# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Wright, Dominic S.' _publ_contact_author_name 'Wright, Dominic S.' _publ_contact_author_email DSW1000@CAM.AC.UK _publ_section_title ; Confinement of halide ions within homologous inverse coordination hosts; modification of halide-ion selectivity ; # Attachment '- 1Br.cif' data_dw0609 _database_code_depnum_ccdc_archive 'CCDC 797471' #TrackingRef '- 1Br.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H188 Al4 Br Li17 O14.50 P12' _chemical_formula_weight 2708.29 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' Li Li -0.0003 0.0001 '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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 35.204(4) _cell_length_b 35.204(4) _cell_length_c 35.204(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 43629(9) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 48194 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11408 _exptl_absorpt_coefficient_mu 0.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 0.816 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 11370 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 5.18 _diffrn_reflns_theta_max 21.00 _reflns_number_total 1848 _reflns_number_gt 1691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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. Four isolated residual maxima of electron density were assigned as partial C- and O-atoms of one THF solvate per cluster anion, highly disordered across a site of -4 symmetry. High displacement parameters associated with light atoms indicated considerable unresolved disorder resulting in poor diffraction at high angle; data in the limited theta range < 21o were used in the full matrix refinement as a chiral twin (53:47%). There was additionally a small disorder of the cluster anion with its enantiomer (ca. 7%) and only the contribition from the metal (Al1') component of the disorder was allowed for in the refinement. ; _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^)+(0.1161P)^2^+136.7211P] 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 1848 _refine_ls_number_parameters 162 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1881 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.137 _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 Br1 Br 0.5000 0.5000 0.5000 0.0560(5) Uani 1 12 d S . . Al1 Al 0.56949(5) 0.56949(5) 0.43051(5) 0.0528(7) Uani 0.93 3 d SP A 1 C1 C 0.60261(17) 0.60261(17) 0.39739(17) 0.069(3) Uani 1 3 d S . . H1A H 0.6037 0.5921 0.3722 0.103 Uiso 0.33 1 calc PR A 1 H1B H 0.6278 0.6037 0.4079 0.103 Uiso 0.33 1 calc PR A 1 H1C H 0.5921 0.6278 0.3963 0.103 Uiso 0.33 1 calc PR A 1 Li2 Li 0.5416(2) 0.5416(2) 0.5416(2) 0.051(3) Uani 1 3 d S . . Li1 Li 0.6123(2) 0.5400(3) 0.5018(4) 0.073(3) Uani 1 1 d . . . P1 P 0.56012(4) 0.59319(4) 0.49500(5) 0.0620(5) Uani 1 1 d . . . C11 C 0.59592(12) 0.63076(10) 0.50728(12) 0.0747(17) Uani 1 1 d G . . C12 C 0.60891(19) 0.63127(15) 0.54456(12) 0.125(3) Uani 1 1 d G A . H12 H 0.6007 0.6129 0.5617 0.150 Uiso 1 1 calc R . . C13 C 0.6342(2) 0.65926(19) 0.55628(16) 0.177(5) Uani 1 1 d G A . H13 H 0.6429 0.6596 0.5812 0.213 Uiso 1 1 calc R . . C14 C 0.64644(17) 0.68674(15) 0.5307(2) 0.141(4) Uani 1 1 d G A . H14 H 0.6633 0.7055 0.5386 0.170 Uiso 1 1 calc R . . C15 C 0.63345(14) 0.68623(11) 0.49344(18) 0.099(2) Uani 1 1 d G A . H15 H 0.6417 0.7046 0.4763 0.119 Uiso 1 1 calc R . . C16 C 0.60819(13) 0.65824(12) 0.48172(12) 0.084(2) Uani 1 1 d G A . H16 H 0.5995 0.6579 0.4568 0.101 Uiso 1 1 calc R . . O1S O 0.66485(10) 0.55634(12) 0.50453(14) 0.0794(12) Uani 1 1 d D A . C1S C 0.6815(2) 0.5812(3) 0.4786(2) 0.112(3) Uani 1 1 d D . . H1S1 H 0.6633 0.6004 0.4708 0.134 Uiso 1 1 calc R A . H1S2 H 0.6897 0.5674 0.4562 0.134 Uiso 1 1 calc R . . C2S C 0.7141(2) 0.5990(3) 0.4970(3) 0.130(3) Uani 1 1 d D A . H2S1 H 0.7346 0.6030 0.4791 0.156 Uiso 1 1 calc R . . H2S2 H 0.7071 0.6232 0.5081 0.156 Uiso 1 1 calc R . . C3S C 0.7251(2) 0.5719(3) 0.5263(3) 0.130(3) Uani 1 1 d D . . H3S1 H 0.7355 0.5851 0.5482 0.156 Uiso 0.80 1 calc PR A 1 H3S2 H 0.7441 0.5545 0.5167 0.156 Uiso 0.80 1 calc PR A 1 H3S3 H 0.7189 0.5805 0.5518 0.156 Uiso 0.20 1 calc PR A 2 H3S4 H 0.7517 0.5647 0.5249 0.156 Uiso 0.20 1 calc PR A 2 C4S C 0.6918(4) 0.5522(6) 0.5363(4) 0.185(8) Uani 0.80 1 d PD A 1 H4S1 H 0.6974 0.5255 0.5407 0.222 Uiso 0.80 1 calc PR A 1 H4S2 H 0.6810 0.5627 0.5594 0.222 Uiso 0.80 1 calc PR A 1 C4S' C 0.6949(7) 0.5370(7) 0.5100(8) 0.048(6) Uiso 0.20 1 d P A 2 H4S3 H 0.7041 0.5257 0.4866 0.057 Uiso 0.20 1 calc PR A 2 H4S4 H 0.6910 0.5172 0.5288 0.057 Uiso 0.20 1 calc PR A 2 Li3 Li 0.7500 0.5000 0.5000 0.100 Uiso 0.17 4 d SP . . Li3Y Li 0.6942 0.8058 0.6942 0.16(10) Uiso 0.12 3 d SPD . . O1T O 0.6536(8) 0.8237(11) 0.7288(8) 0.17(2) Uiso 0.13 1 d PD . . C1T C 0.6530(14) 0.8387(9) 0.7703(10) 0.12(2) Uiso 0.13 1 d PD . . H1T1 H 0.6364 0.8233 0.7860 0.149 Uiso 0.13 1 calc PR . . H1T2 H 0.6784 0.8384 0.7811 0.149 Uiso 0.13 1 calc PR . . C2T C 0.6379(13) 0.8798(10) 0.7671(10) 0.095(17) Uiso 0.13 1 d PD . . H2T1 H 0.6198 0.8849 0.7872 0.114 Uiso 0.13 1 calc PR . . H2T2 H 0.6586 0.8978 0.7691 0.114 Uiso 0.13 1 calc PR . . C3T C 0.6186(12) 0.8834(10) 0.7282(10) 0.074(13) Uiso 0.13 1 d PD . . H3T1 H 0.6328 0.9005 0.7120 0.089 Uiso 0.13 1 calc PR . . H3T2 H 0.5930 0.8932 0.7311 0.089 Uiso 0.13 1 calc PR . . C4T C 0.6177(16) 0.8431(12) 0.7110(14) 0.14(3) Uiso 0.13 1 d PD . . H4T1 H 0.6194 0.8440 0.6835 0.172 Uiso 0.13 1 calc PR . . H4T2 H 0.5946 0.8297 0.7181 0.172 Uiso 0.13 1 calc PR . . O1U O 0.774(2) 1.223(3) 0.539(3) 0.14(3) Uiso 0.08 1 d P . . C1U C 0.759(5) 1.275(4) 0.560(5) 0.17(5) Uiso 0.08 1 d P . . C2U C 0.7579(14) 1.2215(13) 0.4971(19) 0.106(13) Uiso 0.17 1 d P . . C3U C 0.782(2) 1.252(2) 0.527(2) 0.072(18) Uiso 0.08 1 d P . . Al1' Al 0.4317(7) 0.4317(7) 0.5683(7) 0.057(10) Uiso 0.07 3 d SP . 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 Br1 0.0560(5) 0.0560(5) 0.0560(5) 0.000 0.000 0.000 Al1 0.0528(7) 0.0528(7) 0.0528(7) 0.0034(8) 0.0034(8) -0.0034(8) C1 0.069(3) 0.069(3) 0.069(3) 0.003(3) 0.003(3) -0.003(3) Li2 0.051(3) 0.051(3) 0.051(3) -0.008(3) -0.008(3) -0.008(3) Li1 0.051(5) 0.062(5) 0.105(7) -0.007(6) -0.011(6) -0.001(4) P1 0.0588(8) 0.0543(8) 0.0729(10) -0.0029(7) 0.0015(7) -0.0081(6) C11 0.073(4) 0.057(3) 0.095(5) 0.001(3) 0.009(4) -0.004(3) C12 0.181(9) 0.102(6) 0.092(5) 0.000(4) -0.052(6) -0.061(6) C13 0.221(13) 0.141(9) 0.171(11) -0.006(8) -0.085(10) -0.063(9) C14 0.104(7) 0.116(8) 0.204(12) -0.037(8) -0.027(7) -0.028(6) C15 0.079(4) 0.058(4) 0.160(8) -0.007(4) 0.006(5) -0.013(3) C16 0.082(4) 0.061(4) 0.110(5) 0.001(4) 0.015(4) -0.007(3) O1S 0.048(2) 0.089(3) 0.102(3) 0.002(3) 0.000(2) -0.0113(19) C1S 0.072(5) 0.146(7) 0.118(6) 0.045(5) -0.011(4) -0.007(5) C2S 0.068(4) 0.123(6) 0.199(9) 0.007(7) 0.019(7) -0.027(4) C3S 0.069(5) 0.171(9) 0.150(8) -0.007(7) -0.033(5) 0.005(6) C4S 0.091(9) 0.31(2) 0.152(13) 0.074(14) -0.050(9) -0.070(11) _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 Br1 Li2 2.537(14) 2_665 ? Br1 Li2 2.537(14) . ? Br1 Li2 2.537(14) 4_566 ? Br1 Li2 2.537(14) 3_656 ? Al1 C1 2.020(11) . ? Al1 P1 2.441(2) . ? Al1 P1 2.441(2) 11_566 ? Al1 P1 2.441(2) 8_656 ? Al1 Li1 3.107(12) 8_656 ? Al1 Li1 3.107(12) 11_566 ? Al1 Li1 3.107(12) . ? Li2 P1 2.533(3) 5 ? Li2 P1 2.533(3) . ? Li2 P1 2.533(3) 9 ? Li2 Li1 2.856(11) 9 ? Li2 Li1 2.856(11) . ? Li2 Li1 2.856(11) 5 ? Li1 O1S 1.941(9) . ? Li1 P1 2.593(13) 11_566 ? Li1 P1 2.635(9) . ? Li1 P1 2.677(13) 9 ? Li1 Li1 2.816(18) 4_566 ? P1 C11 1.877(3) . ? P1 Li1 2.593(13) 8_656 ? P1 Li1 2.677(13) 5 ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? O1S C4S' 1.27(3) . ? O1S C1S 1.394(8) . ? O1S C4S 1.474(10) . ? C1S C2S 1.460(11) . ? C2S C3S 1.458(10) . ? C3S C4S 1.410(12) . ? C3S C4S' 1.73(3) . ? C4S' Li3 2.36(3) . ? Li3 C4S' 2.36(3) 43_654 ? Li3 C4S' 2.36(3) 4_566 ? Li3 C4S' 2.36(3) 42_645 ? Li3Y O1T 1.981(18) 30_566 ? Li3Y O1T 1.981(18) . ? Li3Y O1T 1.981(18) 84_665 ? O1T C1T 1.55(3) . ? O1T C4T 1.57(3) . ? C1T C2T 1.55(3) . ? C2T C3T 1.53(3) . ? C3T C4T 1.54(3) . ? O1U C3U 1.14(10) . ? O1U C2U 1.77(11) 64_655 ? O1U C2U 1.58(12) . ? O1U C1U 1.37(18) 74_675 ? C1U C3U 1.62(19) . ? C1U O1U 1.37(18) 74_675 ? C1U C2U 2.20(18) 64_655 ? C2U C3U 0.89(8) 39_465 ? C2U O1U 1.77(11) 39_465 ? C2U C2U 1.49(7) 64_655 ? C2U C2U 1.49(7) 39_465 ? C2U C1U 2.20(18) 39_465 ? C2U C3U 1.75(11) . ? C2U C2U 2.08(9) 74_675 ? C3U C2U 0.89(8) 64_655 ? 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 Li2 Br1 Li2 109.471(1) 2_665 . ? Li2 Br1 Li2 109.5 2_665 4_566 ? Li2 Br1 Li2 109.471(3) . 4_566 ? Li2 Br1 Li2 109.471(1) 2_665 3_656 ? Li2 Br1 Li2 109.471(1) . 3_656 ? Li2 Br1 Li2 109.5 4_566 3_656 ? C1 Al1 P1 114.68(7) . . ? C1 Al1 P1 114.68(7) . 11_566 ? P1 Al1 P1 103.79(8) . 11_566 ? C1 Al1 P1 114.68(7) . 8_656 ? P1 Al1 P1 103.79(8) . 8_656 ? P1 Al1 P1 103.79(8) 11_566 8_656 ? C1 Al1 Li1 112.32(19) . 8_656 ? P1 Al1 Li1 54.1(2) . 8_656 ? P1 Al1 Li1 133.0(2) 11_566 8_656 ? P1 Al1 Li1 55.1(2) 8_656 8_656 ? C1 Al1 Li1 112.32(19) . 11_566 ? P1 Al1 Li1 133.0(2) . 11_566 ? P1 Al1 Li1 55.1(2) 11_566 11_566 ? P1 Al1 Li1 54.1(2) 8_656 11_566 ? Li1 Al1 Li1 106.5(2) 8_656 11_566 ? C1 Al1 Li1 112.32(19) . . ? P1 Al1 Li1 55.1(2) . . ? P1 Al1 Li1 54.1(2) 11_566 . ? P1 Al1 Li1 133.0(2) 8_656 . ? Li1 Al1 Li1 106.5(2) 8_656 . ? Li1 Al1 Li1 106.5(2) 11_566 . ? Al1' Li2 P1 79.1(3) 2_665 5 ? Al1' Li2 P1 79.1(3) 2_665 . ? P1 Li2 P1 116.53(19) 5 . ? Al1' Li2 P1 79.1(3) 2_665 9 ? P1 Li2 P1 116.53(19) 5 9 ? P1 Li2 P1 116.53(19) . 9 ? Al1' Li2 Br1 180.0(14) 2_665 . ? P1 Li2 Br1 100.9(3) 5 . ? P1 Li2 Br1 100.9(3) . . ? P1 Li2 Br1 100.9(3) 9 . ? Al1' Li2 Li1 78.0(3) 2_665 9 ? P1 Li2 Li1 59.2(2) 5 9 ? P1 Li2 Li1 157.1(6) . 9 ? P1 Li2 Li1 58.2(2) 9 9 ? Br1 Li2 Li1 102.0(3) . 9 ? Al1' Li2 Li1 78.0(3) 2_665 . ? P1 Li2 Li1 157.1(6) 5 . ? P1 Li2 Li1 58.2(2) . . ? P1 Li2 Li1 59.2(2) 9 . ? Br1 Li2 Li1 102.0(3) . . ? Li1 Li2 Li1 115.8(2) 9 . ? P1 Li2 Li1 58.2(2) 5 5 ? P1 Li2 Li1 59.2(2) . 5 ? P1 Li2 Li1 157.1(6) 9 5 ? Br1 Li2 Li1 102.0(3) . 5 ? Li1 Li2 Li1 115.8(2) 9 5 ? Li1 Li2 Li1 115.8(2) . 5 ? O1S Li1 P1 115.4(6) . 11_566 ? O1S Li1 P1 117.2(4) . . ? P1 Li1 P1 94.6(4) 11_566 . ? O1S Li1 P1 112.2(5) . 9 ? P1 Li1 P1 107.4(3) 11_566 9 ? P1 Li1 P1 108.4(4) . 9 ? O1S Li1 Li2 143.2(7) . . ? P1 Li1 Li2 101.3(4) 11_566 . ? P1 Li1 Li2 54.8(2) . . ? P1 Li1 Li2 54.4(2) 9 . ? O1S Li1 Li1 107.4(3) . 4_566 ? P1 Li1 Li1 59.2(5) 11_566 4_566 ? P1 Li1 Li1 134.9(2) . 4_566 ? P1 Li1 Li1 56.3(4) 9 4_566 ? Li2 Li1 Li1 92.4(4) . 4_566 ? O1S Li1 Al1 113.7(5) . . ? P1 Li1 Al1 49.7(2) 11_566 . ? P1 Li1 Al1 49.48(19) . . ? P1 Li1 Al1 134.1(3) 9 . ? Li2 Li1 Al1 88.1(3) . . ? Li1 Li1 Al1 107.3(6) 4_566 . ? C11 P1 Al1 111.36(16) . . ? C11 P1 Li2 121.9(3) . . ? Al1 P1 Li2 113.1(3) . . ? C11 P1 Li1 119.4(3) . 8_656 ? Al1 P1 Li1 76.2(2) . 8_656 ? Li2 P1 Li1 106.1(3) . 8_656 ? C11 P1 Li1 90.7(2) . . ? Al1 P1 Li1 75.4(3) . . ? Li2 P1 Li1 67.1(3) . . ? Li1 P1 Li1 144.5(3) 8_656 . ? C11 P1 Li1 101.6(3) . 5 ? Al1 P1 Li1 137.7(3) . 5 ? Li2 P1 Li1 66.4(2) . 5 ? Li1 P1 Li1 64.6(3) 8_656 5 ? Li1 P1 Li1 131.2(4) . 5 ? C12 C11 C16 120.0 . . ? C12 C11 P1 116.6(2) . . ? C16 C11 P1 123.4(2) . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C4S' O1S C1S 94.9(12) . . ? C4S' O1S C4S 45.4(13) . . ? C1S O1S C4S 106.9(5) . . ? C4S' O1S Li1 129.8(11) . . ? C1S O1S Li1 123.8(5) . . ? C4S O1S Li1 128.3(6) . . ? O1S C1S C2S 108.0(6) . . ? C3S C2S C1S 104.0(6) . . ? C2S C3S C4S 106.1(6) . . ? C2S C3S C4S' 93.8(10) . . ? C4S C3S C4S' 38.5(11) . . ? O1S C4S C3S 107.2(7) . . ? O1S C4S' C3S 100.4(15) . . ? O1S C4S' Li3 162.7(19) . . ? C3S C4S' Li3 86.3(11) . . ? C4S' Li3 C4S' 132.4(8) 43_654 4_566 ? C4S' Li3 C4S' 69.6(12) 43_654 42_645 ? C4S' Li3 C4S' 132.4(7) 4_566 42_645 ? C4S' Li3 C4S' 132.4(7) 43_654 . ? C4S' Li3 C4S' 69.6(12) 4_566 . ? C4S' Li3 C4S' 132.4(7) 42_645 . ? O1T Li3Y O1T 114.2(8) 30_566 . ? O1T Li3Y O1T 114.2(8) 30_566 84_665 ? O1T Li3Y O1T 114.2(8) . 84_665 ? C1T O1T C4T 102.7(14) . . ? C1T O1T Li3Y 134(3) . . ? C4T O1T Li3Y 118(3) . . ? C2T C1T O1T 104.6(11) . . ? C3T C2T C1T 107.2(8) . . ? C2T C3T C4T 106.5(10) . . ? C3T C4T O1T 103.0(14) . . ? C3U O1U C1U 111(10) . 74_675 ? C2U O1U C1U 115(9) 64_655 74_675 ? C2U O1U C1U 101(9) . 74_675 ? C3U C2U C2U 111(8) 39_465 64_655 ? O1U C2U C2U 111(5) 39_465 64_655 ? C3U C2U C2U 91(8) 39_465 39_465 ? C3U C2U O1U 170(8) 39_465 . ? O1U C2U O1U 156(5) 39_465 . ? C2U C2U O1U 99(6) 39_465 . ? C2U C2U C1U 102(6) 39_465 39_465 ? O1U C2U C1U 137(7) . 39_465 ? C3U C2U C3U 142(8) 39_465 . ? O1U C2U C3U 136(5) 39_465 . ? C1U C2U C3U 103(6) 39_465 . ? C3U C2U C2U 95(6) 39_465 74_675 ? O1U C3U C2U 120(10) . 64_655 ? O1U C3U C1U 95(10) . . ? C2U C3U C1U 119(10) 64_655 . ? O1U C3U C2U 62(6) . . ? C2U C3U C2U 58(6) 64_655 . ? C1U C3U C2U 120(9) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.533 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.051 # Attachment '- 2Br.cif' data_dw0615 _database_code_depnum_ccdc_archive 'CCDC 797472' #TrackingRef '- 2Br.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H196 Br Ga4 Li17 O17 P12' _chemical_formula_weight 3047.42 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' Li Li -0.0003 0.0001 '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' P P 0.1023 0.0942 '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 cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 35.133(4) _cell_length_b 35.133(4) _cell_length_c 35.133(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 43365(9) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 34937 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.488 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12688 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 0.730 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 20149 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3158 _reflns_number_gt 2447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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. Three isolated residual maxima of electron density were assigned as partial C- and O-atoms of one THF solvate per cluster anion, which was highly disordered across a site of -4 symmetry. High displacement parameters associated with the ligand atoms indicated considerable unresolved disorder resulting in poor diffraction at high angle; data in the limited theta range < 21o were used in the full matrix refinement as a chiral twin (51:49%). There was additionally a small disorder of the cluster anion with its enantiomer (ca. 10%) and only the contribition from the metal atom (Ga1') of the minor component was allowed for in the refinement. The H-atoms of the disordered THF solvate and the disordered fourth THF of the [Li(thf)4]+ cation were not included in the refinement. ; _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^)+(0.1437P)^2^+117.5890P] 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 3158 _refine_ls_number_parameters 164 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.2235 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.088 _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 Br1 Br 0.5000 0.5000 0.5000 0.0581(5) Uani 1 12 d S . . Ga1 Ga 0.569741(17) 0.569741(17) 0.430259(17) 0.0499(3) Uani 0.90 3 d SP A 1 C11 C 0.60247(17) 0.60247(17) 0.39753(17) 0.070(3) Uani 1 3 d S . . H11A H 0.6040 0.5916 0.3725 0.105 Uiso 0.33 1 calc PR A 1 H11B H 0.6275 0.6040 0.4084 0.105 Uiso 0.33 1 calc PR A 1 H11C H 0.5916 0.6275 0.3960 0.105 Uiso 0.33 1 calc PR A 1 P1 P 0.56021(4) 0.59291(4) 0.49542(5) 0.0622(4) Uani 1 1 d . . . Li1 Li 0.5407(3) 0.5407(3) 0.5407(3) 0.065(4) Uani 1 3 d S . . Li2 Li 0.6120(2) 0.5402(3) 0.5018(4) 0.069(3) Uani 1 1 d . . . C1 C 0.59551(14) 0.63048(12) 0.50681(14) 0.0729(16) Uani 1 1 d G A . C2 C 0.60822(16) 0.65782(14) 0.48119(14) 0.091(2) Uani 1 1 d G . . H2 H 0.5999 0.6573 0.4561 0.109 Uiso 1 1 calc R A . C3 C 0.63339(16) 0.68592(13) 0.4931(2) 0.102(3) Uani 1 1 d G A . H3 H 0.6419 0.7042 0.4760 0.123 Uiso 1 1 calc R . . C4 C 0.6459(2) 0.68668(18) 0.5307(2) 0.151(5) Uani 1 1 d G . . H4 H 0.6627 0.7055 0.5386 0.181 Uiso 1 1 calc R A . C5 C 0.6332(3) 0.6593(2) 0.55628(18) 0.170(6) Uani 1 1 d G A . H5 H 0.6415 0.6598 0.5814 0.204 Uiso 1 1 calc R . . C6 C 0.6080(2) 0.63123(18) 0.54435(14) 0.142(5) Uani 1 1 d G . . H6 H 0.5995 0.6129 0.5615 0.170 Uiso 1 1 calc R A . O1 O 0.66447(11) 0.55629(13) 0.50397(16) 0.0770(12) Uani 1 1 d . . . C1S C 0.6813(3) 0.5800(3) 0.4783(3) 0.118(3) Uani 1 1 d . A . H1S1 H 0.6631 0.5988 0.4695 0.141 Uiso 1 1 calc R . . H1S2 H 0.6901 0.5656 0.4564 0.141 Uiso 1 1 calc R . . C2S C 0.7143(2) 0.5995(3) 0.4972(4) 0.131(4) Uani 1 1 d . . . H2S1 H 0.7351 0.6036 0.4795 0.157 Uiso 1 1 calc R A . H2S2 H 0.7068 0.6236 0.5083 0.157 Uiso 1 1 calc R . . C3S C 0.7245(3) 0.5716(4) 0.5266(4) 0.142(4) Uani 1 1 d . A . H3S1 H 0.7377 0.5839 0.5475 0.171 Uiso 0.69 1 calc PR B 1 H3S2 H 0.7408 0.5519 0.5161 0.171 Uiso 0.69 1 calc PR B 1 H3S3 H 0.7200 0.5815 0.5520 0.171 Uiso 0.31 1 calc PR B 2 H3S4 H 0.7509 0.5638 0.5244 0.171 Uiso 0.31 1 calc PR B 2 C4S C 0.6907(4) 0.5568(7) 0.5385(5) 0.121(6) Uani 0.69 1 d P A 1 H4S1 H 0.6799 0.5723 0.5586 0.145 Uiso 0.69 1 calc PR A 1 H4S2 H 0.6944 0.5312 0.5482 0.145 Uiso 0.69 1 calc PR A 1 C4S' C 0.6952(7) 0.5367(7) 0.5162(8) 0.073(6) Uiso 0.31 1 d P A 2 H4S3 H 0.7054 0.5204 0.4964 0.088 Uiso 0.31 1 calc PR A 2 H4S4 H 0.6893 0.5215 0.5385 0.088 Uiso 0.31 1 calc PR A 2 Li3Y Li 0.6891 0.6891 0.6891 0.12(4) Uiso 0.25 3 d SPD . . O1T O 0.6583(13) 0.6636(12) 0.7305(12) 0.21(2) Uiso 0.25 1 d PD . . C1T C 0.6499(15) 0.6178(12) 0.7379(13) 0.154(18) Uiso 0.25 1 d PD . . H1T1 H 0.6355 0.6070 0.7169 0.184 Uiso 0.25 1 calc PR . . H1T2 H 0.6735 0.6038 0.7406 0.184 Uiso 0.25 1 calc PR . . C2T C 0.6249(12) 0.6158(10) 0.7777(11) 0.116(12) Uiso 0.25 1 d PD . . H2T1 H 0.6415 0.6122 0.7994 0.140 Uiso 0.25 1 calc PR . . H2T2 H 0.6068 0.5950 0.7768 0.140 Uiso 0.25 1 calc PR . . C3T C 0.6026(13) 0.6568(10) 0.7810(13) 0.129(14) Uiso 0.25 1 d PD . . H3T1 H 0.6012 0.6650 0.8073 0.155 Uiso 0.25 1 calc PR . . H3T2 H 0.5769 0.6546 0.7711 0.155 Uiso 0.25 1 calc PR . . C4T C 0.627(3) 0.6874(10) 0.756(3) 0.42(11) Uiso 0.25 1 d PD . . H4T1 H 0.6103 0.7016 0.7389 0.507 Uiso 0.25 1 calc PR . . H4T2 H 0.6400 0.7053 0.7722 0.507 Uiso 0.25 1 calc PR . . O1W O 0.7222(3) 0.7222(3) 0.7222(3) 0.17(2) Uiso 0.25 3 d SPD . . C1W C 0.7275(15) 0.7725(15) 0.7275(15) 0.20(3) Uiso 0.50 3 d SP . . C2W C 0.7500 0.7500 0.711(3) 0.19(3) Uiso 0.33 2 d SP . . O1X O 0.7522(16) 0.7244(17) 0.5224(18) 0.075(14) Uiso 0.08 1 d P . . C1X C 0.7416(16) 0.7225(16) 0.4967(17) 0.096(12) Uiso 0.17 1 d P . . C2X C 0.7925(19) 0.7278(19) 0.5524(19) 0.113(17) Uiso 0.17 1 d P . . Ga1' Ga 0.43069(16) 0.43069(16) 0.56931(16) 0.056(2) Uani 0.10 3 d SP . 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 Br1 0.0581(5) 0.0581(5) 0.0581(5) 0.000 0.000 0.000 Ga1 0.0499(3) 0.0499(3) 0.0499(3) 0.0049(3) 0.0049(3) -0.0049(3) C11 0.070(3) 0.070(3) 0.070(3) 0.009(3) 0.009(3) -0.009(3) P1 0.0583(8) 0.0528(8) 0.0757(10) -0.0016(7) 0.0012(7) -0.0081(6) Li1 0.065(4) 0.065(4) 0.065(4) 0.000(5) 0.000(5) 0.000(5) Li2 0.044(4) 0.056(5) 0.106(8) 0.014(6) -0.006(5) 0.007(3) C1 0.067(4) 0.061(3) 0.091(5) -0.010(3) 0.001(3) -0.014(3) C2 0.084(5) 0.069(4) 0.120(6) 0.003(4) 0.012(4) -0.015(3) C3 0.083(5) 0.069(4) 0.155(9) -0.013(5) 0.008(5) -0.012(4) C4 0.103(8) 0.111(8) 0.239(16) -0.049(9) -0.040(9) -0.029(6) C5 0.200(14) 0.140(10) 0.171(12) -0.020(9) -0.070(11) -0.074(10) C6 0.199(12) 0.109(7) 0.118(8) -0.003(6) -0.064(8) -0.063(8) O1 0.049(2) 0.081(3) 0.101(3) 0.006(3) 0.000(2) -0.0122(18) C1S 0.071(5) 0.154(9) 0.128(7) 0.049(7) -0.002(5) 0.008(5) C2S 0.069(5) 0.134(7) 0.190(10) 0.017(9) 0.005(7) -0.043(5) C3S 0.083(7) 0.205(13) 0.139(10) 0.007(9) -0.038(6) -0.001(7) C4S 0.077(9) 0.175(16) 0.110(11) 0.020(11) -0.023(7) -0.025(9) Ga1' 0.056(2) 0.056(2) 0.056(2) 0.002(3) 0.002(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Li1 2.48(2) . ? Br1 Li1 2.48(2) 4_566 ? Br1 Li1 2.48(2) 3_656 ? Br1 Li1 2.48(2) 2_665 ? Ga1 C11 1.992(11) . ? Ga1 P1 2.4527(18) . ? Ga1 P1 2.4527(18) 11_566 ? Ga1 P1 2.4527(18) 8_656 ? Ga1 Li2 3.099(12) . ? Ga1 Li2 3.099(12) 11_566 ? Ga1 Li2 3.099(12) 8_656 ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? P1 C1 1.855(4) . ? P1 Li1 2.523(5) . ? P1 Li2 2.600(14) 8_656 ? P1 Li2 2.607(9) . ? P1 Ga1' 2.744(5) 2_665 ? P1 Li2 2.671(12) 5 ? Li1 Ga1' 1.74(2) 2_665 ? Li1 P1 2.523(5) 9 ? Li1 P1 2.523(5) 5 ? Li1 Li2 2.853(12) 5 ? Li1 Li2 2.853(12) . ? Li1 Li2 2.853(12) 9 ? Li2 O1 1.930(10) . ? Li2 P1 2.600(14) 11_566 ? Li2 P1 2.671(12) 9 ? Li2 C1S 2.928(14) . ? Li2 Li2 2.826(19) 4_566 ? Li2 Ga1' 2.987(14) 2_665 ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? O1 C1S 1.365(11) . ? O1 C4S' 1.35(2) . ? O1 C4S 1.525(15) . ? C1S C2S 1.501(15) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S C3S 1.466(16) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S C4S 1.36(2) . ? C3S C4S' 1.64(3) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C3S H3S3 0.9700 . ? C3S H3S4 0.9700 . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? C4S' H4S3 0.9700 . ? C4S' H4S4 0.9700 . ? Li3Y O1T 2.023(18) 5 ? Li3Y O1T 2.023(18) 9 ? Li3Y O1T 2.023(18) . ? Li3Y O1W 2.02(2) . ? O1T C4T 1.64(3) . ? O1T C1T 1.66(3) . ? C1T C2T 1.65(3) . ? C1T H1T1 0.9700 . ? C1T H1T2 0.9700 . ? C2T C3T 1.64(3) . ? C2T H2T1 0.9700 . ? C2T H2T2 0.9700 . ? C3T C4T 1.64(3) . ? C3T H3T1 0.9700 . ? C3T H3T2 0.9700 . ? C4T H4T1 0.9700 . ? C4T H4T2 0.9700 . ? O1W C2W 1.43(3) 9 ? O1W C2W 1.43(3) 5 ? O1W C2W 1.43(3) . ? O1W C1W 1.79(4) 74_665 ? O1W C1W 1.79(4) . ? O1W C1W 1.79(4) 28_566 ? C1W C2W 1.26(5) 35_566 ? C1W C2W 1.26(5) . ? C1W C2W 1.26(5) 5 ? C1W O1W 1.79(4) 74_665 ? C1W O1W 1.79(4) 28_566 ? C2W O1W 1.43(3) 74_665 ? C2W C1W 1.26(5) 74_665 ? O1X C1X 0.98(7) . ? O1X C2X 1.77(9) . ? O1X C1X 1.27(9) 40_645 ? O1X C1X 1.72(8) 63_465 ? C1X O1X 1.27(9) 63_465 ? C1X C2X 1.87(9) 63_465 ? C1X C1X 1.45(8) 40_645 ? C1X C1X 1.45(8) 63_465 ? C1X O1X 1.72(8) 40_645 ? C2X C1X 1.87(9) 40_645 ? 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 Li1 Br1 Li1 109.471(4) . 4_566 ? Li1 Br1 Li1 109.471(2) . 3_656 ? Li1 Br1 Li1 109.471(1) 4_566 3_656 ? Li1 Br1 Li1 109.5 . 2_665 ? Li1 Br1 Li1 109.471(1) 4_566 2_665 ? Li1 Br1 Li1 109.471(1) 3_656 2_665 ? C11 Ga1 P1 115.22(4) . . ? C11 Ga1 P1 115.22(4) . 11_566 ? P1 Ga1 P1 103.16(4) . 11_566 ? C11 Ga1 P1 115.22(4) . 8_656 ? P1 Ga1 P1 103.16(4) . 8_656 ? P1 Ga1 P1 103.16(4) 11_566 8_656 ? C11 Ga1 Li2 112.66(18) . . ? P1 Ga1 Li2 132.12(19) 8_656 . ? C11 Ga1 Li2 112.66(18) . 11_566 ? P1 Ga1 Li2 132.12(19) . 11_566 ? Li2 Ga1 Li2 106.1(2) . 11_566 ? C11 Ga1 Li2 112.66(18) . 8_656 ? P1 Ga1 Li2 132.12(19) 11_566 8_656 ? Li2 Ga1 Li2 106.1(2) . 8_656 ? Li2 Ga1 Li2 106.1(2) 11_566 8_656 ? Ga1 C11 H11A 109.5 . . ? Ga1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Ga1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 P1 Li1 124.2(5) . . ? C1 P1 Ga1 110.25(18) . . ? Li1 P1 Ga1 112.6(4) . . ? C1 P1 Li2 118.7(3) . 8_656 ? Li1 P1 Li2 105.3(4) . 8_656 ? Ga1 P1 Li2 75.6(2) . 8_656 ? C1 P1 Li2 91.2(3) . . ? Li1 P1 Li2 67.6(3) . . ? Ga1 P1 Li2 75.5(3) . . ? Li2 P1 Li2 144.1(3) 8_656 . ? C1 P1 Ga1' 86.2(2) . 2_665 ? Ga1 P1 Ga1' 140.08(12) . 2_665 ? Li2 P1 Ga1' 129.1(3) 8_656 2_665 ? Li2 P1 Ga1' 67.8(3) . 2_665 ? C1 P1 Li2 102.0(3) . 5 ? Li1 P1 Li2 66.6(2) . 5 ? Ga1 P1 Li2 137.5(3) . 5 ? Li2 P1 Li2 64.8(3) 8_656 5 ? Li2 P1 Li2 131.6(5) . 5 ? Br1 Li1 P1 102.2(4) . 9 ? Br1 Li1 P1 102.2(4) . . ? P1 Li1 P1 115.6(3) 9 . ? Br1 Li1 P1 102.2(4) . 5 ? P1 Li1 P1 115.6(3) 9 5 ? P1 Li1 P1 115.6(3) . 5 ? Br1 Li1 Li2 103.1(5) . 5 ? P1 Li1 Li2 154.7(9) 9 5 ? Br1 Li1 Li2 103.1(5) . . ? P1 Li1 Li2 154.7(9) 5 . ? Li2 Li1 Li2 115.0(3) 5 . ? Br1 Li1 Li2 103.1(5) . 9 ? P1 Li1 Li2 154.7(9) . 9 ? Li2 Li1 Li2 115.0(3) 5 9 ? Li2 Li1 Li2 115.0(3) . 9 ? O1 Li2 P1 114.9(6) . 11_566 ? O1 Li2 P1 117.5(4) . . ? P1 Li2 P1 95.1(4) 11_566 . ? O1 Li2 P1 112.5(5) . 9 ? P1 Li2 P1 107.2(3) 11_566 9 ? P1 Li2 P1 108.0(4) . 9 ? P1 Li2 C1S 102.0(5) 11_566 . ? P1 Li2 C1S 102.5(4) . . ? P1 Li2 C1S 135.0(4) 9 . ? O1 Li2 Li2 107.1(3) . 4_566 ? P1 Li2 Li2 134.9(3) . 4_566 ? P1 Li2 Li2 56.4(4) 9 4_566 ? C1S Li2 Li2 117.7(4) . 4_566 ? O1 Li2 Li1 144.8(8) . . ? P1 Li2 Li1 100.3(5) 11_566 . ? C1S Li2 Li1 149.5(6) . . ? Li2 Li2 Li1 91.6(4) 4_566 . ? O1 Li2 Ga1 113.0(5) . . ? P1 Li2 Ga1 134.4(3) 9 . ? C1S Li2 Ga1 90.5(4) . . ? Li2 Li2 Ga1 107.4(6) 4_566 . ? Li1 Li2 Ga1 88.0(3) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 124.5(3) . . ? C6 C1 P1 115.4(3) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C1S O1 C4S' 100.2(12) . . ? C1S O1 C4S 105.0(8) . . ? C1S O1 Li2 124.5(6) . . ? C4S' O1 Li2 128.8(11) . . ? C4S O1 Li2 127.8(8) . . ? O1 C1S C2S 108.6(9) . . ? C2S C1S Li2 137.3(8) . . ? O1 C1S H1S1 110.0 . . ? C2S C1S H1S1 110.0 . . ? Li2 C1S H1S1 82.4 . . ? O1 C1S H1S2 110.0 . . ? C2S C1S H1S2 110.0 . . ? Li2 C1S H1S2 103.8 . . ? H1S1 C1S H1S2 108.4 . . ? C3S C2S C1S 101.5(8) . . ? C3S C2S H2S1 111.5 . . ? C1S C2S H2S1 111.5 . . ? C3S C2S H2S2 111.5 . . ? C1S C2S H2S2 111.5 . . ? H2S1 C2S H2S2 109.3 . . ? C2S C3S C4S 105.0(10) . . ? C2S C3S C4S' 100.8(11) . . ? C2S C3S H3S1 110.7 . . ? C4S C3S H3S1 110.7 . . ? C4S' C3S H3S1 143.1 . . ? C2S C3S H3S2 110.7 . . ? C4S C3S H3S2 110.7 . . ? C4S' C3S H3S2 75.6 . . ? H3S1 C3S H3S2 108.8 . . ? C2S C3S H3S3 111.6 . . ? C4S C3S H3S3 73.3 . . ? C4S' C3S H3S3 111.6 . . ? H3S2 C3S H3S3 134.4 . . ? C2S C3S H3S4 111.6 . . ? C4S C3S H3S4 138.3 . . ? C4S' C3S H3S4 111.6 . . ? H3S1 C3S H3S4 74.3 . . ? H3S3 C3S H3S4 109.4 . . ? C3S C4S O1 106.6(13) . . ? C3S C4S H4S1 110.4 . . ? O1 C4S H4S1 110.4 . . ? C3S C4S H4S2 110.4 . . ? O1 C4S H4S2 110.4 . . ? H4S1 C4S H4S2 108.6 . . ? O1 C4S' C3S 101.1(16) . . ? O1 C4S' H4S3 111.5 . . ? C3S C4S' H4S3 111.5 . . ? O1 C4S' H4S4 111.5 . . ? C3S C4S' H4S4 111.5 . . ? H4S3 C4S' H4S4 109.4 . . ? O1T Li3Y O1T 117.8(8) 5 9 ? O1T Li3Y O1T 117.8(8) 5 . ? O1T Li3Y O1T 117.8(8) 9 . ? O1T Li3Y O1W 98.6(16) 5 . ? O1T Li3Y O1W 98.6(16) 9 . ? O1T Li3Y O1W 98.6(16) . . ? C4T O1T C1T 107.1(9) . . ? C4T O1T Li3Y 121(2) . . ? C1T O1T Li3Y 130(2) . . ? C2T C1T O1T 105.5(11) . . ? C2T C1T H1T1 110.6 . . ? O1T C1T H1T1 110.6 . . ? C2T C1T H1T2 110.6 . . ? O1T C1T H1T2 110.6 . . ? H1T1 C1T H1T2 108.8 . . ? C1T C2T C3T 106.0(11) . . ? C1T C2T H2T1 110.5 . . ? C3T C2T H2T1 110.5 . . ? C1T C2T H2T2 110.5 . . ? C3T C2T H2T2 110.5 . . ? H2T1 C2T H2T2 108.7 . . ? C2T C3T C4T 106.6(11) . . ? C2T C3T H3T1 110.4 . . ? C4T C3T H3T1 110.4 . . ? C2T C3T H3T2 110.4 . . ? C4T C3T H3T2 110.4 . . ? H3T1 C3T H3T2 108.6 . . ? O1T C4T C3T 108.0(7) . . ? O1T C4T H4T1 110.1 . . ? C3T C4T H4T1 110.1 . . ? O1T C4T H4T2 110.1 . . ? C3T C4T H4T2 110.1 . . ? H4T1 C4T H4T2 108.4 . . ? C2W O1W C2W 85(6) 9 5 ? C2W O1W C2W 85(6) 9 . ? C2W O1W C2W 85(6) 5 . ? C2W O1W C1W 97(4) 5 74_665 ? C2W O1W C1W 97(4) 9 . ? C1W O1W C1W 78(4) 74_665 . ? C2W O1W C1W 97(4) . 28_566 ? C1W O1W C1W 78(4) 74_665 28_566 ? C1W O1W C1W 78(4) . 28_566 ? C2W O1W Li3Y 129(4) 9 . ? C2W O1W Li3Y 129(4) 5 . ? C2W O1W Li3Y 129(4) . . ? C1W O1W Li3Y 134(3) 74_665 . ? C1W O1W Li3Y 134(3) . . ? C1W O1W Li3Y 134(3) 28_566 . ? C2W C1W C2W 100(8) 35_566 . ? C2W C1W C2W 100(8) 35_566 5 ? C2W C1W C2W 100(8) . 5 ? C2W C1W O1W 126(9) 5 74_665 ? C2W C1W O1W 126(9) 35_566 . ? O1W C1W O1W 101(3) 74_665 . ? C2W C1W O1W 126(9) . 28_566 ? O1W C1W O1W 101(3) 74_665 28_566 ? O1W C1W O1W 101(3) . 28_566 ? O1W C2W O1W 148(8) 74_665 . ? C1W C2W C1W 126(10) 74_665 . ? C1X O1X C2X 149(7) . . ? C2X O1X C1X 132(5) . 63_465 ? O1X C1X O1X 128(8) . 63_465 ? O1X C1X C2X 166(7) . 63_465 ? O1X C1X C1X 100(5) 63_465 40_645 ? C2X C1X C1X 120(6) 63_465 40_645 ? C2X C1X C1X 106(6) 63_465 63_465 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.090 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.082 # Attachment '- 2I.cif' data_dw0733 _database_code_depnum_ccdc_archive 'CCDC 797473' #TrackingRef '- 2I.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H188 Ga4 I0.50 Li16.50 O14.50 P12' _chemical_formula_weight 2859.32 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' Li Li -0.0003 0.0001 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 35.019(4) _cell_length_b 35.019(4) _cell_length_c 35.019(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 42944(8) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 59007 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 24.11 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11904 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_T_max 0.766 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 31422 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 4.36 _diffrn_reflns_theta_max 20.96 _reflns_number_total 1888 _reflns_number_gt 1653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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. Two isolated maxima of electron density were assigned as partial C- and O-atoms of a half THF solvate per cluster anion, which was highly disordered across a site of -4 symmetry. The H-atoms of this 1/2 THF were not included in refinement. High displacement parameters associated with theligand atoms indicated considerable unresolved disorder resulting in poor diffraction at high angle; data in the limited theta range < 21o were used in the full matrix refinement as a chiral twin (51:49%). There was additionally a small disorder of the cluster anion with its enantiomer (ca. 13%) and only the contribition from the metal atom (Ga1') of the minor component was allowed for in the refinemente. The H-atoms of the highly disordered THF solvate were not included. ; _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^)+(0.1021P)^2^+78.8304P] 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 1888 _refine_ls_number_parameters 178 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.003 _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 I1 I 0.5000 0.5000 0.5000 0.0485(6) Uani 0.50 12 d SP . . Ga1 Ga 0.569999(18) 0.569999(18) 0.430001(18) 0.0557(4) Uani 0.92 3 d SP A 1 P1 P 0.56051(4) 0.59322(4) 0.49517(5) 0.0648(5) Uani 1 1 d . . . C11 C 0.59583(19) 0.63041(17) 0.5060(2) 0.0741(18) Uani 1 1 d . A . C12 C 0.6082(2) 0.6577(2) 0.4820(3) 0.093(2) Uani 1 1 d . . . H12 H 0.5994 0.6582 0.4569 0.112 Uiso 1 1 calc R A . C13 C 0.6350(2) 0.6865(2) 0.4949(5) 0.114(3) Uani 1 1 d . A . H13 H 0.6438 0.7046 0.4777 0.136 Uiso 1 1 calc R . . C14 C 0.6470(3) 0.6877(4) 0.5300(5) 0.142(4) Uani 1 1 d . . . H14 H 0.6635 0.7068 0.5383 0.170 Uiso 1 1 calc R A . C15 C 0.6349(4) 0.6604(4) 0.5539(4) 0.172(5) Uani 1 1 d . A . H15 H 0.6438 0.6606 0.5789 0.207 Uiso 1 1 calc R . . C16 C 0.6104(3) 0.6326(3) 0.5434(3) 0.138(4) Uani 1 1 d . . . H16 H 0.6029 0.6145 0.5613 0.166 Uiso 1 1 calc R A . Li1 Li 0.5411(4) 0.5411(4) 0.5411(4) 0.070(5) Uani 1 3 d S . . Li2 Li 0.6119(3) 0.5393(3) 0.5010(4) 0.072(3) Uani 1 1 d . . . C10 C 0.60304(17) 0.60304(17) 0.39696(17) 0.075(3) Uani 1 3 d S . . H10A H 0.6049 0.5920 0.3720 0.112 Uiso 0.33 1 calc PR A 1 H10B H 0.6280 0.6049 0.4080 0.112 Uiso 0.33 1 calc PR A 1 H10C H 0.5920 0.6280 0.3951 0.112 Uiso 0.33 1 calc PR A 1 O1 O 0.66508(11) 0.55590(12) 0.50370(16) 0.0816(12) Uani 1 1 d . . . C1T C 0.6813(2) 0.5805(3) 0.4780(3) 0.114(3) Uani 1 1 d . A . H1T1 H 0.6627 0.5992 0.4697 0.137 Uiso 1 1 calc R . . H1T2 H 0.6901 0.5665 0.4558 0.137 Uiso 1 1 calc R . . C2T C 0.7146(2) 0.6001(3) 0.4973(4) 0.121(3) Uani 1 1 d . . . H2T1 H 0.7354 0.6045 0.4796 0.145 Uiso 1 1 calc R A . H2T2 H 0.7069 0.6243 0.5085 0.145 Uiso 1 1 calc R . . C3T C 0.7254(3) 0.5729(4) 0.5266(3) 0.141(4) Uani 1 1 d . A . H3TA H 0.7419 0.5533 0.5162 0.169 Uiso 0.50 1 calc PR B 1 H3TB H 0.7385 0.5855 0.5475 0.169 Uiso 0.50 1 calc PR B 1 H3TC H 0.7217 0.5834 0.5519 0.169 Uiso 0.50 1 calc PR B 2 H3TD H 0.7518 0.5651 0.5238 0.169 Uiso 0.50 1 calc PR B 2 C4T C 0.6913(5) 0.5574(5) 0.5388(5) 0.093(5) Uiso 0.50 1 d P A 1 H4T1 H 0.6801 0.5731 0.5586 0.111 Uiso 0.50 1 calc PR A 1 H4T2 H 0.6953 0.5319 0.5490 0.111 Uiso 0.50 1 calc PR A 1 C4T' C 0.6957(5) 0.5364(5) 0.5187(5) 0.094(5) Uiso 0.50 1 d P A 2 H4T3 H 0.7062 0.5183 0.5005 0.113 Uiso 0.50 1 calc PR A 2 H4T4 H 0.6890 0.5232 0.5421 0.113 Uiso 0.50 1 calc PR A 2 Li3Y Li 0.6899(13) 0.8101(13) 0.3101(13) 0.15(10) Uiso 0.12 3 d SPD . . O1S O 0.6565(12) 0.7704(12) 0.3377(10) 0.113(14) Uiso 0.13 1 d PD . . C1S C 0.638(3) 0.737(2) 0.3141(13) 0.24(6) Uiso 0.13 1 d PD . . H1S1 H 0.6575 0.7191 0.3062 0.285 Uiso 0.13 1 calc PR . . H1S2 H 0.6257 0.7474 0.2915 0.285 Uiso 0.13 1 calc PR . . C2S C 0.6083(14) 0.7177(15) 0.3409(11) 0.084(15) Uiso 0.13 1 d PD . . H2S1 H 0.5830 0.7281 0.3365 0.101 Uiso 0.13 1 calc PR . . H2S2 H 0.6076 0.6904 0.3363 0.101 Uiso 0.13 1 calc PR . . C3S C 0.6218(12) 0.7262(11) 0.3825(10) 0.060(12) Uiso 0.13 1 d PD . . H3S1 H 0.6355 0.7045 0.3928 0.073 Uiso 0.13 1 calc PR . . H3S2 H 0.5999 0.7313 0.3988 0.073 Uiso 0.13 1 calc PR . . C4S C 0.6484(14) 0.7620(11) 0.3807(9) 0.073(13) Uiso 0.13 1 d PD . . H4S1 H 0.6361 0.7837 0.3926 0.087 Uiso 0.13 1 calc PR . . H4S2 H 0.6721 0.7569 0.3942 0.087 Uiso 0.13 1 calc PR . . O1W O 0.723(4) 0.777(4) 0.275(6) 0.11(3) Uiso 0.13 3 d SPD C -1 C1W C 0.729(5) 0.733(4) 0.281(5) 0.06(5) Uiso 0.04 1 d PD C -1 H1W1 H 0.7317 0.7266 0.3075 0.068 Uiso 0.04 1 calc PR C -1 H1W2 H 0.7069 0.7188 0.2708 0.068 Uiso 0.04 1 calc PR C -1 C2W C 0.766(3) 0.720(3) 0.258(6) 0.070 Uiso 0.04 1 d PD C -1 H2W1 H 0.7824 0.7051 0.2744 0.084 Uiso 0.04 1 calc PR C -1 H2W2 H 0.7593 0.7056 0.2358 0.084 Uiso 0.04 1 calc PR C -1 C3W C 0.787(4) 0.758(4) 0.246(7) 0.070 Uiso 0.04 1 d PD C -1 H3W1 H 0.7941 0.7571 0.2190 0.084 Uiso 0.04 1 calc PR C -1 H3W2 H 0.8107 0.7612 0.2606 0.084 Uiso 0.04 1 calc PR C -1 C4W C 0.760(6) 0.793(3) 0.254(5) 0.09(7) Uiso 0.04 1 d PD C -1 H4W1 H 0.7722 0.8119 0.2692 0.105 Uiso 0.04 1 calc PR C -1 H4W2 H 0.7521 0.8045 0.2296 0.105 Uiso 0.04 1 calc PR C -1 C1X C 0.7221(15) 0.7609(14) 0.5067(15) 0.073(12) Uiso 0.13 1 d P . . O1X O 0.719(2) 0.7480(18) 0.4747(19) 0.081(17) Uiso 0.04 1 d P . . C2X C 0.719(2) 0.7480(18) 0.4747(19) 0.081(17) Uiso 0.04 1 d P . . GA1' Ga 0.4302(2) 0.4302(2) 0.5698(2) 0.058(3) Uiso 0.08 3 d SP . 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 I1 0.0485(6) 0.0485(6) 0.0485(6) 0.000 0.000 0.000 Ga1 0.0557(4) 0.0557(4) 0.0557(4) 0.0043(3) 0.0043(3) -0.0043(3) P1 0.0612(9) 0.0580(9) 0.0753(11) -0.0030(8) 0.0017(8) -0.0066(7) C11 0.077(4) 0.060(4) 0.085(5) -0.004(4) 0.007(4) -0.010(3) C12 0.085(5) 0.078(5) 0.117(6) 0.000(5) 0.013(4) -0.003(4) C13 0.080(5) 0.064(5) 0.197(12) -0.016(6) 0.002(7) -0.028(4) C14 0.107(8) 0.116(9) 0.202(14) -0.044(9) -0.040(9) -0.025(6) C15 0.205(13) 0.134(9) 0.177(12) -0.017(9) -0.097(10) -0.062(9) C16 0.170(9) 0.119(7) 0.126(8) 0.014(6) -0.060(8) -0.053(7) Li1 0.070(5) 0.070(5) 0.070(5) 0.010(6) 0.010(6) 0.010(6) Li2 0.051(5) 0.062(5) 0.105(7) 0.007(7) -0.002(6) 0.004(4) C10 0.075(3) 0.075(3) 0.075(3) 0.005(4) 0.005(4) -0.005(4) O1 0.053(2) 0.091(3) 0.101(3) 0.010(3) -0.002(3) -0.011(2) C1T 0.077(5) 0.155(8) 0.111(6) 0.038(6) 0.001(5) 0.007(6) C2T 0.077(5) 0.113(6) 0.173(9) -0.001(7) -0.001(7) -0.022(5) C3T 0.072(6) 0.216(12) 0.135(8) -0.002(9) -0.030(5) -0.013(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 I1 Li1 2.50(2) . ? I1 Li1 2.50(2) 3_656 ? I1 Li1 2.50(2) 4_566 ? I1 Li1 2.50(2) 2_665 ? Ga1 C10 2.004(11) . ? Ga1 P1 2.4453(18) . ? Ga1 P1 2.4453(18) 11_566 ? Ga1 P1 2.4453(18) 8_656 ? Ga1 Li2 3.079(12) . ? Ga1 Li2 3.079(12) 8_656 ? Ga1 Li2 3.079(12) 11_566 ? P1 C11 1.835(7) . ? P1 Li1 2.526(5) . ? P1 Li2 2.616(9) . ? P1 Li2 2.677(13) 5 ? P1 Li2 2.554(14) 8_656 ? C11 C16 1.408(12) . ? C11 C12 1.344(10) . ? C12 C13 1.449(12) . ? C13 C14 1.300(17) . ? C14 C15 1.339(17) . ? C15 C16 1.346(14) . ? Li1 P1 2.526(5) 9 ? Li1 P1 2.526(5) 5 ? Li1 Li2 2.851(12) 5 ? Li1 Li2 2.851(12) . ? Li1 Li2 2.851(12) 9 ? Li2 O1 1.953(10) . ? Li2 P1 2.677(13) 9 ? Li2 P1 2.554(14) 11_566 ? Li2 Li2 2.755(18) 4_566 ? O1 C4T' 1.375(17) . ? O1 C1T 1.369(9) . ? O1 C4T 1.536(18) . ? C1T C2T 1.514(14) . ? C2T C3T 1.450(14) . ? C3T C4T 1.38(2) . ? C3T C4T' 1.67(2) . ? Li3Y O1S 2.06(3) 82_656 ? Li3Y O1S 2.06(3) . ? Li3Y O1S 2.06(3) 31_664 ? O1S C1S 1.56(3) . ? O1S C4S 1.56(3) . ? C1S C2S 1.56(3) . ? C2S C3S 1.56(3) . ? C3S C4S 1.56(3) . ? O1W C4W 1.58(5) . ? O1W C1W 1.58(5) . ? C1W C2W 1.58(5) . ? C2W C3W 1.58(5) . ? C3W C4W 1.58(5) . ? C1X O1X 1.21(8) . ? C1X C2X 1.31(8) 63_465 ? C1X O1X 1.31(8) 63_465 ? C1X C1X 1.56(8) 63_465 ? C1X C1X 1.56(8) 40_645 ? O1X C1X 1.31(8) 40_645 ? 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 Li1 I1 Li1 109.471(2) . 3_656 ? Li1 I1 Li1 109.471(5) . 4_566 ? Li1 I1 Li1 109.471(1) 3_656 4_566 ? Li1 I1 Li1 109.5 . 2_665 ? Li1 I1 Li1 109.471(1) 3_656 2_665 ? Li1 I1 Li1 109.471(1) 4_566 2_665 ? Li1 I1 Li2 110.97(15) 3_656 . ? Li1 I1 Li2 69.60(17) 4_566 . ? Li1 I1 Li2 137.01(18) 2_665 . ? Li1 I1 Ga1 70.5 . . ? Li1 I1 Ga1 70.5 3_656 . ? Li1 I1 Ga1 70.5 4_566 . ? Li1 I1 Ga1 180.0(2) 2_665 . ? C10 Ga1 P1 115.17(4) . . ? C10 Ga1 P1 115.17(4) . 11_566 ? P1 Ga1 P1 103.22(5) . 11_566 ? C10 Ga1 P1 115.17(4) . 8_656 ? P1 Ga1 P1 103.22(5) . 8_656 ? P1 Ga1 P1 103.22(5) 11_566 8_656 ? C10 Ga1 Li2 113.09(18) . . ? P1 Ga1 Li2 131.74(19) 8_656 . ? C10 Ga1 Li2 113.09(18) . 8_656 ? P1 Ga1 Li2 131.74(19) 11_566 8_656 ? Li2 Ga1 Li2 105.6(2) . 8_656 ? C10 Ga1 Li2 113.09(18) . 11_566 ? P1 Ga1 Li2 131.74(19) . 11_566 ? Li2 Ga1 Li2 105.6(2) . 11_566 ? Li2 Ga1 Li2 105.6(2) 8_656 11_566 ? C10 Ga1 I1 180.00(16) . . ? P1 Ga1 I1 64.83(4) . . ? P1 Ga1 I1 64.83(4) 11_566 . ? P1 Ga1 I1 64.83(4) 8_656 . ? Li2 Ga1 I1 66.91(18) . . ? Li2 Ga1 I1 66.91(18) 8_656 . ? Li2 Ga1 I1 66.91(18) 11_566 . ? C11 P1 Ga1 109.7(2) . . ? C11 P1 Li1 124.2(5) . . ? Ga1 P1 Li1 113.0(4) . . ? C11 P1 Li2 91.8(3) . . ? Ga1 P1 Li2 74.9(3) . . ? Li1 P1 Li2 67.3(3) . . ? C11 P1 Li2 103.5(3) . 5 ? Ga1 P1 Li2 136.6(3) . 5 ? Li1 P1 Li2 66.4(2) . 5 ? Li2 P1 Li2 131.9(4) . 5 ? C11 P1 Li2 118.9(3) . 8_656 ? Ga1 P1 Li2 76.0(2) . 8_656 ? Li1 P1 Li2 105.1(4) . 8_656 ? Li2 P1 Li2 143.3(4) . 8_656 ? Li2 P1 Li2 63.5(3) 5 8_656 ? C11 P1 P1 112.6(2) . 5 ? Ga1 P1 P1 137.05(4) . 5 ? Li2 P1 P1 96.5(3) . 5 ? Li2 P1 P1 89.9(2) 8_656 5 ? C11 P1 P1 164.2(2) . 2_665 ? Ga1 P1 P1 78.17(4) . 2_665 ? Li2 P1 P1 76.7(2) . 2_665 ? Li2 P1 P1 77.3(2) 5 2_665 ? Li2 P1 P1 75.9(2) 8_656 2_665 ? C16 C11 C12 115.2(7) . . ? C16 C11 P1 118.4(6) . . ? C12 C11 P1 126.4(6) . . ? C13 C12 C11 120.5(9) . . ? C14 C13 C12 122.0(11) . . ? C13 C14 C15 117.6(11) . . ? C16 C15 C14 123.2(12) . . ? C11 C16 C15 121.6(11) . . ? I1 Li1 P1 101.8(5) . 9 ? I1 Li1 P1 101.8(5) . . ? P1 Li1 P1 115.9(3) 9 . ? I1 Li1 P1 101.8(5) . 5 ? P1 Li1 P1 115.9(3) 9 5 ? P1 Li1 P1 115.9(3) . 5 ? I1 Li1 Li2 101.8(5) . 5 ? P1 Li1 Li2 156.4(10) 9 5 ? P1 Li1 Li2 59.4(2) . 5 ? P1 Li1 Li2 57.9(2) 5 5 ? I1 Li1 Li2 101.8(5) . . ? P1 Li1 Li2 59.4(2) 9 . ? P1 Li1 Li2 57.9(2) . . ? P1 Li1 Li2 156.4(10) 5 . ? Li2 Li1 Li2 115.9(3) 5 . ? I1 Li1 Li2 101.8(5) . 9 ? P1 Li1 Li2 57.9(2) 9 9 ? P1 Li1 Li2 156.4(10) . 9 ? P1 Li1 Li2 59.4(2) 5 9 ? Li2 Li1 Li2 115.9(3) 5 9 ? Li2 Li1 Li2 115.9(3) . 9 ? O1 Li2 P1 116.5(4) . . ? O1 Li2 P1 111.5(6) . 9 ? P1 Li2 P1 108.0(4) . 9 ? O1 Li2 P1 115.2(6) . 11_566 ? P1 Li2 P1 95.7(4) . 11_566 ? P1 Li2 P1 108.7(3) 9 11_566 ? O1 Li2 Li1 143.0(8) . . ? P1 Li2 Li1 101.8(5) 11_566 . ? O1 Li2 Li2 107.4(3) . 4_566 ? P1 Li2 Li2 136.0(2) . 4_566 ? P1 Li2 Li2 60.4(5) 11_566 4_566 ? Li1 Li2 Li2 92.0(4) . 4_566 ? O1 Li2 Ga1 113.0(5) . . ? P1 Li2 Ga1 135.5(3) 9 . ? Li1 Li2 Ga1 88.6(3) . . ? Li2 Li2 Ga1 109.2(7) 4_566 . ? O1 Li2 I1 176.9(6) . . ? P1 Li2 I1 65.76(18) . . ? P1 Li2 I1 65.43(19) 9 . ? P1 Li2 I1 66.1(2) 11_566 . ? Li2 Li2 I1 70.63(13) 4_566 . ? Ga1 Li2 I1 70.09(18) . . ? C4T' O1 C1T 103.8(8) . . ? C1T O1 C4T 104.9(8) . . ? C4T' O1 Li2 127.9(8) . . ? C1T O1 Li2 123.4(6) . . ? C4T O1 Li2 128.3(9) . . ? O1 C1T C2T 108.1(7) . . ? C3T C2T C1T 102.5(7) . . ? C4T C3T C2T 104.7(10) . . ? C2T C3T C4T' 103.0(8) . . ? C3T C4T O1 106.4(13) . . ? O1 C4T' C3T 99.7(11) . . ? O1S Li3Y O1S 115.8(16) 82_656 . ? O1S Li3Y O1S 115.8(17) 82_656 31_664 ? O1S Li3Y O1S 115.8(17) . 31_664 ? C1S O1S C4S 107.2(9) . . ? C1S O1S Li3Y 119(3) . . ? C4S O1S Li3Y 133(2) . . ? O1S C1S C2S 106.5(13) . . ? C3S C2S C1S 106.0(12) . . ? C2S C3S C4S 107.3(8) . . ? O1S C4S C3S 107.3(7) . . ? C4W O1W C1W 107.9(5) . . ? C2W C1W O1W 107.7(8) . . ? C3W C2W C1W 107.6(10) . . ? C2W C3W C4W 107.7(8) . . ? O1W C4W C3W 107.9(5) . . ? O1X C1X C2X 135(6) . 63_465 ? O1X C1X O1X 135(6) . 63_465 ? C2X C1X C1X 110(4) 63_465 40_645 ? O1X C1X C1X 110(4) 63_465 40_645 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 20.96 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.940 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.057 # Attachment '- 3Br.cif' data_DW0612 _database_code_depnum_ccdc_archive 'CCDC 797474' #TrackingRef '- 3Br.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H188 Br In4 Li17 O14.50 P12' _chemical_formula_weight 3059.65 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' Li Li -0.0003 0.0001 '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' P P 0.1023 0.0942 '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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 35.110(4) _cell_length_b 35.110(4) _cell_length_c 35.110(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 43282(9) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 52115 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.10 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12560 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 13481 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 20.99 _reflns_number_total 1854 _reflns_number_gt 1345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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. Two isolated maxima density of electron density were assigned as partial C- and O-atoms of a half THF solvate per cluster anion, which was highly disordered across a site of -4 symmetry. High displacement parameters associated with the ligand atoms indicated considerable unresolved disorder resulting in poor diffraction at high angle; data in the limited theta range < 21o were used in the full matrix refinement as a chiral twin (52:48%). There was additionally a small disorder of the cluster anion with its enantiomer (ca. 18%) and only the contribition from the metal atom (In1') of the minor component was allowed for in the refinement. H-atoms of the highly disordered solvate molecule were not included. ` ; _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^)+(0.1226P)^2^+232.3695P] 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 1854 _refine_ls_number_parameters 153 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.2077 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.093 _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 Br1 Br 0.5000 0.5000 0.5000 0.0564(8) Uani 1 12 d S . . In1 In 0.57203(2) 0.57203(2) 0.42797(2) 0.0710(6) Uani 0.82 3 d SP A 1 P1 P 0.56067(8) 0.59567(8) 0.49752(12) 0.0868(9) Uani 1 1 d . . . C11 C 0.5962(3) 0.6334(3) 0.5093(3) 0.108(5) Uani 1 1 d G A . C12 C 0.6124(4) 0.6581(3) 0.4830(4) 0.184(12) Uani 1 1 d G . . H12 H 0.6072 0.6553 0.4572 0.221 Uiso 1 1 calc R A . C13 C 0.6363(3) 0.6872(3) 0.4953(6) 0.176(10) Uani 1 1 d G A . H13 H 0.6471 0.7038 0.4778 0.211 Uiso 1 1 calc R . . C14 C 0.6440(4) 0.6914(4) 0.5339(6) 0.199(12) Uani 1 1 d G . . H14 H 0.6600 0.7109 0.5422 0.238 Uiso 1 1 calc R A . C15 C 0.6279(5) 0.6667(5) 0.5602(4) 0.237(15) Uani 1 1 d G A . H15 H 0.6330 0.6695 0.5860 0.285 Uiso 1 1 calc R . . C16 C 0.6039(4) 0.6376(4) 0.5479(3) 0.198(10) Uani 1 1 d G . . H16 H 0.5931 0.6210 0.5655 0.237 Uiso 1 1 calc R A . Li1 Li 0.5411(6) 0.5411(6) 0.5411(6) 0.082(8) Uani 1 3 d S . . Li2 Li 0.6110(3) 0.5375(4) 0.4996(8) 0.080(5) Uani 1 1 d . . . C1M C 0.6095(4) 0.6095(4) 0.3905(4) 0.112(7) Uani 1 3 d S . . H1M1 H 0.6343 0.6119 0.4018 0.168 Uiso 0.33 1 calc PR A 1 H1M2 H 0.5982 0.6343 0.3881 0.168 Uiso 0.33 1 calc PR A 1 H1M3 H 0.6119 0.5982 0.3657 0.168 Uiso 0.33 1 calc PR A 1 O1 O 0.66465(19) 0.5582(2) 0.5012(3) 0.096(2) Uani 0.51(2) 1 d PD B 1 C1S C 0.6825(4) 0.5823(5) 0.4734(5) 0.168(9) Uani 0.51(2) 1 d PD B 1 H1S1 H 0.6934 0.5667 0.4534 0.202 Uiso 0.51(2) 1 calc PR B 1 H1S2 H 0.6635 0.5988 0.4620 0.202 Uiso 0.51(2) 1 calc PR B 1 C2S C 0.7119(10) 0.6051(10) 0.4904(10) 0.131(7) Uiso 0.51(2) 1 d PD B 1 H2S1 H 0.7341 0.6066 0.4740 0.157 Uiso 0.51(2) 1 calc PR B 1 H2S2 H 0.7028 0.6306 0.4959 0.157 Uiso 0.51(2) 1 calc PR B 1 C3S C 0.7213(8) 0.5829(11) 0.5281(9) 0.147(10) Uiso 0.51(2) 1 d PD B 1 H3S1 H 0.7269 0.6004 0.5488 0.177 Uiso 0.51(2) 1 calc PR B 1 H3S2 H 0.7428 0.5659 0.5246 0.177 Uiso 0.51(2) 1 calc PR B 1 C4S C 0.6871(8) 0.5620(9) 0.5354(6) 0.122(7) Uiso 0.51(2) 1 d PD B 1 H4S1 H 0.6936 0.5370 0.5450 0.147 Uiso 0.51(2) 1 calc PR B 1 H4S2 H 0.6723 0.5751 0.5547 0.147 Uiso 0.51(2) 1 calc PR B 1 O1' O 0.66465(19) 0.5582(2) 0.5012(3) 0.096(2) Uani 0.49(2) 1 d PD B 2 C1S' C 0.6825(4) 0.5823(5) 0.4734(5) 0.168(9) Uani 0.49(2) 1 d PD B 2 H1S3 H 0.6682 0.6027 0.4616 0.202 Uiso 0.49(2) 1 calc PR B 2 H1S4 H 0.7100 0.5822 0.4706 0.202 Uiso 0.49(2) 1 calc PR B 2 C2S' C 0.7173(8) 0.5953(9) 0.4914(10) 0.131(7) Uiso 0.49(2) 1 d PD B 2 H2S3 H 0.7119 0.6189 0.5047 0.157 Uiso 0.49(2) 1 calc PR B 2 H2S4 H 0.7378 0.5997 0.4735 0.157 Uiso 0.49(2) 1 calc PR B 2 C3S' C 0.7273(6) 0.5657(11) 0.5180(9) 0.147(10) Uiso 0.49(2) 1 d PD B 2 H3S3 H 0.7521 0.5552 0.5120 0.177 Uiso 0.49(2) 1 calc PR B 2 H3S4 H 0.7278 0.5755 0.5438 0.177 Uiso 0.49(2) 1 calc PR B 2 C4S' C 0.6975(5) 0.5371(6) 0.5135(9) 0.122(7) Uiso 0.49(2) 1 d PD B 2 H4S3 H 0.7118 0.5139 0.5086 0.147 Uiso 0.49(2) 1 calc PR B 2 H4S4 H 0.6877 0.5342 0.5391 0.147 Uiso 0.49(2) 1 calc PR B 2 Li3Y Li 0.6930(12) 0.8070(12) 0.3070(12) 0.10(9) Uiso 0.13 3 d SPD . . O1T O 0.6566(19) 0.775(2) 0.3394(19) 0.137(17) Uiso 0.13 1 d PD C . C1T C 0.644(3) 0.738(3) 0.320(2) 0.137(17) Uiso 0.13 1 d PD . . H1T1 H 0.6650 0.7202 0.3188 0.164 Uiso 0.13 1 calc PR C . H1T2 H 0.6356 0.7435 0.2941 0.164 Uiso 0.13 1 calc PR . . C2T C 0.612(3) 0.722(3) 0.343(3) 0.137(17) Uiso 0.13 1 d PD C . H2T1 H 0.5873 0.7277 0.3314 0.164 Uiso 0.13 1 calc PR . . H2T2 H 0.6141 0.6948 0.3459 0.164 Uiso 0.13 1 calc PR . . C3T C 0.614(3) 0.741(3) 0.382(3) 0.137(17) Uiso 0.13 1 d PD . . H3T1 H 0.6199 0.7221 0.4016 0.164 Uiso 0.13 1 calc PR C . H3T2 H 0.5891 0.7521 0.3887 0.164 Uiso 0.13 1 calc PR . . C4T C 0.644(3) 0.771(3) 0.381(2) 0.137(17) Uiso 0.13 1 d PD C . H4T1 H 0.6653 0.7646 0.3968 0.164 Uiso 0.13 1 calc PR . . H4T2 H 0.6337 0.7956 0.3896 0.164 Uiso 0.13 1 calc PR . . O1W O 0.743(2) 0.7765(17) 0.302(2) 0.029(17) Uiso 0.04 1 d PD C -1 C1W C 0.741(3) 0.7344(18) 0.311(3) 0.029(17) Uiso 0.04 1 d PD C -1 H1W1 H 0.7171 0.7235 0.3025 0.034 Uiso 0.04 1 calc PR C -1 H1W2 H 0.7428 0.7302 0.3386 0.034 Uiso 0.04 1 calc PR C -1 C2W C 0.774(3) 0.716(2) 0.291(3) 0.029(17) Uiso 0.04 1 d PD C -1 H2W1 H 0.7939 0.7104 0.3091 0.034 Uiso 0.04 1 calc PR C -1 H2W2 H 0.7659 0.6932 0.2786 0.034 Uiso 0.04 1 calc PR C -1 C3W C 0.788(3) 0.744(3) 0.262(3) 0.029(17) Uiso 0.04 1 d PD C -1 H3W1 H 0.8147 0.7500 0.2671 0.034 Uiso 0.04 1 calc PR C -1 H3W2 H 0.7858 0.7337 0.2370 0.034 Uiso 0.04 1 calc PR C -1 C4W C 0.765(2) 0.780(2) 0.266(3) 0.029(17) Uiso 0.04 1 d PD C -1 H4W1 H 0.7810 0.8020 0.2662 0.034 Uiso 0.04 1 calc PR C -1 H4W2 H 0.7475 0.7818 0.2442 0.034 Uiso 0.04 1 calc PR C -1 C1X C 0.7221 0.7609 0.5067 0.07(2) Uiso 0.13 1 d P . . O1X O 0.720(3) 0.733(3) 0.467(4) 0.09(3) Uiso 0.04 1 d P . . C2X C 0.720(3) 0.733(3) 0.467(4) 0.09(3) Uiso 0.04 1 d P . . In1' In 0.42809(12) 0.42809(12) 0.57191(12) 0.0781(18) Uiso 0.18 3 d SP . 2 Li3 Li 0.7500 0.5000 0.5000 0.200 Uiso 0.17 4 d SP . . 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 Br1 0.0564(8) 0.0564(8) 0.0564(8) 0.000 0.000 0.000 In1 0.0710(6) 0.0710(6) 0.0710(6) 0.0064(4) 0.0064(4) -0.0064(4) P1 0.0721(17) 0.0765(18) 0.112(2) -0.011(2) -0.001(2) -0.0060(14) C11 0.097(9) 0.084(8) 0.144(14) 0.015(9) 0.017(10) -0.013(7) C12 0.108(12) 0.119(13) 0.33(4) 0.044(19) -0.025(16) -0.019(11) C13 0.124(13) 0.091(11) 0.31(3) -0.050(17) 0.00(2) -0.044(10) C14 0.132(17) 0.19(2) 0.27(3) -0.06(2) -0.04(2) -0.054(16) C15 0.32(4) 0.24(3) 0.156(19) -0.047(19) -0.05(2) -0.14(3) C16 0.18(2) 0.22(2) 0.19(2) -0.066(18) -0.112(17) -0.039(18) Li1 0.082(8) 0.082(8) 0.082(8) -0.003(9) -0.003(9) -0.003(9) Li2 0.016(6) 0.080(10) 0.143(15) -0.041(14) 0.003(10) 0.002(6) C1M 0.112(7) 0.112(7) 0.112(7) -0.003(9) -0.003(9) 0.003(9) O1 0.060(4) 0.112(5) 0.118(6) 0.003(7) 0.003(5) -0.018(4) C1S 0.059(9) 0.23(2) 0.22(2) 0.040(18) -0.003(11) -0.032(12) O1' 0.060(4) 0.112(5) 0.118(6) 0.003(7) 0.003(5) -0.018(4) C1S' 0.059(9) 0.23(2) 0.22(2) 0.040(18) -0.003(11) -0.032(12) _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 Br1 Li1 2.50(3) . ? Br1 Li1 2.50(3) 4_566 ? Br1 Li1 2.50(3) 3_656 ? Br1 Li1 2.50(3) 2_665 ? In1 C1M 2.28(3) . ? In1 P1 2.610(4) 8_656 ? In1 P1 2.610(4) . ? In1 P1 2.610(4) 11_566 ? In1 Li2 3.11(3) 11_566 ? In1 Li2 3.11(3) . ? In1 Li2 3.11(3) 8_656 ? P1 C11 1.865(8) . ? P1 Li2 2.51(2) 8_656 ? P1 Li1 2.546(9) . ? P1 Li2 2.700(14) . ? P1 Li2 2.62(3) 5 ? P1 In1' 2.770(5) 2_665 ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 In1' 2.701(14) 2_665 ? Li1 In1' 1.87(3) 2_665 ? Li1 P1 2.546(9) 9 ? Li1 P1 2.546(9) 5 ? Li1 Li2 2.855(18) . ? Li1 Li2 2.855(18) 9 ? Li1 Li2 2.855(18) 5 ? Li2 O1 2.021(13) . ? Li2 P1 2.51(2) 11_566 ? Li2 P1 2.62(3) 9 ? Li2 Li2 2.63(3) 4_566 ? Li2 In1' 3.13(2) 2_665 ? O1 C1S 1.434(10) . ? O1 C4S 1.441(13) . ? C1S C2S 1.437(13) . ? C2S C3S 1.57(5) . ? C3S C4S 1.43(2) . ? C2S' C3S' 1.439(13) . ? C3S' C4S' 1.46(3) . ? C3S' Li3 2.52(4) . ? C4S' Li3 2.30(2) . ? Li3Y O1W 2.05(2) . ? Li3Y O1T 2.05(2) 82_656 ? Li3Y O1T 2.05(2) . ? Li3Y O1T 2.05(2) 31_664 ? Li3Y C2W 1.53(12) 8_656 ? Li3Y C2W 1.53(12) 33_554 ? Li3Y C2W 1.53(12) 74_665 ? O1T C1T 1.52(6) . ? O1T C4T 1.52(6) . ? C1T C2T 1.52(6) . ? C2T C3T 1.51(6) . ? C3T C4T 1.51(6) . ? O1W C4W 1.51(2) . ? O1W C1W 1.51(2) . ? C1W C2W 1.499(19) . ? C2W C3W 1.49(2) . ? C3W C4W 1.49(2) . ? C1X O1X 1.70(12) . ? C1X C2X 1.20(12) 63_465 ? C1X O1X 1.20(12) 63_465 ? C1X C1X 1.5599(2) 63_465 ? C1X C1X 1.55991(19) 40_645 ? O1X C1X 1.20(12) 40_645 ? Li3 C4S' 2.30(2) 42_645 ? Li3 C4S' 2.30(2) 43_654 ? Li3 C4S' 2.30(2) 4_566 ? Li3 C3S' 2.52(4) 42_645 ? Li3 C3S' 2.52(4) 43_654 ? Li3 C3S' 2.52(4) 4_566 ? 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 Li1 Br1 Li1 109.471(7) . 4_566 ? Li1 Br1 Li1 109.471(3) . 3_656 ? Li1 Br1 Li1 109.471(1) 4_566 3_656 ? Li1 Br1 Li1 109.471(1) . 2_665 ? Li1 Br1 Li1 109.471(1) 4_566 2_665 ? Li1 Br1 Li1 109.471(1) 3_656 2_665 ? C1M In1 P1 116.41(7) . 8_656 ? C1M In1 P1 116.41(7) . . ? P1 In1 P1 101.72(9) 8_656 . ? C1M In1 P1 116.41(7) . 11_566 ? P1 In1 P1 101.72(9) 8_656 11_566 ? P1 In1 P1 101.72(9) . 11_566 ? C1M In1 Li2 116.0(3) . 11_566 ? P1 In1 Li2 51.1(3) 8_656 11_566 ? P1 In1 Li2 127.5(3) . 11_566 ? P1 In1 Li2 55.5(3) 11_566 11_566 ? C1M In1 Li2 116.0(3) . . ? P1 In1 Li2 127.5(3) 8_656 . ? P1 In1 Li2 55.5(3) . . ? P1 In1 Li2 51.1(3) 11_566 . ? Li2 In1 Li2 102.2(3) 11_566 . ? C1M In1 Li2 116.0(3) . 8_656 ? P1 In1 Li2 55.5(3) 8_656 8_656 ? P1 In1 Li2 51.1(3) . 8_656 ? P1 In1 Li2 127.5(3) 11_566 8_656 ? Li2 In1 Li2 102.2(3) 11_566 8_656 ? Li2 In1 Li2 102.2(3) . 8_656 ? C11 P1 Li2 121.5(5) . 8_656 ? C11 P1 In1 109.3(4) . . ? Li2 P1 In1 74.8(5) 8_656 . ? C11 P1 Li1 125.5(9) . . ? Li2 P1 Li1 103.2(7) 8_656 . ? In1 P1 Li1 111.4(6) . . ? C11 P1 Li2 95.3(5) . . ? Li2 P1 Li2 136.6(6) 8_656 . ? In1 P1 Li2 71.6(6) . . ? Li1 P1 Li2 65.9(5) . . ? C11 P1 Li2 106.5(5) . 5 ? Li2 P1 Li2 61.8(6) 8_656 5 ? In1 P1 Li2 133.8(4) . 5 ? Li1 P1 Li2 67.1(3) . 5 ? Li2 P1 Li2 132.5(6) . 5 ? C12 C11 C16 120.0 . . ? C12 C11 P1 124.8(7) . . ? C16 C11 P1 115.0(7) . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? Br1 Li1 P1 104.0(7) . 9 ? Br1 Li1 P1 104.0(7) . . ? P1 Li1 P1 114.3(6) 9 . ? Br1 Li1 P1 104.0(7) . 5 ? P1 Li1 P1 114.3(6) 9 5 ? P1 Li1 P1 114.3(6) . 5 ? Br1 Li1 Li2 100.1(8) . . ? P1 Li1 Li2 57.7(5) 9 . ? P1 Li1 Li2 59.7(4) . . ? P1 Li1 Li2 155.9(15) 5 . ? Br1 Li1 Li2 100.1(8) . 9 ? P1 Li1 Li2 59.7(4) 9 9 ? P1 Li1 Li2 155.9(15) . 9 ? P1 Li1 Li2 57.7(5) 5 9 ? Li2 Li1 Li2 117.0(5) . 9 ? Br1 Li1 Li2 100.1(8) . 5 ? P1 Li1 Li2 155.9(15) 9 5 ? P1 Li1 Li2 57.7(5) . 5 ? P1 Li1 Li2 59.7(4) 5 5 ? Li2 Li1 Li2 117.0(5) . 5 ? Li2 Li1 Li2 117.0(5) 9 5 ? O1' Li2 O1 137.4(10) 10_656 . ? O1' Li2 P1 36.1(3) 10_656 11_566 ? O1 Li2 P1 113.6(11) . 11_566 ? O1' Li2 P1 68.5(4) 10_656 . ? O1 Li2 P1 109.8(7) . . ? P1 Li2 P1 102.1(8) 11_566 . ? O1' Li2 P1 109.7(3) 10_656 9 ? O1 Li2 P1 111.1(11) . 9 ? P1 Li2 P1 112.6(6) 11_566 9 ? P1 Li2 P1 107.1(7) . 9 ? O1' Li2 Li2 81.7(8) 10_656 4_566 ? O1 Li2 Li2 111.1(5) . 4_566 ? P1 Li2 Li2 61.2(9) 11_566 4_566 ? P1 Li2 Li2 139.2(3) . 4_566 ? P1 Li2 Li2 57.0(10) 9 4_566 ? O1' Li2 Li1 75.5(7) 10_656 . ? O1 Li2 Li1 140.3(13) . . ? P1 Li2 Li1 105.6(8) 11_566 . ? P1 Li2 Li1 54.5(3) . . ? P1 Li2 Li1 55.2(5) 9 . ? Li2 Li2 Li1 92.2(9) 4_566 . ? O1' Li2 In1 36.0(2) 10_656 . ? O1 Li2 In1 107.1(10) . . ? P1 Li2 In1 54.1(5) 11_566 . ? P1 Li2 In1 52.8(4) . . ? P1 Li2 In1 141.4(4) 9 . ? Li2 Li2 In1 113.5(12) 4_566 . ? Li1 Li2 In1 91.1(5) . . ? C1S O1 C4S 105.8(8) . . ? C1S O1 Li2 126.8(11) . . ? C4S O1 Li2 124.7(13) . . ? C2S C1S O1 111.0(17) . . ? C3S C2S C1S 103.0(13) . . ? C2S C3S C4S 103.2(15) . . ? O1 C4S C3S 111.1(17) . . ? C1S' C2S' C3S' 105.5(11) 10_656 . ? C4S' C3S' C2S' 104.5(10) . . ? C4S' C3S' Li3 64.4(17) . . ? C2S' C3S' Li3 125(3) . . ? O1' C4S' C3S' 136.4(8) 10_656 . ? O1' C4S' Li3 118.1(9) 10_656 . ? C3S' C4S' Li3 80.8(17) . . ? O1W Li3Y O1T 83(3) . 82_656 ? O1W Li3Y O1T 107(3) . . ? O1T Li3Y O1T 108(3) 82_656 . ? O1W Li3Y O1T 139(4) . 31_664 ? O1T Li3Y O1T 108(3) 82_656 31_664 ? O1T Li3Y O1T 108(3) . 31_664 ? O1W Li3Y C2W 41(6) . 8_656 ? O1T Li3Y C2W 124(5) 82_656 8_656 ? O1T Li3Y C2W 96(4) . 8_656 ? O1T Li3Y C2W 112(6) 31_664 8_656 ? O1W Li3Y C2W 45(5) . 33_554 ? O1T Li3Y C2W 112(6) 82_656 33_554 ? O1T Li3Y C2W 124(5) . 33_554 ? O1T Li3Y C2W 96(4) 31_664 33_554 ? O1T Li3Y C2W 96(4) 82_656 74_665 ? O1T Li3Y C2W 112(6) . 74_665 ? O1T Li3Y C2W 124(5) 31_664 74_665 ? C1T O1T C4T 106.4(9) . . ? C1T O1T Li3Y 113(5) . . ? C4T O1T Li3Y 139(5) . . ? O1T C1T C2T 106.4(9) . . ? C3T C2T C1T 107.2(7) . . ? C2T C3T C4T 107.9(4) . . ? C3T C4T O1T 107.2(7) . . ? C4W O1W C1W 105.7(17) . . ? C4W O1W Li3Y 118(4) . . ? C1W O1W Li3Y 118(4) . . ? O1W C1W C2W 106.3(16) . . ? C3W C2W C1W 107.8(9) . . ? C4W C3W C2W 108.0(7) . . ? O1W C4W C3W 106.7(14) . . ? O1X C1X C2X 164(8) . 63_465 ? O1X C1X O1X 164(8) . 63_465 ? C2X C1X C1X 127(6) 63_465 40_645 ? O1X C1X C1X 127(6) 63_465 40_645 ? C4S' Li3 C4S' 129.7(8) 42_645 . ? C4S' Li3 C4S' 129.7(8) 43_654 . ? C4S' Li3 C4S' 129.7(8) 42_645 4_566 ? C4S' Li3 C4S' 129.7(8) 43_654 4_566 ? C4S' Li3 C4S' 73.9(13) . 4_566 ? C4S' Li3 C3S' 34.9(8) 42_645 42_645 ? C4S' Li3 C3S' 108.4(8) 43_654 42_645 ? C4S' Li3 C3S' 107.4(7) . 42_645 ? C4S' Li3 C3S' 101.9(9) 4_566 42_645 ? C4S' Li3 C3S' 108.4(8) 42_645 43_654 ? C4S' Li3 C3S' 34.9(8) 43_654 43_654 ? C4S' Li3 C3S' 101.9(9) . 43_654 ? C4S' Li3 C3S' 107.4(7) 4_566 43_654 ? C3S' Li3 C3S' 143.2(10) 42_645 43_654 ? C4S' Li3 C3S' 107.4(7) 42_645 4_566 ? C4S' Li3 C3S' 101.9(9) 43_654 4_566 ? C4S' Li3 C3S' 108.4(8) . 4_566 ? C3S' Li3 C3S' 95.7(3) 42_645 4_566 ? C3S' Li3 C3S' 95.7(3) 43_654 4_566 ? C4S' Li3 C3S' 101.9(9) 42_645 . ? C4S' Li3 C3S' 107.4(7) 43_654 . ? C4S' Li3 C3S' 108.4(8) 4_566 . ? C3S' Li3 C3S' 95.7(3) 42_645 . ? C3S' Li3 C3S' 95.7(3) 43_654 . ? C3S' Li3 C3S' 143.2(10) 4_566 . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 20.99 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.223 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.076 # Attachment '- 3i.cif' data_dw0748 _database_code_depnum_ccdc_archive 'CCDC 797475' #TrackingRef '- 3i.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C138.67 H193.33 I0.67 In4 Li16.67 O15.67 P12' _chemical_formula_weight 3142.12 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' Li Li -0.0003 0.0001 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M F-43c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y+1/2, x+1, z+1' '-y+1/2, -x+1, z+1' 'y+1/2, -x+1, -z+1' '-y+1/2, x+1, -z+1' 'x+1/2, z+1, y+1' '-x+1/2, z+1, -y+1' '-x+1/2, -z+1, y+1' 'x+1/2, -z+1, -y+1' 'z+1/2, y+1, x+1' 'z+1/2, -y+1, -x+1' '-z+1/2, y+1, -x+1' '-z+1/2, -y+1, x+1' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1, x+1/2, z+1' '-y+1, -x+1/2, z+1' 'y+1, -x+1/2, -z+1' '-y+1, x+1/2, -z+1' 'x+1, z+1/2, y+1' '-x+1, z+1/2, -y+1' '-x+1, -z+1/2, y+1' 'x+1, -z+1/2, -y+1' 'z+1, y+1/2, x+1' 'z+1, -y+1/2, -x+1' '-z+1, y+1/2, -x+1' '-z+1, -y+1/2, x+1' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1, x+1, z+1/2' '-y+1, -x+1, z+1/2' 'y+1, -x+1, -z+1/2' '-y+1, x+1, -z+1/2' 'x+1, z+1, y+1/2' '-x+1, z+1, -y+1/2' '-x+1, -z+1, y+1/2' 'x+1, -z+1, -y+1/2' 'z+1, y+1, x+1/2' 'z+1, -y+1, -x+1/2' '-z+1, y+1, -x+1/2' '-z+1, -y+1, x+1/2' _cell_length_a 35.312(4) _cell_length_b 35.312(4) _cell_length_c 35.312(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 44033(9) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6976 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 19.98 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 1.7 _exptl_crystal_size_mid 1.5 _exptl_crystal_size_min 1.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12896 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 7636 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 19.97 _reflns_number_total 1592 _reflns_number_gt 1175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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. Two isolated maxima density of electron density were assigned as partial C- and O-atoms of one THF solvate per cluster anion, which was highly disordered across a site of -4 symmetry. High displacement parameters associated with the ligand atoms indicated considerable unresolved disorder resulting in poor diffraction at high angle; data in the limited theta range < 20o were used in the full matrix refinement as a chiral twin (60:40%). There was additionally a small disorder of the cluster anion with its enantiomer (ca. 18%) and only the contribition from the metal atom (In1') of the minor component was allowed for in the refinement. H-atoms of the highly disordered solvate molecule were not included. The H-atoms of the disordered THF solvate and the fourth, disordered, THF ligand of the counter cation were not included. ; _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^)+(0.1370P)^2^+172.1689P] 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 1592 _refine_ls_number_parameters 156 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2116 _refine_ls_wR_factor_gt 0.1864 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.107 _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 I1 I 0.5000 0.5000 0.5000 0.0579(8) Uiso 0.67 12 d SP . . In1 In 0.57160(2) 0.57160(2) 0.42840(2) 0.0640(5) Uani 0.83 3 d SP A 1 C1 C 0.6082(4) 0.6082(4) 0.3918(4) 0.104(7) Uani 1 3 d S . . H1A H 0.6107 0.5968 0.3673 0.156 Uiso 0.33 1 calc PR A 1 H1B H 0.6327 0.6107 0.4032 0.156 Uiso 0.33 1 calc PR A 1 H1C H 0.5968 0.6327 0.3893 0.156 Uiso 0.33 1 calc PR A 1 Li1 Li 0.5417(5) 0.5417(5) 0.5417(5) 0.079(9) Uani 1 3 d S . . Li2 Li 0.6106(4) 0.5392(4) 0.5007(7) 0.070(4) Uani 1 1 d . . . P1 P 0.56044(8) 0.59522(8) 0.49811(11) 0.0792(8) Uani 1 1 d . . . C11 C 0.5948(2) 0.6322(2) 0.5097(3) 0.099(4) Uani 1 1 d GU . . C12 C 0.6056(4) 0.6353(3) 0.5475(3) 0.194(9) Uani 1 1 d GU . . H12 H 0.5964 0.6182 0.5652 0.233 Uiso 1 1 calc R . . C13 C 0.6302(4) 0.6639(4) 0.5586(3) 0.249(13) Uani 1 1 d GU A . H13 H 0.6374 0.6660 0.5839 0.298 Uiso 1 1 calc R . . C14 C 0.6440(3) 0.6895(3) 0.5321(4) 0.159(8) Uani 1 1 d GU A . H14 H 0.6604 0.7087 0.5395 0.190 Uiso 1 1 calc R . . C15 C 0.6332(3) 0.6865(3) 0.4943(4) 0.143(5) Uani 1 1 d GU A . H15 H 0.6424 0.7036 0.4766 0.171 Uiso 1 1 calc R . . C16 C 0.6086(3) 0.6578(3) 0.4832(3) 0.108(4) Uani 1 1 d GU A . H16 H 0.6013 0.6558 0.4579 0.129 Uiso 1 1 calc R . . O1 O 0.66366(16) 0.55823(19) 0.5017(3) 0.087(2) Uani 0.467(13) 1 d PD A 1 C1T C 0.6864(8) 0.5693(10) 0.5348(5) 0.119(7) Uiso 0.467(13) 1 d PD A 1 H1T1 H 0.6988 0.5475 0.5460 0.143 Uiso 0.467(13) 1 calc PR A 1 H1T2 H 0.6708 0.5816 0.5538 0.143 Uiso 0.467(13) 1 calc PR A 1 C2T C 0.7154(7) 0.5968(9) 0.5183(7) 0.117(7) Uiso 0.467(13) 1 d PD A 1 H2T1 H 0.7065 0.6227 0.5210 0.140 Uiso 0.467(13) 1 calc PR A 1 H2T2 H 0.7394 0.5944 0.5314 0.140 Uiso 0.467(13) 1 calc PR A 1 C3T C 0.7196(6) 0.5880(10) 0.4810(8) 0.129 Uiso 0.467(13) 1 d PD A 1 H3T1 H 0.7263 0.6102 0.4664 0.140 Uiso 0.467(13) 1 calc PR A 1 H3T2 H 0.7391 0.5689 0.4776 0.140 Uiso 0.467(13) 1 calc PR A 1 C4T C 0.6795(9) 0.5721(10) 0.4686(6) 0.125(8) Uiso 0.467(13) 1 d PD A 1 H4T1 H 0.6822 0.5522 0.4500 0.150 Uiso 0.467(13) 1 calc PR A 1 H4T2 H 0.6640 0.5921 0.4580 0.150 Uiso 0.467(13) 1 calc PR A 1 O1' O 0.66366(16) 0.55823(19) 0.5017(3) 0.087(2) Uani 0.533(13) 1 d PD A 2 C1T' C 0.6970(7) 0.5406(6) 0.5193(8) 0.119(7) Uiso 0.533(13) 1 d PD A 2 H1T3 H 0.7050 0.5187 0.5047 0.143 Uiso 0.533(13) 1 calc PR A 2 H1T4 H 0.6911 0.5325 0.5448 0.143 Uiso 0.533(13) 1 calc PR A 2 C2T' C 0.7263(5) 0.5689(7) 0.5196(7) 0.117(7) Uiso 0.533(13) 1 d PD A 2 H2T3 H 0.7489 0.5590 0.5076 0.140 Uiso 0.533(13) 1 calc PR A 2 H2T4 H 0.7325 0.5755 0.5456 0.140 Uiso 0.533(13) 1 calc PR A 2 C3T' C 0.7135(6) 0.6020(6) 0.4998(12) 0.129 Uiso 0.533(13) 1 d PD A 2 H3T3 H 0.7323 0.6103 0.4815 0.140 Uiso 0.533(13) 1 calc PR A 2 H3T4 H 0.7084 0.6225 0.5172 0.140 Uiso 0.533(13) 1 calc PR A 2 C4T' C 0.6771(7) 0.5893(8) 0.4797(8) 0.125(8) Uiso 0.533(13) 1 d PD A 2 H4T3 H 0.6586 0.6096 0.4792 0.150 Uiso 0.533(13) 1 calc PR A 2 H4T4 H 0.6823 0.5815 0.4539 0.150 Uiso 0.533(13) 1 calc PR A 2 Li3Y Li 0.6942 0.8058 0.6942 0.12(9) Uiso 0.17 3 d SP . . O1S O 0.6581(7) 0.8351(7) 0.7291(14) 0.20(4) Uiso 0.08 1 d PD B 1 C1S C 0.6812(7) 0.8654(8) 0.7555(11) 0.10(2) Uiso 0.08 1 d PD B 1 H1S1 H 0.6970 0.8812 0.7394 0.119 Uiso 0.08 1 calc PR B 1 H1S2 H 0.6977 0.8517 0.7726 0.119 Uiso 0.08 1 calc PR B 1 C2S C 0.6528(10) 0.8926(16) 0.7802(15) 0.05(2) Uiso 0.08 1 d PD B 1 H2S1 H 0.6661 0.9156 0.7871 0.056 Uiso 0.08 1 calc PR B 1 H2S2 H 0.6460 0.8796 0.8034 0.056 Uiso 0.08 1 calc PR B 1 C3S C 0.6141(14) 0.9037(18) 0.7571(17) 0.04(2) Uiso 0.08 1 d PD B 1 H3S1 H 0.6133 0.9296 0.7478 0.045 Uiso 0.08 1 calc PR B 1 H3S2 H 0.5907 0.8964 0.7694 0.045 Uiso 0.08 1 calc PR B 1 C4S C 0.631(2) 0.8727(16) 0.727(2) 0.06(2) Uiso 0.08 1 d PD B 1 H4S1 H 0.6435 0.8884 0.7083 0.069 Uiso 0.08 1 calc PR B 1 H4S2 H 0.6083 0.8633 0.7146 0.069 Uiso 0.08 1 calc PR B 1 O1S' O 0.6581(7) 0.8351(7) 0.7291(14) 0.20(4) Uiso 0.08 1 d PD B 2 C1S' C 0.6812(7) 0.8654(8) 0.7555(11) 0.10(2) Uiso 0.08 1 d PD B 2 H1S3 H 0.6822 0.8569 0.7816 0.119 Uiso 0.08 1 calc PR B 2 H1S4 H 0.7068 0.8689 0.7462 0.119 Uiso 0.08 1 calc PR B 2 C2S' C 0.6571(11) 0.9048(10) 0.752(2) 0.05(2) Uiso 0.08 1 d PD B 2 H2S3 H 0.6512 0.9147 0.7770 0.056 Uiso 0.08 1 calc PR B 2 H2S4 H 0.6713 0.9237 0.7381 0.056 Uiso 0.08 1 calc PR B 2 C3S' C 0.6185(14) 0.8932(13) 0.729(2) 0.04(2) Uiso 0.08 1 d PD B 2 H3S3 H 0.6178 0.9069 0.7056 0.045 Uiso 0.08 1 calc PR B 2 H3S4 H 0.5969 0.9012 0.7443 0.045 Uiso 0.08 1 calc PR B 2 C4S' C 0.6145(14) 0.8480(14) 0.721(3) 0.06(2) Uiso 0.08 1 d PD B 2 H4S3 H 0.6072 0.8432 0.6945 0.069 Uiso 0.08 1 calc PR B 2 H4S4 H 0.5966 0.8357 0.7375 0.069 Uiso 0.08 1 calc PR B 2 O1W O 0.7263(15) 0.7737(15) 0.7263(15) 0.10(3) Uiso 0.17 3 d SP . . C2W C 0.7500 0.7500 0.707(3) 0.20(4) Uiso 0.33 2 d SP . . C1W C 0.7500 0.7732 0.7268 0.240 Uiso 0.06 1 d P . . O1X O 0.731(2) 0.720(3) 0.475(3) 0.14(3) Uiso 0.08 1 d P . . C1X C 0.7423(16) 0.7201(17) 0.502(2) 0.113(16) Uiso 0.25 1 d P . . C2X C 0.731(2) 0.720(3) 0.475(3) 0.14(3) Uiso 0.08 1 d P . . In1' In 0.42830(11) 0.42830(11) 0.57170(11) 0.0577(18) Uiso 0.17 3 d SP . 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 In1 0.0640(5) 0.0640(5) 0.0640(5) 0.0070(4) 0.0070(4) -0.0070(4) C1 0.104(7) 0.104(7) 0.104(7) 0.008(8) 0.008(8) -0.008(8) Li1 0.079(9) 0.079(9) 0.079(9) -0.010(9) -0.010(9) -0.010(9) Li2 0.054(8) 0.063(9) 0.094(11) -0.028(12) -0.001(11) -0.032(7) P1 0.0695(18) 0.0677(17) 0.100(2) -0.007(2) 0.002(2) -0.0060(14) C11 0.098(9) 0.045(6) 0.154(13) -0.021(8) 0.021(9) -0.019(6) C12 0.23(2) 0.153(16) 0.197(18) -0.097(14) -0.086(16) -0.042(15) C13 0.36(4) 0.17(2) 0.21(2) -0.039(18) -0.11(2) -0.07(2) C14 0.113(12) 0.129(14) 0.23(2) -0.013(14) 0.005(14) -0.057(11) C15 0.139(6) 0.142(6) 0.148(7) 0.000(5) -0.005(5) -0.003(4) C16 0.106(5) 0.105(6) 0.111(6) -0.004(4) 0.002(4) -0.012(4) O1 0.061(4) 0.094(5) 0.107(5) 0.000(6) 0.001(5) -0.004(4) O1' 0.061(4) 0.094(5) 0.107(5) 0.000(6) 0.001(5) -0.004(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 I1 Li1 2.55(3) . ? I1 Li1 2.55(3) 4_566 ? I1 Li1 2.55(3) 3_656 ? I1 Li1 2.55(3) 2_665 ? In1 C1 2.24(2) . ? In1 P1 2.629(4) . ? In1 P1 2.629(4) 11_566 ? In1 P1 2.629(4) 8_656 ? In1 Li2 3.12(2) . ? In1 Li2 3.12(2) 8_656 ? In1 Li2 3.12(2) 11_566 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? Li1 P1 2.526(8) 9 ? Li1 P1 2.526(8) . ? Li1 P1 2.526(8) 5 ? Li1 Li2 2.833(18) 5 ? Li1 Li2 2.833(18) 9 ? Li1 Li2 2.833(19) . ? Li2 O1 1.992(14) . ? Li2 P1 2.658(16) . ? Li2 P1 2.59(2) 11_566 ? Li2 P1 2.62(2) 9 ? Li2 Li2 2.77(3) 4_566 ? P1 C11 1.830(8) . ? P1 Li2 2.59(2) 8_656 ? P1 Li2 2.62(2) 5 ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? O1 C4T 1.38(3) . ? O1 C1T 1.47(2) . ? C1T C2T 1.53(3) . ? C1T H1T1 0.9700 . ? C1T H1T2 0.9700 . ? C2T C3T 1.36(3) . ? C2T H2T1 0.9700 . ? C2T H2T2 0.9700 . ? C3T C4T 1.58(3) . ? C3T H3T1 0.9700 . ? C3T H3T2 0.9700 . ? C4T H4T1 0.9700 . ? C4T H4T2 0.9700 . ? C1T' C2T' 1.44(3) . ? C1T' H1T3 0.9700 . ? C1T' H1T4 0.9700 . ? C2T' C3T' 1.43(3) . ? C2T' H2T3 0.9700 . ? C2T' H2T4 0.9700 . ? C3T' C4T' 1.54(3) . ? C3T' H3T3 0.9700 . ? C3T' H3T4 0.9700 . ? C4T' H4T3 0.9700 . ? C4T' H4T4 0.9700 . ? Li3Y O1W 1.97(9) . ? Li3Y O1S' 2.05(4) 30_566 ? Li3Y O1S 2.05(4) 30_566 ? Li3Y O1S 2.05(4) . ? Li3Y O1S' 2.05(4) 84_665 ? Li3Y O1S 2.05(4) 84_665 ? O1S C1S 1.64(3) . ? O1S C4S 1.64(3) . ? C1S C2S 1.64(3) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S C3S 1.64(3) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S C4S 1.64(3) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? C2S' C3S' 1.63(3) . ? C2S' H2S3 0.9700 . ? C2S' H2S4 0.9700 . ? C3S' C4S' 1.63(3) . ? C3S' H3S3 0.9700 . ? C3S' H3S4 0.9700 . ? C4S' H4S3 0.9700 . ? C4S' H4S4 0.9700 . ? O1W C1W 0.84(6) . ? O1W C1W 0.84(6) 84_665 ? O1W C1W 0.84(6) 30_566 ? O1W C2W 1.37(6) 35_566 ? O1W C2W 1.37(6) . ? O1W C2W 1.37(6) 5 ? O1W C1W 1.85(7) 35_566 ? O1W C1W 1.85(7) 51_656 ? O1W C1W 1.85(7) 5 ? O1W C1W 1.85(7) 56_656 ? O1W C1W 1.85(7) 74_665 ? O1W C1W 1.85(7) 58_656 ? C2W C1W 1.08(7) 56_656 ? C2W C1W 1.08(7) . ? C2W C1W 1.08(7) 30_566 ? C2W C1W 1.08(7) 74_665 ? C2W O1W 1.37(6) 74_665 ? C2W C1W 1.91(9) 35_566 ? C2W C1W 1.91(9) 84_665 ? C2W C1W 1.91(9) 9 ? C2W C1W 1.91(9) 58_656 ? C2W C2W 2.15(16) 35_566 ? C2W C2W 2.15(16) 79_665 ? C1W C1W 1.6385(2) 51_656 ? C1W C1W 1.63849(18) 74_665 ? C1W C2W 1.91(9) 79_665 ? C1W C2W 1.91(9) 5 ? C1W O1W 1.85(7) 51_656 ? O1X C1X 1.03(9) . ? O1X C1X 1.59(11) 63_465 ? C1X C1X 1.55(8) 40_645 ? C1X C1X 1.55(8) 63_465 ? C1X C2X 1.59(11) 40_645 ? C1X O1X 1.59(11) 40_645 ? C1X C2X 2.04(11) 63_465 ? C1X O1X 2.04(11) 63_465 ? C1X C1X 2.18(12) 74_665 ? 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 Li1 I1 Li1 109.471(6) . 4_566 ? Li1 I1 Li1 109.471(3) . 3_656 ? Li1 I1 Li1 109.471(1) 4_566 3_656 ? Li1 I1 Li1 109.471(1) . 2_665 ? Li1 I1 Li1 109.471(1) 4_566 2_665 ? Li1 I1 Li1 109.471(1) 3_656 2_665 ? C1 In1 P1 116.37(6) . . ? C1 In1 P1 116.37(6) . 11_566 ? P1 In1 P1 101.78(8) . 11_566 ? C1 In1 P1 116.37(6) . 8_656 ? P1 In1 P1 101.78(8) . 8_656 ? P1 In1 P1 101.78(8) 11_566 8_656 ? C1 In1 Li2 115.5(3) . . ? P1 In1 Li2 128.2(3) 8_656 . ? C1 In1 Li2 115.5(3) . 8_656 ? P1 In1 Li2 128.2(3) 11_566 8_656 ? Li2 In1 Li2 102.9(3) . 8_656 ? C1 In1 Li2 115.5(3) . 11_566 ? P1 In1 Li2 128.2(3) . 11_566 ? Li2 In1 Li2 102.9(3) . 11_566 ? Li2 In1 Li2 102.9(3) 8_656 11_566 ? In1 C1 H1A 109.5 . . ? In1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? In1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? I1 Li1 P1 103.4(7) . 9 ? I1 Li1 P1 103.4(7) . . ? P1 Li1 P1 114.8(5) 9 . ? I1 Li1 P1 103.4(7) . 5 ? P1 Li1 P1 114.8(5) 9 5 ? P1 Li1 P1 114.8(5) . 5 ? I1 Li1 Li2 100.5(7) . 5 ? P1 Li1 Li2 156.1(14) 9 5 ? I1 Li1 Li2 100.5(7) . 9 ? P1 Li1 Li2 156.1(14) . 9 ? P1 Li1 Li2 58.1(4) 5 9 ? Li2 Li1 Li2 116.7(4) 5 9 ? I1 Li1 Li2 100.5(7) . . ? P1 Li1 Li2 156.1(14) 5 . ? Li2 Li1 Li2 116.7(4) 5 . ? Li2 Li1 Li2 116.7(4) 9 . ? O1 Li2 P1 112.1(6) . . ? O1 Li2 P1 112.6(10) . 11_566 ? P1 Li2 P1 102.2(7) . 11_566 ? O1 Li2 P1 111.6(9) . 9 ? P1 Li2 P1 107.6(7) . 9 ? P1 Li2 P1 110.3(5) 11_566 9 ? O1 Li2 Li1 142.0(12) . . ? P1 Li2 Li1 105.2(7) 11_566 . ? O1 Li2 Li2 109.8(5) . 4_566 ? P1 Li2 Li2 138.1(3) . 4_566 ? Li1 Li2 Li2 92.3(7) . 4_566 ? O1 Li2 In1 107.8(9) . . ? P1 Li2 In1 140.5(5) 9 . ? Li1 Li2 In1 91.6(5) . . ? Li2 Li2 In1 110.7(10) 4_566 . ? C11 P1 Li1 124.9(8) . . ? C11 P1 In1 109.7(3) . . ? Li1 P1 In1 111.9(6) . . ? C11 P1 Li2 94.7(4) . . ? Li1 P1 Li2 66.2(4) . . ? In1 P1 Li2 72.3(5) . . ? C11 P1 Li2 121.2(5) . 8_656 ? Li1 P1 Li2 104.4(7) . 8_656 ? In1 P1 Li2 73.5(4) . 8_656 ? Li2 P1 Li2 136.9(6) . 8_656 ? C11 P1 Li2 105.2(5) . 5 ? Li1 P1 Li2 66.8(3) . 5 ? In1 P1 Li2 134.9(4) . 5 ? Li2 P1 Li2 132.3(7) . 5 ? Li2 P1 Li2 64.2(6) 8_656 5 ? C12 C11 C16 120.0 . . ? C12 C11 P1 116.9(6) . . ? C16 C11 P1 123.0(6) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C4T O1 C1T 110.8(12) . . ? C4T O1 Li2 119.0(13) . . ? C1T O1 Li2 128.2(12) . . ? O1 C1T C2T 103.4(11) . . ? O1 C1T H1T1 111.1 . . ? C2T C1T H1T1 111.1 . . ? O1 C1T H1T2 111.1 . . ? C2T C1T H1T2 111.1 . . ? H1T1 C1T H1T2 109.0 . . ? C3T C2T C1T 107.3(16) . . ? C3T C2T H2T1 110.2 . . ? C1T C2T H2T1 110.2 . . ? C3T C2T H2T2 110.2 . . ? C1T C2T H2T2 110.2 . . ? H2T1 C2T H2T2 108.5 . . ? C4T C3T C2T 104.4(14) . . ? C4T C3T H3T1 110.9 . . ? C2T C3T H3T1 110.9 . . ? C4T C3T H3T2 110.9 . . ? C2T C3T H3T2 110.9 . . ? H3T1 C3T H3T2 108.9 . . ? C3T C4T O1 104.7(12) . . ? C3T C4T H4T1 110.8 . . ? O1 C4T H4T1 110.8 . . ? C3T C4T H4T2 110.8 . . ? O1 C4T H4T2 110.8 . . ? H4T1 C4T H4T2 108.9 . . ? C2T' C1T' H1T3 110.4 . . ? C2T' C1T' H1T4 110.4 . . ? H1T3 C1T' H1T4 108.6 . . ? C1T' C2T' C3T' 109.5(12) . . ? C1T' C2T' H2T3 109.8 . . ? C3T' C2T' H2T3 109.8 . . ? C1T' C2T' H2T4 109.8 . . ? C3T' C2T' H2T4 109.8 . . ? H2T3 C2T' H2T4 108.2 . . ? C2T' C3T' C4T' 104.6(12) . . ? C2T' C3T' H3T3 110.8 . . ? C4T' C3T' H3T3 110.8 . . ? C2T' C3T' H3T4 110.8 . . ? C4T' C3T' H3T4 110.8 . . ? H3T3 C3T' H3T4 108.9 . . ? C3T' C4T' H4T3 110.9 . . ? C3T' C4T' H4T4 110.9 . . ? H4T3 C4T' H4T4 108.9 . . ? O1W Li3Y O1S' 107.6(12) . 30_566 ? O1W Li3Y O1S 107.6(12) . 30_566 ? O1W Li3Y O1S 107.6(12) . . ? O1S' Li3Y O1S 111.3(11) 30_566 . ? O1S Li3Y O1S 111.3(11) 30_566 . ? O1W Li3Y O1S' 107.6(12) . 84_665 ? O1S' Li3Y O1S' 111.3(11) 30_566 84_665 ? O1S Li3Y O1S' 111.3(11) 30_566 84_665 ? O1S Li3Y O1S' 111.3(11) . 84_665 ? O1W Li3Y O1S 107.6(12) . 84_665 ? O1S' Li3Y O1S 111.3(11) 30_566 84_665 ? O1S Li3Y O1S 111.3(11) 30_566 84_665 ? O1S Li3Y O1S 111.3(11) . 84_665 ? O1S' Li3Y C1W 92.5(12) 30_566 . ? O1S Li3Y C1W 92.5(12) 30_566 . ? O1S Li3Y C1W 115.8(12) . . ? O1S' Li3Y C1W 113.4(12) 84_665 . ? O1S Li3Y C1W 113.4(12) 84_665 . ? O1S' Li3Y C1W 113.4(12) 30_566 84_665 ? O1S Li3Y C1W 113.4(12) 30_566 84_665 ? O1S Li3Y C1W 92.5(12) . 84_665 ? O1S' Li3Y C1W 115.8(12) 84_665 84_665 ? O1S Li3Y C1W 115.8(12) 84_665 84_665 ? O1S' Li3Y C1W 115.8(12) 30_566 30_566 ? O1S Li3Y C1W 115.8(12) 30_566 30_566 ? O1S Li3Y C1W 113.4(12) . 30_566 ? O1S' Li3Y C1W 92.5(12) 84_665 30_566 ? O1S Li3Y C1W 92.5(12) 84_665 30_566 ? C1S O1S Li3Y 111.3(16) . . ? C4S O1S Li3Y 138(4) . . ? O1S C1S C2S 112.4(16) . . ? O1S C1S H1S1 109.1 . . ? C2S C1S H1S1 109.1 . . ? O1S C1S H1S2 109.1 . . ? C2S C1S H1S2 109.1 . . ? H1S1 C1S H1S2 107.8 . . ? C1S C2S C3S 112.6(18) . . ? C1S C2S H2S1 109.1 . . ? C3S C2S H2S1 109.1 . . ? C1S C2S H2S2 109.1 . . ? C3S C2S H2S2 109.1 . . ? H2S1 C2S H2S2 107.8 . . ? C2S C3S C4S 82(3) . . ? C2S C3S H3S1 115.0 . . ? C4S C3S H3S1 115.0 . . ? C2S C3S H3S2 115.0 . . ? C4S C3S H3S2 115.0 . . ? H3S1 C3S H3S2 112.0 . . ? C3S C4S O1S 136(5) . . ? C3S C4S H4S1 103.0 . . ? O1S C4S H4S1 103.0 . . ? C3S C4S H4S2 103.0 . . ? O1S C4S H4S2 103.0 . . ? H4S1 C4S H4S2 105.1 . . ? C3S' C2S' H2S3 110.8 . . ? C3S' C2S' H2S4 110.8 . . ? H2S3 C2S' H2S4 108.8 . . ? C2S' C3S' C4S' 114(3) . . ? C2S' C3S' H3S3 108.7 . . ? C4S' C3S' H3S3 108.7 . . ? C2S' C3S' H3S4 108.7 . . ? C4S' C3S' H3S4 108.7 . . ? H3S3 C3S' H3S4 107.6 . . ? C3S' C4S' H4S3 112.0 . . ? C3S' C4S' H4S4 112.0 . . ? H4S3 C4S' H4S4 109.7 . . ? C1W O1W C2W 119(10) 30_566 35_566 ? C1W O1W C2W 119(10) 84_665 . ? C2W O1W C2W 104(7) 35_566 . ? C1W O1W C2W 119(10) . 5 ? C2W O1W C2W 104(7) 35_566 5 ? C2W O1W C2W 104(7) . 5 ? C2W O1W C1W 100(7) 5 35_566 ? C2W O1W C1W 100(7) . 51_656 ? C2W O1W C1W 100(7) . 5 ? C2W O1W C1W 100(7) 5 56_656 ? C2W O1W C1W 100(7) 35_566 74_665 ? C2W O1W C1W 100(7) 35_566 58_656 ? C1W C2W O1W 98(8) . 74_665 ? C1W C2W O1W 98(8) 30_566 74_665 ? C1W C2W O1W 98(8) 56_656 . ? C1W C2W O1W 98(8) 74_665 . ? O1W C2W O1W 120(10) 74_665 . ? O1W C2W C1W 97(8) 74_665 84_665 ? O1W C2W C1W 97(8) . 9 ? C1W C2W C2W 94(5) 74_665 35_566 ? O1W C2W C2W 94(5) 74_665 35_566 ? C2W C1W C2W 171(9) 35_566 . ? O1W C1W C1W 136(4) . 35_566 ? C2W C1W C1W 117(3) . 35_566 ? C2W C1W C1W 117(3) . 84_665 ? C2W C1W C1W 117(3) 35_566 30_566 ? O1W C1W C1W 136(4) . 56_656 ? C2W C1W C1W 117(3) 35_566 56_656 ? C1W C1W C1W 90.000(1) 30_566 51_656 ? C1W C1W C1W 90.000(1) 56_656 51_656 ? O1W C1W C1W 91(4) . 74_665 ? C2W C1W C1W 131(5) 35_566 74_665 ? O1W C1W C2W 144(5) . 79_665 ? C1W C1W C2W 105.1(18) 84_665 79_665 ? C1W C1W C2W 105.1(18) 30_566 79_665 ? C1W C1W C2W 105.1(18) 35_566 5 ? C1W C1W C2W 105.1(18) 56_656 5 ? C2W C1W C2W 105(4) 79_665 5 ? O1W C1W O1W 118(4) . 51_656 ? C2W C1W O1W 126(4) . 51_656 ? C1W C1W O1W 108.9(17) 30_566 51_656 ? O1X C1X C1X 103(9) . 40_645 ? O1X C1X C2X 140(8) . 40_645 ? C1X C1X C2X 105(5) 63_465 40_645 ? O1X C1X O1X 140(8) . 40_645 ? C1X C1X O1X 105(5) 63_465 40_645 ? O1X C1X C2X 102(7) . 63_465 ? O1X C1X O1X 102(7) . 63_465 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 19.97 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.623 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.081