Supplementary data for Dalton Trans. This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Barbara Albert' _publ_contact_author_email ALBERT@AC.CHEMIE.TU-DARMSTADT.DE _publ_section_title ; Multi-centre, hydrogen, and dihydrogen bonds in lithium closo-hydroborate obtained from liquid ammonia ; _publ_author_address ; Eduard-Zintl-Institute f\"ur Anorganische und Physikalische Chemie, TU Darmstadt, Petersenstrasse 18, D-64287 Darmstadt ; _publ_contact_author_address ; Eduard-Zintl-Institute f\"ur Anorganische und Physikalische Chemie, TU Darmstadt, Petersenstrasse 18, D-64287 Darmstadt ; loop_ _publ_author_name 'Barbara Albert' 'Kathrin Hofmann' 'Monalisa Panda' 'Marc Prosenc' # Attachment '[Li_NH3_42B6H6.CIF' data_[Li(NH3)4]2B6H6*2NH3 _database_code_depnum_ccdc_archive 'CCDC 683416' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'B6 H6, 10(H3 N), 2(Li)' _chemical_formula_sum 'B6 H36 Li2 N10' _chemical_formula_weight 255.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.483(1) _cell_length_b 11.871(2) _cell_length_c 10.605(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.371(3) _cell_angle_gamma 90.00 _cell_volume 937.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7580 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 44.83 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 284 _exptl_absorpt_coefficient_mu 0.056 _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 123(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 'CCD area detector' _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 65525 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0969 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 44.83 _reflns_number_total 7580 _reflns_number_gt 3016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0522P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7580 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1431 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1130 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 0.783 _refine_ls_restrained_S_all 0.783 _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 N1 N 0.72772(6) 0.28503(4) -0.19922(5) 0.02911(10) Uani 1 1 d . . . N2 N 0.25250(6) 0.29167(4) -0.21025(5) 0.02785(10) Uani 1 1 d . . . N3 N 0.49377(6) 0.33816(4) -0.46644(4) 0.02392(9) Uani 1 1 d . . . N5 N 0.87047(8) 0.07009(7) -0.41071(6) 0.04483(14) Uani 1 1 d . . . N4 N 0.44835(8) 0.07760(4) -0.34368(6) 0.03402(11) Uani 1 1 d . . . B6 B -0.09434(6) 0.50465(4) -0.41206(4) 0.02111(9) Uani 1 1 d . . . B7 B 0.01137(7) 0.39787(4) -0.48728(5) 0.02079(9) Uani 1 1 d . . . B8 B 0.13340(6) 0.51230(4) -0.42564(4) 0.01915(9) Uani 1 1 d . . . Li Li 0.48030(11) 0.24936(8) -0.30176(8) 0.02618(17) Uani 1 1 d . . . H8A H 0.2525(10) 0.5220(6) -0.3593(7) 0.0276(15) Uiso 1 1 d . . . H6A H -0.1784(11) 0.5093(6) -0.3327(8) 0.0346(17) Uiso 1 1 d . . . H2C H 0.1820(12) 0.3198(8) -0.2708(9) 0.042(2) Uiso 1 1 d . . . H1C H 0.7939(14) 0.3173(9) -0.2515(10) 0.047(2) Uiso 1 1 d . . . H2B H 0.1935(13) 0.2336(8) -0.1836(9) 0.045(2) Uiso 1 1 d . . . H7A H 0.0258(11) 0.3070(7) -0.4765(8) 0.0391(19) Uiso 1 1 d . . . H1B H 0.7887(13) 0.2274(8) -0.1668(9) 0.045(2) Uiso 1 1 d . . . H1A H 0.7310(14) 0.3346(10) -0.1371(11) 0.057(3) Uiso 1 1 d . . . H3C H 0.5850(13) 0.3803(8) -0.4658(8) 0.041(2) Uiso 1 1 d . . . H3B H 0.4866(12) 0.2993(8) -0.5380(9) 0.042(2) Uiso 1 1 d . . . H2A H 0.2539(15) 0.3420(9) -0.1514(11) 0.057(3) Uiso 1 1 d . . . H3A H 0.4020(12) 0.3822(8) -0.4763(8) 0.0390(19) Uiso 1 1 d . . . H4C H 0.3713(13) 0.0547(8) -0.4048(9) 0.047(2) Uiso 1 1 d . . . H5C H 0.9075(15) 0.0504(10) -0.3334(12) 0.061(3) Uiso 1 1 d . . . H4B H 0.4380(19) 0.0446(13) -0.2805(15) 0.081(4) Uiso 1 1 d . . . H5B H 0.911(2) 0.1320(16) -0.4200(16) 0.095(5) Uiso 1 1 d . . . H4A H 0.553(2) 0.0478(11) -0.3761(12) 0.079(3) Uiso 1 1 d . . . H5A H 0.952(3) 0.039(2) -0.455(2) 0.127(6) 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 N1 0.0288(2) 0.0247(2) 0.0324(2) 0.00520(17) -0.00487(17) 0.00107(16) N2 0.02561(19) 0.0318(2) 0.0262(2) 0.00780(17) 0.00271(16) 0.00329(16) N3 0.02211(18) 0.02707(19) 0.02265(18) 0.00134(15) 0.00256(14) -0.00185(15) N5 0.0392(3) 0.0651(4) 0.0308(3) 0.0086(2) 0.0067(2) -0.0062(3) N4 0.0383(3) 0.0279(2) 0.0350(2) 0.00192(19) -0.0009(2) -0.00125(18) B6 0.0210(2) 0.0247(2) 0.01792(19) -0.00136(16) 0.00338(16) -0.00270(16) B7 0.0252(2) 0.01580(19) 0.0208(2) 0.00016(15) -0.00105(17) -0.00206(16) B8 0.01999(19) 0.01891(19) 0.01819(19) -0.00045(15) -0.00006(15) -0.00201(15) Li 0.0252(4) 0.0274(4) 0.0261(4) 0.0044(3) 0.0032(3) -0.0002(3) _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 N1 Li 2.1007(10) . ? N2 Li 2.0999(10) . ? N3 Li 2.0504(10) . ? N4 Li 2.0957(11) . ? B6 B8 1.7261(7) . ? B6 B7 1.7286(7) 3_564 ? B6 B7 1.7282(7) . ? B6 B8 1.7303(7) 3_564 ? B7 B8 1.7251(7) 3_564 ? B7 B6 1.7286(7) 3_564 ? B7 B8 1.7306(7) . ? B8 B7 1.7251(7) 3_564 ? B8 B6 1.7303(7) 3_564 ? 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 B8 B6 B7 59.91(3) . 3_564 ? B8 B6 B7 60.13(3) . . ? B7 B6 B7 89.98(3) 3_564 . ? B8 B6 B8 89.96(3) . 3_564 ? B7 B6 B8 60.04(3) 3_564 3_564 ? B7 B6 B8 59.84(3) . 3_564 ? B8 B7 B6 59.97(3) 3_564 3_564 ? B8 B7 B6 60.14(3) 3_564 . ? B6 B7 B6 90.02(3) 3_564 . ? B8 B7 B8 89.99(3) 3_564 . ? B6 B7 B8 60.03(3) 3_564 . ? B6 B7 B8 59.87(3) . . ? B7 B8 B6 60.12(3) 3_564 . ? B7 B8 B6 60.02(3) 3_564 3_564 ? B6 B8 B6 90.04(3) . 3_564 ? B7 B8 B7 90.01(3) 3_564 . ? B6 B8 B7 60.00(3) . . ? B6 B8 B7 59.93(3) 3_564 . ? N3 Li N4 109.47(5) . . ? N3 Li N2 112.17(4) . . ? N4 Li N2 104.44(4) . . ? N3 Li N1 103.06(4) . . ? N4 Li N1 112.55(4) . . ? N2 Li N1 115.27(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 44.83 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.241 _refine_diff_density_min -0.110 _refine_diff_density_rms 0.041