#Supplementary Information (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 # 1. SUBMISSION DETAILS data_global _publ_contact_autor ; Prof. Dr. Werner Uhl Phillips-Universitaet Marburg Fachbereich Chemie Hans-Meerwein-Straße D-35043 Marburg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 6421 2825751' _publ_contact_author_fax '049 6421 2828917' _publ_contact_author_email 'Uhl@chemie.uni-marburg.de ' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in J. Chem. Soc. Dalton Trans. as New Crystal Structures. ; #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Unexpected formation of gallium-gallium single bonds by irradiation of the hydride [(Me3C)2GaH]3 ; loop_ _publ_author_name _publ_author_address 'Werner Uhl' ; Phillips-Universitaet Marburg Fachbereich Chemie Hans-Meerwein-Straße D-35043 Marburg Bundesrepublik Deutschland ; 'Lars Cuypers' ; Phillips-Universitaet Marburg Fachbereich Chemie Hans-Meerwein-Straße D-35043 Marburg Bundesrepublik Deutschland ; 'Gertraud Geiseler' ; Phillips-Universitaet Marburg Fachbereich Chemie Hans-Meerwein-Straße D-35043 Marburg Bundesrepublik Deutschland ; 'Klaus Harms' ; Phillips-Universitaet Marburg Fachbereich Chemie Hans-Meerwein-Straße D-35043 Marburg Bundesrepublik Deutschland ; 'Bernhard Neumüller' ; Phillips-Universitaet Marburg Fachbereich Chemie Hans-Meerwein-Straße D-35043 Marburg Bundesrepublik Deutschland ; #=========================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G. M. (1993) Program SHELXL-93, University of G"ttingen. Sheldrick, G. M. (1990) Program SHELXL-86, University of G"ttingen. T. Hahn (Ed.), International Tables for Crystallography, Space Group Symmetry, Kluwer Academic Publishers, Dordrecht-Boston-London, 1989, Bd. A ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #=========================================================================== data_ga6H6tbu8 _database_code_CSD 161949 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H78 Ga6' _chemical_formula_weight 881.26 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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4126(8) _cell_length_b 17.328(2) _cell_length_c 18.3590(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.582(7) _cell_angle_gamma 90.00 _cell_volume 4491.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.39 mm _exptl_crystal_size_mid 0.24 mm _exptl_crystal_size_min 0.21 mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 3.564 _exptl_absorpt_correction_type numeric _exptl_absorpt_correction_T_min 0.332 _exptl_absorpt_correction_T_max 0.509 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21857 _diffrn_reflns_av_R_equivalents 0.1430 _diffrn_reflns_av_sigmaI/netI 0.0985 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.90 _reflns_number_total 4192 _reflns_number_gt 2271 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0704P)^2^+35.2168P] 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 4192 _refine_ls_number_parameters 258 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.860 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.004 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 H1 H 0.471(6) 0.224(5) 0.654(4) 0.08(3) Uiso 1 1 d . . . Ga1 Ga 0.56101(6) 0.13926(6) 0.81403(5) 0.0609(3) Uani 1 1 d . . . C1 C 0.6093(6) 0.0611(5) 0.8941(5) 0.062(2) Uani 1 1 d U . . C11 C 0.5527(9) -0.0139(6) 0.8786(7) 0.108(4) Uani 1 1 d U . . H11A H 0.5610 -0.0350 0.8320 0.129 Uiso 1 1 calc R . . H11B H 0.4868 -0.0034 0.8764 0.129 Uiso 1 1 calc R . . H11C H 0.5749 -0.0502 0.9177 0.129 Uiso 1 1 calc R . . C12 C 0.7105(8) 0.0416(10) 0.8923(9) 0.164(7) Uani 1 1 d U . . H12A H 0.7504 0.0846 0.9106 0.196 Uiso 1 1 calc R . . H12B H 0.7159 0.0305 0.8421 0.196 Uiso 1 1 calc R . . H12C H 0.7297 -0.0027 0.9230 0.196 Uiso 1 1 calc R . . C13 C 0.5986(14) 0.0903(7) 0.9669(5) 0.152(6) Uani 1 1 d U . . H13A H 0.6161 0.0507 1.0037 0.183 Uiso 1 1 calc R . . H13B H 0.5339 0.1050 0.9648 0.183 Uiso 1 1 calc R . . H13C H 0.6389 0.1344 0.9799 0.183 Uiso 1 1 calc R . . Ga2 Ga 0.51312(7) 0.29563(6) 0.68082(5) 0.0604(3) Uani 1 1 d . . . C2 C 0.5092(7) 0.3768(5) 0.6021(5) 0.063(2) Uani 1 1 d . . . C21 C 0.5523(13) 0.4509(8) 0.6426(8) 0.093(6) Uani 0.74(2) 1 d PD A 1 H21A H 0.5521 0.4915 0.6070 0.112 Uiso 0.74(2) 1 calc PR A 1 H21B H 0.6161 0.4408 0.6679 0.112 Uiso 0.74(2) 1 calc PR A 1 H21C H 0.5152 0.4664 0.6781 0.112 Uiso 0.74(2) 1 calc PR A 1 C22 C 0.5680(18) 0.3525(11) 0.5473(11) 0.125(10) Uani 0.74(2) 1 d PD A 1 H22A H 0.5677 0.3927 0.5113 0.150 Uiso 0.74(2) 1 calc PR A 1 H22B H 0.5421 0.3062 0.5225 0.150 Uiso 0.74(2) 1 calc PR A 1 H22C H 0.6318 0.3430 0.5729 0.150 Uiso 0.74(2) 1 calc PR A 1 C23 C 0.4082(10) 0.3961(10) 0.5628(9) 0.098(7) Uani 0.74(2) 1 d PD A 1 H23A H 0.3736 0.4158 0.5983 0.117 Uiso 0.74(2) 1 calc PR A 1 H23B H 0.3777 0.3504 0.5401 0.117 Uiso 0.74(2) 1 calc PR A 1 H23C H 0.4098 0.4344 0.5253 0.117 Uiso 0.74(2) 1 calc PR A 1 C21A C 0.617(3) 0.399(3) 0.602(2) 0.11(2) Uani 0.26(2) 1 d PD A 2 H21D H 0.6198 0.4302 0.5595 0.130 Uiso 0.26(2) 1 calc PR A 2 H21E H 0.6536 0.3532 0.6013 0.130 Uiso 0.26(2) 1 calc PR A 2 H21F H 0.6423 0.4281 0.6466 0.130 Uiso 0.26(2) 1 calc PR A 2 C22A C 0.458(3) 0.4452(19) 0.619(2) 0.077(16) Uani 0.26(2) 1 d PD A 2 H22D H 0.4938 0.4904 0.6112 0.093 Uiso 0.26(2) 1 calc PR A 2 H22E H 0.4508 0.4432 0.6693 0.093 Uiso 0.26(2) 1 calc PR A 2 H22F H 0.3974 0.4469 0.5861 0.093 Uiso 0.26(2) 1 calc PR A 2 C23A C 0.471(4) 0.338(2) 0.529(2) 0.104(18) Uani 0.26(2) 1 d PD A 2 H23D H 0.4072 0.3206 0.5280 0.124 Uiso 0.26(2) 1 calc PR A 2 H23E H 0.5098 0.2943 0.5230 0.124 Uiso 0.26(2) 1 calc PR A 2 H23F H 0.4706 0.3737 0.4890 0.124 Uiso 0.26(2) 1 calc PR A 2 Ga3 Ga 0.72383(6) 0.21307(5) 0.73157(4) 0.0479(3) Uani 1 1 d . B . H31 H 0.666(4) 0.173(3) 0.790(3) 0.017(13) Uiso 1 1 d . . . H32 H 0.621(4) 0.261(3) 0.688(3) 0.026(15) Uiso 1 1 d . . . C3 C 0.7546(7) 0.1409(6) 0.6549(6) 0.078(3) Uani 1 1 d U . . C31 C 0.689(4) 0.156(2) 0.5818(14) 0.19(2) Uani 0.56(3) 1 d PDU B 3 H31A H 0.6755 0.1085 0.5552 0.225 Uiso 0.56(3) 1 calc PR B 3 H31B H 0.7191 0.1912 0.5531 0.225 Uiso 0.56(3) 1 calc PR B 3 H31C H 0.6315 0.1786 0.5904 0.225 Uiso 0.56(3) 1 calc PR B 3 C32 C 0.732(3) 0.0543(13) 0.672(2) 0.164(19) Uani 0.56(3) 1 d PDU B 3 H32A H 0.6659 0.0490 0.6718 0.197 Uiso 0.56(3) 1 calc PR B 3 H32B H 0.7684 0.0399 0.7197 0.197 Uiso 0.56(3) 1 calc PR B 3 H32C H 0.7488 0.0214 0.6344 0.197 Uiso 0.56(3) 1 calc PR B 3 C33 C 0.854(2) 0.138(3) 0.648(3) 0.19(2) Uani 0.56(3) 1 d PDU B 3 H33A H 0.8606 0.1038 0.6080 0.226 Uiso 0.56(3) 1 calc PR B 3 H33B H 0.8923 0.1193 0.6935 0.226 Uiso 0.56(3) 1 calc PR B 3 H33C H 0.8750 0.1887 0.6376 0.226 Uiso 0.56(3) 1 calc PR B 3 C31A C 0.783(4) 0.194(2) 0.599(2) 0.147(19) Uani 0.44(3) 1 d PDU B 4 H31D H 0.7989 0.1639 0.5590 0.176 Uiso 0.44(3) 1 calc PR B 4 H31E H 0.8369 0.2237 0.6220 0.176 Uiso 0.44(3) 1 calc PR B 4 H31F H 0.7313 0.2278 0.5793 0.176 Uiso 0.44(3) 1 calc PR B 4 C32A C 0.680(3) 0.095(3) 0.631(3) 0.19(3) Uani 0.44(3) 1 d PDU B 4 H32D H 0.6841 0.0739 0.5838 0.228 Uiso 0.44(3) 1 calc PR B 4 H32E H 0.6229 0.1245 0.6270 0.228 Uiso 0.44(3) 1 calc PR B 4 H32F H 0.6801 0.0540 0.6664 0.228 Uiso 0.44(3) 1 calc PR B 4 C33A C 0.841(3) 0.097(2) 0.6966(19) 0.14(2) Uani 0.44(3) 1 d PDU B 4 H33D H 0.8274 0.0771 0.7421 0.169 Uiso 0.44(3) 1 calc PR B 4 H33E H 0.8939 0.1316 0.7077 0.169 Uiso 0.44(3) 1 calc PR B 4 H33F H 0.8552 0.0555 0.6664 0.169 Uiso 0.44(3) 1 calc PR B 4 C4 C 0.8125(6) 0.2829(6) 0.7956(5) 0.073(2) Uani 1 1 d U . . C41 C 0.8564(11) 0.3377(9) 0.7455(8) 0.148(6) Uani 1 1 d U B . H41A H 0.8068 0.3639 0.7119 0.177 Uiso 1 1 calc R . . H41B H 0.8938 0.3084 0.7177 0.177 Uiso 1 1 calc R . . H41C H 0.8958 0.3749 0.7759 0.177 Uiso 1 1 calc R . . C42 C 0.8919(9) 0.2401(10) 0.8420(8) 0.149(6) Uani 1 1 d U B . H42A H 0.9381 0.2760 0.8672 0.179 Uiso 1 1 calc R . . H42B H 0.9207 0.2070 0.8109 0.179 Uiso 1 1 calc R . . H42C H 0.8684 0.2095 0.8779 0.179 Uiso 1 1 calc R . . C43 C 0.7618(11) 0.3319(11) 0.8421(9) 0.186(8) Uani 1 1 d U B . H43A H 0.7441 0.3008 0.8804 0.224 Uiso 1 1 calc R . . H43B H 0.7060 0.3534 0.8114 0.224 Uiso 1 1 calc R . . H43C H 0.8027 0.3728 0.8644 0.224 Uiso 1 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 0.0408(5) 0.0772(7) 0.0675(6) 0.0357(5) 0.0174(4) 0.0094(4) C1 0.049(5) 0.073(5) 0.064(5) 0.014(4) 0.011(4) 0.007(4) C11 0.122(9) 0.079(7) 0.111(8) 0.024(6) -0.003(8) -0.005(6) C12 0.060(6) 0.208(16) 0.225(15) 0.140(13) 0.033(8) 0.045(7) C13 0.296(19) 0.099(9) 0.052(6) 0.017(5) 0.012(8) 0.068(11) Ga2 0.0439(6) 0.0725(7) 0.0693(6) 0.0335(5) 0.0220(4) 0.0088(5) C2 0.064(6) 0.077(6) 0.053(5) 0.017(4) 0.020(4) -0.001(5) C21 0.103(15) 0.074(10) 0.102(11) 0.030(8) 0.020(10) -0.013(9) C22 0.17(2) 0.111(15) 0.117(16) 0.065(13) 0.090(17) 0.058(16) C23 0.067(10) 0.116(15) 0.105(13) 0.072(12) 0.005(8) 0.003(9) C21A 0.16(5) 0.10(4) 0.06(3) 0.04(3) 0.03(3) -0.01(4) C22A 0.12(5) 0.05(2) 0.07(3) 0.007(19) 0.05(3) 0.01(2) C23A 0.11(5) 0.08(3) 0.12(4) 0.04(3) 0.03(3) 0.02(3) Ga3 0.0354(5) 0.0545(5) 0.0574(5) 0.0011(4) 0.0175(4) -0.0007(4) C3 0.062(6) 0.086(6) 0.093(6) -0.009(5) 0.030(5) 0.008(5) C31 0.29(5) 0.15(3) 0.087(16) -0.073(16) -0.04(2) 0.10(4) C32 0.25(5) 0.065(11) 0.23(3) -0.011(16) 0.18(4) 0.023(17) C33 0.108(14) 0.25(5) 0.24(5) -0.16(4) 0.12(2) -0.05(2) C31A 0.20(5) 0.20(4) 0.07(2) 0.027(19) 0.09(3) 0.06(3) C32A 0.11(2) 0.17(4) 0.32(7) -0.21(4) 0.11(3) -0.04(2) C33A 0.15(4) 0.14(4) 0.15(3) 0.01(2) 0.06(2) 0.10(3) C4 0.050(5) 0.081(7) 0.084(6) -0.014(5) 0.006(4) -0.013(4) C41 0.147(14) 0.141(12) 0.147(12) 0.011(8) 0.010(9) -0.081(10) C42 0.088(9) 0.203(16) 0.132(11) 0.023(9) -0.037(8) -0.006(8) C43 0.095(10) 0.26(2) 0.201(15) -0.168(14) 0.033(9) -0.039(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 Ga1 C1 2.017(8) . ? Ga1 Ga1 2.6380(19) 2_656 ? Ga1 Ga2 2.9211(14) 2_656 ? Ga1 H31 1.76(5) . ? C1 C13 1.466(13) . ? C1 C12 1.504(14) . ? C1 C11 1.529(14) . ? C11 H11A 0.9599 . ? C11 H11B 0.9599 . ? C11 H11C 0.9599 . ? C12 H12A 0.9599 . ? C12 H12B 0.9599 . ? C12 H12C 0.9599 . ? C13 H13A 0.9599 . ? C13 H13B 0.9599 . ? C13 H13C 0.9599 . ? Ga2 C2 2.010(8) . ? Ga2 Ga2 2.6421(18) 2_656 ? Ga2 Ga1 2.9211(14) 2_656 ? Ga2 H1 1.43(8) . ? Ga2 H32 1.65(6) . ? C2 C22A 1.46(3) . ? C2 C22 1.500(18) . ? C2 C23A 1.51(4) . ? C2 C23 1.526(15) . ? C2 C21 1.551(17) . ? C2 C21A 1.60(4) . ? C21 H21A 0.9599 . ? C21 H21B 0.9599 . ? C21 H21C 0.9599 . ? C22 H22A 0.9599 . ? C22 H22B 0.9599 . ? C22 H22C 0.9599 . ? C23 H23A 0.9599 . ? C23 H23B 0.9599 . ? C23 H23C 0.9599 . ? C21A H21D 0.9599 . ? C21A H21E 0.9599 . ? C21A H21F 0.9599 . ? C22A H22D 0.9599 . ? C22A H22E 0.9599 . ? C22A H22F 0.9599 . ? C23A H23D 0.9599 . ? C23A H23E 0.9599 . ? C23A H23F 0.9599 . ? Ga3 C4 1.969(9) . ? Ga3 C3 1.998(10) . ? Ga3 H31 1.64(5) . ? Ga3 H32 1.75(5) . ? C3 C32A 1.33(3) . ? C3 C33 1.47(3) . ? C3 C31A 1.50(3) . ? C3 C31 1.50(2) . ? C3 C33A 1.52(3) . ? C3 C32 1.58(2) . ? C31 H31A 0.9599 . ? C31 H31B 0.9599 . ? C31 H31C 0.9599 . ? C32 H32A 0.9599 . ? C32 H32B 0.9599 . ? C32 H32C 0.9599 . ? C33 H33A 0.9599 . ? C33 H33B 0.9599 . ? C33 H33C 0.9599 . ? C31A H31D 0.9599 . ? C31A H31E 0.9599 . ? C31A H31F 0.9599 . ? C32A H32D 0.9599 . ? C32A H32E 0.9599 . ? C32A H32F 0.9599 . ? C33A H33D 0.9599 . ? C33A H33E 0.9599 . ? C33A H33F 0.9599 . ? C4 C42 1.482(15) . ? C4 C43 1.495(16) . ? C4 C41 1.542(15) . ? C41 H41A 0.9599 . ? C41 H41B 0.9599 . ? C41 H41C 0.9599 . ? C42 H42A 0.9599 . ? C42 H42B 0.9599 . ? C42 H42C 0.9599 . ? C43 H43A 0.9599 . ? C43 H43B 0.9599 . ? C43 H43C 0.9599 . ? 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 C1 Ga1 Ga1 136.1(3) . 2_656 ? C1 Ga1 Ga2 132.4(3) . 2_656 ? Ga1 Ga1 Ga2 81.15(3) 2_656 2_656 ? C1 Ga1 H31 102.6(16) . . ? Ga1 Ga1 H31 103.1(16) 2_656 . ? Ga2 Ga1 H31 92.3(17) 2_656 . ? C13 C1 C12 112.2(12) . . ? C13 C1 C11 108.3(10) . . ? C12 C1 C11 106.8(10) . . ? C13 C1 Ga1 110.4(7) . . ? C12 C1 Ga1 109.2(7) . . ? C11 C1 Ga1 110.0(6) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 Ga2 Ga2 134.7(3) . 2_656 ? C2 Ga2 Ga1 135.6(3) . 2_656 ? Ga2 Ga2 Ga1 81.08(3) 2_656 2_656 ? C2 Ga2 H1 114(3) . . ? Ga2 Ga2 H1 101(3) 2_656 . ? Ga1 Ga2 H1 22(3) 2_656 . ? C2 Ga2 H32 101.8(19) . . ? Ga2 Ga2 H32 103.6(18) 2_656 . ? Ga1 Ga2 H32 90.3(19) 2_656 . ? H1 Ga2 H32 92(4) . . ? C22A C2 C22 138.0(16) . . ? C22A C2 C23A 116(2) . . ? C22 C2 C23A 55.4(18) . . ? C22A C2 C23 56.5(19) . . ? C22 C2 C23 111.0(13) . . ? C23A C2 C23 62(2) . . ? C22A C2 C21 52.8(18) . . ? C22 C2 C21 109.2(13) . . ? C23A C2 C21 147.1(18) . . ? C23 C2 C21 107.3(11) . . ? C22A C2 C21A 109(2) . . ? C22 C2 C21A 52.6(17) . . ? C23A C2 C21A 107(2) . . ? C23 C2 C21A 141.4(16) . . ? C21 C2 C21A 60(2) . . ? C22A C2 Ga2 111.3(14) . . ? C22 C2 Ga2 110.4(8) . . ? C23A C2 Ga2 106.3(17) . . ? C23 C2 Ga2 112.3(7) . . ? C21 C2 Ga2 106.5(7) . . ? C21A C2 Ga2 106.3(14) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? C2 C21A H21D 109.5 . . ? C2 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C2 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C2 C22A H22D 109.5 . . ? C2 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C2 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C2 C23A H23D 109.5 . . ? C2 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C2 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C4 Ga3 C3 126.6(4) . . ? C4 Ga3 H31 103.2(17) . . ? C3 Ga3 H31 114.0(18) . . ? C4 Ga3 H32 111.7(18) . . ? C3 Ga3 H32 105.4(18) . . ? H31 Ga3 H32 90(3) . . ? C32A C3 C33 133.4(19) . . ? C32A C3 C31A 117(3) . . ? C33 C3 C31A 64(2) . . ? C32A C3 C31 60(3) . . ? C33 C3 C31 112(2) . . ? C31A C3 C31 59.0(17) . . ? C32A C3 C33A 113(3) . . ? C33 C3 C33A 46.6(17) . . ? C31A C3 C33A 110(2) . . ? C31 C3 C33A 147.1(19) . . ? C32A C3 C32 47(2) . . ? C33 C3 C32 103(2) . . ? C31A C3 C32 144(2) . . ? C31 C3 C32 103(2) . . ? C33A C3 C32 67(2) . . ? C32A C3 Ga3 108.8(13) . . ? C33 C3 Ga3 116.3(13) . . ? C31A C3 Ga3 103.4(15) . . ? C31 C3 Ga3 109.4(13) . . ? C33A C3 Ga3 103.3(14) . . ? C32 C3 Ga3 111.9(11) . . ? C3 C31 H31A 109.4 . . ? C3 C31 H31B 109.5 . . ? C3 C31 H31C 109.4 . . ? C3 C32 H32A 109.5 . . ? C3 C32 H32B 109.4 . . ? C3 C32 H32C 109.5 . . ? C3 C33 H33A 109.5 . . ? C3 C33 H33B 109.5 . . ? C3 C33 H33C 109.4 . . ? C3 C31A H31D 109.4 . . ? C3 C31A H31E 109.5 . . ? C3 C31A H31F 109.4 . . ? C3 C32A H32D 109.5 . . ? C3 C32A H32E 109.5 . . ? C3 C32A H32F 109.4 . . ? C3 C33A H33D 109.5 . . ? C3 C33A H33E 109.4 . . ? C3 C33A H33F 109.5 . . ? C42 C4 C43 111.5(12) . . ? C42 C4 C41 106.8(11) . . ? C43 C4 C41 107.3(12) . . ? C42 C4 Ga3 111.7(9) . . ? C43 C4 Ga3 110.9(7) . . ? C41 C4 Ga3 108.5(7) . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C4 C43 H43A 109.5 . . ? C4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ga1 Ga1 C1 C13 -126.7(9) 2_656 . . . ? Ga2 Ga1 C1 C13 3.6(11) 2_656 . . . ? Ga1 Ga1 C1 C12 109.6(9) 2_656 . . . ? Ga2 Ga1 C1 C12 -120.1(9) 2_656 . . . ? Ga1 Ga1 C1 C11 -7.3(9) 2_656 . . . ? Ga2 Ga1 C1 C11 123.1(7) 2_656 . . . ? Ga2 Ga2 C2 C22A -18(2) 2_656 . . . ? Ga1 Ga2 C2 C22A 116(2) 2_656 . . . ? Ga2 Ga2 C2 C22 156.0(13) 2_656 . . . ? Ga1 Ga2 C2 C22 -69.7(14) 2_656 . . . ? Ga2 Ga2 C2 C23A -145(2) 2_656 . . . ? Ga1 Ga2 C2 C23A -11(2) 2_656 . . . ? Ga2 Ga2 C2 C23 -79.5(11) 2_656 . . . ? Ga1 Ga2 C2 C23 54.8(11) 2_656 . . . ? Ga2 Ga2 C2 C21 37.6(10) 2_656 . . . ? Ga1 Ga2 C2 C21 171.9(8) 2_656 . . . ? Ga2 Ga2 C2 C21A 101(2) 2_656 . . . ? Ga1 Ga2 C2 C21A -125(2) 2_656 . . . ? C4 Ga3 C3 C32A 171(3) . . . . ? C4 Ga3 C3 C33 2(3) . . . . ? C4 Ga3 C3 C31A -64(2) . . . . ? C4 Ga3 C3 C31 -126(3) . . . . ? C4 Ga3 C3 C33A 50(2) . . . . ? C4 Ga3 C3 C32 120(2) . . . . ? C3 Ga3 C4 C42 -59.1(11) . . . . ? C3 Ga3 C4 C43 176.0(10) . . . . ? C3 Ga3 C4 C41 58.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.90 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.875 _refine_diff_density_min -1.379 _refine_diff_density_rms 0.115