Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Clara Vinas' 'Gemma Barbera' 'Raikko Kivekas' 'Reijo Sillanpaa' 'Francesc Teixidor' _publ_contact_author_name 'Clara Vinas' _publ_contact_author_address ; Materials Moleculars i Supramoleculars C.S.I.C.(I.C.M.A.B.) I.C.M.A.B. Campus U.A.B. Bellaterra 08193 SPAIN ; _publ_contact_author_email CLARA@ICMAB.ES _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Unprecedented water-stable dinegative dicarbollide ; data_[HNMe3]2[3] _database_code_depnum_ccdc_archive 'CCDC 635883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C2 H3 B9 I8 2-, 2(C3 H10 N 1+)' _chemical_formula_sum 'C8 H23 B9 I8 N2' _chemical_formula_weight 1259.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'A m a 2' _symmetry_space_group_name_Hall 'A 2 -2a' _symmetry_Int_Tables_number 40 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y, z' '-x+1/2, y, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 11.1115(6) _cell_length_b 14.8951(8) _cell_length_c 17.5202(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2899.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1204 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.682 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.886 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 8.559 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998) I/sigma threshold for reflections = 5.000 Delta(U)/lambda**2 = 0.000 Highest even order spherical harmonic = 6 Highest odd order spherical harmonic = 3 ; _exptl_absorpt_correction_T_min 0.1918 _exptl_absorpt_correction_T_max 0.6013 _exptl_absorpt_Rmerge_before 0.0914 _exptl_absorpt_Rmerge_after 0.0486 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_type Mok\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_number 6423 _diffrn_standards_decay_% <1 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 25.66 _reflns_number_total 2364 _reflns_number_gt 1974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowsky & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowsky & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 ; w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+24.2974P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(12) _refine_ls_number_reflns 2364 _refine_ls_number_parameters 142 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.043 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.2500 0.79243(10) 1.0000 0.0500(5) Uani 1 d S . . I2 I 0.54439(12) 0.64866(7) 0.92218(12) 0.0523(4) Uani 1 d . . . I6 I 0.43060(7) 0.88663(5) 0.81601(12) 0.0469(2) Uani 1 d . . . I10 I 0.2500 0.81354(10) 0.62452(9) 0.0517(5) Uani 1 d S . . I11 I 0.54332(12) 0.65479(7) 0.69260(11) 0.0511(4) Uani 1 d . . . B1 B 0.2500 0.7157(15) 0.8915(13) 0.039(7) Uani 1 d S . . B2 B 0.3791(19) 0.6627(11) 0.8603(10) 0.033(4) Uani 1 d D . . B3 B 0.2500 0.6025(13) 0.8859(11) 0.033(5) Uani 1 d SD . . H3 H 0.2500 0.5579 0.9374 0.039 Uiso 1 calc SR . . B6 B 0.3318(11) 0.7602(8) 0.8064(11) 0.033(3) Uani 1 d . . . C7 C 0.3204(10) 0.5787(8) 0.7997(8) 0.035(3) Uani 1 d D . . H7 H 0.374(4) 0.515(2) 0.794(3) 0.042 Uiso 1 d D . . B10 B 0.2500 0.7300(16) 0.7262(12) 0.025(5) Uani 1 d S . . B11 B 0.372(2) 0.6647(11) 0.7556(11) 0.038(5) Uani 1 d . . . N13 N 0.2500 0.6205(13) 1.1529(11) 0.061(5) Uani 1 d SD . . H13 H 0.2500 0.6787 1.1337 0.073 Uiso 1 calc SR . . C14 C 0.2500 0.6318(18) 1.2362(14) 0.076(8) Uani 1 d SD . . H14A H 0.2009 0.5846 1.2596 0.114 Uiso 0.50 calc PR . . H14B H 0.2165 0.6907 1.2492 0.114 Uiso 0.50 calc PR . . H14C H 0.3327 0.6276 1.2554 0.114 Uiso 0.50 calc PR . . C15 C 0.360(2) 0.5769(13) 1.1178(12) 0.077(6) Uani 1 d . . . H15A H 0.3610 0.5129 1.1308 0.115 Uiso 1 calc R . . H15B H 0.4327 0.6058 1.1375 0.115 Uiso 1 calc R . . H15C H 0.3569 0.5837 1.0622 0.115 Uiso 1 calc R . . N16 N 0.2500 0.6003(15) 0.5357(12) 0.088(7) Uani 1 d SDU . . H16 H 0.2500 0.6567 0.5585 0.106 Uiso 1 calc SR . . C17 C 0.2500 0.5336(16) 0.6011(13) 0.070(7) Uani 1 d SD . . H17A H 0.3316 0.5283 0.6219 0.105 Uiso 0.50 calc PR . . H17B H 0.2231 0.4749 0.5825 0.105 Uiso 0.50 calc PR . . H17C H 0.1953 0.5546 0.6412 0.105 Uiso 0.50 calc PR . . C18 C 0.370(3) 0.592(2) 0.497(2) 0.179(16) Uani 1 d DU . . H18A H 0.4327 0.6168 0.5298 0.268 Uiso 1 calc R . . H18B H 0.3679 0.6264 0.4487 0.268 Uiso 1 calc R . . H18C H 0.3866 0.5292 0.4857 0.268 Uiso 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 I1 0.0772(13) 0.0413(8) 0.0315(7) -0.0108(6) 0.000 0.000 I2 0.0487(10) 0.0484(7) 0.0597(7) -0.0030(5) -0.0185(6) 0.0037(5) I6 0.0516(5) 0.0320(4) 0.0570(5) -0.0047(6) 0.0036(7) -0.0109(3) I10 0.0784(13) 0.0428(8) 0.0341(7) 0.0075(7) 0.000 0.000 I11 0.0484(10) 0.0467(6) 0.0582(7) -0.0079(5) 0.0190(6) -0.0011(5) B1 0.07(2) 0.018(11) 0.025(12) -0.015(10) 0.000 0.000 B2 0.034(12) 0.037(9) 0.029(8) -0.007(7) -0.012(8) 0.005(8) B3 0.054(14) 0.026(11) 0.018(9) 0.004(8) 0.000 0.000 B6 0.038(7) 0.023(6) 0.037(7) 0.003(8) -0.021(11) 0.000(5) C7 0.040(6) 0.036(6) 0.028(8) -0.018(6) 0.006(6) 0.003(5) B10 0.014(12) 0.030(12) 0.031(12) 0.000(10) 0.000 0.000 B11 0.053(15) 0.026(9) 0.036(9) 0.001(8) 0.012(9) 0.011(9) N13 0.055(12) 0.048(11) 0.079(14) 0.011(11) 0.000 0.000 C14 0.055(16) 0.058(17) 0.12(2) 0.014(16) 0.000 0.000 C15 0.103(17) 0.076(13) 0.051(10) 0.009(10) 0.010(11) -0.013(12) N16 0.134(14) 0.060(11) 0.070(11) -0.031(10) 0.000 0.000 C17 0.088(19) 0.054(15) 0.068(17) -0.011(12) 0.000 0.000 C18 0.20(3) 0.19(3) 0.15(2) -0.02(2) 0.04(2) -0.06(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 I1 B1 2.22(2) . ? I2 B2 2.143(19) . ? I6 B6 2.186(12) . ? I10 B10 2.17(2) . ? I11 B11 2.20(2) . ? B1 B3 1.69(3) . ? B1 B2 1.73(2) 4 ? B1 B2 1.73(2) . ? B1 B6 1.87(3) 4 ? B1 B6 1.87(3) . ? B2 B3 1.75(2) . ? B2 C7 1.76(2) . ? B2 B6 1.81(2) . ? B2 B11 1.836(16) . ? B3 C7 1.74(2) 4 ? B3 C7 1.74(2) . ? B3 B2 1.75(2) 4 ? B3 H3 1.1200 . ? B6 B10 1.73(2) . ? B6 B11 1.74(2) . ? B6 B6 1.82(2) 4 ? C7 C7 1.57(2) 4 ? C7 B11 1.60(2) . ? C7 H7 1.13(2) . ? B10 B6 1.73(2) 4 ? B10 B11 1.75(2) 4 ? B10 B11 1.75(2) . ? N13 C14 1.47(2) . ? N13 C15 1.51(2) 4 ? N13 C15 1.51(2) . ? N13 H13 0.9300 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N16 C18 1.50(3) 4 ? N16 C18 1.50(3) . ? N16 C17 1.52(2) . ? N16 H16 0.9300 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B3 B1 B2 61.6(9) . 4 ? B3 B1 B2 61.6(9) . . ? B2 B1 B2 112.3(16) 4 . ? B3 B1 B6 107.9(12) . 4 ? B2 B1 B6 60.3(9) 4 4 ? B2 B1 B6 108.3(14) . 4 ? B3 B1 B6 107.9(12) . . ? B2 B1 B6 108.3(14) 4 . ? B2 B1 B6 60.3(9) . . ? B6 B1 B6 58.2(11) 4 . ? B3 B1 I1 124.4(15) . . ? B2 B1 I1 120.5(9) 4 . ? B2 B1 I1 120.5(9) . . ? B6 B1 I1 120.1(11) 4 . ? B6 B1 I1 120.1(11) . . ? B1 B2 B3 58.1(11) . . ? B1 B2 C7 102.0(12) . . ? B3 B2 C7 59.2(9) . . ? B1 B2 B6 63.7(12) . . ? B3 B2 B6 107.9(12) . . ? C7 B2 B6 98.5(10) . . ? B1 B2 B11 105.9(16) . . ? B3 B2 B11 103.3(16) . . ? C7 B2 B11 52.8(9) . . ? B6 B2 B11 56.9(10) . . ? B1 B2 I2 126.6(11) . . ? B3 B2 I2 121.5(10) . . ? C7 B2 I2 123.5(10) . . ? B6 B2 I2 126.2(10) . . ? B11 B2 I2 122.9(17) . . ? B1 B3 C7 104.7(12) . 4 ? B1 B3 C7 104.7(12) . . ? C7 B3 C7 53.6(10) 4 . ? B1 B3 B2 60.3(8) . . ? C7 B3 B2 104.5(12) 4 . ? C7 B3 B2 60.8(8) . . ? B1 B3 B2 60.3(8) . 4 ? C7 B3 B2 60.8(8) 4 4 ? C7 B3 B2 104.5(12) . 4 ? B2 B3 B2 110.1(16) . 4 ? B1 B3 H3 123.0 . . ? C7 B3 H3 125.4 4 . ? C7 B3 H3 125.4 . . ? B2 B3 H3 120.7 . . ? B2 B3 H3 120.7 4 . ? B10 B6 B11 60.5(11) . . ? B10 B6 B2 111.5(12) . . ? B11 B6 B2 62.3(7) . . ? B10 B6 B6 58.3(6) . 4 ? B11 B6 B6 105.0(9) . 4 ? B2 B6 B6 106.8(8) . 4 ? B10 B6 B1 107.4(8) . . ? B11 B6 B1 104.1(11) . . ? B2 B6 B1 55.9(10) . . ? B6 B6 B1 60.9(5) 4 . ? B10 B6 I6 123.4(11) . . ? B11 B6 I6 128.0(11) . . ? B2 B6 I6 120.4(9) . . ? B6 B6 I6 120.1(3) 4 . ? B1 B6 I6 119.2(11) . . ? C7 C7 B11 111.0(10) 4 . ? C7 C7 B3 63.2(5) 4 . ? B11 C7 B3 114.7(11) . . ? C7 C7 B2 111.7(7) 4 . ? B11 C7 B2 65.9(7) . . ? B3 C7 B2 59.9(9) . . ? C7 C7 H7 122(2) 4 . ? B11 C7 H7 116(3) . . ? B3 C7 H7 120(3) . . ? B2 C7 H7 118(2) . . ? B6 B10 B6 63.3(13) . 4 ? B6 B10 B11 108.3(14) . 4 ? B6 B10 B11 59.9(9) 4 4 ? B6 B10 B11 59.9(9) . . ? B6 B10 B11 108.3(14) 4 . ? B11 B10 B11 101.9(18) 4 . ? B6 B10 I10 121.1(11) . . ? B6 B10 I10 121.1(11) 4 . ? B11 B10 I10 124.1(10) 4 . ? B11 B10 I10 124.1(10) . . ? C7 B11 B6 108.3(13) . . ? C7 B11 B10 107.9(16) . . ? B6 B11 B10 59.6(11) . . ? C7 B11 B2 61.3(10) . . ? B6 B11 B2 60.8(10) . . ? B10 B11 B2 109.6(16) . . ? C7 B11 I11 119.9(11) . . ? B6 B11 I11 122.3(12) . . ? B10 B11 I11 124.1(11) . . ? B2 B11 I11 117.6(17) . . ? C14 N13 C15 117.0(13) . 4 ? C14 N13 C15 117.0(12) . . ? C15 N13 C15 107(2) 4 . ? C14 N13 H13 104.7 . . ? C15 N13 H13 104.7 4 . ? C15 N13 H13 104.7 . . ? N13 C14 H14A 109.5 . . ? N13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N13 C15 H15A 109.5 . . ? N13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 N16 C18 125(3) 4 . ? C18 N16 C17 107.1(19) 4 . ? C18 N16 C17 107.1(18) . . ? C18 N16 H16 105.5 4 . ? C18 N16 H16 105.5 . . ? C17 N16 H16 105.5 . . ? N16 C17 H17A 109.5 . . ? N16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N16 C18 H18A 109.5 . . ? N16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13 I1 0.93 2.89 3.706(19) 147.1 . N16 H16 I10 0.93 2.61 3.54(2) 179.1 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.809 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.176 #===END