data_1b _audit_creation_method SHELXL-2014/6 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H25 Al0.84 Ga1.16 N3' _chemical_formula_weight 266.85 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' 'Al' 'Al' 0.0645 0.0514 '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 orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.2256(8) _cell_length_b 12.9136(15) _cell_length_c 17.444(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1402.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_F_000 564 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 2.286 _shelx_estimated_absorpt_T_min 0.462 _shelx_estimated_absorpt_T_max 0.658 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13109 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.962 _diffrn_reflns_theta_max 25.040 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.974 _reflns_number_total 2482 _reflns_number_gt 2334 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.698 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 0.971 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _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^)+(0.0271P)^2^+0.2580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.435(15) _chemical_absolute_configuration ? _refine_ls_number_reflns 2482 _refine_ls_number_parameters 142 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0504 _refine_ls_wR_factor_gt 0.0490 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.002 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 Al1 Al 0.2398(12) 0.4290(9) 0.0350(5) 0.0260(8) Uani 0.844(2) 1 d D . P A 1 Ga1 Ga 0.254(3) 0.4339(18) 0.0443(11) 0.0260(8) Uani 0.156(2) 1 d D . P A 2 H1' H 0.014(3) 0.440(2) 0.0373(16) 0.031 Uiso 1 1 d D U . . . H2' H 0.366(4) 0.3612(19) -0.0094(15) 0.031 Uiso 1 1 d D U . . . Ga2 Ga 0.20888(6) 0.61248(3) 0.17694(2) 0.04468(13) Uani 1 1 d D . . . . H3' H 0.357(4) 0.620(2) 0.2395(14) 0.054 Uiso 1 1 d D U . . . H4' H 0.154(4) 0.7110(17) 0.1457(17) 0.054 Uiso 1 1 d D U . . . H5' H 0.027(4) 0.551(2) 0.1970(16) 0.054 Uiso 1 1 d D U . . . N1 N 0.3043(4) 0.55591(18) -0.04642(13) 0.0375(5) Uani 1 1 d . . . . . N2 N 0.4030(4) 0.52312(18) 0.10749(14) 0.0314(5) Uani 1 1 d . . . . . N3 N 0.2682(4) 0.32177(17) 0.13327(12) 0.0328(5) Uani 1 1 d . . . . . C1 C 0.1045(6) 0.5938(3) -0.0822(2) 0.0544(9) Uani 1 1 d . . . . . H1A H 0.1380 0.6511 -0.1170 0.082 Uiso 1 1 calc R U . . . H1B H 0.0059 0.6180 -0.0422 0.082 Uiso 1 1 calc R U . . . H1C H 0.0369 0.5375 -0.1110 0.082 Uiso 1 1 calc R U . . . C2 C 0.4517(7) 0.5194(3) -0.1073(2) 0.0579(10) Uani 1 1 d . . . . . H2A H 0.4782 0.5757 -0.1437 0.087 Uiso 1 1 calc R U . . . H2B H 0.3865 0.4607 -0.1342 0.087 Uiso 1 1 calc R U . . . H2C H 0.5879 0.4976 -0.0842 0.087 Uiso 1 1 calc R U . . . C3 C 0.4086(5) 0.6396(2) -0.00213(18) 0.0415(7) Uani 1 1 d . . . . . H3A H 0.2980 0.6861 0.0197 0.050 Uiso 1 1 calc R U . . . H3B H 0.5020 0.6811 -0.0363 0.050 Uiso 1 1 calc R U . . . C4 C 0.5411(5) 0.5931(3) 0.06152(18) 0.0419(7) Uani 1 1 d . . . . . H4A H 0.6631 0.5537 0.0397 0.050 Uiso 1 1 calc R U . . . H4B H 0.5996 0.6487 0.0945 0.050 Uiso 1 1 calc R U . . . C5 C 0.5383(5) 0.4558(3) 0.15634(18) 0.0406(8) Uani 1 1 d . . . . . H5A H 0.6099 0.4976 0.1964 0.049 Uiso 1 1 calc R U . . . H5B H 0.6504 0.4219 0.1249 0.049 Uiso 1 1 calc R U . . . C6 C 0.3965(5) 0.3749(2) 0.19306(15) 0.0377(7) Uani 1 1 d . . . . . H6A H 0.4863 0.3238 0.2207 0.045 Uiso 1 1 calc R U . . . H6B H 0.2994 0.4082 0.2306 0.045 Uiso 1 1 calc R U . . . C7 C 0.0556(6) 0.2903(3) 0.16437(19) 0.0485(8) Uani 1 1 d . . . . . H7A H 0.0765 0.2429 0.2076 0.073 Uiso 1 1 calc R U . . . H7B H -0.0273 0.2555 0.1242 0.073 Uiso 1 1 calc R U . . . H7C H -0.0224 0.3518 0.1818 0.073 Uiso 1 1 calc R U . . . C8 C 0.3810(6) 0.2271(2) 0.1066(2) 0.0518(9) Uani 1 1 d . . . . . H8A H 0.3847 0.1761 0.1482 0.078 Uiso 1 1 calc R U . . . H8B H 0.5281 0.2449 0.0916 0.078 Uiso 1 1 calc R U . . . H8C H 0.3046 0.1979 0.0626 0.078 Uiso 1 1 calc R U . . . 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 Al1 0.0313(10) 0.0283(11) 0.019(2) -0.0054(13) -0.0038(11) -0.0005(9) Ga1 0.0313(10) 0.0283(11) 0.019(2) -0.0054(13) -0.0038(11) -0.0005(9) Ga2 0.0560(2) 0.04134(19) 0.03668(18) -0.01090(15) 0.00271(16) 0.00680(16) N1 0.0494(14) 0.0347(12) 0.0284(11) -0.0009(10) 0.0043(12) 0.0010(12) N2 0.0296(12) 0.0326(13) 0.0320(13) -0.0006(10) -0.0034(10) -0.0003(10) N3 0.0374(14) 0.0311(11) 0.0299(12) -0.0004(9) -0.0014(11) 0.0032(11) C1 0.070(2) 0.050(2) 0.0428(19) 0.0071(16) -0.0139(16) 0.0044(18) C2 0.083(3) 0.051(2) 0.040(2) 0.0007(17) 0.0231(19) 0.002(2) C3 0.0526(19) 0.0346(16) 0.0374(17) 0.0024(14) 0.0062(14) -0.0099(13) C4 0.0395(16) 0.0421(19) 0.0441(18) 0.0002(15) 0.0036(13) -0.0095(14) C5 0.0326(15) 0.0443(19) 0.0449(19) 0.0005(14) -0.0119(13) 0.0032(14) C6 0.0437(16) 0.0408(18) 0.0285(15) 0.0019(13) -0.0095(12) 0.0077(14) C7 0.0475(19) 0.054(2) 0.044(2) 0.0113(17) 0.0041(15) -0.0074(16) C8 0.073(2) 0.0327(17) 0.0501(19) 0.0002(15) -0.0026(18) 0.0157(16) _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 Al1 N2 2.027(9) . ? Al1 N1 2.205(12) . ? Al1 N3 2.211(11) . ? Al1 H1' 1.41(2) . ? Al1 H2' 1.41(2) . ? Ga1 N2 1.85(2) . ? Ga1 N3 2.12(2) . ? Ga1 N1 2.25(2) . ? Ga1 H1' 1.50(3) . ? Ga1 H2' 1.50(2) . ? Ga2 N2 2.064(2) . ? Ga2 H3' 1.43(2) . ? Ga2 H4' 1.43(2) . ? Ga2 H5' 1.43(2) . ? N1 C1 1.475(4) . ? N1 C3 1.479(4) . ? N1 C2 1.480(4) . ? N2 C5 1.480(4) . ? N2 C4 1.482(4) . ? N3 C6 1.482(4) . ? N3 C8 1.484(4) . ? N3 C7 1.487(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.508(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.509(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 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 N2 Al1 N1 82.3(4) . . ? N2 Al1 N3 81.5(3) . . ? N1 Al1 N3 161.9(4) . . ? N2 Al1 H1' 114.8(12) . . ? N1 Al1 H1' 97.0(13) . . ? N3 Al1 H1' 97.1(13) . . ? N2 Al1 H2' 115.9(12) . . ? N1 Al1 H2' 90.4(12) . . ? N3 Al1 H2' 89.5(12) . . ? H1' Al1 H2' 129.4(17) . . ? N2 Ga1 N3 88.2(8) . . ? N2 Ga1 N1 85.0(10) . . ? N3 Ga1 N1 169.5(9) . . ? N2 Ga1 H1' 121.0(15) . . ? N3 Ga1 H1' 98.0(16) . . ? N1 Ga1 H1' 92.4(15) . . ? N2 Ga1 H2' 122.0(14) . . ? N3 Ga1 H2' 90.6(15) . . ? N1 Ga1 H2' 86.3(14) . . ? H1' Ga1 H2' 117(2) . . ? N2 Ga2 H3' 96.0(13) . . ? N2 Ga2 H4' 114.5(13) . . ? H3' Ga2 H4' 112.9(12) . . ? N2 Ga2 H5' 107.2(13) . . ? H3' Ga2 H5' 111.1(11) . . ? H4' Ga2 H5' 113.8(12) . . ? C1 N1 C3 110.4(2) . . ? C1 N1 C2 109.0(3) . . ? C3 N1 C2 109.6(3) . . ? C1 N1 Al1 111.4(3) . . ? C3 N1 Al1 106.6(3) . . ? C2 N1 Al1 109.8(3) . . ? C1 N1 Ga1 114.3(4) . . ? C3 N1 Ga1 101.8(5) . . ? C2 N1 Ga1 111.5(4) . . ? C5 N2 C4 109.9(2) . . ? C5 N2 Ga1 105.3(7) . . ? C4 N2 Ga1 110.4(7) . . ? C5 N2 Al1 107.0(3) . . ? C4 N2 Al1 108.6(4) . . ? C5 N2 Ga2 108.88(18) . . ? C4 N2 Ga2 108.45(18) . . ? Ga1 N2 Ga2 113.9(4) . . ? Al1 N2 Ga2 114.1(2) . . ? C6 N3 C8 110.3(2) . . ? C6 N3 C7 110.5(2) . . ? C8 N3 C7 108.1(3) . . ? C6 N3 Ga1 102.8(6) . . ? C8 N3 Ga1 110.6(4) . . ? C7 N3 Ga1 114.6(5) . . ? C6 N3 Al1 107.4(3) . . ? C8 N3 Al1 108.1(3) . . ? C7 N3 Al1 112.5(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.5(2) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C3 108.9(2) . . ? N2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N2 C5 C6 108.6(2) . . ? N2 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N2 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N3 C6 C5 109.7(2) . . ? N3 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N3 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ga1 N2 C5 29.9(5) . . . . ? N1 Ga1 N2 C5 -142.1(3) . . . . ? N3 Ga1 N2 C4 148.4(3) . . . . ? N1 Ga1 N2 C4 -23.6(5) . . . . ? N3 Ga1 N2 Ga2 -89.4(5) . . . . ? N1 Ga1 N2 Ga2 98.7(4) . . . . ? C1 N1 C3 C4 153.2(3) . . . . ? C2 N1 C3 C4 -86.8(3) . . . . ? Al1 N1 C3 C4 32.0(3) . . . . ? Ga1 N1 C3 C4 31.4(4) . . . . ? C5 N2 C4 C3 164.9(2) . . . . ? Ga1 N2 C4 C3 49.2(6) . . . . ? Al1 N2 C4 C3 48.2(4) . . . . ? Ga2 N2 C4 C3 -76.2(3) . . . . ? N1 C3 C4 N2 -53.9(3) . . . . ? C4 N2 C5 C6 -171.4(2) . . . . ? Ga1 N2 C5 C6 -52.6(6) . . . . ? Al1 N2 C5 C6 -53.8(4) . . . . ? Ga2 N2 C5 C6 69.9(3) . . . . ? C8 N3 C6 C5 92.8(3) . . . . ? C7 N3 C6 C5 -147.8(3) . . . . ? Ga1 N3 C6 C5 -25.1(4) . . . . ? Al1 N3 C6 C5 -24.8(3) . . . . ? N2 C5 C6 N3 52.2(3) . . . . ? _refine_diff_density_max 0.258 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.038 _shelxl_version_number 2014/6 _shelx_res_file ; TITL 1b in P2(1)2(1)2(1) Luo et al BRUKER-MIT workshop CELL 0.71073 6.2256 12.9136 17.4444 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0015 0.0021 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N AL GA UNIT 32 100 12 3.36 4.64 TEMP -100 SIZE 0.40 0.30 0.20 L.S. 8 BOND $H FMAP 2 PLAN 10 ACTA CONF LIST 4 HTAB TWIN SADI 0.005 Ga2 H3' Ga2 H4' Ga2 H5' SADI H3' H4' H3' H5' H4' H5' SADI AL1 H1' Al1 H2' SADI Ga1 H1' GA1 H2' EADP Al1 Ga1 WGHT 0.027100 0.258000 BASF 0.43497 FVAR 0.14963 0.84426 PART 1 AL1 4 0.239793 0.429047 0.034998 21.00000 0.03129 0.02827 = 0.01855 -0.00544 -0.00383 -0.00049 PART 2 GA1 5 0.253954 0.433906 0.044270 -21.00000 0.03129 0.02827 = 0.01855 -0.00544 -0.00383 -0.00049 PART 0 H1' 2 0.014423 0.440396 0.037270 11.00000 -1.20000 H2' 2 0.365916 0.361202 -0.009358 11.00000 -1.20000 GA2 5 0.208877 0.612476 0.176941 11.00000 0.05602 0.04134 = 0.03668 -0.01090 0.00271 0.00680 H3' 2 0.357358 0.619562 0.239500 11.00000 -1.20000 H4' 2 0.154224 0.710977 0.145666 11.00000 -1.20000 H5' 2 0.026998 0.550605 0.196963 11.00000 -1.20000 N1 3 0.304302 0.555908 -0.046424 11.00000 0.04943 0.03474 = 0.02842 -0.00089 0.00429 0.00096 N2 3 0.403050 0.523115 0.107491 11.00000 0.02963 0.03259 = 0.03203 -0.00064 -0.00337 -0.00030 N3 3 0.268196 0.321769 0.133270 11.00000 0.03739 0.03106 = 0.02992 -0.00035 -0.00140 0.00323 C1 1 0.104531 0.593800 -0.082157 11.00000 0.07011 0.05016 = 0.04282 0.00714 -0.01388 0.00444 AFIX 137 H1A 2 0.137997 0.651129 -0.116974 11.00000 -1.50000 H1B 2 0.005924 0.617983 -0.042193 11.00000 -1.50000 H1C 2 0.036917 0.537467 -0.111049 11.00000 -1.50000 AFIX 0 C2 1 0.451658 0.519406 -0.107270 11.00000 0.08319 0.05101 = 0.03953 0.00072 0.02313 0.00192 AFIX 137 H2A 2 0.478177 0.575725 -0.143716 11.00000 -1.50000 H2B 2 0.386460 0.460674 -0.134183 11.00000 -1.50000 H2C 2 0.587910 0.497649 -0.084202 11.00000 -1.50000 AFIX 0 C3 1 0.408644 0.639626 -0.002128 11.00000 0.05261 0.03457 = 0.03739 0.00243 0.00622 -0.00989 AFIX 23 H3A 2 0.297956 0.686066 0.019745 11.00000 -1.20000 H3B 2 0.501960 0.681102 -0.036318 11.00000 -1.20000 AFIX 0 C4 1 0.541105 0.593055 0.061521 11.00000 0.03953 0.04210 = 0.04414 0.00019 0.00362 -0.00946 AFIX 23 H4A 2 0.663070 0.553712 0.039659 11.00000 -1.20000 H4B 2 0.599618 0.648654 0.094546 11.00000 -1.20000 AFIX 0 C5 1 0.538263 0.455761 0.156339 11.00000 0.03257 0.04432 = 0.04487 0.00051 -0.01193 0.00316 AFIX 23 H5A 2 0.609941 0.497642 0.196404 11.00000 -1.20000 H5B 2 0.650409 0.421870 0.124883 11.00000 -1.20000 AFIX 0 C6 1 0.396543 0.374928 0.193056 11.00000 0.04374 0.04085 = 0.02853 0.00186 -0.00953 0.00773 AFIX 23 H6A 2 0.486310 0.323799 0.220658 11.00000 -1.20000 H6B 2 0.299407 0.408222 0.230627 11.00000 -1.20000 AFIX 0 C7 1 0.055615 0.290307 0.164373 11.00000 0.04753 0.05385 = 0.04423 0.01126 0.00411 -0.00742 AFIX 137 H7A 2 0.076508 0.242874 0.207586 11.00000 -1.50000 H7B 2 -0.027325 0.255477 0.124185 11.00000 -1.50000 H7C 2 -0.022447 0.351836 0.181846 11.00000 -1.50000 AFIX 0 C8 1 0.380954 0.227138 0.106649 11.00000 0.07254 0.03265 = 0.05010 0.00017 -0.00257 0.01568 AFIX 137 H8A 2 0.384706 0.176122 0.148218 11.00000 -1.50000 H8B 2 0.528069 0.244893 0.091592 11.00000 -1.50000 H8C 2 0.304558 0.197899 0.062556 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1b in P2(1)2(1)2(1) Luo et al BRUKER-MIT workshop REM R1 = 0.0204 for 2334 Fo > 4sig(Fo) and 0.0237 for all 2482 data REM 142 parameters refined using 8 restraints END WGHT 0.0277 0.2519 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.258, deepest hole -0.224, 1-sigma level 0.038 Q1 1 0.3229 0.5732 0.1713 11.00000 0.05 0.26 Q2 1 0.2934 0.6886 0.1768 11.00000 0.05 0.23 Q3 1 0.4650 0.4227 0.1812 11.00000 0.05 0.20 Q4 1 0.0589 0.6570 0.1451 11.00000 0.05 0.19 Q5 1 0.1847 0.5226 0.1811 11.00000 0.05 0.18 Q6 1 0.1200 0.5705 0.1758 11.00000 0.05 0.18 Q7 1 0.1047 0.6779 0.1827 11.00000 0.05 0.17 Q8 1 0.3209 0.3779 0.0362 11.00000 0.05 0.15 Q9 1 0.2200 0.3525 0.1029 11.00000 0.05 0.15 Q10 1 0.2168 0.5676 -0.0546 11.00000 0.05 0.14 ; _shelx_res_checksum 82696 _shelx_hkl_file ; -1 0 0 -0.08 0.05 1 0 0 0.05 0.06 -1 0 0 0.05 0.05 2 0 0 114.06 3.56 -2 0 0 125.59 3.55 -2 0 0 108.92 3.55 -2 0 0 116.42 3.55 -3 0 0 -0.16 0.13 3 0 0 -0.02 0.16 4 0 0 56.90 1.81 -4 0 0 57.65 1.77 -4 0 0 55.38 1.78 5 0 0 0.22 0.31 -5 0 0 -0.05 0.25 6 0 0 17.89 0.67 6 0 0 18.41 0.75 -7 0 0 -0.32 0.33 7 0 0 -0.07 0.38 0 -1 0 0.01 0.02 0 1 0 0.06 0.03 0 1 0 0.04 0.02 1 1 0 901.30 28.72 -1 -1 0 984.42 28.70 1 1 0 942.53 28.69 1 -1 0 928.87 28.72 1 -1 0 952.59 28.86 -1 -1 0 1000.00 28.79 -1 1 0 934.25 28.69 -1 1 0 911.74 28.68 2 1 0 47.21 1.44 -2 -1 0 46.14 1.43 2 -1 0 47.31 1.46 -2 1 0 46.00 1.44 -2 1 0 44.18 1.44 -2 -1 0 47.81 1.44 2 1 0 47.49 1.45 -3 -1 0 72.92 2.30 -3 1 0 75.55 2.29 3 1 0 76.04 2.29 -3 -1 0 74.63 2.28 3 1 0 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