Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name W.Uhl _publ_contact_author_address ; Institute fur Anorganische und Analytische Chemie University of Muenster Muenster 48149 GERMANY ; _publ_contact_author_email UHLW@UNI-MUENSTER.DE _publ_section_title ; The Reactions of Dialkylgallium Hydrides with tert-Butylethynylbenzenes - a Systematic Investigation into the Course of Hydrogallation Reactions ; loop_ _publ_author_name 'W. Uhl' 'Micheal Claesener' 'Sima Haddadpour' 'Alexander Hepp' 'Beate Jasper' # Attachment 'Uhl-2a.cif' data_Uhl-2a _database_code_depnum_ccdc_archive 'CCDC 621972' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H88 Ga3' _chemical_formula_weight 982.43 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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.417(5) _cell_length_b 15.300(5) _cell_length_c 15.668(5) _cell_angle_alpha 104.047(5) _cell_angle_beta 107.164(5) _cell_angle_gamma 94.608(5) _cell_volume 2721.7(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 'all measured' _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 31.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1046 _exptl_absorpt_coefficient_mu 1.507 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1846 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32469 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 31.48 _reflns_number_total 16302 _reflns_number_gt 11376 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0632P)^2^+0.2645P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16302 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.001 _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 Ga1 Ga 0.46299(3) 0.25251(2) 1.02433(2) 0.02369(8) Uani 1 1 d . . . C111 C 0.4117(3) 0.2854(2) 1.1337(2) 0.0348(7) Uani 1 1 d . . . H11A H 0.4130 0.3502 1.1510 0.042 Uiso 1 1 calc R . . H11B H 0.3340 0.2564 1.1166 0.042 Uiso 1 1 calc R . . C112 C 0.4821(4) 0.2594(3) 1.2170(3) 0.0556(11) Uani 1 1 d . . . H11C H 0.4737 0.1940 1.2031 0.067 Uiso 1 1 calc R . . H11D H 0.4565 0.2830 1.2690 0.067 Uiso 1 1 calc R . . H11E H 0.5610 0.2844 1.2322 0.067 Uiso 1 1 calc R . . Ga2 Ga 0.42127(3) 0.34427(2) 0.63212(2) 0.02290(8) Uani 1 1 d . . . C211 C 0.3654(3) 0.4100(2) 0.5384(2) 0.0413(9) Uani 1 1 d . . . H21A H 0.4089 0.4002 0.4964 0.050 Uiso 1 1 calc R . . H21B H 0.2874 0.3835 0.5029 0.050 Uiso 1 1 calc R . . C212 C 0.3712(4) 0.5117(3) 0.5757(3) 0.0588(12) Uani 1 1 d . . . H21C H 0.3255 0.5227 0.6159 0.071 Uiso 1 1 calc R . . H21D H 0.3428 0.5373 0.5249 0.071 Uiso 1 1 calc R . . H21E H 0.4490 0.5396 0.6102 0.071 Uiso 1 1 calc R . . Ga3 Ga 0.71406(3) 0.02809(2) 0.73498(2) 0.02362(8) Uani 1 1 d . . . C311 C 0.8084(3) -0.0631(2) 0.7009(3) 0.0533(11) Uani 1 1 d . . . H31A H 0.7749 -0.0945 0.6359 0.064 Uiso 1 1 calc R . . H31B H 0.8829 -0.0319 0.7101 0.064 Uiso 1 1 calc R . . C312 C 0.8215(6) -0.1318(4) 0.7544(6) 0.127(3) Uani 1 1 d . . . H31C H 0.8621 -0.1019 0.8189 0.153 Uiso 1 1 calc R . . H31D H 0.8635 -0.1764 0.7308 0.153 Uiso 1 1 calc R . . H31E H 0.7474 -0.1616 0.7482 0.153 Uiso 1 1 calc R . . C101 C 0.6291(2) 0.31427(18) 0.93738(18) 0.0188(5) Uani 1 1 d . . . C102 C 0.5948(2) 0.35953(17) 0.86902(18) 0.0187(5) Uani 1 1 d . . . H102 H 0.5500 0.4071 0.8780 0.022 Uiso 1 1 calc R . . C103 C 0.6241(2) 0.33733(18) 0.78784(18) 0.0187(5) Uani 1 1 d . . . C104 C 0.6877(2) 0.26753(18) 0.77554(18) 0.0193(5) Uani 1 1 d . . . H104 H 0.7066 0.2506 0.7193 0.023 Uiso 1 1 calc R . . C105 C 0.7249(2) 0.22117(17) 0.84261(18) 0.0179(5) Uani 1 1 d . . . C106 C 0.6938(2) 0.24431(18) 0.92240(18) 0.0196(5) Uani 1 1 d . . . H106 H 0.7169 0.2118 0.9683 0.024 Uiso 1 1 calc R . . C201 C 0.3975(2) 0.12818(18) 0.83258(19) 0.0202(5) Uani 1 1 d . . . C202 C 0.3509(2) 0.18597(18) 0.78012(19) 0.0199(5) Uani 1 1 d . . . H202 H 0.3098 0.2308 0.8046 0.024 Uiso 1 1 calc R . . C203 C 0.3623(2) 0.18062(18) 0.69340(18) 0.0194(5) Uani 1 1 d . . . C204 C 0.4246(2) 0.11631(18) 0.66014(19) 0.0212(5) Uani 1 1 d . . . H204 H 0.4340 0.1121 0.6007 0.025 Uiso 1 1 calc R . . C205 C 0.4734(2) 0.05794(17) 0.71099(19) 0.0193(5) Uani 1 1 d . . . C206 C 0.4604(2) 0.06577(18) 0.79760(19) 0.0204(5) Uani 1 1 d . . . H206 H 0.4956 0.0273 0.8341 0.024 Uiso 1 1 calc R . . C1 C 0.5894(2) 0.33445(19) 1.01977(19) 0.0216(5) Uani 1 1 d . . . C11 C 0.6307(2) 0.40806(19) 1.0933(2) 0.0250(6) Uani 1 1 d . . . H11 H 0.5913 0.4124 1.1381 0.030 Uiso 1 1 calc R . . C12 C 0.7285(3) 0.48621(19) 1.1190(2) 0.0271(6) Uani 1 1 d . . . C121 C 0.8332(3) 0.4549(2) 1.0971(3) 0.0410(8) Uani 1 1 d . . . H12A H 0.8944 0.5058 1.1197 0.049 Uiso 1 1 calc R . . H12B H 0.8148 0.4309 1.0310 0.049 Uiso 1 1 calc R . . H12C H 0.8564 0.4082 1.1267 0.049 Uiso 1 1 calc R . . C122 C 0.6892(3) 0.5572(2) 1.0678(3) 0.0442(9) Uani 1 1 d . . . H12D H 0.7494 0.6086 1.0882 0.053 Uiso 1 1 calc R . . H12E H 0.6230 0.5771 1.0810 0.053 Uiso 1 1 calc R . . H12F H 0.6705 0.5305 1.0021 0.053 Uiso 1 1 calc R . . C123 C 0.7619(4) 0.5313(3) 1.2236(3) 0.0581(12) Uani 1 1 d . . . H12G H 0.7809 0.4863 1.2565 0.070 Uiso 1 1 calc R . . H12H H 0.6990 0.5572 1.2373 0.070 Uiso 1 1 calc R . . H12I H 0.8268 0.5786 1.2426 0.070 Uiso 1 1 calc R . . C2 C 0.5810(2) 0.38265(18) 0.71353(18) 0.0207(5) Uani 1 1 d . . . C21 C 0.6435(2) 0.44542(19) 0.69299(19) 0.0226(6) Uani 1 1 d . . . H21 H 0.6024 0.4651 0.6406 0.027 Uiso 1 1 calc R . . C22 C 0.7684(2) 0.4909(2) 0.7382(2) 0.0250(6) Uani 1 1 d . . . C221 C 0.7788(3) 0.5838(2) 0.7177(2) 0.0351(7) Uani 1 1 d . . . H22A H 0.7528 0.5749 0.6517 0.042 Uiso 1 1 calc R . . H22B H 0.8572 0.6131 0.7433 0.042 Uiso 1 1 calc R . . H22C H 0.7330 0.6215 0.7454 0.042 Uiso 1 1 calc R . . C222 C 0.8118(3) 0.5077(2) 0.8438(2) 0.0280(6) Uani 1 1 d . . . H22D H 0.7642 0.5437 0.8710 0.034 Uiso 1 1 calc R . . H22E H 0.8890 0.5396 0.8684 0.034 Uiso 1 1 calc R . . H22F H 0.8094 0.4502 0.8583 0.034 Uiso 1 1 calc R . . C223 C 0.9730(3) 0.3246(2) 0.9155(2) 0.0299(7) Uani 1 1 d . . . H22G H 0.9650 0.3224 0.8521 0.036 Uiso 1 1 calc R . . H22H H 1.0358 0.3711 0.9565 0.036 Uiso 1 1 calc R . . H22I H 0.9040 0.3383 0.9278 0.036 Uiso 1 1 calc R . . C3 C 0.7911(2) 0.14616(18) 0.82514(19) 0.0207(5) Uani 1 1 d . . . C31 C 0.9053(2) 0.15314(19) 0.8646(2) 0.0237(6) Uani 1 1 d . . . H31 H 0.9346 0.0977 0.8470 0.028 Uiso 1 1 calc R . . C32 C 0.9955(2) 0.23235(19) 0.9315(2) 0.0242(6) Uani 1 1 d . . . C321 C 1.0042(3) 0.2342(2) 1.0316(2) 0.0381(8) Uani 1 1 d . . . H32A H 0.9346 0.2482 1.0424 0.046 Uiso 1 1 calc R . . H32B H 1.0669 0.2801 1.0742 0.046 Uiso 1 1 calc R . . H32C H 1.0167 0.1756 1.0408 0.046 Uiso 1 1 calc R . . C322 C 0.8415(3) 0.4315(2) 0.6944(2) 0.0333(7) Uani 1 1 d . . . H32D H 0.8354 0.3734 0.7073 0.040 Uiso 1 1 calc R . . H32E H 0.9198 0.4611 0.7199 0.040 Uiso 1 1 calc R . . H32F H 0.8153 0.4225 0.6283 0.040 Uiso 1 1 calc R . . C323 C 1.1096(3) 0.2158(2) 0.9182(3) 0.0378(8) Uani 1 1 d . . . H32G H 1.1276 0.1597 0.9315 0.045 Uiso 1 1 calc R . . H32H H 1.1683 0.2654 0.9595 0.045 Uiso 1 1 calc R . . H32I H 1.1047 0.2120 0.8550 0.045 Uiso 1 1 calc R . . C4 C 0.3875(2) 0.13898(18) 0.92691(19) 0.0213(5) Uani 1 1 d . . . C41 C 0.3319(2) 0.0769(2) 0.9535(2) 0.0257(6) Uani 1 1 d . . . H41 H 0.3383 0.0955 1.0181 0.031 Uiso 1 1 calc R . . C42 C 0.2607(3) -0.0171(2) 0.9009(2) 0.0300(7) Uani 1 1 d . . . C421 C 0.1877(3) -0.0226(2) 0.8021(2) 0.0360(7) Uani 1 1 d . . . H42A H 0.2364 -0.0119 0.7669 0.043 Uiso 1 1 calc R . . H42B H 0.1387 0.0227 0.8039 0.043 Uiso 1 1 calc R . . H42C H 0.1421 -0.0822 0.7733 0.043 Uiso 1 1 calc R . . C422 C 0.1807(3) -0.0366(2) 0.9552(3) 0.0451(9) Uani 1 1 d . . . H42D H 0.1337 -0.0953 0.9237 0.054 Uiso 1 1 calc R . . H42E H 0.1331 0.0096 0.9590 0.054 Uiso 1 1 calc R . . H42F H 0.2256 -0.0363 1.0168 0.054 Uiso 1 1 calc R . . C423 C 0.3385(3) -0.0893(2) 0.9000(3) 0.0418(8) Uani 1 1 d . . . H42G H 0.3849 -0.0815 0.8622 0.050 Uiso 1 1 calc R . . H42H H 0.2928 -0.1490 0.8749 0.050 Uiso 1 1 calc R . . H42I H 0.3867 -0.0828 0.9624 0.050 Uiso 1 1 calc R . . C5 C 0.3164(2) 0.24459(19) 0.63922(19) 0.0227(6) Uani 1 1 d . . . C51 C 0.2056(2) 0.2438(2) 0.5944(2) 0.0270(6) Uani 1 1 d . . . H51 H 0.1935 0.2923 0.5653 0.032 Uiso 1 1 calc R . . C52 C 0.0957(3) 0.1827(2) 0.5799(2) 0.0302(7) Uani 1 1 d . . . C521 C 0.0288(3) 0.1573(3) 0.4755(2) 0.0452(9) Uani 1 1 d . . . H52A H 0.0184 0.2120 0.4565 0.054 Uiso 1 1 calc R . . H52B H -0.0445 0.1223 0.4635 0.054 Uiso 1 1 calc R . . H52C H 0.0705 0.1218 0.4412 0.054 Uiso 1 1 calc R . . C522 C 0.0273(3) 0.2388(3) 0.6329(3) 0.0570(11) Uani 1 1 d . . . H52D H 0.0671 0.2537 0.6985 0.068 Uiso 1 1 calc R . . H52E H -0.0466 0.2039 0.6188 0.068 Uiso 1 1 calc R . . H52F H 0.0187 0.2940 0.6147 0.068 Uiso 1 1 calc R . . C523 C 0.1095(3) 0.0958(3) 0.6092(3) 0.0545(11) Uani 1 1 d . . . H52G H 0.1519 0.0601 0.5757 0.065 Uiso 1 1 calc R . . H52H H 0.0356 0.0612 0.5958 0.065 Uiso 1 1 calc R . . H52I H 0.1499 0.1110 0.6748 0.065 Uiso 1 1 calc R . . C6 C 0.5475(2) -0.00538(18) 0.67880(19) 0.0205(5) Uani 1 1 d . . . C61 C 0.5094(2) -0.08575(19) 0.6131(2) 0.0242(6) Uani 1 1 d . . . H61 H 0.5689 -0.1169 0.5993 0.029 Uiso 1 1 calc R . . C62 C 0.3893(3) -0.1367(2) 0.5566(2) 0.0278(6) Uani 1 1 d . . . C621 C 0.3123(3) -0.1358(3) 0.6167(2) 0.0428(9) Uani 1 1 d . . . H62A H 0.3478 -0.1589 0.6681 0.051 Uiso 1 1 calc R . . H62B H 0.2400 -0.1736 0.5800 0.051 Uiso 1 1 calc R . . H62C H 0.3007 -0.0744 0.6397 0.051 Uiso 1 1 calc R . . C622 C 0.3356(3) -0.0945(2) 0.4785(2) 0.0406(8) Uani 1 1 d . . . H62D H 0.3248 -0.0336 0.5048 0.049 Uiso 1 1 calc R . . H62E H 0.2631 -0.1308 0.4397 0.049 Uiso 1 1 calc R . . H62F H 0.3852 -0.0925 0.4419 0.049 Uiso 1 1 calc R . . C623 C 0.3988(3) -0.2350(2) 0.5137(3) 0.0511(10) Uani 1 1 d . . . H62G H 0.4435 -0.2362 0.4730 0.061 Uiso 1 1 calc R . . H62H H 0.3238 -0.2692 0.4789 0.061 Uiso 1 1 calc R . . H62I H 0.4349 -0.2616 0.5621 0.061 Uiso 1 1 calc R . . CH1 C -0.0203(8) 0.4679(5) 0.4574(4) 0.139(3) Uani 1 1 d . . . HH1A H -0.0692 0.5012 0.4221 0.167 Uiso 1 1 calc R . . HH1B H 0.0464 0.4705 0.4385 0.167 Uiso 1 1 calc R . . CH2 C -0.0693(9) 0.3860(6) 0.4113(7) 0.197(6) Uani 1 1 d . . . HH2A H -0.1433 0.3864 0.4188 0.236 Uiso 1 1 calc R . . HH2B H -0.0311 0.3524 0.4523 0.236 Uiso 1 1 calc R . . CH3 C -0.0963(7) 0.3211(5) 0.3250(5) 0.130(3) Uani 1 1 d . . . HH3A H -0.1272 0.3488 0.2762 0.157 Uiso 1 1 calc R . . HH3B H -0.1517 0.2715 0.3211 0.157 Uiso 1 1 calc R . . HH3C H -0.0285 0.2984 0.3184 0.157 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 0.02357(16) 0.02611(17) 0.02144(16) 0.00396(13) 0.01095(13) -0.00124(12) C111 0.0365(18) 0.0375(18) 0.0322(17) 0.0064(14) 0.0184(14) -0.0009(14) C112 0.060(3) 0.073(3) 0.039(2) 0.021(2) 0.0185(19) 0.015(2) Ga2 0.01972(16) 0.02420(17) 0.02215(16) 0.01034(13) 0.00080(12) 0.00001(12) C211 0.0323(18) 0.048(2) 0.041(2) 0.0285(17) -0.0021(15) -0.0014(15) C212 0.054(3) 0.069(3) 0.077(3) 0.052(3) 0.024(2) 0.031(2) Ga3 0.01834(15) 0.01987(16) 0.02788(17) -0.00016(12) 0.00611(12) 0.00301(12) C311 0.0263(17) 0.038(2) 0.073(3) -0.0174(19) 0.0082(17) 0.0094(15) C312 0.111(5) 0.080(4) 0.224(9) 0.072(5) 0.065(5) 0.070(4) C101 0.0152(12) 0.0193(13) 0.0183(13) 0.0017(10) 0.0047(10) -0.0034(10) C102 0.0172(12) 0.0179(12) 0.0201(13) 0.0048(10) 0.0050(10) 0.0032(10) C103 0.0175(12) 0.0185(13) 0.0177(12) 0.0053(10) 0.0033(10) -0.0014(10) C104 0.0164(12) 0.0206(13) 0.0174(12) 0.0014(10) 0.0049(10) -0.0019(10) C105 0.0148(12) 0.0167(12) 0.0182(12) 0.0018(10) 0.0033(10) -0.0022(9) C106 0.0185(13) 0.0194(13) 0.0203(13) 0.0071(10) 0.0046(10) 0.0013(10) C201 0.0145(12) 0.0194(13) 0.0238(14) 0.0026(11) 0.0065(10) -0.0041(10) C202 0.0166(12) 0.0176(12) 0.0234(13) 0.0020(10) 0.0073(10) -0.0001(10) C203 0.0157(12) 0.0172(12) 0.0214(13) 0.0036(10) 0.0033(10) -0.0023(10) C204 0.0197(13) 0.0207(13) 0.0208(13) 0.0038(11) 0.0058(10) -0.0007(10) C205 0.0152(12) 0.0163(12) 0.0219(13) 0.0015(10) 0.0037(10) -0.0023(10) C206 0.0188(13) 0.0191(13) 0.0226(13) 0.0072(11) 0.0055(11) 0.0001(10) C1 0.0223(13) 0.0251(14) 0.0198(13) 0.0080(11) 0.0087(11) 0.0042(11) C11 0.0260(14) 0.0273(15) 0.0256(15) 0.0079(12) 0.0136(12) 0.0047(12) C12 0.0284(15) 0.0212(14) 0.0285(15) -0.0008(12) 0.0124(12) -0.0024(11) C121 0.0252(16) 0.0328(18) 0.052(2) -0.0009(16) 0.0068(15) -0.0048(14) C122 0.040(2) 0.0348(19) 0.065(3) 0.0177(18) 0.0258(19) 0.0036(15) C123 0.073(3) 0.050(2) 0.034(2) -0.0129(17) 0.0199(19) -0.026(2) C2 0.0205(13) 0.0219(13) 0.0182(13) 0.0055(11) 0.0041(10) 0.0034(10) C21 0.0225(14) 0.0254(14) 0.0179(13) 0.0068(11) 0.0027(11) 0.0042(11) C22 0.0243(14) 0.0263(15) 0.0228(14) 0.0091(12) 0.0046(11) 0.0004(11) C221 0.0351(18) 0.0336(17) 0.0350(18) 0.0146(14) 0.0080(14) -0.0058(14) C222 0.0274(15) 0.0281(15) 0.0239(15) 0.0085(12) 0.0027(12) -0.0030(12) C223 0.0249(15) 0.0241(15) 0.0362(17) 0.0064(13) 0.0068(13) -0.0023(12) C3 0.0207(13) 0.0214(13) 0.0219(13) 0.0073(11) 0.0086(11) 0.0041(10) C31 0.0235(14) 0.0184(13) 0.0280(15) 0.0038(11) 0.0090(12) 0.0035(11) C32 0.0177(13) 0.0237(14) 0.0283(15) 0.0063(12) 0.0046(11) 0.0010(11) C321 0.0368(18) 0.0364(18) 0.0313(17) 0.0098(14) 0.0014(14) -0.0121(14) C322 0.0238(15) 0.0408(19) 0.0334(17) 0.0088(14) 0.0093(13) -0.0002(13) C323 0.0190(15) 0.0335(18) 0.057(2) 0.0102(16) 0.0104(14) 0.0003(13) C4 0.0171(12) 0.0220(13) 0.0243(14) 0.0063(11) 0.0064(11) 0.0019(10) C41 0.0242(14) 0.0292(15) 0.0284(15) 0.0107(12) 0.0133(12) 0.0048(12) C42 0.0299(16) 0.0263(15) 0.0365(17) 0.0101(13) 0.0149(13) -0.0004(12) C421 0.0310(17) 0.0307(17) 0.0403(19) 0.0079(14) 0.0073(14) -0.0050(13) C422 0.047(2) 0.039(2) 0.060(2) 0.0212(18) 0.0309(19) -0.0043(16) C423 0.042(2) 0.0302(18) 0.057(2) 0.0187(16) 0.0159(17) 0.0089(15) C5 0.0207(13) 0.0221(14) 0.0237(14) 0.0063(11) 0.0052(11) 0.0023(11) C51 0.0256(15) 0.0233(14) 0.0292(16) 0.0090(12) 0.0038(12) 0.0032(12) C52 0.0222(15) 0.0280(16) 0.0344(17) 0.0073(13) 0.0032(12) -0.0026(12) C521 0.0336(19) 0.046(2) 0.042(2) 0.0102(17) -0.0042(15) -0.0026(16) C522 0.038(2) 0.059(3) 0.063(3) -0.006(2) 0.0244(19) -0.0112(18) C523 0.0307(19) 0.043(2) 0.074(3) 0.028(2) -0.0102(18) -0.0156(16) C6 0.0201(13) 0.0209(13) 0.0208(13) 0.0064(11) 0.0069(10) 0.0027(10) C61 0.0216(14) 0.0232(14) 0.0276(15) 0.0055(12) 0.0087(11) 0.0046(11) C62 0.0267(15) 0.0233(15) 0.0263(15) 0.0009(12) 0.0041(12) 0.0001(12) C621 0.0296(18) 0.053(2) 0.0337(19) 0.0055(16) 0.0028(14) -0.0134(16) C622 0.0323(18) 0.046(2) 0.0351(19) 0.0101(16) 0.0019(14) -0.0032(15) C623 0.044(2) 0.0308(19) 0.057(3) -0.0090(17) 0.0042(18) -0.0016(16) CH1 0.177(8) 0.125(8) 0.099(6) 0.062(5) -0.003(6) 0.022(7) CH2 0.247(13) 0.083(6) 0.186(11) 0.026(6) -0.034(9) 0.053(7) CH3 0.176(8) 0.107(6) 0.137(7) 0.076(6) 0.055(6) 0.032(6) _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 1.958(3) . ? Ga1 C4 1.958(3) . ? Ga1 C111 1.968(3) . ? C111 C112 1.504(5) . ? C111 H11A 0.9600 . ? C111 H11B 0.9600 . ? C112 H11C 0.9599 . ? C112 H11D 0.9599 . ? C112 H11E 0.9599 . ? Ga2 C211 1.969(3) . ? Ga2 C2 1.965(3) . ? Ga2 C5 1.971(3) . ? C211 C212 1.511(5) . ? C211 H21A 0.9600 . ? C211 H21B 0.9600 . ? C212 H21C 0.9599 . ? C212 H21D 0.9599 . ? C212 H21E 0.9599 . ? Ga3 C6 1.962(3) . ? Ga3 C3 1.965(3) . ? Ga3 C311 1.969(3) . ? C311 C312 1.486(7) . ? C311 H31A 0.9600 . ? C311 H31B 0.9600 . ? C312 H31C 0.9599 . ? C312 H31D 0.9599 . ? C312 H31E 0.9599 . ? C101 C102 1.395(4) . ? C101 C106 1.404(4) . ? C101 C1 1.487(4) . ? C102 C103 1.396(4) . ? C102 H102 0.9600 . ? C103 C104 1.388(4) . ? C103 C2 1.485(4) . ? C104 C105 1.396(4) . ? C104 H104 0.9600 . ? C105 C106 1.389(4) . ? C105 C3 1.483(4) . ? C106 H106 0.9600 . ? C201 C202 1.395(4) . ? C201 C206 1.393(4) . ? C201 C4 1.490(4) . ? C202 C203 1.391(4) . ? C202 H202 0.9600 . ? C203 C204 1.396(4) . ? C203 C5 1.487(4) . ? C204 C205 1.395(4) . ? C204 H204 0.9600 . ? C205 C206 1.391(4) . ? C205 C6 1.490(4) . ? C206 H206 0.9600 . ? C1 C11 1.337(4) . ? C11 C12 1.521(4) . ? C11 H11 0.9600 . ? C12 C121 1.524(4) . ? C12 C123 1.528(4) . ? C12 C122 1.530(5) . ? C121 H12A 0.9599 . ? C121 H12B 0.9599 . ? C121 H12C 0.9599 . ? C122 H12D 0.9599 . ? C122 H12E 0.9599 . ? C122 H12F 0.9599 . ? C123 H12G 0.9599 . ? C123 H12H 0.9599 . ? C123 H12I 0.9599 . ? C2 C21 1.344(4) . ? C21 C22 1.526(4) . ? C21 H21 0.9600 . ? C22 C322 1.522(4) . ? C22 C222 1.529(4) . ? C22 C221 1.535(4) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C222 H22D 0.9599 . ? C222 H22E 0.9599 . ? C222 H22F 0.9599 . ? C223 C32 1.525(4) . ? C223 H22G 0.9599 . ? C223 H22H 0.9599 . ? C223 H22I 0.9599 . ? C3 C31 1.353(4) . ? C31 C32 1.514(4) . ? C31 H31 0.9600 . ? C32 C323 1.524(4) . ? C32 C321 1.533(4) . ? C321 H32A 0.9599 . ? C321 H32B 0.9599 . ? C321 H32C 0.9599 . ? C322 H32D 0.9599 . ? C322 H32E 0.9599 . ? C322 H32F 0.9599 . ? C323 H32G 0.9599 . ? C323 H32H 0.9599 . ? C323 H32I 0.9599 . ? C4 C41 1.344(4) . ? C41 C42 1.523(4) . ? C41 H41 0.9600 . ? C42 C423 1.525(4) . ? C42 C421 1.523(4) . ? C42 C422 1.541(4) . ? C421 H42A 0.9599 . ? C421 H42B 0.9599 . ? C421 H42C 0.9599 . ? C422 H42D 0.9599 . ? C422 H42E 0.9599 . ? C422 H42F 0.9599 . ? C423 H42G 0.9599 . ? C423 H42H 0.9599 . ? C423 H42I 0.9599 . ? C5 C51 1.344(4) . ? C51 C52 1.515(4) . ? C51 H51 0.9600 . ? C52 C523 1.515(5) . ? C52 C522 1.528(5) . ? C52 C521 1.534(4) . ? C521 H52A 0.9599 . ? C521 H52B 0.9599 . ? C521 H52C 0.9599 . ? C522 H52D 0.9599 . ? C522 H52E 0.9599 . ? C522 H52F 0.9599 . ? C523 H52G 0.9599 . ? C523 H52H 0.9599 . ? C523 H52I 0.9599 . ? C6 C61 1.342(4) . ? C61 C62 1.521(4) . ? C61 H61 0.9600 . ? C62 C623 1.520(4) . ? C62 C622 1.526(4) . ? C62 C621 1.526(4) . ? C621 H62A 0.9599 . ? C621 H62B 0.9599 . ? C621 H62C 0.9599 . ? C622 H62D 0.9599 . ? C622 H62E 0.9599 . ? C622 H62F 0.9599 . ? C623 H62G 0.9599 . ? C623 H62H 0.9599 . ? C623 H62I 0.9599 . ? CH1 CH2 1.281(10) . ? CH1 CH1 1.373(14) 2_566 ? CH1 HH1A 0.9600 . ? CH1 HH1B 0.9600 . ? CH2 CH3 1.398(10) . ? CH2 HH2A 0.9600 . ? CH2 HH2B 0.9600 . ? CH3 HH3A 0.9599 . ? CH3 HH3B 0.9599 . ? CH3 HH3C 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 C4 123.32(11) . . ? C1 Ga1 C111 118.00(13) . . ? C4 Ga1 C111 118.67(13) . . ? C112 C111 Ga1 114.7(3) . . ? C112 C111 H11A 108.6 . . ? Ga1 C111 H11A 108.6 . . ? C112 C111 H11B 108.6 . . ? Ga1 C111 H11B 108.6 . . ? H11A C111 H11B 107.6 . . ? C111 C112 H11C 109.5 . . ? C111 C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? C111 C112 H11E 109.5 . . ? H11C C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C211 Ga2 C2 117.19(13) . . ? C211 Ga2 C5 119.06(13) . . ? C2 Ga2 C5 123.75(11) . . ? C212 C211 Ga2 115.9(3) . . ? C212 C211 H21A 108.3 . . ? Ga2 C211 H21A 108.3 . . ? C212 C211 H21B 108.3 . . ? Ga2 C211 H21B 108.3 . . ? H21A C211 H21B 107.4 . . ? C211 C212 H21C 109.5 . . ? C211 C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? C211 C212 H21E 109.5 . . ? H21C C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C6 Ga3 C3 123.64(11) . . ? C6 Ga3 C311 117.90(14) . . ? C3 Ga3 C311 118.45(13) . . ? C312 C311 Ga3 114.5(4) . . ? C312 C311 H31A 108.6 . . ? Ga3 C311 H31A 108.6 . . ? C312 C311 H31B 108.6 . . ? Ga3 C311 H31B 108.6 . . ? H31A C311 H31B 107.6 . . ? C311 C312 H31C 109.5 . . ? C311 C312 H31D 109.5 . . ? H31C C312 H31D 109.5 . . ? C311 C312 H31E 109.5 . . ? H31C C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C102 C101 C106 118.3(2) . . ? C102 C101 C1 120.4(2) . . ? C106 C101 C1 121.1(2) . . ? C103 C102 C101 121.6(2) . . ? C103 C102 H102 119.2 . . ? C101 C102 H102 119.2 . . ? C104 C103 C102 118.3(2) . . ? C104 C103 C2 120.8(2) . . ? C102 C103 C2 120.7(2) . . ? C103 C104 C105 121.9(2) . . ? C103 C104 H104 119.0 . . ? C105 C104 H104 119.0 . . ? C106 C105 C104 118.4(2) . . ? C106 C105 C3 121.9(2) . . ? C104 C105 C3 119.6(2) . . ? C105 C106 C101 121.4(2) . . ? C105 C106 H106 119.3 . . ? C101 C106 H106 119.3 . . ? C202 C201 C206 118.3(2) . . ? C202 C201 C4 120.1(2) . . ? C206 C201 C4 121.4(2) . . ? C203 C202 C201 121.9(2) . . ? C203 C202 H202 119.0 . . ? C201 C202 H202 119.0 . . ? C202 C203 C204 118.0(2) . . ? C202 C203 C5 121.8(2) . . ? C204 C203 C5 120.1(2) . . ? C203 C204 C205 121.7(3) . . ? C203 C204 H204 119.1 . . ? C205 C204 H204 119.1 . . ? C206 C205 C204 118.5(2) . . ? C206 C205 C6 119.8(2) . . ? C204 C205 C6 121.5(2) . . ? C205 C206 C201 121.5(2) . . ? C205 C206 H206 119.3 . . ? C201 C206 H206 119.3 . . ? C11 C1 C101 125.2(3) . . ? C11 C1 Ga1 114.5(2) . . ? C101 C1 Ga1 120.19(19) . . ? C1 C11 C12 131.8(3) . . ? C1 C11 H11 114.1 . . ? C12 C11 H11 114.1 . . ? C121 C12 C11 113.0(2) . . ? C121 C12 C123 108.8(3) . . ? C11 C12 C123 107.6(3) . . ? C121 C12 C122 108.9(3) . . ? C11 C12 C122 110.0(3) . . ? C123 C12 C122 108.5(3) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C12 C122 H12D 109.5 . . ? C12 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C12 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C12 C123 H12G 109.5 . . ? C12 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C12 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C21 C2 C103 125.7(2) . . ? C21 C2 Ga2 115.8(2) . . ? C103 C2 Ga2 118.43(19) . . ? C2 C21 C22 131.4(3) . . ? C2 C21 H21 114.3 . . ? C22 C21 H21 114.3 . . ? C322 C22 C21 108.7(2) . . ? C322 C22 C222 109.7(2) . . ? C21 C22 C222 113.5(2) . . ? C322 C22 C221 109.3(3) . . ? C21 C22 C221 107.6(2) . . ? C222 C22 C221 107.9(2) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 C222 H22D 109.5 . . ? C22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C32 C223 H22G 109.5 . . ? C32 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C32 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C31 C3 C105 124.7(2) . . ? C31 C3 Ga3 115.3(2) . . ? C105 C3 Ga3 119.99(19) . . ? C3 C31 C32 131.8(3) . . ? C3 C31 H31 114.1 . . ? C32 C31 H31 114.1 . . ? C31 C32 C223 113.5(2) . . ? C31 C32 C323 107.7(2) . . ? C223 C32 C323 108.1(2) . . ? C31 C32 C321 109.3(2) . . ? C223 C32 C321 109.8(3) . . ? C323 C32 C321 108.3(3) . . ? C32 C321 H32A 109.5 . . ? C32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? C32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? C22 C322 H32D 109.5 . . ? C22 C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? C22 C322 H32F 109.5 . . ? H32D C322 H32F 109.5 . . ? H32E C322 H32F 109.5 . . ? C32 C323 H32G 109.5 . . ? C32 C323 H32H 109.5 . . ? H32G C323 H32H 109.5 . . ? C32 C323 H32I 109.5 . . ? H32G C323 H32I 109.5 . . ? H32H C323 H32I 109.5 . . ? C41 C4 C201 126.3(3) . . ? C41 C4 Ga1 115.2(2) . . ? C201 C4 Ga1 118.54(18) . . ? C4 C41 C42 132.4(3) . . ? C4 C41 H41 113.8 . . ? C42 C41 H41 113.8 . . ? C423 C42 C421 110.5(3) . . ? C423 C42 C41 109.8(3) . . ? C421 C42 C41 113.0(2) . . ? C423 C42 C422 108.0(3) . . ? C421 C42 C422 108.4(3) . . ? C41 C42 C422 107.0(3) . . ? C42 C421 H42A 109.5 . . ? C42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? C42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? C42 C422 H42D 109.5 . . ? C42 C422 H42E 109.5 . . ? H42D C422 H42E 109.5 . . ? C42 C422 H42F 109.5 . . ? H42D C422 H42F 109.5 . . ? H42E C422 H42F 109.5 . . ? C42 C423 H42G 109.5 . . ? C42 C423 H42H 109.5 . . ? H42G C423 H42H 109.5 . . ? C42 C423 H42I 109.5 . . ? H42G C423 H42I 109.5 . . ? H42H C423 H42I 109.5 . . ? C51 C5 C203 126.1(3) . . ? C51 C5 Ga2 114.0(2) . . ? C203 C5 Ga2 119.86(19) . . ? C5 C51 C52 133.7(3) . . ? C5 C51 H51 113.1 . . ? C52 C51 H51 113.1 . . ? C51 C52 C523 115.8(3) . . ? C51 C52 C522 107.9(3) . . ? C523 C52 C522 109.2(3) . . ? C51 C52 C521 106.4(3) . . ? C523 C52 C521 108.9(3) . . ? C522 C52 C521 108.5(3) . . ? C52 C521 H52A 109.5 . . ? C52 C521 H52B 109.5 . . ? H52A C521 H52B 109.5 . . ? C52 C521 H52C 109.5 . . ? H52A C521 H52C 109.5 . . ? H52B C521 H52C 109.5 . . ? C52 C522 H52D 109.5 . . ? C52 C522 H52E 109.5 . . ? H52D C522 H52E 109.5 . . ? C52 C522 H52F 109.5 . . ? H52D C522 H52F 109.5 . . ? H52E C522 H52F 109.5 . . ? C52 C523 H52G 109.5 . . ? C52 C523 H52H 109.5 . . ? H52G C523 H52H 109.5 . . ? C52 C523 H52I 109.5 . . ? H52G C523 H52I 109.5 . . ? H52H C523 H52I 109.5 . . ? C61 C6 C205 124.9(2) . . ? C61 C6 Ga3 115.9(2) . . ? C205 C6 Ga3 119.16(19) . . ? C6 C61 C62 131.9(3) . . ? C6 C61 H61 114.0 . . ? C62 C61 H61 114.0 . . ? C61 C62 C623 107.8(3) . . ? C61 C62 C622 110.3(3) . . ? C623 C62 C622 108.7(3) . . ? C61 C62 C621 111.9(2) . . ? C623 C62 C621 109.1(3) . . ? C622 C62 C621 109.0(3) . . ? C62 C621 H62A 109.5 . . ? C62 C621 H62B 109.5 . . ? H62A C621 H62B 109.5 . . ? C62 C621 H62C 109.5 . . ? H62A C621 H62C 109.5 . . ? H62B C621 H62C 109.5 . . ? C62 C622 H62D 109.5 . . ? C62 C622 H62E 109.5 . . ? H62D C622 H62E 109.5 . . ? C62 C622 H62F 109.5 . . ? H62D C622 H62F 109.5 . . ? H62E C622 H62F 109.5 . . ? C62 C623 H62G 109.5 . . ? C62 C623 H62H 109.5 . . ? H62G C623 H62H 109.5 . . ? C62 C623 H62I 109.5 . . ? H62G C623 H62I 109.5 . . ? H62H C623 H62I 109.5 . . ? CH2 CH1 CH1 147.2(12) . 2_566 ? CH2 CH1 HH1A 100.0 . . ? CH1 CH1 HH1A 100.0 2_566 . ? CH2 CH1 HH1B 100.0 . . ? CH1 CH1 HH1B 100.0 2_566 . ? HH1A CH1 HH1B 104.2 . . ? CH1 CH2 CH3 143.7(12) . . ? CH1 CH2 HH2A 101.0 . . ? CH3 CH2 HH2A 101.0 . . ? CH1 CH2 HH2B 101.0 . . ? CH3 CH2 HH2B 101.0 . . ? HH2A CH2 HH2B 104.5 . . ? CH2 CH3 HH3A 109.5 . . ? CH2 CH3 HH3B 109.5 . . ? HH3A CH3 HH3B 109.5 . . ? CH2 CH3 HH3C 109.5 . . ? HH3A CH3 HH3C 109.5 . . ? HH3B CH3 HH3C 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 C1 Ga1 C111 C112 -82.0(3) . . . . ? C4 Ga1 C111 C112 96.9(3) . . . . ? C2 Ga2 C211 C212 -59.4(3) . . . . ? C5 Ga2 C211 C212 120.9(3) . . . . ? C6 Ga3 C311 C312 -82.8(4) . . . . ? C3 Ga3 C311 C312 95.8(4) . . . . ? C106 C101 C102 C103 -0.6(4) . . . . ? C1 C101 C102 C103 -175.3(2) . . . . ? C101 C102 C103 C104 0.8(4) . . . . ? C101 C102 C103 C2 176.4(2) . . . . ? C102 C103 C104 C105 -1.6(4) . . . . ? C2 C103 C104 C105 -177.2(2) . . . . ? C103 C104 C105 C106 2.0(4) . . . . ? C103 C104 C105 C3 179.0(2) . . . . ? C104 C105 C106 C101 -1.8(4) . . . . ? C3 C105 C106 C101 -178.7(2) . . . . ? C102 C101 C106 C105 1.1(4) . . . . ? C1 C101 C106 C105 175.8(2) . . . . ? C206 C201 C202 C203 2.3(4) . . . . ? C4 C201 C202 C203 177.4(2) . . . . ? C201 C202 C203 C204 -1.3(4) . . . . ? C201 C202 C203 C5 -177.7(2) . . . . ? C202 C203 C204 C205 0.7(4) . . . . ? C5 C203 C204 C205 177.1(2) . . . . ? C203 C204 C205 C206 -1.0(4) . . . . ? C203 C204 C205 C6 -175.0(2) . . . . ? C204 C205 C206 C201 1.9(4) . . . . ? C6 C205 C206 C201 176.1(2) . . . . ? C202 C201 C206 C205 -2.6(4) . . . . ? C4 C201 C206 C205 -177.6(2) . . . . ? C102 C101 C1 C11 -77.3(4) . . . . ? C106 C101 C1 C11 108.1(3) . . . . ? C102 C101 C1 Ga1 100.2(3) . . . . ? C106 C101 C1 Ga1 -74.4(3) . . . . ? C4 Ga1 C1 C11 -179.2(2) . . . . ? C111 Ga1 C1 C11 -0.4(3) . . . . ? C4 Ga1 C1 C101 3.0(3) . . . . ? C111 Ga1 C1 C101 -178.1(2) . . . . ? C101 C1 C11 C12 -4.3(5) . . . . ? Ga1 C1 C11 C12 178.0(3) . . . . ? C1 C11 C12 C121 -40.6(5) . . . . ? C1 C11 C12 C123 -160.7(3) . . . . ? C1 C11 C12 C122 81.3(4) . . . . ? C104 C103 C2 C21 -76.9(4) . . . . ? C102 C103 C2 C21 107.6(3) . . . . ? C104 C103 C2 Ga2 99.4(3) . . . . ? C102 C103 C2 Ga2 -76.1(3) . . . . ? C211 Ga2 C2 C21 -6.2(3) . . . . ? C5 Ga2 C2 C21 173.5(2) . . . . ? C211 Ga2 C2 C103 177.2(2) . . . . ? C5 Ga2 C2 C103 -3.1(3) . . . . ? C103 C2 C21 C22 -3.0(5) . . . . ? Ga2 C2 C21 C22 -179.4(2) . . . . ? C2 C21 C22 C322 87.5(4) . . . . ? C2 C21 C22 C222 -34.9(4) . . . . ? C2 C21 C22 C221 -154.3(3) . . . . ? C106 C105 C3 C31 -78.9(4) . . . . ? C104 C105 C3 C31 104.2(3) . . . . ? C106 C105 C3 Ga3 103.9(3) . . . . ? C104 C105 C3 Ga3 -73.0(3) . . . . ? C6 Ga3 C3 C31 172.6(2) . . . . ? C311 Ga3 C3 C31 -6.0(3) . . . . ? C6 Ga3 C3 C105 -10.0(3) . . . . ? C311 Ga3 C3 C105 171.4(2) . . . . ? C105 C3 C31 C32 -1.5(5) . . . . ? Ga3 C3 C31 C32 175.8(2) . . . . ? C3 C31 C32 C223 -35.0(4) . . . . ? C3 C31 C32 C323 -154.7(3) . . . . ? C3 C31 C32 C321 87.9(4) . . . . ? C202 C201 C4 C41 117.1(3) . . . . ? C206 C201 C4 C41 -67.9(4) . . . . ? C202 C201 C4 Ga1 -63.9(3) . . . . ? C206 C201 C4 Ga1 111.1(3) . . . . ? C1 Ga1 C4 C41 158.3(2) . . . . ? C111 Ga1 C4 C41 -20.6(3) . . . . ? C1 Ga1 C4 C201 -20.8(3) . . . . ? C111 Ga1 C4 C201 160.3(2) . . . . ? C201 C4 C41 C42 -2.9(5) . . . . ? Ga1 C4 C41 C42 178.1(3) . . . . ? C4 C41 C42 C423 86.3(4) . . . . ? C4 C41 C42 C421 -37.5(5) . . . . ? C4 C41 C42 C422 -156.8(3) . . . . ? C202 C203 C5 C51 -73.3(4) . . . . ? C204 C203 C5 C51 110.5(3) . . . . ? C202 C203 C5 Ga2 104.6(3) . . . . ? C204 C203 C5 Ga2 -71.6(3) . . . . ? C211 Ga2 C5 C51 -15.8(3) . . . . ? C2 Ga2 C5 C51 164.5(2) . . . . ? C211 Ga2 C5 C203 166.1(2) . . . . ? C2 Ga2 C5 C203 -13.6(3) . . . . ? C203 C5 C51 C52 -2.1(5) . . . . ? Ga2 C5 C51 C52 179.9(3) . . . . ? C5 C51 C52 C523 -10.2(5) . . . . ? C5 C51 C52 C522 112.5(4) . . . . ? C5 C51 C52 C521 -131.3(4) . . . . ? C206 C205 C6 C61 106.3(3) . . . . ? C204 C205 C6 C61 -79.8(4) . . . . ? C206 C205 C6 Ga3 -73.4(3) . . . . ? C204 C205 C6 Ga3 100.5(3) . . . . ? C3 Ga3 C6 C61 175.0(2) . . . . ? C311 Ga3 C6 C61 -6.5(3) . . . . ? C3 Ga3 C6 C205 -5.3(3) . . . . ? C311 Ga3 C6 C205 173.3(2) . . . . ? C205 C6 C61 C62 -2.2(5) . . . . ? Ga3 C6 C61 C62 177.6(3) . . . . ? C6 C61 C62 C623 -164.1(3) . . . . ? C6 C61 C62 C622 77.3(4) . . . . ? C6 C61 C62 C621 -44.2(5) . . . . ? CH1 CH1 CH2 CH3 -168.7(18) 2_566 . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 31.48 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 1.691 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.094 # Attachment 'Uhl-2b.cif' data_Uhl-2b _database_code_depnum_ccdc_archive 'CCDC 621973' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H123 Ga3' _chemical_formula_weight 1233.89 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' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 17.6535(3) _cell_length_b 17.6535(3) _cell_length_c 25.9914(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7014.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 'all measured' _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 70.07 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 1.619 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8112 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39035 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 70.07 _reflns_number_total 4456 _reflns_number_gt 3096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0683P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4456 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 0.858 _refine_ls_restrained_S_all 0.858 _refine_ls_shift/su_max 0.001 _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 Ga1 Ga 0.46354(2) 0.10670(2) 1.018129(13) 0.01751(11) Uani 1 1 d . . . C1 C 0.49890(18) 0.17299(17) 1.08315(10) 0.0157(5) Uani 1 1 d . . . C11 C 0.44008(18) 0.14081(18) 1.12106(11) 0.0181(6) Uani 1 1 d . . . H11 H 0.3873 0.0881 1.1121 0.022 Uiso 1 1 calc R . . C12 C 0.44085(19) 0.17200(19) 1.17595(11) 0.0215(6) Uani 1 1 d . . . C121 C 0.5317(2) 0.2158(2) 1.20087(11) 0.0298(7) Uani 1 1 d . . . H12A H 0.5567 0.1787 1.1970 0.036 Uiso 1 1 calc R . . H12B H 0.5266 0.2252 1.2368 0.036 Uiso 1 1 calc R . . H12C H 0.5687 0.2710 1.1844 0.036 Uiso 1 1 calc R . . C122 C 0.3793(2) 0.0922(2) 1.20846(12) 0.0319(8) Uani 1 1 d . . . H12D H 0.3218 0.0642 1.1937 0.038 Uiso 1 1 calc R . . H12E H 0.3769 0.1106 1.2429 0.038 Uiso 1 1 calc R . . H12F H 0.4007 0.0518 1.2092 0.038 Uiso 1 1 calc R . . C123 C 0.4055(3) 0.2358(2) 1.17548(13) 0.0389(9) Uani 1 1 d . . . H12G H 0.4447 0.2873 1.1564 0.047 Uiso 1 1 calc R . . H12H H 0.4008 0.2517 1.2102 0.047 Uiso 1 1 calc R . . H12I H 0.3489 0.2082 1.1595 0.047 Uiso 1 1 calc R . . C13 C 0.58534(17) 0.25585(17) 1.08524(10) 0.0150(6) Uani 1 1 d . . . C14 C 0.66273(18) 0.25291(17) 1.08506(10) 0.0160(6) Uani 1 1 d . . . H14 H 0.6600 0.1972 1.0848 0.019 Uiso 1 1 calc R . . C2 C 0.52718(18) 0.15277(18) 0.95290(10) 0.0167(6) Uani 1 1 d . . . C21 C 0.49989(19) 0.09594(18) 0.91350(11) 0.0207(6) Uani 1 1 d . . . H21 H 0.4544 0.0380 0.9222 0.025 Uiso 1 1 calc R . . C22 C 0.5284(2) 0.1072(2) 0.85738(11) 0.0247(7) Uani 1 1 d . . . C221 C 0.6142(2) 0.1061(2) 0.85227(12) 0.0307(7) Uani 1 1 d . . . H22A H 0.6600 0.1560 0.8697 0.037 Uiso 1 1 calc R . . H22B H 0.6289 0.1082 0.8165 0.037 Uiso 1 1 calc R . . H22C H 0.6076 0.0535 0.8674 0.037 Uiso 1 1 calc R . . C222 C 0.5392(2) 0.1914(2) 0.83391(11) 0.0302(7) Uani 1 1 d . . . H22D H 0.4857 0.1925 0.8378 0.036 Uiso 1 1 calc R . . H22E H 0.5531 0.1936 0.7980 0.036 Uiso 1 1 calc R . . H22F H 0.5857 0.2409 0.8512 0.036 Uiso 1 1 calc R . . C223 C 0.4581(3) 0.0296(2) 0.82733(12) 0.0408(9) Uani 1 1 d . . . H22G H 0.4527 -0.0236 0.8406 0.049 Uiso 1 1 calc R . . H22H H 0.4742 0.0356 0.7917 0.049 Uiso 1 1 calc R . . H22I H 0.4033 0.0281 0.8308 0.049 Uiso 1 1 calc R . . C23 C 0.59890(18) 0.24567(17) 0.95042(10) 0.0159(6) Uani 1 1 d . . . C24 C 0.58026(17) 0.31374(18) 0.95083(10) 0.0163(6) Uani 1 1 d . . . H24 H 0.5204 0.3002 0.9514 0.020 Uiso 1 1 calc R . . C3 C 0.35917(19) -0.01154(19) 1.01469(11) 0.0257(7) Uani 1 1 d . . . H3A H 0.3768 -0.0512 1.0015 0.031 Uiso 1 1 calc R . . H3B H 0.3379 -0.0299 1.0490 0.031 Uiso 1 1 calc R . . C31 C 0.2841(2) -0.0197(2) 0.98184(13) 0.0297(7) Uani 1 1 d . . . H31A H 0.2609 0.0138 0.9974 0.036 Uiso 1 1 calc R . . H31B H 0.3062 0.0049 0.9485 0.036 Uiso 1 1 calc R . . C32 C 0.2108(2) -0.1135(2) 0.97533(15) 0.0394(9) Uani 1 1 d . . . H32A H 0.2333 -0.1472 0.9593 0.047 Uiso 1 1 calc R . . H32B H 0.1656 -0.1147 0.9542 0.047 Uiso 1 1 calc R . . H32C H 0.1871 -0.1380 1.0084 0.047 Uiso 1 1 calc R . . CP1 C 0.1580(4) 0.9343(4) 0.1165(2) 0.0856(17) Uani 1 1 d . . . HP1A H 0.1278 0.9205 0.0841 0.103 Uiso 1 1 calc R . . HP1B H 0.2192 0.9728 0.1101 0.103 Uiso 1 1 calc R . . CP2 C 0.1248(4) 0.9761(4) 0.1500(2) 0.095(2) Uani 1 1 d . . . HP2A H 0.0825 0.9856 0.1323 0.114 Uiso 1 1 calc R . . HP2B H 0.1715 1.0315 0.1617 0.114 Uiso 1 1 calc R . . CP3 C 0.0836(6) 0.9154(7) 0.1941(3) 0.144(3) Uani 1 1 d . . . HP3A H 0.0282 0.9101 0.2024 0.172 Uiso 1 1 calc R . . HP3B H 0.1206 0.9363 0.2238 0.172 Uiso 1 1 calc R . . CP4 C 0.0719(5) 0.8304(5) 0.1775(3) 0.123(3) Uani 1 1 d . . . HP4A H 0.0163 0.7953 0.1610 0.148 Uiso 1 1 calc R . . HP4B H 0.0769 0.7985 0.2059 0.148 Uiso 1 1 calc R . . CP5 C 0.1449(6) 0.8570(5) 0.1406(3) 0.126(3) Uani 1 1 d . . . HP5A H 0.1970 0.8676 0.1583 0.152 Uiso 1 1 calc R . . HP5B H 0.1304 0.8119 0.1155 0.152 Uiso 1 1 calc R . . CH1 C 0.0605(17) 0.988(3) -0.0104(6) 0.239(12) Uani 1 1 d . . . HH1A H 0.1081 0.9782 -0.0025 0.286 Uiso 1 1 calc R . . HH1B H 0.0549 0.9889 -0.0470 0.286 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 0.01756(18) 0.01591(19) 0.01457(17) -0.00028(15) -0.00049(15) 0.00499(15) C1 0.0181(13) 0.0165(13) 0.0136(12) -0.0002(11) -0.0019(11) 0.0095(11) C11 0.0185(13) 0.0170(13) 0.0186(13) 0.0018(12) -0.0018(12) 0.0085(11) C12 0.0249(15) 0.0217(14) 0.0184(14) 0.0047(13) 0.0072(13) 0.0120(13) C121 0.0373(18) 0.0323(17) 0.0139(13) -0.0029(14) 0.0012(14) 0.0130(15) C122 0.0384(19) 0.0306(17) 0.0203(15) 0.0042(14) 0.0083(15) 0.0124(15) C123 0.061(2) 0.046(2) 0.0265(16) 0.0046(16) 0.0104(18) 0.040(2) C13 0.0165(13) 0.0174(13) 0.0085(12) -0.0004(11) -0.0003(11) 0.0066(11) C14 0.0200(13) 0.0168(13) 0.0118(12) -0.0003(11) -0.0010(11) 0.0098(11) C2 0.0182(13) 0.0182(14) 0.0139(13) 0.0001(12) -0.0009(12) 0.0094(11) C21 0.0221(14) 0.0175(14) 0.0197(14) 0.0001(12) 0.0016(13) 0.0079(12) C22 0.0319(17) 0.0219(15) 0.0168(14) -0.0034(13) 0.0014(13) 0.0109(13) C221 0.043(2) 0.0328(17) 0.0202(15) 0.0008(14) 0.0087(15) 0.0218(16) C222 0.044(2) 0.0311(17) 0.0170(14) -0.0001(14) 0.0003(14) 0.0200(16) C223 0.049(2) 0.0331(19) 0.0245(16) -0.0082(16) 0.0007(17) 0.0084(17) C23 0.0182(13) 0.0170(14) 0.0101(12) 0.0007(11) 0.0010(11) 0.0071(12) C24 0.0158(13) 0.0200(14) 0.0126(12) -0.0002(11) -0.0008(11) 0.0086(11) C3 0.0257(16) 0.0176(14) 0.0230(15) 0.0006(13) 0.0006(13) 0.0029(13) C31 0.0222(15) 0.0257(16) 0.0353(17) -0.0021(15) -0.0015(15) 0.0076(13) C32 0.0265(17) 0.0310(18) 0.050(2) -0.0143(18) -0.0033(17) 0.0063(15) CP1 0.084(4) 0.086(4) 0.080(4) 0.001(3) 0.018(3) 0.038(4) CP2 0.109(5) 0.105(5) 0.094(5) 0.002(4) 0.008(4) 0.071(4) CP3 0.157(8) 0.205(10) 0.107(6) 0.043(7) 0.073(6) 0.118(8) CP4 0.120(6) 0.078(5) 0.131(7) 0.032(5) 0.029(5) 0.019(4) CP5 0.216(10) 0.131(7) 0.083(4) 0.000(5) 0.014(6) 0.124(7) CH1 0.220(14) 0.53(3) 0.137(13) 0.10(2) 0.040(13) 0.31(2) _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 1.971(3) . ? Ga1 C1 1.971(3) . ? Ga1 C3 1.978(3) . ? C1 C11 1.335(4) . ? C1 C13 1.496(4) . ? C11 C12 1.527(4) . ? C11 H11 0.9600 . ? C12 C123 1.536(4) . ? C12 C122 1.532(4) . ? C12 C121 1.533(4) . ? C121 H12A 0.9599 . ? C121 H12B 0.9599 . ? C121 H12C 0.9599 . ? C122 H12D 0.9599 . ? C122 H12E 0.9599 . ? C122 H12F 0.9599 . ? C123 H12G 0.9599 . ? C123 H12H 0.9599 . ? C123 H12I 0.9599 . ? C13 C14 1.397(3) 3_665 ? C13 C14 1.393(4) . ? C14 C13 1.397(4) 2_655 ? C14 H14 0.9600 . ? C2 C21 1.343(4) . ? C2 C23 1.490(4) . ? C21 C22 1.523(4) . ? C21 H21 0.9600 . ? C22 C223 1.524(4) . ? C22 C221 1.530(4) . ? C22 C222 1.528(4) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C222 H22D 0.9599 . ? C222 H22E 0.9599 . ? C222 H22F 0.9599 . ? C223 H22G 0.9599 . ? C223 H22H 0.9599 . ? C223 H22I 0.9599 . ? C23 C24 1.395(4) 2_655 ? C23 C24 1.396(4) . ? C24 C23 1.395(4) 3_665 ? C24 H24 0.9600 . ? C3 C31 1.522(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C31 C32 1.518(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C32 H32A 0.9599 . ? C32 H32B 0.9599 . ? C32 H32C 0.9599 . ? CP1 CP5 1.411(8) . ? CP1 CP2 1.443(7) . ? CP1 HP1A 0.9600 . ? CP1 HP1B 0.9600 . ? CP2 CP3 1.487(9) . ? CP2 HP2A 0.9600 . ? CP2 HP2B 0.9600 . ? CP3 CP4 1.474(9) . ? CP3 HP3A 0.9600 . ? CP3 HP3B 0.9600 . ? CP4 CP5 1.482(9) . ? CP4 HP4A 0.9600 . ? CP4 HP4B 0.9600 . ? CP5 HP5A 0.9600 . ? CP5 HP5B 0.9600 . ? CH1 CH1 1.306(17) 9_665 ? CH1 CH1 1.306(17) 8_455 ? CH1 HH1A 0.9600 . ? CH1 HH1B 0.9600 . ? 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 123.13(11) . . ? C2 Ga1 C3 115.76(12) . . ? C1 Ga1 C3 121.10(12) . . ? C11 C1 C13 125.8(2) . . ? C11 C1 Ga1 115.6(2) . . ? C13 C1 Ga1 118.49(19) . . ? C1 C11 C12 132.2(3) . . ? C1 C11 H11 113.9 . . ? C12 C11 H11 113.9 . . ? C11 C12 C123 108.9(2) . . ? C11 C12 C122 108.0(2) . . ? C123 C12 C122 108.5(3) . . ? C11 C12 C121 113.3(2) . . ? C123 C12 C121 109.8(3) . . ? C122 C12 C121 108.2(3) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C12 C122 H12D 109.5 . . ? C12 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C12 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C12 C123 H12G 109.5 . . ? C12 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C12 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C14 C13 C14 118.8(3) 3_665 . ? C14 C13 C1 120.9(2) 3_665 . ? C14 C13 C1 120.2(2) . . ? C13 C14 C13 121.2(3) 2_655 . ? C13 C14 H14 119.4 2_655 . ? C13 C14 H14 119.4 . . ? C21 C2 C23 125.4(3) . . ? C21 C2 Ga1 115.5(2) . . ? C23 C2 Ga1 119.13(19) . . ? C2 C21 C22 131.4(3) . . ? C2 C21 H21 114.3 . . ? C22 C21 H21 114.3 . . ? C21 C22 C223 107.8(3) . . ? C21 C22 C221 110.3(3) . . ? C223 C22 C221 108.1(3) . . ? C21 C22 C222 112.4(2) . . ? C223 C22 C222 108.6(3) . . ? C221 C22 C222 109.5(3) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 C222 H22D 109.5 . . ? C22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C22 C223 H22G 109.5 . . ? C22 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C22 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C24 C23 C24 118.6(3) 2_655 . ? C24 C23 C2 120.6(2) 2_655 . ? C24 C23 C2 120.7(3) . . ? C23 C24 C23 121.4(3) 3_665 . ? C23 C24 H24 119.3 3_665 . ? C23 C24 H24 119.3 . . ? C31 C3 Ga1 115.6(2) . . ? C31 C3 H3A 108.4 . . ? Ga1 C3 H3A 108.4 . . ? C31 C3 H3B 108.4 . . ? Ga1 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C32 C31 C3 113.1(3) . . ? C32 C31 H31A 109.0 . . ? C3 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? C3 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? CP5 CP1 CP2 108.4(5) . . ? CP5 CP1 HP1A 110.0 . . ? CP2 CP1 HP1A 110.0 . . ? CP5 CP1 HP1B 110.0 . . ? CP2 CP1 HP1B 110.0 . . ? HP1A CP1 HP1B 108.4 . . ? CP1 CP2 CP3 105.8(6) . . ? CP1 CP2 HP2A 110.6 . . ? CP3 CP2 HP2A 110.6 . . ? CP1 CP2 HP2B 110.6 . . ? CP3 CP2 HP2B 110.6 . . ? HP2A CP2 HP2B 108.7 . . ? CP2 CP3 CP4 106.1(6) . . ? CP2 CP3 HP3A 110.5 . . ? CP4 CP3 HP3A 110.5 . . ? CP2 CP3 HP3B 110.5 . . ? CP4 CP3 HP3B 110.5 . . ? HP3A CP3 HP3B 108.7 . . ? CP3 CP4 CP5 102.1(6) . . ? CP3 CP4 HP4A 111.4 . . ? CP5 CP4 HP4A 111.4 . . ? CP3 CP4 HP4B 111.4 . . ? CP5 CP4 HP4B 111.4 . . ? HP4A CP4 HP4B 109.2 . . ? CP1 CP5 CP4 106.8(6) . . ? CP1 CP5 HP5A 110.4 . . ? CP4 CP5 HP5A 110.4 . . ? CP1 CP5 HP5B 110.4 . . ? CP4 CP5 HP5B 110.4 . . ? HP5A CP5 HP5B 108.6 . . ? CH1 CH1 CH1 104.2(16) 9_665 8_455 ? CH1 CH1 HH1A 110.9 9_665 . ? CH1 CH1 HH1A 110.9 8_455 . ? CH1 CH1 HH1B 110.9 9_665 . ? CH1 CH1 HH1B 110.9 8_455 . ? HH1A CH1 HH1B 108.9 . . ? 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 C2 Ga1 C1 C11 167.06(19) . . . . ? C3 Ga1 C1 C11 -12.1(3) . . . . ? C2 Ga1 C1 C13 -9.8(3) . . . . ? C3 Ga1 C1 C13 170.96(19) . . . . ? C13 C1 C11 C12 -2.5(5) . . . . ? Ga1 C1 C11 C12 -179.1(2) . . . . ? C1 C11 C12 C123 88.3(4) . . . . ? C1 C11 C12 C122 -154.0(3) . . . . ? C1 C11 C12 C121 -34.2(4) . . . . ? C11 C1 C13 C14 -71.1(4) . . . 3_665 ? Ga1 C1 C13 C14 105.5(3) . . . 3_665 ? C11 C1 C13 C14 111.9(3) . . . . ? Ga1 C1 C13 C14 -71.6(3) . . . . ? C14 C13 C14 C13 0.7(5) 3_665 . . 2_655 ? C1 C13 C14 C13 177.83(17) . . . 2_655 ? C1 Ga1 C2 C21 173.4(2) . . . . ? C3 Ga1 C2 C21 -7.3(3) . . . . ? C1 Ga1 C2 C23 -7.6(3) . . . . ? C3 Ga1 C2 C23 171.6(2) . . . . ? C23 C2 C21 C22 -2.3(5) . . . . ? Ga1 C2 C21 C22 176.6(3) . . . . ? C2 C21 C22 C223 -163.7(3) . . . . ? C2 C21 C22 C221 78.4(4) . . . . ? C2 C21 C22 C222 -44.1(5) . . . . ? C21 C2 C23 C24 -77.2(4) . . . 2_655 ? Ga1 C2 C23 C24 104.0(3) . . . 2_655 ? C21 C2 C23 C24 106.8(3) . . . . ? Ga1 C2 C23 C24 -72.1(3) . . . . ? C24 C23 C24 C23 1.5(5) 2_655 . . 3_665 ? C2 C23 C24 C23 177.63(18) . . . 3_665 ? C2 Ga1 C3 C31 -65.1(3) . . . . ? C1 Ga1 C3 C31 114.1(2) . . . . ? Ga1 C3 C31 C32 172.9(2) . . . . ? CP5 CP1 CP2 CP3 -4.8(9) . . . . ? CP1 CP2 CP3 CP4 -15.9(10) . . . . ? CP2 CP3 CP4 CP5 29.2(9) . . . . ? CP2 CP1 CP5 CP4 23.8(9) . . . . ? CP3 CP4 CP5 CP1 -32.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 70.07 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.630 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.082 # Attachment 'Uhl-4b.cif' data_Uhl-4b _database_code_depnum_ccdc_archive 'CCDC 621974' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 Ga2' _chemical_formula_weight 552.16 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 ? _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 27.889(8) _cell_length_b 12.053(3) _cell_length_c 19.249(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.919(6) _cell_angle_gamma 90.00 _cell_volume 6003(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 'all measured' _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 28.09 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.810 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7261 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29852 _diffrn_reflns_av_R_equivalents 0.2431 _diffrn_reflns_av_sigmaI/netI 0.2345 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.09 _reflns_number_total 7286 _reflns_number_gt 2993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0617P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7286 _refine_ls_number_parameters 318 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.2311 _refine_ls_R_factor_gt 0.0857 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.004 _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 Ga1 Ga 0.12631(3) 0.94057(7) 0.24767(4) 0.0360(3) Uani 1 1 d . B . C1 C 0.1018(3) 0.7805(6) 0.2412(4) 0.0318(17) Uani 1 1 d . . . C11 C 0.1350(3) 0.6949(6) 0.2575(4) 0.0382(19) Uani 1 1 d . . . H11 H 0.1689 0.7152 0.2601 0.046 Uiso 1 1 calc R . . C12 C 0.1301(3) 0.5727(7) 0.2726(4) 0.043(2) Uani 1 1 d . . . C121 C 0.1529(3) 0.5579(7) 0.3578(4) 0.061(2) Uani 1 1 d . . . H12A H 0.1308 0.5930 0.3793 0.073 Uiso 1 1 calc R . . H12B H 0.1866 0.5912 0.3777 0.073 Uiso 1 1 calc R . . H12C H 0.1556 0.4803 0.3697 0.073 Uiso 1 1 calc R . . C122 C 0.0751(3) 0.5292(7) 0.2420(5) 0.065(3) Uani 1 1 d . . . H12D H 0.0558 0.5632 0.2684 0.078 Uiso 1 1 calc R . . H12E H 0.0755 0.4502 0.2486 0.078 Uiso 1 1 calc R . . H12F H 0.0593 0.5467 0.1897 0.078 Uiso 1 1 calc R . . C123 C 0.1615(3) 0.5065(7) 0.2374(5) 0.061(3) Uani 1 1 d . . . H12G H 0.1616 0.4297 0.2507 0.074 Uiso 1 1 calc R . . H12H H 0.1964 0.5339 0.2554 0.074 Uiso 1 1 calc R . . H12I H 0.1465 0.5141 0.1840 0.074 Uiso 1 1 calc R . . C13 C 0.0489(2) 0.7731(5) 0.2438(4) 0.0300(17) Uani 1 1 d . . . C14 C 0.0440(2) 0.7744(6) 0.3126(4) 0.0331(18) Uani 1 1 d . . . H14 H 0.0747 0.7758 0.3571 0.040 Uiso 1 1 calc R . . C15 C -0.0032(2) 0.7738(5) 0.3198(4) 0.0310(17) Uani 1 1 d . . . H15 H -0.0048 0.7739 0.3687 0.037 Uiso 1 1 calc R . . C31 C 0.2014(2) 0.9598(6) 0.3048(4) 0.0399(19) Uani 1 1 d D . . H31A H 0.2202 0.9163 0.2818 0.048 Uiso 1 1 calc R . . H31B H 0.2104 1.0362 0.3026 0.048 Uiso 1 1 calc R . . C32 C 0.2168(3) 0.9259(8) 0.3846(4) 0.062(3) Uani 1 1 d D . . H32A H 0.2136 0.8467 0.3862 0.074 Uiso 1 1 calc R . . H32B H 0.1928 0.9579 0.4038 0.074 Uiso 1 1 calc R . . C33 C 0.2706(3) 0.9574(7) 0.4360(4) 0.064(3) Uani 1 1 d D . . H33A H 0.2953 0.9249 0.4182 0.077 Uiso 1 1 calc R . . H33B H 0.2767 0.9308 0.4856 0.077 Uiso 1 1 calc R . . H33C H 0.2741 1.0367 0.4370 0.077 Uiso 1 1 calc R . . C41 C 0.0810(3) 1.0457(8) 0.2707(5) 0.064(3) Uani 1 1 d D . . H41A H 0.0640 1.0899 0.2268 0.077 Uiso 1 1 calc R A 1 H41B H 0.0547 1.0041 0.2801 0.077 Uiso 1 1 calc R A 1 C42 C 0.1042(6) 1.1196(14) 0.3327(9) 0.073(5) Uani 0.60 1 d PDU B 1 H42A H 0.1356 1.1479 0.3297 0.087 Uiso 0.60 1 calc PR B 1 H42B H 0.1137 1.0770 0.3780 0.087 Uiso 0.60 1 calc PR B 1 C43 C 0.0726(17) 1.216(3) 0.339(3) 0.102(10) Uani 0.60 1 d PDU B 1 H43A H 0.0401 1.2165 0.2978 0.122 Uiso 0.60 1 calc PR B 1 H43B H 0.0908 1.2839 0.3396 0.122 Uiso 0.60 1 calc PR B 1 H43C H 0.0666 1.2103 0.3853 0.122 Uiso 0.60 1 calc PR B 1 C42A C 0.0907(11) 1.1617(13) 0.2855(15) 0.064(7) Uani 0.40 1 d PDU B 2 H42C H 0.0802 1.1996 0.2383 0.077 Uiso 0.40 1 calc PR B 2 H42D H 0.1273 1.1717 0.3098 0.077 Uiso 0.40 1 calc PR B 2 C43A C 0.065(3) 1.218(5) 0.332(5) 0.125(14) Uani 0.40 1 d PDU B 2 H43D H 0.0477 1.2833 0.3071 0.150 Uiso 0.40 1 calc PR B 2 H43E H 0.0908 1.2376 0.3800 0.150 Uiso 0.40 1 calc PR B 2 H43F H 0.0405 1.1680 0.3397 0.150 Uiso 0.40 1 calc PR B 2 Ga2 Ga 0.11925(3) 0.79225(7) 0.11981(4) 0.0368(3) Uani 1 1 d . . . C2 C 0.1035(2) 0.9594(6) 0.1087(4) 0.0339(18) Uani 1 1 d . B . C21 C 0.1425(3) 1.0311(6) 0.1232(4) 0.0336(18) Uani 1 1 d . . . H21 H 0.1752 0.9994 0.1534 0.040 Uiso 1 1 calc R B . C22 C 0.1466(2) 1.1492(6) 0.1033(4) 0.0350(18) Uani 1 1 d . B . C221 C 0.1865(3) 1.2097(7) 0.1709(4) 0.050(2) Uani 1 1 d . . . H22A H 0.1735 1.2150 0.2104 0.060 Uiso 1 1 calc R B . H22B H 0.1924 1.2829 0.1561 0.060 Uiso 1 1 calc R . . H22C H 0.2184 1.1689 0.1883 0.060 Uiso 1 1 calc R . . C222 C 0.1681(3) 1.1508(7) 0.0400(4) 0.063(3) Uani 1 1 d . . . H22D H 0.2008 1.1133 0.0565 0.076 Uiso 1 1 calc R B . H22E H 0.1725 1.2262 0.0275 0.076 Uiso 1 1 calc R . . H22F H 0.1443 1.1138 -0.0033 0.076 Uiso 1 1 calc R . . C223 C 0.0964(3) 1.2174(6) 0.0790(5) 0.062(3) Uani 1 1 d . . . H22G H 0.0721 1.1883 0.0328 0.074 Uiso 1 1 calc R B . H22H H 0.1038 1.2934 0.0720 0.074 Uiso 1 1 calc R . . H22I H 0.0818 1.2129 0.1169 0.074 Uiso 1 1 calc R . . C23 C 0.0504(2) 0.9833(5) 0.0550(4) 0.0278(17) Uani 1 1 d . . . C24 C 0.0077(3) 1.0002(6) 0.0742(4) 0.0365(19) Uani 1 1 d . . . H24 H 0.0122 1.0000 0.1262 0.044 Uiso 1 1 calc R . . C25 C 0.0408(2) 0.9827(6) -0.0210(4) 0.0359(19) Uani 1 1 d . . . H25 H 0.0691 0.9699 -0.0370 0.043 Uiso 1 1 calc R . . C51 C 0.1934(3) 0.7641(6) 0.1406(4) 0.041(2) Uani 1 1 d . B . H51A H 0.2140 0.8002 0.1865 0.049 Uiso 1 1 calc R . . H51B H 0.2000 0.6859 0.1470 0.049 Uiso 1 1 calc R . . C52 C 0.2096(3) 0.8057(7) 0.0782(5) 0.058(2) Uani 1 1 d . . . H52A H 0.1902 0.7666 0.0329 0.069 Uiso 1 1 calc R B . H52B H 0.2011 0.8830 0.0699 0.069 Uiso 1 1 calc R . . C53 C 0.2663(3) 0.7908(8) 0.0947(5) 0.081(3) Uani 1 1 d . B . H53A H 0.2859 0.8263 0.1414 0.097 Uiso 1 1 calc R . . H53B H 0.2748 0.8236 0.0553 0.097 Uiso 1 1 calc R . . H53C H 0.2744 0.7131 0.0981 0.097 Uiso 1 1 calc R . . C61 C 0.0662(3) 0.6960(7) 0.0481(4) 0.051(2) Uani 1 1 d . B . H61A H 0.0466 0.6613 0.0738 0.061 Uiso 1 1 calc R . . H61B H 0.0430 0.7418 0.0093 0.061 Uiso 1 1 calc R . . C62 C 0.0870(4) 0.6073(8) 0.0123(5) 0.079(3) Uani 1 1 d . . . H62A H 0.1097 0.6415 -0.0084 0.095 Uiso 1 1 calc R B . H62B H 0.1073 0.5572 0.0508 0.095 Uiso 1 1 calc R . . C63 C 0.0479(4) 0.5416(8) -0.0475(5) 0.090(3) Uani 1 1 d . B . H63A H 0.0268 0.5013 -0.0267 0.108 Uiso 1 1 calc R . . H63B H 0.0651 0.4904 -0.0686 0.108 Uiso 1 1 calc R . . H63C H 0.0266 0.5907 -0.0859 0.108 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 0.0212(4) 0.0505(6) 0.0329(5) -0.0046(4) 0.0061(4) -0.0025(4) C1 0.023(4) 0.049(5) 0.020(4) 0.000(4) 0.004(3) 0.002(4) C11 0.029(4) 0.055(6) 0.025(4) -0.014(4) 0.004(3) -0.004(4) C12 0.050(5) 0.046(5) 0.027(4) 0.002(4) 0.007(4) 0.011(4) C121 0.060(6) 0.073(7) 0.041(5) 0.018(5) 0.010(4) 0.021(5) C122 0.065(6) 0.043(6) 0.072(7) -0.001(5) 0.008(5) -0.008(5) C123 0.073(6) 0.057(6) 0.051(6) -0.006(5) 0.020(5) 0.016(5) C13 0.019(4) 0.035(5) 0.034(4) 0.001(3) 0.008(3) 0.002(3) C14 0.015(3) 0.051(5) 0.026(4) 0.000(4) -0.001(3) -0.001(3) C15 0.026(4) 0.045(5) 0.020(4) 0.003(3) 0.006(3) -0.004(3) C31 0.034(4) 0.054(5) 0.030(4) -0.006(4) 0.010(4) -0.007(4) C32 0.047(5) 0.087(7) 0.039(5) 0.002(5) 0.001(4) -0.011(5) C33 0.054(6) 0.075(7) 0.040(5) -0.005(5) -0.008(4) -0.001(5) C41 0.044(5) 0.082(7) 0.064(6) -0.033(6) 0.017(5) -0.003(5) C42 0.065(11) 0.086(13) 0.075(13) -0.031(11) 0.035(12) 0.000(9) C43 0.16(2) 0.065(14) 0.107(17) -0.057(14) 0.084(18) -0.008(13) C42A 0.076(15) 0.049(14) 0.076(17) 0.009(12) 0.037(15) -0.018(12) C43A 0.18(3) 0.10(3) 0.13(3) -0.05(2) 0.09(2) -0.03(2) Ga2 0.0241(4) 0.0448(6) 0.0316(5) 0.0000(4) -0.0013(4) 0.0051(4) C2 0.011(3) 0.048(5) 0.038(5) 0.005(4) 0.003(3) 0.004(3) C21 0.022(4) 0.043(5) 0.035(5) 0.001(4) 0.011(3) 0.008(4) C22 0.022(4) 0.046(5) 0.032(4) -0.007(4) 0.004(3) -0.010(4) C221 0.048(5) 0.058(6) 0.038(5) -0.012(4) 0.008(4) 0.002(4) C222 0.078(7) 0.062(6) 0.051(6) 0.005(5) 0.025(5) -0.009(5) C223 0.054(6) 0.049(6) 0.067(6) 0.011(5) 0.004(5) 0.004(5) C23 0.023(4) 0.026(4) 0.030(4) 0.012(3) 0.005(3) 0.008(3) C24 0.024(4) 0.051(5) 0.025(4) -0.001(4) -0.001(3) -0.002(3) C25 0.016(4) 0.052(5) 0.036(5) 0.001(4) 0.006(3) -0.001(3) C51 0.036(4) 0.044(5) 0.035(5) 0.002(4) 0.004(4) 0.011(4) C52 0.058(6) 0.060(6) 0.068(6) -0.002(5) 0.037(5) 0.015(5) C53 0.075(7) 0.103(8) 0.071(7) -0.007(6) 0.035(6) -0.021(6) C61 0.043(5) 0.056(6) 0.047(5) -0.007(4) 0.008(4) 0.000(4) C62 0.081(7) 0.079(8) 0.072(7) -0.032(6) 0.022(6) 0.002(6) C63 0.106(8) 0.092(8) 0.087(8) -0.049(7) 0.053(7) -0.038(7) _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 C41 1.954(8) . ? Ga1 C31 1.981(6) . ? Ga1 C1 2.035(7) . ? Ga1 C2 2.519(7) . ? Ga1 Ga2 2.9885(13) . ? C1 C11 1.343(9) . ? C1 C13 1.499(9) . ? C11 C12 1.517(10) . ? C11 H11 0.9600 . ? C12 C122 1.515(10) . ? C12 C123 1.520(10) . ? C12 C121 1.532(9) . ? C121 H12A 0.9599 . ? C121 H12B 0.9599 . ? C121 H12C 0.9599 . ? C122 H12D 0.9599 . ? C122 H12E 0.9599 . ? C122 H12F 0.9599 . ? C123 H12G 0.9599 . ? C123 H12H 0.9599 . ? C123 H12I 0.9599 . ? C13 C14 1.380(9) . ? C13 C15 1.400(8) 2 ? C14 C15 1.373(8) . ? C14 H14 0.9600 . ? C15 C13 1.400(8) 2 ? C15 H15 0.9600 . ? C31 C32 1.490(9) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C32 C33 1.504(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C33 H33A 0.9599 . ? C33 H33B 0.9599 . ? C33 H33C 0.9599 . ? C41 C42A 1.432(15) . ? C41 C42 1.436(12) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C42 C43 1.496(19) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C43 H43A 0.9599 . ? C43 H43B 0.9599 . ? C43 H43C 0.9599 . ? C42A C43A 1.50(2) . ? C42A H42C 0.9600 . ? C42A H42D 0.9600 . ? C43A H43D 0.9599 . ? C43A H43E 0.9599 . ? C43A H43F 0.9599 . ? Ga2 C61 1.978(7) . ? Ga2 C51 1.984(7) . ? Ga2 C2 2.056(7) . ? C2 C21 1.334(9) . ? C2 C23 1.483(8) . ? C21 C22 1.490(9) . ? C21 H21 0.9600 . ? C22 C223 1.540(10) . ? C22 C221 1.543(9) . ? C22 C222 1.545(10) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C222 H22D 0.9599 . ? C222 H22E 0.9599 . ? C222 H22F 0.9599 . ? C223 H22G 0.9599 . ? C223 H22H 0.9599 . ? C223 H22I 0.9599 . ? C23 C25 1.385(9) . ? C23 C24 1.389(8) . ? C24 C25 1.374(9) 5_575 ? C24 H24 0.9600 . ? C25 C24 1.374(9) 5_575 ? C25 H25 0.9600 . ? C51 C52 1.517(10) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C52 C53 1.503(10) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C53 H53A 0.9599 . ? C53 H53B 0.9599 . ? C53 H53C 0.9599 . ? C61 C62 1.500(10) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C62 C63 1.484(11) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C63 H63A 0.9599 . ? C63 H63B 0.9599 . ? C63 H63C 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 C41 Ga1 C31 115.9(3) . . ? C41 Ga1 C1 113.5(3) . . ? C31 Ga1 C1 113.9(3) . . ? C41 Ga1 C2 104.7(3) . . ? C31 Ga1 C2 112.0(2) . . ? C1 Ga1 C2 94.3(2) . . ? C41 Ga1 Ga2 136.5(2) . . ? C31 Ga1 Ga2 104.9(2) . . ? C1 Ga1 Ga2 57.65(18) . . ? C2 Ga1 Ga2 42.80(17) . . ? C11 C1 C13 123.3(7) . . ? C11 C1 Ga1 121.8(5) . . ? C13 C1 Ga1 111.5(5) . . ? C1 C11 C12 133.3(7) . . ? C1 C11 H11 113.3 . . ? C12 C11 H11 113.3 . . ? C122 C12 C11 114.4(6) . . ? C122 C12 C123 108.3(7) . . ? C11 C12 C123 108.4(6) . . ? C122 C12 C121 109.4(7) . . ? C11 C12 C121 106.7(6) . . ? C123 C12 C121 109.7(6) . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C12 C122 H12D 109.5 . . ? C12 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C12 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C12 C123 H12G 109.5 . . ? C12 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C12 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C14 C13 C15 117.1(6) . 2 ? C14 C13 C1 118.9(6) . . ? C15 C13 C1 123.8(6) 2 . ? C15 C14 C13 122.6(6) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 C13 120.3(6) . 2 ? C14 C15 H15 119.8 . . ? C13 C15 H15 119.8 2 . ? C32 C31 Ga1 112.3(5) . . ? C32 C31 H31A 109.1 . . ? Ga1 C31 H31A 109.1 . . ? C32 C31 H31B 109.1 . . ? Ga1 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 116.3(7) . . ? C31 C32 H32A 108.2 . . ? C33 C32 H32A 108.2 . . ? C31 C32 H32B 108.2 . . ? C33 C32 H32B 108.2 . . ? H32A C32 H32B 107.4 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C42A C41 C42 40.2(10) . . ? C42A C41 Ga1 126.0(12) . . ? C42 C41 Ga1 117.4(8) . . ? C42A C41 H41A 68.2 . . ? C42 C41 H41A 107.9 . . ? Ga1 C41 H41A 107.9 . . ? C42A C41 H41B 125.0 . . ? C42 C41 H41B 107.9 . . ? Ga1 C41 H41B 107.9 . . ? H41A C41 H41B 107.2 . . ? C41 C42 C43 117.2(19) . . ? C41 C42 H42A 108.0 . . ? C43 C42 H42A 108.0 . . ? C41 C42 H42B 108.0 . . ? C43 C42 H42B 108.0 . . ? H42A C42 H42B 107.2 . . ? C41 C42A C43A 117(2) . . ? C41 C42A H42C 107.9 . . ? C43A C42A H42C 107.9 . . ? C41 C42A H42D 107.9 . . ? C43A C42A H42D 107.9 . . ? H42C C42A H42D 107.2 . . ? C42A C43A H43D 109.5 . . ? C42A C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C42A C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C61 Ga2 C51 119.5(3) . . ? C61 Ga2 C2 115.2(3) . . ? C51 Ga2 C2 110.8(3) . . ? C61 Ga2 Ga1 136.7(2) . . ? C51 Ga2 Ga1 101.1(2) . . ? C2 Ga2 Ga1 56.33(19) . . ? C21 C2 C23 122.9(6) . . ? C21 C2 Ga2 119.1(5) . . ? C23 C2 Ga2 112.4(5) . . ? C21 C2 Ga1 88.4(4) . . ? C23 C2 Ga1 123.3(4) . . ? Ga2 C2 Ga1 80.9(2) . . ? C2 C21 C22 134.5(6) . . ? C2 C21 H21 112.8 . . ? C22 C21 H21 112.8 . . ? C21 C22 C223 116.0(6) . . ? C21 C22 C221 109.6(6) . . ? C223 C22 C221 107.0(6) . . ? C21 C22 C222 107.8(6) . . ? C223 C22 C222 109.2(6) . . ? C221 C22 C222 106.9(6) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 C222 H22D 109.5 . . ? C22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? C22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? C22 C223 H22G 109.5 . . ? C22 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? C22 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C25 C23 C24 115.8(6) . . ? C25 C23 C2 119.0(6) . . ? C24 C23 C2 125.1(6) . . ? C25 C24 C23 121.8(7) 5_575 . ? C25 C24 H24 119.1 5_575 . ? C23 C24 H24 119.1 . . ? C24 C25 C23 122.4(6) 5_575 . ? C24 C25 H25 118.8 5_575 . ? C23 C25 H25 118.8 . . ? C52 C51 Ga2 112.3(5) . . ? C52 C51 H51A 109.1 . . ? Ga2 C51 H51A 109.1 . . ? C52 C51 H51B 109.1 . . ? Ga2 C51 H51B 109.1 . . ? H51A C51 H51B 107.9 . . ? C53 C52 C51 113.1(7) . . ? C53 C52 H52A 109.0 . . ? C51 C52 H52A 109.0 . . ? C53 C52 H52B 109.0 . . ? C51 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C62 C61 Ga2 115.0(6) . . ? C62 C61 H61A 108.5 . . ? Ga2 C61 H61A 108.5 . . ? C62 C61 H61B 108.5 . . ? Ga2 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? C63 C62 C61 116.1(8) . . ? C63 C62 H62A 108.3 . . ? C61 C62 H62A 108.3 . . ? C63 C62 H62B 108.3 . . ? C61 C62 H62B 108.3 . . ? H62A C62 H62B 107.4 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 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 C41 Ga1 C1 C11 -151.3(6) . . . . ? C31 Ga1 C1 C11 -15.7(7) . . . . ? C2 Ga1 C1 C11 100.7(6) . . . . ? Ga2 Ga1 C1 C11 77.3(6) . . . . ? C41 Ga1 C1 C13 8.6(6) . . . . ? C31 Ga1 C1 C13 144.2(5) . . . . ? C2 Ga1 C1 C13 -99.5(5) . . . . ? Ga2 Ga1 C1 C13 -122.8(5) . . . . ? C13 C1 C11 C12 8.3(12) . . . . ? Ga1 C1 C11 C12 165.7(6) . . . . ? C1 C11 C12 C122 21.4(11) . . . . ? C1 C11 C12 C123 142.2(8) . . . . ? C1 C11 C12 C121 -99.7(9) . . . . ? C11 C1 C13 C14 76.3(9) . . . . ? Ga1 C1 C13 C14 -83.2(7) . . . . ? C11 C1 C13 C15 -109.1(8) . . . 2 ? Ga1 C1 C13 C15 91.4(7) . . . 2 ? C15 C13 C14 C15 1.5(9) 2 . . . ? C1 C13 C14 C15 176.5(7) . . . . ? C13 C14 C15 C13 -0.8(10) . . . 2 ? C41 Ga1 C31 C32 71.9(7) . . . . ? C1 Ga1 C31 C32 -62.6(6) . . . . ? C2 Ga1 C31 C32 -168.1(5) . . . . ? Ga2 Ga1 C31 C32 -123.4(5) . . . . ? Ga1 C31 C32 C33 -168.6(6) . . . . ? C31 Ga1 C41 C42A 39.2(17) . . . . ? C1 Ga1 C41 C42A 173.9(16) . . . . ? C2 Ga1 C41 C42A -84.7(16) . . . . ? Ga2 Ga1 C41 C42A -119.1(15) . . . . ? C31 Ga1 C41 C42 -7.4(13) . . . . ? C1 Ga1 C41 C42 127.3(11) . . . . ? C2 Ga1 C41 C42 -131.3(12) . . . . ? Ga2 Ga1 C41 C42 -165.7(10) . . . . ? C42A C41 C42 C43 52(3) . . . . ? Ga1 C41 C42 C43 166(2) . . . . ? C42 C41 C42A C43A -63(5) . . . . ? Ga1 C41 C42A C43A -155(4) . . . . ? C41 Ga1 Ga2 C61 -38.8(6) . . . . ? C31 Ga1 Ga2 C61 161.3(4) . . . . ? C1 Ga1 Ga2 C61 52.1(4) . . . . ? C2 Ga1 Ga2 C61 -92.3(4) . . . . ? C41 Ga1 Ga2 C51 161.1(5) . . . . ? C31 Ga1 Ga2 C51 1.3(3) . . . . ? C1 Ga1 Ga2 C51 -107.9(3) . . . . ? C2 Ga1 Ga2 C51 107.7(3) . . . . ? C41 Ga1 Ga2 C2 53.5(5) . . . . ? C31 Ga1 Ga2 C2 -106.4(3) . . . . ? C1 Ga1 Ga2 C2 144.5(3) . . . . ? C61 Ga2 C2 C21 -146.3(6) . . . . ? C51 Ga2 C2 C21 -6.7(7) . . . . ? Ga1 Ga2 C2 C21 83.0(6) . . . . ? C61 Ga2 C2 C23 8.4(6) . . . . ? C51 Ga2 C2 C23 147.9(5) . . . . ? Ga1 Ga2 C2 C23 -122.3(5) . . . . ? C61 Ga2 C2 Ga1 130.7(3) . . . . ? C51 Ga2 C2 Ga1 -89.7(3) . . . . ? C41 Ga1 C2 C21 95.0(5) . . . . ? C31 Ga1 C2 C21 -31.4(5) . . . . ? C1 Ga1 C2 C21 -149.4(4) . . . . ? Ga2 Ga1 C2 C21 -119.9(5) . . . . ? C41 Ga1 C2 C23 -34.2(6) . . . . ? C31 Ga1 C2 C23 -160.6(6) . . . . ? C1 Ga1 C2 C23 81.4(6) . . . . ? Ga2 Ga1 C2 C23 110.9(6) . . . . ? C41 Ga1 C2 Ga2 -145.1(3) . . . . ? C31 Ga1 C2 Ga2 88.5(3) . . . . ? C1 Ga1 C2 Ga2 -29.5(3) . . . . ? C23 C2 C21 C22 8.6(13) . . . . ? Ga2 C2 C21 C22 160.5(6) . . . . ? Ga1 C2 C21 C22 -120.9(8) . . . . ? C2 C21 C22 C223 19.7(12) . . . . ? C2 C21 C22 C221 141.0(8) . . . . ? C2 C21 C22 C222 -103.0(9) . . . . ? C21 C2 C23 C25 72.8(9) . . . . ? Ga2 C2 C23 C25 -80.7(7) . . . . ? Ga1 C2 C23 C25 -174.5(5) . . . . ? C21 C2 C23 C24 -111.3(8) . . . . ? Ga2 C2 C23 C24 95.2(7) . . . . ? Ga1 C2 C23 C24 1.4(10) . . . . ? C25 C23 C24 C25 -1.2(11) . . . 5_575 ? C2 C23 C24 C25 -177.2(7) . . . 5_575 ? C24 C23 C25 C24 1.2(11) . . . 5_575 ? C2 C23 C25 C24 177.4(6) . . . 5_575 ? C61 Ga2 C51 C52 77.1(6) . . . . ? C2 Ga2 C51 C52 -60.5(6) . . . . ? Ga1 Ga2 C51 C52 -118.5(5) . . . . ? Ga2 C51 C52 C53 176.8(6) . . . . ? C51 Ga2 C61 C62 -1.3(8) . . . . ? C2 Ga2 C61 C62 134.5(6) . . . . ? Ga1 Ga2 C61 C62 -158.7(5) . . . . ? Ga2 C61 C62 C63 -173.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.611 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.115