# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2292 data_me2gb2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2 H10 B Ga' _chemical_formula_weight 114.63 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 6.4050(8) _cell_length_b 7.4178(11) _cell_length_c 11.8428(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 562.66(13) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cylinder _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method ? _exptl_crystal_F_000 232 _exptl_absorpt_coefficient_mu 5.273 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.115 _exptl_absorpt_correction_T_max 0.208 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method omega-theta _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2931 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 7.04 _diffrn_reflns_theta_max 60.11 _reflns_number_total 527 _reflns_number_observed 522 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0137P)^2^+0.2273P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0618(25) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.27(13) _refine_ls_number_reflns 525 _refine_ls_number_parameters 58 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_obs 0.0234 _refine_ls_wR_factor_all 0.0589 _refine_ls_wR_factor_obs 0.0532 _refine_ls_goodness_of_fit_all 1.208 _refine_ls_goodness_of_fit_obs 1.210 _refine_ls_restrained_S_all 1.331 _refine_ls_restrained_S_obs 1.210 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.86984(8) 0.57279(6) 0.11975(5) 0.0584(3) Uani 1 d . . B1 B 1.0255(10) 0.8473(7) 0.1268(5) 0.0600(13) Uani 1 d . . H1 H 0.9366(75) 0.7987(63) 0.0508(37) 0.070(13) Uiso 1 d . . H2 H 1.0515(71) 0.7435(67) 0.1847(36) 0.067(13) Uiso 1 d . . H3 H 0.9566(74) 0.9613(65) 0.1731(37) 0.067(13) Uiso 1 d . . H4 H 1.1762(87) 0.8793(75) 0.0840(43) 0.093(17) Uiso 1 d . . C1 C 1.0405(8) 0.3994(6) 0.0413(4) 0.0681(13) Uani 1 d . . H1A H 1.0489(52) 0.4316(31) -0.0379(8) 0.124(14) Uiso 1 calc R . H1B H 0.9790(34) 0.2805(11) 0.0486(28) 0.124(14) Uiso 1 calc R . H1C H 1.1796(20) 0.3988(39) 0.0737(23) 0.124(14) Uiso 1 calc R . C2 C 0.6022(8) 0.5773(7) 0.1932(4) 0.0758(14) Uani 1 d . . H2A H 0.6179(14) 0.6241(58) 0.2692(15) 0.152(17) Uiso 1 calc R . H2B H 0.5459(33) 0.4560(12) 0.1965(34) 0.152(17) Uiso 1 calc R . H2C H 0.5076(23) 0.6540(51) 0.1510(23) 0.152(17) 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 Ga1 0.0537(4) 0.0472(4) 0.0742(5) -0.0037(3) 0.0055(3) -0.0033(3) B1 0.071(3) 0.045(2) 0.064(3) -0.001(3) -0.003(3) -0.006(3) C1 0.067(3) 0.054(2) 0.084(3) -0.008(3) 0.010(3) -0.002(3) C2 0.059(3) 0.088(4) 0.080(3) 0.016(3) 0.004(3) 0.001(4) _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 Ga1 C2 1.923(5) . ? Ga1 C1 1.927(5) . ? Ga1 B1 2.269(5) . ? Ga1 H4 2.74(5) 4_465 ? Ga1 H3 2.82(5) 3_745 ? Ga1 H1 1.91(5) . ? Ga1 H2 1.88(5) . ? B1 H1 1.12(5) . ? B1 H2 1.04(5) . ? B1 H3 1.10(5) . ? B1 H4 1.12(5) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C1 H1C 0.97 . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C2 H2C 0.97 . ? 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 C2 Ga1 C1 137.4(2) . . ? C2 Ga1 B1 111.1(2) . . ? C1 Ga1 B1 111.6(2) . . ? C2 Ga1 H4 89.6(12) . 4_465 ? C1 Ga1 H4 85.3(12) . 4_465 ? B1 Ga1 H4 96.6(11) . 4_465 ? C2 Ga1 H3 87.9(10) . 3_745 ? C1 Ga1 H3 90.0(9) . 3_745 ? B1 Ga1 H3 93.3(10) . 3_745 ? H4 Ga1 H3 170.0(14) 4_465 3_745 ? C2 Ga1 H1 112.2(14) . . ? C1 Ga1 H1 104.6(14) . . ? B1 Ga1 H1 29.6(14) . . ? H4 Ga1 H1 67.1(18) 4_465 . ? H3 Ga1 H1 122.7(17) 3_745 . ? C2 Ga1 H2 110.7(14) . . ? C1 Ga1 H2 107.2(14) . . ? B1 Ga1 H2 27.2(14) . . ? H4 Ga1 H2 123.6(17) 4_465 . ? H3 Ga1 H2 66.3(16) 3_745 . ? H1 Ga1 H2 56.4(20) . . ? Ga1 B1 H1 57.3(24) . . ? Ga1 B1 H2 55.4(25) . . ? H1 B1 H2 111.7(31) . . ? Ga1 B1 H3 122.1(24) . . ? H1 B1 H3 116.3(36) . . ? H2 B1 H3 107.7(29) . . ? Ga1 B1 H4 123.7(29) . . ? H1 B1 H4 98.2(36) . . ? H2 B1 H4 108.5(37) . . ? H3 B1 H4 114.2(38) . . ? Ga1 C1 H1A 109.5(2) . . ? Ga1 C1 H1B 109.47(15) . . ? H1A C1 H1B 109.5 . . ? Ga1 C1 H1C 109.5(2) . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Ga1 C2 H2A 109.5(2) . . ? Ga1 C2 H2B 109.5(2) . . ? H2A C2 H2B 109.5 . . ? Ga1 C2 H2C 109.5(2) . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _refine_diff_density_max 0.187 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.044 #===END data_me2gab _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H20 B Ga O' _chemical_formula_weight 188.75 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4628(12) _cell_length_b 7.8998(13) _cell_length_c 10.539(2) _cell_angle_alpha 87.926(9) _cell_angle_beta 77.525(10) _cell_angle_gamma 64.083(8) _cell_volume 544.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method ? _exptl_crystal_F_000 200 _exptl_absorpt_coefficient_mu 2.469 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.953 _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 ? _diffrn_measurement_method 'omega-theta with profile learning' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2026 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1924 _reflns_number_observed 1659 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.6770P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0254(25) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1908 _refine_ls_number_parameters 103 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_obs 0.0365 _refine_ls_wR_factor_all 0.0866 _refine_ls_wR_factor_obs 0.0735 _refine_ls_goodness_of_fit_all 1.077 _refine_ls_goodness_of_fit_obs 1.064 _refine_ls_restrained_S_all 1.159 _refine_ls_restrained_S_obs 1.064 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.72249(6) 0.86096(6) 0.74424(4) 0.0488(2) Uani 1 d . . C1 C 0.8845(7) 0.8060(6) 0.5658(4) 0.0684(12) Uani 1 d . . H1A H 0.7978(13) 0.8787(33) 0.5067(5) 0.103 Uiso 1 calc R . H1B H 0.9402(39) 0.6710(10) 0.5420(11) 0.103 Uiso 1 calc R . H1C H 0.9971(28) 0.8408(40) 0.5592(8) 0.103 Uiso 1 calc R . C2 C 0.8061(6) 0.7903(6) 0.9087(4) 0.0638(11) Uani 1 d . . H2A H 0.6927(16) 0.8646(29) 0.9810(4) 0.096 Uiso 1 calc R . H2B H 0.9237(28) 0.8149(38) 0.9097(12) 0.096 Uiso 1 calc R . H2C H 0.8442(42) 0.6558(11) 0.9183(13) 0.096 Uiso 1 calc R . B1 B 0.4406(8) 0.8023(7) 0.7431(5) 0.0595(12) Uani 1 d D . H1 H 0.6089(46) 0.6854(49) 0.7256(39) 0.079(13) Uiso 1 d D . H2 H 0.4742(53) 0.9326(42) 0.7490(33) 0.055(10) Uiso 1 d D . H3 H 0.3361(55) 0.8009(55) 0.8306(30) 0.071(12) Uiso 1 d D . H4 H 0.3792(60) 0.8190(57) 0.6580(31) 0.077(13) Uiso 1 d D . C3 C 0.8738(7) 1.2437(7) 0.8192(5) 0.0830(14) Uani 1 d . . H3A H 0.8999(22) 1.2989(45) 0.8908(14) 0.125 Uiso 1 calc R . H3B H 0.8816(18) 1.3151(42) 0.7419(21) 0.125 Uiso 1 calc R . H3C H 0.9763(8) 1.1122(8) 0.7993(33) 0.125 Uiso 1 calc R . C4 C 0.6679(6) 1.2509(6) 0.8576(4) 0.0593(10) Uani 1 d . . H4A H 0.6553(6) 1.1920(6) 0.9415(4) 0.071 Uiso 1 calc R . H4B H 0.5643(6) 1.3844(6) 0.8707(4) 0.071 Uiso 1 calc R . O5 O 0.6271(4) 1.1557(3) 0.7617(2) 0.0493(6) Uani 1 d . . C6 C 0.5431(7) 1.2741(6) 0.6608(4) 0.0631(11) Uani 1 d . . H6A H 0.5721(7) 1.1930(6) 0.5824(4) 0.076 Uiso 1 calc R . H6B H 0.6124(7) 1.3565(6) 0.6370(4) 0.076 Uiso 1 calc R . C7 C 0.3213(7) 1.3926(7) 0.7003(6) 0.092(2) Uani 1 d . . H7A H 0.2515(8) 1.3120(7) 0.7237(36) 0.137 Uiso 1 calc R . H7B H 0.2729(12) 1.4674(40) 0.6280(13) 0.137 Uiso 1 calc R . H7C H 0.2918(8) 1.4773(37) 0.7757(23) 0.137 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 Ga1 0.0518(3) 0.0434(3) 0.0477(3) 0.0036(2) -0.0101(2) -0.0184(2) C1 0.071(3) 0.057(2) 0.056(2) -0.005(2) 0.000(2) -0.015(2) C2 0.064(3) 0.062(3) 0.063(3) 0.014(2) -0.020(2) -0.023(2) B1 0.070(3) 0.066(3) 0.059(3) 0.010(2) -0.019(2) -0.043(3) C3 0.075(3) 0.083(3) 0.113(4) 0.023(3) -0.044(3) -0.045(3) C4 0.073(3) 0.060(2) 0.049(2) 0.002(2) -0.015(2) -0.032(2) O5 0.061(2) 0.0443(13) 0.0470(14) 0.0052(11) -0.0200(12) -0.0238(12) C6 0.077(3) 0.051(2) 0.065(3) 0.013(2) -0.031(2) -0.026(2) C7 0.064(3) 0.066(3) 0.153(5) 0.018(3) -0.054(3) -0.023(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 Ga1 H2 1.67(3) . ? Ga1 C2 1.949(4) . ? Ga1 C1 1.950(4) . ? Ga1 H1 1.95(4) . ? Ga1 O5 2.119(2) . ? Ga1 B1 2.346(5) . ? B1 H4 1.07(3) . ? B1 H3 1.07(3) . ? B1 H1 1.17(3) . ? B1 H2 1.17(3) . ? C3 C4 1.478(6) . ? C4 O5 1.438(4) . ? O5 C6 1.450(4) . ? C6 C7 1.472(6) . ? 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 H2 Ga1 C2 116.0(12) . . ? H2 Ga1 C1 111.7(12) . . ? C2 Ga1 C1 130.4(2) . . ? H2 Ga1 H1 57.5(17) . . ? C2 Ga1 H1 100.5(12) . . ? C1 Ga1 H1 93.6(11) . . ? H2 Ga1 O5 81.7(10) . . ? C2 Ga1 O5 99.99(14) . . ? C1 Ga1 O5 99.40(14) . . ? H1 Ga1 O5 139.1(8) . . ? H2 Ga1 B1 27.9(10) . . ? C2 Ga1 B1 109.2(2) . . ? C1 Ga1 B1 106.3(2) . . ? H1 Ga1 B1 29.7(8) . . ? O5 Ga1 B1 109.58(15) . . ? H4 B1 H3 113.0(31) . . ? H4 B1 H1 112.0(30) . . ? H3 B1 H1 117.6(29) . . ? H4 B1 H2 104.6(28) . . ? H3 B1 H2 110.0(27) . . ? H1 B1 H2 97.8(26) . . ? H4 B1 Ga1 121.3(22) . . ? H3 B1 Ga1 122.9(21) . . ? H1 B1 Ga1 55.9(20) . . ? H2 B1 Ga1 42.1(17) . . ? O5 C4 C3 112.4(4) . . ? C4 O5 C6 113.9(3) . . ? C4 O5 Ga1 124.9(2) . . ? C6 O5 Ga1 120.4(2) . . ? O5 C6 C7 113.1(4) . . ? _refine_diff_density_max 0.503 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.063 #===END data_megath _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C6 H18 B Ga O' _chemical_formula_weight 186.73 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 '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 21/c' 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 11.5311(15) _cell_length_b 7.6473(13) _cell_length_c 12.552(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.422(9) _cell_angle_gamma 90.00 _cell_volume 999.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method ? _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 2.688 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 0.864 _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(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 ? _diffrn_measurement_method 'omega-theta with learnt profile' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3958 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1704 _reflns_number_observed 1492 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.3696P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0173(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1701 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_obs 0.0238 _refine_ls_wR_factor_all 0.0602 _refine_ls_wR_factor_obs 0.0566 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.093 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.093 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.33566(2) 0.89275(3) 0.56992(2) 0.03698(13) Uani 1 d . . B1 B 0.1666(3) 0.7586(5) 0.5926(3) 0.0528(7) Uani 1 d . . H1 H 0.1651(28) 0.8672(36) 0.5280(27) 0.067(9) Uiso 1 d . . H2 H 0.2643(27) 0.7046(36) 0.6377(24) 0.061(8) Uiso 1 d . . H3 H 0.1351(27) 0.8181(38) 0.6560(25) 0.064(8) Uiso 1 d . . H4 H 0.0998(32) 0.6693(43) 0.5296(29) 0.083(10) Uiso 1 d . . C1M C 0.4011(3) 0.7485(3) 0.4801(2) 0.0501(6) Uani 1 d . . H1M1 H 0.3330(6) 0.7290(20) 0.4008(6) 0.075 Uiso 1 calc R . H1M2 H 0.4299(17) 0.6358(10) 0.5200(9) 0.075 Uiso 1 calc R . H1M3 H 0.4736(12) 0.8080(12) 0.4745(14) 0.075 Uiso 1 calc R . C2M C 0.4272(3) 1.0246(4) 0.7145(2) 0.0526(6) Uani 1 d . . H2M1 H 0.4630(16) 0.9438(4) 0.7814(3) 0.079 Uiso 1 calc R . H2M2 H 0.3678(5) 1.1054(18) 0.7263(9) 0.079 Uiso 1 calc R . H2M3 H 0.4969(12) 1.0910(20) 0.7087(7) 0.079 Uiso 1 calc R . O1 O 0.2664(2) 1.1035(2) 0.45069(14) 0.0420(4) Uani 1 d . . C2 C 0.2059(3) 1.0793(4) 0.3234(2) 0.0686(9) Uani 1 d . . H2A H 0.1600(3) 0.9660(4) 0.3028(2) 0.082 Uiso 1 calc R . H2B H 0.2711(3) 1.0811(4) 0.2918(2) 0.082 Uiso 1 calc R . C3 C 0.1149(3) 1.2252(4) 0.2742(2) 0.0709(9) Uani 1 d . . H3A H 0.0262(3) 1.1864(4) 0.2550(2) 0.085 Uiso 1 calc R . H3B H 0.1179(3) 1.2703(4) 0.2015(2) 0.085 Uiso 1 calc R . C4 C 0.1554(3) 1.3617(4) 0.3662(3) 0.0645(8) Uani 1 d . . H4A H 0.0804(3) 1.4275(4) 0.3637(3) 0.077 Uiso 1 calc R . H4B H 0.2158(3) 1.4446(4) 0.3560(3) 0.077 Uiso 1 calc R . C5 C 0.2195(3) 1.2639(4) 0.4792(2) 0.0581(7) Uani 1 d . . H5A H 0.2915(3) 1.3329(4) 0.5373(2) 0.070 Uiso 1 calc R . H5B H 0.1577(3) 1.2382(4) 0.5127(2) 0.070 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 Ga1 0.0386(2) 0.0403(2) 0.0323(2) -0.00062(11) 0.01551(12) -0.00350(11) B1 0.051(2) 0.061(2) 0.055(2) -0.003(2) 0.030(2) -0.013(2) C1M 0.0567(15) 0.0463(14) 0.054(2) -0.0013(12) 0.0300(13) 0.0000(12) C2M 0.059(2) 0.056(2) 0.0378(14) -0.0044(12) 0.0163(12) -0.0072(13) O1 0.0540(10) 0.0395(8) 0.0319(8) 0.0002(7) 0.0178(7) 0.0013(7) C2 0.095(2) 0.067(2) 0.0325(15) -0.0029(13) 0.0162(15) 0.013(2) C3 0.081(2) 0.074(2) 0.042(2) 0.0040(14) 0.0118(15) 0.014(2) C4 0.080(2) 0.050(2) 0.058(2) 0.0081(13) 0.025(2) 0.0094(14) C5 0.074(2) 0.0472(15) 0.046(2) -0.0042(12) 0.0200(14) 0.0130(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 Ga1 C2M 1.944(2) . ? Ga1 C1M 1.946(3) . ? Ga1 O1 2.109(2) . ? Ga1 B1 2.326(3) . ? Ga1 H1 1.82(3) . ? Ga1 H2 2.02(3) . ? B1 H1 1.15(3) . ? B1 H2 1.10(3) . ? B1 H3 1.10(3) . ? B1 H4 1.08(3) . ? C1M H1M1 0.98 . ? C1M H1M2 0.98 . ? C1M H1M3 0.98 . ? C2M H2M1 0.98 . ? C2M H2M2 0.98 . ? C2M H2M3 0.98 . ? O1 C5 1.446(3) . ? O1 C2 1.455(3) . ? C2 C3 1.473(4) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.476(4) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.488(4) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? 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 C2M Ga1 C1M 130.12(12) . . ? C2M Ga1 O1 98.90(9) . . ? C1M Ga1 O1 98.34(9) . . ? C2M Ga1 B1 105.21(12) . . ? C1M Ga1 B1 112.00(12) . . ? O1 Ga1 B1 109.99(10) . . ? C2M Ga1 H1 114.4(9) . . ? C1M Ga1 H1 114.4(9) . . ? O1 Ga1 H1 81.0(9) . . ? B1 Ga1 H1 29.2(9) . . ? C2M Ga1 H2 97.6(8) . . ? C1M Ga1 H2 99.8(8) . . ? O1 Ga1 H2 138.2(8) . . ? B1 Ga1 H2 28.2(8) . . ? H1 Ga1 H2 57.2(12) . . ? Ga1 B1 H1 50.1(15) . . ? Ga1 B1 H2 60.2(14) . . ? H1 B1 H2 109.6(21) . . ? Ga1 B1 H3 117.3(15) . . ? H1 B1 H3 107.4(20) . . ? H2 B1 H3 111.3(21) . . ? Ga1 B1 H4 124.2(18) . . ? H1 B1 H4 98.6(22) . . ? H2 B1 H4 113.0(22) . . ? H3 B1 H4 115.9(23) . . ? Ga1 C1M H1M1 109.47(8) . . ? Ga1 C1M H1M2 109.47(8) . . ? H1M1 C1M H1M2 109.5 . . ? Ga1 C1M H1M3 109.47(8) . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? Ga1 C2M H2M1 109.47(8) . . ? Ga1 C2M H2M2 109.47(9) . . ? H2M1 C2M H2M2 109.5 . . ? Ga1 C2M H2M3 109.47(9) . . ? H2M1 C2M H2M3 109.5 . . ? H2M2 C2M H2M3 109.5 . . ? C5 O1 C2 109.0(2) . . ? C5 O1 Ga1 122.72(14) . . ? C2 O1 Ga1 122.63(15) . . ? O1 C2 C3 106.5(2) . . ? O1 C2 H2A 110.43(15) . . ? C3 C2 H2A 110.4(2) . . ? O1 C2 H2B 110.4(2) . . ? C3 C2 H2B 110.4(2) . . ? H2A C2 H2B 108.6 . . ? C2 C3 C4 106.2(2) . . ? C2 C3 H3A 110.5(2) . . ? C4 C3 H3A 110.5(2) . . ? C2 C3 H3B 110.5(2) . . ? C4 C3 H3B 110.5(2) . . ? H3A C3 H3B 108.7 . . ? C3 C4 C5 104.5(2) . . ? C3 C4 H4A 110.8(2) . . ? C5 C4 H4A 110.8(2) . . ? C3 C4 H4B 110.8(2) . . ? C5 C4 H4B 110.8(2) . . ? H4A C4 H4B 108.9 . . ? O1 C5 C4 106.0(2) . . ? O1 C5 H5A 110.53(14) . . ? C4 C5 H5A 110.5(2) . . ? O1 C5 H5B 110.53(14) . . ? C4 C5 H5B 110.5(2) . . ? H5A C5 H5B 108.7 . . ? _refine_diff_density_max 0.344 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.048 #===END