#--------Gallabenzene_LiDME--------# data_GallaBenz_LiDME _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H66 Ga Li O2 Si2' _chemical_formula_sum 'C36 H66 Ga Li O2 Si2' _chemical_formula_weight 663.72 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' 'Si' 'Si' 0.0817 0.0704 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.7398(16) _cell_length_b 29.690(5) _cell_length_c 15.217(3) _cell_angle_alpha 90 _cell_angle_beta 101.070(4) _cell_angle_gamma 90 _cell_volume 3875.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8791 _cell_measurement_theta_min 2.4718 _cell_measurement_theta_max 31.3686 _exptl_crystal_description 'Platelet' _exptl_crystal_colour 'pale-yellow' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_F_000 1440 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.799 _shelx_estimated_absorpt_T_min 0.857 _shelx_estimated_absorpt_T_max 0.976 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8503 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku VariMax Saturn' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 31909 _diffrn_reflns_av_unetI/netI 0.0671 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.036 _diffrn_reflns_theta_max 27.475 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 8863 _reflns_number_gt 6615 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'RIGAKU CrystalClear' _computing_cell_refinement 'RIGAKU CrystalClear' _computing_data_reduction 'RIGAKU CrystalClear' _computing_structure_solution 'SIR-2004' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Yadokari-XG 2009(Wakita Nemoto et al.)' _computing_publication_material 'Yadokari-XG 2009(Wakita,Nemoto et al.)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+4.0001P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8863 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1143(4) 0.17303(10) 0.1973(2) 0.0285(7) Uani 1 1 d . . . . . C2 C 0.0392(4) 0.16285(11) 0.1097(2) 0.0308(7) Uani 1 1 d . . . . . H2 H 0.0146 0.1879 0.0708 0.037 Uiso 1 1 calc R U . . . C3 C -0.0046(4) 0.12062(11) 0.0716(2) 0.0321(7) Uani 1 1 d . . . . . H3 H -0.0571 0.1204 0.0108 0.038 Uiso 1 1 calc R U . . . C4 C 0.0215(4) 0.07852(11) 0.1144(2) 0.0300(7) Uani 1 1 d . . . . . H4 H -0.0108 0.0530 0.0778 0.036 Uiso 1 1 calc R U . . . C5 C 0.0885(4) 0.06929(11) 0.2034(2) 0.0275(7) Uani 1 1 d . . . . . C6 C 0.2118(4) 0.12160(10) 0.4105(2) 0.0286(7) Uani 1 1 d . . . . . C7 C 0.3691(4) 0.11654(11) 0.4506(2) 0.0315(7) Uani 1 1 d . . . . . C8 C 0.4127(4) 0.11255(12) 0.5431(2) 0.0364(8) Uani 1 1 d . . . . . H8 H 0.5197 0.1084 0.5690 0.044 Uiso 1 1 calc R U . . . C9 C 0.3041(4) 0.11454(11) 0.5987(2) 0.0344(8) Uani 1 1 d . . . . . C10 C 0.1491(5) 0.12067(12) 0.5589(2) 0.0374(8) Uani 1 1 d . . . . . H10 H 0.0731 0.1226 0.5958 0.045 Uiso 1 1 calc R U . . . C11 C 0.1018(4) 0.12399(11) 0.4670(2) 0.0332(7) Uani 1 1 d . . . . . C12 C 0.4964(4) 0.11465(14) 0.3962(3) 0.0439(9) Uani 1 1 d . . . . . H12 H 0.4498 0.1105 0.3328 0.066 Uiso 1 1 calc R U . . . H12A H 0.5663 0.0894 0.4168 0.066 Uiso 1 1 calc R U . . . H12B H 0.5557 0.1429 0.4037 0.066 Uiso 1 1 calc R U . . . C13 C 0.3529(5) 0.11061(14) 0.6990(3) 0.0490(10) Uani 1 1 d . . . . . H13 H 0.3513 0.0789 0.7165 0.073 Uiso 1 1 calc R U . . . H13A H 0.2805 0.1278 0.7280 0.073 Uiso 1 1 calc R U . . . H13B H 0.4585 0.1227 0.7177 0.073 Uiso 1 1 calc R U . . . C14 C -0.0703(5) 0.13047(16) 0.4291(3) 0.0523(11) Uani 1 1 d . . . . . H14 H -0.1316 0.1107 0.4607 0.078 Uiso 1 1 calc R U . . . H14A H -0.0916 0.1230 0.3652 0.078 Uiso 1 1 calc R U . . . H14B H -0.0991 0.1619 0.4370 0.078 Uiso 1 1 calc R U . . . C15 C -0.1651(5) 0.26346(15) 0.1378(4) 0.0664(14) Uani 1 1 d . . . . . H15 H -0.1888 0.2329 0.1150 0.100 Uiso 1 1 calc R U . . . H15A H -0.1161 0.2805 0.0954 0.100 Uiso 1 1 calc R U . . . H15B H -0.2617 0.2785 0.1450 0.100 Uiso 1 1 calc R U . . . C16 C -0.0531(5) 0.26115(13) 0.2288(3) 0.0507(11) Uani 1 1 d . . . . . H16 H -0.0318 0.2928 0.2500 0.061 Uiso 1 1 calc R U . . . C17 C -0.1345(6) 0.23731(17) 0.2970(4) 0.0707(16) Uani 1 1 d . . . . . H17 H -0.2317 0.2531 0.3004 0.106 Uiso 1 1 calc R U . . . H17A H -0.0657 0.2376 0.3560 0.106 Uiso 1 1 calc R U . . . H17B H -0.1578 0.2061 0.2780 0.106 Uiso 1 1 calc R U . . . C18 C 0.4408(6) 0.23492(17) 0.3433(4) 0.0702(15) Uani 1 1 d . . . . . H18 H 0.4803 0.2597 0.3114 0.105 Uiso 1 1 calc R U . . . H18A H 0.4571 0.2063 0.3144 0.105 Uiso 1 1 calc R U . . . H18B H 0.4966 0.2344 0.4057 0.105 Uiso 1 1 calc R U . . . C19 C 0.2675(5) 0.24166(13) 0.3409(3) 0.0440(9) Uani 1 1 d . . . . . H19 H 0.2355 0.2175 0.3794 0.053 Uiso 1 1 calc R U . . . C20 C 0.2441(6) 0.28664(15) 0.3869(3) 0.0624(13) Uani 1 1 d . . . . . H20 H 0.3079 0.2869 0.4473 0.094 Uiso 1 1 calc R U . . . H20A H 0.1340 0.2901 0.3905 0.094 Uiso 1 1 calc R U . . . H20B H 0.2756 0.3115 0.3520 0.094 Uiso 1 1 calc R U . . . C21 C 0.2563(6) 0.31494(13) 0.1551(3) 0.0612(13) Uani 1 1 d . . . . . H21 H 0.3440 0.3177 0.2057 0.092 Uiso 1 1 calc R U . . . H21A H 0.1637 0.3292 0.1705 0.092 Uiso 1 1 calc R U . . . H21B H 0.2825 0.3298 0.1025 0.092 Uiso 1 1 calc R U . . . C22 C 0.2227(5) 0.26466(13) 0.1342(3) 0.0434(9) Uani 1 1 d . . . . . H22 H 0.1375 0.2640 0.0800 0.052 Uiso 1 1 calc R U . . . C23 C 0.3651(6) 0.24272(15) 0.1054(3) 0.0611(13) Uani 1 1 d . . . . . H23 H 0.3882 0.2585 0.0529 0.092 Uiso 1 1 calc R U . . . H23A H 0.3423 0.2110 0.0903 0.092 Uiso 1 1 calc R U . . . H23B H 0.4554 0.2447 0.1546 0.092 Uiso 1 1 calc R U . . . C24 C 0.3959(5) 0.00226(16) 0.3494(3) 0.0585(12) Uani 1 1 d . . . . . H24 H 0.4585 0.0056 0.4098 0.088 Uiso 1 1 calc R U . . . H24A H 0.4182 0.0273 0.3117 0.088 Uiso 1 1 calc R U . . . H24B H 0.4218 -0.0263 0.3236 0.088 Uiso 1 1 calc R U . . . C25 C 0.2221(5) 0.00263(12) 0.3544(3) 0.0408(9) Uani 1 1 d . . . . . H25 H 0.2058 0.0303 0.3889 0.049 Uiso 1 1 calc R U . . . C26 C 0.1856(6) -0.03745(14) 0.4111(3) 0.0573(12) Uani 1 1 d . . . . . H26 H 0.2019 -0.0657 0.3808 0.086 Uiso 1 1 calc R U . . . H26A H 0.0768 -0.0356 0.4185 0.086 Uiso 1 1 calc R U . . . H26B H 0.2547 -0.0365 0.4699 0.086 Uiso 1 1 calc R U . . . C27 C -0.1805(6) 0.01972(19) 0.3173(4) 0.089(2) Uani 1 1 d . . . . . H27 H -0.2097 0.0491 0.2899 0.134 Uiso 1 1 calc R U . . . H27A H -0.1027 0.0239 0.3724 0.134 Uiso 1 1 calc R U . . . H27B H -0.2731 0.0050 0.3316 0.134 Uiso 1 1 calc R U . . . C28 C -0.1117(5) -0.00976(14) 0.2517(3) 0.0536(11) Uani 1 1 d . . . . . H28 H -0.1007 -0.0408 0.2777 0.064 Uiso 1 1 calc R U . . . C29 C -0.2262(5) -0.01319(18) 0.1619(4) 0.0815(18) Uani 1 1 d . . . . . H29 H -0.3281 -0.0231 0.1724 0.122 Uiso 1 1 calc R U . . . H29A H -0.1868 -0.0350 0.1234 0.122 Uiso 1 1 calc R U . . . H29B H -0.2367 0.0164 0.1327 0.122 Uiso 1 1 calc R U . . . C30 C 0.2929(7) -0.01360(18) 0.1163(4) 0.0755(16) Uani 1 1 d . . . . . H30 H 0.3851 -0.0148 0.1644 0.113 Uiso 1 1 calc R U . . . H30A H 0.2769 0.0173 0.0940 0.113 Uiso 1 1 calc R U . . . H30B H 0.3083 -0.0335 0.0674 0.113 Uiso 1 1 calc R U . . . C31 C 0.1499(5) -0.02906(12) 0.1524(3) 0.0441(9) Uani 1 1 d . . . . . H31 H 0.0607 -0.0285 0.1002 0.053 Uiso 1 1 calc R U . . . C32 C 0.1686(6) -0.07847(13) 0.1825(3) 0.0610(13) Uani 1 1 d . . . . . H32 H 0.1848 -0.0973 0.1322 0.091 Uiso 1 1 calc R U . . . H32A H 0.0742 -0.0884 0.2029 0.091 Uiso 1 1 calc R U . . . H32B H 0.2586 -0.0813 0.2317 0.091 Uiso 1 1 calc R U . . . Si1 Si 0.14248(11) 0.23391(3) 0.22533(7) 0.0313(2) Uani 1 1 d . . . . . Si2 Si 0.09153(11) 0.00921(3) 0.24050(7) 0.0307(2) Uani 1 1 d . . . . . Li1 Li 0.2630(7) 0.1194(2) 0.1118(4) 0.0392(14) Uani 1 1 d . . . . . C33 C 0.2197(6) 0.15691(19) -0.0841(3) 0.0704(14) Uani 1 1 d . . . . . H33 H 0.2758 0.1854 -0.0858 0.106 Uiso 1 1 calc R U . . . H33A H 0.1149 0.1630 -0.0729 0.106 Uiso 1 1 calc R U . . . H33B H 0.2116 0.1414 -0.1417 0.106 Uiso 1 1 calc R U . . . C34 C 0.4615(5) 0.12250(15) -0.0221(3) 0.0568(12) Uani 1 1 d . . . . . H34 H 0.5183 0.1515 -0.0160 0.068 Uiso 1 1 calc R U . . . H34A H 0.4673 0.1092 -0.0810 0.068 Uiso 1 1 calc R U . . . C35 C 0.5305(5) 0.09087(15) 0.0526(3) 0.0543(11) Uani 1 1 d . . . . . H35 H 0.4838 0.0606 0.0407 0.065 Uiso 1 1 calc R U . . . H35A H 0.6443 0.0882 0.0555 0.065 Uiso 1 1 calc R U . . . C36 C 0.6206(5) 0.13703(16) 0.1782(3) 0.0554(11) Uani 1 1 d . . . . . H36 H 0.7214 0.1216 0.1870 0.083 Uiso 1 1 calc R U . . . H36A H 0.5991 0.1464 0.2364 0.083 Uiso 1 1 calc R U . . . H36B H 0.6235 0.1636 0.1404 0.083 Uiso 1 1 calc R U . . . O1 O 0.3024(4) 0.12912(10) -0.01422(19) 0.0501(7) Uani 1 1 d . . . . . O2 O 0.5013(3) 0.10734(9) 0.13603(19) 0.0471(7) Uani 1 1 d . . . . . Ga1 Ga 0.14160(4) 0.12205(2) 0.27843(2) 0.02587(12) Uani 1 1 d . . . . . 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 C1 0.0280(16) 0.0267(17) 0.0308(17) 0.0004(13) 0.0057(13) 0.0026(12) C2 0.0321(17) 0.0308(18) 0.0290(17) 0.0048(13) 0.0046(14) 0.0049(13) C3 0.0303(17) 0.0380(19) 0.0251(16) 0.0024(13) -0.0018(13) 0.0001(14) C4 0.0308(17) 0.0304(18) 0.0280(16) -0.0062(13) 0.0033(13) -0.0043(13) C5 0.0262(16) 0.0285(17) 0.0279(16) -0.0007(13) 0.0052(13) -0.0013(12) C6 0.0325(17) 0.0261(17) 0.0261(16) -0.0007(12) 0.0025(13) 0.0003(13) C7 0.0328(17) 0.0306(18) 0.0308(17) -0.0018(13) 0.0052(14) -0.0009(13) C8 0.0333(18) 0.039(2) 0.0327(18) 0.0004(15) -0.0031(14) -0.0019(15) C9 0.045(2) 0.0284(18) 0.0273(17) 0.0001(13) 0.0000(15) -0.0054(15) C10 0.043(2) 0.040(2) 0.0320(18) -0.0005(15) 0.0127(16) -0.0027(15) C11 0.0300(17) 0.0368(19) 0.0329(18) -0.0004(14) 0.0060(14) 0.0019(14) C12 0.0276(18) 0.065(3) 0.039(2) 0.0028(18) 0.0057(15) 0.0003(17) C13 0.062(3) 0.049(2) 0.033(2) -0.0033(17) 0.0026(19) -0.010(2) C14 0.034(2) 0.086(3) 0.039(2) 0.007(2) 0.0093(17) 0.006(2) C15 0.034(2) 0.045(3) 0.112(4) 0.008(3) -0.005(2) 0.0080(18) C16 0.037(2) 0.032(2) 0.086(3) -0.013(2) 0.017(2) 0.0023(16) C17 0.052(3) 0.069(3) 0.103(4) -0.028(3) 0.046(3) -0.015(2) C18 0.058(3) 0.069(3) 0.070(3) -0.020(3) -0.021(2) 0.016(2) C19 0.053(2) 0.034(2) 0.042(2) -0.0055(16) 0.0014(18) -0.0036(17) C20 0.076(3) 0.052(3) 0.058(3) -0.027(2) 0.009(2) -0.010(2) C21 0.073(3) 0.035(2) 0.079(3) 0.010(2) 0.023(3) -0.006(2) C22 0.045(2) 0.039(2) 0.046(2) 0.0057(17) 0.0096(18) -0.0044(17) C23 0.065(3) 0.055(3) 0.072(3) -0.002(2) 0.034(3) -0.008(2) C24 0.040(2) 0.060(3) 0.065(3) 0.010(2) -0.017(2) -0.011(2) C25 0.051(2) 0.0283(19) 0.041(2) 0.0048(15) 0.0033(17) -0.0016(16) C26 0.073(3) 0.051(3) 0.045(2) 0.017(2) 0.007(2) 0.002(2) C27 0.065(4) 0.084(4) 0.137(6) 0.022(4) 0.066(4) 0.013(3) C28 0.035(2) 0.046(2) 0.080(3) 0.022(2) 0.011(2) -0.0021(17) C29 0.035(2) 0.075(4) 0.123(5) 0.039(3) -0.013(3) -0.015(2) C30 0.090(4) 0.073(4) 0.076(4) -0.012(3) 0.047(3) 0.019(3) C31 0.054(2) 0.032(2) 0.043(2) -0.0061(16) -0.0004(18) 0.0079(17) C32 0.077(3) 0.035(2) 0.061(3) -0.0092(19) -0.011(2) 0.010(2) Si1 0.0293(5) 0.0254(5) 0.0388(5) -0.0012(4) 0.0056(4) 0.0006(4) Si2 0.0281(5) 0.0256(5) 0.0376(5) 0.0019(4) 0.0037(4) -0.0005(4) Li1 0.036(3) 0.048(4) 0.034(3) -0.001(3) 0.007(3) 0.005(3) C33 0.080(4) 0.092(4) 0.042(3) 0.018(2) 0.017(2) 0.011(3) C34 0.056(3) 0.070(3) 0.051(3) -0.007(2) 0.028(2) 0.000(2) C35 0.048(2) 0.053(3) 0.067(3) -0.013(2) 0.023(2) 0.0046(19) C36 0.041(2) 0.073(3) 0.054(3) -0.004(2) 0.012(2) 0.001(2) O1 0.0534(18) 0.0603(18) 0.0416(16) 0.0020(13) 0.0219(14) 0.0057(14) O2 0.0387(15) 0.0533(16) 0.0523(17) -0.0033(13) 0.0165(13) 0.0003(12) Ga1 0.02430(19) 0.0276(2) 0.02523(19) -0.00005(13) 0.00344(13) 0.00095(13) _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 C1 C2 1.402(4) . ? C1 Si1 1.863(3) . ? C1 Ga1 1.939(3) . ? C1 Li1 2.562(7) . ? C2 C3 1.403(5) . ? C2 Li1 2.338(7) . ? C2 H2 0.9500 . ? C3 C4 1.408(5) . ? C3 Li1 2.301(7) . ? C3 H3 0.9500 . ? C4 C5 1.396(4) . ? C4 Li1 2.442(7) . ? C4 H4 0.9500 . ? C5 Si2 1.869(3) . ? C5 Ga1 1.941(3) . ? C5 Li1 2.702(7) . ? C6 C7 1.401(5) . ? C6 C11 1.410(5) . ? C6 Ga1 1.985(3) . ? C7 C8 1.392(5) . ? C7 C12 1.510(5) . ? C8 C9 1.389(5) . ? C8 H8 0.9500 . ? C9 C10 1.386(5) . ? C9 C13 1.508(5) . ? C10 C11 1.384(5) . ? C10 H10 0.9500 . ? C11 C14 1.516(5) . ? C12 H12 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.535(6) . ? C15 H15 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.539(6) . ? C16 Si1 1.901(4) . ? C16 H16 1.0000 . ? C17 H17 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.521(6) . ? C18 H18 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.539(5) . ? C19 Si1 1.898(4) . ? C19 H19 1.0000 . ? C20 H20 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.543(6) . ? C21 H21 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.541(6) . ? C22 Si1 1.903(4) . ? C22 H22 1.0000 . ? C23 H23 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.535(6) . ? C24 H24 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.539(5) . ? C25 Si2 1.893(4) . ? C25 H25 1.0000 . ? C26 H26 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.535(7) . ? C27 H27 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.534(7) . ? C28 Si2 1.902(4) . ? C28 H28 1.0000 . ? C29 H29 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C31 1.529(6) . ? C30 H30 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.536(5) . ? C31 Si2 1.900(4) . ? C31 H31 1.0000 . ? C32 H32 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? Li1 O1 2.033(7) . ? Li1 O2 2.075(7) . ? Li1 Ga1 2.931(6) . ? C33 O1 1.428(5) . ? C33 H33 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 O1 1.432(5) . ? C34 C35 1.508(6) . ? C34 H34 0.9900 . ? C34 H34A 0.9900 . ? C35 O2 1.428(5) . ? C35 H35 0.9900 . ? C35 H35A 0.9900 . ? C36 O2 1.421(5) . ? C36 H36 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Si1 116.4(2) . . ? C2 C1 Ga1 114.5(2) . . ? Si1 C1 Ga1 128.13(18) . . ? C2 C1 Li1 64.7(2) . . ? Si1 C1 Li1 131.4(2) . . ? Ga1 C1 Li1 79.97(18) . . ? C1 C2 C3 128.8(3) . . ? C1 C2 Li1 82.4(3) . . ? C3 C2 Li1 71.0(2) . . ? C1 C2 H2 115.6 . . ? C3 C2 H2 115.6 . . ? Li1 C2 H2 122.0 . . ? C2 C3 C4 126.6(3) . . ? C2 C3 Li1 73.8(2) . . ? C4 C3 Li1 78.3(2) . . ? C2 C3 H3 116.7 . . ? C4 C3 H3 116.7 . . ? Li1 C3 H3 122.4 . . ? C5 C4 C3 128.6(3) . . ? C5 C4 Li1 84.8(2) . . ? C3 C4 Li1 67.3(2) . . ? C5 C4 H4 115.7 . . ? C3 C4 H4 115.7 . . ? Li1 C4 H4 123.2 . . ? C4 C5 Si2 117.3(2) . . ? C4 C5 Ga1 114.9(2) . . ? Si2 C5 Ga1 127.19(17) . . ? C4 C5 Li1 64.2(2) . . ? Si2 C5 Li1 134.8(2) . . ? Ga1 C5 Li1 76.36(17) . . ? C7 C6 C11 117.8(3) . . ? C7 C6 Ga1 121.9(2) . . ? C11 C6 Ga1 120.2(2) . . ? C8 C7 C6 120.4(3) . . ? C8 C7 C12 117.6(3) . . ? C6 C7 C12 122.0(3) . . ? C9 C8 C7 121.8(3) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 117.7(3) . . ? C10 C9 C13 121.0(4) . . ? C8 C9 C13 121.3(4) . . ? C11 C10 C9 121.9(3) . . ? C11 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? C10 C11 C6 120.4(3) . . ? C10 C11 C14 118.4(3) . . ? C6 C11 C14 121.2(3) . . ? C7 C12 H12 109.5 . . ? C7 C12 H12A 109.5 . . ? H12 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C13 H13 109.5 . . ? C9 C13 H13A 109.5 . . ? H13 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C14 H14 109.5 . . ? C11 C14 H14A 109.5 . . ? H14 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C16 C15 H15 109.5 . . ? C16 C15 H15A 109.5 . . ? H15 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C15 C16 C17 109.4(4) . . ? C15 C16 Si1 114.5(3) . . ? C17 C16 Si1 110.9(3) . . ? C15 C16 H16 107.2 . . ? C17 C16 H16 107.2 . . ? Si1 C16 H16 107.2 . . ? C16 C17 H17 109.5 . . ? C16 C17 H17A 109.5 . . ? H17 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C19 C18 H18 109.5 . . ? C19 C18 H18A 109.5 . . ? H18 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C18 C19 C20 108.8(4) . . ? C18 C19 Si1 113.6(3) . . ? C20 C19 Si1 115.0(3) . . ? C18 C19 H19 106.3 . . ? C20 C19 H19 106.3 . . ? Si1 C19 H19 106.3 . . ? C19 C20 H20 109.5 . . ? C19 C20 H20A 109.5 . . ? H20 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C22 C21 H21 109.5 . . ? C22 C21 H21A 109.5 . . ? H21 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C23 C22 C21 109.6(3) . . ? C23 C22 Si1 115.8(3) . . ? C21 C22 Si1 113.3(3) . . ? C23 C22 H22 105.7 . . ? C21 C22 H22 105.7 . . ? Si1 C22 H22 105.7 . . ? C22 C23 H23 109.5 . . ? C22 C23 H23A 109.5 . . ? H23 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C25 C24 H24 109.5 . . ? C25 C24 H24A 109.5 . . ? H24 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C24 C25 C26 109.6(3) . . ? C24 C25 Si2 112.6(3) . . ? C26 C25 Si2 116.1(3) . . ? C24 C25 H25 105.9 . . ? C26 C25 H25 105.9 . . ? Si2 C25 H25 105.9 . . ? C25 C26 H26 109.5 . . ? C25 C26 H26A 109.5 . . ? H26 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C28 C27 H27 109.5 . . ? C28 C27 H27A 109.5 . . ? H27 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C29 C28 C27 110.3(4) . . ? C29 C28 Si2 113.6(3) . . ? C27 C28 Si2 112.3(3) . . ? C29 C28 H28 106.7 . . ? C27 C28 H28 106.7 . . ? Si2 C28 H28 106.7 . . ? C28 C29 H29 109.5 . . ? C28 C29 H29A 109.5 . . ? H29 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C31 C30 H30 109.5 . . ? C31 C30 H30A 109.5 . . ? H30 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C30 C31 C32 110.3(4) . . ? C30 C31 Si2 115.0(3) . . ? C32 C31 Si2 112.8(3) . . ? C30 C31 H31 106.0 . . ? C32 C31 H31 106.0 . . ? Si2 C31 H31 106.0 . . ? C31 C32 H32 109.5 . . ? C31 C32 H32A 109.5 . . ? H32 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C1 Si1 C19 110.92(16) . . ? C1 Si1 C16 109.83(16) . . ? C19 Si1 C16 106.5(2) . . ? C1 Si1 C22 110.48(16) . . ? C19 Si1 C22 112.96(19) . . ? C16 Si1 C22 105.96(19) . . ? C5 Si2 C25 110.23(15) . . ? C5 Si2 C31 110.34(16) . . ? C25 Si2 C31 112.82(18) . . ? C5 Si2 C28 110.51(16) . . ? C25 Si2 C28 107.25(19) . . ? C31 Si2 C28 105.5(2) . . ? O1 Li1 O2 81.2(3) . . ? O1 Li1 C3 95.4(3) . . ? O2 Li1 C3 169.7(3) . . ? O1 Li1 C2 101.6(3) . . ? O2 Li1 C2 155.0(3) . . ? C3 Li1 C2 35.20(15) . . ? O1 Li1 C4 112.9(3) . . ? O2 Li1 C4 138.8(3) . . ? C3 Li1 C4 34.36(14) . . ? C2 Li1 C4 63.3(2) . . ? O1 Li1 C1 125.8(3) . . ? O2 Li1 C1 127.3(3) . . ? C3 Li1 C1 62.40(19) . . ? C2 Li1 C1 32.84(13) . . ? C4 Li1 C1 77.1(2) . . ? O1 Li1 C5 141.2(3) . . ? O2 Li1 C5 117.4(3) . . ? C3 Li1 C5 60.02(18) . . ? C2 Li1 C5 76.0(2) . . ? C4 Li1 C5 30.98(13) . . ? C1 Li1 C5 71.85(19) . . ? O1 Li1 Ga1 165.2(3) . . ? O2 Li1 Ga1 111.6(3) . . ? C3 Li1 Ga1 73.22(19) . . ? C2 Li1 Ga1 63.67(17) . . ? C4 Li1 Ga1 62.73(16) . . ? C1 Li1 Ga1 40.63(12) . . ? C5 Li1 Ga1 40.05(11) . . ? O1 C33 H33 109.5 . . ? O1 C33 H33A 109.5 . . ? H33 C33 H33A 109.5 . . ? O1 C33 H33B 109.5 . . ? H33 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O1 C34 C35 106.1(3) . . ? O1 C34 H34 110.5 . . ? C35 C34 H34 110.5 . . ? O1 C34 H34A 110.5 . . ? C35 C34 H34A 110.5 . . ? H34 C34 H34A 108.7 . . ? O2 C35 C34 110.1(3) . . ? O2 C35 H35 109.6 . . ? C34 C35 H35 109.6 . . ? O2 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? H35 C35 H35A 108.2 . . ? O2 C36 H36 109.5 . . ? O2 C36 H36A 109.5 . . ? H36 C36 H36A 109.5 . . ? O2 C36 H36B 109.5 . . ? H36 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 O1 C34 112.2(3) . . ? C33 O1 Li1 129.2(3) . . ? C34 O1 Li1 113.7(3) . . ? C36 O2 C35 111.9(3) . . ? C36 O2 Li1 126.7(3) . . ? C35 O2 Li1 104.2(3) . . ? C1 Ga1 C5 105.63(14) . . ? C1 Ga1 C6 128.75(13) . . ? C5 Ga1 C6 125.62(13) . . ? C1 Ga1 Li1 59.40(15) . . ? C5 Ga1 Li1 63.59(16) . . ? C6 Ga1 Li1 141.47(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si1 C1 C2 C3 -176.3(3) . . . . ? Ga1 C1 C2 C3 -6.7(5) . . . . ? Li1 C1 C2 C3 58.1(4) . . . . ? Si1 C1 C2 Li1 125.6(3) . . . . ? Ga1 C1 C2 Li1 -64.7(2) . . . . ? C1 C2 C3 C4 -1.4(6) . . . . ? Li1 C2 C3 C4 61.5(4) . . . . ? C1 C2 C3 Li1 -62.9(4) . . . . ? C2 C3 C4 C5 3.3(6) . . . . ? Li1 C3 C4 C5 62.8(4) . . . . ? C2 C3 C4 Li1 -59.5(4) . . . . ? C3 C4 C5 Si2 175.4(3) . . . . ? Li1 C4 C5 Si2 -129.1(2) . . . . ? C3 C4 C5 Ga1 3.6(5) . . . . ? Li1 C4 C5 Ga1 59.1(2) . . . . ? C3 C4 C5 Li1 -55.5(4) . . . . ? C11 C6 C7 C8 2.1(5) . . . . ? Ga1 C6 C7 C8 -174.5(2) . . . . ? C11 C6 C7 C12 -178.7(3) . . . . ? Ga1 C6 C7 C12 4.7(4) . . . . ? C6 C7 C8 C9 -1.6(5) . . . . ? C12 C7 C8 C9 179.1(3) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C7 C8 C9 C13 -179.4(3) . . . . ? C8 C9 C10 C11 1.1(5) . . . . ? C13 C9 C10 C11 -179.5(3) . . . . ? C9 C10 C11 C6 -0.6(5) . . . . ? C9 C10 C11 C14 179.7(3) . . . . ? C7 C6 C11 C10 -1.0(5) . . . . ? Ga1 C6 C11 C10 175.7(3) . . . . ? C7 C6 C11 C14 178.7(3) . . . . ? Ga1 C6 C11 C14 -4.7(5) . . . . ? C2 C1 Si1 C19 -172.9(3) . . . . ? Ga1 C1 Si1 C19 19.1(3) . . . . ? Li1 C1 Si1 C19 -94.3(3) . . . . ? C2 C1 Si1 C16 69.7(3) . . . . ? Ga1 C1 Si1 C16 -98.3(3) . . . . ? Li1 C1 Si1 C16 148.3(3) . . . . ? C2 C1 Si1 C22 -46.8(3) . . . . ? Ga1 C1 Si1 C22 145.2(2) . . . . ? Li1 C1 Si1 C22 31.8(3) . . . . ? C18 C19 Si1 C1 78.0(3) . . . . ? C20 C19 Si1 C1 -155.8(3) . . . . ? C18 C19 Si1 C16 -162.5(3) . . . . ? C20 C19 Si1 C16 -36.3(4) . . . . ? C18 C19 Si1 C22 -46.6(4) . . . . ? C20 C19 Si1 C22 79.6(4) . . . . ? C4 C5 Si2 C25 168.4(3) . . . . ? Ga1 C5 Si2 C25 -21.0(3) . . . . ? Li1 C5 Si2 C25 88.7(3) . . . . ? C4 C5 Si2 C31 43.2(3) . . . . ? Ga1 C5 Si2 C31 -146.2(2) . . . . ? Li1 C5 Si2 C31 -36.6(3) . . . . ? C4 C5 Si2 C28 -73.2(3) . . . . ? Ga1 C5 Si2 C28 97.4(3) . . . . ? Li1 C5 Si2 C28 -152.9(3) . . . . ? C24 C25 Si2 C5 -77.7(3) . . . . ? C26 C25 Si2 C5 154.8(3) . . . . ? C24 C25 Si2 C31 46.1(3) . . . . ? C26 C25 Si2 C31 -81.3(4) . . . . ? C24 C25 Si2 C28 161.9(3) . . . . ? C26 C25 Si2 C28 34.4(4) . . . . ? O1 C34 C35 O2 -51.8(5) . . . . ? C35 C34 O1 C33 -177.1(4) . . . . ? C35 C34 O1 Li1 25.3(4) . . . . ? C34 C35 O2 C36 -88.6(4) . . . . ? C34 C35 O2 Li1 51.4(4) . . . . ? _refine_diff_density_max 0.819 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.090 _shelxl_version_number 2013-4 _shelx_res_file ; TITL REM Yadorkari-X generated CELL 0.71075 8.7398 29.6899 15.2171 90.0000 101.0695 90.0000 ZERR 4.0 0.0016 0.0052 0.0028 0.0000 0.0035 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H Li O Si Ga UNIT 144 264 4 8 8 4 SIZE 0.20 0.03 0.03 TEMP -100.0 L.S. 50 FMAP 2 PLAN -25 ACTA CONF WPDB -1 BOND $H MERG 2 OMIT -10.000000 55.000000 WGHT 0.063100 4.000100 FVAR 3.91979 C1 1 0.114337 0.173026 0.197330 11.00000 0.02796 0.02670 = 0.03081 0.00044 0.00567 0.00263 C2 1 0.039228 0.162848 0.109670 11.00000 0.03208 0.03076 = 0.02899 0.00478 0.00463 0.00490 AFIX 43 H2 2 0.014645 0.187939 0.070778 11.00000 -1.20000 AFIX 0 C3 1 -0.004552 0.120620 0.071602 11.00000 0.03032 0.03795 = 0.02505 0.00237 -0.00179 0.00014 AFIX 43 H3 2 -0.057063 0.120426 0.010845 11.00000 -1.20000 AFIX 0 C4 1 0.021507 0.078516 0.114380 11.00000 0.03080 0.03038 = 0.02803 -0.00620 0.00334 -0.00430 AFIX 43 H4 2 -0.010778 0.053002 0.077829 11.00000 -1.20000 AFIX 0 C5 1 0.088527 0.069290 0.203422 11.00000 0.02623 0.02850 = 0.02790 -0.00068 0.00521 -0.00134 C6 1 0.211834 0.121602 0.410457 11.00000 0.03246 0.02610 = 0.02608 -0.00075 0.00247 0.00028 C7 1 0.369104 0.116543 0.450580 11.00000 0.03278 0.03061 = 0.03077 -0.00184 0.00515 -0.00093 C8 1 0.412733 0.112553 0.543121 11.00000 0.03331 0.03931 = 0.03272 0.00040 -0.00315 -0.00186 AFIX 43 H8 2 0.519670 0.108359 0.568961 11.00000 -1.20000 AFIX 0 C9 1 0.304076 0.114539 0.598730 11.00000 0.04476 0.02838 = 0.02725 0.00012 0.00001 -0.00540 C10 1 0.149073 0.120667 0.558889 11.00000 0.04256 0.03971 = 0.03204 -0.00051 0.01273 -0.00270 AFIX 43 H10 2 0.073072 0.122645 0.595757 11.00000 -1.20000 AFIX 0 C11 1 0.101751 0.123991 0.466959 11.00000 0.02995 0.03680 = 0.03292 -0.00039 0.00597 0.00190 C12 1 0.496405 0.114647 0.396221 11.00000 0.02764 0.06533 = 0.03855 0.00280 0.00575 0.00028 AFIX 137 H12 2 0.449826 0.110463 0.332848 11.00000 -1.50000 H12A 2 0.566330 0.089391 0.416811 11.00000 -1.50000 H12B 2 0.555706 0.142857 0.403716 11.00000 -1.50000 AFIX 0 C13 1 0.352889 0.110612 0.699027 11.00000 0.06237 0.04858 = 0.03339 -0.00325 0.00261 -0.01030 AFIX 137 H13 2 0.351337 0.078874 0.716528 11.00000 -1.50000 H13A 2 0.280517 0.127754 0.727989 11.00000 -1.50000 H13B 2 0.458530 0.122655 0.717730 11.00000 -1.50000 AFIX 0 C14 1 -0.070345 0.130470 0.429098 11.00000 0.03365 0.08565 = 0.03858 0.00674 0.00934 0.00647 AFIX 137 H14 2 -0.131612 0.110717 0.460677 11.00000 -1.50000 H14A 2 -0.091584 0.122969 0.365193 11.00000 -1.50000 H14B 2 -0.099083 0.161914 0.436951 11.00000 -1.50000 AFIX 0 C15 1 -0.165057 0.263464 0.137799 11.00000 0.03439 0.04538 = 0.11209 0.00787 -0.00462 0.00800 AFIX 137 H15 2 -0.188850 0.232886 0.114966 11.00000 -1.50000 H15A 2 -0.116073 0.280460 0.095393 11.00000 -1.50000 H15B 2 -0.261686 0.278519 0.144981 11.00000 -1.50000 AFIX 0 C16 1 -0.053133 0.261155 0.228757 11.00000 0.03685 0.03153 = 0.08574 -0.01260 0.01674 0.00233 AFIX 13 H16 2 -0.031813 0.292823 0.249986 11.00000 -1.20000 AFIX 0 C17 1 -0.134464 0.237309 0.296984 11.00000 0.05232 0.06887 = 0.10325 -0.02845 0.04602 -0.01481 AFIX 137 H17 2 -0.231665 0.253076 0.300389 11.00000 -1.50000 H17A 2 -0.065696 0.237556 0.355995 11.00000 -1.50000 H17B 2 -0.157829 0.206110 0.278019 11.00000 -1.50000 AFIX 0 C18 1 0.440793 0.234918 0.343322 11.00000 0.05812 0.06940 = 0.06976 -0.02024 -0.02120 0.01645 AFIX 137 H18 2 0.480320 0.259689 0.311415 11.00000 -1.50000 H18A 2 0.457102 0.206283 0.314434 11.00000 -1.50000 H18B 2 0.496596 0.234435 0.405665 11.00000 -1.50000 AFIX 0 C19 1 0.267475 0.241665 0.340919 11.00000 0.05345 0.03355 = 0.04186 -0.00545 0.00136 -0.00361 AFIX 13 H19 2 0.235514 0.217483 0.379442 11.00000 -1.20000 AFIX 0 C20 1 0.244109 0.286637 0.386859 11.00000 0.07562 0.05222 = 0.05767 -0.02716 0.00883 -0.00968 AFIX 137 H20 2 0.307870 0.286939 0.447328 11.00000 -1.50000 H20A 2 0.133983 0.290064 0.390517 11.00000 -1.50000 H20B 2 0.275594 0.311549 0.351989 11.00000 -1.50000 AFIX 0 C21 1 0.256272 0.314940 0.155132 11.00000 0.07334 0.03489 = 0.07879 0.01013 0.02348 -0.00556 AFIX 137 H21 2 0.343996 0.317743 0.205704 11.00000 -1.50000 H21A 2 0.163695 0.329169 0.170495 11.00000 -1.50000 H21B 2 0.282451 0.329849 0.102487 11.00000 -1.50000 AFIX 0 C22 1 0.222701 0.264660 0.134208 11.00000 0.04541 0.03893 = 0.04623 0.00573 0.00959 -0.00445 AFIX 13 H22 2 0.137463 0.263996 0.079992 11.00000 -1.20000 AFIX 0 C23 1 0.365091 0.242722 0.105400 11.00000 0.06499 0.05520 = 0.07150 -0.00238 0.03406 -0.00845 AFIX 137 H23 2 0.388203 0.258531 0.052937 11.00000 -1.50000 H23A 2 0.342255 0.211030 0.090294 11.00000 -1.50000 H23B 2 0.455369 0.244653 0.154649 11.00000 -1.50000 AFIX 0 C24 1 0.395866 0.002262 0.349409 11.00000 0.03968 0.06022 = 0.06470 0.01043 -0.01726 -0.01057 AFIX 137 H24 2 0.458539 0.005609 0.409771 11.00000 -1.50000 H24A 2 0.418181 0.027257 0.311733 11.00000 -1.50000 H24B 2 0.421813 -0.026316 0.323551 11.00000 -1.50000 AFIX 0 C25 1 0.222131 0.002629 0.354377 11.00000 0.05065 0.02827 = 0.04127 0.00482 0.00328 -0.00160 AFIX 13 H25 2 0.205770 0.030289 0.388920 11.00000 -1.20000 AFIX 0 C26 1 0.185565 -0.037448 0.411052 11.00000 0.07322 0.05139 = 0.04547 0.01677 0.00688 0.00175 AFIX 137 H26 2 0.201910 -0.065681 0.380787 11.00000 -1.50000 H26A 2 0.076836 -0.035649 0.418535 11.00000 -1.50000 H26B 2 0.254662 -0.036541 0.469931 11.00000 -1.50000 AFIX 0 C27 1 -0.180485 0.019723 0.317347 11.00000 0.06511 0.08427 = 0.13667 0.02174 0.06603 0.01294 AFIX 137 H27 2 -0.209671 0.049126 0.289926 11.00000 -1.50000 H27A 2 -0.102671 0.023864 0.372387 11.00000 -1.50000 H27B 2 -0.273052 0.004999 0.331634 11.00000 -1.50000 AFIX 0 C28 1 -0.111665 -0.009756 0.251709 11.00000 0.03534 0.04554 = 0.07972 0.02198 0.01086 -0.00208 AFIX 13 H28 2 -0.100658 -0.040787 0.277709 11.00000 -1.20000 AFIX 0 C29 1 -0.226158 -0.013192 0.161949 11.00000 0.03482 0.07514 = 0.12336 0.03907 -0.01305 -0.01478 AFIX 137 H29 2 -0.328114 -0.023099 0.172415 11.00000 -1.50000 H29A 2 -0.186811 -0.035027 0.123384 11.00000 -1.50000 H29B 2 -0.236701 0.016354 0.132696 11.00000 -1.50000 AFIX 0 C30 1 0.292876 -0.013604 0.116309 11.00000 0.09011 0.07316 = 0.07576 -0.01163 0.04703 0.01863 AFIX 137 H30 2 0.385110 -0.014751 0.164423 11.00000 -1.50000 H30A 2 0.276876 0.017340 0.094024 11.00000 -1.50000 H30B 2 0.308317 -0.033498 0.067363 11.00000 -1.50000 AFIX 0 C31 1 0.149857 -0.029056 0.152370 11.00000 0.05360 0.03221 = 0.04259 -0.00606 -0.00040 0.00788 AFIX 13 H31 2 0.060708 -0.028459 0.100206 11.00000 -1.20000 AFIX 0 C32 1 0.168557 -0.078466 0.182503 11.00000 0.07674 0.03529 = 0.06115 -0.00919 -0.01113 0.01047 AFIX 137 H32 2 0.184825 -0.097257 0.132151 11.00000 -1.50000 H32A 2 0.074219 -0.088378 0.202858 11.00000 -1.50000 H32B 2 0.258554 -0.081282 0.231722 11.00000 -1.50000 AFIX 0 SI1 5 0.142479 0.233907 0.225331 11.00000 0.02934 0.02544 = 0.03880 -0.00125 0.00560 0.00057 SI2 5 0.091533 0.009214 0.240496 11.00000 0.02808 0.02555 = 0.03757 0.00195 0.00370 -0.00050 LI1 3 0.263043 0.119402 0.111825 11.00000 0.03573 0.04751 = 0.03447 -0.00112 0.00736 0.00504 C33 1 0.219675 0.156906 -0.084121 11.00000 0.07957 0.09218 = 0.04158 0.01844 0.01667 0.01145 AFIX 137 H33 2 0.275756 0.185383 -0.085760 11.00000 -1.50000 H33A 2 0.114909 0.163015 -0.072907 11.00000 -1.50000 H33B 2 0.211615 0.141389 -0.141669 11.00000 -1.50000 AFIX 0 C34 1 0.461453 0.122502 -0.022111 11.00000 0.05635 0.07004 = 0.05089 -0.00705 0.02774 -0.00029 AFIX 23 H34 2 0.518285 0.151524 -0.016035 11.00000 -1.20000 H34A 2 0.467308 0.109166 -0.081002 11.00000 -1.20000 AFIX 0 C35 1 0.530491 0.090873 0.052600 11.00000 0.04788 0.05272 = 0.06710 -0.01272 0.02342 0.00457 AFIX 23 H35 2 0.483787 0.060579 0.040671 11.00000 -1.20000 H35A 2 0.644280 0.088236 0.055533 11.00000 -1.20000 AFIX 0 C36 1 0.620606 0.137034 0.178232 11.00000 0.04068 0.07263 = 0.05406 -0.00385 0.01200 0.00069 AFIX 137 H36 2 0.721447 0.121561 0.187005 11.00000 -1.50000 H36A 2 0.599128 0.146410 0.236413 11.00000 -1.50000 H36B 2 0.623507 0.163606 0.140382 11.00000 -1.50000 AFIX 0 O1 4 0.302358 0.129121 -0.014220 11.00000 0.05340 0.06033 = 0.04157 0.00198 0.02189 0.00572 O2 4 0.501312 0.107340 0.136029 11.00000 0.03867 0.05326 = 0.05232 -0.00326 0.01646 0.00030 GA1 6 0.141602 0.122045 0.278429 11.00000 0.02430 0.02755 = 0.02523 -0.00005 0.00344 0.00095 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM R1 = 0.0633 for 6615 Fo > 4sig(Fo) and 0.0888 for all 8863 data REM 396 parameters refined using 0 restraints END WGHT 0.0631 3.9988 REM Highest difference peak 0.819, deepest hole -0.782, 1-sigma level 0.090 Q1 1 0.3622 0.1342 0.2213 11.00000 0.05 0.82 Q2 1 -0.1801 0.1200 0.2798 11.00000 0.05 0.61 Q3 1 0.4744 0.1239 0.2771 11.00000 0.05 0.60 Q4 1 0.5655 0.2353 0.2217 11.00000 0.05 0.47 Q5 1 0.4052 0.2488 0.2600 11.00000 0.05 0.45 Q6 1 0.3656 0.0224 0.2743 11.00000 0.05 0.45 Q7 1 0.8795 0.1389 0.2404 11.00000 0.05 0.43 Q8 1 0.5852 0.1205 0.2757 11.00000 0.05 0.42 Q9 1 0.1857 0.0097 0.3153 11.00000 0.05 0.40 Q10 1 -0.3761 0.0092 0.2035 11.00000 0.05 0.39 Q11 1 0.2436 0.0990 0.7400 11.00000 0.05 0.36 Q12 1 0.1409 0.2349 0.3284 11.00000 0.05 0.35 Q13 1 0.2891 0.0792 0.2002 11.00000 0.05 0.34 Q14 1 0.2398 0.1578 0.2650 11.00000 0.05 0.34 Q15 1 0.1473 0.1224 0.1723 11.00000 0.05 0.32 Q16 1 0.5048 0.2209 0.2781 11.00000 0.05 0.31 Q17 1 0.0310 0.1223 0.4577 11.00000 0.05 0.31 Q18 1 0.5491 0.1152 0.6663 11.00000 0.05 0.30 Q19 1 0.1168 0.0310 -0.0002 11.00000 0.05 0.30 Q20 1 0.0995 -0.1020 0.2821 11.00000 0.05 0.29 Q21 1 0.7937 0.1206 0.1782 11.00000 0.05 0.29 Q22 1 0.3726 0.3618 0.2247 11.00000 0.05 0.29 Q23 1 0.1015 0.2336 0.0777 11.00000 0.05 0.29 Q24 1 0.3997 0.0868 0.3160 11.00000 0.05 0.29 Q25 1 0.4364 0.0095 0.2277 11.00000 0.05 0.28 ; _shelx_res_checksum 99632 _shelx_hkl_file ; 0 0 3 842.70 504.38 0 0 -3 337.09 275.57 0 0 3 296.89 349.52 0 0 -3 693.32 438.70 0 0 465426.29 2501.31 0 0 -465843.86 2706.28 0 0 464196.46 2437.47 0 0 -463047.35 2376.02 0 0 5 -87.19 234.74 0 0 -5 487.29 290.83 0 0 5 477.22 377.57 0 0 -5 -51.50 474.23 0 0 6182135.9 3515.86 0 0 -6187977.7 3602.07 0 0 6191384.0 3786.54 0 0 -6180884.1 3512.33 0 0 7 -290.33 439.73 0 0 -7 -184.92 391.70 0 0 7 94.53 391.75 0 0 820212.80 1533.41 0 0 -818629.92 1460.86 0 0 821447.22 1572.32 0 0 9 -475.77 451.43 0 0 9 143.11 460.16 0 0 10 773.08 561.97 0 0 10 -201.93 855.40 0 0 11 305.01 620.59 0 0 11 144.20 728.22 0 0 1215026.09 2976.35 0 0 1214694.78 3943.42 0 0 13 967.25 561.97 0 0 13 1917.59 787.71 0 0 1415393.11 927.92 0 0 1417183.45 3366.39 0 0 15 650.50 518.47 0 0 15 492.83 589.49 0 0 1630577.09 2816.02 0 0 1629626.84 2725.84 0 0 17 -842.61 571.48 0 0 17 733.20 1009.99 0 0 18 8944.79 3063.23 0 0 1811776.19 3427.83 0 0 19 964.93 518.48 0 0 19 911.15 624.63 0 -1 3 452.14 272.75 0 1 -3 763.59 436.89 0 1 3 1266.22 581.34 0 -1 -3 827.04 559.99 0 1 3 866.40 481.94 0 -1 3 1397.10 669.11 0 -1 -3 64.23 363.21 0 1 -3 155.48 238.69 0 -1 4 54.49 306.61 0 1 4 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-10 13 1 3802.11 1514.27 -10 13 1 3046.46 1760.50 -10 -13 1 3358.82 1720.95 10 13 0 1314.56 568.54 -10 13 0 458.50 826.99 -10 13 0 2019.96 911.60 -10 -13 0 669.18 1029.53 10 13 1 2494.28 997.35 -10 13 -1 2230.34 1361.49 -10 -13 -1 940.84 893.05 -10 13 -1 1780.80 1137.80 10 13 2 1101.73 802.87 -10 13 -2-1870.51 1032.11 -10 -13 -2 174.13 620.56 -10 13 -2-2544.95 1062.96 10 -13 3 449.09 543.68 10 13 3 324.23 548.56 -10 13 -3 24.40 541.89 -10 -13 -3 -844.10 918.18 -10 14 9 908.30 738.09 -10 14 9 893.83 758.79 -10 -14 9 2215.22 1152.13 -10 14 8 209.80 307.81 -10 14 8 475.81 624.00 -10 -14 8 200.76 743.61 -10 14 7 1666.11 1113.65 -10 14 7 2101.46 1135.50 -10 -14 7 2594.38 1229.99 -10 14 6 984.05 941.18 -10 14 6 -573.61 994.12 -10 -14 6 980.23 830.09 -10 14 5 -556.16 1075.79 -10 -14 5-1275.67 1099.64 -10 14 5 695.75 878.73 -10 14 4 2737.22 1342.85 -10 14 4 1925.77 1188.47 -10 -14 4 3097.69 1687.29 -10 14 3 1970.68 1414.49 -10 14 3 3088.17 1384.08 -10 -14 3 4593.89 1688.21 -10 -14 2 6026.00 1866.09 -10 14 2 5706.40 1653.68 10 14 -1 816.49 454.41 -10 14 1 840.74 704.36 -10 14 1 1080.02 720.05 -10 -14 1 1490.03 1649.23 10 14 0 3363.12 850.36 -10 14 0 4512.60 1045.28 -10 14 0 4340.13 2339.67 -10 -14 0 2959.34 1014.30 10 14 1 5301.10 2524.91 -10 14 -1 6300.56 2531.03 -10 14 -1 5351.62 3961.14 -10 -14 -1 5934.25 2547.63 10 14 2 445.12 677.92 -10 14 -2 257.87 491.99 -10 -14 -2 2737.70 764.52 -10 14 -2 1373.99 1189.65 -10 15 8 3042.59 914.64 -10 15 8 2546.29 1190.32 -10 -15 8 1691.36 1312.99 -10 15 7 4738.10 1601.05 -10 -15 7 3840.78 2310.04 -10 15 7 3574.68 1089.06 -10 15 6 8037.43 2353.82 -10 15 6 7816.63 2312.51 -10 -15 6 6126.52 3247.88 -10 15 5 662.35 629.03 -10 -15 5 945.25 912.99 -10 15 4 7358.15 4875.58 -10 -15 411777.04 3792.11 -10 15 4 7898.17 2862.85 -10 15 3 1173.24 756.66 -10 15 3 811.48 886.82 -10 -15 3 -489.18 926.10 -10 15 2 5279.82 1878.31 -10 -15 2 4413.96 2054.13 -10 15 2 4864.69 2525.54 -10 15 1-2127.23 1013.47 -10 -15 1 1249.68 697.34 -10 15 1 987.77 748.20 10 15 0 571.11 546.88 -10 15 0 446.57 797.72 -10 15 0 1000.69 727.11 -10 -15 0 1382.98 1129.92 10 15 1 801.87 566.82 -10 15 -1 832.64 729.30 -10 15 -1 970.48 839.20 -10 -15 -1 1417.40 720.96 -10 16 7 2446.41 1020.55 -10 -16 7 2343.31 1003.58 -10 16 7 1624.63 1388.10 -10 16 6 916.32 713.44 -10 16 6 1140.30 550.00 -10 -16 6 781.08 731.51 -10 16 5 4481.86 2491.52 -10 16 5 4119.64 946.75 -10 -16 5 3317.63 1379.77 -10 16 4 -349.38 1137.21 -10 -16 4 868.51 680.93 -10 16 4 1534.76 794.06 -10 16 3 1829.23 610.37 -10 16 3 2619.39 945.48 -10 -16 3 2093.53 794.64 -10 16 2 229.37 961.60 -10 -16 2 -678.11 849.04 -10 16 1 1457.55 1048.28 -10 -16 1 2713.80 1453.85 -10 16 1 1614.75 953.41 -10 16 0 -154.44 513.58 -10 16 0 1654.17 923.05 -10 -16 0 754.14 956.03 -10 17 6 699.63 866.16 -10 17 6 1167.75 573.30 -10 -17 6 1859.04 708.02 -10 17 5 3801.47 1557.87 -10 17 5 7152.91 2587.77 -10 -17 5 4315.11 1854.06 -10 17 4 1389.26 910.67 -10 -17 4 1078.84 545.94 -10 17 4 1686.97 919.98 -10 17 3 6116.54 1896.92 -10 17 3 8773.33 2861.15 -10 -17 3 5131.57 2530.38 -10 17 2-1085.33 1100.48 -10 17 2 450.13 641.61 -10 -17 2 1187.50 674.19 -10 17 1 995.33 487.68 -10 -17 1 1309.02 698.05 -10 17 1 1143.69 873.57 -10 18 4 -619.33 1103.75 -10 -18 4 -174.71 549.35 -10 18 4 -973.48 813.28 -10 18 3 3967.32 1134.70 -10 18 3 2954.65 685.57 -10 -18 3 1401.21 777.19 -11 0 8 -210.53 1002.95 -11 0 7 4152.24 2976.20 -11 0 6 236.62 311.79 -11 0 6 -542.56 1021.35 -11 0 5 504.21 443.94 -11 0 5 394.31 747.58 -11 0 4 362.41 537.02 -11 0 4 430.41 676.04 -11 0 3 548.78 777.62 -11 0 3 -46.10 751.02 11 0 -2 1090.18 496.54 -11 0 2 -258.39 974.02 11 0 -1 1016.23 627.21 -11 0 1 -400.80 786.91 11 0 0 648.38 634.26 -11 0 0 -686.15 1071.72 11 0 1 4580.04 1404.20 -11 0 -1 872.12 1085.45 -11 -1 8 2167.38 1307.34 -11 1 8 2811.15 1054.54 -11 1 7 5246.03 1060.56 -11 -1 7 3891.74 1322.56 -11 1 6 -123.64 557.27 -11 -1 6 598.73 1057.96 -11 1 6 569.35 675.52 -11 -1 5 4372.47 1073.69 -11 1 5 2363.69 705.97 -11 1 5 2595.22 1363.14 -11 -1 5 3295.86 1049.16 -11 -1 4 11.76 463.58 -11 1 4 229.45 512.45 -11 1 4 1533.55 898.44 -11 -1 4 798.67 603.58 11 1 -310684.43 3551.73 -11 1 3 8528.35 3377.53 -11 1 317553.09 1870.19 -11 -1 3 9497.33 3634.38 11 -1 -2 1090.86 382.92 11 1 -2 -327.78 810.18 -11 1 2 770.38 877.85 -11 -1 2 91.88 883.89 11 -1 -1 6262.44 2991.35 11 1 -1 7252.44 2748.77 -11 1 1 6924.88 3057.06 -11 -1 1 4224.82 2576.78 11 1 0 1418.02 773.08 11 -1 0 4822.10 964.76 -11 1 0 1044.69 931.16 -11 -1 0 287.10 619.52 11 -1 1 3867.03 2226.32 11 1 1 6667.33 2095.55 -11 1 -1 4228.77 2614.37 -11 -1 -1 5698.05 2641.16 -11 2 813324.36 5019.59 -11 -2 811059.45 4937.73 -11 2 7 1112.53 604.19 -11 2 7 2210.70 1098.43 -11 -2 7 873.30 1236.00 -11 2 6 2406.02 1271.87 -11 2 6 2923.71 1090.32 -11 -2 6 3070.44 1264.59 -11 -2 5 -532.90 538.26 -11 2 5 341.21 628.95 -11 2 5 1291.51 700.40 -11 -2 5 -119.51 1172.45 -11 -2 4 906.59 528.67 -11 2 4 722.43 729.25 -11 2 4 2299.53 614.54 -11 -2 4 1397.10 761.28 11 2 -3 581.80 911.29 -11 2 3 -49.12 792.70 -11 2 3 -416.42 930.89 -11 -2 3 -383.15 1139.57 11 -2 -2 1531.26 958.85 11 2 -2 222.45 361.20 -11 2 2 312.54 806.30 -11 -2 2 832.90 941.87 11 2 -1 549.82 650.06 11 -2 -1 601.44 1020.29 -11 2 1 -131.68 1061.54 -11 -2 1 1040.29 905.60 11 2 0 -358.12 746.41 11 -2 0 530.41 500.97 -11 2 0-2559.98 1046.81 -11 -2 0 578.77 594.08 -11 3 8 2615.69 856.12 -11 -3 8 2935.82 1434.27 -11 3 7 1418.09 754.14 -11 3 7 2191.83 1048.03 -11 -3 7 2946.14 781.36 -11 3 6 4027.02 1566.59 -11 3 6 4121.99 1457.61 -11 -3 6 7161.10 2923.78 -11 3 5 325.88 468.46 -11 -3 5 145.58 382.64 -11 3 5 1006.06 662.20 -11 -3 5 434.27 723.61 -11 -3 414052.65 1814.56 -11 3 411293.39 3509.04 -11 3 412549.28 3655.45 -11 -3 4 9469.00 5062.00 11 3 -3 947.26 529.69 -11 3 3 1353.52 2272.52 -11 3 3 1060.79 705.56 -11 -3 3 724.24 752.74 11 3 -2 5863.32 2810.77 -11 3 2 7851.90 3037.48 -11 3 2 6910.58 2653.31 -11 -3 2 5441.27 2292.37 11 -3 -1 281.25 367.34 11 3 -1 1210.69 1116.17 -11 3 1 -522.58 921.79 -11 -3 1-1240.95 1097.04 11 -3 0 6433.93 2952.64 11 3 0 6591.51 3091.19 -11 3 0 7020.40 3109.23 -11 -3 0 5338.66 2829.50 -11 4 7 6342.28 2531.80 -11 4 711125.11 2983.06 -11 -4 710749.29 4041.01 -11 4 6 207.10 466.84 -11 4 6 1400.76 1067.48 -11 -4 6 888.89 866.53 -11 4 5 6057.86 2710.20 -11 4 5 3777.00 1905.89 -11 -4 5 6501.98 3178.43 -11 -4 4 329.39 383.88 -11 4 4 565.66 565.18 -11 4 4 583.68 591.81 -11 -4 4 1480.46 837.77 11 4 -3 589.13 1267.72 -11 4 3 84.70 482.77 -11 4 3 1185.84 712.61 -11 -4 3 1613.92 1092.15 11 4 -2 -281.55 771.12 -11 4 2 1122.10 650.33 -11 4 2 158.41 748.37 -11 -4 2 78.99 588.78 11 4 -1 265.89 358.80 11 -4 -1 1002.62 707.80 -11 4 1 917.92 985.53 -11 -4 1 -298.67 1039.12 11 -4 0 179.84 581.68 11 4 0 1468.22 562.93 -11 4 0 208.47 730.57 -11 -4 0 1525.41 560.03 -11 5 7 2063.34 914.79 -11 5 7 778.55 898.60 -11 -5 7 4116.67 1806.47 -11 5 6 3015.22 1116.79 -11 5 6 1110.83 944.15 -11 -5 6 3226.20 1331.81 -11 5 5 1207.52 741.78 -11 5 5 272.01 416.67 -11 -5 5 1822.57 900.98 -11 5 4 5746.43 3015.02 -11 5 4 9539.34 4280.45 -11 -5 4 6598.00 3191.86 11 5 -3 1015.77 493.43 -11 5 3 809.00 693.42 -11 5 3 559.35 928.46 -11 -5 3 1616.70 886.77 11 5 -2 3849.29 1871.79 -11 5 2 2253.15 1330.82 -11 -5 2 2920.72 1475.93 11 -5 -1 1557.05 818.89 11 5 -1 2234.96 1217.71 -11 5 1 834.24 597.52 -11 -5 1 392.89 836.23 11 -5 0 3013.12 1134.78 11 5 0 4532.96 1182.68 -11 5 0 3321.26 890.72 -11 -5 0 2716.77 1116.40 -11 6 7 794.94 628.75 -11 6 7 -243.76 898.95 -11 -6 7-1983.39 972.33 -11 6 6 2473.28 1458.49 -11 6 6 2781.53 830.14 -11 -6 6 4630.35 2020.01 -11 6 5 1045.40 734.80 -11 6 5-2091.55 983.09 -11 -6 5-2054.09 1072.03 -11 6 4 2726.03 932.97 -11 6 4 3000.93 1213.11 -11 -6 4 1347.07 1309.50 11 6 -3 1547.54 656.61 -11 6 3 -895.49 806.50 -11 6 3 1476.85 899.94 -11 -6 3 981.17 579.48 11 6 -2 599.43 507.02 -11 6 2 901.29 541.12 -11 -6 2 -320.07 1003.51 -11 6 2 119.08 666.89 11 6 -1 704.52 804.98 -11 6 1 876.26 540.01 -11 6 1 796.26 890.39 -11 -6 1 -164.69 682.25 -11 7 6 551.36 660.66 -11 7 6 -12.00 905.06 -11 -7 6 1586.34 728.31 -11 7 5 2616.37 1107.56 -11 7 5 3006.41 1446.76 -11 -7 5 3421.58 1553.18 -11 7 4 961.69 415.71 -11 7 4 381.67 429.75 -11 -7 4 516.12 923.01 -11 7 314612.58 3793.30 -11 7 314621.20 5498.94 -11 -7 312459.63 5272.56 11 7 -2 7.25 395.77 -11 7 2-1684.93 816.45 -11 -7 2 -1.54 971.96 -11 7 2 74.59 668.94 11 7 -1 8043.66 2426.14 -11 7 1 5398.89 2553.58 -11 7 1 5506.90 3168.91 -11 -7 1 7412.75 2537.77 -11 8 6 -650.03 757.17 -11 8 6-1126.66 948.86 -11 -8 6 548.51 787.38 -11 8 5 559.79 468.63 -11 8 5 2005.80 1082.47 -11 -8 5 288.87 561.04 -11 8 4 396.89 571.76 -11 8 4 289.30 605.22 -11 -8 4 110.76 619.43 -11 8 3 1547.44 662.78 -11 8 3 3019.71 1067.67 -11 -8 3 665.12 769.43 11 8 -2 713.53 535.45 -11 8 2 430.56 884.68 -11 -8 2 1132.29 932.66 -11 8 2 -638.28 925.80 -11 9 4 1906.25 1229.67 -11 9 4 2136.55 1128.65 -11 -9 4 1738.59 794.76 -11 9 3 1755.00 1238.11 -11 9 3 2090.52 839.43 -11 -9 3 2331.24 1512.25 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 12132 #--------Gallabenzene_LiDME3--------# data_GallaBenz_LiDME3 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H56 Ga Si2, C12 H30 Li O6' _chemical_formula_sum 'C44 H86 Ga Li O6 Si2' _chemical_formula_weight 843.96 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' 'Si' 'Si' 0.0817 0.0704 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.000(2) _cell_length_b 28.938(5) _cell_length_c 13.964(2) _cell_angle_alpha 90 _cell_angle_beta 108.411(2) _cell_angle_gamma 90 _cell_volume 4984.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 12951 _cell_measurement_theta_min 2.5872 _cell_measurement_theta_max 31.1552 _exptl_crystal_description 'Platelet' _exptl_crystal_colour 'Pale-yellow' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_F_000 1840 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.640 _shelx_estimated_absorpt_T_min 0.877 _shelx_estimated_absorpt_T_max 0.987 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7304 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku VariMax Saturn' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 40799 _diffrn_reflns_av_unetI/netI 0.0694 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.078 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 11386 _reflns_number_gt 8770 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'RIGAKU CrystalClear' _computing_cell_refinement 'RIGAKU CrystalClear' _computing_data_reduction 'RIGAKU CrystalClear' _computing_structure_solution 'SIR-2004' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Yadokari-XG 2009(Wakita Nemoto et al.)' _computing_publication_material 'Yadokari-XG 2009(Wakita,Nemoto et al.)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+1.7300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11386 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1425 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6081(2) 0.34431(9) 0.9120(2) 0.0170(5) Uani 1 1 d . . . . . C2 C 0.6606(2) 0.31508(9) 0.9936(2) 0.0178(5) Uani 1 1 d . . . . . H2 H 0.6262 0.3120 1.0440 0.021 Uiso 1 1 calc R U . . . C3 C 0.7574(2) 0.28988(9) 1.0103(2) 0.0175(5) Uani 1 1 d . . . . . H3 H 0.7809 0.2723 1.0708 0.021 Uiso 1 1 calc R U . . . C4 C 0.8233(2) 0.28778(9) 0.9476(2) 0.0185(5) Uani 1 1 d . . . . . H4 H 0.8852 0.2684 0.9707 0.022 Uiso 1 1 calc R U . . . C5 C 0.8101(2) 0.31042(9) 0.8551(2) 0.0176(5) Uani 1 1 d . . . . . C6 C 0.6426(2) 0.38749(9) 0.6876(2) 0.0188(5) Uani 1 1 d . . . . . C7 C 0.5670(2) 0.37328(9) 0.5954(2) 0.0203(6) Uani 1 1 d . . . . . C8 C 0.5497(2) 0.39920(11) 0.5073(2) 0.0258(6) Uani 1 1 d . . . . . H8 H 0.4994 0.3883 0.4462 0.031 Uiso 1 1 calc R U . . . C9 C 0.6035(2) 0.44039(11) 0.5064(2) 0.0282(7) Uani 1 1 d . . . . . C10 C 0.6762(2) 0.45529(10) 0.5971(2) 0.0255(6) Uani 1 1 d . . . . . H10 H 0.7136 0.4836 0.5986 0.031 Uiso 1 1 calc R U . . . C11 C 0.6963(2) 0.42980(9) 0.6865(2) 0.0213(6) Uani 1 1 d . . . . . C12 C 0.5018(2) 0.32908(11) 0.5890(2) 0.0289(7) Uani 1 1 d . . . . . H12 H 0.5298 0.3119 0.6525 0.043 Uiso 1 1 calc R U . . . H12A H 0.5083 0.3100 0.5332 0.043 Uiso 1 1 calc R U . . . H12B H 0.4255 0.3368 0.5774 0.043 Uiso 1 1 calc R U . . . C13 C 0.5816(3) 0.46952(12) 0.4117(3) 0.0380(8) Uani 1 1 d . . . . . H13 H 0.5582 0.4495 0.3521 0.057 Uiso 1 1 calc R U . . . H13A H 0.6479 0.4858 0.4126 0.057 Uiso 1 1 calc R U . . . H13B H 0.5244 0.4920 0.4090 0.057 Uiso 1 1 calc R U . . . C14 C 0.7762(2) 0.44924(10) 0.7819(2) 0.0285(7) Uani 1 1 d . . . . . H14 H 0.8414 0.4598 0.7675 0.043 Uiso 1 1 calc R U . . . H14A H 0.7959 0.4252 0.8339 0.043 Uiso 1 1 calc R U . . . H14B H 0.7430 0.4753 0.8059 0.043 Uiso 1 1 calc R U . . . C15 C 0.3646(2) 0.29159(10) 0.9372(2) 0.0265(6) Uani 1 1 d . . . . . H15 H 0.3004 0.2720 0.9107 0.040 Uiso 1 1 calc R U . . . H15A H 0.3688 0.3026 1.0046 0.040 Uiso 1 1 calc R U . . . H15B H 0.4298 0.2737 0.9412 0.040 Uiso 1 1 calc R U . . . C16 C 0.3566(2) 0.33292(10) 0.8670(2) 0.0213(6) Uani 1 1 d . . . . . H16 H 0.2917 0.3514 0.8674 0.026 Uiso 1 1 calc R U . . . C17 C 0.3367(3) 0.31554(11) 0.7586(2) 0.0287(7) Uani 1 1 d . . . . . H17 H 0.3980 0.2964 0.7561 0.043 Uiso 1 1 calc R U . . . H17A H 0.3294 0.3420 0.7132 0.043 Uiso 1 1 calc R U . . . H17B H 0.2700 0.2971 0.7374 0.043 Uiso 1 1 calc R U . . . C18 C 0.3855(2) 0.41101(12) 1.0586(3) 0.0337(7) Uani 1 1 d . . . . . H18 H 0.3923 0.4135 1.1303 0.050 Uiso 1 1 calc R U . . . H18A H 0.3219 0.3922 1.0241 0.050 Uiso 1 1 calc R U . . . H18B H 0.3769 0.4419 1.0284 0.050 Uiso 1 1 calc R U . . . C19 C 0.4878(2) 0.38819(10) 1.0474(2) 0.0231(6) Uani 1 1 d . . . . . H19 H 0.4946 0.3580 1.0839 0.028 Uiso 1 1 calc R U . . . C20 C 0.5885(2) 0.41637(11) 1.1071(3) 0.0317(7) Uani 1 1 d . . . . . H20 H 0.5848 0.4472 1.0774 0.048 Uiso 1 1 calc R U . . . H20A H 0.6542 0.4006 1.1042 0.048 Uiso 1 1 calc R U . . . H20B H 0.5904 0.4191 1.1776 0.048 Uiso 1 1 calc R U . . . C21 C 0.3365(3) 0.44343(11) 0.7933(3) 0.0327(7) Uani 1 1 d . . . . . H21 H 0.3235 0.4566 0.8530 0.049 Uiso 1 1 calc R U . . . H21A H 0.2841 0.4187 0.7658 0.049 Uiso 1 1 calc R U . . . H21B H 0.3283 0.4676 0.7422 0.049 Uiso 1 1 calc R U . . . C22 C 0.4520(2) 0.42370(10) 0.8229(2) 0.0243(6) Uani 1 1 d . . . . . H22 H 0.4620 0.4121 0.7589 0.029 Uiso 1 1 calc R U . . . C23 C 0.5348(3) 0.46298(11) 0.8601(3) 0.0342(8) Uani 1 1 d . . . . . H23 H 0.5278 0.4850 0.8051 0.051 Uiso 1 1 calc R U . . . H23A H 0.6083 0.4501 0.8822 0.051 Uiso 1 1 calc R U . . . H23B H 0.5210 0.4789 0.9169 0.051 Uiso 1 1 calc R U . . . C24 C 1.0935(3) 0.32264(12) 0.9635(2) 0.0320(7) Uani 1 1 d . . . . . H24 H 1.1629 0.3388 0.9904 0.048 Uiso 1 1 calc R U . . . H24A H 1.1047 0.2894 0.9753 0.048 Uiso 1 1 calc R U . . . H24B H 1.0430 0.3339 0.9975 0.048 Uiso 1 1 calc R U . . . C25 C 1.0464(2) 0.33175(10) 0.8502(2) 0.0248(6) Uani 1 1 d . . . . . H25 H 1.0999 0.3200 0.8180 0.030 Uiso 1 1 calc R U . . . C26 C 1.0359(3) 0.38392(11) 0.8323(3) 0.0329(7) Uani 1 1 d . . . . . H26 H 0.9848 0.3966 0.8641 0.049 Uiso 1 1 calc R U . . . H26A H 1.0092 0.3901 0.7596 0.049 Uiso 1 1 calc R U . . . H26B H 1.1069 0.3985 0.8616 0.049 Uiso 1 1 calc R U . . . C27 C 0.9509(3) 0.31697(12) 0.6018(2) 0.0336(7) Uani 1 1 d . . . . . H27 H 0.9729 0.2850 0.5955 0.050 Uiso 1 1 calc R U . . . H27A H 1.0139 0.3348 0.6421 0.050 Uiso 1 1 calc R U . . . H27B H 0.9221 0.3308 0.5345 0.050 Uiso 1 1 calc R U . . . C28 C 0.8630(2) 0.31757(10) 0.6540(2) 0.0240(6) Uani 1 1 d . . . . . H28 H 0.8405 0.3506 0.6544 0.029 Uiso 1 1 calc R U . . . C29 C 0.7614(3) 0.29133(11) 0.5899(2) 0.0308(7) Uani 1 1 d . . . . . H29 H 0.7305 0.3071 0.5250 0.046 Uiso 1 1 calc R U . . . H29A H 0.7076 0.2905 0.6257 0.046 Uiso 1 1 calc R U . . . H29B H 0.7814 0.2597 0.5782 0.046 Uiso 1 1 calc R U . . . C30 C 1.0467(3) 0.22024(11) 0.7675(3) 0.0367(8) Uani 1 1 d . . . . . H30 H 1.0684 0.1885 0.7889 0.055 Uiso 1 1 calc R U . . . H30A H 1.1090 0.2409 0.7940 0.055 Uiso 1 1 calc R U . . . H30B H 1.0213 0.2218 0.6936 0.055 Uiso 1 1 calc R U . . . C31 C 0.9551(2) 0.23514(10) 0.8081(2) 0.0232(6) Uani 1 1 d . . . . . H31 H 0.9840 0.2302 0.8827 0.028 Uiso 1 1 calc R U . . . C32 C 0.8609(3) 0.20107(11) 0.7701(3) 0.0372(8) Uani 1 1 d . . . . . H32 H 0.8281 0.2045 0.6969 0.056 Uiso 1 1 calc R U . . . H32A H 0.8064 0.2075 0.8033 0.056 Uiso 1 1 calc R U . . . H32B H 0.8879 0.1694 0.7856 0.056 Uiso 1 1 calc R U . . . Ga1 Ga 0.68201(2) 0.34843(2) 0.81245(2) 0.01584(10) Uani 1 1 d . . . . . Si1 Si 0.48015(6) 0.37244(2) 0.91262(6) 0.01753(16) Uani 1 1 d . . . . . Si2 Si 0.91358(6) 0.29889(3) 0.79129(6) 0.01842(17) Uani 1 1 d . . . . . Li1 Li 0.5256(4) 0.10793(16) 0.8043(4) 0.0232(10) Uani 1 1 d . . . . . C33 C 0.3100(3) 0.16629(11) 0.7870(3) 0.0317(7) Uani 1 1 d . . . . . H33 H 0.2315 0.1611 0.7611 0.048 Uiso 1 1 calc R U . . . H33A H 0.3325 0.1849 0.7385 0.048 Uiso 1 1 calc R U . . . H33B H 0.3280 0.1827 0.8516 0.048 Uiso 1 1 calc R U . . . C34 C 0.3319(3) 0.09280(11) 0.8669(3) 0.0321(7) Uani 1 1 d . . . . . H34 H 0.2528 0.0956 0.8544 0.038 Uiso 1 1 calc R U . . . H34A H 0.3698 0.1009 0.9383 0.038 Uiso 1 1 calc R U . . . C35 C 0.3603(3) 0.04435(11) 0.8451(3) 0.0351(8) Uani 1 1 d . . . . . H35 H 0.3428 0.0223 0.8920 0.042 Uiso 1 1 calc R U . . . H35A H 0.3182 0.0356 0.7752 0.042 Uiso 1 1 calc R U . . . C36 C 0.5072(3) -0.00199(12) 0.8382(4) 0.0494(11) Uani 1 1 d . . . . . H36 H 0.4941 -0.0241 0.8862 0.074 Uiso 1 1 calc R U . . . H36A H 0.5847 -0.0014 0.8456 0.074 Uiso 1 1 calc R U . . . H36B H 0.4660 -0.0113 0.7692 0.074 Uiso 1 1 calc R U . . . C37 C 0.5423(3) 0.20424(10) 0.7027(2) 0.0290(7) Uani 1 1 d . . . . . H37 H 0.4831 0.2242 0.7075 0.044 Uiso 1 1 calc R U . . . H37A H 0.5168 0.1851 0.6420 0.044 Uiso 1 1 calc R U . . . H37B H 0.6031 0.2234 0.6991 0.044 Uiso 1 1 calc R U . . . C38 C 0.5946(3) 0.20151(10) 0.8811(2) 0.0274(6) Uani 1 1 d . . . . . H38 H 0.5243 0.2105 0.8889 0.033 Uiso 1 1 calc R U . . . H38A H 0.6361 0.2299 0.8784 0.033 Uiso 1 1 calc R U . . . C39 C 0.6571(2) 0.17166(10) 0.9679(2) 0.0266(6) Uani 1 1 d . . . . . H39 H 0.7328 0.1680 0.9675 0.032 Uiso 1 1 calc R U . . . H39A H 0.6587 0.1862 1.0325 0.032 Uiso 1 1 calc R U . . . C40 C 0.6508(3) 0.09905(12) 1.0432(3) 0.0357(8) Uani 1 1 d . . . . . H40 H 0.7294 0.0971 1.0571 0.054 Uiso 1 1 calc R U . . . H40A H 0.6193 0.0680 1.0300 0.054 Uiso 1 1 calc R U . . . H40B H 0.6353 0.1124 1.1017 0.054 Uiso 1 1 calc R U . . . C41 C 0.3706(3) 0.09439(12) 0.5759(2) 0.0325(7) Uani 1 1 d . . . . . H41 H 0.3735 0.1052 0.5103 0.049 Uiso 1 1 calc R U . . . H41A H 0.3232 0.1148 0.5993 0.049 Uiso 1 1 calc R U . . . H41B H 0.3419 0.0628 0.5693 0.049 Uiso 1 1 calc R U . . . C42 C 0.5521(3) 0.06789(11) 0.6160(2) 0.0288(7) Uani 1 1 d . . . . . H42 H 0.5444 0.0744 0.5445 0.035 Uiso 1 1 calc R U . . . H42A H 0.5381 0.0346 0.6227 0.035 Uiso 1 1 calc R U . . . C43 C 0.6632(2) 0.08025(11) 0.6820(3) 0.0303(7) Uani 1 1 d . . . . . H43 H 0.7178 0.0613 0.6641 0.036 Uiso 1 1 calc R U . . . H43A H 0.6782 0.1132 0.6730 0.036 Uiso 1 1 calc R U . . . C44 C 0.7745(2) 0.08179(11) 0.8512(3) 0.0321(7) Uani 1 1 d . . . . . H44 H 0.8285 0.0641 0.8309 0.048 Uiso 1 1 calc R U . . . H44A H 0.7785 0.0732 0.9202 0.048 Uiso 1 1 calc R U . . . H44B H 0.7892 0.1149 0.8486 0.048 Uiso 1 1 calc R U . . . O1 O 0.36513(16) 0.12283(7) 0.80137(17) 0.0275(5) Uani 1 1 d . . . . . O2 O 0.47316(17) 0.04308(7) 0.85790(18) 0.0296(5) Uani 1 1 d . . . . . O3 O 0.57733(16) 0.17498(7) 0.79041(15) 0.0225(4) Uani 1 1 d . . . . . O4 O 0.60513(17) 0.12741(7) 0.95759(16) 0.0279(5) Uani 1 1 d . . . . . O5 O 0.47746(16) 0.09499(7) 0.64748(16) 0.0269(5) Uani 1 1 d . . . . . O6 O 0.66871(15) 0.07173(7) 0.78418(16) 0.0247(4) Uani 1 1 d . . . . . 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 C1 0.0180(13) 0.0125(13) 0.0194(13) -0.0013(9) 0.0045(11) -0.0003(9) C2 0.0187(13) 0.0191(14) 0.0171(13) -0.0034(10) 0.0077(11) -0.0030(10) C3 0.0190(13) 0.0151(13) 0.0169(13) 0.0016(10) 0.0034(10) -0.0009(10) C4 0.0171(13) 0.0171(14) 0.0193(13) -0.0003(10) 0.0027(10) 0.0009(10) C5 0.0188(13) 0.0171(13) 0.0173(13) -0.0008(10) 0.0061(10) -0.0023(10) C6 0.0175(13) 0.0204(14) 0.0196(13) 0.0036(10) 0.0072(11) 0.0045(10) C7 0.0172(13) 0.0224(15) 0.0212(14) 0.0017(11) 0.0059(11) 0.0028(10) C8 0.0210(15) 0.0354(17) 0.0185(14) 0.0041(12) 0.0027(11) 0.0083(12) C9 0.0271(16) 0.0333(17) 0.0282(16) 0.0152(13) 0.0145(13) 0.0134(12) C10 0.0252(15) 0.0188(15) 0.0356(17) 0.0080(12) 0.0141(13) 0.0036(11) C11 0.0198(14) 0.0193(14) 0.0258(15) 0.0043(11) 0.0085(12) 0.0029(10) C12 0.0237(16) 0.0367(18) 0.0241(15) -0.0028(13) 0.0045(12) -0.0076(13) C13 0.043(2) 0.041(2) 0.0344(18) 0.0203(15) 0.0186(16) 0.0164(15) C14 0.0303(17) 0.0202(15) 0.0322(17) 0.0020(12) 0.0061(13) -0.0051(12) C15 0.0291(16) 0.0223(15) 0.0304(16) 0.0007(12) 0.0127(13) -0.0057(12) C16 0.0179(14) 0.0235(15) 0.0228(14) -0.0006(11) 0.0067(11) 0.0018(11) C17 0.0295(17) 0.0313(17) 0.0243(15) -0.0033(12) 0.0071(13) -0.0041(12) C18 0.0260(17) 0.042(2) 0.0367(18) -0.0167(15) 0.0156(14) -0.0043(13) C19 0.0224(15) 0.0218(15) 0.0261(15) -0.0031(11) 0.0091(12) -0.0002(11) C20 0.0245(16) 0.0353(18) 0.0333(17) -0.0119(14) 0.0062(13) 0.0027(13) C21 0.0323(17) 0.0260(17) 0.0391(18) 0.0095(13) 0.0101(15) 0.0103(13) C22 0.0238(15) 0.0208(15) 0.0301(16) 0.0036(11) 0.0110(12) 0.0034(11) C23 0.0359(19) 0.0212(16) 0.047(2) 0.0084(14) 0.0158(16) 0.0005(13) C24 0.0237(16) 0.0367(19) 0.0320(17) -0.0039(13) 0.0037(13) -0.0034(13) C25 0.0206(15) 0.0291(16) 0.0267(15) -0.0018(12) 0.0104(12) -0.0024(11) C26 0.0350(18) 0.0297(17) 0.0341(18) -0.0055(13) 0.0111(15) -0.0103(13) C27 0.0399(19) 0.0405(19) 0.0267(16) 0.0024(14) 0.0195(15) -0.0028(14) C28 0.0298(16) 0.0212(15) 0.0224(14) 0.0006(11) 0.0105(12) -0.0001(11) C29 0.0351(18) 0.0328(18) 0.0244(16) -0.0043(13) 0.0094(13) 0.0027(13) C30 0.0335(18) 0.0272(18) 0.057(2) -0.0065(15) 0.0248(17) 0.0021(13) C31 0.0219(14) 0.0235(15) 0.0257(15) 0.0023(11) 0.0096(12) 0.0041(11) C32 0.0330(18) 0.0205(16) 0.063(2) 0.0042(15) 0.0219(17) 0.0014(13) Ga1 0.01669(17) 0.01445(17) 0.01607(16) 0.00113(10) 0.00476(12) -0.00003(10) Si1 0.0178(4) 0.0156(4) 0.0199(4) 0.0004(3) 0.0069(3) 0.0012(3) Si2 0.0183(4) 0.0191(4) 0.0192(4) 0.0003(3) 0.0078(3) 0.0006(3) Li1 0.024(3) 0.020(2) 0.026(3) -0.0024(19) 0.009(2) -0.0002(18) C33 0.0276(17) 0.0281(17) 0.0391(19) 0.0003(14) 0.0102(14) 0.0082(13) C34 0.0263(17) 0.0323(18) 0.0432(19) -0.0008(14) 0.0189(15) -0.0015(13) C35 0.0299(18) 0.0286(18) 0.049(2) 0.0006(14) 0.0161(16) -0.0066(13) C36 0.053(2) 0.0231(18) 0.086(3) 0.0025(18) 0.042(2) 0.0038(16) C37 0.0386(18) 0.0206(15) 0.0272(16) 0.0066(12) 0.0095(13) 0.0059(12) C38 0.0310(17) 0.0221(15) 0.0258(15) -0.0057(12) 0.0044(13) -0.0017(12) C39 0.0262(16) 0.0240(16) 0.0244(15) -0.0034(12) 0.0006(12) -0.0067(12) C40 0.0390(19) 0.039(2) 0.0273(17) 0.0067(14) 0.0074(15) 0.0029(14) C41 0.0276(17) 0.0348(18) 0.0296(17) -0.0009(13) 0.0012(13) 0.0014(13) C42 0.0348(17) 0.0265(16) 0.0271(16) 0.0006(12) 0.0125(13) 0.0075(13) C43 0.0281(16) 0.0300(17) 0.0385(18) 0.0078(13) 0.0185(14) 0.0071(12) C44 0.0236(16) 0.0256(17) 0.046(2) 0.0036(14) 0.0095(14) 0.0020(12) O1 0.0229(11) 0.0241(11) 0.0373(12) 0.0024(9) 0.0118(9) 0.0027(8) O2 0.0257(11) 0.0193(11) 0.0465(14) -0.0010(9) 0.0150(10) -0.0020(8) O3 0.0270(11) 0.0181(10) 0.0215(10) -0.0002(8) 0.0061(8) 0.0004(8) O4 0.0341(12) 0.0230(11) 0.0233(11) 0.0030(8) 0.0044(9) -0.0035(9) O5 0.0220(11) 0.0292(12) 0.0277(11) -0.0037(9) 0.0054(9) 0.0058(8) O6 0.0191(10) 0.0234(11) 0.0319(11) 0.0028(9) 0.0086(9) 0.0002(8) _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 C1 C2 1.411(4) . ? C1 Si1 1.854(3) . ? C1 Ga1 1.927(3) . ? C2 C3 1.409(4) . ? C2 H2 0.9500 . ? C3 C4 1.406(4) . ? C3 H3 0.9500 . ? C4 C5 1.409(4) . ? C4 H4 0.9500 . ? C5 Si2 1.863(3) . ? C5 Ga1 1.927(3) . ? C6 C7 1.412(4) . ? C6 C11 1.412(4) . ? C6 Ga1 2.004(3) . ? C7 C8 1.397(4) . ? C7 C12 1.521(4) . ? C8 C9 1.384(4) . ? C8 H8 0.9500 . ? C9 C10 1.388(5) . ? C9 C13 1.518(4) . ? C10 C11 1.402(4) . ? C10 H10 0.9500 . ? C11 C14 1.515(4) . ? C12 H12 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.529(4) . ? C15 H15 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.537(4) . ? C16 Si1 1.909(3) . ? C16 H16 1.0000 . ? C17 H17 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 C19 1.537(4) . ? C18 H18 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.544(4) . ? C19 Si1 1.908(3) . ? C19 H19 1.0000 . ? C20 H20 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.536(4) . ? C21 H21 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.539(4) . ? C22 Si1 1.901(3) . ? C22 H22 1.0000 . ? C23 H23 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.528(4) . ? C24 H24 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.529(4) . ? C25 Si2 1.914(3) . ? C25 H25 1.0000 . ? C26 H26 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 C28 1.538(4) . ? C27 H27 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C28 C29 1.542(4) . ? C28 Si2 1.898(3) . ? C28 H28 1.0000 . ? C29 H29 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C30 C31 1.534(4) . ? C30 H30 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.531(4) . ? C31 Si2 1.916(3) . ? C31 H31 1.0000 . ? C32 H32 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? Li1 O3 2.082(5) . ? Li1 O5 2.113(5) . ? Li1 O1 2.118(5) . ? Li1 O4 2.137(5) . ? Li1 O2 2.207(5) . ? Li1 O6 2.229(5) . ? C33 O1 1.430(4) . ? C33 H33 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 O1 1.425(4) . ? C34 C35 1.505(5) . ? C34 H34 0.9900 . ? C34 H34A 0.9900 . ? C35 O2 1.422(4) . ? C35 H35 0.9900 . ? C35 H35A 0.9900 . ? C36 O2 1.431(4) . ? C36 H36 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 O3 1.439(3) . ? C37 H37 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 O3 1.436(3) . ? C38 C39 1.501(4) . ? C38 H38 0.9900 . ? C38 H38A 0.9900 . ? C39 O4 1.434(4) . ? C39 H39 0.9900 . ? C39 H39A 0.9900 . ? C40 O4 1.417(4) . ? C40 H40 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 O5 1.432(4) . ? C41 H41 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C42 O5 1.420(3) . ? C42 C43 1.491(4) . ? C42 H42 0.9900 . ? C42 H42A 0.9900 . ? C43 O6 1.427(4) . ? C43 H43 0.9900 . ? C43 H43A 0.9900 . ? C44 O6 1.428(4) . ? C44 H44 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Si1 117.7(2) . . ? C2 C1 Ga1 113.31(19) . . ? Si1 C1 Ga1 128.96(15) . . ? C3 C2 C1 128.5(2) . . ? C3 C2 H2 115.7 . . ? C1 C2 H2 115.7 . . ? C4 C3 C2 127.4(2) . . ? C4 C3 H3 116.3 . . ? C2 C3 H3 116.3 . . ? C3 C4 C5 129.0(2) . . ? C3 C4 H4 115.5 . . ? C5 C4 H4 115.5 . . ? C4 C5 Si2 117.2(2) . . ? C4 C5 Ga1 113.06(19) . . ? Si2 C5 Ga1 129.68(15) . . ? C7 C6 C11 116.6(2) . . ? C7 C6 Ga1 122.8(2) . . ? C11 C6 Ga1 120.4(2) . . ? C8 C7 C6 121.2(3) . . ? C8 C7 C12 117.9(3) . . ? C6 C7 C12 120.8(2) . . ? C9 C8 C7 121.9(3) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 117.4(3) . . ? C8 C9 C13 122.0(3) . . ? C10 C9 C13 120.6(3) . . ? C9 C10 C11 122.0(3) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C10 C11 C6 120.8(3) . . ? C10 C11 C14 118.1(3) . . ? C6 C11 C14 121.1(3) . . ? C7 C12 H12 109.5 . . ? C7 C12 H12A 109.5 . . ? H12 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C13 H13 109.5 . . ? C9 C13 H13A 109.5 . . ? H13 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C14 H14 109.5 . . ? C11 C14 H14A 109.5 . . ? H14 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C16 C15 H15 109.5 . . ? C16 C15 H15A 109.5 . . ? H15 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C15 C16 C17 109.3(2) . . ? C15 C16 Si1 112.0(2) . . ? C17 C16 Si1 112.8(2) . . ? C15 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? Si1 C16 H16 107.5 . . ? C16 C17 H17 109.5 . . ? C16 C17 H17A 109.5 . . ? H17 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C19 C18 H18 109.5 . . ? C19 C18 H18A 109.5 . . ? H18 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C18 C19 C20 109.4(2) . . ? C18 C19 Si1 115.2(2) . . ? C20 C19 Si1 115.4(2) . . ? C18 C19 H19 105.2 . . ? C20 C19 H19 105.2 . . ? Si1 C19 H19 105.2 . . ? C19 C20 H20 109.5 . . ? C19 C20 H20A 109.5 . . ? H20 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C22 C21 H21 109.5 . . ? C22 C21 H21A 109.5 . . ? H21 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C21 C22 C23 109.6(2) . . ? C21 C22 Si1 115.8(2) . . ? C23 C22 Si1 112.6(2) . . ? C21 C22 H22 106.0 . . ? C23 C22 H22 106.0 . . ? Si1 C22 H22 106.0 . . ? C22 C23 H23 109.5 . . ? C22 C23 H23A 109.5 . . ? H23 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C25 C24 H24 109.5 . . ? C25 C24 H24A 109.5 . . ? H24 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C24 C25 C26 109.0(3) . . ? C24 C25 Si2 111.8(2) . . ? C26 C25 Si2 113.5(2) . . ? C24 C25 H25 107.4 . . ? C26 C25 H25 107.4 . . ? Si2 C25 H25 107.4 . . ? C25 C26 H26 109.5 . . ? C25 C26 H26A 109.5 . . ? H26 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C28 C27 H27 109.5 . . ? C28 C27 H27A 109.5 . . ? H27 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C27 C28 C29 110.4(3) . . ? C27 C28 Si2 113.8(2) . . ? C29 C28 Si2 114.0(2) . . ? C27 C28 H28 106.0 . . ? C29 C28 H28 106.0 . . ? Si2 C28 H28 106.0 . . ? C28 C29 H29 109.5 . . ? C28 C29 H29A 109.5 . . ? H29 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C31 C30 H30 109.5 . . ? C31 C30 H30A 109.5 . . ? H30 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C32 C31 C30 108.7(3) . . ? C32 C31 Si2 114.5(2) . . ? C30 C31 Si2 116.6(2) . . ? C32 C31 H31 105.4 . . ? C30 C31 H31 105.4 . . ? Si2 C31 H31 105.4 . . ? C31 C32 H32 109.5 . . ? C31 C32 H32A 109.5 . . ? H32 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C5 Ga1 C1 108.72(11) . . ? C5 Ga1 C6 123.33(11) . . ? C1 Ga1 C6 127.87(11) . . ? C1 Si1 C22 108.99(12) . . ? C1 Si1 C19 110.01(13) . . ? C22 Si1 C19 113.77(13) . . ? C1 Si1 C16 113.36(12) . . ? C22 Si1 C16 106.31(13) . . ? C19 Si1 C16 104.39(13) . . ? C5 Si2 C28 111.09(13) . . ? C5 Si2 C25 113.24(12) . . ? C28 Si2 C25 105.69(13) . . ? C5 Si2 C31 109.39(12) . . ? C28 Si2 C31 113.10(13) . . ? C25 Si2 C31 104.16(13) . . ? O3 Li1 O5 93.8(2) . . ? O3 Li1 O1 98.8(2) . . ? O5 Li1 O1 92.8(2) . . ? O3 Li1 O4 77.26(18) . . ? O5 Li1 O4 167.4(3) . . ? O1 Li1 O4 97.3(2) . . ? O3 Li1 O2 165.4(3) . . ? O5 Li1 O2 100.3(2) . . ? O1 Li1 O2 76.80(18) . . ? O4 Li1 O2 89.3(2) . . ? O3 Li1 O6 96.9(2) . . ? O5 Li1 O6 76.81(18) . . ? O1 Li1 O6 161.7(3) . . ? O4 Li1 O6 95.2(2) . . ? O2 Li1 O6 90.16(19) . . ? O1 C33 H33 109.5 . . ? O1 C33 H33A 109.5 . . ? H33 C33 H33A 109.5 . . ? O1 C33 H33B 109.5 . . ? H33 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O1 C34 C35 107.2(3) . . ? O1 C34 H34 110.3 . . ? C35 C34 H34 110.3 . . ? O1 C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? H34 C34 H34A 108.5 . . ? O2 C35 C34 107.9(2) . . ? O2 C35 H35 110.1 . . ? C34 C35 H35 110.1 . . ? O2 C35 H35A 110.1 . . ? C34 C35 H35A 110.1 . . ? H35 C35 H35A 108.4 . . ? O2 C36 H36 109.5 . . ? O2 C36 H36A 109.5 . . ? H36 C36 H36A 109.5 . . ? O2 C36 H36B 109.5 . . ? H36 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O3 C37 H37 109.5 . . ? O3 C37 H37A 109.5 . . ? H37 C37 H37A 109.5 . . ? O3 C37 H37B 109.5 . . ? H37 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O3 C38 C39 107.4(2) . . ? O3 C38 H38 110.2 . . ? C39 C38 H38 110.2 . . ? O3 C38 H38A 110.2 . . ? C39 C38 H38A 110.2 . . ? H38 C38 H38A 108.5 . . ? O4 C39 C38 108.4(2) . . ? O4 C39 H39 110.0 . . ? C38 C39 H39 110.0 . . ? O4 C39 H39A 110.0 . . ? C38 C39 H39A 110.0 . . ? H39 C39 H39A 108.4 . . ? O4 C40 H40 109.5 . . ? O4 C40 H40A 109.5 . . ? H40 C40 H40A 109.5 . . ? O4 C40 H40B 109.5 . . ? H40 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O5 C41 H41 109.5 . . ? O5 C41 H41A 109.5 . . ? H41 C41 H41A 109.5 . . ? O5 C41 H41B 109.5 . . ? H41 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O5 C42 C43 107.4(3) . . ? O5 C42 H42 110.2 . . ? C43 C42 H42 110.2 . . ? O5 C42 H42A 110.2 . . ? C43 C42 H42A 110.2 . . ? H42 C42 H42A 108.5 . . ? O6 C43 C42 108.0(2) . . ? O6 C43 H43 110.1 . . ? C42 C43 H43 110.1 . . ? O6 C43 H43A 110.1 . . ? C42 C43 H43A 110.1 . . ? H43 C43 H43A 108.4 . . ? O6 C44 H44 109.5 . . ? O6 C44 H44A 109.5 . . ? H44 C44 H44A 109.5 . . ? O6 C44 H44B 109.5 . . ? H44 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C34 O1 C33 112.7(2) . . ? C34 O1 Li1 111.1(2) . . ? C33 O1 Li1 129.0(2) . . ? C35 O2 C36 111.6(2) . . ? C35 O2 Li1 110.7(2) . . ? C36 O2 Li1 124.2(2) . . ? C38 O3 C37 110.8(2) . . ? C38 O3 Li1 112.4(2) . . ? C37 O3 Li1 127.1(2) . . ? C40 O4 C39 112.0(2) . . ? C40 O4 Li1 129.3(2) . . ? C39 O4 Li1 113.5(2) . . ? C42 O5 C41 112.6(2) . . ? C42 O5 Li1 114.2(2) . . ? C41 O5 Li1 129.0(2) . . ? C43 O6 C44 110.7(2) . . ? C43 O6 Li1 105.4(2) . . ? C44 O6 Li1 119.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si1 C1 C2 C3 179.7(2) . . . . ? Ga1 C1 C2 C3 0.5(4) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 1.1(5) . . . . ? C3 C4 C5 Si2 -179.3(2) . . . . ? C3 C4 C5 Ga1 -0.7(4) . . . . ? C11 C6 C7 C8 2.2(4) . . . . ? Ga1 C6 C7 C8 -173.4(2) . . . . ? C11 C6 C7 C12 -177.9(3) . . . . ? Ga1 C6 C7 C12 6.5(4) . . . . ? C6 C7 C8 C9 -1.5(4) . . . . ? C12 C7 C8 C9 178.6(3) . . . . ? C7 C8 C9 C10 0.0(4) . . . . ? C7 C8 C9 C13 -177.6(3) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? C13 C9 C10 C11 178.3(3) . . . . ? C9 C10 C11 C6 0.0(4) . . . . ? C9 C10 C11 C14 -179.3(3) . . . . ? C7 C6 C11 C10 -1.5(4) . . . . ? Ga1 C6 C11 C10 174.2(2) . . . . ? C7 C6 C11 C14 177.9(3) . . . . ? Ga1 C6 C11 C14 -6.4(4) . . . . ? C2 C1 Si1 C22 161.2(2) . . . . ? Ga1 C1 Si1 C22 -19.7(2) . . . . ? C2 C1 Si1 C19 35.8(2) . . . . ? Ga1 C1 Si1 C19 -145.05(17) . . . . ? C2 C1 Si1 C16 -80.6(2) . . . . ? Ga1 C1 Si1 C16 98.50(19) . . . . ? C4 C5 Si2 C28 163.6(2) . . . . ? Ga1 C5 Si2 C28 -14.7(2) . . . . ? C4 C5 Si2 C25 -77.6(2) . . . . ? Ga1 C5 Si2 C25 104.0(2) . . . . ? C4 C5 Si2 C31 38.1(2) . . . . ? Ga1 C5 Si2 C31 -140.27(18) . . . . ? C27 C28 Si2 C5 169.9(2) . . . . ? C29 C28 Si2 C5 -62.3(2) . . . . ? C27 C28 Si2 C25 46.7(2) . . . . ? C29 C28 Si2 C25 174.5(2) . . . . ? C27 C28 Si2 C31 -66.6(2) . . . . ? C29 C28 Si2 C31 61.1(2) . . . . ? O1 C34 C35 O2 56.2(4) . . . . ? O3 C38 C39 O4 -48.8(3) . . . . ? O5 C42 C43 O6 57.9(3) . . . . ? C35 C34 O1 C33 158.7(3) . . . . ? C35 C34 O1 Li1 -48.1(3) . . . . ? C34 C35 O2 C36 -179.8(3) . . . . ? C34 C35 O2 Li1 -37.0(3) . . . . ? C39 C38 O3 C37 -165.7(2) . . . . ? C39 C38 O3 Li1 45.7(3) . . . . ? C38 C39 O4 C40 -172.5(3) . . . . ? C38 C39 O4 Li1 30.5(3) . . . . ? C43 C42 O5 C41 166.3(2) . . . . ? C43 C42 O5 Li1 -34.4(3) . . . . ? C42 C43 O6 C44 178.5(2) . . . . ? C42 C43 O6 Li1 -51.1(3) . . . . ? _refine_diff_density_max 0.929 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.107 _shelxl_version_number 2013-4 _shelx_res_file ; TITL REM Yadorkari-X generated CELL 0.71075 13.0005 28.9375 13.9637 90.0000 108.4113 90.0000 ZERR 4.0 0.0021 0.0048 0.0024 0.0000 0.0021 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H Li O Si Ga UNIT 176 344 4 24 8 4 SIZE 0.21 0.06 0.02 TEMP -180.0 L.S. 100 FMAP 2 PLAN -25 ACTA CONF BOND $H MERG 2 OMIT -10.000000 55.000000 WGHT 0.080200 1.730000 FVAR 3.87002 C1 1 0.608092 0.344310 0.911977 11.00000 0.01805 0.01249 = 0.01941 -0.00132 0.00445 -0.00028 C2 1 0.660627 0.315084 0.993641 11.00000 0.01871 0.01907 = 0.01713 -0.00337 0.00766 -0.00301 AFIX 43 H2 2 0.626199 0.311988 1.044035 11.00000 -1.20000 AFIX 0 C3 1 0.757440 0.289881 1.010297 11.00000 0.01900 0.01506 = 0.01692 0.00162 0.00336 -0.00089 AFIX 43 H3 2 0.780912 0.272312 1.070798 11.00000 -1.20000 AFIX 0 C4 1 0.823276 0.287776 0.947555 11.00000 0.01709 0.01705 = 0.01935 -0.00028 0.00275 0.00092 AFIX 43 H4 2 0.885196 0.268399 0.970699 11.00000 -1.20000 AFIX 0 C5 1 0.810130 0.310422 0.855120 11.00000 0.01882 0.01708 = 0.01729 -0.00081 0.00612 -0.00226 C6 1 0.642604 0.387486 0.687554 11.00000 0.01748 0.02038 = 0.01955 0.00363 0.00721 0.00447 C7 1 0.566990 0.373279 0.595391 11.00000 0.01719 0.02240 = 0.02123 0.00173 0.00591 0.00278 C8 1 0.549661 0.399204 0.507312 11.00000 0.02102 0.03539 = 0.01847 0.00411 0.00268 0.00828 AFIX 43 H8 2 0.499435 0.388256 0.446226 11.00000 -1.20000 AFIX 0 C9 1 0.603546 0.440385 0.506445 11.00000 0.02713 0.03331 = 0.02820 0.01521 0.01450 0.01345 C10 1 0.676233 0.455287 0.597086 11.00000 0.02525 0.01876 = 0.03560 0.00805 0.01407 0.00360 AFIX 43 H10 2 0.713560 0.483637 0.598592 11.00000 -1.20000 AFIX 0 C11 1 0.696298 0.429800 0.686525 11.00000 0.01982 0.01928 = 0.02583 0.00425 0.00852 0.00291 C12 1 0.501846 0.329079 0.589050 11.00000 0.02368 0.03672 = 0.02413 -0.00277 0.00446 -0.00765 AFIX 137 H12 2 0.529813 0.311891 0.652468 11.00000 -1.50000 H12A 2 0.508270 0.310035 0.533183 11.00000 -1.50000 H12B 2 0.425485 0.336834 0.577414 11.00000 -1.50000 AFIX 0 C13 1 0.581578 0.469518 0.411651 11.00000 0.04270 0.04134 = 0.03443 0.02025 0.01862 0.01641 AFIX 137 H13 2 0.558171 0.449470 0.352118 11.00000 -1.50000 H13A 2 0.647936 0.485850 0.412620 11.00000 -1.50000 H13B 2 0.524449 0.492036 0.409033 11.00000 -1.50000 AFIX 0 C14 1 0.776217 0.449239 0.781872 11.00000 0.03031 0.02023 = 0.03218 0.00202 0.00612 -0.00514 AFIX 137 H14 2 0.841443 0.459800 0.767487 11.00000 -1.50000 H14A 2 0.795884 0.425172 0.833873 11.00000 -1.50000 H14B 2 0.743026 0.475322 0.805939 11.00000 -1.50000 AFIX 0 C15 1 0.364641 0.291585 0.937165 11.00000 0.02907 0.02230 = 0.03042 0.00073 0.01273 -0.00573 AFIX 137 H15 2 0.300417 0.271990 0.910673 11.00000 -1.50000 H15A 2 0.368825 0.302614 1.004649 11.00000 -1.50000 H15B 2 0.429814 0.273654 0.941156 11.00000 -1.50000 AFIX 0 C16 1 0.356636 0.332919 0.866997 11.00000 0.01787 0.02351 = 0.02277 -0.00061 0.00669 0.00176 AFIX 13 H16 2 0.291741 0.351365 0.867439 11.00000 -1.20000 AFIX 0 C17 1 0.336694 0.315536 0.758589 11.00000 0.02950 0.03127 = 0.02431 -0.00330 0.00713 -0.00409 AFIX 137 H17 2 0.397983 0.296386 0.756133 11.00000 -1.50000 H17A 2 0.329360 0.342012 0.713153 11.00000 -1.50000 H17B 2 0.270028 0.297131 0.737383 11.00000 -1.50000 AFIX 0 C18 1 0.385483 0.411014 1.058553 11.00000 0.02602 0.04229 = 0.03670 -0.01668 0.01564 -0.00425 AFIX 137 H18 2 0.392310 0.413489 1.130294 11.00000 -1.50000 H18A 2 0.321939 0.392173 1.024050 11.00000 -1.50000 H18B 2 0.376940 0.441937 1.028436 11.00000 -1.50000 AFIX 0 C19 1 0.487805 0.388190 1.047386 11.00000 0.02243 0.02181 = 0.02613 -0.00314 0.00911 -0.00022 AFIX 13 H19 2 0.494551 0.358041 1.083858 11.00000 -1.20000 AFIX 0 C20 1 0.588520 0.416368 1.107071 11.00000 0.02445 0.03528 = 0.03325 -0.01191 0.00617 0.00272 AFIX 137 H20 2 0.584838 0.447250 1.077366 11.00000 -1.50000 H20A 2 0.654197 0.400615 1.104160 11.00000 -1.50000 H20B 2 0.590442 0.419122 1.177565 11.00000 -1.50000 AFIX 0 C21 1 0.336536 0.443427 0.793269 11.00000 0.03231 0.02599 = 0.03908 0.00949 0.01006 0.01030 AFIX 137 H21 2 0.323499 0.456647 0.853014 11.00000 -1.50000 H21A 2 0.284106 0.418661 0.765756 11.00000 -1.50000 H21B 2 0.328316 0.467563 0.742159 11.00000 -1.50000 AFIX 0 C22 1 0.452008 0.423697 0.822851 11.00000 0.02375 0.02076 = 0.03014 0.00359 0.01099 0.00342 AFIX 13 H22 2 0.461971 0.412129 0.758874 11.00000 -1.20000 AFIX 0 C23 1 0.534792 0.462985 0.860149 11.00000 0.03589 0.02121 = 0.04743 0.00836 0.01577 0.00053 AFIX 137 H23 2 0.527830 0.484998 0.805124 11.00000 -1.50000 H23A 2 0.608263 0.450099 0.882216 11.00000 -1.50000 H23B 2 0.521004 0.478878 0.916860 11.00000 -1.50000 AFIX 0 C24 1 1.093460 0.322636 0.963510 11.00000 0.02366 0.03667 = 0.03196 -0.00390 0.00369 -0.00336 AFIX 137 H24 2 1.162939 0.338766 0.990360 11.00000 -1.50000 H24A 2 1.104685 0.289362 0.975310 11.00000 -1.50000 H24B 2 1.042955 0.333936 0.997513 11.00000 -1.50000 AFIX 0 C25 1 1.046378 0.331749 0.850236 11.00000 0.02060 0.02911 = 0.02666 -0.00177 0.01041 -0.00237 AFIX 13 H25 2 1.099911 0.320033 0.817989 11.00000 -1.20000 AFIX 0 C26 1 1.035895 0.383922 0.832263 11.00000 0.03500 0.02971 = 0.03414 -0.00554 0.01111 -0.01035 AFIX 137 H26 2 0.984784 0.396606 0.864095 11.00000 -1.50000 H26A 2 1.009240 0.390073 0.759551 11.00000 -1.50000 H26B 2 1.106945 0.398515 0.861626 11.00000 -1.50000 AFIX 0 C27 1 0.950947 0.316974 0.601800 11.00000 0.03991 0.04048 = 0.02672 0.00244 0.01948 -0.00282 AFIX 137 H27 2 0.972863 0.285003 0.595549 11.00000 -1.50000 H27A 2 1.013910 0.334764 0.642057 11.00000 -1.50000 H27B 2 0.922093 0.330774 0.534511 11.00000 -1.50000 AFIX 0 C28 1 0.863001 0.317569 0.654042 11.00000 0.02980 0.02123 = 0.02244 0.00056 0.01049 -0.00011 AFIX 13 H28 2 0.840514 0.350598 0.654423 11.00000 -1.20000 AFIX 0 C29 1 0.761386 0.291331 0.589896 11.00000 0.03506 0.03283 = 0.02443 -0.00427 0.00938 0.00275 AFIX 137 H29 2 0.730539 0.307093 0.525004 11.00000 -1.50000 H29A 2 0.707618 0.290543 0.625727 11.00000 -1.50000 H29B 2 0.781404 0.259677 0.578179 11.00000 -1.50000 AFIX 0 C30 1 1.046727 0.220235 0.767454 11.00000 0.03349 0.02725 = 0.05680 -0.00646 0.02476 0.00214 AFIX 137 H30 2 1.068442 0.188476 0.788862 11.00000 -1.50000 H30A 2 1.108963 0.240910 0.793971 11.00000 -1.50000 H30B 2 1.021297 0.221799 0.693566 11.00000 -1.50000 AFIX 0 C31 1 0.955114 0.235142 0.808100 11.00000 0.02187 0.02352 = 0.02570 0.00226 0.00958 0.00407 AFIX 13 H31 2 0.984008 0.230167 0.882709 11.00000 -1.20000 AFIX 0 C32 1 0.860900 0.201070 0.770062 11.00000 0.03296 0.02050 = 0.06286 0.00423 0.02189 0.00140 AFIX 137 H32 2 0.828107 0.204505 0.696892 11.00000 -1.50000 H32A 2 0.806371 0.207458 0.803322 11.00000 -1.50000 H32B 2 0.887912 0.169434 0.785621 11.00000 -1.50000 AFIX 0 GA1 6 0.682007 0.348428 0.812448 11.00000 0.01669 0.01445 = 0.01607 0.00113 0.00476 -0.00003 SI1 5 0.480151 0.372441 0.912616 11.00000 0.01776 0.01565 = 0.01987 0.00036 0.00692 0.00124 SI2 5 0.913581 0.298888 0.791295 11.00000 0.01831 0.01911 = 0.01917 0.00029 0.00781 0.00057 LI1 3 0.525635 0.107930 0.804337 11.00000 0.02387 0.02048 = 0.02600 -0.00239 0.00882 -0.00023 C33 1 0.309962 0.166292 0.787031 11.00000 0.02763 0.02808 = 0.03911 0.00026 0.01020 0.00822 AFIX 137 H33 2 0.231531 0.161069 0.761118 11.00000 -1.50000 H33A 2 0.332540 0.184892 0.738516 11.00000 -1.50000 H33B 2 0.328016 0.182696 0.851632 11.00000 -1.50000 AFIX 0 C34 1 0.331865 0.092799 0.866903 11.00000 0.02626 0.03235 = 0.04317 -0.00076 0.01893 -0.00149 AFIX 23 H34 2 0.252802 0.095555 0.854427 11.00000 -1.20000 H34A 2 0.369830 0.100859 0.938256 11.00000 -1.20000 AFIX 0 C35 1 0.360253 0.044353 0.845122 11.00000 0.02989 0.02864 = 0.04928 0.00063 0.01610 -0.00659 AFIX 23 H35 2 0.342755 0.022329 0.891982 11.00000 -1.20000 H35A 2 0.318178 0.035580 0.775178 11.00000 -1.20000 AFIX 0 C36 1 0.507159 -0.001990 0.838172 11.00000 0.05314 0.02307 = 0.08604 0.00250 0.04182 0.00381 AFIX 137 H36 2 0.494100 -0.024131 0.886170 11.00000 -1.50000 H36A 2 0.584671 -0.001399 0.845614 11.00000 -1.50000 H36B 2 0.465980 -0.011296 0.769227 11.00000 -1.50000 AFIX 0 C37 1 0.542280 0.204243 0.702740 11.00000 0.03861 0.02059 = 0.02717 0.00662 0.00947 0.00591 AFIX 137 H37 2 0.483134 0.224175 0.707473 11.00000 -1.50000 H37A 2 0.516758 0.185074 0.641951 11.00000 -1.50000 H37B 2 0.603082 0.223409 0.699097 11.00000 -1.50000 AFIX 0 C38 1 0.594628 0.201507 0.881060 11.00000 0.03102 0.02205 = 0.02584 -0.00569 0.00442 -0.00167 AFIX 23 H38 2 0.524290 0.210547 0.888925 11.00000 -1.20000 H38A 2 0.636064 0.229914 0.878368 11.00000 -1.20000 AFIX 0 C39 1 0.657148 0.171664 0.967861 11.00000 0.02621 0.02395 = 0.02443 -0.00341 0.00060 -0.00668 AFIX 23 H39 2 0.732756 0.168036 0.967527 11.00000 -1.20000 H39A 2 0.658667 0.186156 1.032517 11.00000 -1.20000 AFIX 0 C40 1 0.650783 0.099053 1.043202 11.00000 0.03895 0.03881 = 0.02726 0.00671 0.00735 0.00289 AFIX 137 H40 2 0.729418 0.097126 1.057143 11.00000 -1.50000 H40A 2 0.619255 0.068025 1.030015 11.00000 -1.50000 H40B 2 0.635258 0.112388 1.101674 11.00000 -1.50000 AFIX 0 C41 1 0.370588 0.094386 0.575939 11.00000 0.02764 0.03481 = 0.02961 -0.00086 0.00115 0.00145 AFIX 137 H41 2 0.373462 0.105159 0.510297 11.00000 -1.50000 H41A 2 0.323242 0.114779 0.599304 11.00000 -1.50000 H41B 2 0.341945 0.062809 0.569272 11.00000 -1.50000 AFIX 0 C42 1 0.552054 0.067892 0.616036 11.00000 0.03483 0.02652 = 0.02706 0.00065 0.01249 0.00750 AFIX 23 H42 2 0.544444 0.074437 0.544536 11.00000 -1.20000 H42A 2 0.538141 0.034597 0.622657 11.00000 -1.20000 AFIX 0 C43 1 0.663205 0.080247 0.681990 11.00000 0.02812 0.02996 = 0.03851 0.00777 0.01852 0.00706 AFIX 23 H43 2 0.717840 0.061301 0.664059 11.00000 -1.20000 H43A 2 0.678177 0.113229 0.672978 11.00000 -1.20000 AFIX 0 C44 1 0.774526 0.081786 0.851217 11.00000 0.02356 0.02557 = 0.04616 0.00362 0.00954 0.00199 AFIX 137 H44 2 0.828502 0.064121 0.830866 11.00000 -1.50000 H44A 2 0.778473 0.073237 0.920197 11.00000 -1.50000 H44B 2 0.789210 0.114899 0.848583 11.00000 -1.50000 AFIX 0 O1 4 0.365126 0.122831 0.801373 11.00000 0.02290 0.02408 = 0.03727 0.00237 0.01180 0.00268 O2 4 0.473164 0.043076 0.857899 11.00000 0.02566 0.01926 = 0.04648 -0.00099 0.01501 -0.00195 O3 4 0.577325 0.174978 0.790406 11.00000 0.02696 0.01807 = 0.02145 -0.00021 0.00607 0.00036 O4 4 0.605129 0.127414 0.957588 11.00000 0.03414 0.02302 = 0.02332 0.00296 0.00435 -0.00350 O5 4 0.477456 0.094987 0.647482 11.00000 0.02201 0.02917 = 0.02771 -0.00366 0.00539 0.00584 O6 4 0.668713 0.071730 0.784182 11.00000 0.01908 0.02342 = 0.03195 0.00276 0.00861 0.00025 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM R1 = 0.0610 for 8770 Fo > 4sig(Fo) and 0.0825 for all 11386 data REM 508 parameters refined using 0 restraints END WGHT 0.0802 1.7375 REM Highest difference peak 0.929, deepest hole -1.138, 1-sigma level 0.107 Q1 1 0.7614 0.3468 0.8187 11.00000 0.05 0.72 Q2 1 0.8153 0.4555 0.6870 11.00000 0.05 0.67 Q3 1 0.9573 0.3485 0.5599 11.00000 0.05 0.67 Q4 1 0.4794 0.3230 0.9061 11.00000 0.05 0.59 Q5 1 0.4816 -0.0679 0.9164 11.00000 0.05 0.55 Q6 1 0.9166 0.3978 0.7919 11.00000 0.05 0.54 Q7 1 0.5969 0.3484 0.8070 11.00000 0.05 0.54 Q8 1 0.8876 0.3728 0.7175 11.00000 0.05 0.54 Q9 1 0.9158 0.0036 0.7910 11.00000 0.05 0.51 Q10 1 1.1594 0.3731 0.4589 11.00000 0.05 0.51 Q11 1 0.4589 0.2991 0.8377 11.00000 0.05 0.47 Q12 1 0.7579 0.2640 0.7179 11.00000 0.05 0.47 Q13 1 1.0262 0.3488 0.4594 11.00000 0.05 0.42 Q14 1 0.3868 0.4030 0.4770 11.00000 0.05 0.39 Q15 1 0.5581 0.3736 0.9245 11.00000 0.05 0.38 Q16 1 0.7816 0.4796 0.6022 11.00000 0.05 0.36 Q17 1 0.6049 0.3470 0.7265 11.00000 0.05 0.36 Q18 1 0.7212 0.2980 0.5855 11.00000 0.05 0.35 Q19 1 0.7758 0.2027 0.7609 11.00000 0.05 0.35 Q20 1 0.6131 0.3919 0.6844 11.00000 0.05 0.35 Q21 1 0.2908 0.3465 1.0100 11.00000 0.05 0.34 Q22 1 0.8472 0.3025 0.8007 11.00000 0.05 0.34 Q23 1 0.7075 0.3479 1.0861 11.00000 0.05 0.34 Q24 1 0.6041 0.2815 0.8031 11.00000 0.05 0.34 Q25 1 0.7616 0.3490 0.8996 11.00000 0.05 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1036715.25 3026.48 15 7 -9 6197.17 1653.98 15 7 -9 6829.92 1735.08 15 -7 -9 4693.53 1807.14 15 7 -8 1614.88 490.23 15 7 -8-1300.13 1455.17 15 -7 -8 2273.22 960.90 15 7 -7 8891.43 5315.71 15 7 -7 9779.93 3308.80 15 -7 -710390.04 2460.79 15 7 -628991.77 3309.63 15 7 -629188.38 3143.21 15 -7 -623609.77 4092.41 15 -7 -5 -632.75 1450.83 15 7 -5 876.08 957.76 15 7 -430211.98 4605.25 15 -7 -435884.28 3695.67 15 7 -3 89.83 1073.18 15 -7 -3 2673.51 1706.83 15 7 -239543.57 3823.56 15 -7 -240158.54 4352.36 15 7 -1 535.12 1436.28 15 -7 -1 1825.78 1396.88 15 7 0 4331.09 1798.20 15 -7 0 6481.79 2880.37 15 7 1 1979.37 1818.36 15 -7 1 920.91 627.90 15 7 2 2330.52 1472.33 15 -7 2 2706.90 2517.28 15 8 -12 4661.06 1511.87 -15 -8 12 3937.99 2190.05 -15 8 12 5182.97 1560.86 15 8 -11 942.34 596.87 -15 -8 11-1280.24 1804.84 -15 8 11 1451.54 1235.16 15 8 -1024720.73 4266.92 15 8 -1028391.24 2630.54 -15 8 1030102.43 4178.52 15 8 -9 6346.13 1636.44 15 8 -9 5629.93 1656.79 15 -8 -9 4621.66 2825.19 15 8 -867390.94 4634.35 15 8 -862711.44 4399.58 15 -8 -859834.07 6453.89 15 8 -7 1042.63 594.44 15 8 -7 2717.96 1144.37 15 -8 -7 197.96 1209.46 15 8 -6 7810.90 2778.56 15 8 -6 9706.01 2702.24 15 -8 -6 7819.06 2920.34 15 -8 -5 1591.09 1617.48 15 8 -5 3445.71 1034.99 15 8 -4-1525.67 1249.50 15 -8 -4 -244.43 1459.61 15 8 -3 2358.39 1983.82 15 -8 -3 4556.20 2281.63 15 -8 -212455.00 5701.47 15 8 -2 8890.61 2166.95 15 8 -1 2222.15 1416.51 15 -8 -1 216.54 1233.02 15 8 022442.17 4390.11 15 -8 024890.55 2098.61 15 8 1 7725.65 3712.80 15 -8 1 7907.48 3592.24 15 9 -1110401.51 3414.36 -15 -9 1110894.14 6196.16 -15 9 1113264.18 3375.86 15 9 -10 942.93 829.22 15 9 -10 2585.61 1383.37 -15 9 10 2071.58 1017.62 15 9 -9 -204.25 973.79 15 9 -9-2284.43 1370.10 15 -9 -9 896.85 964.88 15 9 -8 -342.13 689.48 15 9 -8 442.48 774.56 15 -9 -8 1475.44 827.53 15 9 -7 8471.84 2845.83 15 -9 -715768.57 4619.76 15 9 -719688.96 4849.95 15 9 -610243.47 2438.63 15 9 -6 9689.17 1734.70 15 -9 -6 7642.36 2774.45 15 -9 -520674.17 5035.16 15 9 -520385.53 4501.06 15 9 -4 6547.58 1903.44 15 -9 -4 9195.96 2391.71 15 9 -3 8086.72 2190.74 15 -9 -310577.99 2980.08 15 -9 -2 925.72 1090.75 15 9 -2 -67.01 1181.55 15 9 -111452.54 5111.18 15 -9 -112094.99 4744.85 15 9 0 3562.76 1272.72 15 -9 0 4609.76 2064.68 15 9 122988.81 1713.10 15 -9 122802.06 1787.10 15 10 -11 8296.82 2458.90 -15 -10 11 7128.74 3518.96 -15 10 1110373.43 3277.62 15 10 -10 821.36 646.54 15 10 -10-2226.77 1328.35 -15 10 10 1636.90 699.17 15 10 -916127.36 1833.09 15 10 -9 9797.94 3521.91 15 -10 -9 9176.39 4478.30 15 10 -8 678.07 638.21 15 10 -8 815.55 794.10 15 -10 -8 48.82 511.07 15 10 -720559.56 3133.08 15 -10 -721915.23 1936.93 15 10 -720170.41 4464.83 15 10 -6 7473.34 2370.68 15 -10 -6 6299.15 2284.89 15 10 -5 7327.65 2297.77 15 -10 -5 9541.64 2388.89 15 10 -510292.98 1417.16 15 10 -4-1399.87 1213.40 15 -10 -4 -587.64 926.73 15 10 -3 1955.23 1189.64 15 -10 -3 1018.10 894.37 15 -10 -2 9495.64 2577.75 15 10 -2 5222.27 1884.32 15 10 -125576.31 4894.94 15 -10 -128215.12 3171.32 15 10 0-1738.10 1220.53 15 -10 0 -18.00 1033.09 15 10 141324.37 2193.52 15 -10 136474.57 1640.29 15 11 -11 4170.01 1402.82 -15 -11 11 3314.77 1436.09 15 11 -1016476.45 1508.51 15 11 -1013145.47 5035.15 -15 11 1014658.54 3774.65 15 11 -9 3220.34 1158.65 15 11 -9 3443.49 942.24 15 11 -8 786.68 850.32 15 11 -8 640.14 766.76 15 -11 -8 1607.96 902.37 15 11 -7 780.63 798.24 15 -11 -7 1369.65 951.93 15 11 -7 -484.40 1273.99 15 11 -6 3042.63 943.24 15 11 -6 1199.97 714.24 15 -11 -6 2139.89 855.72 15 11 -538562.74 2690.94 15 11 -539924.36 2877.24 15 -11 -538481.12 4907.85 15 11 -4 55.22 821.43 15 -11 -4 1038.00 1039.78 15 11 -319968.27 3881.46 15 -11 -321407.07 4821.47 15 11 -2 1581.51 1024.65 15 -11 -2 1325.04 918.77 15 11 -1 1314.95 856.18 15 -11 -1-1367.83 1001.53 15 11 0 1585.38 871.97 15 -11 0 50.69 805.10 15 12 -10 3216.99 792.06 15 12 -10 3451.52 1812.44 -15 12 10 3079.43 720.06 15 12 -9 1732.08 909.52 15 12 -9 1484.09 1019.07 -15 12 9 2137.50 954.61 15 12 -817870.40 1094.00 15 12 -820866.38 1779.20 15 -12 -817558.78 3031.43 15 12 -710026.08 3417.66 15 -12 -710353.75 3479.86 15 12 -714508.85 3552.58 15 12 -6 7057.71 2071.73 15 12 -6 4561.28 1705.33 15 -12 -6 5024.84 1450.67 15 12 -5 1268.18 815.77 15 12 -5 211.14 740.89 15 -12 -5 2846.86 1065.30 15 -12 -4 1813.29 907.98 15 12 -4 2136.89 835.46 15 12 -317788.31 4027.74 15 -12 -316676.50 3682.84 15 12 -2 1251.42 940.17 15 -12 -2 1515.65 1174.75 15 12 -1 1537.56 1170.05 15 -12 -1 843.32 1161.39 15 12 0 7598.64 2927.54 15 -12 0 9373.07 3422.61 15 13 -10 556.58 916.79 15 13 -10 1185.38 1038.94 -15 13 10 977.69 805.43 15 13 -9 2527.98 1174.89 15 13 -9 4842.24 1190.41 -15 13 9 2745.27 1381.54 15 13 -8 274.27 650.13 15 13 -8 2531.27 1331.77 15 -13 -8 494.97 537.64 15 13 -7 670.38 687.04 15 -13 -7 753.40 630.65 15 13 -7 1693.44 642.50 15 13 -612139.49 3625.00 15 13 -612531.99 2829.82 15 -13 -613475.6310402.70 15 13 -5 -172.61 769.11 15 13 -5 791.49 956.67 15 -13 -5 -464.14 576.68 15 13 -4 6800.31 1636.14 15 -13 -4 5523.57 1485.56 15 13 -4 5947.17 1628.36 15 13 -3 1523.73 1049.33 15 -13 -3-2534.35 994.89 15 13 -2 8969.07 3652.98 15 -13 -211243.85 2533.64 15 13 -1 7418.12 2347.31 15 -13 -1 4558.99 1885.14 15 13 0 -67.68 1220.95 15 -13 0 337.46 368.89 15 14 -912026.30 4821.57 15 14 -912033.22 4934.40 -15 14 911839.42 5154.16 15 14 -8 5357.98 1500.33 15 14 -8 4393.42 1168.15 15 -14 -8 3789.23 1660.68 15 14 -714902.90 3652.49 15 -14 -718460.18 1103.24 15 14 -721228.30 3694.79 15 14 -618423.25 2815.21 15 -14 -621752.59 4512.49 15 14 -621063.34 3814.96 15 14 -5 -127.50 782.93 15 14 -5 -657.67 1025.46 15 -14 -5 613.71 816.48 15 14 -4 1767.54 607.23 15 -14 -4 1281.13 1211.90 15 14 -4 2375.51 1515.11 15 14 -3 1464.33 1432.33 15 -14 -3 1746.54 983.19 15 14 -212746.99 5480.33 15 -14 -216435.28 3968.92 15 -14 -1 4389.52 1775.96 15 14 -1 4176.65 1702.32 15 15 -8 478.67 1163.44 15 15 -8-1894.63 1286.34 15 -15 -8 375.05 742.82 15 15 -7 1180.86 761.18 15 -15 -7 965.05 641.05 15 15 -7 1115.17 837.99 15 15 -620880.26 1822.35 15 -15 -614859.50 3430.55 15 15 -617481.92 3587.62 15 15 -5 7440.22 2290.36 15 15 -5 9953.35 4379.53 15 -15 -5 8983.94 2981.36 15 15 -420838.63 1835.71 15 -15 -416520.25 4329.94 15 15 -418257.43 4233.23 15 15 -3 9991.89 2132.57 15 -15 -3 8065.55 1997.43 15 15 -2 1666.15 1001.43 15 -15 -2 1015.49 741.20 15 16 -714372.35 3864.88 15 -16 -715820.71 1907.67 15 16 -716211.23 5356.92 15 16 -6 975.99 612.07 15 -16 -6 382.08 614.83 15 16 -6 1271.09 840.75 15 16 -5 2641.53 1015.32 15 16 -5 4379.33 1211.17 15 -16 -5 1675.47 809.10 15 16 -4 1941.83 1026.78 15 -16 -4 1951.66 716.61 15 16 -4 3313.81 1304.00 15 16 -3 957.53 806.61 15 -16 -3 1941.79 745.67 15 17 -6 2173.73 1301.81 15 -17 -6 1771.71 1122.77 15 17 -6 4638.98 1617.42 15 17 -5 1020.48 840.43 15 17 -5 3880.17 1542.77 15 -17 -5 826.63 722.60 15 17 -4 1571.77 705.77 15 -17 -4 565.95 533.23 15 17 -4 329.72 802.94 16 0 -10-1775.10 1417.84 16 0 -9 2692.66 1376.82 16 0 -858645.8442913.98 16 0 -7 -248.12 914.62 16 0 -6 6848.65 2857.23 16 0 -5 742.84 617.09 16 0 -4 1529.26 1343.12 16 0 -3 1106.70 627.28 16 0 -2 7991.71 2650.99 16 0 -1-2387.09 1348.13 16 0 0 251.40 1244.95 16 1 -10 8765.94 5358.43 16 -1 -1010319.48 3282.11 16 1 -9 9922.02 3310.25 16 -1 -9 6747.52 3127.86 16 1 -8 5713.69 2208.65 16 -1 -8 3060.07 1598.50 16 1 -7 2284.92 1487.90 16 -1 -7-1333.64 1265.32 16 1 -6 -155.20 824.72 16 -1 -6 1587.30 1019.07 16 1 -5 771.35 977.18 16 -1 -5 1232.09 1052.83 16 1 -411945.30 2840.56 16 -1 -414106.34 3104.80 16 1 -3 1793.18 1879.76 16 -1 -3 2557.89 1630.59 16 1 -2-1963.87 1436.86 16 -1 -2 256.10 745.20 16 1 -1 496.89 1129.62 16 -1 -1 -614.27 803.95 16 1 023107.38 1595.33 16 -1 021708.59 1835.16 16 2 -10-1483.61 1431.83 16 -2 -10 -297.62 1406.28 16 2 -9 -57.87 1604.36 16 -2 -9 -738.27 1396.16 16 2 -8 3915.81 1740.69 16 -2 -8 3598.62 1608.95 16 2 -720255.77 3988.02 16 -2 -716645.81 5366.85 16 2 -6 1636.18 1100.54 16 -2 -6 2007.08 819.15 16 2 -5 8454.08 1840.82 16 -2 -5 8600.42 3480.65 16 2 -4 2563.20 1478.16 16 -2 -4 1594.83 1035.96 16 2 -316129.69 6796.80 16 -2 -316188.91 5451.79 16 -2 -2 2282.76 1349.14 16 2 -2 2172.27 1234.79 16 2 -1-3137.05 1500.58 16 -2 -1 469.70 1041.02 16 3 -10 -280.89 1339.93 16 -3 -10 226.94 906.35 16 3 -932919.77 2764.19 16 -3 -930404.41 3989.85 16 3 -8-1944.01 1626.25 16 -3 -8 1785.81 906.68 16 3 -7 4428.03 2074.89 16 -3 -7 6143.34 2000.51 16 3 -6 1726.26 1009.42 16 -3 -6 749.76 737.32 16 3 -5 1121.33 620.81 16 -3 -5 804.72 970.64 16 3 -4 1445.13 1232.03 16 -3 -4 1235.87 1644.64 16 3 -3 2313.29 1684.70 16 -3 -3 6633.87 2758.40 16 3 -2 4111.33 1394.97 16 -3 -2 6165.21 4975.12 16 3 -111909.71 4239.74 16 -3 -1 9712.61 4596.04 16 4 -10 303.48 793.07 16 -4 -10-2294.90 1597.36 16 -4 -9 6711.93 2954.70 16 4 -822545.86 5405.87 16 -4 -826554.08 4016.01 16 4 -710275.14 4067.28 16 -4 -717687.37 4107.95 16 4 -6 6995.92 2639.41 16 -4 -6 8337.36 3072.64 16 -4 -5 6843.08 3688.00 16 4 -5 6430.31 2655.82 16 4 -4 -214.64 1682.75 16 -4 -4 458.28 784.63 16 4 -3 8823.13 5182.14 16 -4 -310469.84 3826.40 16 -4 -2 -966.57 1611.64 16 4 -2 -102.88 900.82 16 4 -1 2563.83 1428.00 16 -4 -1 1978.23 1320.38 16 5 -10 4836.38 2321.27 16 5 -10 5186.64 2669.14 16 -5 -10 5381.42 2499.30 16 5 -9 1752.93 1555.95 16 -5 -9 2329.44 1580.48 16 5 -8 6327.97 3131.29 16 -5 -812539.44 4043.73 16 5 -731146.01 4835.50 16 -5 -730773.98 5609.36 16 5 -6 316.73 1295.16 16 -5 -6 295.08 894.81 16 -5 -5 7705.86 2760.44 16 5 -5 6159.21 5283.21 16 5 -420543.12 3518.25 16 -5 -428225.82 7048.43 16 5 -3 2157.28 2160.79 16 -5 -3 4210.77 2358.91 16 -5 -2 5723.94 2378.60 16 5 -2 6480.80 2737.26 16 5 -1 2821.45 1795.86 16 -5 -1 2959.53 1626.00 16 6 -10 -426.05 785.75 16 6 -10 1409.02 920.54 16 6 -9 947.56 1252.91 16 -6 -9 2171.31 1587.10 16 6 -8 4865.29 1578.51 16 -6 -8 1300.30 2394.61 16 6 -7 2221.15 1065.05 16 -6 -7 855.50 1120.93 16 6 -6 2972.74 2136.51 16 -6 -6 6098.09 3449.13 16 -6 -5-1409.05 1542.88 16 6 -5-2330.87 1530.99 16 6 -4 9431.55 2650.62 16 -6 -4 6568.47 3842.58 16 6 -3 3110.50 1839.20 16 -6 -3 1988.93 965.69 16 -6 -2 -180.81 1567.65 16 6 -2 1107.33 805.59 16 6 -1 508.67 1068.59 16 -6 -1 971.60 1411.91 16 7 -9 6917.68 3277.45 16 -7 -9 7332.37 4252.66 16 7 -8 1520.38 1105.74 16 -7 -8 470.51 1214.88 16 7 -7 4457.96 1321.41 16 -7 -7 3627.46 1700.75 16 7 -6 5688.90 1769.58 16 -7 -6 3869.03 3399.35 16 -7 -510371.16 2636.24 16 7 -515422.47 3788.63 16 7 -4 1041.54 841.57 16 -7 -4 1503.28 605.32 16 7 -3 8315.88 2258.27 16 -7 -313842.76 3026.37 16 7 -2 1836.19 1096.77 16 -7 -2 1788.40 883.83 16 8 -9 9192.36 3613.56 16 8 -912459.67 3494.64 16 -8 -9 9746.60 4194.02 16 8 -8 -427.88 1324.49 16 -8 -8 1330.36 849.04 16 8 -718967.84 4643.25 16 -8 -716000.83 5179.65 16 8 -6 2269.27 1092.65 16 -8 -6 2383.59 1186.43 16 -8 -5-1275.13 1271.62 16 8 -5 955.01 1071.45 16 8 -4 4527.16 1535.06 16 -8 -4 4280.76 1450.11 16 8 -3 1192.42 921.37 16 -8 -3 1011.18 645.40 16 8 -2 -651.32 1376.75 16 -8 -2 -181.65 832.15 16 9 -8 1013.27 744.41 16 -9 -8 428.06 578.16 16 -9 -7 782.36 974.40 16 9 -7 2347.07 748.84 16 9 -614899.40 4155.77 16 -9 -614809.16 3840.88 16 9 -5 1272.97 763.13 16 -9 -5 271.65 666.81 16 -9 -4 -963.08 1083.44 16 9 -3 4981.88 1442.43 16 -9 -3 5772.57 1703.58 16 9 -2-2134.81 1344.28 16 -9 -2 287.36 808.26 16 10 -8 1702.27 1112.45 16 10 -8 1545.91 895.72 16 -10 -8 458.76 1254.17 16 -10 -7 33.05 1093.66 16 10 -7 2128.69 900.83 16 10 -6 3954.61 1898.13 16 -10 -6 1261.66 1022.14 16 10 -5 8671.05 1998.92 16 -10 -5 6983.78 1891.04 16 10 -4 609.04 1469.65 16 -10 -4 1551.93 914.27 16 10 -3 -762.49 1184.20 16 -10 -3 1375.08 839.58 16 -11 -7 -922.77 1044.43 16 11 -7 2463.16 1022.83 16 11 -6 302.70 1066.19 16 -11 -6 852.36 791.02 16 11 -510079.73 2857.99 16 -11 -512617.52 2251.78 16 -11 -4 2533.75 801.57 16 11 -4 4735.98 1542.94 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 25240 #--------GallaCHD--------# data_GaCHD _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H51 Cl Ga N Si2' _chemical_formula_sum 'C28 H51 Cl Ga N Si2' _chemical_formula_weight 563.04 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1431(16) _cell_length_b 13.6702(14) _cell_length_c 17.1961(19) _cell_angle_alpha 90 _cell_angle_beta 112.4196(13) _cell_angle_gamma 90 _cell_volume 3073.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 9136 _cell_measurement_theta_min 2.3645 _cell_measurement_theta_max 31.1855 _exptl_crystal_description 'Platelet' _exptl_crystal_colour 'Colorless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_F_000 1208 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.170 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 1.077 _shelx_estimated_absorpt_T_min 0.838 _shelx_estimated_absorpt_T_max 0.958 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8922 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Rigaku VariMax Saturn' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 24833 _diffrn_reflns_av_unetI/netI 0.0393 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.116 _diffrn_reflns_theta_max 27.474 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 7001 _reflns_number_gt 5885 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'RIGAKU CrystalClear' _computing_cell_refinement 'RIGAKU CrystalClear' _computing_data_reduction 'RIGAKU CrystalClear' _computing_structure_solution 'SIR-2004' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'Yadokari-XG 2009(Wakita Nemoto et al.)' _computing_publication_material 'Yadokari-XG 2009(Wakita,Nemoto et al.)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.1527P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7001 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.002 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.11560(13) 0.32246(13) 0.65362(10) 0.0130(4) Uani 1 1 d . . . . . C2 C 0.14741(14) 0.41594(13) 0.66098(11) 0.0144(4) Uani 1 1 d . . . . . H43 H 0.1119 0.4593 0.6836 0.017 Uiso 1 1 calc R U . . . C3 C 0.23029(14) 0.46269(13) 0.63908(11) 0.0153(4) Uani 1 1 d . . . . . H51 H 0.2780 0.4939 0.6912 0.018 Uiso 1 1 calc R U . . . H52 H 0.1975 0.5164 0.5994 0.018 Uiso 1 1 calc R U . . . C4 C 0.29559(14) 0.40706(13) 0.60204(11) 0.0146(4) Uani 1 1 d . . . . . H45 H 0.3454 0.4458 0.5917 0.018 Uiso 1 1 calc R U . . . C5 C 0.29545(13) 0.31189(13) 0.58105(10) 0.0125(4) Uani 1 1 d . . . . . C6 C -0.16479(16) 0.38443(16) 0.70348(14) 0.0277(5) Uani 1 1 d . . . . . H1 H -0.2042 0.4450 0.6968 0.041 Uiso 1 1 calc R U . . . H2 H -0.1337 0.3672 0.7632 0.041 Uiso 1 1 calc R U . . . H3 H -0.2103 0.3316 0.6724 0.041 Uiso 1 1 calc R U . . . C7 C -0.08005(14) 0.39948(13) 0.66891(12) 0.0161(4) Uani 1 1 d . . . . . H37 H -0.0381 0.4556 0.7015 0.019 Uiso 1 1 calc R U . . . C8 C -0.12546(16) 0.43372(15) 0.57712(12) 0.0239(4) Uani 1 1 d . . . . . H4 H -0.1720 0.3835 0.5424 0.036 Uiso 1 1 calc R U . . . H5 H -0.0702 0.4447 0.5570 0.036 Uiso 1 1 calc R U . . . H6 H -0.1633 0.4948 0.5733 0.036 Uiso 1 1 calc R U . . . C9 C 0.11220(18) 0.36996(16) 0.85840(12) 0.0284(5) Uani 1 1 d . . . . . H7 H 0.1391 0.3567 0.9190 0.043 Uiso 1 1 calc R U . . . H8 H 0.0577 0.4190 0.8447 0.043 Uiso 1 1 calc R U . . . H9 H 0.1673 0.3946 0.8424 0.043 Uiso 1 1 calc R U . . . C10 C 0.06920(14) 0.27569(14) 0.81032(12) 0.0170(4) Uani 1 1 d . . . . . H38 H 0.0132 0.2531 0.8281 0.020 Uiso 1 1 calc R U . . . C11 C 0.15147(16) 0.19572(16) 0.83603(13) 0.0245(4) Uani 1 1 d . . . . . H10 H 0.2068 0.2143 0.8179 0.037 Uiso 1 1 calc R U . . . H11 H 0.1212 0.1338 0.8093 0.037 Uiso 1 1 calc R U . . . H12 H 0.1789 0.1880 0.8973 0.037 Uiso 1 1 calc R U . . . C12 C -0.09995(18) 0.11470(16) 0.69842(15) 0.0321(5) Uani 1 1 d . . . . . H13 H -0.1560 0.1528 0.7034 0.048 Uiso 1 1 calc R U . . . H14 H -0.0473 0.1036 0.7545 0.048 Uiso 1 1 calc R U . . . H15 H -0.1262 0.0516 0.6718 0.048 Uiso 1 1 calc R U . . . C13 C -0.05303(15) 0.17162(14) 0.64391(12) 0.0202(4) Uani 1 1 d . . . . . H39 H 0.0021 0.1289 0.6395 0.024 Uiso 1 1 calc R U . . . C14 C -0.13479(16) 0.18002(15) 0.55451(13) 0.0251(5) Uani 1 1 d . . . . . H16 H -0.1521 0.1146 0.5299 0.038 Uiso 1 1 calc R U . . . H17 H -0.1083 0.2198 0.5199 0.038 Uiso 1 1 calc R U . . . H18 H -0.1962 0.2111 0.5567 0.038 Uiso 1 1 calc R U . . . C15 C 0.55679(15) 0.39352(15) 0.64637(13) 0.0249(5) Uani 1 1 d . . . . . H19 H 0.6072 0.3414 0.6702 0.037 Uiso 1 1 calc R U . . . H20 H 0.5129 0.3988 0.6786 0.037 Uiso 1 1 calc R U . . . H21 H 0.5923 0.4558 0.6490 0.037 Uiso 1 1 calc R U . . . C16 C 0.49098(14) 0.36940(14) 0.55435(12) 0.0179(4) Uani 1 1 d . . . . . H40 H 0.4497 0.4294 0.5304 0.021 Uiso 1 1 calc R U . . . C17 C 0.56009(16) 0.35413(15) 0.50458(13) 0.0245(4) Uani 1 1 d . . . . . H22 H 0.6081 0.4089 0.5153 0.037 Uiso 1 1 calc R U . . . H23 H 0.5178 0.3508 0.4443 0.037 Uiso 1 1 calc R U . . . H24 H 0.5984 0.2929 0.5224 0.037 Uiso 1 1 calc R U . . . C18 C 0.49062(17) 0.16144(16) 0.69600(13) 0.0314(5) Uani 1 1 d . . . . . H25 H 0.5100 0.0969 0.7221 0.047 Uiso 1 1 calc R U . . . H26 H 0.4347 0.1881 0.7099 0.047 Uiso 1 1 calc R U . . . H27 H 0.5496 0.2055 0.7172 0.047 Uiso 1 1 calc R U . . . C19 C 0.45562(15) 0.15178(14) 0.60061(13) 0.0215(4) Uani 1 1 d . . . . . H41 H 0.4007 0.1009 0.5832 0.026 Uiso 1 1 calc R U . . . C20 C 0.5432(2) 0.11034(17) 0.57815(17) 0.0410(6) Uani 1 1 d . . . . . H28 H 0.6022 0.1543 0.5994 0.061 Uiso 1 1 calc R U . . . H29 H 0.5204 0.1046 0.5169 0.061 Uiso 1 1 calc R U . . . H30 H 0.5626 0.0456 0.6038 0.061 Uiso 1 1 calc R U . . . C21 C 0.27721(18) 0.32116(18) 0.37243(13) 0.0353(6) Uani 1 1 d . . . . . H31 H 0.2528 0.3037 0.3127 0.053 Uiso 1 1 calc R U . . . H32 H 0.3220 0.3785 0.3830 0.053 Uiso 1 1 calc R U . . . H33 H 0.2186 0.3364 0.3875 0.053 Uiso 1 1 calc R U . . . C22 C 0.33661(16) 0.23556(15) 0.42546(13) 0.0219(4) Uani 1 1 d . . . . . H42 H 0.3948 0.2222 0.4075 0.026 Uiso 1 1 calc R U . . . C23 C 0.26962(17) 0.14298(17) 0.40494(14) 0.0335(5) Uani 1 1 d . . . . . H34 H 0.2110 0.1530 0.4212 0.050 Uiso 1 1 calc R U . . . H35 H 0.3101 0.0873 0.4361 0.050 Uiso 1 1 calc R U . . . H36 H 0.2451 0.1297 0.3444 0.050 Uiso 1 1 calc R U . . . C24 C 0.02109(15) 0.28562(14) 0.44231(12) 0.0177(4) Uani 1 1 d . . . . . H46 H 0.0436 0.3494 0.4631 0.021 Uiso 1 1 calc R U . . . C25 C -0.06270(16) 0.27621(15) 0.36786(12) 0.0232(4) Uani 1 1 d . . . . . H47 H -0.0982 0.3324 0.3386 0.028 Uiso 1 1 calc R U . . . C26 C -0.09410(16) 0.18315(16) 0.33661(13) 0.0265(5) Uani 1 1 d . . . . . H48 H -0.1516 0.1744 0.2855 0.032 Uiso 1 1 calc R U . . . C27 C -0.04055(16) 0.10362(15) 0.38087(13) 0.0245(5) Uani 1 1 d . . . . . H49 H -0.0600 0.0393 0.3601 0.029 Uiso 1 1 calc R U . . . C28 C 0.04146(15) 0.11824(14) 0.45557(12) 0.0194(4) Uani 1 1 d . . . . . H50 H 0.0775 0.0630 0.4862 0.023 Uiso 1 1 calc R U . . . Ga1 Ga 0.18690(2) 0.23920(2) 0.60091(2) 0.01189(7) Uani 1 1 d . . . . . Cl1 Cl 0.22509(4) 0.08873(3) 0.65215(3) 0.02067(11) Uani 1 1 d . . . . . Si1 Si 0.01102(4) 0.29141(4) 0.69203(3) 0.01305(11) Uani 1 1 d . . . . . Si2 Si 0.39504(4) 0.26704(4) 0.54151(3) 0.01348(11) Uani 1 1 d . . . . . N1 N 0.07209(11) 0.20812(11) 0.48645(9) 0.0142(3) Uani 1 1 d . . . . . 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 C1 0.0115(8) 0.0181(9) 0.0092(8) 0.0021(7) 0.0038(7) 0.0009(7) C2 0.0146(9) 0.0167(9) 0.0140(9) -0.0016(7) 0.0079(7) 0.0011(7) C3 0.0168(9) 0.0134(9) 0.0170(9) -0.0024(7) 0.0079(8) -0.0011(7) C4 0.0131(9) 0.0174(9) 0.0145(9) -0.0001(7) 0.0065(7) -0.0027(7) C5 0.0131(9) 0.0153(9) 0.0095(8) 0.0006(7) 0.0046(7) -0.0016(7) C6 0.0221(11) 0.0343(12) 0.0312(12) 0.0078(10) 0.0153(10) 0.0095(9) C7 0.0147(9) 0.0162(9) 0.0189(9) 0.0014(7) 0.0079(8) 0.0034(7) C8 0.0240(11) 0.0238(10) 0.0228(10) 0.0068(8) 0.0078(9) 0.0075(8) C9 0.0345(13) 0.0335(12) 0.0147(10) 0.0009(9) 0.0065(9) 0.0003(10) C10 0.0155(9) 0.0229(10) 0.0145(9) 0.0047(8) 0.0080(7) 0.0020(8) C11 0.0215(10) 0.0329(12) 0.0208(10) 0.0090(9) 0.0098(9) 0.0097(9) C12 0.0338(13) 0.0281(12) 0.0384(13) 0.0022(10) 0.0181(11) -0.0127(10) C13 0.0186(10) 0.0189(10) 0.0257(10) 0.0020(8) 0.0112(8) -0.0010(8) C14 0.0216(11) 0.0291(11) 0.0257(11) -0.0062(9) 0.0103(9) -0.0067(9) C15 0.0169(10) 0.0297(11) 0.0298(11) -0.0103(9) 0.0108(9) -0.0082(8) C16 0.0158(9) 0.0185(9) 0.0228(10) -0.0020(8) 0.0112(8) -0.0025(7) C17 0.0246(11) 0.0231(11) 0.0338(12) -0.0026(9) 0.0201(9) -0.0049(9) C18 0.0278(12) 0.0322(12) 0.0285(12) 0.0113(10) 0.0045(10) 0.0050(10) C19 0.0222(10) 0.0175(10) 0.0291(11) 0.0023(8) 0.0147(9) 0.0022(8) C20 0.0436(15) 0.0307(13) 0.0625(18) 0.0147(12) 0.0360(14) 0.0175(11) C21 0.0342(13) 0.0506(15) 0.0170(10) 0.0022(10) 0.0053(9) 0.0020(11) C22 0.0188(10) 0.0333(12) 0.0173(9) -0.0088(8) 0.0110(8) -0.0061(8) C23 0.0295(12) 0.0446(14) 0.0318(12) -0.0213(10) 0.0177(10) -0.0163(11) C24 0.0198(10) 0.0167(9) 0.0168(9) -0.0018(7) 0.0072(8) -0.0002(8) C25 0.0242(11) 0.0285(11) 0.0155(9) 0.0021(8) 0.0062(8) 0.0029(9) C26 0.0221(11) 0.0357(12) 0.0186(10) -0.0087(9) 0.0044(8) -0.0085(9) C27 0.0266(11) 0.0227(10) 0.0252(11) -0.0098(9) 0.0111(9) -0.0092(9) C28 0.0204(10) 0.0161(9) 0.0233(10) -0.0036(8) 0.0104(8) -0.0037(8) Ga1 0.01175(10) 0.01204(11) 0.01301(11) 0.00035(7) 0.00597(8) -0.00053(7) Cl1 0.0206(2) 0.0151(2) 0.0283(3) 0.00722(19) 0.0116(2) 0.00262(18) Si1 0.0116(2) 0.0154(2) 0.0136(2) 0.00235(19) 0.0063(2) 0.00105(19) Si2 0.0132(2) 0.0149(2) 0.0143(2) -0.00238(19) 0.0074(2) -0.00160(19) N1 0.0135(8) 0.0150(8) 0.0152(8) -0.0018(6) 0.0067(6) -0.0026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.345(2) . ? C1 Si1 1.8840(18) . ? C1 Ga1 1.9574(18) . ? C2 C3 1.504(2) . ? C2 H43 0.9500 . ? C3 C4 1.512(2) . ? C3 H51 0.9900 . ? C3 H52 0.9900 . ? C4 C5 1.350(2) . ? C4 H45 0.9500 . ? C5 Si2 1.8848(18) . ? C5 Ga1 1.9649(17) . ? C6 C7 1.541(3) . ? C6 H1 0.9800 . ? C6 H2 0.9800 . ? C6 H3 0.9800 . ? C7 C8 1.533(3) . ? C7 Si1 1.8997(19) . ? C7 H37 1.0000 . ? C8 H4 0.9800 . ? C8 H5 0.9800 . ? C8 H6 0.9800 . ? C9 C10 1.527(3) . ? C9 H7 0.9800 . ? C9 H8 0.9800 . ? C9 H9 0.9800 . ? C10 C11 1.534(3) . ? C10 Si1 1.8932(19) . ? C10 H38 1.0000 . ? C11 H10 0.9800 . ? C11 H11 0.9800 . ? C11 H12 0.9800 . ? C12 C13 1.549(3) . ? C12 H13 0.9800 . ? C12 H14 0.9800 . ? C12 H15 0.9800 . ? C13 C14 1.535(3) . ? C13 Si1 1.901(2) . ? C13 H39 1.0000 . ? C14 H16 0.9800 . ? C14 H17 0.9800 . ? C14 H18 0.9800 . ? C15 C16 1.535(3) . ? C15 H19 0.9800 . ? C15 H20 0.9800 . ? C15 H21 0.9800 . ? C16 C17 1.539(2) . ? C16 Si2 1.9024(19) . ? C16 H40 1.0000 . ? C17 H22 0.9800 . ? C17 H23 0.9800 . ? C17 H24 0.9800 . ? C18 C19 1.528(3) . ? C18 H25 0.9800 . ? C18 H26 0.9800 . ? C18 H27 0.9800 . ? C19 C20 1.539(3) . ? C19 Si2 1.8936(19) . ? C19 H41 1.0000 . ? C20 H28 0.9800 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C21 C22 1.524(3) . ? C21 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C22 C23 1.539(3) . ? C22 Si2 1.896(2) . ? C22 H42 1.0000 . ? C23 H34 0.9800 . ? C23 H35 0.9800 . ? C23 H36 0.9800 . ? C24 N1 1.342(2) . ? C24 C25 1.379(3) . ? C24 H46 0.9500 . ? C25 C26 1.386(3) . ? C25 H47 0.9500 . ? C26 C27 1.377(3) . ? C26 H48 0.9500 . ? C27 C28 1.378(3) . ? C27 H49 0.9500 . ? C28 N1 1.343(2) . ? C28 H50 0.9500 . ? Ga1 N1 2.0624(15) . ? Ga1 Cl1 2.2218(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Si1 117.42(13) . . ? C2 C1 Ga1 112.53(13) . . ? Si1 C1 Ga1 130.04(10) . . ? C1 C2 C3 130.18(16) . . ? C1 C2 H43 114.9 . . ? C3 C2 H43 114.9 . . ? C2 C3 C4 123.47(15) . . ? C2 C3 H51 106.5 . . ? C4 C3 H51 106.5 . . ? C2 C3 H52 106.5 . . ? C4 C3 H52 106.5 . . ? H51 C3 H52 106.5 . . ? C5 C4 C3 131.19(16) . . ? C5 C4 H45 114.4 . . ? C3 C4 H45 114.4 . . ? C4 C5 Si2 119.00(13) . . ? C4 C5 Ga1 111.25(13) . . ? Si2 C5 Ga1 129.73(10) . . ? C7 C6 H1 109.5 . . ? C7 C6 H2 109.5 . . ? H1 C6 H2 109.5 . . ? C7 C6 H3 109.5 . . ? H1 C6 H3 109.5 . . ? H2 C6 H3 109.5 . . ? C8 C7 C6 110.85(16) . . ? C8 C7 Si1 115.93(13) . . ? C6 C7 Si1 112.36(13) . . ? C8 C7 H37 105.6 . . ? C6 C7 H37 105.6 . . ? Si1 C7 H37 105.6 . . ? C7 C8 H4 109.5 . . ? C7 C8 H5 109.5 . . ? H4 C8 H5 109.5 . . ? C7 C8 H6 109.5 . . ? H4 C8 H6 109.5 . . ? H5 C8 H6 109.5 . . ? C10 C9 H7 109.5 . . ? C10 C9 H8 109.5 . . ? H7 C9 H8 109.5 . . ? C10 C9 H9 109.5 . . ? H7 C9 H9 109.5 . . ? H8 C9 H9 109.5 . . ? C9 C10 C11 110.11(17) . . ? C9 C10 Si1 113.97(13) . . ? C11 C10 Si1 111.21(13) . . ? C9 C10 H38 107.1 . . ? C11 C10 H38 107.1 . . ? Si1 C10 H38 107.1 . . ? C10 C11 H10 109.5 . . ? C10 C11 H11 109.5 . . ? H10 C11 H11 109.5 . . ? C10 C11 H12 109.5 . . ? H10 C11 H12 109.5 . . ? H11 C11 H12 109.5 . . ? C13 C12 H13 109.5 . . ? C13 C12 H14 109.5 . . ? H13 C12 H14 109.5 . . ? C13 C12 H15 109.5 . . ? H13 C12 H15 109.5 . . ? H14 C12 H15 109.5 . . ? C14 C13 C12 108.10(17) . . ? C14 C13 Si1 115.04(13) . . ? C12 C13 Si1 114.35(14) . . ? C14 C13 H39 106.2 . . ? C12 C13 H39 106.2 . . ? Si1 C13 H39 106.2 . . ? C13 C14 H16 109.5 . . ? C13 C14 H17 109.5 . . ? H16 C14 H17 109.5 . . ? C13 C14 H18 109.5 . . ? H16 C14 H18 109.5 . . ? H17 C14 H18 109.5 . . ? C16 C15 H19 109.5 . . ? C16 C15 H20 109.5 . . ? H19 C15 H20 109.5 . . ? C16 C15 H21 109.5 . . ? H19 C15 H21 109.5 . . ? H20 C15 H21 109.5 . . ? C15 C16 C17 109.78(16) . . ? C15 C16 Si2 113.76(13) . . ? C17 C16 Si2 114.32(13) . . ? C15 C16 H40 106.1 . . ? C17 C16 H40 106.1 . . ? Si2 C16 H40 106.1 . . ? C16 C17 H22 109.5 . . ? C16 C17 H23 109.5 . . ? H22 C17 H23 109.5 . . ? C16 C17 H24 109.5 . . ? H22 C17 H24 109.5 . . ? H23 C17 H24 109.5 . . ? C19 C18 H25 109.5 . . ? C19 C18 H26 109.5 . . ? H25 C18 H26 109.5 . . ? C19 C18 H27 109.5 . . ? H25 C18 H27 109.5 . . ? H26 C18 H27 109.5 . . ? C18 C19 C20 109.82(19) . . ? C18 C19 Si2 113.54(14) . . ? C20 C19 Si2 114.48(14) . . ? C18 C19 H41 106.1 . . ? C20 C19 H41 106.1 . . ? Si2 C19 H41 106.1 . . ? C19 C20 H28 109.5 . . ? C19 C20 H29 109.5 . . ? H28 C20 H29 109.5 . . ? C19 C20 H30 109.5 . . ? H28 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? C22 C21 H31 109.5 . . ? C22 C21 H32 109.5 . . ? H31 C21 H32 109.5 . . ? C22 C21 H33 109.5 . . ? H31 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? C21 C22 C23 110.09(19) . . ? C21 C22 Si2 112.03(14) . . ? C23 C22 Si2 114.28(14) . . ? C21 C22 H42 106.6 . . ? C23 C22 H42 106.6 . . ? Si2 C22 H42 106.6 . . ? C22 C23 H34 109.5 . . ? C22 C23 H35 109.5 . . ? H34 C23 H35 109.5 . . ? C22 C23 H36 109.5 . . ? H34 C23 H36 109.5 . . ? H35 C23 H36 109.5 . . ? N1 C24 C25 122.51(18) . . ? N1 C24 H46 118.7 . . ? C25 C24 H46 118.7 . . ? C24 C25 C26 118.69(19) . . ? C24 C25 H47 120.7 . . ? C26 C25 H47 120.7 . . ? C27 C26 C25 118.88(19) . . ? C27 C26 H48 120.6 . . ? C25 C26 H48 120.6 . . ? C26 C27 C28 119.40(18) . . ? C26 C27 H49 120.3 . . ? C28 C27 H49 120.3 . . ? N1 C28 C27 122.08(19) . . ? N1 C28 H50 119.0 . . ? C27 C28 H50 119.0 . . ? C1 Ga1 C5 111.17(7) . . ? C1 Ga1 N1 101.81(7) . . ? C5 Ga1 N1 108.74(6) . . ? C1 Ga1 Cl1 116.42(5) . . ? C5 Ga1 Cl1 116.70(5) . . ? N1 Ga1 Cl1 99.88(4) . . ? C1 Si1 C10 108.94(8) . . ? C1 Si1 C7 108.16(8) . . ? C10 Si1 C7 107.17(8) . . ? C1 Si1 C13 110.42(8) . . ? C10 Si1 C13 108.04(9) . . ? C7 Si1 C13 113.97(9) . . ? C5 Si2 C19 108.93(8) . . ? C5 Si2 C22 111.59(8) . . ? C19 Si2 C22 107.60(9) . . ? C5 Si2 C16 108.48(8) . . ? C19 Si2 C16 113.14(9) . . ? C22 Si2 C16 107.12(9) . . ? C24 N1 C28 118.42(17) . . ? C24 N1 Ga1 115.77(12) . . ? C28 N1 Ga1 125.70(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si1 C1 C2 C3 177.89(15) . . . . ? Ga1 C1 C2 C3 -3.2(3) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C3 C4 C5 Si2 -176.49(15) . . . . ? C3 C4 C5 Ga1 2.0(2) . . . . ? N1 C24 C25 C26 -1.4(3) . . . . ? C24 C25 C26 C27 -0.1(3) . . . . ? C25 C26 C27 C28 1.1(3) . . . . ? C26 C27 C28 N1 -0.9(3) . . . . ? C2 C1 Si1 C10 -80.72(16) . . . . ? Ga1 C1 Si1 C10 100.60(12) . . . . ? C2 C1 Si1 C7 35.45(16) . . . . ? Ga1 C1 Si1 C7 -143.23(11) . . . . ? C2 C1 Si1 C13 160.79(14) . . . . ? Ga1 C1 Si1 C13 -17.90(14) . . . . ? C9 C10 Si1 C1 67.12(16) . . . . ? C11 C10 Si1 C1 -58.06(16) . . . . ? C9 C10 Si1 C7 -49.69(16) . . . . ? C11 C10 Si1 C7 -174.86(14) . . . . ? C9 C10 Si1 C13 -172.90(14) . . . . ? C11 C10 Si1 C13 61.92(16) . . . . ? C8 C7 Si1 C1 55.06(16) . . . . ? C6 C7 Si1 C1 -176.05(14) . . . . ? C8 C7 Si1 C10 172.37(14) . . . . ? C6 C7 Si1 C10 -58.74(16) . . . . ? C8 C7 Si1 C13 -68.15(17) . . . . ? C6 C7 Si1 C13 60.74(16) . . . . ? C4 C5 Si2 C19 131.39(15) . . . . ? Ga1 C5 Si2 C19 -46.81(14) . . . . ? C4 C5 Si2 C22 -109.95(15) . . . . ? Ga1 C5 Si2 C22 71.84(13) . . . . ? C4 C5 Si2 C16 7.83(17) . . . . ? Ga1 C5 Si2 C16 -170.37(11) . . . . ? C18 C19 Si2 C5 -49.40(17) . . . . ? C20 C19 Si2 C5 -176.61(16) . . . . ? C18 C19 Si2 C22 -170.53(15) . . . . ? C20 C19 Si2 C22 62.26(19) . . . . ? C18 C19 Si2 C16 71.33(17) . . . . ? C20 C19 Si2 C16 -55.87(19) . . . . ? C21 C22 Si2 C5 55.42(17) . . . . ? C23 C22 Si2 C5 -70.67(17) . . . . ? C21 C22 Si2 C19 174.87(15) . . . . ? C23 C22 Si2 C19 48.78(18) . . . . ? C21 C22 Si2 C16 -63.18(17) . . . . ? C23 C22 Si2 C16 170.73(15) . . . . ? C25 C24 N1 C28 1.6(3) . . . . ? C25 C24 N1 Ga1 -174.83(15) . . . . ? C27 C28 N1 C24 -0.5(3) . . . . ? C27 C28 N1 Ga1 175.58(15) . . . . ? _refine_diff_density_max 0.335 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.095 _shelxl_version_number 2013-4 _shelx_res_file ; TITL REM Yadorkari-X generated CELL 0.71075 14.1431 13.6702 17.1961 90.0000 112.4196 90.0000 ZERR 4.0 0.0016 0.0014 0.0019 0.0000 0.0013 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H N Si Cl Ga UNIT 112 204 4 8 4 4 SIZE 0.17 0.17 0.04 TEMP -180.0 L.S. 14 FMAP 2 PLAN -25 ACTA CONF WPDB -1 BOND $H MERG 2 OMIT -10.000000 55.000000 WGHT 0.044100 0.152700 FVAR 3.06183 C1 1 0.115598 0.322465 0.653622 11.00000 0.01148 0.01807 = 0.00916 0.00207 0.00376 0.00093 C2 1 0.147411 0.415939 0.660979 11.00000 0.01464 0.01669 = 0.01404 -0.00159 0.00793 0.00111 AFIX 43 H43 2 0.111929 0.459279 0.683572 11.00000 -1.20000 AFIX 0 C3 1 0.230291 0.462690 0.639085 11.00000 0.01684 0.01340 = 0.01701 -0.00237 0.00788 -0.00106 AFIX 23 H51 2 0.278017 0.493870 0.691249 11.00000 -1.20000 H52 2 0.197488 0.516440 0.599356 11.00000 -1.20000 AFIX 0 C4 1 0.295589 0.407064 0.602043 11.00000 0.01311 0.01738 = 0.01446 -0.00010 0.00649 -0.00269 AFIX 43 H45 2 0.345362 0.445814 0.591750 11.00000 -1.20000 AFIX 0 C5 1 0.295452 0.311888 0.581053 11.00000 0.01308 0.01528 = 0.00946 0.00064 0.00463 -0.00164 C6 1 -0.164790 0.384434 0.703482 11.00000 0.02207 0.03430 = 0.03124 0.00785 0.01533 0.00948 AFIX 137 H1 2 -0.204204 0.444991 0.696806 11.00000 -1.50000 H2 2 -0.133748 0.367190 0.763248 11.00000 -1.50000 H3 2 -0.210300 0.331553 0.672371 11.00000 -1.50000 AFIX 0 C7 1 -0.080048 0.399480 0.668913 11.00000 0.01468 0.01617 = 0.01886 0.00136 0.00792 0.00345 AFIX 13 H37 2 -0.038090 0.455556 0.701490 11.00000 -1.20000 AFIX 0 C8 1 -0.125455 0.433720 0.577122 11.00000 0.02399 0.02381 = 0.02283 0.00676 0.00778 0.00753 AFIX 137 H4 2 -0.171960 0.383507 0.542427 11.00000 -1.50000 H5 2 -0.070170 0.444746 0.556990 11.00000 -1.50000 H6 2 -0.163265 0.494796 0.573264 11.00000 -1.50000 AFIX 0 C9 1 0.112201 0.369956 0.858403 11.00000 0.03451 0.03353 = 0.01473 0.00088 0.00651 0.00033 AFIX 137 H7 2 0.139147 0.356746 0.918988 11.00000 -1.50000 H8 2 0.057744 0.419036 0.844684 11.00000 -1.50000 H9 2 0.167317 0.394599 0.842403 11.00000 -1.50000 AFIX 0 C10 1 0.069198 0.275691 0.810317 11.00000 0.01548 0.02293 = 0.01451 0.00474 0.00797 0.00203 AFIX 13 H38 2 0.013246 0.253085 0.828110 11.00000 -1.20000 AFIX 0 C11 1 0.151467 0.195722 0.836029 11.00000 0.02146 0.03291 = 0.02085 0.00903 0.00985 0.00970 AFIX 137 H10 2 0.206783 0.214317 0.817876 11.00000 -1.50000 H11 2 0.121249 0.133795 0.809332 11.00000 -1.50000 H12 2 0.178941 0.187952 0.897309 11.00000 -1.50000 AFIX 0 C12 1 -0.099948 0.114699 0.698416 11.00000 0.03379 0.02807 = 0.03838 0.00224 0.01809 -0.01266 AFIX 137 H13 2 -0.156045 0.152846 0.703383 11.00000 -1.50000 H14 2 -0.047279 0.103594 0.754514 11.00000 -1.50000 H15 2 -0.126203 0.051639 0.671841 11.00000 -1.50000 AFIX 0 C13 1 -0.053034 0.171624 0.643905 11.00000 0.01859 0.01889 = 0.02570 0.00204 0.01118 -0.00101 AFIX 13 H39 2 0.002142 0.128945 0.639513 11.00000 -1.20000 AFIX 0 C14 1 -0.134790 0.180018 0.554506 11.00000 0.02164 0.02914 = 0.02574 -0.00623 0.01032 -0.00666 AFIX 137 H16 2 -0.152091 0.114591 0.529855 11.00000 -1.50000 H17 2 -0.108292 0.219758 0.519877 11.00000 -1.50000 H18 2 -0.196167 0.211062 0.556729 11.00000 -1.50000 AFIX 0 C15 1 0.556792 0.393524 0.646370 11.00000 0.01695 0.02975 = 0.02976 -0.01027 0.01084 -0.00824 AFIX 137 H19 2 0.607219 0.341447 0.670192 11.00000 -1.50000 H20 2 0.512919 0.398753 0.678628 11.00000 -1.50000 H21 2 0.592261 0.455779 0.649047 11.00000 -1.50000 AFIX 0 C16 1 0.490984 0.369395 0.554352 11.00000 0.01578 0.01847 = 0.02282 -0.00203 0.01121 -0.00252 AFIX 13 H40 2 0.449715 0.429416 0.530425 11.00000 -1.20000 AFIX 0 C17 1 0.560087 0.354134 0.504578 11.00000 0.02457 0.02309 = 0.03375 -0.00262 0.02008 -0.00494 AFIX 137 H22 2 0.608088 0.408921 0.515275 11.00000 -1.50000 H23 2 0.517811 0.350829 0.444329 11.00000 -1.50000 H24 2 0.598356 0.292934 0.522439 11.00000 -1.50000 AFIX 0 C18 1 0.490621 0.161438 0.696002 11.00000 0.02783 0.03220 = 0.02854 0.01134 0.00451 0.00502 AFIX 137 H25 2 0.509989 0.096923 0.722094 11.00000 -1.50000 H26 2 0.434684 0.188083 0.709928 11.00000 -1.50000 H27 2 0.549641 0.205505 0.717175 11.00000 -1.50000 AFIX 0 C19 1 0.455620 0.151777 0.600609 11.00000 0.02224 0.01747 = 0.02915 0.00227 0.01474 0.00225 AFIX 13 H41 2 0.400655 0.100908 0.583246 11.00000 -1.20000 AFIX 0 C20 1 0.543170 0.110335 0.578146 11.00000 0.04363 0.03070 = 0.06254 0.01471 0.03595 0.01750 AFIX 137 H28 2 0.602228 0.154348 0.599398 11.00000 -1.50000 H29 2 0.520426 0.104632 0.516899 11.00000 -1.50000 H30 2 0.562608 0.045635 0.603837 11.00000 -1.50000 AFIX 0 C21 1 0.277214 0.321157 0.372428 11.00000 0.03420 0.05058 = 0.01701 0.00217 0.00528 0.00204 AFIX 137 H31 2 0.252805 0.303681 0.312710 11.00000 -1.50000 H32 2 0.321998 0.378476 0.382973 11.00000 -1.50000 H33 2 0.218640 0.336363 0.387498 11.00000 -1.50000 AFIX 0 C22 1 0.336615 0.235558 0.425456 11.00000 0.01881 0.03333 = 0.01735 -0.00885 0.01097 -0.00613 AFIX 13 H42 2 0.394831 0.222204 0.407525 11.00000 -1.20000 AFIX 0 C23 1 0.269616 0.142976 0.404936 11.00000 0.02947 0.04464 = 0.03176 -0.02125 0.01771 -0.01635 AFIX 137 H34 2 0.211035 0.152984 0.421214 11.00000 -1.50000 H35 2 0.310084 0.087284 0.436097 11.00000 -1.50000 H36 2 0.245070 0.129715 0.344431 11.00000 -1.50000 AFIX 0 C24 1 0.021093 0.285615 0.442309 11.00000 0.01984 0.01667 = 0.01678 -0.00177 0.00716 -0.00024 AFIX 43 H46 2 0.043563 0.349390 0.463135 11.00000 -1.20000 AFIX 0 C25 1 -0.062700 0.276210 0.367857 11.00000 0.02419 0.02851 = 0.01552 0.00214 0.00620 0.00293 AFIX 43 H47 2 -0.098191 0.332387 0.338572 11.00000 -1.20000 AFIX 0 C26 1 -0.094100 0.183150 0.336610 11.00000 0.02214 0.03569 = 0.01864 -0.00873 0.00440 -0.00850 AFIX 43 H48 2 -0.151598 0.174415 0.285517 11.00000 -1.20000 AFIX 0 C27 1 -0.040555 0.103624 0.380871 11.00000 0.02659 0.02266 = 0.02522 -0.00980 0.01109 -0.00924 AFIX 43 H49 2 -0.059967 0.039250 0.360107 11.00000 -1.20000 AFIX 0 C28 1 0.041462 0.118241 0.455571 11.00000 0.02043 0.01614 = 0.02331 -0.00362 0.01035 -0.00368 AFIX 43 H50 2 0.077478 0.062997 0.486196 11.00000 -1.20000 AFIX 0 GA1 6 0.186898 0.239200 0.600911 11.00000 0.01175 0.01204 = 0.01301 0.00035 0.00597 -0.00053 CL1 5 0.225087 0.088727 0.652154 11.00000 0.02059 0.01515 = 0.02832 0.00722 0.01162 0.00262 SI1 4 0.011016 0.291407 0.692027 11.00000 0.01155 0.01542 = 0.01357 0.00235 0.00633 0.00105 SI2 4 0.395043 0.267045 0.541512 11.00000 0.01322 0.01486 = 0.01431 -0.00238 0.00744 -0.00160 N1 3 0.072086 0.208120 0.486446 11.00000 0.01350 0.01500 = 0.01520 -0.00183 0.00671 -0.00263 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM R1 = 0.0351 for 5885 Fo > 4sig(Fo) and 0.0436 for all 7001 data REM 310 parameters refined using 0 restraints END WGHT 0.0441 0.1527 REM Highest difference peak 0.335, deepest hole -0.650, 1-sigma level 0.095 Q1 1 0.0601 0.3455 0.5516 11.00000 0.05 0.33 Q2 1 0.0587 0.2984 0.7624 11.00000 0.05 0.33 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