# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email J.D.Kennedy@chemistry.leeds.ac.uk _publ_contact_author_name 'Professor John D. Kennedy' _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.D.Kennedy A.Franken C.Kilner data_c:AFXV93A _database_code_depnum_ccdc_archive 'CCDC 211907' _chemical_name_common '(NEt4)+(2-(HOOC-C6H4)-closo-2-CB9H9)- * (NEt4)+Br-' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ; 3(C8H20N)+, 2(C8H14B9O2)-, Br- ; _chemical_formula_sum 'C40 H88 B18 Br N3 O4' _chemical_formula_weight 949.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.2400(4) _cell_length_b 20.6240(4) _cell_length_c 11.8850(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.3860(10) _cell_angle_gamma 90.00 _cell_volume 5541.74(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51672 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7994 _exptl_absorpt_correction_T_max 0.9330 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 54783 _diffrn_reflns_av_R_equivalents 0.1082 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6354 _reflns_number_gt 4834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0709P)^2^+13.7191P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6354 _refine_ls_number_parameters 301 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.031 _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 Br1 Br 1.0000 0.48075(2) -0.2500 0.05427(18) Uani 1 2 d S . . O1 O 1.00993(10) 0.32403(11) -0.0937(2) 0.0496(5) Uani 1 1 d . . . N1 N 0.84781(10) 0.39737(11) 0.38716(19) 0.0315(5) Uani 1 1 d . . . B1 B 0.85156(15) 0.07528(17) 0.1294(4) 0.0464(9) Uani 1 1 d . . . H1 H 0.8633 0.0534 0.0514 0.056 Uiso 1 1 calc R . . O2 O 0.92465(11) 0.37763(12) -0.1443(2) 0.0585(6) Uani 1 1 d . . . C2 C 0.85391(11) 0.14990(13) 0.1773(2) 0.0340(6) Uani 1 1 d . . . B3 B 0.89336(15) 0.08840(17) 0.2640(4) 0.0462(9) Uani 1 1 d . . . H3 H 0.9408 0.0727 0.2826 0.055 Uiso 1 1 calc R . . B4 B 0.82566(16) 0.04092(18) 0.2376(4) 0.0481(9) Uani 1 1 d . . . H4 H 0.8180 -0.0127 0.2354 0.058 Uiso 1 1 calc R . . B5 B 0.78660(15) 0.10613(18) 0.1471(3) 0.0433(8) Uani 1 1 d . . . H5 H 0.7475 0.1049 0.0715 0.052 Uiso 1 1 calc R . . B6 B 0.87392(14) 0.16153(16) 0.3274(3) 0.0391(7) Uani 1 1 d . . . H6 H 0.9090 0.1968 0.3695 0.047 Uiso 1 1 calc R . . B7 B 0.85312(17) 0.08292(19) 0.3745(4) 0.0498(9) Uani 1 1 d . . . H7 H 0.8712 0.0547 0.4554 0.060 Uiso 1 1 calc R . . B8 B 0.77666(16) 0.09561(18) 0.2906(3) 0.0455(8) Uani 1 1 d . . . H8 H 0.7335 0.0774 0.3047 0.055 Uiso 1 1 calc R . . B9 B 0.79743(13) 0.17474(16) 0.2436(3) 0.0363(7) Uani 1 1 d . . . H9 H 0.7714 0.2203 0.2188 0.044 Uiso 1 1 calc R . . B10 B 0.81455(16) 0.15197(18) 0.3841(3) 0.0455(8) Uani 1 1 d . . . H10 H 0.8034 0.1757 0.4612 0.055 Uiso 1 1 calc R . . C21 C 0.87770(11) 0.19839(13) 0.1060(2) 0.0325(6) Uani 1 1 d . . . C22 C 0.93873(11) 0.19963(14) 0.1141(2) 0.0340(6) Uani 1 1 d . . . H22 H 0.9636 0.1699 0.1639 0.041 Uiso 1 1 calc R . . C23 C 0.96318(12) 0.24306(14) 0.0510(2) 0.0351(6) Uani 1 1 d . . . H23 H 1.0048 0.2433 0.0584 0.042 Uiso 1 1 calc R . . C24 C 0.92790(12) 0.28675(14) -0.0235(2) 0.0365(6) Uani 1 1 d . . . C25 C 0.86718(13) 0.28544(15) -0.0332(3) 0.0433(7) Uani 1 1 d . . . H25 H 0.8424 0.3148 -0.0841 0.052 Uiso 1 1 calc R . . C26 C 0.84254(12) 0.24182(16) 0.0307(3) 0.0430(7) Uani 1 1 d . . . H26 H 0.8009 0.2415 0.0229 0.052 Uiso 1 1 calc R . . C27 C 0.95886(14) 0.33093(15) -0.0896(3) 0.0411(7) Uani 1 1 d . . . C28 C 0.88233(12) 0.34196(13) 0.3497(2) 0.0328(6) Uani 1 1 d . . . H28A H 0.9086 0.3230 0.4195 0.039 Uiso 1 1 calc R . . H28B H 0.8540 0.3079 0.3138 0.039 Uiso 1 1 calc R . . C29 C 0.91937(16) 0.36021(16) 0.2657(3) 0.0497(8) Uani 1 1 d . . . H29A H 0.8937 0.3770 0.1944 0.074 Uiso 1 1 calc R . . H29B H 0.9405 0.3219 0.2479 0.074 Uiso 1 1 calc R . . H29C H 0.9480 0.3936 0.3003 0.074 Uiso 1 1 calc R . . C30 C 0.80916(15) 0.43137(16) 0.2839(3) 0.0465(8) Uani 1 1 d . . . H30A H 0.7853 0.4645 0.3126 0.056 Uiso 1 1 calc R . . H30B H 0.8351 0.4544 0.2417 0.056 Uiso 1 1 calc R . . C31 C 0.76775(18) 0.3882(2) 0.1993(3) 0.0683(12) Uani 1 1 d . . . H31A H 0.7908 0.3566 0.1665 0.102 Uiso 1 1 calc R . . H31B H 0.7441 0.4146 0.1370 0.102 Uiso 1 1 calc R . . H31C H 0.7415 0.3652 0.2395 0.102 Uiso 1 1 calc R . . C32 C 0.89122(14) 0.44638(15) 0.4554(3) 0.0444(7) Uani 1 1 d . . . H32A H 0.9185 0.4234 0.5193 0.053 Uiso 1 1 calc R . . H32B H 0.9152 0.4645 0.4040 0.053 Uiso 1 1 calc R . . C33 C 0.86261(19) 0.5020(2) 0.5059(4) 0.0661(11) Uani 1 1 d . . . H33A H 0.8369 0.5264 0.4432 0.099 Uiso 1 1 calc R . . H33B H 0.8934 0.5308 0.5494 0.099 Uiso 1 1 calc R . . H33C H 0.8391 0.4848 0.5577 0.099 Uiso 1 1 calc R . . C34 C 0.80842(13) 0.36865(16) 0.4602(3) 0.0411(7) Uani 1 1 d . . . H34A H 0.7829 0.4035 0.4791 0.049 Uiso 1 1 calc R . . H34B H 0.7823 0.3358 0.4136 0.049 Uiso 1 1 calc R . . C35 C 0.84124(17) 0.3375(2) 0.5711(3) 0.0629(10) Uani 1 1 d . . . H35A H 0.8658 0.3021 0.5535 0.094 Uiso 1 1 calc R . . H35B H 0.8128 0.3204 0.6129 0.094 Uiso 1 1 calc R . . H35C H 0.8665 0.3699 0.6192 0.094 Uiso 1 1 calc R . . N1A N 1.0000 0.12367(16) 0.7500 0.0378(7) Uiso 1 2 d SD . . C1A C 1.0296(3) 0.0648(3) 0.7164(5) 0.0455(14) Uiso 0.50 1 d PDU A -1 H1A1 H 1.0035 0.0268 0.7152 0.055 Uiso 0.50 1 calc PR A -1 H1A2 H 1.0667 0.0566 0.7754 0.055 Uiso 0.50 1 calc PR A -1 C2A C 1.0439(4) 0.0717(5) 0.5997(8) 0.057(3) Uiso 0.50 1 d PDU A -1 H2A1 H 1.0101 0.0911 0.5453 0.086 Uiso 0.50 1 calc PR A -1 H2A2 H 1.0522 0.0289 0.5714 0.086 Uiso 0.50 1 calc PR A -1 H2A3 H 1.0786 0.0997 0.6064 0.086 Uiso 0.50 1 calc PR A -1 C3A C 1.0322(3) 0.1850(4) 0.7378(7) 0.0597(18) Uiso 0.50 1 d PDU A -1 H3A1 H 1.0287 0.1918 0.6540 0.072 Uiso 0.50 1 calc PR A -1 H3A2 H 1.0102 0.2207 0.7645 0.072 Uiso 0.50 1 calc PR A -1 C4A C 1.0907(4) 0.1932(5) 0.7912(8) 0.066(2) Uiso 0.50 1 d PDU A -1 H4A1 H 1.0962 0.1863 0.8746 0.099 Uiso 0.50 1 calc PR A -1 H4A2 H 1.1031 0.2373 0.7771 0.099 Uiso 0.50 1 calc PR A -1 H4A3 H 1.1147 0.1619 0.7600 0.099 Uiso 0.50 1 calc PR A -1 C1B C 1.0632(3) 0.1273(4) 0.8154(7) 0.0589(18) Uiso 0.50 1 d PDU A -2 H1B1 H 1.0796 0.0829 0.8164 0.071 Uiso 0.50 1 calc PR A -2 H1B2 H 1.0629 0.1382 0.8964 0.071 Uiso 0.50 1 calc PR A -2 C4B C 1.0294(4) 0.0615(4) 0.5826(8) 0.053(2) Uiso 0.50 1 d PDU A -2 H4B1 H 1.0716 0.0641 0.6201 0.080 Uiso 0.50 1 calc PR A -2 H4B2 H 1.0244 0.0620 0.4984 0.080 Uiso 0.50 1 calc PR A -2 H4B3 H 1.0130 0.0212 0.6058 0.080 Uiso 0.50 1 calc PR A -2 C3B C 0.9983(3) 0.1172(3) 0.6180(5) 0.0423(13) Uiso 0.50 1 d PDU A -2 H3B1 H 0.9564 0.1151 0.5753 0.051 Uiso 0.50 1 calc PR A -2 H3B2 H 1.0153 0.1573 0.5930 0.051 Uiso 0.50 1 calc PR A -2 C2B C 1.1072(4) 0.1723(5) 0.7798(8) 0.067(2) Uiso 0.50 1 d PDU A -2 H2B1 H 1.1298 0.1484 0.7333 0.101 Uiso 0.50 1 calc PR A -2 H2B2 H 1.1342 0.1897 0.8490 0.101 Uiso 0.50 1 calc PR A -2 H2B3 H 1.0859 0.2081 0.7340 0.101 Uiso 0.50 1 calc PR A -2 H2 H 0.9486 0.4047 -0.1848 0.18(3) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0838(4) 0.0330(2) 0.0502(3) 0.000 0.0242(2) 0.000 O1 0.0425(13) 0.0530(13) 0.0553(13) 0.0055(11) 0.0153(10) -0.0010(10) N1 0.0324(11) 0.0320(11) 0.0320(11) 0.0004(9) 0.0115(9) 0.0070(9) B1 0.0382(18) 0.0368(18) 0.070(2) -0.0145(16) 0.0253(17) -0.0098(14) O2 0.0507(14) 0.0550(15) 0.0698(16) 0.0146(12) 0.0143(12) 0.0079(11) C2 0.0227(12) 0.0344(14) 0.0447(15) -0.0062(11) 0.0071(11) -0.0031(10) B3 0.0326(17) 0.0315(16) 0.075(3) 0.0080(16) 0.0143(17) -0.0010(13) B4 0.0414(19) 0.0350(17) 0.073(3) -0.0083(16) 0.0236(18) -0.0099(14) B5 0.0313(16) 0.0479(19) 0.053(2) -0.0175(16) 0.0147(15) -0.0133(14) B6 0.0318(16) 0.0371(17) 0.0450(18) -0.0007(13) 0.0022(13) -0.0062(13) B7 0.047(2) 0.0427(19) 0.060(2) 0.0067(16) 0.0131(18) -0.0105(16) B8 0.0369(18) 0.0446(19) 0.058(2) -0.0109(16) 0.0176(16) -0.0134(15) B9 0.0256(14) 0.0396(17) 0.0444(17) -0.0109(13) 0.0097(13) -0.0049(12) B10 0.0439(19) 0.047(2) 0.0467(19) -0.0056(15) 0.0126(16) -0.0101(15) C21 0.0242(12) 0.0333(13) 0.0394(14) -0.0060(11) 0.0064(10) 0.0003(10) C22 0.0238(12) 0.0379(14) 0.0393(14) -0.0026(11) 0.0048(11) 0.0011(10) C23 0.0246(12) 0.0408(15) 0.0392(14) -0.0065(11) 0.0060(11) -0.0017(11) C24 0.0345(14) 0.0369(14) 0.0388(14) -0.0074(11) 0.0098(12) -0.0021(11) C25 0.0363(15) 0.0434(16) 0.0478(17) 0.0052(13) 0.0052(13) 0.0093(13) C26 0.0236(13) 0.0503(17) 0.0544(18) 0.0016(14) 0.0075(12) 0.0048(12) C27 0.0421(17) 0.0383(15) 0.0393(15) -0.0028(12) 0.0020(13) 0.0015(12) C28 0.0330(14) 0.0295(13) 0.0382(14) -0.0017(11) 0.0127(11) 0.0062(10) C29 0.060(2) 0.0409(17) 0.060(2) -0.0029(14) 0.0383(17) 0.0073(15) C30 0.0569(19) 0.0467(17) 0.0372(15) 0.0086(13) 0.0137(14) 0.0242(15) C31 0.068(2) 0.087(3) 0.0404(18) -0.0095(18) -0.0064(17) 0.037(2) C32 0.0457(17) 0.0387(16) 0.0517(18) -0.0131(13) 0.0171(14) -0.0007(13) C33 0.069(2) 0.053(2) 0.076(3) -0.0290(19) 0.018(2) 0.0071(18) C34 0.0333(14) 0.0525(18) 0.0420(16) 0.0055(13) 0.0177(12) 0.0060(12) C35 0.056(2) 0.090(3) 0.050(2) 0.0257(19) 0.0276(17) 0.017(2) _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 C27 1.207(4) . ? N1 C30 1.515(3) . ? N1 C34 1.520(3) . ? N1 C28 1.521(3) . ? N1 C32 1.523(4) . ? B1 C2 1.637(4) . ? B1 B3 1.690(6) . ? B1 B5 1.696(5) . ? B1 B4 1.696(5) . ? O2 C27 1.320(4) . ? C2 C21 1.497(4) . ? C2 B6 1.752(4) . ? C2 B3 1.753(5) . ? C2 B9 1.756(4) . ? C2 B5 1.769(4) . ? B3 B7 1.784(5) . ? B3 B6 1.790(5) . ? B3 B4 1.818(5) . ? B4 B8 1.816(5) . ? B4 B7 1.823(6) . ? B4 B5 1.827(6) . ? B5 B8 1.787(5) . ? B5 B9 1.802(5) . ? B6 B10 1.682(5) . ? B6 B7 1.817(5) . ? B6 B9 1.846(5) . ? B7 B10 1.701(6) . ? B7 B8 1.844(5) . ? B8 B10 1.705(5) . ? B8 B9 1.826(5) . ? B9 B10 1.692(5) . ? C21 C26 1.390(4) . ? C21 C22 1.400(4) . ? C22 C23 1.372(4) . ? C23 C24 1.390(4) . ? C24 C25 1.389(4) . ? C24 C27 1.492(4) . ? C25 C26 1.384(4) . ? C28 C29 1.509(4) . ? C30 C31 1.511(5) . ? C32 C33 1.518(4) . ? C34 C35 1.505(4) . ? N1A C3A 1.494(7) . ? N1A C3A 1.494(7) 2_756 ? N1A C1A 1.495(6) 2_756 ? N1A C1A 1.495(6) . ? N1A C1B 1.497(7) . ? N1A C1B 1.497(7) 2_756 ? N1A C3B 1.566(6) . ? N1A C3B 1.566(6) 2_756 ? C1A C2A 1.506(10) . ? C3A C4A 1.371(10) . ? C1B C2B 1.512(11) . ? C4B C3B 1.470(10) . ? 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 C30 N1 C34 108.7(2) . . ? C30 N1 C28 111.4(2) . . ? C34 N1 C28 107.6(2) . . ? C30 N1 C32 108.6(2) . . ? C34 N1 C32 111.5(2) . . ? C28 N1 C32 109.0(2) . . ? C2 B1 B3 63.6(2) . . ? C2 B1 B5 64.10(19) . . ? B3 B1 B5 99.0(3) . . ? C2 B1 B4 96.8(3) . . ? B3 B1 B4 65.0(2) . . ? B5 B1 B4 65.2(2) . . ? C21 C2 B1 114.7(2) . . ? C21 C2 B6 116.0(2) . . ? B1 C2 B6 117.5(3) . . ? C21 C2 B3 127.2(2) . . ? B1 C2 B3 59.7(2) . . ? B6 C2 B3 61.4(2) . . ? C21 C2 B9 118.1(2) . . ? B1 C2 B9 117.5(2) . . ? B6 C2 B9 63.48(18) . . ? B3 C2 B9 106.9(2) . . ? C21 C2 B5 130.6(2) . . ? B1 C2 B5 59.55(19) . . ? B6 C2 B5 106.9(2) . . ? B3 C2 B5 93.9(2) . . ? B9 C2 B5 61.46(17) . . ? B1 B3 C2 56.76(19) . . ? B1 B3 B7 113.7(3) . . ? C2 B3 B7 100.7(2) . . ? B1 B3 B6 112.8(3) . . ? C2 B3 B6 59.27(18) . . ? B7 B3 B6 61.1(2) . . ? B1 B3 B4 57.7(2) . . ? C2 B3 B4 88.5(2) . . ? B7 B3 B4 60.8(2) . . ? B6 B3 B4 103.5(2) . . ? B1 B4 B8 111.4(3) . . ? B1 B4 B3 57.4(2) . . ? B8 B4 B3 101.1(2) . . ? B1 B4 B7 111.4(2) . . ? B8 B4 B7 60.9(2) . . ? B3 B4 B7 58.7(2) . . ? B1 B4 B5 57.4(2) . . ? B8 B4 B5 58.7(2) . . ? B3 B4 B5 89.8(2) . . ? B7 B4 B5 101.5(2) . . ? B1 B5 C2 56.34(17) . . ? B1 B5 B8 112.9(3) . . ? C2 B5 B8 99.9(2) . . ? B1 B5 B9 112.1(2) . . ? C2 B5 B9 58.91(16) . . ? B8 B5 B9 61.18(19) . . ? B1 B5 B4 57.4(2) . . ? C2 B5 B4 87.8(2) . . ? B8 B5 B4 60.3(2) . . ? B9 B5 B4 103.1(2) . . ? B10 B6 C2 110.1(2) . . ? B10 B6 B3 112.4(2) . . ? C2 B6 B3 59.32(19) . . ? B10 B6 B7 58.0(2) . . ? C2 B6 B7 99.5(2) . . ? B3 B6 B7 59.3(2) . . ? B10 B6 B9 57.1(2) . . ? C2 B6 B9 58.36(16) . . ? B3 B6 B9 101.7(2) . . ? B7 B6 B9 90.4(2) . . ? B10 B7 B3 111.8(3) . . ? B10 B7 B6 57.0(2) . . ? B3 B7 B6 59.6(2) . . ? B10 B7 B4 112.2(3) . . ? B3 B7 B4 60.5(2) . . ? B6 B7 B4 102.2(3) . . ? B10 B7 B8 57.4(2) . . ? B3 B7 B8 101.4(3) . . ? B6 B7 B8 89.9(2) . . ? B4 B7 B8 59.4(2) . . ? B10 B8 B5 112.2(3) . . ? B10 B8 B4 112.3(3) . . ? B5 B8 B4 60.9(2) . . ? B10 B8 B9 57.1(2) . . ? B5 B8 B9 59.82(19) . . ? B4 B8 B9 102.6(2) . . ? B10 B8 B7 57.1(2) . . ? B5 B8 B7 102.2(2) . . ? B4 B8 B7 59.7(2) . . ? B9 B8 B7 90.1(2) . . ? B10 B9 C2 109.4(2) . . ? B10 B9 B5 112.1(3) . . ? C2 B9 B5 59.63(17) . . ? B10 B9 B8 57.8(2) . . ? C2 B9 B8 98.9(2) . . ? B5 B9 B8 59.00(19) . . ? B10 B9 B6 56.6(2) . . ? C2 B9 B6 58.16(17) . . ? B5 B9 B6 101.7(2) . . ? B8 B9 B6 89.6(2) . . ? B6 B10 B9 66.3(2) . . ? B6 B10 B7 65.0(2) . . ? B9 B10 B7 100.0(3) . . ? B6 B10 B8 99.6(3) . . ? B9 B10 B8 65.0(2) . . ? B7 B10 B8 65.5(2) . . ? C26 C21 C22 117.9(3) . . ? C26 C21 C2 123.8(2) . . ? C22 C21 C2 118.4(2) . . ? C23 C22 C21 121.1(3) . . ? C22 C23 C24 120.9(2) . . ? C25 C24 C23 118.5(3) . . ? C25 C24 C27 124.9(3) . . ? C23 C24 C27 116.5(2) . . ? C26 C25 C24 120.6(3) . . ? C25 C26 C21 121.1(3) . . ? O1 C27 O2 123.5(3) . . ? O1 C27 C24 123.2(3) . . ? O2 C27 C24 113.3(3) . . ? C29 C28 N1 115.2(2) . . ? C31 C30 N1 115.6(3) . . ? C33 C32 N1 114.6(3) . . ? C35 C34 N1 114.6(2) . . ? C3A N1A C3A 64.3(6) . 2_756 ? C3A N1A C1A 170.3(4) . 2_756 ? C3A N1A C1A 112.9(4) 2_756 2_756 ? C3A N1A C1A 112.9(4) . . ? C3A N1A C1A 170.3(4) 2_756 . ? C1A N1A C1A 71.4(5) 2_756 . ? C3A N1A C1B 63.6(4) . . ? C3A N1A C1B 111.2(5) 2_756 . ? C1A N1A C1B 111.0(4) 2_756 . ? C1A N1A C1B 73.8(4) . . ? C3A N1A C1B 111.2(5) . 2_756 ? C3A N1A C1B 63.6(4) 2_756 2_756 ? C1A N1A C1B 73.8(4) 2_756 2_756 ? C1A N1A C1B 111.0(4) . 2_756 ? C1B N1A C1B 174.3(6) . 2_756 ? C3A N1A C3B 82.6(4) . . ? C3A N1A C3B 105.8(4) 2_756 . ? C1A N1A C3B 107.0(4) 2_756 . ? C1A N1A C3B 64.5(3) . . ? C1B N1A C3B 108.6(4) . . ? C1B N1A C3B 72.0(4) 2_756 . ? C3A N1A C3B 105.8(4) . 2_756 ? C3A N1A C3B 82.6(4) 2_756 2_756 ? C1A N1A C3B 64.5(3) 2_756 2_756 ? C1A N1A C3B 107.0(4) . 2_756 ? C1B N1A C3B 72.0(4) . 2_756 ? C1B N1A C3B 108.6(4) 2_756 2_756 ? C3B N1A C3B 170.3(5) . 2_756 ? N1A C1A C2A 112.4(5) . . ? C4A C3A N1A 121.7(7) . . ? N1A C1B C2B 122.1(6) . . ? C4B C3B N1A 116.9(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.195 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.064 data_C:AFIX32D _database_code_depnum_ccdc_archive 'CCDC 211908' _chemical_name_common (NEt4)+(2-HOOC-closo-2-CB9H9)- _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_melting_point ? _chemical_formula_moiety '2(C8H20N)+, 2(C2H10B9O2)-' _chemical_formula_sum 'C20 H60 B18 N2 O4' _chemical_formula_weight 587.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.0062(3) _cell_length_b 15.1936(2) _cell_length_c 16.7407(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.0290(10) _cell_angle_gamma 90.00 _cell_volume 7074.93(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39439 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2532 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9734 _exptl_absorpt_correction_T_max 0.9887 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 66863 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6957 _reflns_number_gt 5668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.1523P)^2^+6.7867P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0101(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6957 _refine_ls_number_parameters 491 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.2306 _refine_ls_wR_factor_gt 0.2059 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1A O -0.06091(5) 0.41017(9) -0.04666(9) 0.0332(4) Uani 1 1 d . . . O1B O 0.04712(5) 0.38815(10) 0.07168(9) 0.0333(4) Uani 1 1 d . . . O2A O -0.02206(5) 0.28322(10) -0.01942(10) 0.0334(4) Uani 1 1 d . . . O2B O 0.11592(6) 0.45460(11) 0.11722(11) 0.0400(4) Uani 1 1 d . . . N1 N 0.0000 0.00656(15) 0.2500 0.0291(5) Uani 1 2 d S . . N2 N 0.0000 0.50440(16) 0.2500 0.0359(6) Uani 1 2 d S . . N3 N 0.25274(6) -0.00636(11) 0.50336(11) 0.0323(4) Uani 1 1 d D . . C1 C 0.21307(15) 0.0576(2) 0.4887(2) 0.0589(10) Uani 0.75 1 d PDU A 1 H1A H 0.2096 0.0954 0.4385 0.071 Uiso 0.75 1 calc PR A 1 H1B H 0.2201 0.0957 0.5399 0.071 Uiso 0.75 1 calc PR A 1 C2 C 0.16439(12) 0.0030(3) 0.4711(3) 0.0632(11) Uani 0.75 1 d PDU A 1 H2A H 0.1567 -0.0317 0.4182 0.095 Uiso 0.75 1 calc PR A 1 H2B H 0.1380 0.0439 0.4646 0.095 Uiso 0.75 1 calc PR A 1 H2C H 0.1688 -0.0366 0.5197 0.095 Uiso 0.75 1 calc PR A 1 C3 C 0.24479(15) -0.0629(3) 0.4262(2) 0.0552(9) Uani 0.75 1 d PDU A 1 H3A H 0.2153 -0.0982 0.4151 0.066 Uiso 0.75 1 calc PR A 1 H3B H 0.2721 -0.1045 0.4400 0.066 Uiso 0.75 1 calc PR A 1 C4 C 0.2397(3) -0.0137(7) 0.3433(4) 0.0310(16) Uani 0.50 1 d PDU A 1 H4A H 0.2130 0.0283 0.3290 0.047 Uiso 0.50 1 calc PR A 1 H4B H 0.2332 -0.0560 0.2960 0.047 Uiso 0.50 1 calc PR A 1 H4C H 0.2695 0.0180 0.3517 0.047 Uiso 0.50 1 calc PR A 1 C5 C 0.29253(15) 0.0600(3) 0.5196(3) 0.0639(10) Uani 0.75 1 d PDU A 1 C6 C 0.33807(12) 0.0114(3) 0.5358(3) 0.0650(11) Uani 0.75 1 d PDU A 1 H6A H 0.3461 -0.0237 0.5885 0.097 Uiso 0.75 1 calc PR A 1 H6B H 0.3640 0.0534 0.5426 0.097 Uiso 0.75 1 calc PR A 1 H6C H 0.3341 -0.0277 0.4870 0.097 Uiso 0.75 1 calc PR A 1 C7 C 0.26026(14) -0.0673(3) 0.5774(3) 0.0598(10) Uani 0.75 1 d PDU A 1 H7A H 0.2883 -0.1053 0.5848 0.072 Uiso 0.75 1 calc PR A 1 H7B H 0.2317 -0.1059 0.5633 0.072 Uiso 0.75 1 calc PR A 1 C8 C 0.2687(7) -0.0197(12) 0.6640(8) 0.038(3) Uani 0.50 1 d PDU A 1 H8A H 0.2955 0.0218 0.6766 0.056 Uiso 0.50 1 calc PR A 1 H8B H 0.2764 -0.0632 0.7104 0.056 Uiso 0.50 1 calc PR A 1 H8C H 0.2395 0.0124 0.6596 0.056 Uiso 0.50 1 calc PR A 1 C9 C 0.2241(3) -0.0898(5) 0.4840(6) 0.040(2) Uani 0.25 1 d PDU A 2 H9A H 0.2003 -0.0849 0.4242 0.048 Uiso 0.25 1 calc PR A 2 H9B H 0.2057 -0.0912 0.5221 0.048 Uiso 0.25 1 calc PR A 2 C10 C 0.2482(2) -0.1784(4) 0.4915(4) 0.0557(14) Uani 0.50 1 d PDU A 2 H10A H 0.2679 -0.1788 0.4562 0.084 Uiso 0.50 1 calc PR A 2 H10B H 0.2237 -0.2245 0.4714 0.084 Uiso 0.50 1 calc PR A 2 H10C H 0.2688 -0.1893 0.5518 0.084 Uiso 0.50 1 calc PR A 2 C11 C 0.2834(2) -0.0063(5) 0.4470(4) 0.0667(17) Uani 0.50 1 d PDU A 2 H11A H 0.3043 -0.0589 0.4620 0.080 Uiso 0.50 1 calc PR A 2 H11B H 0.3046 0.0461 0.4624 0.080 Uiso 0.50 1 calc PR A 2 C12 C 0.2577(6) 0.0657(8) 0.5709(8) 0.085(4) Uani 0.25 1 d PDU A 2 H12A H 0.2892 0.0615 0.6194 0.102 Uiso 0.25 1 calc PR A 2 H12B H 0.2318 0.0605 0.5939 0.102 Uiso 0.25 1 calc PR A 2 C13 C 0.2532(3) 0.1557(4) 0.5203(6) 0.097(3) Uani 0.50 1 d PDU A 2 H13A H 0.2462 0.1434 0.4593 0.146 Uiso 0.50 1 calc PR A 2 H13B H 0.2836 0.1882 0.5446 0.146 Uiso 0.50 1 calc PR A 2 H13C H 0.2272 0.1911 0.5256 0.146 Uiso 0.50 1 calc PR A 2 C14 C 0.2556(6) -0.0058(18) 0.3483(9) 0.044(4) Uani 0.25 1 d PDU A 2 H14A H 0.2335 -0.0560 0.3319 0.065 Uiso 0.25 1 calc PR A 2 H14B H 0.2784 -0.0101 0.3192 0.065 Uiso 0.25 1 calc PR A 2 H14C H 0.2373 0.0491 0.3313 0.065 Uiso 0.25 1 calc PR A 2 C15 C 0.2941(2) -0.0172(5) 0.5915(4) 0.0271(16) Uani 0.25 1 d PDU A 3 H15A H 0.3171 0.0321 0.6008 0.033 Uiso 0.25 1 calc PR A 3 H15B H 0.3114 -0.0728 0.5922 0.033 Uiso 0.25 1 calc PR A 3 C16 C 0.2747(14) -0.018(2) 0.6647(17) 0.037(6) Uani 0.25 1 d PDU A 3 H16A H 0.2514 0.0293 0.6559 0.056 Uiso 0.25 1 calc PR A 3 H16B H 0.3014 -0.0105 0.7201 0.056 Uiso 0.25 1 calc PR A 3 H16C H 0.2589 -0.0750 0.6645 0.056 Uiso 0.25 1 calc PR A 3 C1C C 0.00837(8) 0.06296(15) 0.18248(15) 0.0378(5) Uani 1 1 d . . . H1C1 H 0.0372 0.0997 0.2116 0.045 Uiso 1 1 calc R . . H1C2 H 0.0158 0.0235 0.1421 0.045 Uiso 1 1 calc R . . C2A C -0.09832(7) 0.28023(13) -0.12189(12) 0.0264(4) Uani 1 1 d . . . C2B C 0.11589(7) 0.30460(13) 0.14695(12) 0.0272(4) Uani 1 1 d . . . C2C C -0.03167(10) 0.12205(17) 0.13113(18) 0.0507(6) Uani 1 1 d . . . H2C1 H -0.0598 0.0866 0.0978 0.076 Uiso 1 1 calc R . . H2C2 H -0.0217 0.1573 0.0917 0.076 Uiso 1 1 calc R . . H2C3 H -0.0399 0.1612 0.1700 0.076 Uiso 1 1 calc R . . C3A C -0.05915(7) 0.33154(13) -0.06010(12) 0.0266(4) Uani 1 1 d . . . C3B C 0.08951(7) 0.38541(13) 0.10823(12) 0.0269(4) Uani 1 1 d . . . C3C C 0.04334(8) -0.04974(14) 0.28999(15) 0.0368(5) Uani 1 1 d . . . H3C1 H 0.0719 -0.0109 0.3104 0.044 Uiso 1 1 calc R . . H3C2 H 0.0464 -0.0882 0.2446 0.044 Uiso 1 1 calc R . . C4C C 0.04455(10) -0.10709(18) 0.36400(19) 0.0524(7) Uani 1 1 d . . . H4C1 H 0.0443 -0.0700 0.4117 0.079 Uiso 1 1 calc R . . H4C2 H 0.0738 -0.1429 0.3832 0.079 Uiso 1 1 calc R . . H4C3 H 0.0163 -0.1457 0.3453 0.079 Uiso 1 1 calc R . . C5C C 0.04330(10) 0.44757(16) 0.27247(16) 0.0448(6) Uani 1 1 d . . . H5C1 H 0.0721 0.4858 0.2888 0.054 Uiso 1 1 calc R . . H5C2 H 0.0414 0.4142 0.2205 0.054 Uiso 1 1 calc R . . C6C C 0.05019(13) 0.38299(19) 0.34489(19) 0.0625(8) Uani 1 1 d . . . H6C1 H 0.0537 0.4153 0.3976 0.094 Uiso 1 1 calc R . . H6C2 H 0.0791 0.3478 0.3546 0.094 Uiso 1 1 calc R . . H6C3 H 0.0222 0.3440 0.3293 0.094 Uiso 1 1 calc R . . C7C C 0.00197(9) 0.56124(15) 0.32624(14) 0.0367(5) Uani 1 1 d . . . H7C1 H -0.0279 0.5964 0.3088 0.044 Uiso 1 1 calc R . . H7C2 H 0.0023 0.5218 0.3735 0.044 Uiso 1 1 calc R . . C8C C 0.04316(10) 0.62185(17) 0.36035(17) 0.0477(6) Uani 1 1 d . . . H8C1 H 0.0730 0.5878 0.3842 0.072 Uiso 1 1 calc R . . H8C2 H 0.0395 0.6584 0.4057 0.072 Uiso 1 1 calc R . . H8C3 H 0.0444 0.6596 0.3137 0.072 Uiso 1 1 calc R . . B1A B -0.12735(9) 0.22445(17) -0.07600(16) 0.0355(5) Uani 1 1 d . . . H1 H -0.1238 0.2174 -0.0073 0.043 Uiso 1 1 calc R . . B1B B 0.13955(11) 0.25468(19) 0.08794(18) 0.0432(6) Uani 1 1 d . . . H2 H 0.1399 0.2689 0.0225 0.052 Uiso 1 1 calc R . . B3A B -0.15844(8) 0.29836(17) -0.15234(15) 0.0322(5) Uani 1 1 d . . . H3 H -0.1804 0.3487 -0.1346 0.039 Uiso 1 1 calc R . . B3B B 0.10190(10) 0.19364(17) 0.11687(18) 0.0392(6) Uani 1 1 d . . . H4 H 0.0718 0.1597 0.0646 0.047 Uiso 1 1 calc R . . B4A B -0.16552(9) 0.17974(18) -0.16790(16) 0.0378(6) Uani 1 1 d . . . H5 H -0.1937 0.1339 -0.1633 0.045 Uiso 1 1 calc R . . B4B B 0.16436(11) 0.17365(19) 0.1589(2) 0.0468(7) Uani 1 1 d . . . H6 H 0.1859 0.1227 0.1408 0.056 Uiso 1 1 calc R . . B5A B -0.10281(9) 0.16513(16) -0.13453(16) 0.0343(5) Uani 1 1 d . . . H5A H -0.0792 0.1082 -0.1025 0.041 Uiso 1 1 calc R . . B5B B 0.17631(9) 0.28884(19) 0.18658(18) 0.0407(6) Uani 1 1 d . . . H5B H 0.2075 0.3317 0.1908 0.049 Uiso 1 1 calc R . . B6A B -0.12879(8) 0.32913(16) -0.22268(14) 0.0302(5) Uani 1 1 d . . . H9 H -0.1252 0.4001 -0.2372 0.036 Uiso 1 1 calc R . . B6B B 0.09319(8) 0.24024(15) 0.20833(16) 0.0310(5) Uani 1 1 d . . . H10 H 0.0557 0.2487 0.2065 0.037 Uiso 1 1 calc R . . B7A B -0.17846(9) 0.25423(17) -0.25926(15) 0.0341(5) Uani 1 1 d . . . H11 H -0.2164 0.2648 -0.3049 0.041 Uiso 1 1 calc R . . B7B B 0.12936(10) 0.14316(17) 0.22092(19) 0.0418(6) Uani 1 1 d . . . H12 H 0.1224 0.0722 0.2304 0.050 Uiso 1 1 calc R . . B8A B -0.13872(9) 0.16057(17) -0.24657(16) 0.0349(5) Uani 1 1 d . . . H13 H -0.1439 0.0964 -0.2818 0.042 Uiso 1 1 calc R . . B8B B 0.18192(9) 0.21074(19) 0.27008(19) 0.0433(6) Uani 1 1 d . . . H14 H 0.2181 0.1939 0.3193 0.052 Uiso 1 1 calc R . . B9A B -0.08915(8) 0.23506(16) -0.20938(15) 0.0301(5) Uani 1 1 d . . . H15 H -0.0527 0.2316 -0.2131 0.036 Uiso 1 1 calc R . . B9B B 0.14567(8) 0.30784(17) 0.25779(15) 0.0331(5) Uani 1 1 d . . . H16 H 0.1513 0.3702 0.2960 0.040 Uiso 1 1 calc R . . B10A B -0.13584(9) 0.25392(17) -0.30058(15) 0.0352(5) Uani 1 1 d . . . H17 H -0.1380 0.2631 -0.3683 0.042 Uiso 1 1 calc R . . B10B B 0.13633(10) 0.21408(19) 0.30304(18) 0.0409(6) Uani 1 1 d . . . H18 H 0.1350 0.2023 0.3681 0.049 Uiso 1 1 calc R . . H7 H 0.1013(11) 0.495(2) 0.102(2) 0.049(9) Uiso 1 1 d . . . H8 H -0.0014(11) 0.319(2) 0.0131(19) 0.056(8) Uiso 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 0.0326(8) 0.0264(8) 0.0342(8) -0.0002(6) 0.0052(6) 0.0005(6) O1B 0.0238(8) 0.0330(8) 0.0360(8) -0.0004(6) 0.0030(6) -0.0001(6) O2A 0.0255(7) 0.0303(8) 0.0362(8) -0.0004(6) 0.0022(6) 0.0005(6) O2B 0.0264(8) 0.0289(9) 0.0582(10) 0.0081(7) 0.0085(7) -0.0010(6) N1 0.0260(12) 0.0254(12) 0.0370(13) 0.000 0.0131(10) 0.000 N2 0.0506(16) 0.0309(13) 0.0383(14) 0.000 0.0307(12) 0.000 N3 0.0309(9) 0.0339(10) 0.0285(9) -0.0012(7) 0.0071(7) -0.0028(7) C1 0.086(3) 0.046(2) 0.0395(17) 0.0060(15) 0.0178(18) 0.0328(19) C2 0.0249(16) 0.095(3) 0.064(2) 0.007(2) 0.0100(16) 0.0114(17) C3 0.055(2) 0.058(2) 0.051(2) -0.0097(16) 0.0183(17) 0.0002(17) C4 0.030(4) 0.037(3) 0.024(2) -0.0039(19) 0.007(2) -0.006(4) C5 0.059(2) 0.070(3) 0.066(2) -0.005(2) 0.0269(19) -0.0187(19) C6 0.0296(17) 0.100(3) 0.066(2) -0.003(2) 0.0195(16) -0.0090(18) C7 0.047(2) 0.068(2) 0.064(2) 0.0314(19) 0.0213(18) 0.0120(18) C8 0.036(5) 0.048(7) 0.029(5) 0.008(4) 0.012(4) 0.002(4) C9 0.029(4) 0.055(5) 0.030(4) -0.003(4) 0.004(3) -0.016(4) C10 0.064(4) 0.044(3) 0.047(3) -0.003(2) 0.007(3) -0.010(2) C11 0.047(3) 0.071(4) 0.080(4) 0.014(3) 0.022(3) -0.008(3) C12 0.101(11) 0.100(9) 0.046(7) -0.018(6) 0.017(7) 0.035(9) C13 0.092(6) 0.041(3) 0.115(6) -0.017(4) -0.012(5) 0.009(3) C14 0.041(10) 0.045(8) 0.043(6) -0.005(5) 0.014(6) -0.003(9) C15 0.010(3) 0.032(4) 0.030(4) -0.007(3) -0.003(3) -0.004(3) C16 0.041(12) 0.032(11) 0.030(10) -0.010(8) 0.004(7) 0.000(7) C1C 0.0377(12) 0.0367(12) 0.0429(12) 0.0032(9) 0.0195(10) -0.0054(9) C2A 0.0236(9) 0.0291(10) 0.0256(9) 0.0006(7) 0.0084(7) 0.0006(8) C2B 0.0236(9) 0.0298(10) 0.0286(10) -0.0014(7) 0.0101(8) -0.0004(7) C2C 0.0491(15) 0.0466(14) 0.0526(15) 0.0164(11) 0.0145(12) -0.0012(11) C3A 0.0259(10) 0.0287(10) 0.0247(9) 0.0029(7) 0.0090(7) -0.0010(7) C3B 0.0256(10) 0.0294(10) 0.0258(9) -0.0008(7) 0.0097(8) -0.0011(7) C3C 0.0304(11) 0.0324(11) 0.0453(12) -0.0013(9) 0.0116(9) 0.0069(8) C4C 0.0486(15) 0.0433(14) 0.0583(16) 0.0140(12) 0.0122(12) 0.0075(11) C5C 0.0608(16) 0.0394(13) 0.0481(13) 0.0035(10) 0.0364(12) 0.0129(11) C6C 0.094(2) 0.0519(16) 0.0594(17) 0.0172(13) 0.0492(17) 0.0291(15) C7C 0.0488(13) 0.0347(11) 0.0370(11) -0.0020(9) 0.0280(10) 0.0033(9) C8C 0.0550(15) 0.0498(14) 0.0447(13) -0.0077(11) 0.0260(12) -0.0031(11) B1A 0.0341(12) 0.0424(14) 0.0311(12) 0.0030(10) 0.0136(10) -0.0081(10) B1B 0.0479(15) 0.0479(16) 0.0421(14) 0.0022(11) 0.0265(12) 0.0123(12) B3A 0.0234(11) 0.0419(13) 0.0321(11) -0.0023(9) 0.0112(9) -0.0009(9) B3B 0.0412(14) 0.0292(12) 0.0450(14) -0.0086(10) 0.0137(11) 0.0043(10) B4A 0.0327(12) 0.0435(14) 0.0364(13) 0.0006(10) 0.0121(10) -0.0094(10) B4B 0.0451(15) 0.0439(15) 0.0602(17) 0.0038(13) 0.0297(14) 0.0154(12) B5A 0.0334(12) 0.0272(12) 0.0372(12) 0.0008(9) 0.0074(10) -0.0043(9) B5B 0.0268(12) 0.0483(15) 0.0514(15) 0.0118(12) 0.0199(11) 0.0060(10) B6A 0.0262(11) 0.0352(12) 0.0273(11) 0.0028(9) 0.0079(9) 0.0018(9) B6B 0.0272(11) 0.0266(11) 0.0420(13) 0.0024(9) 0.0161(10) 0.0002(9) B7A 0.0273(11) 0.0422(14) 0.0299(11) -0.0010(9) 0.0073(9) -0.0008(10) B7B 0.0373(13) 0.0305(13) 0.0618(17) 0.0086(11) 0.0232(12) 0.0084(10) B8A 0.0293(12) 0.0367(13) 0.0348(12) -0.0078(10) 0.0077(10) -0.0050(10) B8B 0.0299(13) 0.0478(16) 0.0502(15) 0.0139(12) 0.0127(11) 0.0096(11) B9A 0.0262(11) 0.0327(12) 0.0320(11) -0.0051(9) 0.0115(9) -0.0003(9) B9B 0.0268(11) 0.0386(13) 0.0297(11) -0.0001(9) 0.0058(9) -0.0013(9) B10A 0.0306(12) 0.0463(14) 0.0274(11) -0.0032(10) 0.0095(9) -0.0017(10) B10B 0.0385(14) 0.0462(15) 0.0402(13) 0.0123(11) 0.0174(11) 0.0076(11) _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 C3A 1.221(2) . ? O1B C3B 1.188(2) . ? O2A C3A 1.293(2) . ? O2B C3B 1.291(2) . ? N1 C3C 1.489(2) . ? N1 C3C 1.489(2) 2 ? N1 C1C 1.513(2) . ? N1 C1C 1.513(2) 2 ? N2 C5C 1.486(3) . ? N2 C5C 1.486(3) 2 ? N2 C7C 1.524(2) . ? N2 C7C 1.524(2) 2 ? N3 C1 1.484(4) . ? N3 C3 1.494(4) . ? N3 C7 1.494(4) . ? N3 C9 1.497(8) . ? N3 C5 1.508(4) . ? N3 C15 1.539(6) . ? N3 C12 1.541(12) . ? N3 C11 1.545(6) . ? C1 C2 1.608(6) . ? C3 C4 1.533(8) . ? C5 C6 1.487(6) . ? C7 C8 1.554(11) . ? C9 C10 1.512(9) . ? C11 C14 1.545(13) . ? C12 C13 1.589(12) . ? C15 C16 1.542(14) . ? C1C C2C 1.488(3) . ? C2A C3A 1.465(3) . ? C2A B1A 1.603(3) . ? C2A B3A 1.703(3) . ? C2A B9A 1.730(3) . ? C2A B6A 1.754(3) . ? C2A B5A 1.761(3) . ? C2B C3B 1.473(3) . ? C2B B1B 1.606(3) . ? C2B B5B 1.698(3) . ? C2B B9B 1.732(3) . ? C2B B6B 1.732(3) . ? C2B B3B 1.765(3) . ? C3C C4C 1.504(3) . ? C5C C6C 1.512(3) . ? C7C C8C 1.474(3) . ? B1A B4A 1.679(3) . ? B1A B5A 1.690(4) . ? B1A B3A 1.694(3) . ? B1B B3B 1.668(4) . ? B1B B4B 1.678(4) . ? B1B B5B 1.687(4) . ? B3A B6A 1.784(3) . ? B3A B7A 1.791(3) . ? B3A B4A 1.822(4) . ? B3B B4B 1.764(4) . ? B3B B6B 1.793(3) . ? B3B B7B 1.796(4) . ? B4A B5A 1.764(4) . ? B4A B8A 1.806(4) . ? B4A B7A 1.824(4) . ? B4B B7B 1.793(4) . ? B4B B5B 1.812(4) . ? B4B B8B 1.824(4) . ? B5A B8A 1.780(3) . ? B5A B9A 1.803(3) . ? B5B B9B 1.781(3) . ? B5B B8B 1.793(4) . ? B6A B10A 1.686(3) . ? B6A B7A 1.791(3) . ? B6A B9A 1.819(3) . ? B6B B10B 1.676(4) . ? B6B B7B 1.796(3) . ? B6B B9B 1.800(3) . ? B7A B10A 1.667(3) . ? B7A B8A 1.817(4) . ? B7B B10B 1.697(4) . ? B7B B8B 1.801(4) . ? B8A B10A 1.702(4) . ? B8A B9A 1.785(3) . ? B8B B10B 1.657(4) . ? B8B B9B 1.798(4) . ? B9A B10A 1.665(3) . ? B9B B10B 1.686(4) . ? 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 C3C N1 C3C 109.9(2) . 2 ? C3C N1 C1C 107.43(12) . . ? C3C N1 C1C 110.56(12) 2 . ? C3C N1 C1C 110.56(12) . 2 ? C3C N1 C1C 107.43(12) 2 2 ? C1C N1 C1C 111.0(2) . 2 ? C5C N2 C5C 109.0(3) . 2 ? C5C N2 C7C 111.21(13) . . ? C5C N2 C7C 107.27(12) 2 . ? C5C N2 C7C 107.27(12) . 2 ? C5C N2 C7C 111.21(13) 2 2 ? C7C N2 C7C 110.9(2) . 2 ? C1 N3 C3 112.0(2) . . ? C1 N3 C7 113.9(2) . . ? C3 N3 C7 106.6(3) . . ? C1 N3 C9 99.1(4) . . ? C3 N3 C9 55.5(4) . . ? C7 N3 C9 63.3(4) . . ? C1 N3 C5 97.1(3) . . ? C3 N3 C5 113.5(2) . . ? C7 N3 C5 113.7(3) . . ? C9 N3 C5 163.1(4) . . ? C1 N3 C15 122.4(3) . . ? C3 N3 C15 125.3(4) . . ? C7 N3 C15 47.3(3) . . ? C9 N3 C15 107.9(4) . . ? C5 N3 C15 66.4(3) . . ? C1 N3 C12 60.4(6) . . ? C3 N3 C12 169.6(5) . . ? C7 N3 C12 83.6(5) . . ? C9 N3 C12 130.5(7) . . ? C5 N3 C12 62.7(7) . . ? C15 N3 C12 63.3(6) . . ? C1 N3 C11 121.5(3) . . ? C3 N3 C11 53.9(3) . . ? C7 N3 C11 124.6(3) . . ? C9 N3 C11 107.0(4) . . ? C5 N3 C11 59.8(3) . . ? C15 N3 C11 97.8(4) . . ? C12 N3 C11 122.2(7) . . ? N3 C1 C2 108.0(3) . . ? N3 C3 C4 115.6(5) . . ? C6 C5 N3 108.1(3) . . ? N3 C7 C8 114.0(7) . . ? N3 C9 C10 121.2(6) . . ? N3 C11 C14 116.5(8) . . ? N3 C12 C13 104.7(7) . . ? N3 C15 C16 110.8(16) . . ? C2C C1C N1 116.69(18) . . ? C3A C2A B1A 112.28(16) . . ? C3A C2A B3A 127.18(17) . . ? B1A C2A B3A 61.57(14) . . ? C3A C2A B9A 117.94(16) . . ? B1A C2A B9A 118.91(17) . . ? B3A C2A B9A 107.32(15) . . ? C3A C2A B6A 116.38(16) . . ? B1A C2A B6A 120.26(16) . . ? B3A C2A B6A 62.10(13) . . ? B9A C2A B6A 62.93(13) . . ? C3A C2A B5A 128.19(16) . . ? B1A C2A B5A 60.10(14) . . ? B3A C2A B5A 95.74(15) . . ? B9A C2A B5A 62.20(13) . . ? B6A C2A B5A 108.44(15) . . ? C3B C2B B1B 114.30(17) . . ? C3B C2B B5B 127.48(17) . . ? B1B C2B B5B 61.34(16) . . ? C3B C2B B9B 115.08(16) . . ? B1B C2B B9B 120.18(17) . . ? B5B C2B B9B 62.56(14) . . ? C3B C2B B6B 117.75(15) . . ? B1B C2B B6B 117.45(17) . . ? B5B C2B B6B 106.76(16) . . ? B9B C2B B6B 62.62(13) . . ? C3B C2B B3B 129.77(17) . . ? B1B C2B B3B 59.08(15) . . ? B5B C2B B3B 94.69(16) . . ? B9B C2B B3B 107.74(16) . . ? B6B C2B B3B 61.68(14) . . ? O1A C3A O2A 123.14(18) . . ? O1A C3A C2A 124.91(18) . . ? O2A C3A C2A 111.94(17) . . ? O1B C3B O2B 121.57(19) . . ? O1B C3B C2B 123.44(18) . . ? O2B C3B C2B 114.99(17) . . ? N1 C3C C4C 116.76(18) . . ? N2 C5C C6C 115.06(19) . . ? C8C C7C N2 116.23(17) . . ? C2A B1A B4A 94.66(16) . . ? C2A B1A B5A 64.58(14) . . ? B4A B1A B5A 63.17(15) . . ? C2A B1A B3A 62.12(13) . . ? B4A B1A B3A 65.39(15) . . ? B5A B1A B3A 98.77(17) . . ? C2B B1B B3B 65.19(15) . . ? C2B B1B B4B 95.31(18) . . ? B3B B1B B4B 63.62(17) . . ? C2B B1B B5B 62.00(14) . . ? B3B B1B B5B 98.77(19) . . ? B4B B1B B5B 65.14(18) . . ? B1A B3A C2A 56.30(13) . . ? B1A B3A B6A 113.69(17) . . ? C2A B3A B6A 60.36(12) . . ? B1A B3A B7A 112.90(18) . . ? C2A B3A B7A 99.16(15) . . ? B6A B3A B7A 60.12(13) . . ? B1A B3A B4A 56.90(14) . . ? C2A B3A B4A 86.35(15) . . ? B6A B3A B4A 103.01(16) . . ? B7A B3A B4A 60.62(14) . . ? B1B B3B B4B 58.48(16) . . ? B1B B3B C2B 55.72(13) . . ? B4B B3B C2B 86.97(17) . . ? B1B B3B B6B 111.09(18) . . ? B4B B3B B6B 101.60(18) . . ? C2B B3B B6B 58.28(12) . . ? B1B B3B B7B 113.9(2) . . ? B4B B3B B7B 60.50(15) . . ? C2B B3B B7B 99.07(17) . . ? B6B B3B B7B 60.07(14) . . ? B1A B4A B5A 58.72(14) . . ? B1A B4A B8A 113.35(17) . . ? B5A B4A B8A 59.80(14) . . ? B1A B4A B3A 57.71(14) . . ? B5A B4A B3A 91.48(15) . . ? B8A B4A B3A 101.77(16) . . ? B1A B4A B7A 112.02(18) . . ? B5A B4A B7A 102.12(16) . . ? B8A B4A B7A 60.09(14) . . ? B3A B4A B7A 58.85(13) . . ? B1B B4B B3B 57.90(16) . . ? B1B B4B B7B 113.48(19) . . ? B3B B4B B7B 60.64(16) . . ? B1B B4B B5B 57.67(16) . . ? B3B B4B B5B 90.83(16) . . ? B7B B4B B5B 101.76(18) . . ? B1B B4B B8B 112.2(2) . . ? B3B B4B B8B 102.16(18) . . ? B7B B4B B8B 59.74(16) . . ? B5B B4B B8B 59.09(15) . . ? B1A B5A C2A 55.32(12) . . ? B1A B5A B4A 58.11(14) . . ? C2A B5A B4A 86.43(15) . . ? B1A B5A B8A 114.12(18) . . ? C2A B5A B8A 98.87(16) . . ? B4A B5A B8A 61.25(14) . . ? B1A B5A B9A 110.53(17) . . ? C2A B5A B9A 58.08(12) . . ? B4A B5A B9A 101.49(16) . . ? B8A B5A B9A 59.75(13) . . ? B1B B5B C2B 56.66(14) . . ? B1B B5B B9B 113.12(18) . . ? C2B B5B B9B 59.67(12) . . ? B1B B5B B8B 113.3(2) . . ? C2B B5B B8B 99.92(16) . . ? B9B B5B B8B 60.42(15) . . ? B1B B5B B4B 57.19(16) . . ? C2B B5B B4B 87.50(17) . . ? B9B B5B B4B 103.05(18) . . ? B8B B5B B4B 60.79(16) . . ? B10A B6A C2A 109.01(17) . . ? B10A B6A B3A 112.57(18) . . ? C2A B6A B3A 57.54(12) . . ? B10A B6A B7A 57.18(14) . . ? C2A B6A B7A 97.27(15) . . ? B3A B6A B7A 60.14(13) . . ? B10A B6A B9A 56.56(13) . . ? C2A B6A B9A 57.89(12) . . ? B3A B6A B9A 100.28(16) . . ? B7A B6A B9A 87.98(15) . . ? B10B B6B C2B 111.05(17) . . ? B10B B6B B3B 113.96(18) . . ? C2B B6B B3B 60.04(13) . . ? B10B B6B B7B 58.39(15) . . ? C2B B6B B7B 100.28(16) . . ? B3B B6B B7B 60.05(15) . . ? B10B B6B B9B 57.88(14) . . ? C2B B6B B9B 58.68(12) . . ? B3B B6B B9B 103.63(16) . . ? B7B B6B B9B 91.65(16) . . ? B10A B7A B6A 58.26(14) . . ? B10A B7A B3A 113.20(17) . . ? B6A B7A B3A 59.74(13) . . ? B10A B7A B8A 58.28(14) . . ? B6A B7A B8A 91.84(15) . . ? B3A B7A B8A 102.53(16) . . ? B10A B7A B4A 113.02(18) . . ? B6A B7A B4A 102.68(16) . . ? B3A B7A B4A 60.53(14) . . ? B8A B7A B4A 59.46(14) . . ? B10B B7B B4B 112.6(2) . . ? B10B B7B B3B 112.77(18) . . ? B4B B7B B3B 58.87(15) . . ? B10B B7B B6B 57.26(14) . . ? B4B B7B B6B 100.32(17) . . ? B3B B7B B6B 59.88(14) . . ? B10B B7B B8B 56.44(16) . . ? B4B B7B B8B 60.97(16) . . ? B3B B7B B8B 101.79(18) . . ? B6B B7B B8B 88.42(16) . . ? B10A B8A B5A 113.34(17) . . ? B10A B8A B9A 56.98(13) . . ? B5A B8A B9A 60.78(13) . . ? B10A B8A B4A 112.23(18) . . ? B5A B8A B4A 58.95(14) . . ? B9A B8A B4A 100.61(16) . . ? B10A B8A B7A 56.42(14) . . ? B5A B8A B7A 101.77(16) . . ? B9A B8A B7A 88.20(16) . . ? B4A B8A B7A 60.44(14) . . ? B10B B8B B5B 113.06(18) . . ? B10B B8B B9B 58.23(15) . . ? B5B B8B B9B 59.47(14) . . ? B10B B8B B7B 58.58(16) . . ? B5B B8B B7B 102.18(18) . . ? B9B B8B B7B 91.54(16) . . ? B10B B8B B4B 113.0(2) . . ? B5B B8B B4B 60.12(16) . . ? B9B B8B B4B 101.89(17) . . ? B7B B8B B4B 59.29(16) . . ? B10A B9A C2A 111.21(16) . . ? B10A B9A B8A 58.98(14) . . ? C2A B9A B8A 99.82(15) . . ? B10A B9A B5A 113.97(17) . . ? C2A B9A B5A 59.72(13) . . ? B8A B9A B5A 59.47(13) . . ? B10A B9A B6A 57.70(13) . . ? C2A B9A B6A 59.18(12) . . ? B8A B9A B6A 91.98(15) . . ? B5A B9A B6A 103.85(16) . . ? B10B B9B C2B 110.58(18) . . ? B10B B9B B5B 112.23(19) . . ? C2B B9B B5B 57.77(13) . . ? B10B B9B B8B 56.67(15) . . ? C2B B9B B8B 98.40(17) . . ? B5B B9B B8B 60.11(15) . . ? B10B B9B B6B 57.35(14) . . ? C2B B9B B6B 58.70(12) . . ? B5B B9B B6B 100.47(17) . . ? B8B B9B B6B 88.38(16) . . ? B9A B10A B7A 97.63(17) . . ? B9A B10A B6A 65.74(14) . . ? B7A B10A B6A 64.56(14) . . ? B9A B10A B8A 64.03(15) . . ? B7A B10A B8A 65.30(15) . . ? B6A B10A B8A 99.82(17) . . ? B8B B10B B6B 97.67(18) . . ? B8B B10B B9B 65.10(16) . . ? B6B B10B B9B 64.78(14) . . ? B8B B10B B7B 64.98(17) . . ? B6B B10B B7B 64.36(16) . . ? B9B B10B B7B 99.40(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.971 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.118