# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Colin Raston' _publ_contact_author_address ; Department of Chemistry University of Western Australia Crawley Perth Western Australia 6009 AUSTRALIA ; _publ_contact_author_email CLRASTON@CHEM.UWA.EDU.AU _publ_section_title ; Icosahedral Galloxane Clusters ; loop_ _publ_author_name 'Colin Raston' 'J. L. Atwood' 'Scott Dalgarno' 'Robert M. McKinlay' 'Peter J. Nichols' ; S.Papadopoulos ; data_1 _database_code_depnum_ccdc_archive 'CCDC 634232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H44 Ga6 O13' _chemical_formula_sum 'C42 H44 Ga6 O13' _chemical_formula_weight 1175.09 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.252(3) _cell_length_b 15.578(3) _cell_length_c 15.739(3) _cell_angle_alpha 62.67(3) _cell_angle_beta 81.12(3) _cell_angle_gamma 66.97(3) _cell_volume 2655.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 3.053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5803 _exptl_absorpt_correction_T_max 0.6574 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12758 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1850 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 28.30 _reflns_number_total 12758 _reflns_number_gt 6311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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. From the residual electron density, it was clear that there were two very badly disordered molecules of tetrahydrofuran. These could not be adequately modelled and the routine SQUEEZE was applied to the data to account for this. ; _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^)+(0.0710P)^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 12758 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1412 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 0.891 _refine_ls_restrained_S_all 0.891 _refine_ls_shift/su_max 0.000 _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 Ga2 Ga 0.38163(5) 0.47554(5) 0.19353(5) 0.01963(17) Uani 1 1 d . . . Ga1 Ga 0.44074(5) 0.30677(5) 0.10957(5) 0.02065(17) Uani 1 1 d . . . Ga5 Ga 0.41215(5) 0.43109(5) -0.12411(5) 0.01851(16) Uani 1 1 d . . . Ga4 Ga 0.65326(5) 0.29629(5) -0.01111(5) 0.02009(17) Uani 1 1 d . . . Ga3 Ga 0.63498(5) 0.32157(5) 0.18599(5) 0.02000(17) Uani 1 1 d . . . Ga6 Ga 0.25232(5) 0.55305(5) -0.00348(5) 0.01994(17) Uani 1 1 d . . . O2 O 0.4970(3) 0.3412(3) -0.0125(3) 0.0199(9) Uani 1 1 d . . . O1 O 0.4814(3) 0.3660(3) 0.1721(3) 0.0202(9) Uani 1 1 d . . . O7 O 0.3230(3) 0.5766(3) 0.0723(3) 0.0197(9) Uani 1 1 d . . . O6 O 0.3367(3) 0.5533(3) -0.1106(3) 0.0184(9) Uani 1 1 d . . . O4 O 0.4802(3) 0.5279(3) 0.2121(3) 0.0202(9) Uani 1 1 d . . . O12 O 0.3594(3) 0.2305(3) -0.0523(3) 0.0296(11) Uani 1 1 d . . . C30 C 0.3205(5) 0.2939(5) -0.1442(5) 0.0281(15) Uani 1 1 d . . . O8 O 0.2820(4) 0.2335(3) 0.2518(3) 0.0347(11) Uani 1 1 d . . . O3 O 0.2933(3) 0.4052(3) 0.0697(3) 0.0237(10) Uani 1 1 d . . . O13 O 0.0568(3) 0.5039(4) 0.1065(3) 0.0369(12) Uani 1 1 d . . . O5 O 0.6815(3) 0.2509(3) 0.1143(3) 0.0300(11) Uani 1 1 d . . . C1 C 0.4439(5) 0.1655(5) 0.1825(4) 0.0255(15) Uani 1 1 d . . . O11 O 0.8859(3) 0.2085(3) -0.0567(3) 0.0378(12) Uani 1 1 d . . . C36 C 0.0960(5) 0.6319(5) -0.0331(5) 0.0292(16) Uani 1 1 d . . . O10 O 0.6176(4) 0.1351(3) 0.3535(3) 0.0356(11) Uani 1 1 d . . . C22 C 0.7162(5) 0.2019(5) -0.0710(5) 0.0277(15) Uani 1 1 d . . . C16 C 0.6988(5) 0.1559(5) 0.3774(4) 0.0254(15) Uani 1 1 d . . . O9 O 0.4032(4) 0.3211(4) 0.3994(3) 0.0417(12) Uani 1 1 d . . . C34 C 0.2964(5) 0.4582(5) -0.2826(5) 0.0294(15) Uani 1 1 d . . . H34 H 0.3045 0.5222 -0.3122 0.035 Uiso 1 1 calc R . . C2 C 0.3598(6) 0.1470(5) 0.2442(5) 0.0310(16) Uani 1 1 d . . . C8 C 0.2683(5) 0.4614(5) 0.2873(5) 0.0264(15) Uani 1 1 d . . . C41 C 0.0609(5) 0.7249(5) -0.1157(5) 0.0337(17) Uani 1 1 d . . . H41 H 0.1125 0.7508 -0.1546 0.040 Uiso 1 1 calc R . . C29 C 0.3364(4) 0.3896(5) -0.1861(4) 0.0231(14) Uani 1 1 d . . . C31 C 0.2675(5) 0.2684(5) -0.1960(5) 0.0351(17) Uani 1 1 d . . . H31 H 0.2572 0.2053 -0.1679 0.042 Uiso 1 1 calc R . . C37 C 0.0175(5) 0.5961(5) 0.0240(5) 0.0338(17) Uani 1 1 d . . . C15 C 0.7135(5) 0.2473(4) 0.3102(4) 0.0250(15) Uani 1 1 d . . . C39 C -0.1261(6) 0.7401(6) -0.0826(6) 0.049(2) Uani 1 1 d . . . H39 H -0.2004 0.7756 -0.0992 0.059 Uiso 1 1 calc R . . C32 C 0.2308(5) 0.3398(5) -0.2904(5) 0.0324(16) Uani 1 1 d . . . H32 H 0.1954 0.3239 -0.3246 0.039 Uiso 1 1 calc R . . C17 C 0.7636(6) 0.0901(5) 0.4604(5) 0.0419(19) Uani 1 1 d . . . H17 H 0.7535 0.0291 0.5040 0.050 Uiso 1 1 calc R . . C9 C 0.2949(6) 0.3818(6) 0.3823(5) 0.0354(17) Uani 1 1 d . . . C20 C 0.7944(5) 0.2701(5) 0.3297(5) 0.0298(16) Uani 1 1 d . . . H20 H 0.8059 0.3303 0.2860 0.036 Uiso 1 1 calc R . . C42 C -0.0207(6) 0.4701(7) 0.1729(6) 0.053(2) Uani 1 1 d . . . H42A H -0.0640 0.5228 0.1932 0.080 Uiso 1 1 calc R . . H42B H 0.0172 0.4074 0.2274 0.080 Uiso 1 1 calc R . . H42C H -0.0677 0.4573 0.1431 0.080 Uiso 1 1 calc R . . C13 C 0.1592(5) 0.5278(6) 0.2659(5) 0.0389(18) Uani 1 1 d . . . H13 H 0.1394 0.5804 0.2042 0.047 Uiso 1 1 calc R . . C18 C 0.8445(6) 0.1181(6) 0.4767(5) 0.043(2) Uani 1 1 d . . . H18 H 0.8879 0.0754 0.5325 0.052 Uiso 1 1 calc R . . C38 C -0.0948(5) 0.6497(6) -0.0002(6) 0.044(2) Uani 1 1 d . . . H38 H -0.1467 0.6243 0.0387 0.053 Uiso 1 1 calc R . . C40 C -0.0522(6) 0.7809(6) -0.1418(6) 0.045(2) Uani 1 1 d . . . H40 H -0.0756 0.8431 -0.1970 0.054 Uiso 1 1 calc R . . C25 C 0.8139(6) 0.0630(6) -0.1537(6) 0.048(2) Uani 1 1 d . . . H25 H 0.8464 0.0165 -0.1803 0.058 Uiso 1 1 calc R . . C3 C 0.3539(6) 0.0488(6) 0.2941(5) 0.0411(19) Uani 1 1 d . . . H3 H 0.2948 0.0389 0.3325 0.049 Uiso 1 1 calc R . . C26 C 0.7016(6) 0.0951(5) -0.1389(5) 0.0426(19) Uani 1 1 d . . . H26 H 0.6582 0.0712 -0.1569 0.051 Uiso 1 1 calc R . . C28 C 0.9993(5) 0.1826(6) -0.0753(6) 0.050(2) Uani 1 1 d . . . H28A H 1.0364 0.1088 -0.0417 0.076 Uiso 1 1 calc R . . H28B H 1.0289 0.2170 -0.0541 0.076 Uiso 1 1 calc R . . H28C H 1.0094 0.2043 -0.1428 0.076 Uiso 1 1 calc R . . C27 C 0.6549(5) 0.1622(5) -0.0976(5) 0.0312(16) Uani 1 1 d . . . H27 H 0.5799 0.1818 -0.0870 0.037 Uiso 1 1 calc R . . C12 C 0.0792(6) 0.5176(8) 0.3340(7) 0.066(3) Uani 1 1 d . . . H12 H 0.0069 0.5637 0.3189 0.079 Uiso 1 1 calc R . . C19 C 0.8607(5) 0.2056(6) 0.4132(5) 0.0384(18) Uani 1 1 d . . . H19 H 0.9151 0.2230 0.4247 0.046 Uiso 1 1 calc R . . C33 C 0.2460(5) 0.4323(6) -0.3333(5) 0.0354(17) Uani 1 1 d . . . H33 H 0.2225 0.4778 -0.3965 0.042 Uiso 1 1 calc R . . C10 C 0.2154(7) 0.3678(7) 0.4521(6) 0.052(2) Uani 1 1 d . . . H10 H 0.2336 0.3142 0.5136 0.063 Uiso 1 1 calc R . . C21 C 0.6041(7) 0.0377(5) 0.4127(5) 0.051(2) Uani 1 1 d . . . H21A H 0.6734 -0.0181 0.4216 0.076 Uiso 1 1 calc R . . H21B H 0.5522 0.0307 0.3824 0.076 Uiso 1 1 calc R . . H21C H 0.5777 0.0355 0.4738 0.076 Uiso 1 1 calc R . . C23 C 0.8287(5) 0.1687(5) -0.0862(5) 0.0312(16) Uani 1 1 d . . . C5 C 0.5249(7) -0.0198(5) 0.2281(5) 0.046(2) Uani 1 1 d . . . H5 H 0.5818 -0.0763 0.2240 0.056 Uiso 1 1 calc R . . C24 C 0.8764(6) 0.1013(5) -0.1283(6) 0.045(2) Uani 1 1 d . . . H24 H 0.9512 0.0817 -0.1395 0.054 Uiso 1 1 calc R . . C14 C 0.4366(7) 0.2399(6) 0.4930(5) 0.069(3) Uani 1 1 d . . . H14A H 0.4209 0.2689 0.5379 0.104 Uiso 1 1 calc R . . H14B H 0.5139 0.2017 0.4949 0.104 Uiso 1 1 calc R . . H14C H 0.3975 0.1941 0.5095 0.104 Uiso 1 1 calc R . . C7 C 0.2099(6) 0.2183(6) 0.3302(5) 0.051(2) Uani 1 1 d . . . H7A H 0.1619 0.1890 0.3231 0.076 Uiso 1 1 calc R . . H7B H 0.1671 0.2837 0.3313 0.076 Uiso 1 1 calc R . . H7C H 0.2521 0.1718 0.3890 0.076 Uiso 1 1 calc R . . C6 C 0.5288(6) 0.0805(5) 0.1748(5) 0.0358(17) Uani 1 1 d . . . H6 H 0.5871 0.0902 0.1351 0.043 Uiso 1 1 calc R . . C11 C 0.1096(8) 0.4367(9) 0.4256(7) 0.072(3) Uani 1 1 d . . . H11 H 0.0556 0.4291 0.4709 0.086 Uiso 1 1 calc R . . C4 C 0.4398(7) -0.0354(6) 0.2850(5) 0.047(2) Uani 1 1 d . . . H4 H 0.4379 -0.1019 0.3181 0.057 Uiso 1 1 calc R . . C35 C 0.3562(6) 0.1287(5) -0.0097(6) 0.046(2) Uani 1 1 d . . . H35A H 0.2815 0.1335 -0.0077 0.069 Uiso 1 1 calc R . . H35B H 0.3871 0.0916 0.0542 0.069 Uiso 1 1 calc R . . H35C H 0.3977 0.0926 -0.0469 0.069 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 Ga2 0.0191(3) 0.0232(4) 0.0198(4) -0.0122(3) 0.0024(3) -0.0082(3) Ga1 0.0255(4) 0.0193(3) 0.0195(4) -0.0095(3) 0.0034(3) -0.0102(3) Ga5 0.0182(3) 0.0208(3) 0.0191(4) -0.0110(3) 0.0016(3) -0.0074(3) Ga4 0.0197(3) 0.0197(3) 0.0228(4) -0.0127(3) -0.0002(3) -0.0046(3) Ga3 0.0202(3) 0.0200(3) 0.0188(4) -0.0093(3) -0.0014(3) -0.0047(3) Ga6 0.0159(3) 0.0242(4) 0.0227(4) -0.0140(3) 0.0009(3) -0.0058(3) O2 0.019(2) 0.022(2) 0.017(2) -0.0083(18) 0.0030(18) -0.0073(17) O1 0.020(2) 0.022(2) 0.023(2) -0.0133(19) -0.0017(18) -0.0079(17) O7 0.020(2) 0.020(2) 0.020(2) -0.0088(18) -0.0042(18) -0.0066(17) O6 0.018(2) 0.021(2) 0.014(2) -0.0079(18) 0.0023(17) -0.0063(17) O4 0.018(2) 0.025(2) 0.020(2) -0.0088(19) 0.0032(18) -0.0136(17) O12 0.035(3) 0.027(2) 0.031(3) -0.014(2) 0.002(2) -0.016(2) C30 0.022(3) 0.031(4) 0.033(4) -0.020(3) 0.004(3) -0.006(3) O8 0.040(3) 0.043(3) 0.030(3) -0.019(2) 0.012(2) -0.025(2) O3 0.023(2) 0.028(2) 0.025(2) -0.016(2) 0.0054(19) -0.0116(18) O13 0.028(2) 0.058(3) 0.044(3) -0.035(3) 0.021(2) -0.027(2) O5 0.040(3) 0.025(2) 0.019(2) -0.009(2) -0.003(2) -0.004(2) C1 0.042(4) 0.031(4) 0.017(3) -0.013(3) 0.001(3) -0.023(3) O11 0.029(2) 0.044(3) 0.054(3) -0.037(3) 0.005(2) -0.011(2) C36 0.022(3) 0.048(4) 0.035(4) -0.034(4) 0.007(3) -0.013(3) O10 0.047(3) 0.033(3) 0.026(3) -0.007(2) 0.002(2) -0.021(2) C22 0.030(4) 0.026(3) 0.032(4) -0.019(3) 0.005(3) -0.009(3) C16 0.029(3) 0.034(4) 0.020(4) -0.019(3) 0.001(3) -0.010(3) O9 0.046(3) 0.044(3) 0.020(3) -0.006(2) 0.006(2) -0.015(2) C34 0.028(3) 0.038(4) 0.035(4) -0.027(3) 0.008(3) -0.014(3) C2 0.044(4) 0.030(4) 0.024(4) -0.011(3) 0.003(3) -0.019(3) C8 0.030(4) 0.040(4) 0.026(4) -0.022(3) 0.013(3) -0.025(3) C41 0.029(4) 0.034(4) 0.043(5) -0.023(4) -0.004(3) -0.007(3) C29 0.015(3) 0.028(3) 0.026(4) -0.016(3) 0.000(3) -0.002(3) C31 0.028(4) 0.049(4) 0.049(5) -0.035(4) 0.013(3) -0.022(3) C37 0.022(3) 0.047(4) 0.047(5) -0.042(4) 0.001(3) -0.002(3) C15 0.030(3) 0.025(3) 0.015(3) -0.011(3) 0.001(3) -0.002(3) C39 0.018(4) 0.071(6) 0.067(6) -0.056(5) -0.017(4) 0.013(4) C32 0.030(4) 0.056(5) 0.028(4) -0.027(4) 0.007(3) -0.025(3) C17 0.057(5) 0.027(4) 0.033(4) -0.005(3) -0.014(4) -0.011(3) C9 0.042(4) 0.051(4) 0.028(4) -0.021(4) 0.019(3) -0.032(4) C20 0.034(4) 0.028(4) 0.030(4) -0.016(3) 0.005(3) -0.012(3) C42 0.041(4) 0.092(6) 0.063(6) -0.056(5) 0.025(4) -0.042(4) C13 0.027(4) 0.062(5) 0.046(5) -0.043(4) 0.019(3) -0.017(3) C18 0.043(4) 0.057(5) 0.014(4) -0.009(4) -0.015(3) -0.005(4) C38 0.020(4) 0.075(6) 0.069(6) -0.064(5) 0.000(4) -0.008(4) C40 0.033(4) 0.046(4) 0.050(5) -0.034(4) -0.026(4) 0.017(4) C25 0.046(5) 0.046(5) 0.072(6) -0.043(5) 0.000(4) -0.014(4) C3 0.057(5) 0.050(5) 0.025(4) -0.006(4) 0.000(4) -0.039(4) C26 0.060(5) 0.040(4) 0.052(5) -0.032(4) 0.014(4) -0.031(4) C28 0.027(4) 0.064(5) 0.081(6) -0.053(5) 0.004(4) -0.011(4) C27 0.033(4) 0.034(4) 0.038(4) -0.023(3) 0.008(3) -0.018(3) C12 0.031(4) 0.126(8) 0.073(7) -0.077(7) 0.023(5) -0.027(5) C19 0.041(4) 0.055(5) 0.024(4) -0.015(4) -0.003(3) -0.024(4) C33 0.030(4) 0.053(5) 0.028(4) -0.022(4) 0.002(3) -0.015(3) C10 0.051(5) 0.087(6) 0.051(5) -0.047(5) 0.029(4) -0.045(5) C21 0.075(6) 0.044(4) 0.031(5) 0.003(4) -0.005(4) -0.041(4) C23 0.032(4) 0.028(4) 0.034(4) -0.018(3) 0.006(3) -0.008(3) C5 0.083(6) 0.024(4) 0.029(4) -0.011(3) -0.018(4) -0.009(4) C24 0.043(4) 0.040(4) 0.059(5) -0.037(4) 0.004(4) -0.005(3) C14 0.084(7) 0.065(6) 0.025(5) -0.006(4) -0.011(5) -0.005(5) C7 0.055(5) 0.072(6) 0.045(5) -0.032(5) 0.019(4) -0.041(4) C6 0.054(5) 0.025(4) 0.024(4) -0.010(3) -0.003(3) -0.010(3) C11 0.070(7) 0.144(10) 0.071(7) -0.088(8) 0.054(6) -0.076(7) C4 0.092(7) 0.032(4) 0.029(5) -0.008(4) -0.014(5) -0.034(5) C35 0.061(5) 0.036(4) 0.056(5) -0.027(4) 0.011(4) -0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga2 O1 1.843(4) . ? Ga2 O7 1.862(4) . ? Ga2 O4 1.904(4) . ? Ga2 C8 1.938(6) . ? Ga1 O2 1.860(4) . ? Ga1 O1 1.870(4) . ? Ga1 O3 1.927(4) . ? Ga1 C1 1.946(6) . ? Ga5 O2 1.852(4) . ? Ga5 O6 1.867(4) . ? Ga5 O4 1.911(4) 2_665 ? Ga5 C29 1.940(6) . ? Ga4 O5 1.810(4) . ? Ga4 O7 1.895(4) 2_665 ? Ga4 O2 1.909(4) . ? Ga4 C22 1.954(6) . ? Ga3 O5 1.806(4) . ? Ga3 O1 1.889(4) . ? Ga3 O6 1.913(4) 2_665 ? Ga3 C15 1.963(6) . ? Ga6 O7 1.858(4) . ? Ga6 O6 1.873(4) . ? Ga6 O3 1.925(4) . ? Ga6 C36 1.949(6) . ? O7 Ga4 1.895(4) 2_665 ? O6 Ga3 1.913(4) 2_665 ? O4 Ga5 1.911(4) 2_665 ? O12 C30 1.361(7) . ? O12 C35 1.425(7) . ? C30 C29 1.415(9) . ? C30 C31 1.418(8) . ? O8 C2 1.384(8) . ? O8 C7 1.427(8) . ? O13 C37 1.390(8) . ? O13 C42 1.418(8) . ? C1 C2 1.389(9) . ? C1 C6 1.404(9) . ? O11 C23 1.385(7) . ? O11 C28 1.416(8) . ? C36 C37 1.381(10) . ? C36 C41 1.391(9) . ? O10 C16 1.383(7) . ? O10 C21 1.438(8) . ? C22 C23 1.395(8) . ? C22 C27 1.398(8) . ? C16 C17 1.387(8) . ? C16 C15 1.398(9) . ? O9 C9 1.360(8) . ? O9 C14 1.421(8) . ? C34 C33 1.385(8) . ? C34 C29 1.429(8) . ? C2 C3 1.391(9) . ? C8 C13 1.391(8) . ? C8 C9 1.420(9) . ? C41 C40 1.419(8) . ? C31 C32 1.401(9) . ? C37 C38 1.403(9) . ? C15 C20 1.367(8) . ? C39 C38 1.367(11) . ? C39 C40 1.376(11) . ? C32 C33 1.365(9) . ? C17 C18 1.400(9) . ? C9 C10 1.403(10) . ? C20 C19 1.400(8) . ? C13 C12 1.387(11) . ? C18 C19 1.347(10) . ? C25 C24 1.381(9) . ? C25 C26 1.392(10) . ? C3 C4 1.412(10) . ? C26 C27 1.375(9) . ? C12 C11 1.394(12) . ? C10 C11 1.373(11) . ? C23 C24 1.390(9) . ? C5 C4 1.355(11) . ? C5 C6 1.413(10) . ? 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 O1 Ga2 O7 104.11(17) . . ? O1 Ga2 O4 99.46(16) . . ? O7 Ga2 O4 100.64(16) . . ? O1 Ga2 C8 123.3(2) . . ? O7 Ga2 C8 111.6(2) . . ? O4 Ga2 C8 114.8(2) . . ? O2 Ga1 O1 110.71(17) . . ? O2 Ga1 O3 96.26(17) . . ? O1 Ga1 O3 98.91(16) . . ? O2 Ga1 C1 117.0(2) . . ? O1 Ga1 C1 118.5(2) . . ? O3 Ga1 C1 111.6(2) . . ? O2 Ga5 O6 104.51(16) . . ? O2 Ga5 O4 100.92(16) . 2_665 ? O6 Ga5 O4 99.35(17) . 2_665 ? O2 Ga5 C29 124.0(2) . . ? O6 Ga5 C29 118.46(19) . . ? O4 Ga5 C29 105.3(2) 2_665 . ? O5 Ga4 O7 104.08(17) . 2_665 ? O5 Ga4 O2 100.49(18) . . ? O7 Ga4 O2 102.53(16) 2_665 . ? O5 Ga4 C22 120.2(2) . . ? O7 Ga4 C22 116.5(2) 2_665 . ? O2 Ga4 C22 110.5(2) . . ? O5 Ga3 O1 100.86(17) . . ? O5 Ga3 O6 104.33(18) . 2_665 ? O1 Ga3 O6 103.09(16) . 2_665 ? O5 Ga3 C15 113.3(2) . . ? O1 Ga3 C15 123.6(2) . . ? O6 Ga3 C15 109.6(2) 2_665 . ? O7 Ga6 O6 108.80(17) . . ? O7 Ga6 O3 98.51(16) . . ? O6 Ga6 O3 98.11(17) . . ? O7 Ga6 C36 118.8(2) . . ? O6 Ga6 C36 114.0(2) . . ? O3 Ga6 C36 115.7(2) . . ? Ga5 O2 Ga1 124.0(2) . . ? Ga5 O2 Ga4 122.4(2) . . ? Ga1 O2 Ga4 112.65(18) . . ? Ga2 O1 Ga1 121.83(18) . . ? Ga2 O1 Ga3 124.21(19) . . ? Ga1 O1 Ga3 112.77(19) . . ? Ga6 O7 Ga2 122.1(2) . . ? Ga6 O7 Ga4 114.93(19) . 2_665 ? Ga2 O7 Ga4 122.50(19) . 2_665 ? Ga5 O6 Ga6 121.3(2) . . ? Ga5 O6 Ga3 123.1(2) . 2_665 ? Ga6 O6 Ga3 114.18(19) . 2_665 ? Ga2 O4 Ga5 125.5(2) . 2_665 ? C30 O12 C35 117.6(5) . . ? O12 C30 C29 115.1(5) . . ? O12 C30 C31 123.8(6) . . ? C29 C30 C31 121.2(6) . . ? C2 O8 C7 118.5(5) . . ? Ga6 O3 Ga1 125.5(2) . . ? C37 O13 C42 117.9(5) . . ? Ga3 O5 Ga4 129.0(2) . . ? C2 C1 C6 118.3(6) . . ? C2 C1 Ga1 119.5(5) . . ? C6 C1 Ga1 122.2(5) . . ? C23 O11 C28 117.3(5) . . ? C37 C36 C41 118.1(6) . . ? C37 C36 Ga6 121.8(5) . . ? C41 C36 Ga6 120.1(5) . . ? C16 O10 C21 119.3(5) . . ? C23 C22 C27 117.1(6) . . ? C23 C22 Ga4 119.4(5) . . ? C27 C22 Ga4 123.5(5) . . ? O10 C16 C17 123.0(6) . . ? O10 C16 C15 115.1(5) . . ? C17 C16 C15 121.9(6) . . ? C9 O9 C14 117.9(6) . . ? C33 C34 C29 122.1(6) . . ? O8 C2 C1 115.1(6) . . ? O8 C2 C3 122.5(7) . . ? C1 C2 C3 122.3(7) . . ? C13 C8 C9 117.2(6) . . ? C13 C8 Ga2 122.5(5) . . ? C9 C8 Ga2 120.4(5) . . ? C36 C41 C40 121.3(7) . . ? C30 C29 C34 116.5(5) . . ? C30 C29 Ga5 124.9(4) . . ? C34 C29 Ga5 118.6(5) . . ? C32 C31 C30 118.8(6) . . ? C36 C37 O13 115.8(5) . . ? C36 C37 C38 121.9(7) . . ? O13 C37 C38 122.3(7) . . ? C20 C15 C16 117.3(5) . . ? C20 C15 Ga3 123.8(5) . . ? C16 C15 Ga3 118.1(4) . . ? C38 C39 C40 122.8(6) . . ? C33 C32 C31 121.6(6) . . ? C16 C17 C18 118.2(6) . . ? O9 C9 C10 123.3(7) . . ? O9 C9 C8 114.4(6) . . ? C10 C9 C8 122.3(7) . . ? C15 C20 C19 122.2(6) . . ? C12 C13 C8 121.9(8) . . ? C19 C18 C17 121.3(6) . . ? C39 C38 C37 118.3(8) . . ? C39 C40 C41 117.7(7) . . ? C24 C25 C26 119.0(7) . . ? C2 C3 C4 118.3(7) . . ? C27 C26 C25 120.0(6) . . ? C26 C27 C22 122.2(6) . . ? C13 C12 C11 118.5(8) . . ? C18 C19 C20 119.1(6) . . ? C32 C33 C34 119.9(6) . . ? C11 C10 C9 117.1(8) . . ? O11 C23 C24 124.3(6) . . ? O11 C23 C22 114.7(5) . . ? C24 C23 C22 121.0(6) . . ? C4 C5 C6 121.3(7) . . ? C25 C24 C23 120.7(7) . . ? C1 C6 C5 119.3(7) . . ? C10 C11 C12 123.0(8) . . ? C5 C4 C3 120.2(7) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.730 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.168 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 634233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Isopropylgalloxane _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 Ga2 O3' _chemical_formula_sum 'C6 H15 Ga2 O3' _chemical_formula_weight 274.62 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pa-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-y+1/2, -z, x+1/2' 'z+1/2, -x+1/2, -y' '-y, z+1/2, -x+1/2' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' 'y-1/2, z, -x-1/2' '-z-1/2, x-1/2, y' 'y, -z-1/2, x-1/2' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y-1/2, z-1/2, x' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.044(3) _cell_length_b 19.044(2) _cell_length_c 19.044(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6906.2(14) _cell_formula_units_Z 24 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 4.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3895 _exptl_absorpt_correction_T_max 0.4566 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5024 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2836 _reflns_number_gt 1789 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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. The galloxane clusters pack so as to form an interstitial space that is occupied by disordered water molecules. One of these water molecules was been modelled over three posi- tions. The routine SQUEEZE was then applied to the data to remove the rem- aining diffuse electron density found in this region of the extended stru- cture. ; _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^)+(0.1261P)^2^+0.0871P] 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 2836 _refine_ls_number_parameters 95 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.2064 _refine_ls_wR_factor_gt 0.1856 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.001 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 0.97591(4) 0.45172(4) 0.15455(3) 0.0459(3) Uani 1 1 d . A . O1 O 0.9225(2) 0.4225(2) 0.0775(2) 0.0430(16) Uani 1 3 d S . . C1 C 1.2046(4) 0.3747(5) 0.1096(5) 0.072(2) Uani 1 1 d D . . Ga2 Ga 1.11563(4) 0.40631(4) 0.06863(4) 0.0484(3) Uani 1 1 d . A . O2 O 0.9381(3) 0.5447(2) 0.1634(2) 0.0532(11) Uani 1 1 d . . . C2 C 1.1952(8) 0.3409(8) 0.1818(8) 0.134(5) Uiso 1 1 d . A . H2A H 1.1628 0.3010 0.1780 0.201 Uiso 1 1 calc R . . H2B H 1.1759 0.3755 0.2146 0.201 Uiso 1 1 calc R . . H2C H 1.2408 0.3244 0.1991 0.201 Uiso 1 1 calc R . . O3 O 1.0636(2) 0.4751(2) 0.1158(2) 0.0434(10) Uani 1 1 d . . . C3 C 1.2373(8) 0.3194(8) 0.0698(8) 0.077(4) Uiso 0.60 1 d PD A 1 H3A H 1.2169 0.3178 0.0226 0.116 Uiso 0.60 1 calc PR . . H3B H 1.2293 0.2743 0.0934 0.116 Uiso 0.60 1 calc PR . . H3C H 1.2878 0.3283 0.0664 0.116 Uiso 0.60 1 calc PR . . O4 O 0.8963(12) 0.5679(11) 0.3042(10) 0.056(5) Uiso 0.33 1 d P . . C4 C 0.9729(5) 0.3953(5) 0.2405(4) 0.073(2) Uani 1 1 d . . . H4 H 0.9899 0.3472 0.2279 0.087 Uiso 1 1 calc R A . O5 O 0.8825(10) 0.5896(10) 0.2950(9) 0.051(4) Uiso 0.33 1 d P . . C5 C 1.0233(7) 0.4241(7) 0.2986(7) 0.117(4) Uiso 1 1 d . A . H5A H 0.9955 0.4462 0.3359 0.175 Uiso 1 1 calc R . . H5B H 1.0552 0.4588 0.2780 0.175 Uiso 1 1 calc R . . H5C H 1.0506 0.3852 0.3184 0.175 Uiso 1 1 calc R . . O6 O 0.9159(10) 0.5897(10) 0.3075(8) 0.051(4) Uiso 0.33 1 d P . . C6 C 0.8989(7) 0.3877(7) 0.2654(8) 0.124(4) Uiso 1 1 d . A . H6A H 0.8978 0.3573 0.3070 0.186 Uiso 1 1 calc R . . H6B H 0.8703 0.3668 0.2281 0.186 Uiso 1 1 calc R . . H6C H 0.8801 0.4341 0.2776 0.186 Uiso 1 1 calc R . . C7 C 1.2692(14) 0.4192(17) 0.1072(18) 0.120(10) Uiso 0.40 1 d PD A 2 H7A H 1.2648 0.4577 0.1410 0.180 Uiso 0.00 1 calc PR A 2 H7B H 1.2750 0.4384 0.0598 0.180 Uiso 0.00 1 calc PR A 2 H7C H 1.3102 0.3905 0.1192 0.180 Uiso 0.00 1 calc PR A 2 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 0.0517(5) 0.0498(5) 0.0362(4) 0.0050(3) 0.0002(3) -0.0023(3) O1 0.0430(16) 0.0430(16) 0.0430(16) 0.0040(18) 0.0040(18) -0.0040(18) C1 0.046(4) 0.101(7) 0.070(5) 0.021(5) 0.000(4) 0.025(4) Ga2 0.0421(4) 0.0511(5) 0.0518(5) 0.0076(3) -0.0056(3) 0.0089(3) O2 0.060(3) 0.054(3) 0.045(2) -0.002(2) 0.010(2) 0.005(2) O3 0.040(2) 0.044(2) 0.045(2) 0.0018(18) -0.0028(18) -0.0007(18) C4 0.099(6) 0.078(5) 0.041(4) 0.010(4) 0.004(4) -0.012(5) _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 O1 1.8701(8) . ? Ga1 O3 1.879(4) . ? Ga1 O2 1.918(5) . ? Ga1 C4 1.959(8) . ? O1 Ga1 1.8701(8) 9_556 ? O1 Ga1 1.8701(8) 8_645 ? C1 C3 1.439(13) . ? C1 C7 1.495(18) . ? C1 C2 1.529(16) . ? C1 Ga2 1.959(7) . ? Ga2 O3 1.871(4) 20_675 ? Ga2 O3 1.872(4) . ? Ga2 O2 1.899(5) 9_556 ? O2 Ga2 1.899(5) 8_645 ? O3 Ga2 1.871(4) 21_764 ? O4 O5 0.52(2) . ? O4 O6 0.56(2) . ? C4 C6 1.495(16) . ? C4 C5 1.563(15) . ? O5 O6 0.68(2) . ? 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 O1 Ga1 O3 104.2(2) . . ? O1 Ga1 O2 98.03(16) . . ? O3 Ga1 O2 98.60(19) . . ? O1 Ga1 C4 118.5(3) . . ? O3 Ga1 C4 118.9(3) . . ? O2 Ga1 C4 115.0(3) . . ? Ga1 O1 Ga1 119.89(2) . 9_556 ? Ga1 O1 Ga1 119.89(2) . 8_645 ? Ga1 O1 Ga1 119.89(2) 9_556 8_645 ? C3 C1 C7 92.4(15) . . ? C3 C1 C2 102.4(10) . . ? C7 C1 C2 111.3(15) . . ? C3 C1 Ga2 112.9(8) . . ? C7 C1 Ga2 121.7(15) . . ? C2 C1 Ga2 112.7(7) . . ? O3 Ga2 O3 104.1(2) 20_675 . ? O3 Ga2 O2 98.7(2) 20_675 9_556 ? O3 Ga2 O2 98.34(19) . 9_556 ? O3 Ga2 C1 118.1(3) 20_675 . ? O3 Ga2 C1 118.7(3) . . ? O2 Ga2 C1 115.3(3) 9_556 . ? Ga2 O2 Ga1 128.4(2) 8_645 . ? Ga2 O3 Ga2 120.2(2) 21_764 . ? Ga2 O3 Ga1 119.9(2) 21_764 . ? Ga2 O3 Ga1 119.6(2) . . ? O5 O4 O6 78(4) . . ? C6 C4 C5 112.8(9) . . ? C6 C4 Ga1 110.2(8) . . ? C5 C4 Ga1 112.4(7) . . ? O4 O5 O6 54(3) . . ? O4 O6 O5 49(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.175 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.167 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 634234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C67.67 H78 Br2.34 Ga7 O10.50' _chemical_formula_sum 'C67.67 H78 Br2.34 Ga7 O10.50' _chemical_formula_weight 1733.91 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.011(3) _cell_length_b 16.203(3) _cell_length_c 16.717(3) _cell_angle_alpha 77.42(3) _cell_angle_beta 61.60(3) _cell_angle_gamma 74.52(3) _cell_volume 3655.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1733 _exptl_absorpt_coefficient_mu 3.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4446 _exptl_absorpt_correction_T_max 0.5116 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19696 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0992 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 30.10 _reflns_number_total 19696 _reflns_number_gt 11636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.0707P)^2^+17.9185P] 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 19696 _refine_ls_number_parameters 814 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1434 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.024 _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 Ga2 Ga 0.47880(5) -0.00055(4) 0.19374(4) 0.02404(15) Uani 1 1 d . . . Ga3 Ga 0.33766(5) 0.13772(4) 0.12087(4) 0.02457(15) Uani 1 1 d . . . Ga1 Ga 0.56380(5) 0.15137(4) 0.03323(4) 0.02429(15) Uani 1 1 d . . . Ga5 Ga 0.68533(5) 0.06056(4) -0.15442(4) 0.02441(15) Uani 1 1 d . . . Ga6 Ga 0.68659(5) -0.05670(4) 0.02671(4) 0.02422(15) Uani 1 1 d . . . Ga4 Ga 0.47200(5) 0.17958(4) -0.10802(4) 0.02483(15) Uani 1 1 d . . . O2 O 0.5769(3) 0.1351(3) -0.0801(3) 0.0256(9) Uani 1 1 d . . . O5 O 0.3728(3) 0.2098(2) 0.0092(3) 0.0253(9) Uani 1 1 d . . . O1 O 0.4587(3) 0.0997(2) 0.1205(3) 0.0247(9) Uani 1 1 d . . . O7 O 0.5656(3) -0.0816(2) 0.1117(3) 0.0241(9) Uani 1 1 d . . . O6 O 0.3156(3) 0.0470(3) 0.0859(3) 0.0241(9) Uani 1 1 d . . . O4 O 0.3625(3) -0.0400(3) 0.2313(3) 0.0269(9) Uani 1 1 d . . . C8 C 0.5203(4) 0.0055(4) 0.2842(4) 0.0261(13) Uani 1 1 d . . . O3 O 0.6664(3) 0.0620(3) 0.0373(3) 0.0263(9) Uani 1 1 d . . . O9 O 0.2582(3) -0.0492(3) 0.4051(3) 0.0358(11) Uani 1 1 d . . . C15 C 0.2377(4) 0.1827(4) 0.2344(4) 0.0271(13) Uani 1 1 d . . . C1 C 0.5585(5) 0.2668(4) 0.0538(4) 0.0281(13) Uani 1 1 d . . . C22 C 0.4974(5) 0.2687(4) -0.2093(4) 0.0301(14) Uani 1 1 d . . . C29 C 0.8125(4) 0.0909(4) -0.2102(4) 0.0282(13) Uani 1 1 d . . . C37 C 0.8860(5) -0.1546(4) -0.0278(4) 0.0329(14) Uani 1 1 d . . . H37 H 0.8966 -0.1334 -0.0888 0.039 Uiso 1 1 calc R . . C30 C 0.8279(5) 0.1734(4) -0.2174(5) 0.0368(16) Uani 1 1 d . . . H30 H 0.7741 0.2194 -0.1970 0.044 Uiso 1 1 calc R . . C9 C 0.5255(5) 0.0825(4) 0.3043(4) 0.0311(14) Uani 1 1 d . . . H9 H 0.5016 0.1357 0.2779 0.037 Uiso 1 1 calc R . . C36 C 0.7952(5) -0.1313(4) 0.0437(4) 0.0309(14) Uani 1 1 d . . . C16 C 0.2618(5) 0.1883(4) 0.3028(4) 0.0343(15) Uani 1 1 d . . . H16 H 0.3273 0.1718 0.2928 0.041 Uiso 1 1 calc R . . C5 C 0.4675(6) 0.3974(5) 0.1251(5) 0.050(2) Uani 1 1 d . . . H5 H 0.4070 0.4287 0.1642 0.060 Uiso 1 1 calc R . . O10 O 0.2515(4) 0.3526(3) 0.0209(4) 0.0612(16) Uani 1 1 d . . . C38 C 0.9616(5) -0.2084(5) -0.0118(5) 0.0405(16) Uani 1 1 d . . . H38 H 1.0227 -0.2233 -0.0621 0.049 Uiso 1 1 calc R . . C2 C 0.6405(5) 0.3041(4) 0.0120(5) 0.0415(17) Uani 1 1 d . . . H2 H 0.7007 0.2731 -0.0278 0.050 Uiso 1 1 calc R . . C12 C 0.5959(5) -0.0714(5) 0.3820(4) 0.0368(15) Uani 1 1 d . . . H12 H 0.6197 -0.1245 0.4085 0.044 Uiso 1 1 calc R . . C20 C 0.1403(5) 0.2068(4) 0.2520(4) 0.0331(14) Uani 1 1 d . . . H20 H 0.1222 0.2030 0.2067 0.040 Uiso 1 1 calc R . . C10 C 0.5650(5) 0.0828(5) 0.3620(5) 0.0351(15) Uani 1 1 d . . . H10 H 0.5666 0.1361 0.3756 0.042 Uiso 1 1 calc R . . C50 C 0.1569(5) -0.0127(5) 0.4438(5) 0.0413(17) Uani 1 1 d . . . H50A H 0.1403 0.0259 0.3966 0.050 Uiso 1 1 calc R . . H50B H 0.1395 0.0213 0.4939 0.050 Uiso 1 1 calc R . . C11 C 0.6024(5) 0.0060(5) 0.4006(4) 0.0361(16) Uani 1 1 d . . . C25 C 0.5425(6) 0.4040(4) -0.3544(5) 0.0387(17) Uani 1 1 d . . . C4 C 0.5475(6) 0.4353(5) 0.0851(5) 0.0454(19) Uani 1 1 d . . . C33 C 0.9862(5) 0.0418(5) -0.2783(5) 0.0382(16) Uani 1 1 d . . . H33 H 1.0401 -0.0042 -0.2981 0.046 Uiso 1 1 calc R . . C34 C 0.8938(5) 0.0257(4) -0.2428(5) 0.0360(15) Uani 1 1 d . . . H34 H 0.8855 -0.0308 -0.2406 0.043 Uiso 1 1 calc R . . C23 C 0.4273(6) 0.3225(5) -0.2335(5) 0.0488(19) Uani 1 1 d . . . H23 H 0.3625 0.3135 -0.2009 0.059 Uiso 1 1 calc R . . C18 C 0.0940(5) 0.2431(5) 0.4027(5) 0.0376(16) Uani 1 1 d . . . C32 C 1.0014(5) 0.1239(5) -0.2854(5) 0.0424(17) Uani 1 1 d . . . C27 C 0.5905(6) 0.2847(5) -0.2610(5) 0.0475(19) Uani 1 1 d . . . H27 H 0.6409 0.2500 -0.2469 0.057 Uiso 1 1 calc R . . C48 C 0.1813(6) -0.1658(5) 0.4568(5) 0.0443(18) Uani 1 1 d . . . H48A H 0.1642 -0.2136 0.5064 0.053 Uiso 1 1 calc R . . H48B H 0.1934 -0.1851 0.3993 0.053 Uiso 1 1 calc R . . C13 C 0.5549(5) -0.0715(4) 0.3250(4) 0.0330(14) Uani 1 1 d . . . H13 H 0.5505 -0.1247 0.3136 0.040 Uiso 1 1 calc R . . C41 C 0.7834(6) -0.1639(5) 0.1313(5) 0.0458(19) Uani 1 1 d . . . H41 H 0.7223 -0.1494 0.1817 0.055 Uiso 1 1 calc R . . C19 C 0.0697(5) 0.2362(5) 0.3346(5) 0.0383(16) Uani 1 1 d . . . H19 H 0.0041 0.2519 0.3451 0.046 Uiso 1 1 calc R . . C17 C 0.1903(5) 0.2182(5) 0.3860(5) 0.0382(16) Uani 1 1 d . . . H17 H 0.2081 0.2214 0.4318 0.046 Uiso 1 1 calc R . . C49 C 0.1022(5) -0.0869(5) 0.4805(5) 0.0435(17) Uani 1 1 d . . . H49A H 0.0617 -0.0882 0.5474 0.052 Uiso 1 1 calc R . . H49B H 0.0604 -0.0822 0.4505 0.052 Uiso 1 1 calc R . . C31 C 0.9207(5) 0.1892(5) -0.2538(5) 0.0454(18) Uani 1 1 d . . . H31 H 0.9293 0.2458 -0.2572 0.054 Uiso 1 1 calc R . . C3 C 0.6341(6) 0.3878(5) 0.0288(6) 0.0482(19) Uani 1 1 d . . . H3 H 0.6908 0.4120 0.0006 0.058 Uiso 1 1 calc R . . C14 C 0.6496(5) 0.0060(6) 0.4591(5) 0.049(2) Uani 1 1 d . . . H14A H 0.6541 -0.0507 0.4940 0.074 Uiso 1 1 calc R . . H14B H 0.6110 0.0501 0.5014 0.074 Uiso 1 1 calc R . . H14C H 0.7147 0.0187 0.4202 0.074 Uiso 1 1 calc R . . C24 C 0.4499(7) 0.3890(5) -0.3044(6) 0.058(2) Uani 1 1 d . . . H24 H 0.3999 0.4249 -0.3183 0.070 Uiso 1 1 calc R . . C26 C 0.6124(6) 0.3507(5) -0.3333(6) 0.056(2) Uani 1 1 d . . . H26 H 0.6775 0.3583 -0.3685 0.067 Uiso 1 1 calc R . . C51 C 0.2136(9) 0.4019(6) 0.0972(7) 0.085(4) Uani 1 1 d . . . H51A H 0.2519 0.4467 0.0821 0.102 Uiso 0.50 1 calc PR . . H51B H 0.2152 0.3640 0.1517 0.102 Uiso 0.50 1 calc PR . . C6 C 0.4724(5) 0.3147(5) 0.1100(5) 0.0422(17) Uani 1 1 d . . . H6 H 0.4155 0.2908 0.1389 0.051 Uiso 1 1 calc R . . C35 C 1.1033(6) 0.1426(6) -0.3269(7) 0.067(3) Uani 1 1 d . . . H35A H 1.1350 0.1112 -0.2884 0.100 Uiso 1 1 calc R . . H35B H 1.0995 0.2045 -0.3304 0.100 Uiso 1 1 calc R . . H35C H 1.1407 0.1240 -0.3885 0.100 Uiso 1 1 calc R . . C39 C 0.9492(7) -0.2405(5) 0.0756(6) 0.057(2) Uani 1 1 d . . . C21 C 0.0177(6) 0.2761(6) 0.4918(5) 0.058(2) Uani 1 1 d . . . H21A H -0.0350 0.3165 0.4818 0.087 Uiso 1 1 calc R . . H21B H 0.0461 0.3056 0.5154 0.087 Uiso 1 1 calc R . . H21C H -0.0076 0.2277 0.5361 0.087 Uiso 1 1 calc R . . C47 C 0.2679(5) -0.1367(5) 0.4458(5) 0.0412(17) Uani 1 1 d . . . H47A H 0.2675 -0.1399 0.5058 0.049 Uiso 1 1 calc R . . H47B H 0.3286 -0.1725 0.4055 0.049 Uiso 1 1 calc R . . C54 C 0.1857(8) 0.3696(6) -0.0197(8) 0.072(3) Uani 1 1 d . . . H54A H 0.1834 0.3162 -0.0376 0.087 Uiso 0.50 1 calc PR . . H54B H 0.2046 0.4126 -0.0741 0.087 Uiso 0.50 1 calc PR . . C40 C 0.8582(7) -0.2169(6) 0.1471(6) 0.065(3) Uani 1 1 d . . . H40 H 0.8475 -0.2379 0.2082 0.079 Uiso 1 1 calc R . . C28 C 0.5675(7) 0.4766(5) -0.4305(6) 0.061(2) Uani 1 1 d . . . H28A H 0.6125 0.5049 -0.4271 0.092 Uiso 1 1 calc R . . H28B H 0.5084 0.5185 -0.4241 0.092 Uiso 1 1 calc R . . H28C H 0.5977 0.4536 -0.4896 0.092 Uiso 1 1 calc R . . C52 C 0.1103(13) 0.4426(12) 0.1148(11) 0.161(9) Uani 1 1 d D . . H52A H 0.0656 0.4306 0.1801 0.193 Uiso 0.50 1 calc PR . . H52B H 0.1037 0.5058 0.0990 0.193 Uiso 0.50 1 calc PR . . C7 C 0.5417(8) 0.5239(5) 0.1038(6) 0.064(3) Uani 1 1 d . . . H7A H 0.6004 0.5256 0.1076 0.095 Uiso 1 1 calc R . . H7B H 0.4851 0.5375 0.1618 0.095 Uiso 1 1 calc R . . H7C H 0.5359 0.5662 0.0541 0.095 Uiso 1 1 calc R . . Ga7 Ga 0.77236(7) 0.33343(6) 0.28501(7) 0.0591(3) Uani 1 1 d D . . O8 O 0.7895(3) 0.1266(3) 0.0473(3) 0.0398(11) Uani 1 1 d . . . C46 C 0.7580(5) 0.1440(5) 0.1402(5) 0.0399(17) Uani 1 1 d . . . H46A H 0.6867 0.1610 0.1721 0.048 Uiso 1 1 calc R . . H46B H 0.7874 0.1906 0.1402 0.048 Uiso 1 1 calc R . . C59 C 0.6382(6) 0.3152(5) 0.3488(6) 0.0460(19) Uani 1 1 d . A . C60 C 0.5932(6) 0.2969(4) 0.4412(6) 0.0424(18) Uani 1 1 d . . . H60 H 0.6286 0.2889 0.4754 0.051 Uiso 1 1 calc R A . C64 C 0.5822(8) 0.3251(6) 0.3000(7) 0.065(3) Uani 1 1 d . . . H64 H 0.6105 0.3382 0.2354 0.078 Uiso 1 1 calc R A . C45 C 0.7924(6) 0.0607(5) 0.1848(6) 0.050(2) Uani 1 1 d . . . H45A H 0.7488 0.0195 0.2039 0.061 Uiso 1 1 calc R . . H45B H 0.7980 0.0698 0.2387 0.061 Uiso 1 1 calc R . . C61 C 0.4940(6) 0.2894(4) 0.4876(6) 0.051(2) Uani 1 1 d . A . H61 H 0.4643 0.2780 0.5524 0.061 Uiso 1 1 calc R . . C43 C 0.8829(5) 0.0711(6) 0.0211(6) 0.056(2) Uani 1 1 d . . . H43A H 0.9348 0.1047 -0.0172 0.067 Uiso 1 1 calc R . . H43B H 0.8893 0.0262 -0.0143 0.067 Uiso 1 1 calc R . . C44 C 0.8899(6) 0.0302(6) 0.1093(7) 0.066(3) Uani 1 1 d . . . H44A H 0.9044 -0.0334 0.1121 0.079 Uiso 1 1 calc R . . H44B H 0.9413 0.0491 0.1138 0.079 Uiso 1 1 calc R . . C63 C 0.4846(7) 0.3152(6) 0.3488(8) 0.066(3) Uani 1 1 d . A . H63 H 0.4486 0.3206 0.3157 0.080 Uiso 1 1 calc R . . C62 C 0.4403(7) 0.2984(5) 0.4413(8) 0.063(3) Uani 1 1 d . . . C42 C 1.0341(9) -0.2963(8) 0.0920(8) 0.099(4) Uani 1 1 d . . . H42A H 1.0392 -0.3565 0.0861 0.149 Uiso 1 1 calc R . . H42B H 1.0236 -0.2914 0.1537 0.149 Uiso 1 1 calc R . . H42C H 1.0940 -0.2768 0.0468 0.149 Uiso 1 1 calc R . . C65 C 0.3352(8) 0.2940(7) 0.4900(10) 0.097(4) Uani 1 1 d . A . H65A H 0.2994 0.3419 0.4647 0.145 Uiso 1 1 calc R . . H65B H 0.3109 0.2979 0.5553 0.145 Uiso 1 1 calc R . . H65C H 0.3265 0.2392 0.4819 0.145 Uiso 1 1 calc R . . C53 C 0.0885(9) 0.4047(11) 0.0572(13) 0.136(6) Uani 1 1 d D . . H53A H 0.0488 0.4487 0.0317 0.164 Uiso 0.50 1 calc PR . . H53B H 0.0525 0.3576 0.0931 0.164 Uiso 0.50 1 calc PR . . Br1 Br 0.88113(6) 0.19728(5) 0.27859(5) 0.04663(19) Uani 1 1 d . A . Br4 Br 0.8104(2) 0.3981(2) 0.3810(2) 0.0604(10) Uani 0.33 1 d P A 2 Br2 Br 0.80383(13) 0.38501(11) 0.12280(12) 0.0695(4) Uani 0.67 1 d P A 1 Br3 Br 0.8244(3) 0.4036(2) 0.1536(2) 0.0680(10) Uani 0.33 1 d PD A 3 C57 C 0.2120(16) 0.5806(11) 0.2963(15) 0.081(7) Uani 0.50 1 d PD . . H57A H 0.1618 0.6296 0.3266 0.098 Uiso 0.50 1 calc PR . . H57B H 0.2731 0.6012 0.2543 0.098 Uiso 0.50 1 calc PR . . O11 O 0.1527(17) 0.4625(12) 0.3931(14) 0.141(8) Uani 0.50 1 d PD . . C56 C 0.1822(19) 0.5407(13) 0.2499(12) 0.088(7) Uani 0.50 1 d PD . . H56A H 0.2322 0.5336 0.1862 0.105 Uiso 0.50 1 calc PR . . H56B H 0.1207 0.5737 0.2493 0.105 Uiso 0.50 1 calc PR . . C58 C 0.2260(17) 0.5080(11) 0.3657(17) 0.093(8) Uani 0.50 1 d PD . . H58A H 0.2903 0.4704 0.3377 0.111 Uiso 0.50 1 calc PR . . H58B H 0.2207 0.5310 0.4185 0.111 Uiso 0.50 1 calc PR . . C55 C 0.169(2) 0.4540(12) 0.3077(13) 0.096(9) Uani 0.50 1 d PD . . H55A H 0.1138 0.4352 0.3103 0.115 Uiso 0.50 1 calc PR . . H55B H 0.2280 0.4101 0.2801 0.115 Uiso 0.50 1 calc PR . . C72 C 0.9130(15) 0.6070(13) 0.3806(14) 0.103(6) Uiso 0.67 1 d P A 1 H72A H 0.9836 0.5998 0.3476 0.154 Uiso 0.67 1 calc PR A 1 H72B H 0.8929 0.6010 0.4466 0.154 Uiso 0.67 1 calc PR A 1 H72C H 0.8837 0.6642 0.3619 0.154 Uiso 0.67 1 calc PR A 1 C69 C 0.8814(13) 0.5407(10) 0.3593(11) 0.086(5) Uiso 0.67 1 d PD A 1 C71 C 0.8313(9) 0.4059(8) 0.3863(8) 0.017(3) Uiso 0.67 1 d PD A 1 H71 H 0.8158 0.3550 0.4265 0.021 Uiso 0.67 1 calc PR A 1 C67 C 0.8150(14) 0.5042(10) 0.2688(13) 0.107(6) Uiso 0.67 1 d PD A 1 H67 H 0.7981 0.5228 0.2195 0.128 Uiso 0.67 1 calc PR A 1 C68 C 0.8489(7) 0.5594(6) 0.2969(7) 0.118(7) Uiso 0.67 1 d PD A 1 H68 H 0.8483 0.6166 0.2674 0.142 Uiso 0.67 1 calc PR A 1 C70 C 0.8793(7) 0.4593(6) 0.4079(7) 0.121(7) Uiso 0.67 1 d PRD A 1 H70 H 0.9005 0.4348 0.4537 0.146 Uiso 1 1 d R A 1 C66 C 0.8069(7) 0.4215(6) 0.3155(7) 0.059(3) Uiso 0.67 1 d PRD A 1 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 Ga2 0.0282(3) 0.0245(3) 0.0194(3) -0.0031(3) -0.0097(3) -0.0062(3) Ga3 0.0274(3) 0.0235(3) 0.0207(3) -0.0043(3) -0.0084(3) -0.0047(3) Ga1 0.0285(3) 0.0219(3) 0.0223(3) -0.0033(3) -0.0098(3) -0.0065(3) Ga5 0.0271(3) 0.0244(3) 0.0203(3) -0.0015(3) -0.0085(3) -0.0073(3) Ga6 0.0266(3) 0.0236(3) 0.0224(3) -0.0028(3) -0.0105(3) -0.0053(3) Ga4 0.0298(4) 0.0221(3) 0.0214(3) -0.0015(3) -0.0102(3) -0.0060(3) O2 0.027(2) 0.024(2) 0.022(2) -0.0052(17) -0.0077(18) -0.0047(17) O5 0.029(2) 0.022(2) 0.019(2) -0.0026(16) -0.0067(18) -0.0039(17) O1 0.029(2) 0.021(2) 0.024(2) -0.0002(16) -0.0109(18) -0.0066(17) O7 0.027(2) 0.022(2) 0.018(2) -0.0054(16) -0.0036(17) -0.0069(17) O6 0.029(2) 0.024(2) 0.020(2) -0.0019(16) -0.0105(18) -0.0059(17) O4 0.029(2) 0.030(2) 0.021(2) -0.0012(17) -0.0095(18) -0.0091(18) C8 0.027(3) 0.034(3) 0.017(3) -0.003(2) -0.009(3) -0.005(3) O3 0.030(2) 0.023(2) 0.028(2) -0.0025(17) -0.0152(19) -0.0050(18) O9 0.030(2) 0.046(3) 0.025(2) 0.003(2) -0.008(2) -0.011(2) C15 0.029(3) 0.021(3) 0.026(3) -0.002(2) -0.007(3) -0.006(2) C1 0.042(4) 0.021(3) 0.029(3) 0.000(2) -0.021(3) -0.008(3) C22 0.042(4) 0.023(3) 0.027(3) 0.000(3) -0.017(3) -0.008(3) C29 0.024(3) 0.036(3) 0.021(3) 0.002(3) -0.007(3) -0.011(3) C37 0.034(4) 0.035(4) 0.027(3) -0.002(3) -0.013(3) -0.006(3) C30 0.034(4) 0.026(3) 0.041(4) 0.001(3) -0.011(3) -0.007(3) C9 0.033(3) 0.029(3) 0.037(4) -0.009(3) -0.019(3) -0.004(3) C36 0.039(4) 0.025(3) 0.029(3) 0.000(3) -0.017(3) -0.006(3) C16 0.032(4) 0.041(4) 0.031(4) -0.010(3) -0.011(3) -0.009(3) C5 0.062(5) 0.034(4) 0.042(4) -0.015(3) -0.006(4) -0.013(4) O10 0.067(4) 0.035(3) 0.067(4) -0.015(3) -0.028(3) 0.016(3) C38 0.027(3) 0.043(4) 0.045(4) -0.009(3) -0.013(3) 0.001(3) C2 0.043(4) 0.029(4) 0.047(4) -0.007(3) -0.013(4) -0.009(3) C12 0.039(4) 0.045(4) 0.027(3) 0.001(3) -0.019(3) -0.006(3) C20 0.030(3) 0.038(4) 0.030(3) -0.010(3) -0.011(3) -0.004(3) C10 0.029(3) 0.043(4) 0.035(4) -0.014(3) -0.012(3) -0.007(3) C50 0.035(4) 0.040(4) 0.034(4) -0.005(3) -0.005(3) -0.006(3) C11 0.027(3) 0.059(5) 0.021(3) -0.012(3) -0.006(3) -0.007(3) C25 0.062(5) 0.023(3) 0.031(4) 0.001(3) -0.021(4) -0.009(3) C4 0.071(6) 0.032(4) 0.039(4) -0.006(3) -0.025(4) -0.017(4) C33 0.025(3) 0.044(4) 0.037(4) -0.003(3) -0.011(3) 0.002(3) C34 0.046(4) 0.028(3) 0.038(4) 0.000(3) -0.025(3) -0.005(3) C23 0.049(5) 0.051(5) 0.050(5) 0.014(4) -0.028(4) -0.018(4) C18 0.034(4) 0.042(4) 0.032(4) -0.017(3) -0.006(3) -0.008(3) C32 0.030(4) 0.051(5) 0.042(4) 0.009(3) -0.015(3) -0.013(3) C27 0.042(4) 0.041(4) 0.047(4) 0.019(3) -0.019(4) -0.009(3) C48 0.053(5) 0.043(4) 0.036(4) -0.001(3) -0.018(4) -0.013(4) C13 0.037(4) 0.034(4) 0.029(3) -0.005(3) -0.015(3) -0.005(3) C41 0.049(4) 0.046(4) 0.026(4) -0.003(3) -0.013(3) 0.009(4) C19 0.029(3) 0.046(4) 0.038(4) -0.016(3) -0.012(3) 0.000(3) C17 0.041(4) 0.046(4) 0.034(4) -0.012(3) -0.017(3) -0.011(3) C49 0.034(4) 0.048(4) 0.038(4) -0.003(3) -0.008(3) -0.009(3) C31 0.042(4) 0.040(4) 0.056(5) 0.006(4) -0.021(4) -0.020(3) C3 0.057(5) 0.035(4) 0.060(5) 0.001(4) -0.026(4) -0.024(4) C14 0.037(4) 0.082(6) 0.030(4) -0.018(4) -0.013(3) -0.007(4) C24 0.067(6) 0.048(5) 0.071(6) 0.011(4) -0.049(5) -0.008(4) C26 0.051(5) 0.045(5) 0.056(5) 0.017(4) -0.018(4) -0.016(4) C51 0.119(10) 0.044(5) 0.063(6) -0.023(5) -0.021(6) 0.008(6) C6 0.042(4) 0.037(4) 0.039(4) -0.013(3) -0.005(3) -0.012(3) C35 0.036(4) 0.069(6) 0.086(7) 0.006(5) -0.024(5) -0.016(4) C39 0.068(6) 0.050(5) 0.050(5) -0.008(4) -0.039(5) 0.020(4) C21 0.048(5) 0.078(6) 0.040(4) -0.033(4) -0.003(4) -0.012(4) C47 0.045(4) 0.049(4) 0.024(3) 0.006(3) -0.012(3) -0.014(3) C54 0.081(7) 0.048(5) 0.090(8) -0.016(5) -0.049(6) 0.010(5) C40 0.080(7) 0.066(6) 0.036(4) -0.007(4) -0.034(5) 0.027(5) C28 0.090(7) 0.035(4) 0.057(5) 0.015(4) -0.037(5) -0.016(4) C52 0.160(15) 0.158(15) 0.122(13) -0.076(12) -0.074(12) 0.109(13) C7 0.103(8) 0.037(4) 0.059(5) -0.012(4) -0.032(5) -0.029(5) Ga7 0.0492(5) 0.0475(5) 0.0690(7) -0.0268(5) -0.0135(5) 0.0007(4) O8 0.029(2) 0.045(3) 0.044(3) -0.018(2) -0.009(2) -0.008(2) C46 0.030(4) 0.045(4) 0.049(4) -0.016(3) -0.014(3) -0.012(3) C59 0.042(4) 0.034(4) 0.062(5) -0.022(4) -0.023(4) 0.005(3) C60 0.060(5) 0.019(3) 0.065(5) 0.005(3) -0.047(4) -0.004(3) C64 0.093(8) 0.048(5) 0.057(6) -0.018(4) -0.041(6) 0.009(5) C45 0.042(4) 0.044(4) 0.062(5) -0.005(4) -0.022(4) -0.006(4) C61 0.062(5) 0.024(4) 0.070(6) -0.001(4) -0.037(5) -0.001(3) C43 0.033(4) 0.056(5) 0.074(6) -0.031(5) -0.009(4) -0.010(4) C44 0.036(4) 0.052(5) 0.096(8) 0.002(5) -0.025(5) -0.003(4) C63 0.068(6) 0.050(5) 0.113(9) -0.027(6) -0.067(7) 0.007(5) C62 0.069(6) 0.034(4) 0.106(8) 0.003(5) -0.059(6) -0.010(4) C42 0.099(9) 0.104(9) 0.087(8) -0.018(7) -0.068(7) 0.050(7) C65 0.077(7) 0.073(7) 0.155(12) 0.029(8) -0.072(8) -0.027(6) C53 0.050(7) 0.137(13) 0.199(18) -0.085(13) -0.028(9) 0.020(7) Br1 0.0487(4) 0.0460(4) 0.0458(4) -0.0123(3) -0.0253(4) 0.0044(3) Br4 0.0511(19) 0.0591(18) 0.092(2) -0.0519(16) -0.0452(17) 0.0192(14) Br2 0.0706(10) 0.0553(9) 0.0580(10) 0.0048(8) -0.0223(8) 0.0051(8) Br3 0.092(3) 0.0617(19) 0.0524(18) -0.0129(14) -0.0439(18) 0.0099(17) C57 0.074(13) 0.040(10) 0.13(2) 0.023(11) -0.057(15) -0.021(10) O11 0.21(2) 0.091(13) 0.16(2) -0.004(13) -0.103(19) -0.064(15) C56 0.115(19) 0.112(19) 0.037(10) 0.014(11) -0.028(12) -0.050(16) C58 0.12(2) 0.030(9) 0.15(2) 0.027(12) -0.092(19) -0.023(11) C55 0.18(3) 0.049(12) 0.064(14) 0.012(10) -0.061(16) -0.036(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga2 O1 1.862(4) . ? Ga2 O7 1.881(4) . ? Ga2 O4 1.902(4) . ? Ga2 C8 1.948(6) . ? Ga3 O6 1.863(4) . ? Ga3 O1 1.868(4) . ? Ga3 O5 1.889(4) . ? Ga3 C15 1.946(6) . ? Ga1 O2 1.874(4) . ? Ga1 O1 1.883(4) . ? Ga1 O3 1.895(4) . ? Ga1 C1 1.947(6) . ? Ga5 O6 1.865(4) 2_655 ? Ga5 O2 1.870(4) . ? Ga5 O4 1.900(4) 2_655 ? Ga5 C29 1.945(6) . ? Ga6 O7 1.866(4) . ? Ga6 O6 1.871(4) 2_655 ? Ga6 O3 1.896(4) . ? Ga6 C36 1.940(7) . ? Ga4 O7 1.864(4) 2_655 ? Ga4 O2 1.874(4) . ? Ga4 O5 1.910(4) . ? Ga4 C22 1.927(6) . ? O7 Ga4 1.864(4) 2_655 ? O6 Ga5 1.865(4) 2_655 ? O6 Ga6 1.871(4) 2_655 ? O4 Ga5 1.900(4) 2_655 ? C8 C9 1.393(8) . ? C8 C13 1.395(9) . ? O9 C50 1.433(8) . ? O9 C47 1.436(8) . ? C15 C16 1.396(9) . ? C15 C20 1.399(9) . ? C1 C6 1.378(10) . ? C1 C2 1.394(9) . ? C22 C27 1.385(10) . ? C22 C23 1.392(10) . ? C29 C30 1.393(9) . ? C29 C34 1.396(9) . ? C37 C36 1.391(9) . ? C37 C38 1.393(9) . ? C30 C31 1.385(10) . ? C9 C10 1.384(9) . ? C36 C41 1.383(9) . ? C16 C17 1.401(9) . ? C5 C4 1.375(11) . ? C5 C6 1.393(10) . ? O10 C51 1.443(11) . ? O10 C54 1.447(11) . ? C38 C39 1.376(11) . ? C2 C3 1.411(10) . ? C12 C13 1.390(9) . ? C12 C11 1.397(10) . ? C20 C19 1.388(9) . ? C10 C11 1.393(10) . ? C50 C49 1.523(10) . ? C11 C14 1.495(9) . ? C25 C26 1.360(11) . ? C25 C24 1.372(11) . ? C25 C28 1.509(10) . ? C4 C3 1.381(11) . ? C4 C7 1.504(10) . ? C33 C34 1.382(10) . ? C33 C32 1.385(10) . ? C23 C24 1.393(11) . ? C18 C17 1.389(10) . ? C18 C19 1.399(10) . ? C18 C21 1.504(9) . ? C32 C31 1.390(11) . ? C32 C35 1.526(10) . ? C27 C26 1.400(10) . ? C48 C47 1.498(10) . ? C48 C49 1.508(11) . ? C41 C40 1.376(11) . ? C51 C52 1.514(18) . ? C39 C40 1.394(12) . ? C39 C42 1.527(11) . ? C54 C53 1.530(16) . ? C52 C53 1.456(15) . ? Ga7 C66 1.899(8) . ? Ga7 C59 1.965(8) . ? Ga7 Br3 2.118(4) . ? Ga7 Br1 2.4053(15) . ? Ga7 Br4 2.459(3) . ? Ga7 Br2 2.498(2) . ? O8 C43 1.437(9) . ? O8 C46 1.453(8) . ? C46 C45 1.496(11) . ? C59 C60 1.359(11) . ? C59 C64 1.434(12) . ? C60 C61 1.423(11) . ? C64 C63 1.414(14) . ? C45 C44 1.504(12) . ? C61 C62 1.371(12) . ? C43 C44 1.523(13) . ? C63 C62 1.358(14) . ? C62 C65 1.494(14) . ? C57 C56 1.409(17) . ? C57 C58 1.514(16) . ? O11 C55 1.355(16) . ? O11 C58 1.390(17) . ? C56 C55 1.525(16) . ? C72 C69 1.47(2) . ? C69 C68 1.322(14) . ? C69 C70 1.389(14) . ? C71 C66 1.370(11) . ? C71 C70 1.491(11) . ? C67 C66 1.401(15) . ? C67 C68 1.413(15) . ? 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 O1 Ga2 O7 105.24(18) . . ? O1 Ga2 O4 99.40(18) . . ? O7 Ga2 O4 98.89(17) . . ? O1 Ga2 C8 118.6(2) . . ? O7 Ga2 C8 112.0(2) . . ? O4 Ga2 C8 120.0(2) . . ? O6 Ga3 O1 105.58(18) . . ? O6 Ga3 O5 98.98(17) . . ? O1 Ga3 O5 99.48(18) . . ? O6 Ga3 C15 116.7(2) . . ? O1 Ga3 C15 113.1(2) . . ? O5 Ga3 C15 120.5(2) . . ? O2 Ga1 O1 104.80(17) . . ? O2 Ga1 O3 97.75(18) . . ? O1 Ga1 O3 98.95(18) . . ? O2 Ga1 C1 118.3(2) . . ? O1 Ga1 C1 114.9(2) . . ? O3 Ga1 C1 119.0(2) . . ? O6 Ga5 O2 106.31(18) 2_655 . ? O6 Ga5 O4 98.52(17) 2_655 2_655 ? O2 Ga5 O4 99.40(18) . 2_655 ? O6 Ga5 C29 111.2(2) 2_655 . ? O2 Ga5 C29 119.9(2) . . ? O4 Ga5 C29 118.8(2) 2_655 . ? O7 Ga6 O6 103.61(17) . 2_655 ? O7 Ga6 O3 100.74(18) . . ? O6 Ga6 O3 98.89(17) 2_655 . ? O7 Ga6 C36 114.9(2) . . ? O6 Ga6 C36 119.0(2) 2_655 . ? O3 Ga6 C36 116.9(2) . . ? O7 Ga4 O2 103.70(18) 2_655 . ? O7 Ga4 O5 98.82(17) 2_655 . ? O2 Ga4 O5 100.09(17) . . ? O7 Ga4 C22 120.1(2) 2_655 . ? O2 Ga4 C22 113.3(2) . . ? O5 Ga4 C22 117.9(2) . . ? Ga5 O2 Ga4 120.8(2) . . ? Ga5 O2 Ga1 119.5(2) . . ? Ga4 O2 Ga1 118.9(2) . . ? Ga3 O5 Ga4 126.9(2) . . ? Ga2 O1 Ga3 119.1(2) . . ? Ga2 O1 Ga1 120.2(2) . . ? Ga3 O1 Ga1 119.9(2) . . ? Ga4 O7 Ga6 120.6(2) 2_655 . ? Ga4 O7 Ga2 120.9(2) 2_655 . ? Ga6 O7 Ga2 118.3(2) . . ? Ga3 O6 Ga5 120.0(2) . 2_655 ? Ga3 O6 Ga6 120.9(2) . 2_655 ? Ga5 O6 Ga6 118.5(2) 2_655 2_655 ? Ga5 O4 Ga2 127.0(2) 2_655 . ? C9 C8 C13 118.1(5) . . ? C9 C8 Ga2 123.4(5) . . ? C13 C8 Ga2 118.3(5) . . ? Ga1 O3 Ga6 128.5(2) . . ? C50 O9 C47 107.0(5) . . ? C16 C15 C20 118.0(6) . . ? C16 C15 Ga3 119.8(5) . . ? C20 C15 Ga3 122.1(5) . . ? C6 C1 C2 117.8(6) . . ? C6 C1 Ga1 120.5(5) . . ? C2 C1 Ga1 121.7(5) . . ? C27 C22 C23 115.9(6) . . ? C27 C22 Ga4 119.4(5) . . ? C23 C22 Ga4 124.7(5) . . ? C30 C29 C34 117.5(6) . . ? C30 C29 Ga5 124.1(5) . . ? C34 C29 Ga5 118.3(5) . . ? C36 C37 C38 121.5(6) . . ? C31 C30 C29 120.8(7) . . ? C10 C9 C8 121.1(6) . . ? C41 C36 C37 117.0(6) . . ? C41 C36 Ga6 119.2(5) . . ? C37 C36 Ga6 123.8(5) . . ? C15 C16 C17 120.6(6) . . ? C4 C5 C6 122.0(7) . . ? C51 O10 C54 111.3(8) . . ? C39 C38 C37 121.1(7) . . ? C1 C2 C3 120.2(7) . . ? C13 C12 C11 120.7(6) . . ? C19 C20 C15 121.2(6) . . ? C9 C10 C11 121.0(6) . . ? O9 C50 C49 107.5(6) . . ? C10 C11 C12 118.2(6) . . ? C10 C11 C14 121.2(7) . . ? C12 C11 C14 120.6(7) . . ? C26 C25 C24 117.7(7) . . ? C26 C25 C28 120.4(8) . . ? C24 C25 C28 121.9(7) . . ? C5 C4 C3 117.3(6) . . ? C5 C4 C7 121.5(8) . . ? C3 C4 C7 121.2(7) . . ? C34 C33 C32 121.1(6) . . ? C33 C34 C29 121.3(6) . . ? C22 C23 C24 121.6(7) . . ? C17 C18 C19 118.2(6) . . ? C17 C18 C21 120.9(6) . . ? C19 C18 C21 120.9(7) . . ? C33 C32 C31 117.9(6) . . ? C33 C32 C35 121.4(7) . . ? C31 C32 C35 120.8(7) . . ? C22 C27 C26 121.8(7) . . ? C47 C48 C49 104.2(6) . . ? C12 C13 C8 120.9(6) . . ? C40 C41 C36 121.5(7) . . ? C20 C19 C18 120.9(6) . . ? C18 C17 C16 121.1(6) . . ? C48 C49 C50 103.7(6) . . ? C30 C31 C32 121.4(7) . . ? C4 C3 C2 121.5(7) . . ? C25 C24 C23 121.5(7) . . ? C25 C26 C27 121.5(8) . . ? O10 C51 C52 105.8(10) . . ? C1 C6 C5 121.2(7) . . ? C38 C39 C40 117.3(7) . . ? C38 C39 C42 120.3(8) . . ? C40 C39 C42 122.4(8) . . ? O9 C47 C48 104.0(6) . . ? O10 C54 C53 103.1(10) . . ? C41 C40 C39 121.6(7) . . ? C53 C52 C51 106.5(10) . . ? C66 Ga7 C59 120.1(4) . . ? C66 Ga7 Br3 82.6(3) . . ? C59 Ga7 Br3 120.5(3) . . ? C66 Ga7 Br1 113.0(3) . . ? C59 Ga7 Br1 109.6(2) . . ? Br3 Ga7 Br1 108.52(11) . . ? C66 Ga7 Br4 25.3(3) . . ? C59 Ga7 Br4 111.2(2) . . ? Br3 Ga7 Br4 106.86(15) . . ? Br1 Ga7 Br4 97.70(9) . . ? C66 Ga7 Br2 101.4(3) . . ? C59 Ga7 Br2 105.9(3) . . ? Br3 Ga7 Br2 19.42(10) . . ? Br1 Ga7 Br2 105.16(7) . . ? Br4 Ga7 Br2 126.09(11) . . ? C43 O8 C46 106.1(6) . . ? O8 C46 C45 104.4(6) . . ? C60 C59 C64 117.3(8) . . ? C60 C59 Ga7 121.5(6) . . ? C64 C59 Ga7 121.1(7) . . ? C59 C60 C61 121.2(7) . . ? C63 C64 C59 119.5(9) . . ? C46 C45 C44 101.9(7) . . ? C62 C61 C60 121.7(9) . . ? O8 C43 C44 106.6(7) . . ? C45 C44 C43 105.1(7) . . ? C62 C63 C64 122.5(8) . . ? C63 C62 C61 117.8(9) . . ? C63 C62 C65 120.3(9) . . ? C61 C62 C65 121.9(11) . . ? C52 C53 C54 106.6(11) . . ? C56 C57 C58 102.1(15) . . ? C55 O11 C58 96(2) . . ? C57 C56 C55 101.6(15) . . ? O11 C58 C57 105.3(16) . . ? O11 C55 C56 108.7(16) . . ? C68 C69 C70 118.7(12) . . ? C68 C69 C72 120.2(13) . . ? C70 C69 C72 121.0(12) . . ? C66 C71 C70 127.7(10) . . ? C66 C67 C68 118.3(13) . . ? C69 C68 C67 127.6(10) . . ? C69 C70 C71 113.1(8) . . ? C71 C66 C67 113.5(9) . . ? C71 C66 Ga7 120.4(7) . . ? C67 C66 Ga7 126.1(8) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.595 _refine_diff_density_min -1.689 _refine_diff_density_rms 0.157