) 0.0417(11) 0.0415(10) -0.0093(9) -0.0021(8) -0.0024(8) C9 0.0420(10) 0.0372(11) 0.0481(11) -0.0106(9) 0.0084(9) -0.0074(8) C10 0.0496(11) 0.0338(10) 0.0371(10) -0.0021(8) 0.0107(9) 0.0009(8) C11 0.0359(9) 0.0367(10) 0.0319(9) -0.0021(8) 0.0050(7) 0.0048(8) C12 0.0297(9) 0.0343(10) 0.0273(9) -0.0053(7) 0.0019(7) 0.0061(7) C13 0.0379(10) 0.0590(14) 0.0482(12) -0.0010(10) -0.0167(9) -0.0025(9) C14 0.0272(8) 0.0345(10) 0.0355(9) 0.0050(7) -0.0042(7) -0.0077(7) C15 0.0380(10) 0.0428(12) 0.0449(11) 0.0040(9) -0.0065(8) -0.0003(8) C16 0.0448(11) 0.0412(12) 0.0637(14) -0.0007(10) -0.0042(10) 0.0058(9) C17 0.0444(11) 0.0430(12) 0.0617(13) -0.0092(10) 0.0107(10) -0.0042(9) C18 0.0482(11) 0.0403(11) 0.0405(10) -0.0045(8) 0.0056(9) -0.0126(9) C19 0.0316(9) 0.0339(10) 0.0347(9) 0.0026(8) -0.0009(8) -0.0133(7) C20 0.0319(8) 0.0312(9) 0.0350(9) 0.0062(7) -0.0085(7) -0.0105(7) C21 0.0537(11) 0.0389(11) 0.0423(11) 0.0105(9) -0.0216(9) -0.0074(9) C22 0.0528(12) 0.0418(12) 0.0663(15) 0.0067(10) -0.0245(11) 0.0080(10) C23 0.0409(11) 0.0419(12) 0.0667(14) -0.0025(10) -0.0113(10) 0.0065(9) C24 0.0334(9) 0.0385(11) 0.0421(10) -0.0003(8) -0.0073(8) -0.0064(8) C25 0.0276(8) 0.0310(9) 0.0339(9) 0.0043(7) -0.0058(7) -0.0090(7) C26 0.0656(14) 0.100(2) 0.0308(11) 0.0123(12) -0.0006(10) 0.0061(14) B1 0.0240(9) 0.0385(11) 0.0251(9) -0.0034(8) 0.0009(8) 0.0076(8) B2 0.0267(9) 0.0380(12) 0.0302(10) 0.0079(8) -0.0049(8) -0.0100(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 B1 1.376(2) . ? O1 B2 1.378(2) . ? N1 C6 1.393(2) . ? N1 C7 1.402(2) . ? N1 C13 1.468(2) . ? N2 C20 1.390(2) . ? N2 C19 1.396(2) . ? N2 C26 1.467(2) . ? C1 C2 1.400(2) . ? C1 C6 1.419(2) . ? C1 B1 1.528(2) . ? C2 C3 1.369(2) . ? C2 H2A 0.9500 . ? C3 C4 1.387(3) . ? C3 H3A 0.9500 . ? C4 C5 1.372(3) . ? C4 H4A 0.9500 . ? C5 C6 1.410(2) . ? C5 H5A 0.9500 . ? C7 C8 1.408(2) . ? C7 C12 1.414(2) . ? C8 C9 1.373(3) . ? C8 H8A 0.9500 . ? C9 C10 1.391(3) . ? C9 H9A 0.9500 . ? C10 C11 1.372(3) . ? C10 H10A 0.9500 . ? C11 C12 1.412(2) . ? C11 H11A 0.9500 . ? C12 B1 1.526(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.406(2) . ? C14 C19 1.417(2) . ? C14 B2 1.526(3) . ? C15 C16 1.371(3) . ? C15 H15A 0.9500 . ? C16 C17 1.387(3) . ? C16 H16A 0.9500 . ? C17 C18 1.367(3) . ? C17 H17A 0.9500 . ? C18 C19 1.412(3) . ? C18 H18A 0.9500 . ? C20 C21 1.412(2) . ? C20 C25 1.413(2) . ? C21 C22 1.364(3) . ? C21 H21A 0.9500 . ? C22 C23 1.387(3) . ? C22 H22A 0.9500 . ? C23 C24 1.374(3) . ? C23 H23A 0.9500 . ? C24 C25 1.403(3) . ? C24 H24A 0.9500 . ? C25 B2 1.527(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 B1 O1 B2 136.15(14) . . ? C6 N1 C7 122.87(13) . . ? C6 N1 C13 118.85(14) . . ? C7 N1 C13 118.23(14) . . ? C20 N2 C19 123.22(14) . . ? C20 N2 C26 118.23(15) . . ? C19 N2 C26 118.39(16) . . ? C2 C1 C6 119.02(15) . . ? C2 C1 B1 121.38(15) . . ? C6 C1 B1 119.59(15) . . ? C3 C2 C1 122.30(16) . . ? C3 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C2 C3 C4 118.37(17) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? C5 C4 C3 121.62(17) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 120.79(16) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? N1 C6 C5 121.10(15) . . ? N1 C6 C1 121.00(15) . . ? C5 C6 C1 117.89(16) . . ? N1 C7 C8 119.71(15) . . ? N1 C7 C12 121.47(15) . . ? C8 C7 C12 118.82(16) . . ? C9 C8 C7 120.70(17) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 121.30(17) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C11 C10 C9 118.55(18) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? C10 C11 C12 122.34(17) . . ? C10 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C11 C12 C7 118.20(16) . . ? C11 C12 B1 122.64(15) . . ? C7 C12 B1 119.17(15) . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.94(16) . . ? C15 C14 B2 122.99(16) . . ? C19 C14 B2 119.06(15) . . ? C16 C15 C14 122.53(18) . . ? C16 C15 H15A 118.7 . . ? C14 C15 H15A 118.7 . . ? C15 C16 C17 118.38(19) . . ? C15 C16 H16A 120.8 . . ? C17 C16 H16A 120.8 . . ? C18 C17 C16 121.71(19) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 120.32(18) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? N2 C19 C18 120.25(16) . . ? N2 C19 C14 120.90(15) . . ? C18 C19 C14 118.84(16) . . ? N2 C20 C21 119.93(16) . . ? N2 C20 C25 121.52(15) . . ? C21 C20 C25 118.55(17) . . ? C22 C21 C20 120.73(19) . . ? C22 C21 H21A 119.6 . . ? C20 C21 H21A 119.6 . . ? C21 C22 C23 121.56(18) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C24 C23 C22 118.37(19) . . ? C24 C23 H23A 120.8 . . ? C22 C23 H23A 120.8 . . ? C23 C24 C25 122.41(18) . . ? C23 C24 H24A 118.8 . . ? C25 C24 H24A 118.8 . . ? C24 C25 C20 118.34(16) . . ? C24 C25 B2 122.90(16) . . ? C20 C25 B2 118.72(16) . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 B1 C12 123.53(16) . . ? O1 B1 C1 120.63(16) . . ? C12 B1 C1 115.79(15) . . ? O1 B2 C14 122.54(15) . . ? O1 B2 C25 121.29(17) . . ? C14 B2 C25 116.16(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.8(2) . . . . ? B1 C1 C2 C3 -179.90(16) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C3 C4 C5 C6 -0.1(3) . . . . ? C7 N1 C6 C5 179.49(15) . . . . ? C13 N1 C6 C5 -3.1(2) . . . . ? C7 N1 C6 C1 -1.5(2) . . . . ? C13 N1 C6 C1 175.89(15) . . . . ? C4 C5 C6 N1 178.51(17) . . . . ? C4 C5 C6 C1 -0.5(3) . . . . ? C2 C1 C6 N1 -178.08(14) . . . . ? B1 C1 C6 N1 1.1(2) . . . . ? C2 C1 C6 C5 0.9(2) . . . . ? B1 C1 C6 C5 -179.91(15) . . . . ? C6 N1 C7 C8 179.57(15) . . . . ? C13 N1 C7 C8 2.1(2) . . . . ? C6 N1 C7 C12 -0.9(2) . . . . ? C13 N1 C7 C12 -178.35(16) . . . . ? N1 C7 C8 C9 176.68(15) . . . . ? C12 C7 C8 C9 -2.8(2) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? C8 C9 C10 C11 1.9(3) . . . . ? C9 C10 C11 C12 -1.3(3) . . . . ? C10 C11 C12 C7 -1.3(2) . . . . ? C10 C11 C12 B1 178.93(16) . . . . ? N1 C7 C12 C11 -176.19(15) . . . . ? C8 C7 C12 C11 3.3(2) . . . . ? N1 C7 C12 B1 3.6(2) . . . . ? C8 C7 C12 B1 -176.89(15) . . . . ? C19 C14 C15 C16 -2.6(3) . . . . ? B2 C14 C15 C16 177.05(17) . . . . ? C14 C15 C16 C17 -2.1(3) . . . . ? C15 C16 C17 C18 4.1(3) . . . . ? C16 C17 C18 C19 -1.1(3) . . . . ? C20 N2 C19 C18 176.77(15) . . . . ? C26 N2 C19 C18 -7.9(2) . . . . ? C20 N2 C19 C14 -1.9(2) . . . . ? C26 N2 C19 C14 173.45(17) . . . . ? C17 C18 C19 N2 177.56(16) . . . . ? C17 C18 C19 C14 -3.8(3) . . . . ? C15 C14 C19 N2 -175.84(16) . . . . ? B2 C14 C19 N2 4.5(2) . . . . ? C15 C14 C19 C18 5.5(2) . . . . ? B2 C14 C19 C18 -174.16(15) . . . . ? C19 N2 C20 C21 -178.12(15) . . . . ? C26 N2 C20 C21 6.6(2) . . . . ? C19 N2 C20 C25 2.0(2) . . . . ? C26 N2 C20 C25 -173.35(17) . . . . ? N2 C20 C21 C22 -178.28(17) . . . . ? C25 C20 C21 C22 1.7(3) . . . . ? C20 C21 C22 C23 0.1(3) . . . . ? C21 C22 C23 C24 -1.1(3) . . . . ? C22 C23 C24 C25 0.4(3) . . . . ? C23 C24 C25 C20 1.3(3) . . . . ? C23 C24 C25 B2 -176.31(17) . . . . ? N2 C20 C25 C24 177.65(15) . . . . ? C21 C20 C25 C24 -2.3(2) . . . . ? N2 C20 C25 B2 -4.6(2) . . . . ? C21 C20 C25 B2 175.43(16) . . . . ? B2 O1 B1 C12 -48.7(3) . . . . ? B2 O1 B1 C1 133.9(2) . . . . ? C11 C12 B1 O1 -1.5(3) . . . . ? C7 C12 B1 O1 178.72(15) . . . . ? C11 C12 B1 C1 176.00(15) . . . . ? C7 C12 B1 C1 -3.8(2) . . . . ? C2 C1 B1 O1 -1.8(2) . . . . ? C6 C1 B1 O1 179.09(15) . . . . ? C2 C1 B1 C12 -179.36(15) . . . . ? C6 C1 B1 C12 1.5(2) . . . . ? B1 O1 B2 C14 -43.4(3) . . . . ? B1 O1 B2 C25 135.7(2) . . . . ? C15 C14 B2 O1 -7.4(3) . . . . ? C19 C14 B2 O1 172.30(15) . . . . ? C15 C14 B2 C25 173.46(16) . . . . ? C19 C14 B2 C25 -6.9(2) . . . . ? C24 C25 B2 O1 5.3(3) . . . . ? C20 C25 B2 O1 -172.25(15) . . . . ? C24 C25 B2 C14 -175.47(15) . . . . ? C20 C25 B2 C14 6.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 66.11 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.271 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.044 _iucr_refine_instructions_details ; TITL cu_d1221_0m in Pbca CELL 1.54178 10.6981 14.3379 26.3743 90.000 90.000 90.000 ZERR 8.00 0.0004 0.0007 0.0011 0.000 0.000 0.000 LATT 1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H O B N UNIT 208 176 8 16 16 TEMP -123.140 SIZE 0.030 0.090 0.100 ACTA L.S. 12 FMAP 2 PLAN 20 HTAB BOND $H CONF WGHT 0.065100 0.716000 FVAR 0.09577 O1 3 0.357356 0.380148 0.096768 11.00000 0.02809 0.05455 = 0.02861 0.00727 -0.00495 -0.00173 N1 5 0.054181 0.362585 -0.008042 11.00000 0.02795 0.03609 = 0.03058 -0.00598 -0.00593 0.00196 N2 5 0.391611 0.374343 0.257473 11.00000 0.03728 0.04718 = 0.02815 0.00920 -0.00370 -0.00891 C1 1 0.249787 0.437507 0.017518 11.00000 0.02571 0.03392 = 0.02457 -0.00497 -0.00114 0.00577 C2 1 0.339764 0.506405 0.008337 11.00000 0.02899 0.03920 = 0.02949 -0.00179 -0.00219 0.00345 AFIX 43 H2A 2 0.407410 0.512943 0.031400 11.00000 -1.20000 AFIX 0 C3 1 0.333654 0.564671 -0.032713 11.00000 0.04072 0.04223 = 0.03797 0.00610 -0.00394 -0.00452 AFIX 43 H3A 2 0.395879 0.610852 -0.038199 11.00000 -1.20000 AFIX 0 C4 1 0.234358 0.554615 -0.066101 11.00000 0.05422 0.05318 = 0.03673 0.01399 -0.01005 -0.00356 AFIX 43 H4A 2 0.229299 0.594378 -0.094841 11.00000 -1.20000 AFIX 0 C5 1 0.143261 0.488637 -0.058635 11.00000 0.04319 0.04846 = 0.03151 0.00311 -0.01353 0.00141 AFIX 43 H5A 2 0.076335 0.483592 -0.082150 11.00000 -1.20000 AFIX 0 C6 1 0.147808 0.428266 -0.016493 11.00000 0.02976 0.03335 = 0.02708 -0.00610 -0.00229 0.00563 C7 1 0.055729 0.300810 0.033166 11.00000 0.02982 0.03149 = 0.03179 -0.00861 0.00195 0.00420 C8 1 -0.042702 0.236631 0.039481 11.00000 0.03482 0.04165 = 0.04151 -0.00933 -0.00209 -0.00239 AFIX 43 H8A 2 -0.111684 0.237820 0.016808 11.00000 -1.20000 AFIX 0 C9 1 -0.040030 0.172359 0.078059 11.00000 0.04203 0.03719 = 0.04814 -0.01060 0.00839 -0.00736 AFIX 43 H9A 2 -0.107262 0.129560 0.081578 11.00000 -1.20000 AFIX 0 C10 1 0.059187 0.168680 0.112092 11.00000 0.04956 0.03382 = 0.03706 -0.00210 0.01073 0.00095 AFIX 43 H10A 2 0.061464 0.122786 0.138056 11.00000 -1.20000 AFIX 0 C11 1 0.153679 0.232779 0.107340 11.00000 0.03593 0.03669 = 0.03194 -0.00207 0.00504 0.00480 AFIX 43 H11A 2 0.220747 0.231353 0.130936 11.00000 -1.20000 AFIX 0 C12 1 0.154787 0.300779 0.068634 11.00000 0.02974 0.03429 = 0.02726 -0.00527 0.00185 0.00614 C13 1 -0.053625 0.360100 -0.042442 11.00000 0.03792 0.05904 = 0.04817 -0.00102 -0.01672 -0.00254 AFIX 137 H13A 2 -0.039598 0.403371 -0.070637 11.00000 -1.50000 H13B 2 -0.129131 0.378529 -0.023941 11.00000 -1.50000 H13C 2 -0.064123 0.296742 -0.055715 11.00000 -1.50000 AFIX 0 C14 1 0.288259 0.441090 0.183074 11.00000 0.02717 0.03454 = 0.03553 0.00498 -0.00424 -0.00769 C15 1 0.198970 0.504296 0.164401 11.00000 0.03799 0.04280 = 0.04485 0.00402 -0.00645 -0.00029 AFIX 43 H15A 2 0.192979 0.513416 0.128807 11.00000 -1.20000 AFIX 0 C16 1 0.120222 0.553272 0.195574 11.00000 0.04476 0.04122 = 0.06367 -0.00074 -0.00425 0.00580 AFIX 43 H16A 2 0.062640 0.597134 0.182034 11.00000 -1.20000 AFIX 0 C17 1 0.126661 0.537222 0.247386 11.00000 0.04439 0.04300 = 0.06169 -0.00920 0.01073 -0.00424 AFIX 43 H17A 2 0.068911 0.567687 0.269168 11.00000 -1.20000 AFIX 0 C18 1 0.213918 0.478730 0.267900 11.00000 0.04825 0.04032 = 0.04054 -0.00453 0.00558 -0.01260 AFIX 43 H18A 2 0.217021 0.469925 0.303578 11.00000 -1.20000 AFIX 0 C19 1 0.299473 0.431325 0.236328 11.00000 0.03163 0.03385 = 0.03473 0.00257 -0.00089 -0.01332 C20 1 0.474839 0.322175 0.228573 11.00000 0.03186 0.03118 = 0.03496 0.00624 -0.00846 -0.01049 C21 1 0.563111 0.263996 0.252721 11.00000 0.05372 0.03892 = 0.04233 0.01045 -0.02164 -0.00744 AFIX 43 H21A 2 0.563667 0.259480 0.288656 11.00000 -1.20000 AFIX 0 C22 1 0.647630 0.214184 0.225013 11.00000 0.05276 0.04184 = 0.06635 0.00667 -0.02445 0.00805 AFIX 43 H22A 2 0.706088 0.175457 0.242099 11.00000 -1.20000 AFIX 0 C23 1 0.650225 0.218745 0.172509 11.00000 0.04087 0.04194 = 0.06671 -0.00248 -0.01132 0.00645 AFIX 43 H23A 2 0.710430 0.184569 0.153645 11.00000 -1.20000 AFIX 0 C24 1 0.563566 0.273920 0.148430 11.00000 0.03337 0.03846 = 0.04209 -0.00029 -0.00727 -0.00643 AFIX 43 H24A 2 0.564500 0.277050 0.112452 11.00000 -1.20000 AFIX 0 C25 1 0.473765 0.325795 0.175035 11.00000 0.02763 0.03097 = 0.03394 0.00431 -0.00577 -0.00901 C26 1 0.407506 0.374860 0.312712 11.00000 0.06558 0.10031 = 0.03084 0.01228 -0.00064 0.00606 AFIX 137 H26A 2 0.496226 0.367308 0.321002 11.00000 -1.50000 H26B 2 0.359659 0.323399 0.327589 11.00000 -1.50000 H26C 2 0.377253 0.434220 0.326450 11.00000 -1.50000 AFIX 0 B1 4 0.258429 0.373357 0.063646 11.00000 0.02403 0.03853 = 0.02509 -0.00339 0.00085 0.00760 B2 4 0.372213 0.382824 0.148663 11.00000 0.02667 0.03801 = 0.03023 0.00790 -0.00491 -0.01004 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM cu_d1221_0m in Pbca REM R1 = 0.0445 for 2630 Fo > 4sig(Fo) and 0.0595 for all 3362 data REM 282 parameters refined using 0 restraints END WGHT 0.0669 0.9105 REM Highest difference peak 0.271, deepest hole -0.251, 1-sigma level 0.044 Q1 1 -0.0939 0.4351 -0.0438 11.00000 0.05 0.27 Q2 1 -0.0187 0.3543 -0.0873 11.00000 0.05 0.24 Q3 1 0.4114 0.2912 0.3164 11.00000 0.05 0.21 Q4 1 0.3127 0.3587 0.3284 11.00000 0.05 0.21 Q5 1 0.6650 0.1385 0.2529 11.00000 0.05 0.12 Q6 1 0.0400 0.5135 -0.0694 11.00000 0.05 0.12 Q7 1 0.3958 0.5242 0.2876 11.00000 0.05 0.12 Q8 1 0.5160 0.4015 0.3222 11.00000 0.05 0.11 Q9 1 0.4524 0.1952 0.1490 11.00000 0.05 0.11 Q10 1 0.1802 0.3523 0.0728 11.00000 0.05 0.11 Q11 1 0.2961 0.2385 0.1958 11.00000 0.05 0.11 Q12 1 0.1646 0.4004 0.2938 11.00000 0.05 0.11 Q13 1 0.4517 0.3734 0.1645 11.00000 0.05 0.11 Q14 1 0.7504 0.1037 0.2438 11.00000 0.05 0.10 Q15 1 0.2155 0.4231 -0.0002 11.00000 0.05 0.10 Q16 1 0.6937 0.3179 0.2622 11.00000 0.05 0.10 Q17 1 0.8195 0.2233 0.2903 11.00000 0.05 0.10 Q18 1 0.3763 0.6576 -0.0237 11.00000 0.05 0.10 Q19 1 0.5138 0.2584 0.3093 11.00000 0.05 0.10 Q20 1 -0.0560 0.2393 0.0710 11.00000 0.05 0.10 ; _vrf_PLAT029_d1221 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.951 RESPONSE: Data were collected on a very small crystal using CuKalpha radiation using a Bruker Microsource system eqipped with multi layer optics. Without this type of instrumentation we would not have been able to collect sufficient data to aquire a crystal structure. We feel that the precision of the structure is good enough to support any claims made regadring the geometry of the molecule and the intermolecular distances. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 935004'