data_4000050 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_formula_sum 'C36 H84 O12 Ga4' _chemical_formula_weight 987.91 _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4(1)2(1)2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.5566(6) _cell_length_b 12.5566(6) _cell_length_c 32.0324(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5050.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6003 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 22.53 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 2.159 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7044 _exptl_absorpt_correction_T_max 0.8972 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega and an exposure time of 30 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 6003 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 4/mmm, and from the systematic absences noted the space group was shown to be either P4(1)2(1)2 or P4(3)2(1)2. The asymmetric unit consists of one-half molecule situated about a two-fold axis. Several of the alkoxide ligands are disordered over two different orientations, which was modeled using distance constraints with occupancies based on the observed isotropic temperature factors. Acknowledgment for use of MRSEC/TCSUH Facilities: This work made use of MRSEC/TCSUH Shared Experimental Facilities supported by the National Science Foundation under Award Number DMR-9632667 and the Texas Center for Superconductivity at the University of Houston. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens omitted. Only the major orientation of each disordered ligand is shown at any site. Fig. 2 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(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 'Siemens SMART CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 21320 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 22.53 _reflns_number_total 3333 _reflns_number_gt 2857 _reflns_threshold_expression >4sigma(I) _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^)+(0.0406P)^2^+4.1979P] 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 SHELXL _refine_ls_extinction_coef 0.00011(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.506(19) _refine_ls_number_reflns 3312 _refine_ls_number_parameters 261 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.185 _refine_ls_shift/su_mean 0.023 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 0.53649(4) 0.53649(4) 0.0000 0.03619(17) Uani 1 2 d S A . Ga2 Ga 0.70663(4) 0.70663(4) 0.0000 0.0495(2) Uani 1 2 d S A . Ga3 Ga 0.37748(4) 0.52927(4) 0.070228(16) 0.04655(16) Uani 1 1 d . . . O1 O 0.6531(2) 0.5980(2) 0.03493(9) 0.0456(8) Uani 1 1 d . . . O2 O 0.4788(2) 0.4404(2) 0.04419(9) 0.0442(7) Uani 1 1 d . A . O3 O 0.4250(2) 0.6242(2) 0.02820(9) 0.0438(8) Uani 1 1 d . A . O4 O 0.6664(3) 0.8396(3) 0.01085(14) 0.0819(13) Uani 1 1 d . . . O5 O 0.2394(4) 0.5115(5) 0.05514(16) 0.0589(14) Uani 0.70 1 d PD A 1 O5' O 0.2507(11) 0.4680(12) 0.0745(5) 0.073(4) Uiso 0.30 1 d PD A 2 O6 O 0.4379(8) 0.5614(9) 0.1214(3) 0.063(3) Uiso 0.50 1 d P A 1 O6' O 0.4223(9) 0.5337(9) 0.1214(3) 0.069(4) Uiso 0.50 1 d P A 2 C1 C 0.6831(4) 0.5806(4) 0.07858(14) 0.0531(13) Uani 1 1 d . A . H1A H 0.6236 0.5449 0.0932 0.064 Uiso 1 1 calc R . . C2 C 0.7803(5) 0.5093(6) 0.07999(19) 0.095(2) Uani 1 1 d . . . H2A H 0.7642 0.4421 0.0665 0.143 Uiso 1 1 calc R A . H2B H 0.8001 0.4964 0.1088 0.143 Uiso 1 1 calc R . . H2C H 0.8389 0.5437 0.0656 0.143 Uiso 1 1 calc R . . C3 C 0.7051(6) 0.6860(5) 0.09950(18) 0.0865(19) Uani 1 1 d . . . H3A H 0.6414 0.7296 0.0988 0.130 Uiso 1 1 calc R A . H3B H 0.7622 0.7223 0.0849 0.130 Uiso 1 1 calc R . . H3C H 0.7259 0.6738 0.1283 0.130 Uiso 1 1 calc R . . C4 C 0.4932(4) 0.3261(4) 0.05128(16) 0.0505(13) Uani 1 1 d . . . H4A H 0.5376 0.2969 0.0284 0.061 Uiso 1 1 calc R A . C5 C 0.3899(6) 0.2700(5) 0.0512(2) 0.097(2) Uani 1 1 d . A . H5A H 0.3542 0.2820 0.0248 0.145 Uiso 1 1 calc R . . H5B H 0.3460 0.2968 0.0738 0.145 Uiso 1 1 calc R . . H5C H 0.4018 0.1943 0.0550 0.145 Uiso 1 1 calc R . . C6 C 0.5505(6) 0.3096(5) 0.0916(2) 0.093(2) Uani 1 1 d . A . H6A H 0.6180 0.3470 0.0909 0.139 Uiso 1 1 calc R . . H6B H 0.5631 0.2341 0.0958 0.139 Uiso 1 1 calc R . . H6C H 0.5075 0.3369 0.1144 0.139 Uiso 1 1 calc R . . C7 C 0.4056(4) 0.7383(4) 0.02652(15) 0.0512(12) Uani 1 1 d . . . H7A H 0.4625 0.7725 0.0099 0.061 Uiso 1 1 calc R A . C8 C 0.2989(4) 0.7595(4) 0.00578(19) 0.0716(16) Uani 1 1 d . A . H8A H 0.2998 0.7313 -0.0224 0.107 Uiso 1 1 calc R . . H8B H 0.2860 0.8357 0.0049 0.107 Uiso 1 1 calc R . . H8C H 0.2428 0.7252 0.0216 0.107 Uiso 1 1 calc R . . C9 C 0.4066(5) 0.7848(5) 0.07053(18) 0.0806(18) Uani 1 1 d . A . H9A H 0.4755 0.7720 0.0833 0.121 Uiso 1 1 calc R . . H9B H 0.3514 0.7511 0.0871 0.121 Uiso 1 1 calc R . . H9C H 0.3935 0.8608 0.0692 0.121 Uiso 1 1 calc R . . C10 C 0.7274(11) 0.9288(8) 0.0215(4) 0.080(4) Uani 0.65 1 d PD A 1 H10A H 0.7825 0.9058 0.0417 0.096 Uiso 0.65 1 calc PR A 1 C11 C 0.7832(13) 0.9808(11) -0.0151(5) 0.094(4) Uani 0.65 1 d PD A 1 H11A H 0.8302 0.9295 -0.0283 0.140 Uiso 0.65 1 calc PR A 1 H11B H 0.8245 1.0410 -0.0053 0.140 Uiso 0.65 1 calc PR A 1 H11C H 0.7306 1.0050 -0.0351 0.140 Uiso 0.65 1 calc PR A 1 C12 C 0.6542(11) 1.0060(9) 0.0435(4) 0.089(4) Uani 0.65 1 d PD A 1 H12A H 0.6198 0.9703 0.0667 0.133 Uiso 0.65 1 calc PR A 1 H12B H 0.6005 1.0312 0.0241 0.133 Uiso 0.65 1 calc PR A 1 H12C H 0.6952 1.0659 0.0538 0.133 Uiso 0.65 1 calc PR A 1 C10' C 0.705(2) 0.925(2) 0.0338(8) 0.065(7) Uiso 0.35 1 d PD A 2 H10B H 0.7591 0.9003 0.0542 0.078 Uiso 0.35 1 calc PR A 2 C11' C 0.758(3) 0.991(3) 0.0000(10) 0.109(12) Uiso 0.35 1 d PD A 2 H11D H 0.8139 0.9497 -0.0134 0.164 Uiso 0.35 1 calc PR A 2 H11E H 0.7892 1.0547 0.0123 0.164 Uiso 0.35 1 calc PR A 2 H11F H 0.7056 1.0118 -0.0207 0.164 Uiso 0.35 1 calc PR A 2 C12' C 0.6201(19) 0.990(2) 0.0555(8) 0.090(9) Uiso 0.35 1 d PD A 2 H12D H 0.5884 0.9484 0.0777 0.135 Uiso 0.35 1 calc PR A 2 H12E H 0.5656 1.0100 0.0355 0.135 Uiso 0.35 1 calc PR A 2 H12F H 0.6518 1.0541 0.0672 0.135 Uiso 0.35 1 calc PR A 2 C13 C 0.1562(5) 0.4700(7) 0.0808(3) 0.063(2) Uani 0.70 1 d PD A 1 H13A H 0.1857 0.4174 0.1007 0.075 Uiso 0.70 1 calc PR A 1 C14 C 0.0777(18) 0.416(2) 0.0516(7) 0.108(12) Uani 0.70 1 d PD A 1 H14A H 0.1133 0.3589 0.0367 0.162 Uiso 0.70 1 calc PR A 1 H14B H 0.0505 0.4676 0.0318 0.162 Uiso 0.70 1 calc PR A 1 H14C H 0.0191 0.3869 0.0677 0.162 Uiso 0.70 1 calc PR A 1 C15 C 0.1030(18) 0.5601(17) 0.1045(7) 0.092(5) Uani 0.70 1 d PD A 1 H15A H 0.1525 0.5891 0.1248 0.138 Uiso 0.70 1 calc PR A 1 H15B H 0.0405 0.5332 0.1188 0.138 Uiso 0.70 1 calc PR A 1 H15C H 0.0821 0.6155 0.0851 0.138 Uiso 0.70 1 calc PR A 1 C13' C 0.1511(16) 0.514(2) 0.0619(8) 0.077(7) Uiso 0.30 1 d PD A 2 H13B H 0.1576 0.5550 0.0355 0.093 Uiso 0.30 1 calc PR A 2 C14' C 0.080(6) 0.417(5) 0.057(2) 0.12(3) Uiso 0.30 1 d PD A 2 H14D H 0.1087 0.3714 0.0351 0.181 Uiso 0.30 1 calc PR A 2 H14E H 0.0088 0.4389 0.0497 0.181 Uiso 0.30 1 calc PR A 2 H14F H 0.0787 0.3775 0.0831 0.181 Uiso 0.30 1 calc PR A 2 C15' C 0.101(6) 0.580(5) 0.0965(16) 0.13(2) Uiso 0.30 1 d PD A 2 H15D H 0.1391 0.6473 0.0991 0.189 Uiso 0.30 1 calc PR A 2 H15E H 0.1055 0.5416 0.1227 0.189 Uiso 0.30 1 calc PR A 2 H15F H 0.0271 0.5943 0.0899 0.189 Uiso 0.30 1 calc PR A 2 C16 C 0.3776(14) 0.5954(16) 0.1577(5) 0.106(8) Uiso 0.50 1 d PD A 1 H16A H 0.3298 0.6545 0.1496 0.127 Uiso 0.50 1 calc PR A 1 C17 C 0.3156(11) 0.5156(12) 0.1833(5) 0.082(4) Uiso 0.50 1 d PD A 1 H17A H 0.2579 0.4868 0.1666 0.124 Uiso 0.50 1 calc PR A 1 H17B H 0.2866 0.5505 0.2078 0.124 Uiso 0.50 1 calc PR A 1 H17C H 0.3625 0.4582 0.1919 0.124 Uiso 0.50 1 calc PR A 1 C18 C 0.4657(12) 0.6387(13) 0.1854(5) 0.089(5) Uiso 0.50 1 d PD A 1 H18A H 0.5058 0.6921 0.1702 0.133 Uiso 0.50 1 calc PR A 1 H18B H 0.5128 0.5810 0.1935 0.133 Uiso 0.50 1 calc PR A 1 H18C H 0.4347 0.6706 0.2101 0.133 Uiso 0.50 1 calc PR A 1 C16' C 0.3954(10) 0.5712(11) 0.1603(4) 0.057(4) Uiso 0.50 1 d PD A 2 H16B H 0.3456 0.6321 0.1584 0.068 Uiso 0.50 1 calc PR A 2 C17' C 0.3412(14) 0.4738(12) 0.1783(5) 0.108(6) Uiso 0.50 1 d PD A 2 H17D H 0.2818 0.4538 0.1606 0.162 Uiso 0.50 1 calc PR A 2 H17E H 0.3154 0.4898 0.2061 0.162 Uiso 0.50 1 calc PR A 2 H17F H 0.3918 0.4155 0.1796 0.162 Uiso 0.50 1 calc PR A 2 C18' C 0.4936(12) 0.5995(14) 0.1862(5) 0.101(5) Uiso 0.50 1 d PD A 2 H18D H 0.5278 0.6619 0.1744 0.152 Uiso 0.50 1 calc PR A 2 H18E H 0.5431 0.5402 0.1859 0.152 Uiso 0.50 1 calc PR A 2 H18F H 0.4723 0.6143 0.2147 0.152 Uiso 0.50 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 0.0363(2) 0.0363(2) 0.0360(3) 0.0027(2) -0.0027(2) 0.0018(3) Ga2 0.0492(3) 0.0492(3) 0.0502(4) 0.0047(3) -0.0047(3) -0.0109(4) Ga3 0.0439(3) 0.0501(3) 0.0456(3) -0.0019(3) 0.0066(2) 0.0014(3) O1 0.0471(19) 0.0480(19) 0.0416(17) 0.0049(14) -0.0095(14) -0.0048(14) O2 0.0448(17) 0.0394(18) 0.0485(18) 0.0053(13) 0.0066(14) 0.0043(14) O3 0.0470(17) 0.0387(17) 0.0457(18) -0.0010(14) -0.0002(14) 0.0086(14) O4 0.087(3) 0.049(2) 0.110(3) -0.009(2) -0.003(2) -0.017(2) O5 0.036(3) 0.090(4) 0.051(3) 0.016(3) 0.006(2) -0.004(3) C1 0.050(3) 0.069(3) 0.040(3) 0.012(2) -0.012(2) -0.007(2) C2 0.083(4) 0.135(6) 0.068(4) 0.005(4) -0.024(3) 0.046(4) C3 0.114(5) 0.085(5) 0.061(3) -0.011(3) -0.032(4) -0.013(4) C4 0.059(3) 0.036(3) 0.056(3) 0.013(2) 0.016(2) 0.005(2) C5 0.111(6) 0.066(4) 0.112(5) 0.036(4) -0.030(4) -0.032(4) C6 0.109(5) 0.054(4) 0.114(5) 0.030(4) -0.033(4) 0.010(4) C7 0.058(3) 0.039(3) 0.057(3) -0.003(2) 0.000(3) 0.007(2) C8 0.076(4) 0.053(3) 0.086(4) 0.000(3) -0.016(3) 0.019(3) C9 0.108(5) 0.060(4) 0.074(4) -0.026(3) -0.014(4) 0.017(3) C10 0.117(11) 0.056(6) 0.069(8) 0.014(6) 0.013(7) -0.033(7) C11 0.100(10) 0.068(7) 0.113(12) 0.020(8) 0.011(9) -0.010(7) C12 0.124(11) 0.068(7) 0.074(8) -0.026(6) 0.029(7) -0.025(7) C13 0.038(4) 0.080(6) 0.071(5) 0.020(5) 0.013(4) 0.004(4) C14 0.048(8) 0.131(17) 0.145(19) -0.026(9) 0.016(7) -0.039(8) C15 0.072(9) 0.122(12) 0.082(8) -0.020(10) 0.021(6) 0.041(8)