# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Severin, Kay' 'Icli, Burcak' 'Sheepwash, Erin' 'Riis-Johannessen, Thomas' 'Schenk, Kurt' 'Filinchuk, Yaroslav' 'Scopelliti, Rosario' _publ_contact_author_name 'Dr Kay Severin' _publ_contact_author_email kay.severin@epfl.ch _publ_section_title ; Dative Boron-Nitrogen Bonds in Structural Supramolecular Chemistry: Multicomponent Assembly of Prismatic Organic Cages ; # Attachment '- 1.cif' data_bi111 _database_code_depnum_ccdc_archive 'CCDC 827248' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H48 B6 Cl12 N12 O12' _chemical_formula_weight 1979.66 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.4133(9) _cell_length_b 13.4133(9) _cell_length_c 92.656(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14437(2) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 91 _cell_measurement_theta_min 3.047 _cell_measurement_theta_max 20.030 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6012 _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7999 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS 2008, Bruker AXS, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55409 _diffrn_reflns_av_R_equivalents 0.1313 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -102 _diffrn_reflns_limit_l_max 102 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 23.25 _reflns_number_total 2302 _reflns_number_gt 2069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _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^)+(0.0374P)^2^+133.9157P] 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 2302 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0900 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.264 _refine_ls_shift/su_max 0.002 _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 B1 B 0.3527(5) 0.2159(4) 0.94894(6) 0.0163(12) Uani 1 1 d . . . C11 C 0.2354(5) 0.1775(5) 0.92515(5) 0.0297(13) Uani 1 1 d . . . H15 H 0.1672 0.1447 0.9308 0.036 Uiso 1 1 calc R . . C12 C 0.3422(4) 0.2288(4) 0.93203(5) 0.0196(11) Uani 1 1 d . . . C13 C 0.4399(5) 0.2798(4) 0.92342(6) 0.0302(13) Uani 1 1 d . . . H13 H 0.5137 0.3182 0.9278 0.036 Uiso 1 1 calc R . . C21 C 0.4366(4) 0.3054(4) 0.96977(5) 0.0164(11) Uani 1 1 d . . . C22 C 0.3169(4) 0.2580(4) 0.97113(5) 0.0195(11) Uani 1 1 d . . . C23 C 0.2682(4) 0.2591(4) 0.98428(5) 0.0215(12) Uani 1 1 d . . . H9A H 0.1878 0.2299 0.9852 0.026 Uiso 1 1 calc R . . C24 C 0.3433(4) 0.3055(4) 0.99617(5) 0.0222(12) Uani 1 1 d . . . C25 C 0.4610(4) 0.3500(4) 0.99484(5) 0.0206(12) Uani 1 1 d . . . C26 C 0.5105(4) 0.3529(4) 0.98131(5) 0.0206(12) Uani 1 1 d . . . H10A H 0.5913 0.3861 0.9802 0.025 Uiso 1 1 calc R . . O27 O 0.4643(3) 0.2971(3) 0.95567(3) 0.0176(8) Uani 1 1 d . . . O28 O 0.2620(3) 0.2133(3) 0.95826(3) 0.0174(8) Uani 1 1 d . . . Cl29 Cl 0.28322(12) 0.30533(13) 1.012745(14) 0.0341(4) Uani 1 1 d . . . Cl30 Cl 0.55181(11) 0.40284(11) 1.009677(14) 0.0292(4) Uani 1 1 d . . . N31 N 0.4364(3) -0.2312(3) 0.95355(4) 0.0123(9) Uani 1 1 d . . . C32 C 0.3342(4) -0.2353(4) 0.95356(4) 0.0098(10) Uani 1 1 d . . . C33 C 0.3364(4) -0.1232(4) 0.95281(5) 0.0130(10) Uani 1 1 d . . . C34 C 0.2348(4) -0.1180(4) 0.95307(5) 0.0152(11) Uani 1 1 d . . . H1A H 0.1621 -0.1864 0.9538 0.018 Uiso 1 1 calc R . . C35 C 0.2420(4) -0.0118(4) 0.95226(5) 0.0165(11) Uani 1 1 d . . . H6A H 0.1731 -0.0080 0.9525 0.020 Uiso 1 1 calc R . . N36 N 0.3436(3) 0.0864(3) 0.95118(4) 0.0124(9) Uani 1 1 d . . . C37 C 0.4415(4) 0.0818(4) 0.95084(5) 0.0173(11) Uani 1 1 d . . . H5A H 0.5132 0.1511 0.9499 0.021 Uiso 1 1 calc R . . C38 C 0.4397(4) -0.0220(4) 0.95176(5) 0.0174(11) Uani 1 1 d . . . H2A H 0.5098 -0.0234 0.9517 0.021 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 B1 0.023(3) 0.008(3) 0.019(3) 0.003(2) 0.003(2) 0.008(2) C11 0.031(3) 0.046(4) 0.021(3) 0.008(3) 0.006(2) 0.026(3) C12 0.029(3) 0.012(3) 0.024(3) 0.002(2) 0.001(2) 0.015(2) C13 0.025(3) 0.021(3) 0.028(3) -0.006(2) -0.003(2) 0.000(3) C21 0.023(3) 0.013(3) 0.018(3) -0.001(2) -0.002(2) 0.013(2) C22 0.028(3) 0.014(3) 0.023(3) 0.002(2) 0.004(2) 0.016(2) C23 0.020(3) 0.023(3) 0.028(3) 0.000(2) 0.000(2) 0.016(2) C24 0.029(3) 0.024(3) 0.017(3) 0.002(2) 0.005(2) 0.017(3) C25 0.023(3) 0.019(3) 0.022(3) -0.002(2) -0.002(2) 0.013(2) C26 0.022(3) 0.010(3) 0.034(3) -0.002(2) 0.001(2) 0.011(2) O27 0.0233(19) 0.0122(18) 0.0172(17) -0.0006(14) 0.0043(14) 0.0087(15) O28 0.0224(19) 0.0209(18) 0.0147(17) -0.0026(14) -0.0005(15) 0.0151(16) Cl29 0.0374(9) 0.0555(10) 0.0206(7) -0.0028(6) 0.0047(6) 0.0317(8) Cl30 0.0317(8) 0.0320(8) 0.0272(7) -0.0078(6) -0.0074(6) 0.0184(7) N31 0.011(2) 0.011(2) 0.015(2) -0.0007(16) -0.0001(16) 0.0050(17) C32 0.011(3) 0.009(2) 0.010(2) -0.0002(19) 0.0021(19) 0.005(2) C33 0.010(2) 0.012(2) 0.017(2) 0.000(2) 0.0012(19) 0.006(2) C34 0.011(2) 0.010(2) 0.022(3) 0.000(2) 0.001(2) 0.003(2) C35 0.010(3) 0.019(3) 0.025(3) 0.003(2) 0.000(2) 0.010(2) N36 0.015(2) 0.010(2) 0.014(2) -0.0016(16) -0.0007(17) 0.0077(18) C37 0.013(2) 0.015(3) 0.024(3) 0.000(2) 0.002(2) 0.007(2) C38 0.011(2) 0.014(3) 0.028(3) -0.001(2) 0.004(2) 0.007(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 B1 O28 1.478(6) . ? B1 O27 1.479(7) . ? B1 C12 1.591(7) . ? B1 N36 1.691(6) . ? C11 C12 1.395(7) . ? C11 C13 1.415(7) 12_556 ? C12 C13 1.387(7) . ? C13 C11 1.415(7) 12_556 ? C21 C26 1.378(7) . ? C21 O27 1.378(5) . ? C21 C22 1.406(7) . ? C22 O28 1.372(6) . ? C22 C23 1.386(7) . ? C23 C24 1.410(7) . ? C24 C25 1.386(7) . ? C24 Cl29 1.734(5) . ? C25 C26 1.409(7) . ? C25 Cl30 1.736(5) . ? N31 C32 1.343(5) 3_655 ? N31 C32 1.345(6) . ? C32 N31 1.343(6) 2_545 ? C32 C33 1.491(6) . ? C33 C38 1.375(7) . ? C33 C34 1.400(6) . ? C34 C35 1.381(6) . ? C35 N36 1.345(6) . ? N36 C37 1.345(6) . ? C37 C38 1.383(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O28 B1 O27 106.8(4) . . ? O28 B1 C12 117.5(4) . . ? O27 B1 C12 116.6(4) . . ? O28 B1 N36 105.6(4) . . ? O27 B1 N36 103.4(4) . . ? C12 B1 N36 105.5(4) . . ? C12 C11 C13 121.3(5) . 12_556 ? C13 C12 C11 117.7(5) . . ? C13 C12 B1 120.4(5) . . ? C11 C12 B1 121.4(5) . . ? C12 C13 C11 121.0(5) . 12_556 ? C26 C21 O27 127.8(4) . . ? C26 C21 C22 122.3(4) . . ? O27 C21 C22 109.9(4) . . ? O28 C22 C23 128.0(5) . . ? O28 C22 C21 111.3(4) . . ? C23 C22 C21 120.7(5) . . ? C22 C23 C24 117.1(5) . . ? C25 C24 C23 121.9(4) . . ? C25 C24 Cl29 120.5(4) . . ? C23 C24 Cl29 117.6(4) . . ? C24 C25 C26 120.7(5) . . ? C24 C25 Cl30 121.4(4) . . ? C26 C25 Cl30 118.0(4) . . ? C21 C26 C25 117.2(5) . . ? C21 O27 B1 104.2(4) . . ? C22 O28 B1 104.0(4) . . ? C32 N31 C32 115.0(5) 3_655 . ? N31 C32 N31 125.0(4) 2_545 . ? N31 C32 C33 118.0(4) 2_545 . ? N31 C32 C33 116.9(4) . . ? C38 C33 C34 118.5(4) . . ? C38 C33 C32 120.1(4) . . ? C34 C33 C32 121.4(4) . . ? C35 C34 C33 118.9(4) . . ? N36 C35 C34 121.9(4) . . ? C35 N36 C37 119.4(4) . . ? C35 N36 B1 122.1(4) . . ? C37 N36 B1 118.3(4) . . ? N36 C37 C38 121.3(4) . . ? C33 C38 C37 120.0(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.432 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.081 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 115.7 -1.3 2 -0.333 0.333 0.083 287.0 5.4 3 0.000 1.000 0.250 295.1 4.6 4 0.333 0.667 0.417 287.0 5.5 5 0.000 0.000 0.500 115.7 -1.4 6 -0.333 0.333 0.583 287.0 5.4 7 0.000 0.000 0.750 295.1 4.6 8 0.333 0.667 0.917 287.0 5.5 9 0.333 0.667 0.167 115.2 -1.3 10 0.333 0.667 0.667 115.2 -1.3 11 0.667 0.333 0.333 115.2 -1.3 12 0.667 0.333 0.833 115.1 -1.3 _platon_squeeze_details ; ; # Attachment '- 2.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 827249' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H60 B6 Cl12 N12 O12' _chemical_formula_weight 2280.00 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' N N 0.0311 0.0180 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 14.3139(9) _cell_length_b 14.3139(9) _cell_length_c 30.848(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5473.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4782 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 47.96 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.201 _exptl_crystal_size_mid 0.198 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2316 _exptl_absorpt_coefficient_mu 3.330 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.9632 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0040 0 1 0 0.0780 0 -1 0 0.0520 1 0 0 0.0710 -1 0 0 0.0580 1 -1 0 0.0580 -1 1 0 0.0690 0 0 1 0.0150 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.54186 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 1 _diffrn_source_power 0.05 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 248 frames, detector distance = 130 mm ; _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6112 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 47.97 _reflns_number_total 1664 _reflns_number_gt 781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0633P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00013(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1664 _refine_ls_number_parameters 248 _refine_ls_number_restraints 360 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 0.796 _refine_ls_restrained_S_all 0.744 _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 B1 B 0.6176(7) 0.8086(6) 0.8474(2) 0.090(2) Uani 1 1 d U . . C11 C 0.6204(5) 0.8187(4) 0.79629(19) 0.0864(15) Uani 1 1 d U . . C12 C 0.5257(5) 0.7738(4) 0.77266(15) 0.0919(17) Uani 1 1 d U . . H12 H 0.4602 0.7428 0.7873 0.110 Uiso 1 1 calc R . . C13 C 0.7154(5) 0.8643(4) 0.77300(16) 0.0935(17) Uani 1 1 d U . . H13 H 0.7808 0.8958 0.7878 0.112 Uiso 1 1 calc R . . C21 C 0.6621(7) 0.9007(5) 0.9088(3) 0.0935(18) Uani 1 1 d U . . C22 C 0.5506(7) 0.8364(5) 0.9082(2) 0.0909(17) Uani 1 1 d U . . C23 C 0.4878(5) 0.8274(4) 0.9431(3) 0.0982(18) Uani 1 1 d U . . H23 H 0.4131 0.7857 0.9416 0.118 Uiso 1 1 calc R . . C24 C 0.5374(8) 0.8814(6) 0.9804(2) 0.117(2) Uani 1 1 d U . . C25 C 0.6475(9) 0.9485(6) 0.9805(2) 0.124(2) Uani 1 1 d U . . C26 C 0.7129(5) 0.9609(5) 0.9447(3) 0.118(2) Uani 1 1 d U . . H26 H 0.7870 1.0077 0.9452 0.142 Uiso 1 1 calc R . . O27 O 0.7076(3) 0.8978(3) 0.87072(15) 0.0978(12) Uani 1 1 d U . . O28 O 0.5179(3) 0.7871(3) 0.86871(13) 0.0904(11) Uani 1 1 d U . . Cl29 Cl 0.45838(16) 0.86531(16) 1.02567(6) 0.1630(8) Uani 1 1 d U . . Cl30 Cl 0.71071(19) 1.02085(18) 1.02831(6) 0.2002(10) Uani 1 1 d U . . N31 N 0.7579(5) 0.4340(4) 0.86549(12) 0.0784(12) Uani 1 1 d U . . C32 C 0.6566(10) 0.4166(7) 0.86569(14) 0.0780(14) Uani 1 1 d U . . C33 C 0.6479(6) 0.5161(5) 0.86430(15) 0.0770(15) Uani 1 1 d U . . C34 C 0.5468(5) 0.5082(5) 0.86233(15) 0.0885(16) Uani 1 1 d U . . H34 H 0.4841 0.4412 0.8635 0.106 Uiso 1 1 calc R . . C35 C 0.5413(5) 0.6019(6) 0.85861(15) 0.0877(16) Uani 1 1 d U . . H35 H 0.4738 0.5962 0.8567 0.105 Uiso 1 1 calc R . . N36 N 0.6277(5) 0.6987(4) 0.85765(11) 0.0827(12) Uani 1 1 d U . . C37 C 0.7255(6) 0.7074(5) 0.86001(15) 0.0912(16) Uani 1 1 d U . . H37 H 0.7867 0.7756 0.8594 0.109 Uiso 1 1 calc R . . C38 C 0.7376(5) 0.6178(6) 0.86334(15) 0.0931(17) Uani 1 1 d U . . H38 H 0.8062 0.6261 0.8649 0.112 Uiso 1 1 calc R . . C41 C 0.5100(12) 0.9650(9) 0.2500 0.143(4) Uani 1 2 d SU . . H41 H 0.5339 1.0386 0.2500 0.172 Uiso 1 2 calc SR . . C42 C 0.5847(12) 0.9316(12) 0.2500 0.166(5) Uani 1 2 d SU . . H42 H 0.6575 0.9838 0.2500 0.200 Uiso 1 2 calc SR . . C43 C 0.5587(11) 0.8307(12) 0.2500 0.144(4) Uani 1 2 d SU . . C44 C 0.4429(7) 0.7487(11) 0.2500 0.094(2) Uani 1 2 d SU . . C45 C 0.4136(11) 0.6405(13) 0.2500 0.094(2) Uani 1 2 d SU . . C46 C 0.4922(12) 0.5992(13) 0.2500 0.144(4) Uani 1 2 d SU . . C47 C 0.5903(12) 0.6765(14) 0.2500 0.166(5) Uani 1 2 d SU . . H47 H 0.6420 0.6553 0.2500 0.199 Uiso 1 2 calc SR . . C48 C 0.6305(9) 0.7866(11) 0.2500 0.146(4) Uani 1 2 d SU . . H48 H 0.7048 0.8331 0.2500 0.176 Uiso 1 2 calc SR . . 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 B1 0.094(6) 0.080(6) 0.100(6) -0.002(4) -0.004(5) 0.046(5) C11 0.098(5) 0.074(4) 0.100(5) 0.002(3) -0.005(4) 0.052(4) C12 0.099(4) 0.084(4) 0.093(4) 0.006(3) 0.003(3) 0.047(3) C13 0.097(4) 0.089(4) 0.107(4) 0.000(3) -0.004(3) 0.057(3) C21 0.114(6) 0.079(5) 0.084(6) -0.005(4) -0.013(5) 0.045(5) C22 0.105(6) 0.088(5) 0.090(6) -0.001(4) 0.001(5) 0.057(5) C23 0.115(5) 0.092(5) 0.093(5) -0.009(4) -0.006(5) 0.055(4) C24 0.155(7) 0.114(6) 0.075(6) -0.016(4) 0.006(5) 0.063(5) C25 0.166(7) 0.098(6) 0.087(6) -0.029(4) -0.043(6) 0.050(6) C26 0.134(6) 0.111(5) 0.096(5) -0.001(5) 0.004(6) 0.052(5) O27 0.117(3) 0.088(3) 0.090(3) 0.005(2) 0.006(3) 0.052(3) O28 0.105(3) 0.096(3) 0.079(3) -0.003(2) -0.003(3) 0.057(2) Cl29 0.205(2) 0.1747(18) 0.1024(13) -0.0103(12) 0.0238(13) 0.0903(15) Cl30 0.216(2) 0.201(2) 0.1124(14) -0.0520(14) -0.0274(14) 0.0509(18) N31 0.083(5) 0.073(5) 0.087(3) 0.001(2) -0.002(3) 0.046(4) C32 0.102(6) 0.082(6) 0.065(4) -0.002(3) -0.005(4) 0.059(6) C33 0.081(4) 0.084(5) 0.063(3) 0.000(3) -0.003(3) 0.040(4) C34 0.101(5) 0.080(5) 0.085(4) 0.004(3) 0.005(3) 0.046(4) C35 0.072(4) 0.089(5) 0.090(4) 0.007(4) 0.010(3) 0.032(5) N36 0.083(4) 0.092(4) 0.076(3) -0.001(3) 0.002(3) 0.046(4) C37 0.090(5) 0.072(5) 0.103(4) 0.003(3) -0.003(3) 0.033(4) C38 0.095(5) 0.101(5) 0.094(4) 0.003(4) -0.002(3) 0.057(5) C41 0.156(11) 0.116(8) 0.097(6) 0.000 0.000 0.023(8) C42 0.171(11) 0.149(10) 0.094(7) 0.000 0.000 0.016(9) C43 0.139(9) 0.165(9) 0.070(5) 0.000 0.000 0.033(8) C44 0.079(7) 0.113(9) 0.064(5) 0.000 0.000 0.028(8) C45 0.106(8) 0.141(8) 0.075(5) 0.000 0.000 0.091(8) C46 0.154(10) 0.178(11) 0.076(6) 0.000 0.000 0.066(9) C47 0.142(10) 0.217(12) 0.122(7) 0.000 0.000 0.077(9) C48 0.086(7) 0.210(10) 0.117(7) 0.000 0.000 0.053(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 B1 O28 1.458(7) . ? B1 O27 1.471(7) . ? B1 C11 1.581(8) . ? B1 N36 1.680(7) . ? C11 C13 1.379(6) . ? C11 C12 1.382(6) . ? C12 C12 1.398(9) 10_557 ? C13 C13 1.419(10) 10_557 ? C21 O27 1.354(7) . ? C21 C26 1.366(7) . ? C21 C22 1.388(7) . ? C22 C23 1.366(7) . ? C22 O28 1.369(6) . ? C23 C24 1.370(7) . ? C24 C25 1.376(8) . ? C24 Cl29 1.739(6) . ? C25 C26 1.402(8) . ? C25 Cl30 1.768(6) . ? N31 C32 1.312(6) 3_665 ? N31 C32 1.342(6) . ? C32 N31 1.312(6) 2_655 ? C32 C33 1.492(7) . ? C33 C38 1.379(6) . ? C33 C34 1.395(6) . ? C34 C35 1.387(6) . ? C35 N36 1.318(6) . ? N36 C37 1.344(6) . ? C37 C38 1.381(6) . ? C41 C42 1.372(15) . ? C41 C46 1.377(13) 2_665 ? C42 C43 1.300(13) . ? C43 C48 1.450(14) . ? C43 C44 1.476(13) . ? C44 C45 1.388(9) . ? C44 C45 1.402(9) 2_665 ? C45 C44 1.402(9) 3_565 ? C45 C46 1.509(15) . ? C46 C47 1.281(13) . ? C46 C41 1.377(13) 3_565 ? C47 C48 1.381(15) . ? 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 O28 B1 O27 107.6(5) . . ? O28 B1 C11 116.5(6) . . ? O27 B1 C11 116.0(6) . . ? O28 B1 N36 104.5(5) . . ? O27 B1 N36 105.8(5) . . ? C11 B1 N36 105.3(5) . . ? C13 C11 C12 116.8(5) . . ? C13 C11 B1 122.4(6) . . ? C12 C11 B1 120.6(6) . . ? C11 C12 C12 121.8(3) . 10_557 ? C11 C13 C13 121.4(3) . 10_557 ? O27 C21 C26 127.6(8) . . ? O27 C21 C22 112.3(7) . . ? C26 C21 C22 120.1(7) . . ? C23 C22 O28 127.8(7) . . ? C23 C22 C21 122.5(7) . . ? O28 C22 C21 109.7(7) . . ? C22 C23 C24 118.5(6) . . ? C23 C24 C25 119.1(6) . . ? C23 C24 Cl29 118.7(8) . . ? C25 C24 Cl29 122.2(8) . . ? C24 C25 C26 123.0(6) . . ? C24 C25 Cl30 118.9(8) . . ? C26 C25 Cl30 118.1(8) . . ? C21 C26 C25 116.6(7) . . ? C21 O27 B1 103.1(5) . . ? C22 O28 B1 104.3(5) . . ? C32 N31 C32 111.8(6) 3_665 . ? N31 C32 N31 128.2(6) 2_655 . ? N31 C32 C33 116.9(9) 2_655 . ? N31 C32 C33 114.9(9) . . ? C38 C33 C34 117.8(5) . . ? C38 C33 C32 122.0(7) . . ? C34 C33 C32 120.2(7) . . ? C35 C34 C33 118.9(6) . . ? N36 C35 C34 122.8(6) . . ? C35 N36 C37 118.8(5) . . ? C35 N36 B1 120.9(6) . . ? C37 N36 B1 119.8(6) . . ? N36 C37 C38 121.8(5) . . ? C33 C38 C37 119.9(5) . . ? C42 C41 C46 122.0(14) . 2_665 ? C43 C42 C41 123.2(16) . . ? C42 C43 C48 127.8(16) . . ? C42 C43 C44 117.9(16) . . ? C48 C43 C44 114.4(13) . . ? C45 C44 C45 117.3(9) . 2_665 ? C45 C44 C43 118.7(15) . . ? C45 C44 C43 124.0(15) 2_665 . ? C44 C45 C44 122.7(9) . 3_565 ? C44 C45 C46 124.6(15) . . ? C44 C45 C46 112.7(15) 3_565 . ? C47 C46 C41 127.9(17) . 3_565 ? C47 C46 C45 111.8(15) . . ? C41 C46 C45 120.2(13) 3_565 . ? C46 C47 C48 129.6(16) . . ? C47 C48 C43 120.9(12) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 47.97 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.197 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.033 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.004 536.0 113.1 _platon_squeeze_details ; ; # Attachment '- 3.cif' data_rbar3c _database_code_depnum_ccdc_archive 'CCDC 827250' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H60 B6 Cl12 N12 O12' _chemical_formula_weight 2207.94 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' N N 0.0311 0.0180 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.5162(6) _cell_length_b 13.5162(6) _cell_length_c 93.155(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14738.2(11) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5619 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 51.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.020 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6732 _exptl_absorpt_coefficient_mu 3.688 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9398 _exptl_absorpt_correction_T_max 0.9847 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0150 0 0 -1 0.0070 -4 0 -3 0.0550 -5 5 -1 0.0360 3 -5 -1 0.0490 9 -1 6 0.1030 1 4 3 0.0630 _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 1 _diffrn_source_power 0.05 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54186 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter' _diffrn_ambient_temperature 0 _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 217 frames, detector distance = 100 mm ; _diffrn_reflns_number 7164 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -71 _diffrn_reflns_limit_l_max 82 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 51.50 _reflns_number_total 1729 _reflns_number_gt 1081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0972P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.000013(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1729 _refine_ls_number_parameters 227 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.858 _refine_ls_shift/su_max 0.002 _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 B1 B 0.8563(5) 0.2092(5) 0.94862(6) 0.0441(16) Uani 1 1 d . . . C11 C 0.8752(4) 0.2183(4) 0.93194(5) 0.0415(13) Uani 1 1 d . . . C12 C 0.9298(4) 0.1677(4) 0.92495(6) 0.0527(15) Uani 1 1 d . . . H12 H 0.9648 0.1364 0.9304 0.063 Uiso 1 1 calc R . . C13 C 0.8289(4) 0.2673(4) 0.92321(7) 0.0537(15) Uani 1 1 d . . . H13 H 0.7932 0.3038 0.9274 0.064 Uiso 1 1 calc R . . C21 C 0.9366(4) 0.2536(4) 0.97059(6) 0.0450(13) Uani 1 1 d . . . C22 C 0.8649(4) 0.3007(4) 0.96925(6) 0.0439(13) Uani 1 1 d . . . C23 C 0.8405(4) 0.3488(4) 0.98064(6) 0.0517(14) Uani 1 1 d . . . H23 H 0.7944 0.3814 0.9796 0.062 Uiso 1 1 calc R . . C24 C 0.8877(5) 0.3469(5) 0.99387(6) 0.0613(17) Uani 1 1 d . . . C25 C 0.9614(5) 0.3025(5) 0.99522(6) 0.0591(16) Uani 1 1 d . . . C26 C 0.9865(4) 0.2573(5) 0.98345(6) 0.0583(16) Uani 1 1 d . . . H26 H 1.0368 0.2295 0.9843 0.070 Uiso 1 1 calc R . . O27 O 0.9441(2) 0.2080(3) 0.95774(4) 0.0475(10) Uani 1 1 d . . . O28 O 0.8287(3) 0.2911(2) 0.95533(4) 0.0454(9) Uani 1 1 d . . . Cl29 Cl 0.85306(14) 0.40123(15) 1.008610(17) 0.0857(6) Uani 1 1 d . . . Cl30 Cl 1.01989(15) 0.30265(19) 1.011515(17) 0.1007(7) Uani 1 1 d . . . N31 N 0.3325(3) -0.2326(3) 0.95458(4) 0.0322(10) Uani 1 1 d . . . C32 C 0.4285(4) -0.2374(4) 0.95456(4) 0.0284(11) Uani 1 1 d . . . C33 C 0.5369(4) -0.1267(4) 0.95386(4) 0.0299(11) Uani 1 1 d . . . C34 C 0.6429(4) -0.1204(4) 0.95386(5) 0.0377(12) Uani 1 1 d . . . H34 H 0.6479 -0.1863 0.9547 0.045 Uiso 1 1 calc R . . C35 C 0.7396(4) -0.0157(4) 0.95261(5) 0.0398(13) Uani 1 1 d . . . H35 H 0.8101 -0.0121 0.9525 0.048 Uiso 1 1 calc R . . N36 N 0.7367(3) 0.0815(3) 0.95159(4) 0.0346(10) Uani 1 1 d . . . C37 C 0.6360(4) 0.0757(4) 0.95169(5) 0.0399(13) Uani 1 1 d . . . H37 H 0.6334 0.1429 0.9509 0.048 Uiso 1 1 calc R . . C38 C 0.5360(4) -0.0255(4) 0.95286(5) 0.0372(13) Uani 1 1 d . . . H38 H 0.4669 -0.0261 0.9530 0.045 Uiso 1 1 calc R . . C41 C 0.5750(6) 0.9649(5) 0.91666(9) 0.120(4) Uani 1 1 d DU . . H41 H 0.6155 1.0444 0.9167 0.145 Uiso 1 1 calc R . . C42 C 0.4564(6) 0.9079(5) 0.91658(6) 0.090(2) Uani 1 1 d DU . . H42 H 0.4178 0.9487 0.9165 0.108 Uiso 1 1 calc R . . C43 C 0.3954(4) 0.7881(4) 0.91667(5) 0.0455(13) Uani 1 1 d DU . . 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 B1 0.030(4) 0.033(4) 0.057(5) 0.001(3) -0.002(3) 0.006(3) C11 0.030(3) 0.026(3) 0.046(3) 0.001(2) 0.000(3) -0.002(2) C12 0.044(3) 0.051(4) 0.051(5) 0.007(3) -0.002(3) 0.014(3) C13 0.053(4) 0.045(3) 0.050(4) -0.001(3) -0.003(3) 0.016(3) C21 0.028(3) 0.047(3) 0.040(4) 0.002(3) 0.004(3) 0.003(3) C22 0.037(3) 0.032(3) 0.045(4) 0.003(3) -0.002(3) 0.004(3) C23 0.045(3) 0.045(3) 0.048(4) -0.005(3) -0.001(3) 0.010(3) C24 0.051(4) 0.062(4) 0.046(4) -0.008(3) 0.003(3) 0.010(3) C25 0.044(4) 0.076(4) 0.042(4) -0.004(3) -0.006(3) 0.019(3) C26 0.037(3) 0.074(4) 0.052(5) 0.002(3) -0.003(3) 0.019(3) O27 0.027(2) 0.050(2) 0.050(3) 0.0005(17) -0.0004(16) 0.0076(16) O28 0.046(2) 0.031(2) 0.046(3) -0.0013(15) -0.0050(17) 0.0095(16) Cl29 0.0786(12) 0.0989(13) 0.0666(11) -0.0225(9) -0.0010(8) 0.0347(10) Cl30 0.0889(13) 0.1637(19) 0.0536(12) -0.0091(11) -0.0198(9) 0.0663(13) N31 0.020(3) 0.027(3) 0.047(3) 0.0000(17) 0.0000(17) 0.009(3) C32 0.025(4) 0.025(3) 0.030(3) 0.003(2) 0.002(2) 0.008(3) C33 0.027(3) 0.027(3) 0.037(3) -0.001(2) -0.001(2) 0.014(3) C34 0.033(3) 0.029(3) 0.051(3) 0.004(2) -0.002(2) 0.016(3) C35 0.026(3) 0.037(3) 0.053(4) 0.000(2) -0.001(2) 0.014(3) N36 0.029(3) 0.028(3) 0.039(3) 0.0004(17) 0.0010(17) 0.009(2) C37 0.033(3) 0.031(3) 0.054(4) -0.002(2) -0.002(2) 0.014(3) C38 0.025(3) 0.026(3) 0.059(4) -0.003(2) 0.002(2) 0.012(3) C41 0.140(6) 0.059(4) 0.060(4) -0.006(4) 0.009(6) -0.027(4) C42 0.135(5) 0.053(4) 0.057(4) -0.002(3) 0.001(4) 0.028(4) C43 0.059(3) 0.033(3) 0.032(3) 0.002(2) 0.000(3) 0.013(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 B1 O27 1.466(7) . ? B1 O28 1.473(7) . ? B1 C11 1.569(8) . ? B1 N36 1.696(7) . ? C11 C13 1.381(7) . ? C11 C12 1.392(7) . ? C12 C13 1.386(7) 10_546 ? C13 C12 1.386(7) 10_546 ? C21 C26 1.363(7) . ? C21 O27 1.373(6) . ? C21 C22 1.407(7) . ? C22 O28 1.369(6) . ? C22 C23 1.368(7) . ? C23 C24 1.394(7) . ? C24 C25 1.402(8) . ? C24 Cl29 1.729(6) . ? C25 C26 1.378(8) . ? C25 Cl30 1.711(6) . ? N31 C32 1.330(6) 2_545 ? N31 C32 1.332(5) . ? C32 N31 1.330(5) 3_655 ? C32 C33 1.482(6) . ? C33 C38 1.377(6) . ? C33 C34 1.391(6) . ? C34 C35 1.369(6) . ? C35 N36 1.338(6) . ? N36 C37 1.323(6) . ? C37 C38 1.364(6) . ? C41 C41 1.325(13) 10_456 ? C41 C42 1.389(9) . ? C42 C43 1.402(7) . ? C43 C43 1.390(9) 10_456 ? C43 C43 1.453(9) 12_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O27 B1 O28 105.8(4) . . ? O27 B1 C11 118.2(5) . . ? O28 B1 C11 117.0(5) . . ? O27 B1 N36 105.0(4) . . ? O28 B1 N36 103.0(4) . . ? C11 B1 N36 106.1(4) . . ? C13 C11 C12 116.0(5) . . ? C13 C11 B1 121.7(5) . . ? C12 C11 B1 122.0(5) . . ? C13 C12 C11 122.6(5) 10_546 . ? C12 C13 C11 121.4(5) 10_546 . ? C26 C21 O27 129.5(5) . . ? C26 C21 C22 120.1(5) . . ? O27 C21 C22 110.4(5) . . ? O28 C22 C23 128.3(5) . . ? O28 C22 C21 109.6(5) . . ? C23 C22 C21 122.1(5) . . ? C22 C23 C24 117.1(5) . . ? C23 C24 C25 121.2(5) . . ? C23 C24 Cl29 118.1(5) . . ? C25 C24 Cl29 120.8(5) . . ? C26 C25 C24 120.2(5) . . ? C26 C25 Cl30 119.4(5) . . ? C24 C25 Cl30 120.4(5) . . ? C21 C26 C25 119.2(6) . . ? C21 O27 B1 105.0(4) . . ? C22 O28 B1 105.1(4) . . ? C32 N31 C32 114.3(4) 2_545 . ? N31 C32 N31 125.7(4) 3_655 . ? N31 C32 C33 117.8(5) 3_655 . ? N31 C32 C33 116.5(5) . . ? C38 C33 C34 117.3(4) . . ? C38 C33 C32 120.7(4) . . ? C34 C33 C32 122.0(4) . . ? C35 C34 C33 119.1(4) . . ? N36 C35 C34 122.6(4) . . ? C37 N36 C35 118.4(4) . . ? C37 N36 B1 119.3(4) . . ? C35 N36 B1 122.0(4) . . ? N36 C37 C38 122.3(4) . . ? C37 C38 C33 120.3(4) . . ? C41 C41 C42 121.2(4) 10_456 . ? C41 C42 C43 119.4(6) . . ? C42 C43 C43 119.4(4) . 10_456 ? C42 C43 C43 120.6(4) . 12_556 ? C43 C43 C43 120.00(3) 10_456 12_556 ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 51.50 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.384 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.058 # Attachment '- 4.cif' data_hex _database_code_depnum_ccdc_archive 'CCDC 827251' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H84 B6 Cl12 N12 O12' _chemical_formula_weight 2664.49 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' N N 0.0311 0.0180 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 13.5417(3) _cell_length_b 13.5417(3) _cell_length_c 118.223(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 18774.9(10) _cell_formula_units_Z 6 _cell_measurement_temperature 270(2) _cell_measurement_reflns_used 18880 _cell_measurement_theta_min 3.79 _cell_measurement_theta_max 47.44 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8172 _exptl_absorpt_coefficient_mu 2.999 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3610 _exptl_absorpt_correction_T_max 0.7088 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 0 1 0.1410 0 1 -4 0.1080 1 -1 -4 0.0890 0 0 -1 0.0170 0 0 1 0.0500 0 -2 5 0.1540 -2 2 -5 0.1460 1 0 4 0.0900 _exptl_special_details ; ? ; _diffrn_ambient_temperature 270(2) _diffrn_radiation_wavelength 1.54186 _diffrn_source_voltage 50 _diffrn_source_current 1 _diffrn_source_power 0.05 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter' _diffrn_measurement_details ; 396 frames, detector distance = 140 mm ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_detector_type STOE _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11423 _diffrn_reflns_av_R_equivalents 0.1216 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -107 _diffrn_reflns_limit_l_max 100 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 47.02 _reflns_number_total 1849 _reflns_number_gt 1650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1156P)^2^+17.2304P] 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 SHELXL _refine_ls_extinction_coef 0.000025(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1849 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.005 _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 B1 B 0.3583(4) 0.2104(4) 0.96019(4) 0.0525(13) Uani 1 1 d . . . C11 C 0.3517(4) 0.2225(3) 0.94697(3) 0.0547(11) Uani 1 1 d . . . C12 C 0.4453(4) 0.2541(4) 0.94008(4) 0.0669(13) Uani 1 1 d . . . H12 H 0.5155 0.2767 0.9435 0.080 Uiso 1 1 calc R . . C13 C 0.4393(4) 0.2535(4) 0.92849(4) 0.0694(13) Uani 1 1 d . . . H13 H 0.5048 0.2738 0.9243 0.083 Uiso 1 1 calc R . . C14 C 0.3375(4) 0.2232(3) 0.92286(3) 0.0591(12) Uani 1 1 d . . . C15 C 0.2423(4) 0.1924(4) 0.92968(4) 0.0696(13) Uani 1 1 d . . . H15 H 0.1724 0.1715 0.9263 0.084 Uiso 1 1 calc R . . C16 C 0.2497(4) 0.1924(4) 0.94139(4) 0.0691(13) Uani 1 1 d . . . H16 H 0.1845 0.1715 0.9457 0.083 Uiso 1 1 calc R . . C21 C 0.4381(4) 0.3009(3) 0.97635(3) 0.0532(11) Uani 1 1 d . . . C22 C 0.3205(4) 0.2547(3) 0.97722(3) 0.0533(11) Uani 1 1 d . . . C23 C 0.2718(4) 0.2570(4) 0.98724(4) 0.0682(13) Uani 1 1 d . . . H23 H 0.1937 0.2287 0.9878 0.082 Uiso 1 1 calc R . . C24 C 0.3441(5) 0.3039(4) 0.99660(4) 0.0695(13) Uani 1 1 d . . . C25 C 0.4602(5) 0.3470(4) 0.99573(4) 0.0662(12) Uani 1 1 d . . . C26 C 0.5090(4) 0.3485(3) 0.98544(4) 0.0591(12) Uani 1 1 d . . . H26 H 0.5876 0.3809 0.9847 0.071 Uiso 1 1 calc R . . O27 O 0.4674(2) 0.2910(2) 0.96556(2) 0.0540(8) Uani 1 1 d . . . O28 O 0.2686(2) 0.2099(2) 0.96713(2) 0.0569(8) Uani 1 1 d . . . Cl29 Cl 0.28259(13) 0.30382(15) 1.009458(10) 0.1050(7) Uani 1 1 d . . . Cl30 Cl 0.54748(12) 0.40145(12) 1.007509(10) 0.0904(6) Uani 1 1 d . . . N31 N 0.4351(2) -0.2334(2) 0.96315(2) 0.0450(9) Uani 1 1 d . . . C32 C 0.3347(4) -0.2367(3) 0.96314(3) 0.0428(10) Uani 1 1 d . . . C33 C 0.3383(3) -0.1257(3) 0.96292(3) 0.0436(10) Uani 1 1 d . . . C34 C 0.2397(3) -0.1189(3) 0.96294(3) 0.0507(11) Uani 1 1 d . . . H34 H 0.1686 -0.1847 0.9632 0.061 Uiso 1 1 calc R . . C35 C 0.2481(3) -0.0141(4) 0.96253(3) 0.0506(11) Uani 1 1 d . . . H35 H 0.1816 -0.0101 0.9626 0.061 Uiso 1 1 calc R . . N36 N 0.3483(3) 0.0828(3) 0.96205(2) 0.0447(8) Uani 1 1 d . . . C37 C 0.4428(4) 0.0756(3) 0.96211(3) 0.0510(11) Uani 1 1 d . . . H37 H 0.5129 0.1426 0.9619 0.061 Uiso 1 1 calc R . . C38 C 0.4412(3) -0.0258(3) 0.96251(3) 0.0503(11) Uani 1 1 d . . . H38 H 0.5091 -0.0273 0.9625 0.060 Uiso 1 1 calc R . . C41 C 0.9041(5) 0.4249(5) 0.06730(4) 0.0841(15) Uani 1 1 d . . . H41 H 0.9340 0.3762 0.0672 0.101 Uiso 1 1 calc R . . C42 C 0.7876(4) 0.3794(4) 0.06726(3) 0.0661(12) Uani 1 1 d . . . C43 C 0.7113(4) 0.2572(4) 0.06735(3) 0.0664(12) Uani 1 1 d . . . C44 C 0.7500(5) 0.1797(5) 0.06745(4) 0.0883(16) Uani 1 1 d . . . H44 H 0.8283 0.2081 0.0675 0.106 Uiso 1 1 calc R . . C45 C 0.6795(5) 0.0638(5) 0.06753(5) 0.0901(16) Uani 1 1 d . . . H45 H 0.7094 0.0151 0.0677 0.108 Uiso 1 1 calc R . . C46 C 0.5648(6) 0.0216(5) 0.06743(5) 0.0984(17) Uani 1 1 d . . . H46 H 0.5154 -0.0569 0.0675 0.118 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 B1 0.059(3) 0.047(3) 0.052(3) 0.002(2) 0.008(3) 0.027(2) C11 0.072(3) 0.050(2) 0.052(3) 0.002(2) 0.000(3) 0.038(2) C12 0.081(3) 0.076(3) 0.052(3) 0.007(2) 0.001(3) 0.046(3) C13 0.086(4) 0.078(3) 0.052(3) 0.010(2) 0.013(3) 0.047(3) C14 0.084(3) 0.059(3) 0.045(2) 0.005(2) 0.007(3) 0.044(2) C15 0.092(4) 0.082(3) 0.053(3) 0.000(2) -0.004(3) 0.057(3) C16 0.095(4) 0.079(3) 0.050(3) 0.006(2) 0.014(3) 0.056(3) C21 0.078(4) 0.049(2) 0.041(3) 0.002(2) 0.007(2) 0.038(2) C22 0.077(4) 0.063(3) 0.036(3) 0.002(2) 0.004(2) 0.047(3) C23 0.082(3) 0.082(3) 0.061(3) 0.004(3) 0.004(3) 0.056(3) C24 0.097(4) 0.086(3) 0.046(3) -0.001(2) 0.007(3) 0.062(3) C25 0.090(4) 0.072(3) 0.051(3) -0.009(2) -0.009(3) 0.051(3) C26 0.073(3) 0.058(3) 0.053(3) -0.004(2) 0.005(3) 0.039(2) O27 0.0678(19) 0.0454(16) 0.0468(19) 0.0012(12) 0.0084(14) 0.0268(14) O28 0.0747(19) 0.0637(18) 0.0460(19) 0.0028(14) 0.0026(15) 0.0448(15) Cl29 0.1242(12) 0.1664(15) 0.0533(9) -0.0085(8) 0.0122(7) 0.0945(11) Cl30 0.1156(11) 0.1068(11) 0.0642(9) -0.0213(6) -0.0207(7) 0.0673(9) N31 0.044(2) 0.041(2) 0.051(2) 0.0007(13) -0.0014(14) 0.0222(18) C32 0.047(3) 0.047(3) 0.037(2) 0.0011(16) 0.0001(17) 0.024(3) C33 0.048(3) 0.050(3) 0.035(2) 0.0010(17) 0.0017(17) 0.027(2) C34 0.052(3) 0.045(3) 0.055(3) 0.0020(18) 0.0024(18) 0.024(2) C35 0.045(3) 0.063(3) 0.050(3) 0.000(2) 0.0020(18) 0.033(3) N36 0.049(2) 0.048(2) 0.0397(19) 0.0014(14) 0.0019(14) 0.026(2) C37 0.050(3) 0.046(3) 0.054(3) 0.0021(18) 0.0011(19) 0.023(2) C38 0.045(3) 0.048(3) 0.060(3) 0.0004(18) -0.0021(18) 0.025(2) C41 0.076(4) 0.079(4) 0.097(4) 0.003(3) 0.002(3) 0.039(3) C42 0.067(4) 0.073(4) 0.052(3) -0.002(2) -0.004(2) 0.030(4) C43 0.071(4) 0.079(4) 0.054(3) 0.001(2) 0.000(2) 0.042(4) C44 0.086(4) 0.096(5) 0.090(4) 0.002(3) -0.002(3) 0.050(4) C45 0.090(4) 0.066(4) 0.118(5) 0.007(3) -0.002(3) 0.042(3) C46 0.102(5) 0.075(4) 0.112(4) 0.007(3) 0.006(3) 0.040(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O28 1.462(5) . ? B1 O27 1.472(5) . ? B1 C11 1.579(6) . ? B1 N36 1.680(5) . ? C11 C12 1.383(6) . ? C11 C16 1.394(6) . ? C12 C13 1.373(6) . ? C13 C14 1.396(6) . ? C14 C15 1.396(6) . ? C14 C14 1.467(8) 12_556 ? C15 C16 1.389(6) . ? C21 O27 1.363(4) . ? C21 C26 1.369(6) . ? C21 C22 1.393(6) . ? C22 O28 1.364(5) . ? C22 C23 1.364(6) . ? C23 C24 1.401(7) . ? C24 C25 1.381(7) . ? C24 Cl29 1.733(4) . ? C25 C26 1.379(6) . ? C25 Cl30 1.734(5) . ? N31 C32 1.329(4) 3_655 ? N31 C32 1.338(4) . ? C32 N31 1.329(4) 2_545 ? C32 C33 1.480(5) . ? C33 C38 1.375(5) . ? C33 C34 1.384(5) . ? C34 C35 1.365(5) . ? C35 N36 1.336(5) . ? N36 C37 1.330(5) . ? C37 C38 1.363(5) . ? C41 C42 1.377(6) . ? C41 C46 1.403(7) 2_655 ? C42 C43 1.416(6) 2_655 ? C42 C43 1.448(6) . ? C43 C44 1.388(7) . ? C43 C42 1.416(6) 3_665 ? C44 C45 1.370(7) . ? C45 C46 1.361(7) . ? C46 C41 1.403(7) 3_665 ? 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 O28 B1 O27 106.6(3) . . ? O28 B1 C11 117.8(4) . . ? O27 B1 C11 116.0(3) . . ? O28 B1 N36 106.4(3) . . ? O27 B1 N36 103.9(3) . . ? C11 B1 N36 104.8(3) . . ? C12 C11 C16 115.7(4) . . ? C12 C11 B1 121.6(4) . . ? C16 C11 B1 122.5(4) . . ? C13 C12 C11 122.9(4) . . ? C12 C13 C14 121.7(4) . . ? C13 C14 C15 116.2(4) . . ? C13 C14 C14 122.2(5) . 12_556 ? C15 C14 C14 121.5(5) . 12_556 ? C16 C15 C14 121.3(4) . . ? C15 C16 C11 122.2(4) . . ? O27 C21 C26 127.6(4) . . ? O27 C21 C22 110.4(4) . . ? C26 C21 C22 121.9(4) . . ? O28 C22 C23 128.5(4) . . ? O28 C22 C21 110.7(3) . . ? C23 C22 C21 120.7(4) . . ? C22 C23 C24 117.4(4) . . ? C25 C24 C23 121.5(4) . . ? C25 C24 Cl29 120.7(4) . . ? C23 C24 Cl29 117.7(4) . . ? C26 C25 C24 120.5(4) . . ? C26 C25 Cl30 118.8(4) . . ? C24 C25 Cl30 120.6(4) . . ? C21 C26 C25 117.8(4) . . ? C21 O27 B1 104.0(3) . . ? C22 O28 B1 104.3(3) . . ? C32 N31 C32 115.1(4) 3_655 . ? N31 C32 N31 124.9(3) 2_545 . ? N31 C32 C33 118.4(4) 2_545 . ? N31 C32 C33 116.7(4) . . ? C38 C33 C34 118.1(3) . . ? C38 C33 C32 120.2(4) . . ? C34 C33 C32 121.7(4) . . ? C35 C34 C33 119.1(4) . . ? N36 C35 C34 122.6(3) . . ? C37 N36 C35 118.0(3) . . ? C37 N36 B1 119.4(3) . . ? C35 N36 B1 122.4(3) . . ? N36 C37 C38 122.8(4) . . ? C37 C38 C33 119.3(4) . . ? C42 C41 C46 121.2(5) . 2_655 ? C41 C42 C43 119.1(5) . 2_655 ? C41 C42 C43 120.9(5) . . ? C43 C42 C43 120.0(5) 2_655 . ? C44 C43 C42 117.3(5) . 3_665 ? C44 C43 C42 122.7(5) . . ? C42 C43 C42 120.0(5) 3_665 . ? C45 C44 C43 123.8(5) . . ? C46 C45 C44 118.5(5) . . ? C45 C46 C41 120.2(5) . 3_665 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 47.02 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.344 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.067