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 D.Rankin F.Blockhuys A.R.Cowley A.Downs Hans-Jorg Himmel H.E.Robertson C.Y.Tang 'Van Alsenoy, C.' D.A.Wann _publ_contact_author_name 'David Rankin' _publ_contact_author_address ; School of Chemistry University of Edinburgh West Mains Road Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_email D.W.H.RANKIN@ED.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; adducts with metal trihydrides, MH3 (M = B, Al or Ga), studied by gas-phase electron diffraction, X-ray diffraction and quantum chemical calculations ; data_arc1344 _database_code_depnum_ccdc_archive 'CCDC 635246' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _chemical_absolute_configuration unk _exptl_crystal_thermal_history ; The material was crystallised at ambient temperature. A suitable crystal was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. ; _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #============================================================= _cell_length_a 9.2919(4) _cell_angle_alpha 90 _cell_length_b 9.2919(4) _cell_angle_beta 90 _cell_length_c 9.2919(4) _cell_angle_gamma 90 _cell_volume 802.26(6) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P 21 3 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z y,z,x z,x,y x+1/2,-y+1/2,-z y+1/2,-z+1/2,-x z+1/2,-x+1/2,-y -y,z+1/2,-x+1/2 -z,x+1/2,-y+1/2 -z+1/2,-x,y+1/2 -x+1/2,-y,z+1/2 -y+1/2,-z,x+1/2 -x,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C7 H16 B N ' _chemical_formula_moiety ' C7 H16 B N ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 125.02 _cell_measurement_reflns_used 2063 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' octahedron ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.035 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 0.058 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.99 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 2063 _reflns_number_total 354 #360 unqiue reflections including absences _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_theta_min 5.375 _diffrn_reflns_theta_max 27.421 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.421 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _reflns_limit_h_min 0 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 8 _reflns_limit_l_min 2 _reflns_limit_l_max 12 _refine_diff_density_min -0.10 _refine_diff_density_max 0.10 _refine_ls_number_reflns 274 _refine_ls_number_restraints 0 _refine_ls_number_parameters 32 #_refine_ls_R_factor_ref 0.0333 _refine_ls_wR_factor_ref 0.0354 _refine_ls_goodness_of_fit_ref 1.1445 #_reflns_number_all 355 _refine_ls_R_factor_all 0.0475 _refine_ls_wR_factor_all 0.0471 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 274 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_gt 0.0354 _refine_ls_shift/su_max 0.002192 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.330 0.031 0.112 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp B1 B 0.5879(2) 0.0879(2) 0.4121(2) 0.0420 1.0000 Uani S T N1 N 0.68782(14) 0.18782(14) 0.31218(14) 0.0256 1.0000 Uani S T C1 C 0.67891(19) 0.34236(19) 0.35833(18) 0.0323 1.0000 Uani . . C2 C 0.7903(2) 0.43414(18) 0.2794(2) 0.0360 1.0000 Uani . . C3 C 0.84827(19) 0.34827(19) 0.15173(19) 0.0340 1.0000 Uani S T H1 H 0.597(3) -0.025(3) 0.362(2) 0.058(7) 1.0000 Uiso . . H11 H 0.6969 0.3485 0.4643 0.0388 1.0000 Uiso . . H12 H 0.5805 0.3800 0.3365 0.0388 1.0000 Uiso . . H21 H 0.8710 0.4586 0.3462 0.0432 1.0000 Uiso . . H22 H 0.7442 0.5248 0.2441 0.0432 1.0000 Uiso . . H31 H 0.9104 0.4104 0.0896 0.0408 1.0000 Uiso . . 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 0.0420(10) 0.0420(10) 0.0420(10) 0.0084(10) 0.0084(10) -0.0084(10) N1 0.0256(5) 0.0256(5) 0.0256(5) -0.0023(6) -0.0023(6) 0.0023(6) C1 0.0366(9) 0.0288(9) 0.0315(9) -0.0049(7) 0.0032(7) 0.0039(8) C2 0.0420(11) 0.0257(9) 0.0402(10) -0.0022(7) -0.0025(9) -0.0016(8) C3 0.0340(7) 0.0340(7) 0.0340(7) 0.0034(8) 0.0034(8) -0.0034(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag B1 . N1 . 1.608(5) yes B1 . H1 . 1.15(2) no B1 . H1 5_556 1.15(2) no B1 . H1 8_645 1.15(2) no N1 . C1 . 1.5009(18) yes N1 . C1 5_556 1.5009(18) yes N1 . C1 8_645 1.5009(18) yes C1 . C2 . 1.529(2) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C3 . 1.528(2) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . H31 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . B1 . H1 . 104.5(12) no N1 . B1 . H1 5_556 104.5(12) no H1 . B1 . H1 5_556 114.0(10) no N1 . B1 . H1 8_645 104.5(12) no H1 . B1 . H1 8_645 114.0(10) no H1 5_556 B1 . H1 8_645 114.0(10) no B1 . N1 . C1 . 110.83(11) yes B1 . N1 . C1 5_556 110.83(11) yes C1 . N1 . C1 5_556 108.08(11) yes B1 . N1 . C1 8_645 110.83(11) yes C1 . N1 . C1 8_645 108.08(11) yes C1 5_556 N1 . C1 8_645 108.08(11) yes N1 . C1 . C2 . 111.06(15) yes N1 . C1 . H11 . 109.074 no C2 . C1 . H11 . 109.074 no N1 . C1 . H12 . 109.075 no C2 . C1 . H12 . 109.075 no H11 . C1 . H12 . 109.467 no C1 . C2 . C3 . 108.66(16) yes C1 . C2 . H21 . 109.675 no C3 . C2 . H21 . 109.675 no C1 . C2 . H22 . 109.675 no C3 . C2 . H22 . 109.675 no H21 . C2 . H22 . 109.467 no C2 . C3 . C2 5_556 108.42(13) yes C2 . C3 . C2 8_645 108.42(13) yes C2 5_556 C3 . C2 8_645 108.42(13) yes C2 . C3 . H31 . 110.506 no C2 5_556 C3 . H31 . 110.506 no C2 8_645 C3 . H31 . 110.506 no