Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_p2b10h9c8 _database_code_CSD 173484 data_global _audit_creation_date 'Jule 25, 2000' _audit_creation_method 'SHELXL97 and manual editing' _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Gruner, Bohumir' ; Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 250 68 Rez u Prahy Czech Republic ; 'Hnyk, Drahomir' ; Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 250 68 Rez u Prahy Czech Republic ; 'Cisarova, Ivana' ; Charles University Faculty of Science Hlavova 2030 128 40 Praha 2 Czech Republic ; 'Plzak, Zbynek' ; Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 250 68 Rez u Prahy Czech Republic ; 'Stibr, Bohumil' ; Institute of Inorganic Chemistry Academy of Sciences of the Czech Republic 250 68 Rez u Prahy Czech Republic ; _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Dr Bohumir Gruner' _publ_contact_author_address ; Syntheses Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic Institute of Inorganic Chemistry AS Rez near Prague Czech Republic 250 68 CZECH REPUBLIC ; _publ_contact_author_email 'gruner@iic.cas.cz' _publ_contact_author_fax '420 2 20 94 15 02' _publ_contact_author_phone '(420 2)6617 3104' #TITLE AND AUTHOR LIST _publ_section_title ; Phosphaborane chemistry. syntheses and molecular structures of mono-and dichloro derivatives of 1,2-diphospha-closo-dodecaborane(10), 1,2-closo-P2B10H10, determined byquantum chemical calculations of various quantities. Crystal structure of 3,6-Cl2-closo-1,2-P2B10H8 and verification of the structures of 1,2-closo-P2B10H10 and 1,7-closo-P2B10H10 by NMR shifts calculations ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,6-dichloro-closo-1,2-diphosphadodecaborane(12) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H8 B10 Cl2 P2' _chemical_formula_weight 249.00 _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 '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' 'P' 'P' 0.1023 0.0942 '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 'orthorhombic' _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.2830(5) _cell_length_b 12.3110(3) _cell_length_c 13.7860(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2254.38(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9129 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 '\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 16748 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2566 _reflns_number_gt 2030 _reflns_threshold_expression >2sigma(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^)+(0.0608P)^2^+1.9683P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2566 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P -0.35370(6) 0.82394(6) 0.20412(5) 0.0449(2) Uani 1 1 d . . . P2 P -0.45287(5) 0.67150(6) 0.20848(5) 0.0436(2) Uani 1 1 d . . . Cl3 Cl -0.21589(6) 0.60517(7) 0.22862(7) 0.0658(3) Uani 1 1 d . . . Cl6 Cl -0.59176(7) 0.88997(8) 0.19112(7) 0.0747(3) Uani 1 1 d . . . B3 B -0.3052(2) 0.6719(2) 0.1527(2) 0.0410(6) Uani 1 1 d . . . B4 B -0.2761(2) 0.7933(3) 0.0816(2) 0.0487(7) Uani 1 1 d . . . B5 B -0.3894(3) 0.8793(3) 0.0690(3) 0.0501(8) Uani 1 1 d . . . B6 B -0.4951(2) 0.8134(3) 0.1340(2) 0.0452(7) Uani 1 1 d . . . B7 B -0.4028(2) 0.5978(3) 0.0868(2) 0.0437(7) Uani 1 1 d . . . B8 B -0.3037(3) 0.6661(3) 0.0254(2) 0.0506(8) Uani 1 1 d . . . B9 B -0.3526(3) 0.7879(3) -0.0245(3) 0.0534(8) Uani 1 1 d . . . B10 B -0.4817(3) 0.7991(3) 0.0067(2) 0.0489(7) Uani 1 1 d . . . B11 B -0.5168(2) 0.6815(3) 0.0757(2) 0.0425(7) Uani 1 1 d . . . B12 B -0.4288(3) 0.6704(3) -0.0213(2) 0.0483(7) Uani 1 1 d . . . H4 H -0.207(3) 0.821(3) 0.084(2) 0.062(10) Uiso 1 1 d . . . H5 H -0.386(2) 0.948(3) 0.067(2) 0.051(9) Uiso 1 1 d . . . H7 H -0.407(2) 0.514(3) 0.095(3) 0.073(10) Uiso 1 1 d . . . H8 H -0.247(3) 0.621(3) -0.004(3) 0.075(11) Uiso 1 1 d . . . H9 H -0.324(3) 0.816(3) -0.090(3) 0.088(12) Uiso 1 1 d . . . H10 H -0.528(2) 0.836(2) -0.037(3) 0.061(9) Uiso 1 1 d . . . H11 H -0.585(2) 0.648(2) 0.075(2) 0.056(9) Uiso 1 1 d . . . H12 H -0.450(2) 0.625(2) -0.089(2) 0.056(9) 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 P1 0.0479(4) 0.0462(4) 0.0408(4) -0.0078(3) -0.0036(3) -0.0039(3) P2 0.0410(4) 0.0515(4) 0.0382(4) 0.0025(3) 0.0041(3) -0.0033(3) Cl3 0.0556(5) 0.0770(5) 0.0647(5) -0.0069(4) -0.0104(4) 0.0188(4) Cl6 0.0636(5) 0.0826(6) 0.0780(6) -0.0186(5) 0.0003(4) 0.0289(4) B3 0.0334(14) 0.0482(16) 0.0414(15) -0.0046(12) -0.0006(12) 0.0025(11) B4 0.0396(17) 0.0633(19) 0.0433(16) -0.0016(14) 0.0044(13) -0.0127(14) B5 0.061(2) 0.0438(18) 0.0453(18) 0.0044(14) -0.0069(15) -0.0076(14) B6 0.0419(16) 0.0509(17) 0.0428(17) -0.0035(13) -0.0034(13) 0.0057(13) B7 0.0472(17) 0.0410(16) 0.0429(17) -0.0071(12) 0.0006(13) -0.0041(12) B8 0.0446(17) 0.066(2) 0.0407(17) -0.0108(15) 0.0081(14) 0.0001(15) B9 0.058(2) 0.066(2) 0.0365(16) 0.0056(15) 0.0017(14) -0.0163(16) B10 0.0497(18) 0.0577(18) 0.0392(16) 0.0051(14) -0.0061(14) -0.0032(15) B11 0.0382(16) 0.0521(17) 0.0373(15) -0.0019(12) -0.0020(12) -0.0051(12) B12 0.0513(18) 0.0586(19) 0.0350(15) -0.0064(13) -0.0001(13) -0.0118(14) _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 P1 B4 2.014(3) . Y P1 B5 2.039(4) . Y P1 B3 2.102(3) . Y P1 B6 2.117(3) . Y P1 P2 2.2936(10) . Y P2 B7 2.020(3) . Y P2 B11 2.022(3) . Y P2 B6 2.103(3) . Y P2 B3 2.106(3) . Y Cl3 B3 1.782(3) . Y Cl6 B6 1.777(3) . Y B3 B8 1.757(5) . Y B3 B7 1.827(4) . Y B3 B4 1.829(5) . Y B4 B9 1.782(5) . Y B4 B8 1.785(5) . Y B4 B5 1.848(5) . Y B4 H4 0.98(3) . ? B5 B9 1.780(5) . Y B5 B10 1.793(5) . Y B5 B6 1.852(5) . Y B5 H5 0.85(3) . ? B6 B10 1.772(5) . Y B6 B11 1.835(4) . Y B7 B12 1.772(5) . Y B7 B8 1.776(5) . Y B7 B11 1.838(5) . Y B7 H7 1.04(4) . ? B8 B9 1.773(6) . Y B8 B12 1.782(5) . Y B8 H8 1.02(4) . ? B9 B12 1.766(5) . Y B9 B10 1.773(5) . Y B9 H9 1.03(4) . ? B10 B12 1.776(5) . Y B10 B11 1.794(5) . Y B10 H10 0.97(3) . ? B11 B12 1.782(5) . Y B11 H11 1.00(3) . ? B12 H12 1.12(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 B4 P1 B5 54.24(15) . . Y B4 P1 B3 52.70(14) . . Y B5 P1 B3 93.50(14) . . Y B4 P1 B6 93.40(13) . . Y B5 P1 B6 52.89(14) . . Y B3 P1 B6 93.64(12) . . Y B4 P1 P2 99.35(10) . . Y B5 P1 P2 99.43(10) . . Y B3 P1 P2 57.06(9) . . Y B6 P1 P2 56.80(9) . . Y B7 P2 B11 54.09(13) . . Y B7 P2 B6 93.17(13) . . Y B11 P2 B6 52.79(12) . . Y B7 P2 B3 52.53(12) . . Y B11 P2 B3 93.48(13) . . Y B6 P2 B3 93.91(12) . . Y B7 P2 P1 99.02(9) . . Y B11 P2 P1 99.67(10) . . Y B6 P2 P1 57.36(9) . . Y B3 P2 P1 56.89(8) . . Y B8 B3 Cl3 124.1(2) . . ? B8 B3 B7 59.38(18) . . ? Cl3 B3 B7 122.3(2) . . ? B8 B3 B4 59.69(19) . . ? Cl3 B3 B4 123.4(2) . . ? B7 B3 B4 106.9(2) . . ? B8 B3 P1 112.1(2) . . ? Cl3 B3 P1 114.61(15) . . ? B7 B3 P1 113.25(17) . . ? B4 B3 P1 61.16(14) . . ? B8 B3 P2 112.02(19) . . ? Cl3 B3 P2 113.87(16) . . ? B7 B3 P2 61.30(13) . . ? B4 B3 P2 113.21(18) . . ? P1 B3 P2 66.05(9) . . ? B9 B4 B8 59.6(2) . . ? B9 B4 B3 106.8(2) . . ? B8 B4 B3 58.15(18) . . Y B9 B4 B5 58.7(2) . . ? B8 B4 B5 107.1(2) . . ? B3 B4 B5 110.3(2) . . ? B9 B4 P1 113.8(2) . . ? B8 B4 P1 115.0(2) . . Y B3 B4 P1 66.14(14) . . ? B5 B4 P1 63.57(16) . . ? B9 B4 H4 125(2) . . ? B8 B4 H4 120.4(19) . . ? B3 B4 H4 117.7(19) . . ? B5 B4 H4 124.7(19) . . ? P1 B4 H4 113(2) . . ? B9 B5 B10 59.5(2) . . ? B9 B5 B4 58.8(2) . . ? B10 B5 B4 106.6(2) . . ? B9 B5 B6 106.4(2) . . ? B10 B5 B6 58.14(18) . . ? B4 B5 B6 108.7(2) . . ? B9 B5 P1 112.8(2) . . ? B10 B5 P1 114.4(2) . . ? B4 B5 P1 62.18(15) . . ? B6 B5 P1 65.72(15) . . ? B9 B5 H5 126(2) . . ? B10 B5 H5 125(2) . . ? B4 B5 H5 122(2) . . ? B6 B5 H5 120(2) . . ? P1 B5 H5 111(2) . . ? B10 B6 Cl6 124.4(2) . . ? B10 B6 B11 59.63(18) . . ? Cl6 B6 B11 123.4(2) . . ? B10 B6 B5 59.26(19) . . ? Cl6 B6 B5 122.0(2) . . ? B11 B6 B5 107.2(2) . . ? B10 B6 P2 112.0(2) . . ? Cl6 B6 P2 114.62(17) . . ? B11 B6 P2 61.33(14) . . ? B5 B6 P2 113.41(19) . . ? B10 B6 P1 111.7(2) . . Y Cl6 B6 P1 113.96(16) . . ? B11 B6 P1 113.17(18) . . ? B5 B6 P1 61.39(14) . . ? P2 B6 P1 65.84(10) . . ? B12 B7 B8 60.30(19) . . ? B12 B7 B3 107.7(2) . . ? B8 B7 B3 58.33(17) . . ? B12 B7 B11 59.12(18) . . ? B8 B7 B11 107.8(2) . . ? B3 B7 B11 110.3(2) . . ? B12 B7 P2 114.1(2) . . ? B8 B7 P2 115.27(19) . . Y B3 B7 P2 66.18(14) . . ? B11 B7 P2 63.02(14) . . ? B12 B7 H7 126(2) . . ? B8 B7 H7 124.0(19) . . ? B3 B7 H7 118.2(19) . . ? B11 B7 H7 121.7(19) . . ? P2 B7 H7 110(2) . . ? B3 B8 B9 110.5(2) . . ? B3 B8 B7 62.29(18) . . ? B9 B8 B7 108.3(2) . . ? B3 B8 B12 110.5(2) . . ? B9 B8 B12 59.55(19) . . ? B7 B8 B12 59.73(19) . . ? B3 B8 B4 62.16(19) . . ? B9 B8 B4 60.1(2) . . ? B7 B8 B4 111.1(2) . . Y B12 B8 B4 108.8(2) . . ? B3 B8 H8 116(2) . . ? B9 B8 H8 125(2) . . ? B7 B8 H8 119(2) . . ? B12 B8 H8 124(2) . . ? B4 B8 H8 120(2) . . ? B12 B9 B10 60.2(2) . . ? B12 B9 B8 60.5(2) . . ? B10 B9 B8 109.0(2) . . ? B12 B9 B5 110.0(2) . . ? B10 B9 B5 60.6(2) . . ? B8 B9 B5 110.7(2) . . ? B12 B9 B4 109.7(2) . . ? B10 B9 B4 110.4(2) . . ? B8 B9 B4 60.3(2) . . ? B5 B9 B4 62.5(2) . . Y B12 B9 H9 120(2) . . ? B10 B9 H9 123(2) . . ? B8 B9 H9 119(2) . . ? B5 B9 H9 121(2) . . ? B4 B9 H9 119(2) . . ? B6 B10 B9 110.2(2) . . Y B6 B10 B12 110.1(2) . . ? B9 B10 B12 59.7(2) . . ? B6 B10 B5 62.6(2) . . ? B9 B10 B5 59.9(2) . . ? B12 B10 B5 109.0(2) . . ? B6 B10 B11 61.95(18) . . ? B9 B10 B11 108.5(2) . . ? B12 B10 B11 59.88(19) . . ? B5 B10 B11 111.6(2) . . ? B6 B10 H10 120(2) . . ? B9 B10 H10 120(2) . . ? B12 B10 H10 122(2) . . ? B5 B10 H10 118.2(19) . . ? B11 B10 H10 122.7(19) . . ? B12 B11 B10 59.55(19) . . Y B12 B11 B6 107.0(2) . . ? B10 B11 B6 58.42(18) . . ? B12 B11 B7 58.60(18) . . ? B10 B11 B7 106.4(2) . . ? B6 B11 B7 109.3(2) . . ? B12 B11 P2 113.52(19) . . ? B10 B11 P2 114.78(19) . . ? B6 B11 P2 65.88(14) . . ? B7 B11 P2 62.88(14) . . ? B12 B11 H11 124.2(19) . . ? B10 B11 H11 124.5(19) . . ? B6 B11 H11 120.7(18) . . ? B7 B11 H11 121.4(18) . . ? P2 B11 H11 111.3(19) . . ? B9 B12 B7 108.8(2) . . ? B9 B12 B10 60.1(2) . . ? B7 B12 B10 110.1(2) . . ? B9 B12 B11 109.4(2) . . ? B7 B12 B11 62.28(18) . . ? B10 B12 B11 60.57(19) . . ? B9 B12 B8 60.0(2) . . ? B7 B12 B8 59.97(19) . . ? B10 B12 B8 108.5(2) . . ? B11 B12 B8 110.0(2) . . ? B9 B12 H12 122.0(16) . . ? B7 B12 H12 119.9(16) . . ? B10 B12 H12 121.6(16) . . ? B11 B12 H12 119.7(16) . . ? B8 B12 H12 121.4(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.353 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.062