Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email STIBR@IIC.CAS.CZ _publ_contact_author_name 'Prof Bohumil Stibr' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name B.Stibr I.Cisarova B.Gruner L.Mikulasek data_3-I-1 _database_code_CSD 198853 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H8 As2 B7 I' _chemical_formula_weight 384.49 _chemical_compound_source 'synthesized by the authors' 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' As As 0.0499 2.0058 '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 'P b a m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' _cell_length_a 10.0670(2) _cell_length_b 19.87000(10) _cell_length_c 9.9910(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1998.51(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19696 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description bar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 9.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.267 _exptl_absorpt_correction_T_max 0.503 _exptl_absorpt_process_details '(SORTAV; Blessing 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71070 _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 '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36133 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2413 _reflns_number_gt 2250 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0271P)^2^+2.9029P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00338(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2413 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0545 _refine_ls_wR_factor_gt 0.0533 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 B11 B 0.2352(4) 0.1842(2) 0.0000 0.0195(9) Uani 1 2 d S . . H11 H 0.2751 0.2357 0.0000 0.023 Uiso 1 2 calc SR . . B21 B 0.2428(3) 0.13465(16) 0.1478(3) 0.0188(6) Uani 1 1 d . . . H21 H 0.2837 0.1554 0.2412 0.023 Uiso 1 1 calc R . . B31 B 0.3488(4) 0.1166(2) 0.0000 0.0168(8) Uani 1 2 d S . . B61 B 0.0850(3) 0.16043(16) 0.0865(3) 0.0198(6) Uani 1 1 d . . . H61 H 0.0226 0.1970 0.1402 0.024 Uiso 1 1 calc R . . As71 As 0.28105(3) 0.028599(13) 0.12067(3) 0.01850(9) Uani 1 1 d . . . B101 B 0.0253(5) 0.0862(2) 0.0000 0.0198(9) Uani 1 2 d S . . H101 H -0.084(5) 0.074(2) 0.0000 0.026(12) Uiso 1 2 d S . . C111 C 0.1098(3) 0.07978(14) 0.1359(3) 0.0192(6) Uani 1 1 d . . . H111 H 0.070(3) 0.0696(17) 0.220(4) 0.026(9) Uiso 1 1 d . . . I1 I 0.56089(2) 0.138480(13) 0.0000 0.01942(9) Uani 1 2 d S . . B12 B 0.3701(5) 0.3671(2) 0.5000 0.0196(9) Uani 1 2 d S . . H12 H 0.4687 0.3909 0.5000 0.023 Uiso 1 2 calc SR . . B22 B 0.2725(3) 0.36771(16) 0.3533(3) 0.0183(6) Uani 1 1 d . . . H22 H 0.3108 0.3902 0.2604 0.022 Uiso 1 1 calc R . . B32 B 0.2277(4) 0.4197(2) 0.5000 0.0163(8) Uani 1 2 d S . . B62 B 0.3351(3) 0.28980(16) 0.4133(3) 0.0210(6) Uani 1 1 d . . . H62 H 0.4114 0.2609 0.3594 0.025 Uiso 1 1 calc R . . As72 As 0.06059(3) 0.379115(16) 0.37916(3) 0.01874(10) Uani 1 1 d . . . B102 B 0.1934(5) 0.2538(2) 0.5000 0.0225(10) Uani 1 2 d S . . H102 H 0.184(4) 0.203(2) 0.5000 0.018(11) Uiso 1 2 d S . . C112 C 0.1745(3) 0.29689(14) 0.3639(3) 0.0195(6) Uani 1 1 d . . . H12' H 0.160(3) 0.2761(17) 0.278(4) 0.025(9) Uiso 1 1 d . . . I2 I 0.25723(3) 0.528598(12) 0.5000 0.02063(9) Uani 1 2 d S . . 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 B11 0.019(2) 0.016(2) 0.024(2) 0.000 0.000 0.0020(17) B21 0.0186(16) 0.0200(16) 0.0179(15) -0.0030(12) 0.0013(12) 0.0014(12) B31 0.018(2) 0.015(2) 0.017(2) 0.000 0.000 -0.0031(16) B61 0.0173(14) 0.0200(15) 0.0220(16) -0.0025(12) 0.0001(12) 0.0014(12) As71 0.02235(18) 0.01641(16) 0.01675(16) 0.00251(10) 0.00012(10) 0.00047(11) B101 0.019(2) 0.018(2) 0.022(2) 0.000 0.000 -0.0025(17) C111 0.0189(14) 0.0202(14) 0.0186(14) 0.0010(10) 0.0016(11) -0.0019(11) I1 0.01628(15) 0.02202(15) 0.01996(15) 0.000 0.000 -0.00128(9) B12 0.017(2) 0.020(2) 0.022(2) 0.000 0.000 0.0007(17) B22 0.0153(15) 0.0225(16) 0.0172(15) -0.0013(12) 0.0025(12) -0.0009(12) B32 0.017(2) 0.017(2) 0.015(2) 0.000 0.000 -0.0026(16) B62 0.0149(15) 0.0200(14) 0.0279(17) -0.0036(13) 0.0024(12) 0.0024(12) As72 0.01556(17) 0.02196(16) 0.01870(16) -0.00144(10) -0.00341(10) 0.00133(10) B102 0.023(2) 0.015(2) 0.029(2) 0.000 0.000 -0.0014(18) C112 0.0179(14) 0.0192(13) 0.0214(14) -0.0033(11) -0.0019(11) -0.0011(11) I2 0.02714(16) 0.01565(14) 0.01910(15) 0.000 0.000 -0.00259(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B11 B31 1.765(6) . Y B11 B21 1.777(4) . Y B11 B21 1.777(4) 6 N B11 B61 1.804(5) . Y B11 B61 1.804(5) 6 ? B11 H11 1.1000 . ? B21 C111 1.730(4) . Y B21 B61 1.778(4) . Y B21 B31 1.857(4) . Y B21 As71 2.159(3) . Y B21 H21 1.1000 . ? B31 B21 1.857(4) 6 ? B31 I1 2.179(4) . Y B31 As71 2.230(3) 6 ? B31 As71 2.230(3) . Y B61 C111 1.695(4) . Y B61 B61 1.728(6) 6 ? B61 B101 1.813(5) . Y B61 H61 1.1000 . ? As71 C111 2.007(3) . Y As71 As71 2.4111(6) 6 ? B101 C111 1.608(4) 6 ? B101 C111 1.608(4) . Y B101 B61 1.813(5) 6 ? B101 H101 1.13(5) . ? C111 H111 0.95(4) . ? B12 B22 1.765(4) . Y B12 B22 1.765(4) 6_556 ? B12 B32 1.774(6) . Y B12 B62 1.798(5) . Y B12 B62 1.798(5) 6_556 ? B12 H12 1.1000 . ? B22 C112 1.722(4) . Y B22 B62 1.776(5) . Y B22 B32 1.849(4) . Y B22 As72 2.161(3) . Y B22 H22 1.1000 . ? B32 B22 1.849(4) 6_556 ? B32 I2 2.185(4) . Y B32 As72 2.222(4) . Y B32 As72 2.222(4) 6_556 ? B62 C112 1.696(4) . Y B62 B62 1.732(7) 6_556 ? B62 B102 1.816(5) . Y B62 H62 1.1000 . ? As72 C112 2.002(3) . Y As72 As72 2.4147(5) 6_556 ? B102 C112 1.618(4) . Y B102 C112 1.618(4) 6_556 ? B102 B62 1.816(5) 6_556 ? B102 H102 1.02(4) . ? C112 H12 0.96(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B31 B11 B21 63.25(17) . . ? B31 B11 B21 63.25(17) . 6 ? B21 B11 B21 112.5(3) . 6 ? B31 B11 B61 110.1(3) . . ? B21 B11 B61 59.52(17) . . ? B21 B11 B61 106.8(3) 6 . ? B31 B11 B61 110.1(3) . 6 ? B21 B11 B61 106.8(3) . 6 ? B21 B11 B61 59.52(17) 6 6 ? B61 B11 B61 57.2(2) . 6 ? B31 B11 H11 118.1 . . ? B21 B11 H11 120.0 . . ? B21 B11 H11 120.0 6 . ? B61 B11 H11 123.4 . . ? B61 B11 H11 123.4 6 . ? C111 B21 B11 105.0(2) . . N C111 B21 B61 57.78(17) . . N B11 B21 B61 61.0(2) . . ? C111 B21 B31 105.5(2) . . N B11 B21 B31 58.1(2) . . ? B61 B21 B31 107.2(2) . . ? C111 B21 As71 60.95(14) . . N B11 B21 As71 116.4(2) . . N B61 B21 As71 113.40(19) . . N B31 B21 As71 66.97(16) . . N C111 B21 H21 125.8 . . ? B11 B21 H21 120.9 . . ? B61 B21 H21 121.3 . . ? B31 B21 H21 122.1 . . ? As71 B21 H21 113.9 . . ? B11 B31 B21 58.69(17) . 6 ? B11 B31 B21 58.68(17) . . ? B21 B31 B21 105.4(3) 6 . ? B11 B31 I1 118.9(3) . . ? B21 B31 I1 121.63(16) 6 . ? B21 B31 I1 121.62(16) . . ? B11 B31 As71 113.5(2) . 6 N B21 B31 As71 63.00(13) 6 6 N B21 B31 As71 113.9(2) . 6 N I1 B31 As71 117.15(17) . 6 ? B11 B31 As71 113.5(2) . . N B21 B31 As71 113.9(2) 6 . ? B21 B31 As71 63.00(13) . . N I1 B31 As71 117.15(17) . . ? As71 B31 As71 65.44(12) 6 . N C111 B61 B61 106.94(14) . 6 N C111 B61 B21 59.71(17) . . N B61 B61 B21 110.17(15) 6 . ? C111 B61 B11 105.3(2) . . N B61 B61 B11 61.38(12) 6 . ? B21 B61 B11 59.48(18) . . ? C111 B61 B101 54.44(17) . . ? B61 B61 B101 61.53(12) 6 . ? B21 B61 B101 103.1(2) . . ? B11 B61 B101 105.2(2) . . ? C111 B61 H61 124.5 . . ? B61 B61 H61 119.2 6 . ? B21 B61 H61 122.2 . . ? B11 B61 H61 122.7 . . ? B101 B61 H61 125.4 . . ? C111 As71 B21 48.91(12) . . Y C111 As71 B31 84.64(14) . . Y B21 As71 B31 50.03(12) . . Y C111 As71 As71 94.36(8) . 6 Y B21 As71 As71 97.22(9) . 6 Y B31 As71 As71 57.28(6) . 6 Y C111 B101 C111 115.3(3) 6 . Y C111 B101 B61 106.9(3) 6 . Y C111 B101 B61 59.06(18) . . Y C111 B101 B61 59.06(18) 6 6 N C111 B101 B61 106.9(3) . 6 Y B61 B101 B61 56.9(2) . 6 Y C111 B101 H101 120.0(6) 6 . ? C111 B101 H101 120.0(6) . . ? B61 B101 H101 120(2) . . ? B61 B101 H101 120(2) 6 . ? B101 C111 B61 66.5(2) . . Y B101 C111 B21 114.7(3) . . Y B61 C111 B21 62.51(18) . . Y B101 C111 As71 115.5(2) . . Y B61 C111 As71 125.68(19) . . Y B21 C111 As71 70.14(15) . . Y B101 C111 H111 122(2) . . ? B61 C111 H111 113(2) . . ? B21 C111 H111 114(2) . . ? As71 C111 H111 109(2) . . ? B22 B12 B22 112.3(3) . 6_556 ? B22 B12 B32 62.98(17) . . ? B22 B12 B32 62.98(17) 6_556 . ? B22 B12 B62 59.79(17) . . ? B22 B12 B62 107.3(3) 6_556 . ? B32 B12 B62 110.1(3) . . ? B22 B12 B62 107.3(3) . 6_556 ? B22 B12 B62 59.79(17) 6_556 6_556 ? B32 B12 B62 110.1(3) . 6_556 ? B62 B12 B62 57.6(3) . 6_556 ? B22 B12 H12 120.0 . . ? B22 B12 H12 120.0 6_556 . ? B32 B12 H12 118.4 . . ? B62 B12 H12 123.0 . . ? B62 B12 H12 123.0 6_556 . ? C112 B22 B12 105.2(2) . . ? C112 B22 B62 57.99(17) . . ? B12 B22 B62 61.0(2) . . ? C112 B22 B32 105.5(2) . . ? B12 B22 B32 58.7(2) . . ? B62 B22 B32 107.8(2) . . ? C112 B22 As72 60.85(13) . . ? B12 B22 As72 116.8(2) . . ? B62 B22 As72 113.66(19) . . ? B32 B22 As72 66.78(16) . . ? C112 B22 H22 125.8 . . ? B12 B22 H22 120.5 . . ? B62 B22 H22 121.0 . . ? B32 B22 H22 121.8 . . ? As72 B22 H22 113.9 . . ? B12 B32 B22 58.27(17) . . ? B12 B32 B22 58.27(17) . 6_556 ? B22 B32 B22 104.9(3) . 6_556 ? B12 B32 I2 118.3(3) . . ? B22 B32 I2 121.32(16) . . ? B22 B32 I2 121.32(16) 6_556 . ? B12 B32 As72 113.5(2) . . ? B22 B32 As72 63.34(13) . . ? B22 B32 As72 114.4(2) 6_556 . ? I2 B32 As72 117.53(17) . . ? B12 B32 As72 113.5(2) . 6_556 ? B22 B32 As72 114.4(2) . 6_556 ? B22 B32 As72 63.34(13) 6_556 6_556 ? I2 B32 As72 117.53(17) . 6_556 ? As72 B32 As72 65.83(12) . 6_556 ? C112 B62 B62 106.94(15) . 6_556 ? C112 B62 B22 59.41(17) . . ? B62 B62 B22 109.76(15) 6_556 . ? C112 B62 B12 104.9(2) . . ? B62 B62 B12 61.20(13) 6_556 . ? B22 B62 B12 59.20(18) . . ? C112 B62 B102 54.75(17) . . ? B62 B62 B102 61.51(13) 6_556 . ? B22 B62 B102 103.0(2) . . ? B12 B62 B102 105.1(2) . . ? C112 B62 H62 124.5 . . ? B62 B62 H62 119.3 6_556 . ? B22 B62 H62 122.5 . . ? B12 B62 H62 122.9 . . ? B102 B62 H62 125.3 . . ? C112 As72 B22 48.68(12) . . Y C112 As72 B32 84.47(14) . . Y B22 As72 B32 49.88(12) . . Y C112 As72 As72 94.37(8) . 6_556 Y B22 As72 As72 96.88(9) . 6_556 Y B32 As72 As72 57.09(6) . 6_556 Y C112 B102 C112 114.4(3) . 6_556 Y C112 B102 B62 106.5(3) . 6_556 Y C112 B102 B62 58.86(18) 6_556 6_556 ? C112 B102 B62 58.86(18) . . Y C112 B102 B62 106.5(3) 6_556 . ? B62 B102 B62 57.0(3) 6_556 . Y C112 B102 H102 121.1(5) . . ? C112 B102 H102 121.1(5) 6_556 . ? B62 B102 H102 118(2) 6_556 . ? B62 B102 H102 118(2) . . ? B102 C112 B62 66.4(2) . . Y B102 C112 B22 114.6(3) . . Y B62 C112 B22 62.61(18) . . Y B102 C112 As72 115.8(2) . . Y B62 C112 As72 126.26(18) . . Y B22 C112 As72 70.47(14) . . Y B102 C112 H12 123(2) . . ? B62 C112 H12 112(2) . . ? B22 C112 H12 112(2) . . ? As72 C112 H12 109(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.684 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.122