data_MOF520_100K _publ_requested_journal ‘ACS Central Science’ _publ_contact_author_name 'Omar M. Yaghi' _publ_contact_author_address ;Department of Chemistry, University of California, Berkeley, Berkeley, CA 94720 USA ; _publ_contact_author_email yaghi@berkeley.edu loop_ _publ_author_name _publ_author_address _publ_author_id_iucr 'Kapustin, Eugene A.' ;Department of Chemistry, University of California-Berkeley Berkeley, California 94720, United States Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720, United States Kavli Energy NanoSciences Institute at Berkeley, Berkeley, California 94720, United States Global Science Institute at Berkeley, Berkeley, California 94720, United States ; ? 'Lee, Seungkyu' ;Department of Chemistry, University of California-Berkeley Berkeley, California 94720, United States Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720, United States Kavli Energy NanoSciences Institute at Berkeley, Berkeley, California 94720, United States Global Science Institute at Berkeley, Berkeley, California 94720, United States ; ? 'Alshammari, Ahmad S.' ;King Abdulaziz City for Science and Technology, Riyadh 11442, Saudi Arabia ; ? 'Yaghi, Omar M.' ;Department of Chemistry, University of California-Berkeley, Berkeley, California 94720, United States Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720, United States Kavli Energy NanoSciences Institute at Berkeley, Berkeley, California 94720, United States Global Science Institute at Berkeley, Berkeley, California 94720, United States King Abdulaziz City for Science and Technology, Riyadh 11442, Saudi Arabia ; ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common 'MOF-520_100K' _chemical_name_systematic ? _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0090 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.1200 0.1100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 94 _space_group_name_H-M_alt 'P 42 21 2' _space_group_name_Hall 'P 4n 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 18.3754(6) _cell_length_b 18.3754(6) _cell_length_c 37.6893(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 12726.0(9) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9729 _cell_measurement_theta_max 38.603 _cell_measurement_theta_min 2.86 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.593 _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_absorpt_coefficient_mu 0.190 _shelx_estimated_absorpt_T_max 0.7476 _shelx_estimated_absorpt_T_min 0.6638 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 0.7476 _exptl_absorpt_correction_T_min 0.6638 _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0931 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.8879. The \l/2 correction factor is Not present. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.0332 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 11.3.1 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker D8 with PHOTON 100 detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_detector_area_resol_mean 10.42 _diffrn_reflns_number 107906 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_theta_full 38.603 _diffrn_reflns_theta_max 38.603 _diffrn_reflns_theta_min 2.250 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _reflns_number_total 11720 _reflns_number_gt 10185 _diffrn_standards_number 0 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.771 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.996 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_diff_density_max 0.227 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.040 _refine_ls_abs_structure_details ; Flack x determined using 4075 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.086(15) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 11720 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0338 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0750P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1066 _refine_ls_wR_factor_ref 0.1094 _refine_special_details ; Before applying solvent masking instruction, the structure of MOF-520 was refined anisotropically, hydrogen were placed into geometrically calculated positions and the structure was moved into center of gravity. Once solvent masking instruction was introduced, the weight scheme was refined to convergence. The void volume is estimated to be 8866.0 A^3 with 8218.7 electrons removed during masking. Some reflections were omitted due to non-ideal solvent masking, beamstop clipping and the minor presence of diffuse scattering. The threshold (Iobs-Icalc)/sigmaW > 10 was chosen for omitting these reflections. Omission of these reflections did not affect the refinement; the fraction of omitted reflections is less than 0.1% of whole dataset. See _olex2_refinement_description for further details for hydrogen restraints. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C26(H26), C23(H23), C25(H25), C22(H22), C7(H7), C16(H16), C18(H18), C3(H3), C4(H4), C6(H6), C13(H13), C19(H19), C15(H15), C11(H11), C9(H9), C28(H28) ; # start Validation Reply Form _vrf_PLAT250_MOF520_delta_ambient ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.3 Note RESPONSE: This is caused by flexibility of BTB linker ; _vrf_PLAT911_MOF520_delta_ambient ; PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 5 Report RESPONSE: Some reflections are missing due to non-ideal solvent masking, beamstop clipping and the minor presence of diffuse scattering. ; _vrf_PLAT918_MOF520_delta_ambient ; PROBLEM: Reflection(s) with I(obs) much Smaller I(calc) . 1 Check RESPONSE: Non-ideal solvent masking ; _vrf_PLAT420_MOF520_delta_ambient ; PROBLEM: D-H Without Acceptor O1 -- H1 ... Please Check RESPONSE: Acceptor is a disordered solvent molecule in the pore, which was accounted for by the Olex2 solvent masking instruction. ; _vrf_PLAT430_MOF520_delta_ambient ; PROBLEM: Short Inter D...A Contact O5 .. O8 .. 2.63 Ang. RESPONSE: Proximity is due to octahedral Al atom environment. For charge-balancing reasons both oxygens from the carboxylate group of the organic linker should be deprotonated ; _vrf_PLAT919_MOF520_delta_ambient ; PROBLEM: Reflection # Likely Affected by the Beamstop ... 1 Check RESPONSE: Some reflections were omitted due to non-ideal solvent masking, beamstop clipping and the minor presence of diffuse scattering ; _vrf_PLAT934_MOF520_delta_ambient ; PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers .... 10 Check RESPONSE: Non-ideal solvent masking ; # end Validation Reply Form _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.66447(3) 0.33553(3) 0.5000 0.0374(2) Uani 1 2 d S T P . . Al2 Al 0.63693(4) 0.40980(3) 0.42095(2) 0.03669(16) Uani 1 1 d . . . . . Al3 Al 0.5000 0.5000 0.38618(2) 0.0390(2) Uani 1 2 d S T P . . O2 O 0.56884(8) 0.48359(7) 0.42037(3) 0.0373(3) Uani 1 1 d . . . . . H2 H 0.5696 0.5158 0.4394 0.045 Uiso 1 1 calc R . . . . O3 O 0.67059(9) 0.43825(9) 0.37522(4) 0.0448(4) Uani 1 1 d . . . . . O1 O 0.60716(8) 0.37568(8) 0.46485(3) 0.0389(3) Uani 1 1 d . . . . . H1 H 0.5577 0.3792 0.4697 0.047 Uiso 1 1 calc R . . . . O4 O 0.56867(10) 0.48167(9) 0.34931(4) 0.0482(4) Uani 1 1 d . . . . . C1 C 0.63438(14) 0.46068(12) 0.34901(6) 0.0443(5) Uani 1 1 d . . . . . C26 C 0.79197(15) 0.65909(14) 0.14833(7) 0.0563(6) Uani 1 1 d . . . . . H26 H 0.7895 0.6654 0.1728 0.068 Uiso 1 1 calc R . . . . C23 C 0.79242(16) 0.64165(14) 0.07508(6) 0.0551(6) Uani 1 1 d . . . . . H23 H 0.7912 0.6355 0.0506 0.066 Uiso 1 1 calc R . . . . C20 C 1.00900(13) 0.15439(12) 0.11559(5) 0.0419(5) Uani 1 1 d . . . . . C25 C 0.78721(15) 0.71979(13) 0.12536(6) 0.0485(6) Uani 1 1 d . . . . . H25 H 0.7838 0.7665 0.1347 0.058 Uiso 1 1 calc R . . . . C22 C 0.79925(18) 0.58108(15) 0.09740(7) 0.0632(8) Uani 1 1 d . . . . . H22 H 0.8031 0.5346 0.0878 0.076 Uiso 1 1 calc R . . . . C24 C 0.78755(14) 0.71008(13) 0.08952(6) 0.0438(5) Uani 1 1 d . . . . . C27 C 0.79120(12) 0.77570(12) 0.06610(5) 0.0399(5) Uani 1 1 d . . . . . C17 C 0.97538(14) 0.22229(13) 0.13049(6) 0.0491(6) Uani 1 1 d . . . . . C7 C 0.64196(16) 0.49769(16) 0.28502(6) 0.0609(7) Uani 1 1 d . . . . . H7 H 0.5972 0.5208 0.2875 0.073 Uiso 1 1 calc R . . . . C21 C 0.80025(14) 0.59058(14) 0.13414(6) 0.0510(6) Uani 1 1 d . . . . . C5 C 0.74427(18) 0.46443(14) 0.24862(7) 0.0618(8) Uani 1 1 d . . . . . C16 C 0.90918(15) 0.21431(15) 0.14922(7) 0.0571(7) Uani 1 1 d . . . . . H16 H 0.8889 0.1684 0.1522 0.069 Uiso 1 1 calc R . . . . C8 C 0.78211(17) 0.46499(14) 0.21344(7) 0.0605(7) Uani 1 1 d . . . . . C2 C 0.67291(15) 0.46285(13) 0.31416(6) 0.0504(6) Uani 1 1 d . . . . . C18 C 1.00439(16) 0.29184(13) 0.12625(6) 0.0546(6) Uani 1 1 d . . . . . H18 H 1.0483 0.2975 0.1143 0.065 Uiso 1 1 calc R . . . . C3 C 0.74190(16) 0.43040(14) 0.31014(6) 0.0572(7) Uani 1 1 d . . . . . H3 H 0.7643 0.4086 0.3295 0.069 Uiso 1 1 calc R . . . . C4 C 0.77597(16) 0.43073(15) 0.27807(7) 0.0603(7) Uani 1 1 d . . . . . H4 H 0.8210 0.4082 0.2757 0.072 Uiso 1 1 calc R . . . . C14 C 0.90312(18) 0.34349(14) 0.15795(7) 0.0651(8) Uani 1 1 d . . . . . C6 C 0.67622(18) 0.49846(17) 0.25303(6) 0.0651(8) Uani 1 1 d . . . . . H6 H 0.6545 0.5217 0.2339 0.078 Uiso 1 1 calc R . . . . C13 C 0.77411(16) 0.52470(15) 0.19077(6) 0.0614(7) Uani 1 1 d . . . . . H13 H 0.7449 0.5635 0.1977 0.074 Uiso 1 1 calc R . . . . C19 C 0.96997(16) 0.35118(14) 0.13912(6) 0.0585(7) Uani 1 1 d . . . . . H19 H 0.9899 0.3972 0.1357 0.070 Uiso 1 1 calc R . . . . C10 C 0.86035(18) 0.40793(15) 0.17013(7) 0.0680(8) Uani 1 1 d . . . . . C15 C 0.87517(17) 0.27395(15) 0.16286(7) 0.0649(8) Uani 1 1 d . . . . . H15 H 0.8324 0.2680 0.1757 0.078 Uiso 1 1 calc R . . . . C12 C 0.80902(17) 0.52720(14) 0.15789(7) 0.0597(7) Uani 1 1 d . . . . . C11 C 0.85318(17) 0.46817(14) 0.14817(7) 0.0626(8) Uani 1 1 d . . . . . H11 H 0.8780 0.4694 0.1267 0.075 Uiso 1 1 calc R . . . . C9 C 0.82613(18) 0.40743(15) 0.20293(7) 0.0641(8) Uani 1 1 d . . . . . H9 H 0.8327 0.3680 0.2181 0.077 Uiso 1 1 calc R . . . . O8 O 0.79135(8) 0.83704(8) 0.08108(4) 0.0429(4) Uani 1 1 d . . . . . O10 O 0.73993(8) 0.40702(9) 0.49033(4) 0.0444(4) Uani 1 1 d . . . . . O5 O 1.07230(9) 0.15976(8) 0.10215(3) 0.0400(3) Uani 1 1 d . . . . . O6 O 0.97260(9) 0.09859(9) 0.11736(4) 0.0468(4) Uani 1 1 d . . . . . O9 O 0.70837(9) 0.47271(9) 0.44125(4) 0.0462(4) Uani 1 1 d . . . . . O7 O 0.79624(9) 0.76656(8) 0.03257(4) 0.0446(4) Uani 1 1 d . . . . . C28 C 0.74561(14) 0.45887(14) 0.46932(7) 0.0512(6) Uani 1 1 d . . . . . H28 H 0.7819 0.4924 0.4747 0.061 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0437(3) 0.0437(3) 0.0247(4) -0.0028(3) -0.0028(3) 0.0014(4) Al2 0.0467(4) 0.0380(3) 0.0254(3) -0.0005(3) 0.0012(3) 0.0005(3) Al3 0.0520(6) 0.0398(5) 0.0251(4) 0.000 0.000 0.0042(4) O2 0.0531(9) 0.0355(7) 0.0233(7) -0.0018(6) 0.0010(6) -0.0003(6) O3 0.0553(9) 0.0463(9) 0.0328(8) 0.0042(7) 0.0077(7) 0.0039(7) O1 0.0434(8) 0.0476(9) 0.0256(7) -0.0013(6) -0.0023(6) 0.0054(7) O4 0.0619(11) 0.0595(10) 0.0231(7) 0.0007(7) 0.0045(7) 0.0115(8) C1 0.0596(15) 0.0422(12) 0.0310(11) 0.0001(9) 0.0069(10) 0.0103(11) C26 0.0766(18) 0.0550(15) 0.0374(12) 0.0035(11) 0.0151(12) 0.0093(13) C23 0.0836(18) 0.0533(15) 0.0283(11) 0.0016(10) 0.0082(12) -0.0073(13) C20 0.0523(14) 0.0411(12) 0.0323(10) -0.0040(9) 0.0022(10) 0.0050(11) C25 0.0707(16) 0.0387(12) 0.0360(12) 0.0055(10) 0.0050(11) 0.0039(11) C22 0.101(2) 0.0436(14) 0.0447(14) 0.0006(11) 0.0245(14) 0.0053(14) C24 0.0549(14) 0.0434(13) 0.0330(11) 0.0065(10) 0.0009(10) -0.0014(10) C27 0.0477(13) 0.0442(13) 0.0280(10) 0.0050(9) -0.0030(9) -0.0073(10) C17 0.0664(16) 0.0503(14) 0.0307(11) -0.0001(10) 0.0141(10) 0.0028(12) C7 0.0708(17) 0.0653(16) 0.0466(13) 0.0099(13) 0.0209(13) 0.0269(14) C21 0.0653(16) 0.0500(14) 0.0375(12) 0.0105(11) 0.0179(11) 0.0065(12) C5 0.092(2) 0.0508(15) 0.0424(13) 0.0164(11) 0.0270(13) 0.0213(14) C16 0.0711(17) 0.0500(14) 0.0504(14) 0.0045(12) 0.0212(13) -0.0038(13) C8 0.0809(19) 0.0506(15) 0.0500(14) 0.0094(12) 0.0279(13) 0.0166(13) C2 0.0686(16) 0.0496(14) 0.0331(11) 0.0103(10) 0.0138(11) 0.0099(12) C18 0.0718(17) 0.0449(14) 0.0471(13) 0.0006(11) 0.0200(13) 0.0022(12) C3 0.0869(19) 0.0499(14) 0.0347(12) 0.0117(11) 0.0130(12) 0.0195(13) C4 0.0762(18) 0.0562(16) 0.0485(14) 0.0075(12) 0.0170(13) 0.0227(14) C14 0.098(2) 0.0483(15) 0.0484(14) 0.0105(12) 0.0363(15) 0.0139(14) C6 0.095(2) 0.0670(17) 0.0340(12) 0.0146(12) 0.0161(13) 0.0289(17) C13 0.085(2) 0.0613(16) 0.0373(13) 0.0135(11) 0.0182(13) 0.0249(14) C19 0.0823(19) 0.0512(15) 0.0420(13) 0.0082(11) 0.0317(13) 0.0036(13) C10 0.095(2) 0.0527(16) 0.0559(16) 0.0080(12) 0.0351(15) 0.0167(15) C15 0.082(2) 0.0517(15) 0.0606(16) 0.0087(13) 0.0428(15) 0.0045(14) C12 0.086(2) 0.0479(15) 0.0455(14) 0.0061(11) 0.0219(13) 0.0068(13) C11 0.084(2) 0.0560(16) 0.0473(14) 0.0069(12) 0.0289(14) 0.0125(14) C9 0.094(2) 0.0493(15) 0.0491(14) 0.0144(12) 0.0341(14) 0.0130(14) O8 0.0518(9) 0.0435(8) 0.0334(7) -0.0001(7) 0.0031(7) -0.0045(7) O10 0.0428(8) 0.0540(10) 0.0363(8) 0.0001(7) 0.0004(6) -0.0027(7) O5 0.0524(9) 0.0400(8) 0.0276(7) -0.0024(6) 0.0079(7) 0.0012(7) O6 0.0592(10) 0.0415(9) 0.0398(8) -0.0060(7) 0.0092(7) -0.0030(8) O9 0.0468(9) 0.0492(9) 0.0427(8) -0.0025(7) 0.0021(7) -0.0056(7) O7 0.0587(10) 0.0485(9) 0.0264(8) 0.0026(6) -0.0010(7) -0.0107(7) C28 0.0507(14) 0.0548(15) 0.0482(14) -0.0052(12) -0.0025(11) -0.0077(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.8462(15) 8_666 ? Al1 O1 1.8462(15) . ? Al1 O10 1.9444(16) . ? Al1 O10 1.9444(16) 8_666 ? Al1 O7 1.9063(16) 6_645 ? Al1 O7 1.9063(16) 2_645 ? Al2 O2 1.8450(16) . ? Al2 O3 1.9043(15) . ? Al2 O1 1.8518(15) . ? Al2 O8 1.8789(16) 6_645 ? Al2 O5 1.9502(16) 5_455 ? Al2 O9 1.9091(17) . ? Al3 O2 1.8307(16) . ? Al3 O2 1.8308(15) 3_665 ? Al3 O4 1.9071(16) . ? Al3 O4 1.9070(16) 3_665 ? Al3 O6 1.8850(16) 6_655 ? Al3 O6 1.8850(16) 5_455 ? O3 C1 1.260(3) . ? O4 C1 1.268(3) . ? C1 C2 1.493(3) . ? C26 C25 1.415(3) . ? C26 C21 1.376(4) . ? C23 C22 1.401(4) . ? C23 C24 1.373(3) . ? C20 C17 1.501(3) . ? C20 O5 1.272(3) . ? C20 O6 1.226(3) . ? C25 C24 1.362(3) . ? C22 C21 1.396(3) . ? C24 C27 1.496(3) . ? C27 O8 1.261(3) . ? C27 O7 1.278(2) . ? C17 C16 1.414(3) . ? C17 C18 1.394(3) . ? C7 C2 1.393(3) . ? C7 C6 1.360(3) . ? C21 C12 1.478(3) . ? C5 C8 1.497(3) . ? C5 C4 1.398(4) . ? C5 C6 1.408(4) . ? C16 C15 1.362(4) . ? C8 C13 1.398(3) . ? C8 C9 1.389(4) . ? C2 C3 1.409(4) . ? C18 C19 1.351(4) . ? C3 C4 1.361(3) . ? C14 C19 1.426(4) . ? C14 C10 1.494(4) . ? C14 C15 1.390(4) . ? C13 C12 1.396(3) . ? C10 C11 1.389(4) . ? C10 C9 1.387(3) . ? C12 C11 1.403(4) . ? O8 Al2 1.8788(16) 6_655 ? O10 C28 1.243(3) . ? O5 Al2 1.9502(16) 5 ? O6 Al3 1.8851(16) 5 ? O9 C28 1.285(3) . ? O7 Al1 1.9064(16) 4_564 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 93.39(9) 8_666 . ? O1 Al1 O10 91.96(7) . 8_666 ? O1 Al1 O10 91.96(7) 8_666 . ? O1 Al1 O10 90.13(7) 8_666 8_666 ? O1 Al1 O10 90.13(7) . . ? O1 Al1 O7 173.02(7) 8_666 6_645 ? O1 Al1 O7 91.12(6) 8_666 2_645 ? O1 Al1 O7 173.02(7) . 2_645 ? O1 Al1 O7 91.12(6) . 6_645 ? O10 Al1 O10 176.96(11) 8_666 . ? O7 Al1 O10 93.35(7) 6_645 . ? O7 Al1 O10 93.35(7) 2_645 8_666 ? O7 Al1 O10 84.40(7) 2_645 . ? O7 Al1 O10 84.40(7) 6_645 8_666 ? O7 Al1 O7 84.90(10) 6_645 2_645 ? O2 Al2 O3 90.45(7) . . ? O2 Al2 O1 93.38(7) . . ? O2 Al2 O8 176.45(7) . 6_645 ? O2 Al2 O5 93.63(7) . 5_455 ? O2 Al2 O9 91.50(7) . . ? O3 Al2 O5 88.48(7) . 5_455 ? O3 Al2 O9 88.46(7) . . ? O1 Al2 O3 175.90(8) . . ? O1 Al2 O8 90.15(7) . 6_645 ? O1 Al2 O5 89.83(7) . 5_455 ? O1 Al2 O9 92.87(7) . . ? O8 Al2 O3 86.03(7) 6_645 . ? O8 Al2 O5 86.71(7) 6_645 5_455 ? O8 Al2 O9 87.99(7) 6_645 . ? O9 Al2 O5 174.06(8) . 5_455 ? O2 Al3 O2 90.52(9) . 3_665 ? O2 Al3 O4 177.70(7) 3_665 . ? O2 Al3 O4 91.53(6) 3_665 3_665 ? O2 Al3 O4 177.70(7) . 3_665 ? O2 Al3 O4 91.53(6) . . ? O2 Al3 O6 91.36(7) . 6_655 ? O2 Al3 O6 94.36(7) . 5_455 ? O2 Al3 O6 91.36(7) 3_665 5_455 ? O2 Al3 O6 94.36(7) 3_665 6_655 ? O4 Al3 O4 86.45(10) 3_665 . ? O6 Al3 O4 86.64(7) 6_655 . ? O6 Al3 O4 87.44(7) 6_655 3_665 ? O6 Al3 O4 87.44(7) 5_455 . ? O6 Al3 O4 86.64(7) 5_455 3_665 ? O6 Al3 O6 171.87(11) 5_455 6_655 ? Al3 O2 Al2 126.72(8) . . ? C1 O3 Al2 128.88(15) . . ? Al1 O1 Al2 127.44(9) . . ? C1 O4 Al3 133.67(14) . . ? O3 C1 O4 126.5(2) . . ? O3 C1 C2 116.6(2) . . ? O4 C1 C2 116.8(2) . . ? C21 C26 C25 119.4(2) . . ? C24 C23 C22 119.7(2) . . ? O5 C20 C17 117.4(2) . . ? O6 C20 C17 116.8(2) . . ? O6 C20 O5 125.8(2) . . ? C24 C25 C26 120.2(2) . . ? C21 C22 C23 119.8(2) . . ? C23 C24 C27 120.09(19) . . ? C25 C24 C23 120.9(2) . . ? C25 C24 C27 118.7(2) . . ? O8 C27 C24 117.18(18) . . ? O8 C27 O7 124.05(19) . . ? O7 C27 C24 118.7(2) . . ? C16 C17 C20 117.0(2) . . ? C18 C17 C20 124.2(2) . . ? C18 C17 C16 118.8(2) . . ? C6 C7 C2 121.0(2) . . ? C26 C21 C22 119.9(2) . . ? C26 C21 C12 119.8(2) . . ? C22 C21 C12 120.3(2) . . ? C4 C5 C8 120.8(2) . . ? C4 C5 C6 118.2(2) . . ? C6 C5 C8 120.9(2) . . ? C15 C16 C17 120.0(2) . . ? C13 C8 C5 119.8(2) . . ? C9 C8 C5 121.2(2) . . ? C9 C8 C13 119.0(2) . . ? C7 C2 C1 120.8(2) . . ? C7 C2 C3 118.5(2) . . ? C3 C2 C1 120.7(2) . . ? C19 C18 C17 121.3(2) . . ? C4 C3 C2 120.5(2) . . ? C3 C4 C5 121.0(3) . . ? C19 C14 C10 121.9(2) . . ? C15 C14 C19 118.4(2) . . ? C15 C14 C10 119.6(2) . . ? C7 C6 C5 120.7(2) . . ? C12 C13 C8 121.3(2) . . ? C18 C19 C14 120.1(2) . . ? C11 C10 C14 119.9(2) . . ? C9 C10 C14 120.5(2) . . ? C9 C10 C11 119.6(2) . . ? C16 C15 C14 121.3(2) . . ? C13 C12 C21 120.9(2) . . ? C13 C12 C11 118.2(2) . . ? C11 C12 C21 120.9(2) . . ? C10 C11 C12 121.0(2) . . ? C10 C9 C8 120.9(2) . . ? C27 O8 Al2 128.29(14) . 6_655 ? C28 O10 Al1 134.19(16) . . ? C20 O5 Al2 133.13(14) . 5 ? C20 O6 Al3 130.86(15) . 5 ? C28 O9 Al2 125.17(16) . . ? C27 O7 Al1 125.22(14) . 4_564 ? O10 C28 O9 129.1(2) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.153 -0.207 -0.106 8866.0 8218.7 None _shelx_res_file ; ek_mof5x_nonbridged_ambient_mo.res created by SHELXL-2014/7 TITL ek_mof5x_nonbridged_ambient_mo in P42212 #94 REM reset to P42212 #94 CELL 1.0332 18.3754 18.3754 37.6893 90 90 90 ZERR 8 0.0006 0.0006 0.0012 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.12 0.11 744.346 DISP C 0.009 0.004 30.879 DISP H -0 0 0.639 DISP O 0.025 0.014 100.516 UNIT 224 144 80 16 L.S. 14 PLAN 20 TEMP 25 BOND fmap 2 ACTA 52 ABIN REM REM REM WGHT 0.075000 FVAR 0.09730 AL1 4 0.664468 0.335532 0.500000 10.50000 0.04370 0.04370 = 0.02470 -0.00277 -0.00277 0.00136 AL2 4 0.636934 0.409805 0.420953 11.00000 0.04668 0.03803 = 0.02536 -0.00048 0.00122 0.00045 AL3 4 0.500000 0.500000 0.386183 10.50000 0.05203 0.03982 = 0.02515 0.00000 0.00000 0.00425 O2 3 0.568839 0.483586 0.420374 11.00000 0.05310 0.03548 = 0.02330 -0.00184 0.00102 -0.00028 AFIX 43 H2 2 0.569561 0.515761 0.439418 11.00000 -1.20000 AFIX 0 O3 3 0.670594 0.438248 0.375223 11.00000 0.05525 0.04630 = 0.03277 0.00415 0.00768 0.00393 O1 3 0.607163 0.375682 0.464846 11.00000 0.04344 0.04759 = 0.02558 -0.00131 -0.00225 0.00545 AFIX 43 H1 2 0.557681 0.379168 0.469742 11.00000 -1.20000 AFIX 0 O4 3 0.568669 0.481672 0.349311 11.00000 0.06194 0.05947 = 0.02308 0.00071 0.00450 0.01145 C1 1 0.634378 0.460682 0.349012 11.00000 0.05956 0.04223 = 0.03103 0.00013 0.00690 0.01031 C26 1 0.791975 0.659092 0.148327 11.00000 0.07663 0.05496 = 0.03737 0.00350 0.01510 0.00926 AFIX 43 H26 2 0.789540 0.665424 0.172780 11.00000 -1.20000 AFIX 0 C23 1 0.792420 0.641649 0.075076 11.00000 0.08358 0.05334 = 0.02829 0.00156 0.00823 -0.00727 AFIX 43 H23 2 0.791186 0.635542 0.050588 11.00000 -1.20000 AFIX 0 C20 1 1.009002 0.154389 0.115591 11.00000 0.05226 0.04105 = 0.03234 -0.00403 0.00217 0.00496 C25 1 0.787209 0.719787 0.125356 11.00000 0.07070 0.03866 = 0.03599 0.00550 0.00496 0.00391 AFIX 43 H25 2 0.783829 0.766468 0.134747 11.00000 -1.20000 AFIX 0 C22 1 0.799252 0.581077 0.097399 11.00000 0.10122 0.04362 = 0.04468 0.00057 0.02449 0.00526 AFIX 43 H22 2 0.803113 0.534646 0.087762 11.00000 -1.20000 AFIX 0 C24 1 0.787555 0.710076 0.089519 11.00000 0.05487 0.04343 = 0.03305 0.00646 0.00087 -0.00137 C27 1 0.791198 0.775697 0.066104 11.00000 0.04767 0.04422 = 0.02795 0.00496 -0.00297 -0.00728 C17 1 0.975376 0.222294 0.130490 11.00000 0.06640 0.05029 = 0.03069 -0.00014 0.01407 0.00277 C7 1 0.641964 0.497687 0.285023 11.00000 0.07078 0.06526 = 0.04657 0.00987 0.02092 0.02694 AFIX 43 H7 2 0.597205 0.520771 0.287472 11.00000 -1.20000 AFIX 0 C21 1 0.800250 0.590578 0.134136 11.00000 0.06528 0.05004 = 0.03755 0.01050 0.01786 0.00650 C5 1 0.744275 0.464429 0.248618 11.00000 0.09226 0.05075 = 0.04236 0.01642 0.02704 0.02129 C16 1 0.909184 0.214313 0.149224 11.00000 0.07107 0.04997 = 0.05037 0.00446 0.02115 -0.00377 AFIX 43 H16 2 0.888880 0.168366 0.152234 11.00000 -1.20000 AFIX 0 C8 1 0.782113 0.464995 0.213440 11.00000 0.08095 0.05058 = 0.05000 0.00939 0.02790 0.01660 C2 1 0.672910 0.462847 0.314164 11.00000 0.06858 0.04964 = 0.03311 0.01033 0.01383 0.00994 C18 1 1.004389 0.291842 0.126252 11.00000 0.07177 0.04488 = 0.04709 0.00056 0.02002 0.00219 AFIX 43 H18 2 1.048332 0.297499 0.114324 11.00000 -1.20000 AFIX 0 C3 1 0.741902 0.430402 0.310136 11.00000 0.08690 0.04992 = 0.03472 0.01168 0.01303 0.01946 AFIX 43 H3 2 0.764327 0.408598 0.329536 11.00000 -1.20000 AFIX 0 C4 1 0.775973 0.430732 0.278068 11.00000 0.07622 0.05620 = 0.04846 0.00754 0.01704 0.02269 AFIX 43 H4 2 0.821030 0.408194 0.275712 11.00000 -1.20000 AFIX 0 C14 1 0.903123 0.343486 0.157948 11.00000 0.09848 0.04829 = 0.04844 0.01045 0.03627 0.01387 C6 1 0.676222 0.498460 0.253033 11.00000 0.09452 0.06697 = 0.03395 0.01462 0.01613 0.02885 AFIX 43 H6 2 0.654451 0.521726 0.233861 11.00000 -1.20000 AFIX 0 C13 1 0.774110 0.524705 0.190770 11.00000 0.08542 0.06133 = 0.03734 0.01345 0.01815 0.02487 AFIX 43 H13 2 0.744950 0.563527 0.197733 11.00000 -1.20000 AFIX 0 C19 1 0.969971 0.351180 0.139120 11.00000 0.08228 0.05121 = 0.04204 0.00819 0.03171 0.00361 AFIX 43 H19 2 0.989922 0.397158 0.135691 11.00000 -1.20000 AFIX 0 C10 1 0.860350 0.407931 0.170131 11.00000 0.09525 0.05274 = 0.05594 0.00796 0.03506 0.01674 C15 1 0.875165 0.273951 0.162863 11.00000 0.08225 0.05169 = 0.06062 0.00867 0.04281 0.00446 AFIX 43 H15 2 0.832377 0.268006 0.175719 11.00000 -1.20000 AFIX 0 C12 1 0.809018 0.527201 0.157894 11.00000 0.08566 0.04793 = 0.04553 0.00606 0.02186 0.00685 C11 1 0.853177 0.468169 0.148166 11.00000 0.08445 0.05597 = 0.04733 0.00694 0.02893 0.01246 AFIX 43 H11 2 0.878018 0.469415 0.126675 11.00000 -1.20000 AFIX 0 C9 1 0.826125 0.407430 0.202930 11.00000 0.09396 0.04933 = 0.04913 0.01441 0.03414 0.01300 AFIX 43 H9 2 0.832727 0.368039 0.218085 11.00000 -1.20000 AFIX 0 O8 3 0.791353 0.837043 0.081077 11.00000 0.05177 0.04348 = 0.03344 -0.00005 0.00305 -0.00452 O10 3 0.739926 0.407015 0.490327 11.00000 0.04276 0.05401 = 0.03629 0.00015 0.00038 -0.00271 O5 3 1.072295 0.159757 0.102154 11.00000 0.05235 0.03998 = 0.02756 -0.00243 0.00789 0.00116 O6 3 0.972599 0.098592 0.117358 11.00000 0.05915 0.04146 = 0.03977 -0.00605 0.00925 -0.00299 O9 3 0.708367 0.472713 0.441253 11.00000 0.04678 0.04920 = 0.04270 -0.00249 0.00207 -0.00563 O7 3 0.796244 0.766557 0.032567 11.00000 0.05874 0.04852 = 0.02642 0.00263 -0.00099 -0.01069 C28 1 0.745608 0.458865 0.469317 11.00000 0.05068 0.05480 = 0.04823 -0.00516 -0.00247 -0.00772 AFIX 43 H28 2 0.781933 0.492358 0.474663 11.00000 -1.20000 AFIX 0 HKLF 4 REM ek_mof5x_nonbridged_ambient_mo in P42212 #94 REM R1 = 0.0338 for 10185 Fo > 4sig(Fo) and 0.0390 for all 11720 data REM 362 parameters refined using 0 restraints END WGHT 0.0754 0.0000 REM Highest difference peak 0.227, deepest hole -0.219, 1-sigma level 0.040 Q1 1 0.5144 0.5141 0.3465 11.00000 0.05 0.23 Q2 1 0.9422 0.1111 0.1456 11.00000 0.05 0.23 Q3 1 0.5365 0.5276 0.3446 11.00000 0.05 0.23 Q4 1 0.5371 0.4771 0.3390 11.00000 0.05 0.22 Q5 1 0.7403 0.4730 0.3425 11.00000 0.05 0.21 Q6 1 0.8789 0.0726 0.1500 11.00000 0.05 0.21 Q7 1 0.9574 0.0833 0.1497 11.00000 0.05 0.21 Q8 1 0.9599 0.1606 0.1478 11.00000 0.05 0.20 Q9 1 0.6768 0.5321 0.3422 11.00000 0.05 0.20 Q10 1 0.5215 0.4490 0.3651 11.00000 0.05 0.20 Q11 1 0.5962 0.4720 0.3382 11.00000 0.05 0.20 Q12 1 0.6008 0.5487 0.3444 11.00000 0.05 0.19 Q13 1 1.0206 0.2203 0.1534 11.00000 0.05 0.19 Q14 1 1.0305 0.3050 0.1551 11.00000 0.05 0.18 Q15 1 0.8059 0.7799 0.1550 11.00000 0.05 0.18 Q16 1 0.5397 0.4325 0.3591 11.00000 0.05 0.18 Q17 1 0.6124 0.3291 0.5209 11.00000 0.05 0.18 Q18 1 0.6198 0.3802 0.5000 10.50000 0.05 0.17 Q19 1 0.6730 0.4235 0.3389 11.00000 0.05 0.17 Q20 1 0.8600 0.1495 0.1491 11.00000 0.05 0.17 ; _shelx_res_checksum 13489 _shelx_hkl_file ; -1 -1 0 499.42 20.64 1 -1 0 641.39 20.41 1 1 0 604.80 20.44 0 2 0 9.91 0.36 0 2 0 9.43 0.37 2 0 0 9.12 0.35 -2 0 0 9.81 0.42 0 -2 0 10.31 0.40 -2 0 0 9.96 0.38 2 0 0 9.70 0.42 0 2 0 10.19 0.37 -2 -1 0 375.88 13.37 2 -1 0 350.66 13.36 2 1 0 375.77 13.36 -1 2 0 373.22 13.15 1 2 0 384.56 13.22 1 -2 0 382.96 13.19 -1 -2 0 361.03 13.18 2 -2 0 198.83 7.46 -2 -2 0 202.60 7.52 2 2 0 198.22 7.47 0 3 0 -0.23 0.13 0 3 0 -0.13 0.13 3 0 0 0.09 0.08 0 3 0 0.18 0.10 0 -3 0 0.02 0.12 1 3 0 18.46 0.69 -3 1 0 17.80 0.69 -1 3 0 19.97 0.68 -3 1 0 17.52 0.69 1 3 0 20.78 0.74 -1 3 0 19.62 0.67 3 1 0 19.07 0.68 3 1 0 17.26 0.66 1 -3 0 19.85 0.72 3 -1 0 17.09 0.65 -1 -3 0 20.39 0.73 -3 -1 0 17.41 0.69 -3 -1 0 16.43 0.76 1 3 0 18.78 0.68 3 -1 0 16.60 0.75 3 1 0 17.51 0.77 -3 1 0 16.96 0.76 -1 3 0 18.10 0.69 -1 3 0 18.70 0.72 2 -3 0 457.66 16.18 2 3 0 462.45 16.20 -3 -2 0 442.19 16.34 -2 3 0 465.35 16.15 3 -2 0 446.05 16.35 3 2 0 443.79 16.31 -2 -3 0 438.01 16.17 3 3 0 14.00 0.55 -3 3 0 13.15 0.55 3 -3 0 12.13 0.51 3 3 0 13.07 0.54 3 -3 0 12.24 0.63 -3 3 0 12.83 0.58 -3 -3 0 15.90 0.68 -3 3 0 13.21 0.65 -3 -3 0 14.93 0.56 0 4 0 12.82 0.52 -4 0 0 10.34 0.54 4 0 0 11.76 0.47 0 4 0 13.84 0.49 0 -4 0 13.65 0.58 0 4 0 12.77 0.53 -4 1 0 76.73 2.82 -4 -1 0 77.41 2.76 -1 4 0 73.72 2.75 1 4 0 76.11 2.75 -4 1 0 78.53 2.75 -1 4 0 79.40 2.74 4 1 0 78.30 2.73 4 1 0 80.87 2.75 4 1 0 79.73 2.83 4 -1 0 76.81 2.82 -4 -1 0 73.57 2.82 -4 1 0 79.64 2.76 -1 4 0 80.77 2.74 4 -1 0 78.30 2.72 1 -4 0 79.05 2.78 1 4 0 81.08 2.80 -1 -4 0 79.89 2.79 1 4 0 75.51 2.74 -2 4 0 5.80 0.41 4 -2 0 4.61 0.45 4 2 0 5.85 0.29 2 4 0 5.58 0.31 2 4 0 5.18 0.33 -2 4 0 5.28 0.35 -4 -2 0 4.95 0.34 -2 4 0 6.07 0.30 -4 2 0 5.24 0.36 -4 2 0 5.89 0.34 -4 2 0 4.51 0.47 -4 -2 0 4.46 0.47 2 -4 0 5.07 0.38 4 -2 0 5.84 0.25 3 -4 0 173.26 6.16 -3 4 0 167.14 6.12 -4 3 0 174.82 6.12 -4 -3 0 171.23 6.11 4 3 0 185.30 6.20 3 4 0 172.66 6.10 4 3 0 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1.13 5 -3 0 31.34 1.08 5 3 0 33.92 1.28 -5 3 0 31.87 1.14 -3 -5 0 30.10 1.12 -5 -3 0 28.17 1.22 5 3 0 30.92 1.10 -3 -5 0 31.46 1.21 -3 5 0 28.75 1.14 -5 3 0 29.83 1.24 3 -5 0 27.93 1.17 -3 5 0 30.69 1.12 5 4 0 46.77 1.68 -4 5 0 47.28 1.70 4 5 0 46.44 1.69 -5 4 0 46.21 1.80 -5 4 0 47.88 1.71 4 5 0 47.66 1.70 4 -5 0 45.69 1.76 -4 -5 0 46.44 1.70 4 5 0 49.13 1.81 5 -4 0 45.67 1.78 -5 4 0 45.85 1.72 5 4 0 47.71 1.70 -4 5 0 45.29 1.71 5 4 0 50.89 1.84 5 -4 0 46.51 1.66 -5 -4 0 45.76 1.79 -5 -4 0 46.05 1.71 -4 -5 0 47.94 1.79 4 -5 0 46.19 1.67 -4 5 0 46.83 1.79 -5 5 0 14.77 0.62 -5 -5 0 13.11 0.61 -5 5 0 14.03 0.65 5 5 0 14.96 0.78 5 5 0 14.63 0.59 5 5 0 14.24 0.61 -5 5 0 14.05 0.74 5 -5 0 13.62 0.71 5 -5 0 14.48 0.55 -5 -5 0 13.66 0.72 0 6 0 15.63 0.67 0 -6 0 16.45 0.74 6 0 0 17.54 0.84 0 6 0 15.92 0.69 6 0 0 17.12 0.63 -6 0 0 16.74 0.82 -6 0 0 17.14 0.71 6 0 0 17.40 0.68 0 -6 0 16.03 0.73 0 6 0 16.02 0.64 -1 6 0 437.89 15.92 -1 -6 0 443.66 15.94 6 -1 0 424.56 16.78 6 1 0 435.07 16.79 -1 6 0 468.64 15.89 6 2 0 94.03 3.36 6 2 0 95.40 3.38 -2 6 0 93.58 3.39 -2 -6 0 95.28 3.43 6 -2 0 92.98 3.35 -2 -6 0 96.02 3.37 2 -6 0 99.14 3.43 2 6 0 98.42 3.39 -2 6 0 103.91 3.37 2 6 0 100.29 3.46 -6 -2 0 94.80 3.39 2 6 0 94.71 3.37 6 2 0 100.33 3.50 -6 2 0 94.97 3.40 6 -2 0 89.25 3.47 -6 -2 0 89.86 3.47 -2 6 0 101.92 3.44 -6 2 0 90.25 3.48 3 -6 0 113.40 4.00 3 6 0 114.58 4.02 6 -3 0 113.44 4.10 -3 -6 0 117.91 4.08 -3 6 0 111.18 4.08 -3 6 0 107.29 4.02 3 6 0 110.97 4.00 6 -3 0 112.76 3.98 -3 6 0 114.66 4.01 -6 3 0 116.70 4.03 3 -6 0 109.66 4.06 6 3 0 123.02 4.14 -6 -3 0 114.70 4.02 6 3 0 108.88 3.99 -3 -6 0 116.49 4.01 6 3 0 121.34 4.01 -6 3 0 111.95 4.12 -6 -3 0 109.02 4.10 3 6 0 118.95 4.10 -6 3 0 114.42 4.03 6 4 0 2.98 0.65 6 -4 0 3.45 0.22 -4 6 0 3.15 0.44 6 4 0 3.32 0.28 -4 -6 0 3.28 0.37 -4 6 0 3.39 0.30 -6 4 0 3.14 0.35 6 -4 0 3.12 0.45 6 4 0 3.16 0.33 -6 -4 0 3.03 0.33 4 -6 0 2.74 0.34 -6 4 0 3.02 0.48 -6 4 0 3.38 0.33 -6 -4 0 2.80 0.46 4 6 0 3.02 0.31 -4 6 0 3.19 0.40 4 6 0 3.35 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68.10 2.44 -9 -2 0 63.67 2.56 2 9 0 68.00 2.54 -2 9 0 66.12 2.45 -2 9 0 66.77 2.41 -9 -2 0 66.00 2.45 2 -9 0 68.48 2.49 9 -2 0 62.03 2.38 9 3 0 14.16 0.87 -3 -9 0 11.87 0.72 -3 -9 0 12.20 0.58 -9 3 0 12.84 0.64 9 -3 0 12.20 0.77 -9 3 0 12.79 0.64 3 9 0 12.62 0.74 3 -9 0 12.22 0.72 -9 -3 0 12.62 0.78 -3 9 0 12.36 0.56 3 9 0 12.24 0.59 9 -3 0 11.60 0.52 -9 3 0 12.46 0.79 9 3 0 12.93 0.63 -3 9 0 11.70 0.61 3 -9 0 12.75 0.67 -9 -3 0 12.57 0.63 9 3 0 12.77 0.55 3 -9 0 11.94 0.55 3 9 0 12.30 0.60 9 4 0 44.93 1.83 -9 4 0 43.57 1.65 9 4 0 43.18 1.60 -4 9 0 44.93 1.73 -4 9 0 43.85 1.65 4 9 0 44.06 1.62 -4 -9 0 46.06 1.74 -9 -4 0 41.42 1.76 9 -4 0 40.09 1.75 9 -4 0 42.78 1.57 4 9 0 43.84 1.63 -9 -4 0 42.60 1.65 -9 4 0 44.43 1.66 -4 -9 0 45.42 1.62 4 -9 0 44.88 1.59 -4 9 0 44.92 1.61 -9 4 0 41.98 1.79 4 -9 0 43.07 1.70 9 4 0 43.69 1.64 5 9 0 31.61 1.32 -5 9 0 29.64 1.27 -9 -5 0 27.21 1.15 -9 5 0 29.03 1.16 9 5 0 29.17 1.11 -5 -9 0 32.06 1.13 -9 5 0 28.55 1.32 -5 -9 0 33.36 1.28 9 -5 0 27.51 1.27 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37.19 1.38 6 -12 0 36.90 1.62 12 -6 0 36.35 1.62 6 12 0 38.64 1.47 -12 6 0 38.15 1.50 -6 -12 0 40.48 1.62 -12 6 0 35.55 1.66 -7 12 0 3.89 0.47 -12 -7 0 3.71 0.57 -7 -12 0 4.62 0.41 12 -7 0 3.12 0.35 7 12 0 4.75 0.43 7 12 0 4.61 0.45 -12 7 0 4.51 0.69 12 7 0 4.32 0.42 7 12 0 4.02 0.72 -7 12 0 3.70 0.43 7 -12 0 3.86 0.36 12 7 0 4.21 0.49 -12 7 0 3.72 0.47 8 12 0 2.48 0.73 8 12 0 3.54 0.45 -8 12 0 3.09 0.43 8 -12 0 3.22 0.34 -12 8 0 2.83 0.47 -12 8 0 2.43 0.48 -12 8 0 3.40 0.70 -8 12 0 3.02 0.67 8 12 0 2.89 0.41 -8 -12 0 3.83 0.42 -12 -8 0 2.37 0.45 -8 12 0 2.80 0.46 -9 12 0 0.10 0.33 9 12 0 0.64 0.33 -12 9 0 -0.22 0.35 -12 9 0 -0.23 0.37 -12 9 0 0.26 0.57 9 12 0 -0.36 0.38 -9 12 0 0.15 0.35 -9 -12 0 0.19 0.36 12 9 0 0.38 0.31 9 12 0 0.30 0.31 9 -12 0 -0.11 0.25 -12 -9 0 0.05 0.35 -12 10 0 2.50 0.53 -10 12 0 2.19 0.48 -12 10 0 1.92 0.48 10 -12 0 1.98 0.36 -12 -10 0 2.44 0.44 10 12 0 2.12 0.41 12 10 0 2.41 0.39 -10 12 0 1.37 0.38 -12 11 0 3.09 0.50 11 12 0 3.52 0.46 -11 12 0 3.82 0.54 11 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5.50 0.55 -3 2 -28 6.20 0.52 2 -3 28 6.13 0.47 2 3 -28 5.01 0.88 -2 3 28 5.37 0.40 -3 2 -28 6.25 0.75 -2 -3 28 5.97 0.40 3 2 -28 5.82 0.72 -2 -3 28 4.91 0.47 2 3 28 6.04 0.53 -3 2 28 6.19 0.58 3 2 -28 5.74 0.78 2 -3 -28 6.01 0.57 2 3 28 6.13 0.43 -2 3 -28 6.07 0.72 -2 3 -28 6.41 0.53 -3 -2 -28 6.70 0.52 3 -3 28 8.61 0.49 -3 3 -28 8.95 0.59 3 3 -28 8.82 0.85 3 -3 -28 8.15 0.64 -3 3 -28 8.58 0.82 3 3 28 8.05 0.50 -3 3 -28 8.73 0.58 -3 3 28 8.77 0.59 3 3 28 8.70 0.62 -3 -3 28 8.81 0.48 -3 -3 28 7.64 0.55 3 3 -28 9.30 0.79 3 3 -28 8.03 0.65 0 -4 -28 8.73 0.63 0 -4 28 7.87 0.56 -4 0 28 9.24 0.59 4 0 -28 7.47 0.91 4 0 -28 9.22 0.83 -4 0 -28 8.87 0.83 0 4 28 8.47 0.49 0 4 -28 10.38 0.79 0 4 28 8.75 0.60 4 0 -28 9.38 1.04 0 4 -28 8.65 0.63 4 0 28 8.85 0.51 0 -4 28 8.77 0.49 4 -1 -28 3.64 0.69 1 -4 28 2.98 0.38 4 1 28 3.40 0.38 -4 1 -28 3.11 0.68 1 4 -28 2.02 0.68 -1 -4 -28 2.35 0.50 -4 1 -28 3.16 0.49 -4 -1 28 2.54 0.31 -1 4 28 3.10 0.44 -1 4 28 2.27 0.35 -4 -1 28 2.92 0.43 1 4 -28 4.20 0.64 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0.62 -4 3 28 7.14 0.55 -3 -4 28 6.81 0.52 4 -3 28 7.14 0.46 4 3 -28 8.17 0.87 4 3 -28 7.95 0.75 3 4 28 7.44 0.59 -3 4 -28 7.42 0.79 -3 4 -28 7.39 0.56 4 3 -28 6.94 0.62 -3 4 -28 7.12 0.56 3 4 28 6.99 0.48 -3 -4 28 7.60 0.46 4 -4 28 1.88 0.30 -4 4 -28 1.81 0.41 4 4 -28 2.23 0.70 -4 4 28 1.51 0.38 -4 4 -28 2.67 0.68 -4 4 -28 2.17 0.45 4 4 28 2.19 0.33 4 4 -28 1.05 0.40 -4 -4 28 2.03 0.40 -4 -4 28 2.24 0.37 -5 0 -28 5.76 1.32 0 5 28 7.40 0.56 5 0 28 6.91 0.45 0 5 28 7.22 0.46 0 -5 28 5.97 0.54 -5 0 -28 6.78 0.60 -5 0 -28 6.41 0.80 0 5 -28 7.43 0.59 0 -5 -28 6.65 0.60 5 0 -28 6.83 0.61 -5 -1 28 1.29 0.37 5 -1 -28 1.14 0.42 -5 1 -28 1.42 0.43 5 1 28 1.74 0.30 1 -5 28 1.54 0.29 -1 5 28 1.61 0.37 -1 -5 -28 1.29 0.42 -5 1 -28 0.96 0.40 1 5 -28 1.52 0.41 -1 5 28 1.08 0.28 1 5 28 1.05 0.36 5 1 -28 1.45 0.43 5 1 -28 1.11 0.52 5 1 -28 1.87 0.66 -1 -5 28 1.08 0.39 5 -1 28 1.91 0.31 1 -5 -28 1.84 0.45 -5 1 28 1.65 0.40 -1 -5 28 1.56 0.29 1 5 28 1.27 0.29 -5 -2 28 32.64 1.34 5 2 28 33.01 1.26 2 5 -28 32.65 1.37 -5 2 -28 33.86 1.61 -5 2 -28 33.41 1.32 2 -5 28 33.68 1.26 5 -2 -28 33.27 1.39 -5 2 -28 27.60 1.60 -5 2 -28 31.46 1.34 -2 5 28 32.05 1.34 2 -5 -28 33.48 1.38 5 2 -28 33.75 1.65 -5 2 28 33.11 1.35 -2 -5 28 30.51 1.31 -2 5 -28 31.44 1.37 2 5 28 32.15 1.26 -5 -2 -28 31.80 1.36 -2 -5 28 33.99 1.26 5 2 -28 31.67 1.53 5 -2 28 34.11 1.26 2 5 28 32.15 1.34 5 2 -28 32.49 1.38 -5 3 -28 9.16 0.66 3 -5 28 10.24 0.54 5 -3 -28 10.82 0.71 -3 5 28 10.20 0.64 5 3 28 10.43 0.56 -5 3 -28 10.97 0.91 -5 -3 28 9.86 0.62 -5 3 -28 10.33 0.63 3 5 -28 9.86 0.71 -5 -3 28 10.88 0.57 -5 3 28 9.89 0.65 5 3 -28 9.61 0.68 -3 -5 28 9.38 0.61 5 -3 28 10.37 0.55 -3 -5 28 10.56 0.55 -5 -3 -28 8.99 0.69 5 3 -28 11.52 0.96 3 -5 -28 9.94 0.70 3 5 28 10.00 0.66 5 3 -28 10.85 0.86 -3 5 -28 9.99 0.65 5 4 28 9.89 0.56 5 -4 -28 10.49 0.72 -4 5 28 10.44 0.66 4 5 -28 10.14 0.71 4 -5 28 10.70 0.55 -5 4 -28 10.34 0.64 -5 -4 28 9.77 0.63 -5 4 -28 8.35 0.66 -5 -4 28 10.66 0.54 5 -4 28 10.47 0.55 4 5 28 10.51 0.57 5 4 -28 11.67 0.86 5 4 -28 9.65 0.71 5 4 -28 11.52 0.97 -5 4 28 10.25 0.67 -5 -4 -28 8.69 0.71 -4 -5 28 11.53 0.56 -4 -5 28 11.02 0.64 4 -5 -28 10.53 0.72 -4 5 -28 10.76 0.66 -5 -5 28 24.52 0.93 5 5 28 22.23 0.93 5 -5 28 21.49 0.91 5 5 -28 21.79 1.05 5 -5 -28 22.54 1.07 -5 5 28 21.16 1.02 -5 5 -28 21.68 1.00 -5 -5 28 20.60 0.99 0 -6 28 8.11 0.47 6 0 -28 6.56 0.62 0 6 -28 7.41 0.60 0 -6 -28 6.30 0.62 6 0 28 6.52 0.47 0 6 28 7.06 0.48 0 6 28 8.25 0.58 -6 0 28 7.51 0.57 1 6 -28 2.53 0.53 -6 -1 28 3.01 0.46 6 -1 -28 3.56 0.55 1 -6 28 3.37 0.37 -6 1 -28 2.19 0.51 -1 6 28 2.33 0.38 6 1 28 3.40 0.39 -1 6 28 3.27 0.48 -1 -6 28 2.79 0.37 -6 -1 -28 2.39 0.53 -6 1 28 3.16 0.46 1 6 28 3.34 0.48 6 1 -28 3.11 0.57 1 6 28 2.61 0.39 6 -1 28 3.10 0.38 1 -6 -28 2.74 0.54 -1 6 -28 3.05 0.51 -2 6 28 3.45 0.47 -6 2 -28 2.13 0.52 2 6 -28 2.79 0.54 6 -2 -28 3.54 0.56 6 2 28 3.80 0.40 2 -6 28 3.03 0.38 -6 -2 28 2.81 0.47 6 -2 28 3.57 0.38 6 2 -28 3.37 0.78 6 2 -28 3.79 0.57 2 -6 -28 2.45 0.49 -2 6 -28 2.43 0.49 -6 2 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0.8094 -0.0946 19 5 16 -1.0407 2.6606 19 5 17 0.4132 -0.4180 19 5 18 0.4065 0.5640 19 5 19 -2.5431 0.1628 19 5 20 0.8173 0.7224 19 5 21 -0.9792 -1.5785 19 6 0 4.0697 0.0000 19 6 1 0.9328 -5.4806 19 6 2 -2.7933 3.7561 19 6 3 -0.2404 3.6452 19 6 4 0.4849 -0.0749 19 6 5 -0.2685 -0.1887 19 6 6 -3.6647 2.0260 19 6 7 -0.6677 1.5043 19 6 8 -3.2332 -2.5507 19 6 9 -2.7611 -2.3072 19 6 10 -1.1519 0.7674 19 6 11 0.0910 2.7329 19 6 12 -0.7334 0.3543 19 6 13 -0.2522 2.5160 19 6 14 -1.6816 3.9397 19 6 15 -0.3641 -0.6063 19 6 16 0.3039 0.7437 19 6 17 0.2348 2.7754 19 6 18 2.8366 -1.0708 19 6 19 1.3394 2.2151 19 7 0 2.0407 0.0000 19 7 1 0.1609 -3.7779 19 7 2 1.0290 0.0526 19 7 3 3.1040 0.5790 19 7 4 1.1304 2.1896 19 7 5 -1.1984 -0.9465 19 7 6 0.4493 -2.4511 19 7 7 -2.3066 1.9534 19 7 8 1.2753 0.5453 19 7 9 -2.4781 0.0322 19 7 10 3.1464 -0.8018 19 7 11 -0.1002 1.8736 19 7 12 1.6853 -1.5535 19 7 13 -1.6642 1.3675 19 7 14 -0.9771 1.0812 19 7 15 -0.8172 0.6622 19 7 16 -0.9199 -2.3942 19 7 17 1.8715 -0.0362 19 7 18 -2.5493 -1.3808 19 8 0 -0.3130 0.0000 19 8 1 0.7736 -2.0279 19 8 2 -1.4918 1.8890 19 8 3 0.1411 -1.4483 19 8 4 -1.6470 -0.0984 19 8 5 -2.0524 1.5403 19 8 6 -0.6755 -3.8563 19 8 7 1.8529 3.4947 19 8 8 0.1312 -1.8690 19 8 9 -1.5527 -0.4828 19 8 10 -0.6050 -0.0524 19 8 11 0.3448 1.2608 19 8 12 0.2872 0.4034 19 8 13 -2.0126 0.2903 19 8 14 0.3026 -1.4572 19 8 15 -0.4048 0.9773 19 8 16 -1.9996 0.4459 19 9 0 2.9763 -0.0000 19 9 1 -0.6080 1.8401 19 9 2 -4.2643 1.7121 19 9 3 0.1469 -0.0224 19 9 4 -2.8302 0.6033 19 9 5 0.9970 1.9757 19 9 6 -2.2197 -1.2800 19 9 7 -1.5346 -2.2369 19 9 8 -0.1622 -1.0395 19 9 9 -1.7204 0.7823 19 9 10 -1.4388 -1.5479 19 9 11 -0.7484 -4.0514 19 9 12 -0.8384 1.0391 19 9 13 0.5783 -0.8957 19 9 14 -1.5669 -1.8786 19 10 0 -2.2191 0.0000 19 10 1 1.3289 0.9389 19 10 2 0.0870 1.1048 19 10 3 2.1350 0.6740 19 10 4 -3.0632 0.0910 19 10 5 1.0046 -0.1237 19 10 6 0.8127 0.4579 19 10 7 -0.9434 1.0429 19 10 8 2.7829 1.8999 19 10 9 -2.2790 2.4732 19 10 10 -2.2575 2.2436 19 10 11 -0.9534 1.9389 19 11 0 -2.1124 -0.0000 19 11 1 -1.5440 1.4349 19 11 2 0.0053 -1.3166 19 11 3 -0.1320 -2.0806 19 11 4 -2.1336 -1.0102 19 11 5 -1.1714 0.6983 19 11 6 2.1079 -1.1252 20 0 0 5.3616 0.0000 20 0 1 0.0000 0.6891 20 0 2 1.3304 0.0000 20 0 3 0.0000 1.1986 20 0 4 2.2426 -0.0000 20 0 5 0.0000 3.9588 20 0 6 1.1651 0.0000 20 0 7 0.0000 3.2828 20 0 8 0.6282 -0.0000 20 0 9 0.0000 1.8390 20 0 10 -0.3818 0.0000 20 0 11 0.0000 3.2213 20 0 12 0.1223 -0.0000 20 0 13 0.0000 2.2263 20 0 14 1.6341 -0.0000 20 0 15 -0.0000 -1.8434 20 0 16 0.1594 0.0000 20 0 17 0.0000 1.0776 20 0 18 -1.0272 0.0000 20 0 19 -0.0000 -1.1986 20 1 0 -2.6203 -0.0000 20 1 1 -0.4549 -0.8972 20 1 2 -1.0592 -1.5439 20 1 3 -0.3658 -1.4060 20 1 4 0.4005 -1.1608 20 1 5 1.0279 -2.4453 20 1 6 -2.0472 2.3836 20 1 7 -3.6561 0.2170 20 1 8 1.5756 4.3189 20 1 9 0.9573 0.8217 20 1 10 -0.8500 2.9484 20 1 11 1.1856 -0.5990 20 1 12 2.9545 -0.4758 20 1 13 -0.2331 -0.3366 20 1 14 -0.6492 -0.9094 20 1 15 0.9329 1.4541 20 1 16 -0.0922 -0.4844 20 1 17 -2.3186 -0.9648 20 1 18 1.0950 0.1025 20 1 19 -2.6991 -0.0265 20 2 0 0.2802 -0.0000 20 2 1 1.1861 0.1292 20 2 2 0.4199 -1.0724 20 2 3 -0.6114 -3.1349 20 2 4 -0.6527 1.8736 20 2 5 0.7873 0.8934 20 2 6 -1.0747 1.0282 20 2 7 -0.0112 0.3137 20 2 8 1.7223 1.3178 20 2 9 -1.6848 1.8309 20 2 10 0.8229 -0.5903 20 2 11 0.8308 3.4877 20 2 12 2.2997 -1.1021 20 2 13 1.2235 -1.3208 20 2 14 1.7252 2.0582 20 2 15 -0.8788 0.4820 20 2 16 0.7109 -1.0409 20 2 17 -0.8147 -1.6725 20 2 18 1.7833 1.6019 20 2 19 -2.5595 -1.4518 20 3 0 2.1265 -0.0000 20 3 1 -2.9090 4.1782 20 3 2 -1.6053 0.3974 20 3 3 -2.0558 -1.6668 20 3 4 -1.0401 0.5250 20 3 5 -0.9834 -1.4593 20 3 6 3.0612 1.6259 20 3 7 -1.0699 -2.5667 20 3 8 2.8032 -2.9551 20 3 9 -1.9289 2.1136 20 3 10 0.3789 -0.2796 20 3 11 2.1235 0.1536 20 3 12 1.9426 0.5243 20 3 13 -1.1568 -1.2163 20 3 14 2.5135 2.8858 20 3 15 3.1771 2.3005 20 3 16 -0.6713 0.5655 20 3 17 1.5866 2.4485 20 3 18 0.4160 1.2269 20 4 0 -4.7132 -0.0000 20 4 1 -0.5465 -0.3616 20 4 2 1.3961 -1.0338 20 4 3 0.1234 2.2617 20 4 4 -0.1483 -1.5667 20 4 5 -1.6780 -1.1076 20 4 6 1.6705 0.2299 20 4 7 0.1841 -0.6215 20 4 8 -0.0003 -0.4163 20 4 9 -0.8647 -0.7650 20 4 10 0.4996 -1.0913 20 4 11 2.1793 -0.6492 20 4 12 0.8638 -2.4531 20 4 13 -0.5149 -2.0451 20 4 14 -0.6903 0.4721 20 4 15 4.8533 -0.3662 20 4 16 -0.1036 -0.1469 20 4 17 1.2809 -2.7393 20 5 0 -0.7717 0.0000 20 5 1 2.4859 -1.9976 20 5 2 0.1636 0.8977 20 5 3 -3.3944 0.0103 20 5 4 0.7476 -2.6930 20 5 5 -1.0925 0.5328 20 5 6 -1.0597 -1.4037 20 5 7 1.0528 1.9955 20 5 8 1.6204 2.6695 20 5 9 -0.2281 -1.9422 20 5 10 -1.0527 0.2403 20 5 11 -1.4738 2.2496 20 5 12 1.8707 -0.7723 20 5 13 1.8314 -0.3028 20 5 14 0.3560 1.2165 20 5 15 -0.8018 0.6662 20 5 16 -0.9759 -1.5573 20 6 0 -1.6060 -0.0000 20 6 1 -1.0376 -1.1336 20 6 2 1.4561 3.5399 20 6 3 -2.5236 -2.3881 20 6 4 -0.9155 3.2815 20 6 5 2.6303 -0.2108 20 6 6 0.3665 1.3478 20 6 7 0.3822 -0.9794 20 6 8 0.1513 1.0168 20 6 9 -1.0002 -0.1391 20 6 10 -1.3146 1.2711 20 6 11 -2.9706 -0.1634 20 6 12 -3.5524 -3.2865 20 6 13 -1.0981 -4.0017 20 6 14 1.0345 0.5400 20 6 15 -0.0268 -2.1561 20 7 0 -0.7937 -0.0000 20 7 1 0.7093 -0.3328 20 7 2 -2.0213 -0.4047 20 7 3 0.8576 -2.1303 20 7 4 1.0750 -0.9490 20 7 5 2.3153 -2.1069 20 7 6 -1.4776 -1.6765 20 7 7 -2.1144 2.0742 20 7 8 -0.9957 -1.6311 20 7 9 -1.6544 2.9666 20 7 10 -0.6612 0.3465 20 7 11 -0.5951 2.5408 20 7 12 -3.2193 -0.2964 20 7 13 -3.1172 2.4293 20 8 0 -0.1807 -0.0000 20 8 1 0.9261 -0.4593 20 8 2 1.7963 -1.7070 20 8 3 3.2271 -5.0128 20 8 4 -0.3270 1.2918 20 8 5 -0.4551 0.1870 20 8 6 -0.3787 -1.0743 20 8 7 0.6628 1.0329 20 8 8 1.3149 0.3792 20 8 9 -1.7099 0.2607 20 8 10 0.9245 2.7515 20 9 0 1.1891 0.0000 20 9 1 0.5871 -0.3716 20 9 2 -3.8503 -0.9672 20 9 3 1.7000 -2.0990 20 9 4 -2.1265 2.5839 20 9 5 1.0379 -0.0636 20 9 6 -1.2463 -0.9381 21 0 1 0.9461 0.0000 21 0 2 0.0000 1.0110 21 0 3 1.5254 0.0000 21 0 4 -0.0000 -0.7249 21 0 5 3.4314 -0.0000 21 0 6 -0.0000 -0.4387 21 0 7 0.1464 0.0000 21 0 8 0.0000 0.3776 21 0 9 -0.4997 -0.0000 21 0 10 0.0000 2.1933 21 0 11 0.1839 0.0000 21 0 12 0.0000 3.2221 21 0 13 0.5493 0.0000 21 0 14 0.0000 0.5961 21 1 0 -0.9451 0.0000 21 1 1 -1.1260 1.0427 21 1 2 2.6128 -1.1984 21 1 3 1.3125 2.0672 21 1 4 -1.3398 -0.3665 21 1 5 0.7415 1.8329 21 1 6 -0.5624 1.0865 21 1 7 -0.7331 -0.1700 21 1 8 1.5926 1.4283 21 1 9 2.2400 -2.6728 21 1 10 -0.9534 2.2950 21 1 11 -0.3004 -2.3773 21 1 12 -0.3702 1.8947 21 1 13 0.6091 0.8573 21 1 14 -2.0528 -0.9922 21 2 0 0.4161 -0.0000 21 2 1 -1.1338 0.9021 21 2 2 -2.2721 0.7674 21 2 3 -1.5711 -0.7849 21 2 4 -0.3123 2.9491 21 2 5 -2.1075 0.0978 21 2 6 -1.0616 -0.5248 21 2 7 -0.9098 0.9121 21 2 8 -0.4701 -0.3704 21 2 9 -0.2915 -0.5223 21 2 10 -0.9021 -0.6687 21 2 11 0.4813 -0.0444 21 2 12 -1.6667 1.1738 21 2 13 0.0808 -0.9375 21 3 0 0.6751 0.0000 21 3 1 -0.8517 -0.1485 21 3 2 1.2835 -3.4076 21 3 3 0.5641 0.1304 21 3 4 -1.4730 -0.0804 21 3 5 -2.0599 -4.6727 21 3 6 1.0984 -0.0595 21 3 7 -1.8876 1.0845 21 3 8 -0.1162 1.2379 21 3 9 -3.2569 0.3235 21 3 10 2.1936 2.6519 21 3 11 4.7890 2.2705 21 3 12 -0.6491 0.5649 21 3 13 0.3501 2.0629 21 4 0 -3.2590 -0.0000 21 4 1 -1.7694 -0.0981 21 4 2 -3.7895 2.3765 21 4 3 0.0324 1.7272 21 4 4 -1.1915 -1.0868 21 4 5 0.6796 1.0639 21 4 6 1.4137 1.3541 21 4 7 1.4764 1.3715 21 4 8 2.1790 -1.1511 21 4 9 1.0220 -3.2286 21 4 10 0.3087 -1.1089 21 4 11 -0.5719 -1.2340 21 4 12 -3.2927 -1.5481 21 5 0 0.1996 0.0000 21 5 1 -0.5284 -1.8675 21 5 2 -2.5049 1.4300 21 5 3 -2.1902 -1.3105 21 5 4 0.9940 -1.0713 21 5 5 0.1749 -0.9962 21 5 6 -4.3327 -2.1014 21 5 7 -0.7826 -3.3521 21 5 8 1.3189 -0.5371 21 5 9 1.5557 0.6167 21 5 10 -1.3454 1.2903 21 6 0 -5.3100 0.0000 21 6 1 -1.6944 2.0920 21 6 2 -1.7415 -0.4650 21 6 3 -1.1778 1.9256 21 6 4 -5.4359 -0.6286 21 6 5 -3.0076 4.2810 21 6 6 0.3545 2.0312 21 6 7 1.6588 -0.1299 21 7 0 -0.9646 0.0000 21 7 1 2.8261 1.4506 21 7 2 0.1130 1.8626 22 0 0 3.3359 0.0000 22 0 1 0.0000 1.9639 22 0 2 1.6790 0.0000 22 0 3 0.0000 1.4212 22 0 4 1.2753 0.0000 22 0 5 0.0000 1.7097 22 1 0 1.3869 -0.0000 22 1 1 1.2518 -0.1677 22 1 2 2.6317 -0.5571 22 1 3 0.0596 1.0578 22 1 4 1.1516 -1.7896 22 1 5 0.0334 -1.5050 22 2 0 1.7213 -0.0000 22 2 1 0.5499 -2.6081 22 2 2 0.1934 -0.3008 22 2 3 1.6502 2.3526 ; _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #END data_MOF520_after_closing_the_DAC _chemical_name_common 'MOF-520_10-4 GPa' _chemical_name_systematic ? _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0090 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.1200 0.1100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 94 _space_group_name_H-M_alt 'P 42 21 2' _space_group_name_Hall 'P 4n 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 18.920(3) _cell_length_b 18.920(3) _cell_length_c 37.190(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13313(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2476 _cell_measurement_theta_max 13.43 _cell_measurement_theta_min 2.27 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.567 _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 0.029 _shelx_estimated_absorpt_T_max 0.7437 _shelx_estimated_absorpt_T_min 0.4612 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_correction_T_min 0.4612 _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1346 before and 0.0833 after correction. The Ratio of minimum to maximum transmission is 0.6201. The \l/2 correction factor is Not present. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Perkin Elmer CMOS' _diffrn_measurement_method '\w 80 degrees scan' _diffrn_detector_area_resol_mean ? _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 0.0001 GPa was measured via ruby method. The sample was collected by rotating 80 degrees. The data sets were merged in XPREP to produce the final data set. ; _diffrn_reflns_number 13052 _diffrn_reflns_av_R_equivalents 0.1343 _diffrn_reflns_av_unetI/netI 0.1762 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_theta_full 17.311 _diffrn_reflns_theta_max 13.660 _diffrn_reflns_theta_min 1.062 _diffrn_measured_fraction_theta_full 0.436 _diffrn_measured_fraction_theta_max 0.849 _diffrn_reflns_Laue_measured_fraction_full 0.436 _diffrn_reflns_Laue_measured_fraction_max 0.849 _diffrn_reflns_point_group_measured_fraction_full 0.424 _diffrn_reflns_point_group_measured_fraction_max 0.851 _reflns_number_total 5124 _reflns_number_gt 2572 _diffrn_standards_number 0 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.730 _reflns_Friedel_fraction_full 0.410 _reflns_Friedel_fraction_max 0.853 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_diff_density_max 0.075 _refine_diff_density_min -0.099 _refine_diff_density_rms 0.013 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack 0.70(13) _refine_ls_extinction_coef 0.0018(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.669 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 363 _refine_ls_number_reflns 5124 _refine_ls_number_restraints 324 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0407 _refine_ls_restrained_S_all 0.672 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.0918 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2 3. Rigid body (RIGU) restrains C5, Al1, O1, O10, Al2, O2, O3, Al3, C1, O4, C2, C7, C3, H7, C6, H3, C4, H6, H4, C8, C9, C13, C10, H9, H13, C12, C14, C11, C21, C19, C15, H11, C26, C22, C18, H19, C16, H15, H26, C25, C23, H22, C17, H18, H16, H25, C24, H23, C20, O5, C27, O6, O8, O7, Al1, O1, Al1, O10, Al2, O1, O1, O10, Al2, O2, Al2, O3, Al2, Al3, O2, O2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C3, C2, C7, H7, C7, C6, C3, H3, C4, C3, C6, C5, C6, H6, C5, C4, C4, H4, C8, C5, C8, C13, C9, C8, C9, C10, C9, H9, C13, H13, C13, C12, C14, C10, C11, C10, C21, C12, C12, C11, C19, C14, C15, C14, C11, H11, C26, C21, C22, C21, C19, C18, C19, H19, C16, C15, C15, H15, C26, H26, C26, C25, C23, C22, C22, H22, C18, C17, C18, H18, C17, C16, C16, H16, C25, H25, C25, C24, C23, H23, C24, C23, C20, C17, C27, C24, O5, C20, O6, C20, O8, C27, O7, C27 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C0AA, O0AA, O10 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Aromatic/amide H refined with riding coordinates: C26(H26), C23(H23), C25(H25), C22(H22), C7(H7), C16(H16), C18(H18), C3(H3), C4(H4), C6(H6), C13(H13), C19(H19), C15(H15), C11(H11), C9(H9), C0AA(H0AA) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.66019(10) 0.33981(10) 0.5000 0.0695(12) Uani 1 2 d S TU P . . Al2 Al 0.63132(10) 0.40952(10) 0.41912(9) 0.0775(10) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38061(11) 0.0603(11) Uani 1 2 d S TU P . . O2 O 0.56711(16) 0.48370(16) 0.41636(14) 0.0598(15) Uani 1 1 d . U . . . O3 O 0.6641(2) 0.4304(2) 0.3705(2) 0.0915(19) Uani 1 1 d . U . . . O1 O 0.60316(19) 0.38326(18) 0.46291(14) 0.0707(16) Uani 1 1 d . U . . . O4 O 0.5670(2) 0.4861(2) 0.34289(16) 0.0780(18) Uani 1 1 d . U . . . C1 C 0.6277(5) 0.4642(4) 0.3422(3) 0.093(3) Uani 1 1 d . U . . . C26 C 0.8082(3) 0.6617(4) 0.1522(3) 0.115(3) Uani 1 1 d . U . . . H26 H 0.8047 0.6711 0.1767 0.138 Uiso 1 1 calc R U . . . C23 C 0.8096(4) 0.6462(4) 0.0705(3) 0.122(4) Uani 1 1 d . U . . . H23 H 0.8136 0.6391 0.0459 0.147 Uiso 1 1 calc R U . . . C20 C 1.0119(5) 0.1540(4) 0.1139(3) 0.079(3) Uani 1 1 d . U . . . C25 C 0.8062(5) 0.7188(5) 0.1214(3) 0.102(4) Uani 1 1 d . U . . . H25 H 0.8111 0.7648 0.1298 0.123 Uiso 1 1 calc R U . . . C22 C 0.8133(5) 0.5852(5) 0.0996(4) 0.135(4) Uani 1 1 d . U . . . H22 H 0.8138 0.5387 0.0915 0.162 Uiso 1 1 calc R U . . . C24 C 0.7992(5) 0.7155(6) 0.0877(4) 0.101(4) Uani 1 1 d . U . . . C27 C 0.8004(5) 0.7742(7) 0.0664(4) 0.085(4) Uani 1 1 d . U . . . C17 C 0.9718(4) 0.2243(4) 0.1291(3) 0.090(3) Uani 1 1 d . U . . . C7 C 0.6441(4) 0.4981(3) 0.2816(3) 0.084(3) Uani 1 1 d . U . . . H7 H 0.6009 0.5210 0.2837 0.101 Uiso 1 1 calc R U . . . C21 C 0.8158(4) 0.5977(6) 0.1375(4) 0.110(4) Uani 1 1 d . U . . . C5 C 0.7485(5) 0.4612(4) 0.2468(3) 0.098(3) Uani 1 1 d . U . . . C16 C 0.9044(4) 0.2113(4) 0.1462(3) 0.107(3) Uani 1 1 d . U . . . H16 H 0.8834 0.1670 0.1481 0.129 Uiso 1 1 calc R U . . . C8 C 0.7896(4) 0.4695(4) 0.2118(3) 0.095(3) Uani 1 1 d . U . . . C2 C 0.6717(4) 0.4609(4) 0.3095(3) 0.079(3) Uani 1 1 d . U . . . C18 C 1.0045(3) 0.2884(4) 0.1252(2) 0.085(3) Uani 1 1 d . U . . . H18 H 1.0489 0.2917 0.1146 0.102 Uiso 1 1 calc R U . . . C3 C 0.7379(5) 0.4255(3) 0.3048(3) 0.099(3) Uani 1 1 d . U . . . H3 H 0.7553 0.3995 0.3241 0.119 Uiso 1 1 calc R U . . . C4 C 0.7738(5) 0.4271(4) 0.2768(4) 0.103(3) Uani 1 1 d . U . . . H4 H 0.8177 0.4051 0.2761 0.123 Uiso 1 1 calc R U . . . C14 C 0.9061(5) 0.3442(4) 0.1554(3) 0.110(4) Uani 1 1 d . U . . . C6 C 0.6851(4) 0.5008(4) 0.2476(3) 0.114(3) Uani 1 1 d . U . . . H6 H 0.6699 0.5271 0.2279 0.136 Uiso 1 1 calc R U . . . C13 C 0.7887(4) 0.5302(4) 0.1851(3) 0.090(3) Uani 1 1 d . U . . . H13 H 0.7584 0.5679 0.1896 0.108 Uiso 1 1 calc R U . . . C19 C 0.9671(4) 0.3525(4) 0.1384(2) 0.084(3) Uani 1 1 d . U . . . H19 H 0.9861 0.3973 0.1348 0.100 Uiso 1 1 calc R U . . . C10 C 0.8735(4) 0.4104(4) 0.1701(3) 0.096(3) Uani 1 1 d . U . . . C15 C 0.8713(4) 0.2813(4) 0.1610(3) 0.106(3) Uani 1 1 d . U . . . H15 H 0.8287 0.2803 0.1735 0.127 Uiso 1 1 calc R U . . . C12 C 0.8272(4) 0.5323(5) 0.1569(3) 0.096(3) Uani 1 1 d . U . . . C11 C 0.8639(4) 0.4713(4) 0.1470(3) 0.107(3) Uani 1 1 d . U . . . H11 H 0.8835 0.4697 0.1240 0.129 Uiso 1 1 calc R U . . . C9 C 0.8299(4) 0.4077(4) 0.2013(3) 0.087(3) Uani 1 1 d . U . . . H9 H 0.8273 0.3665 0.2149 0.104 Uiso 1 1 calc R U . . . O8 O 0.80066(18) 0.8386(2) 0.08543(16) 0.0763(19) Uani 1 1 d . U . . . O10 O 0.73561(18) 0.40784(19) 0.49010(16) 0.0840(19) Uani 1 1 d . U . . . O5 O 1.0665(3) 0.1595(2) 0.10067(17) 0.081(2) Uani 1 1 d . U . . . O6 O 0.9730(2) 0.0975(2) 0.12222(15) 0.0701(17) Uani 1 1 d . U . . . O7 O 0.8022(3) 0.7737(3) 0.0364(2) 0.084(3) Uani 1 1 d . U . . . O0AA O 0.7008(3) 0.4734(3) 0.4339(2) 0.093(3) Uani 1 1 d . U . . . C0AA C 0.7311(6) 0.4664(7) 0.4580(4) 0.163(6) Uani 1 1 d . U . . . H0AA H 0.7630 0.5032 0.4614 0.196 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0689(12) 0.0689(12) 0.071(4) -0.0090(14) -0.0090(14) -0.0016(14) Al2 0.0776(17) 0.0618(15) 0.093(4) -0.0009(16) -0.0072(16) 0.0096(11) Al3 0.064(2) 0.061(2) 0.055(4) 0.000 0.000 0.0024(13) O2 0.064(3) 0.051(3) 0.064(5) -0.008(2) 0.010(3) 0.0107(17) O3 0.109(4) 0.074(4) 0.091(6) 0.006(3) 0.016(4) 0.002(2) O1 0.081(3) 0.072(3) 0.060(5) 0.001(3) -0.017(3) 0.006(2) O4 0.084(4) 0.100(4) 0.050(6) 0.000(3) 0.007(3) -0.004(3) C1 0.098(6) 0.090(6) 0.090(8) -0.003(5) 0.007(5) -0.014(5) C26 0.135(7) 0.081(6) 0.129(10) 0.017(6) -0.005(6) 0.004(5) C23 0.153(7) 0.094(6) 0.120(11) -0.005(6) 0.014(6) -0.010(5) C20 0.109(6) 0.062(5) 0.067(9) -0.008(4) 0.013(6) 0.017(4) C25 0.118(7) 0.076(6) 0.113(10) 0.002(6) 0.016(7) 0.031(4) C22 0.172(8) 0.098(7) 0.134(11) 0.001(7) -0.002(8) -0.005(5) C24 0.096(6) 0.088(6) 0.118(10) 0.007(6) 0.011(7) -0.020(5) C27 0.048(5) 0.095(6) 0.111(10) 0.003(6) 0.000(7) -0.013(4) C17 0.133(6) 0.068(5) 0.070(10) -0.015(5) 0.013(5) 0.014(4) C7 0.099(6) 0.075(5) 0.078(9) 0.002(5) 0.021(5) 0.023(4) C21 0.095(6) 0.098(6) 0.137(10) 0.016(6) 0.017(7) -0.005(5) C5 0.098(6) 0.089(6) 0.107(9) 0.020(5) 0.025(5) 0.020(4) C16 0.134(7) 0.099(6) 0.089(11) 0.008(5) 0.025(6) 0.023(5) C8 0.097(6) 0.086(6) 0.102(9) 0.010(5) 0.014(5) 0.004(4) C2 0.089(6) 0.071(6) 0.076(8) -0.001(5) 0.011(5) -0.002(4) C18 0.099(5) 0.077(5) 0.078(10) 0.010(5) 0.012(5) 0.016(4) C3 0.109(7) 0.080(5) 0.108(10) 0.033(6) 0.032(5) 0.021(4) C4 0.110(7) 0.100(7) 0.098(10) 0.017(6) 0.025(6) 0.014(5) C14 0.110(7) 0.085(6) 0.136(11) -0.002(5) 0.035(6) 0.020(5) C6 0.111(7) 0.144(7) 0.086(10) 0.034(6) 0.021(5) 0.041(5) C13 0.073(6) 0.086(5) 0.112(10) 0.012(5) 0.014(5) 0.012(4) C19 0.098(6) 0.078(5) 0.075(10) -0.009(5) -0.003(5) 0.013(4) C10 0.098(6) 0.090(5) 0.101(10) -0.006(5) 0.003(5) -0.007(4) C15 0.101(6) 0.108(6) 0.108(11) -0.003(6) -0.006(5) 0.025(5) C12 0.086(7) 0.090(6) 0.112(10) 0.002(5) 0.006(5) -0.007(4) C11 0.124(7) 0.091(6) 0.107(10) 0.007(5) 0.041(6) 0.007(5) C9 0.094(6) 0.068(5) 0.098(9) 0.007(5) 0.009(5) -0.004(4) O8 0.066(3) 0.063(3) 0.100(7) 0.019(3) 0.007(3) -0.012(2) O10 0.072(3) 0.071(3) 0.109(7) -0.005(3) -0.003(3) -0.014(2) O5 0.095(4) 0.060(3) 0.088(7) -0.024(3) 0.016(4) 0.011(3) O6 0.097(3) 0.051(3) 0.062(6) -0.010(3) -0.005(3) 0.010(2) O7 0.093(4) 0.057(3) 0.104(8) 0.006(4) 0.007(5) -0.010(2) O0AA 0.082(4) 0.085(4) 0.113(9) -0.002(4) -0.019(4) -0.012(3) C0AA 0.175(10) 0.167(9) 0.147(10) 0.013(7) -0.029(7) -0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.935(4) 8_666 ? Al1 O1 1.935(4) . ? Al1 O10 1.957(4) . ? Al1 O10 1.957(4) 8_666 ? Al1 O7 1.976(7) 2_645 ? Al1 O7 1.976(7) 6_645 ? Al2 O2 1.859(4) . ? Al2 O3 1.950(7) . ? Al2 O1 1.784(5) . ? Al2 O8 1.867(4) 6_645 ? Al2 O5 1.936(5) 5_455 ? Al2 O0AA 1.867(6) . ? Al3 O2 1.864(6) 3_665 ? Al3 O2 1.864(6) . ? Al3 O4 1.909(6) 3_665 ? Al3 O4 1.909(6) . ? Al3 O6 1.916(4) 5_455 ? Al3 O6 1.916(4) 6_655 ? O3 C1 1.413(11) . ? O4 C1 1.221(9) . ? C1 C2 1.475(13) . ? C26 C25 1.574(12) . ? C26 C21 1.338(11) . ? C23 C22 1.580(13) . ? C23 C24 1.471(12) . ? C20 C17 1.633(10) . ? C20 O5 1.148(7) . ? C20 O6 1.336(8) . ? C25 C24 1.263(14) . ? C22 C21 1.433(14) . ? C24 C27 1.364(14) . ? C27 O8 1.410(12) . ? C27 O7 1.114(13) . ? C17 C16 1.444(9) . ? C17 C18 1.370(8) . ? C7 C2 1.358(12) . ? C7 C6 1.483(11) . ? C21 C12 1.446(13) . ? C5 C8 1.525(13) . ? C5 C4 1.374(14) . ? C5 C6 1.415(9) . ? C16 C15 1.567(9) . ? C8 C13 1.516(11) . ? C8 C9 1.450(9) . ? C2 C3 1.430(9) . ? C18 C19 1.487(8) . ? C3 C4 1.244(12) . ? C14 C19 1.327(9) . ? C14 C10 1.499(10) . ? C14 C15 1.376(8) . ? C13 C12 1.280(12) . ? C10 C11 1.449(11) . ? C10 C9 1.426(11) . ? C12 C11 1.396(9) . ? O8 Al2 1.867(4) 6_655 ? O10 C0AA 1.633(13) . ? O5 Al2 1.936(5) 5 ? O6 Al3 1.916(4) 5 ? O7 Al1 1.976(7) 4_564 ? O0AA C0AA 1.071(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 92.0(3) 8_666 . ? O1 Al1 O10 94.42(19) . 8_666 ? O1 Al1 O10 89.6(2) . . ? O1 Al1 O10 89.6(2) 8_666 8_666 ? O1 Al1 O10 94.43(19) 8_666 . ? O1 Al1 O7 88.9(2) 8_666 2_645 ? O1 Al1 O7 88.9(2) . 6_645 ? O1 Al1 O7 174.1(2) 8_666 6_645 ? O1 Al1 O7 174.1(2) . 2_645 ? O10 Al1 O10 174.2(3) 8_666 . ? O10 Al1 O7 84.5(2) 8_666 6_645 ? O10 Al1 O7 84.5(2) . 2_645 ? O10 Al1 O7 91.4(2) . 6_645 ? O10 Al1 O7 91.4(2) 8_666 2_645 ? O7 Al1 O7 90.8(4) 2_645 6_645 ? O2 Al2 O3 90.2(2) . . ? O2 Al2 O8 171.1(3) . 6_645 ? O2 Al2 O5 94.3(2) . 5_455 ? O2 Al2 O0AA 89.3(2) . . ? O1 Al2 O2 93.8(2) . . ? O1 Al2 O3 175.4(2) . . ? O1 Al2 O8 95.1(2) . 6_645 ? O1 Al2 O5 88.3(2) . 5_455 ? O1 Al2 O0AA 97.0(3) . . ? O8 Al2 O3 80.9(2) 6_645 . ? O8 Al2 O5 85.3(2) 6_645 5_455 ? O8 Al2 O0AA 90.4(2) 6_645 . ? O5 Al2 O3 89.2(3) 5_455 . ? O0AA Al2 O3 85.3(3) . . ? O0AA Al2 O5 173.4(3) . 5_455 ? O2 Al3 O2 89.0(3) . 3_665 ? O2 Al3 O4 177.8(3) . 3_665 ? O2 Al3 O4 92.8(2) . . ? O2 Al3 O4 177.8(3) 3_665 . ? O2 Al3 O4 92.8(2) 3_665 3_665 ? O2 Al3 O6 93.53(19) . 5_455 ? O2 Al3 O6 93.53(19) 3_665 6_655 ? O2 Al3 O6 90.96(17) . 6_655 ? O2 Al3 O6 90.96(17) 3_665 5_455 ? O4 Al3 O4 85.4(4) . 3_665 ? O4 Al3 O6 85.1(2) 3_665 5_455 ? O4 Al3 O6 85.1(2) . 6_655 ? O4 Al3 O6 90.2(2) . 5_455 ? O4 Al3 O6 90.2(2) 3_665 6_655 ? O6 Al3 O6 173.7(4) 5_455 6_655 ? Al2 O2 Al3 127.5(3) . . ? C1 O3 Al2 128.9(6) . . ? Al2 O1 Al1 127.1(2) . . ? C1 O4 Al3 133.4(7) . . ? O3 C1 C2 108.8(9) . . ? O4 C1 O3 126.5(10) . . ? O4 C1 C2 124.3(11) . . ? C21 C26 C25 109.1(11) . . ? C24 C23 C22 111.2(11) . . ? O5 C20 C17 119.6(8) . . ? O5 C20 O6 131.9(7) . . ? O6 C20 C17 108.3(7) . . ? C24 C25 C26 133.8(11) . . ? C21 C22 C23 123.7(10) . . ? C25 C24 C23 117.4(11) . . ? C25 C24 C27 122.3(13) . . ? C27 C24 C23 118.2(13) . . ? C24 C27 O8 114.3(12) . . ? O7 C27 C24 125.1(14) . . ? O7 C27 O8 120.5(12) . . ? C16 C17 C20 115.1(7) . . ? C18 C17 C20 118.3(8) . . ? C18 C17 C16 126.6(7) . . ? C2 C7 C6 117.9(8) . . ? C26 C21 C22 123.2(12) . . ? C26 C21 C12 126.0(13) . . ? C22 C21 C12 110.8(11) . . ? C4 C5 C8 124.3(9) . . ? C4 C5 C6 121.8(11) . . ? C6 C5 C8 113.3(10) . . ? C17 C16 C15 111.4(6) . . ? C13 C8 C5 129.1(8) . . ? C9 C8 C5 114.4(8) . . ? C9 C8 C13 116.2(9) . . ? C7 C2 C1 113.0(9) . . ? C7 C2 C3 119.1(10) . . ? C3 C2 C1 127.9(10) . . ? C17 C18 C19 118.2(7) . . ? C4 C3 C2 124.7(11) . . ? C3 C4 C5 120.0(11) . . ? C19 C14 C10 115.6(8) . . ? C19 C14 C15 126.3(8) . . ? C15 C14 C10 118.1(8) . . ? C5 C6 C7 116.2(9) . . ? C12 C13 C8 123.6(8) . . ? C14 C19 C18 118.3(7) . . ? C11 C10 C14 120.0(10) . . ? C9 C10 C14 120.2(8) . . ? C9 C10 C11 116.2(8) . . ? C14 C15 C16 119.1(8) . . ? C13 C12 C21 110.5(9) . . ? C13 C12 C11 118.3(10) . . ? C11 C12 C21 130.5(11) . . ? C12 C11 C10 124.2(10) . . ? C10 C9 C8 119.5(8) . . ? C27 O8 Al2 125.3(5) . 6_655 ? C0AA O10 Al1 123.1(5) . . ? C20 O5 Al2 132.2(5) . 5 ? C20 O6 Al3 127.7(5) . 5 ? C27 O7 Al1 133.8(9) . 4_564 ? C0AA O0AA Al2 122.9(10) . . ? O0AA C0AA O10 136.3(13) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.981 -0.582 -0.057 9391.5 9172.6 ? _shelx_res_file ; TITL P1_25keV_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 18.92 18.92 37.19 90 90 90 ZERR 8 0.00268 0.00268 0.00744 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.12 0.11 744.346 DISP C 0.009 0.004 30.879 DISP H -0 0 0.639 DISP O 0.025 0.014 100.516 UNIT 224 144 80 16 RIGU C5 Al1 O1 O10 Al2 O2 O3 Al3 C1 O4 C2 C7 C3 H7 C6 H3 C4 H6 H4 C8 C9 C13 = C10 H9 H13 C12 C14 C11 C21 C19 C15 H11 C26 C22 C18 H19 C16 H15 H26 C25 C23 = H22 C17 H18 H16 H25 C24 H23 C20 O5 C27 O6 O8 O7 AL1 O1 AL1 O10 AL2 O1 O1 O10 = AL2 O2 AL2 O3 AL2 AL3 O2 O2 O3 C1 AL3 O4 O4 C1 C2 C1 C7 C2 C3 C2 C7 H7 C7 C6 = C3 H3 C4 C3 C6 C5 C6 H6 C5 C4 C4 H4 C8 C5 C8 C13 C9 C8 C9 C10 C9 H9 C13 H13 = C13 C12 C14 C10 C11 C10 C21 C12 C12 C11 C19 C14 C15 C14 C11 H11 C26 C21 C22 = C21 C19 C18 C19 H19 C16 C15 C15 H15 C26 H26 C26 C25 C23 C22 C22 H22 C18 C17 = C18 H18 C17 C16 C16 H16 C25 H25 C25 C24 C23 H23 C24 C23 C20 C17 C27 C24 O5 = C20 O6 C20 O8 C27 O7 C27 RIGU C0AA O0AA O10 ISOR 0.01 0.2 C0AA L.S. 24 PLAN 120 TEMP 23 BOND ABIN fmap 2 acta REM REM REM WGHT 0.000000 EXTI 0.001777 FVAR 0.10898 AL1 4 0.660190 0.339810 0.500000 10.50000 0.06891 0.06891 = 0.07080 -0.00898 -0.00898 -0.00161 AL2 4 0.631319 0.409517 0.419120 11.00000 0.07756 0.06185 = 0.09297 -0.00093 -0.00722 0.00964 AL3 4 0.500000 0.500000 0.380613 10.50000 0.06422 0.06143 = 0.05510 0.00000 0.00000 0.00236 O2 3 0.567111 0.483700 0.416362 11.00000 0.06401 0.05115 = 0.06422 -0.00801 0.01040 0.01072 O3 3 0.664104 0.430390 0.370548 11.00000 0.10918 0.07400 = 0.09142 0.00605 0.01625 0.00164 O1 3 0.603160 0.383256 0.462907 11.00000 0.08052 0.07185 = 0.05987 0.00091 -0.01674 0.00642 O4 3 0.567019 0.486077 0.342889 11.00000 0.08429 0.09979 = 0.04990 0.00004 0.00706 -0.00364 C1 1 0.627717 0.464194 0.342174 11.00000 0.09794 0.09045 = 0.08960 -0.00279 0.00708 -0.01351 C26 1 0.808209 0.661743 0.152210 11.00000 0.13510 0.08058 = 0.12872 0.01747 -0.00499 0.00359 AFIX 43 H26 2 0.804689 0.671116 0.176692 11.00000 -1.20000 AFIX 0 C23 1 0.809627 0.646156 0.070550 11.00000 0.15268 0.09368 = 0.12043 -0.00462 0.01394 -0.01012 AFIX 43 H23 2 0.813552 0.639119 0.045881 11.00000 -1.20000 AFIX 0 C20 1 1.011923 0.154014 0.113860 11.00000 0.10906 0.06158 = 0.06678 -0.00798 0.01271 0.01729 C25 1 0.806154 0.718768 0.121394 11.00000 0.11816 0.07597 = 0.11315 0.00188 0.01610 0.03062 AFIX 43 H25 2 0.811110 0.764763 0.129845 11.00000 -1.20000 AFIX 0 C22 1 0.813270 0.585216 0.099550 11.00000 0.17246 0.09758 = 0.13447 0.00057 -0.00182 -0.00476 AFIX 43 H22 2 0.813780 0.538672 0.091514 11.00000 -1.20000 AFIX 0 C24 1 0.799220 0.715452 0.087667 11.00000 0.09602 0.08803 = 0.11764 0.00666 0.01079 -0.01963 C27 1 0.800439 0.774157 0.066372 11.00000 0.04835 0.09550 = 0.11056 0.00309 -0.00026 -0.01338 C17 1 0.971777 0.224274 0.129116 11.00000 0.13289 0.06776 = 0.06991 -0.01466 0.01253 0.01415 C7 1 0.644122 0.498051 0.281563 11.00000 0.09936 0.07519 = 0.07821 0.00228 0.02064 0.02335 AFIX 43 H7 2 0.600879 0.521043 0.283691 11.00000 -1.20000 AFIX 0 C21 1 0.815830 0.597652 0.137529 11.00000 0.09471 0.09838 = 0.13688 0.01627 0.01684 -0.00497 C5 1 0.748519 0.461230 0.246804 11.00000 0.09846 0.08929 = 0.10733 0.02018 0.02514 0.02039 C16 1 0.904419 0.211291 0.146162 11.00000 0.13438 0.09862 = 0.08904 0.00751 0.02482 0.02258 AFIX 43 H16 2 0.883406 0.167011 0.148058 11.00000 -1.20000 AFIX 0 C8 1 0.789620 0.469539 0.211786 11.00000 0.09746 0.08558 = 0.10202 0.00976 0.01375 0.00445 C2 1 0.671722 0.460888 0.309468 11.00000 0.08874 0.07099 = 0.07621 -0.00058 0.01108 -0.00197 C18 1 1.004512 0.288385 0.125236 11.00000 0.09892 0.07696 = 0.07804 0.00952 0.01209 0.01573 AFIX 43 H18 2 1.048917 0.291731 0.114648 11.00000 -1.20000 AFIX 0 C3 1 0.737864 0.425529 0.304793 11.00000 0.10891 0.07968 = 0.10794 0.03292 0.03199 0.02122 AFIX 43 H3 2 0.755290 0.399511 0.324068 11.00000 -1.20000 AFIX 0 C4 1 0.773785 0.427078 0.276774 11.00000 0.11005 0.09991 = 0.09806 0.01660 0.02494 0.01357 AFIX 43 H4 2 0.817742 0.405116 0.276118 11.00000 -1.20000 AFIX 0 C14 1 0.906066 0.344201 0.155440 11.00000 0.10970 0.08463 = 0.13597 -0.00150 0.03471 0.01974 C6 1 0.685073 0.500841 0.247585 11.00000 0.11081 0.14439 = 0.08603 0.03430 0.02062 0.04149 AFIX 43 H6 2 0.669923 0.527124 0.227909 11.00000 -1.20000 AFIX 0 C13 1 0.788682 0.530184 0.185145 11.00000 0.07259 0.08624 = 0.11231 0.01166 0.01393 0.01179 AFIX 43 H13 2 0.758447 0.567940 0.189594 11.00000 -1.20000 AFIX 0 C19 1 0.967136 0.352518 0.138412 11.00000 0.09761 0.07826 = 0.07537 -0.00907 -0.00328 0.01310 AFIX 43 H19 2 0.986090 0.397314 0.134807 11.00000 -1.20000 AFIX 0 C10 1 0.873461 0.410440 0.170071 11.00000 0.09751 0.08963 = 0.10113 -0.00595 0.00277 -0.00680 C15 1 0.871267 0.281293 0.161050 11.00000 0.10123 0.10820 = 0.10805 -0.00315 -0.00556 0.02462 AFIX 43 H15 2 0.828656 0.280348 0.173507 11.00000 -1.20000 AFIX 0 C12 1 0.827193 0.532304 0.156870 11.00000 0.08575 0.09036 = 0.11235 0.00150 0.00575 -0.00708 C11 1 0.863932 0.471329 0.146956 11.00000 0.12418 0.09088 = 0.10735 0.00735 0.04052 0.00653 AFIX 43 H11 2 0.883543 0.469704 0.124041 11.00000 -1.20000 AFIX 0 C9 1 0.829861 0.407675 0.201321 11.00000 0.09402 0.06781 = 0.09769 0.00675 0.00883 -0.00374 AFIX 43 H9 2 0.827265 0.366468 0.214891 11.00000 -1.20000 AFIX 0 O8 3 0.800662 0.838613 0.085426 11.00000 0.06566 0.06314 = 0.10017 0.01936 0.00747 -0.01203 O10 3 0.735606 0.407839 0.490096 11.00000 0.07248 0.07093 = 0.10858 -0.00525 -0.00295 -0.01418 O5 3 1.066518 0.159471 0.100671 11.00000 0.09505 0.06030 = 0.08779 -0.02425 0.01646 0.01053 O6 3 0.972987 0.097461 0.122217 11.00000 0.09730 0.05106 = 0.06195 -0.01029 -0.00475 0.00981 O7 3 0.802208 0.773743 0.036428 11.00000 0.09292 0.05703 = 0.10352 0.00596 0.00736 -0.01046 O0AA 3 0.700775 0.473359 0.433889 11.00000 0.08152 0.08504 = 0.11311 -0.00184 -0.01934 -0.01159 C0AA 1 0.731099 0.466446 0.457956 11.00000 0.17514 0.16703 = 0.14686 0.01322 -0.02939 -0.01564 AFIX 43 H0AA 2 0.763002 0.503212 0.461430 11.00000 -1.20000 AFIX 0 HKLF 4 REM P1_25keV_0m in P42212 #94 REM R1 = 0.0407 for 2572 Fo > 4sig(Fo) and 0.0962 for all 5124 data REM 363 parameters refined using 324 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 0.075, deepest hole -0.099, 1-sigma level 0.013 Q1 1 0.5000 0.5000 0.3940 10.50000 0.05 0.07 Q2 1 0.6190 0.4846 0.4272 11.00000 0.05 0.07 Q3 1 0.4933 0.4623 0.3788 11.00000 0.05 0.07 Q4 1 1.0990 0.2776 0.1305 11.00000 0.05 0.06 Q5 1 0.6166 0.4032 0.4772 11.00000 0.05 0.06 Q6 1 0.5394 0.4725 0.4381 11.00000 0.05 0.06 Q7 1 0.5402 0.4197 0.4651 11.00000 0.05 0.06 Q8 1 0.9812 0.1000 0.1359 11.00000 0.05 0.06 Q9 1 0.5432 0.4273 0.4173 11.00000 0.05 0.05 Q10 1 0.6212 0.5624 0.4142 11.00000 0.05 0.05 Q11 1 0.6225 0.3920 0.4066 11.00000 0.05 0.05 Q12 1 0.5000 0.5000 0.4517 10.50000 0.05 0.05 Q13 1 0.5243 0.3671 0.4449 11.00000 0.05 0.05 Q14 1 0.9001 0.2439 0.1564 11.00000 0.05 0.05 Q15 1 1.0221 0.0861 0.1230 11.00000 0.05 0.05 Q16 1 0.7360 0.5774 0.1019 11.00000 0.05 0.05 Q17 1 0.8503 0.8392 0.1124 11.00000 0.05 0.05 Q18 1 1.0791 0.1872 0.0810 11.00000 0.05 0.05 Q19 1 0.7537 0.3865 0.4745 11.00000 0.05 0.05 Q20 1 0.7187 0.8337 0.0484 11.00000 0.05 0.05 Q21 1 0.6310 0.3663 0.3286 11.00000 0.05 0.05 Q22 1 0.6825 0.4660 0.5123 11.00000 0.05 0.05 Q23 1 0.9141 0.6824 0.1697 11.00000 0.05 0.05 Q24 1 0.8538 0.7150 0.1535 11.00000 0.05 0.05 Q25 1 0.6399 0.4119 0.3543 11.00000 0.05 0.05 Q26 1 0.9005 0.0966 0.1632 11.00000 0.05 0.05 Q27 1 0.6012 0.3482 0.4599 11.00000 0.05 0.04 Q28 1 0.6306 0.3604 0.4453 11.00000 0.05 0.04 Q29 1 1.1002 0.3291 0.0843 11.00000 0.05 0.04 Q30 1 0.5000 0.5000 0.3159 10.50000 0.05 0.04 Q31 1 0.8179 0.8256 0.0685 11.00000 0.05 0.04 Q32 1 0.8159 0.6006 0.0770 11.00000 0.05 0.04 Q33 1 0.9641 0.1515 0.0841 11.00000 0.05 0.04 Q34 1 0.7977 0.2905 0.1974 11.00000 0.05 0.04 Q35 1 0.8100 0.3978 0.4904 11.00000 0.05 0.04 Q36 1 0.7620 0.3756 0.3633 11.00000 0.05 0.04 Q37 1 0.6993 0.4206 0.5013 11.00000 0.05 0.04 Q38 1 1.0152 0.2484 0.1214 11.00000 0.05 0.04 Q39 1 0.7469 0.4052 0.5183 11.00000 0.05 0.04 Q40 1 0.8984 0.1665 0.1751 11.00000 0.05 0.04 Q41 1 0.7803 0.4507 0.2725 11.00000 0.05 0.04 Q42 1 0.5550 0.4535 0.3382 11.00000 0.05 0.04 Q43 1 0.9165 0.3540 0.1753 11.00000 0.05 0.04 Q44 1 0.7211 0.6383 0.1326 11.00000 0.05 0.04 Q45 1 0.9605 0.3367 0.1217 11.00000 0.05 0.04 Q46 1 0.8796 0.6305 0.0517 11.00000 0.05 0.04 Q47 1 0.5544 0.5309 0.4219 11.00000 0.05 0.04 Q48 1 1.0384 0.4363 0.1200 11.00000 0.05 0.04 Q49 1 0.7671 0.4612 0.2694 11.00000 0.05 0.04 Q50 1 0.9943 0.1864 0.1298 11.00000 0.05 0.04 Q51 1 1.0720 0.2683 0.0974 11.00000 0.05 0.04 Q52 1 0.9660 0.0922 0.1021 11.00000 0.05 0.04 Q53 1 0.6961 0.5567 0.4245 11.00000 0.05 0.04 Q54 1 0.6865 0.5265 0.3129 11.00000 0.05 0.04 Q55 1 0.7913 0.3971 0.5343 11.00000 0.05 0.04 Q56 1 0.5962 0.4695 0.4920 11.00000 0.05 0.04 Q57 1 0.8484 0.7786 0.1294 11.00000 0.05 0.04 Q58 1 0.7533 0.4452 0.3509 11.00000 0.05 0.04 Q59 1 0.7328 0.3899 0.3211 11.00000 0.05 0.04 Q60 1 0.7367 0.5864 0.1481 11.00000 0.05 0.04 Q61 1 0.6591 0.4027 0.2868 11.00000 0.05 0.04 Q62 1 0.7877 0.2815 0.1912 11.00000 0.05 0.04 Q63 1 0.7971 0.2587 0.1765 11.00000 0.05 0.04 Q64 1 0.5737 0.4805 0.3516 11.00000 0.05 0.04 Q65 1 0.5625 0.4693 0.4843 11.00000 0.05 0.04 Q66 1 0.8219 0.6522 0.1369 11.00000 0.05 0.04 Q67 1 0.8733 0.3319 0.1483 11.00000 0.05 0.04 Q68 1 0.8472 0.4844 0.0837 11.00000 0.05 0.04 Q69 1 0.6984 0.3953 0.4576 11.00000 0.05 0.04 Q70 1 0.9553 0.2512 0.1367 11.00000 0.05 0.04 Q71 1 0.6670 0.4507 0.3186 11.00000 0.05 0.04 Q72 1 0.5672 0.4002 0.2828 11.00000 0.05 0.04 Q73 1 0.7021 0.7579 0.1297 11.00000 0.05 0.04 Q74 1 0.8201 0.1610 0.1539 11.00000 0.05 0.04 Q75 1 0.7247 0.7493 0.0609 11.00000 0.05 0.04 Q76 1 0.8417 0.8128 0.0773 11.00000 0.05 0.04 Q77 1 0.8006 0.4691 0.4653 11.00000 0.05 0.04 Q78 1 0.8026 0.3591 0.2994 11.00000 0.05 0.03 Q79 1 0.5000 0.5000 0.1688 10.50000 0.05 0.03 Q80 1 0.8271 0.2238 0.1910 11.00000 0.05 0.03 Q81 1 0.7612 0.4054 0.2844 11.00000 0.05 0.03 Q82 1 1.0619 0.1260 0.1570 11.00000 0.05 0.03 Q83 1 0.5108 0.5809 0.3092 11.00000 0.05 0.03 Q84 1 0.6394 0.4395 0.4309 11.00000 0.05 0.03 Q85 1 0.7822 0.7227 0.0434 11.00000 0.05 0.03 Q86 1 0.7120 0.5160 0.1567 11.00000 0.05 0.03 Q87 1 0.5801 0.4545 0.2588 11.00000 0.05 0.03 Q88 1 0.7455 0.5458 0.4565 11.00000 0.05 0.03 Q89 1 0.7400 0.4154 0.4125 11.00000 0.05 0.03 Q90 1 0.7866 0.4188 0.2047 11.00000 0.05 0.03 Q91 1 0.7158 0.7667 0.1367 11.00000 0.05 0.03 Q92 1 0.9643 0.4294 0.1119 11.00000 0.05 0.03 Q93 1 0.7164 0.3619 0.2601 11.00000 0.05 0.03 Q94 1 0.5378 0.3902 0.5010 11.00000 0.05 0.03 Q95 1 0.9210 0.4836 0.1805 11.00000 0.05 0.03 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17.60 1.76 2 4 -4 15.75 1.67 -2 -4 4 14.56 1.69 -4 2 4 20.64 1.98 2 -4 -4 17.25 1.81 4 2 -4 15.59 1.74 -3 4 4 34.84 3.49 -4 -3 4 34.26 3.44 3 4 -4 35.39 3.39 -4 3 4 34.62 3.50 3 -4 -4 37.40 3.47 4 3 -4 33.97 3.43 -3 -4 4 34.49 3.42 -4 -4 4 -0.01 0.49 -4 4 4 1.24 0.86 4 4 -4 0.39 0.50 4 -4 -4 0.70 0.65 -5 0 4 157.12 15.50 0 5 -4 172.25 15.39 5 0 -4 168.11 15.54 1 5 -4 60.94 5.24 5 -1 -4 48.57 5.33 -1 -5 4 52.19 5.31 -5 1 4 60.40 5.41 -5 -2 4 0.74 1.14 5 -2 -4 1.24 0.63 2 5 -4 0.52 0.52 -2 -5 4 0.55 0.49 5 2 -4 1.81 0.65 2 -5 -4 1.69 0.74 -5 2 4 0.31 0.62 5 -3 -4 107.38 9.95 -3 5 4 108.99 10.06 3 5 -4 108.86 9.90 3 -5 -4 100.06 9.93 5 3 -4 107.15 9.98 -3 -5 4 104.31 9.92 -5 -4 4 102.64 9.60 5 -4 -4 101.55 9.56 4 5 -4 103.43 9.54 -4 5 4 98.75 9.55 5 4 -4 103.69 9.58 -4 -5 4 99.10 9.55 4 -5 -4 102.72 9.55 -5 4 4 101.28 9.63 5 5 -4 51.27 5.02 -5 -5 4 52.35 5.07 -5 5 4 51.34 5.13 5 -5 -4 52.64 5.01 6 0 -4 109.79 10.37 -6 -1 4 21.03 2.18 6 -1 -4 14.17 1.77 1 6 -4 14.67 1.52 -1 -6 4 14.02 1.77 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1.19 3 -7 -4 7.20 1.20 7 3 -4 10.86 1.69 7 -4 -4 41.72 4.16 -4 7 4 43.36 4.37 -7 -4 4 40.50 4.20 4 7 -4 38.16 4.04 7 4 -4 44.65 4.31 4 -7 -4 42.38 4.05 -4 -7 4 40.89 4.06 -7 4 4 39.69 4.19 5 7 -4 34.09 3.61 -5 7 4 35.74 3.66 7 -5 -4 36.73 3.68 -7 5 4 34.51 3.70 -5 -7 4 35.41 3.60 5 -7 -4 37.31 3.59 7 5 -4 36.55 3.74 -6 7 4 28.38 3.05 7 -6 -4 27.01 2.79 -7 -6 4 23.39 2.78 -6 -7 4 24.96 2.74 -7 6 4 23.57 2.80 6 -7 -4 24.93 2.67 -7 7 4 63.72 6.38 -7 -7 4 61.87 6.25 7 -7 -4 64.85 6.20 -8 0 4 19.12 2.59 8 0 -4 16.54 2.45 -8 -1 4 29.05 3.03 1 8 -4 20.35 1.95 8 -1 -4 17.86 2.28 -8 1 4 19.45 2.43 8 1 -4 17.70 2.36 2 8 -4 20.06 2.14 8 -2 -4 24.79 2.66 -8 -2 4 22.80 2.50 -2 -8 4 20.83 2.20 2 -8 -4 23.90 2.31 -8 2 4 18.99 2.47 8 2 -4 19.04 2.42 8 -3 -4 39.11 3.85 -8 -3 4 30.22 3.61 3 8 -4 34.81 3.36 3 -8 -4 33.17 3.42 -3 -8 4 32.64 3.39 -8 3 4 36.65 3.74 -8 -4 4 58.01 5.37 -4 8 4 41.24 5.13 8 -4 -4 59.40 5.25 -4 -8 4 47.76 4.89 4 -8 -4 50.82 4.88 8 4 -4 54.16 5.18 -8 4 4 46.63 5.06 8 -5 -4 111.37 10.39 -5 8 4 114.11 10.28 -8 -5 4 96.20 10.28 -8 5 4 99.97 10.29 -5 -8 4 107.49 10.19 5 -8 -4 117.06 10.16 -8 -6 4 50.27 5.23 8 -6 -4 49.67 5.10 -6 8 4 51.57 5.25 -6 -8 4 50.43 5.07 6 -8 -4 54.25 5.03 -8 6 4 50.97 5.22 8 -7 -4 3.16 0.97 -7 8 4 4.09 1.59 -8 -7 4 5.22 1.35 -8 7 4 4.66 1.64 7 -8 -4 4.75 1.42 -7 -8 4 4.56 1.33 -8 8 4 3.46 1.85 8 -8 -4 2.51 1.43 -8 -8 4 5.76 1.42 9 0 -4 2.64 1.76 -9 0 4 -1.50 2.00 9 -1 -4 11.05 1.87 -9 -1 4 12.19 2.16 -9 1 4 15.66 2.20 1 -9 -4 13.76 1.99 9 1 -4 10.43 1.90 9 -2 -4 20.41 2.65 -9 -2 4 10.97 2.04 -2 -9 4 10.74 1.58 -9 2 4 18.52 2.58 9 2 -4 15.53 2.53 2 -9 -4 11.66 1.56 -9 -3 4 45.09 4.78 9 -3 -4 48.34 4.73 -9 3 4 45.94 4.75 3 -9 -4 49.66 4.50 -3 9 -4 44.74 4.36 9 3 -4 49.14 4.84 -3 -9 4 40.95 4.49 -4 9 4 16.22 2.93 9 -4 -4 11.98 2.00 -9 -4 4 19.34 2.98 -9 4 4 13.20 2.22 4 -9 -4 15.16 1.66 -4 -9 4 12.11 1.64 -4 9 -4 13.92 1.61 9 4 -4 11.97 2.12 -9 -5 4 43.37 4.05 -5 9 4 30.53 3.70 -5 9 -4 29.45 3.15 -5 -9 4 29.14 3.20 5 -9 -4 30.96 3.18 -9 5 4 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1.4675 15 4 0 10.0815 -0.0000 15 4 1 -2.9064 -2.1668 15 4 4 -1.5149 -2.7849 15 4 5 -6.7253 -9.2834 15 4 6 1.1470 8.1604 15 4 7 -3.2969 7.3041 15 4 8 5.5393 5.1897 15 4 9 -7.0509 0.8106 15 4 10 8.7179 -2.3567 15 4 11 -2.5897 1.1506 15 4 12 -0.5905 8.6829 15 4 13 -2.5568 -2.2504 15 4 14 -0.8899 -0.8166 15 4 15 -3.9325 8.0640 15 4 16 -0.9813 7.0327 15 4 17 -2.0880 -1.4426 15 5 0 -4.4592 0.0000 15 5 1 1.1840 6.0790 15 5 5 -3.6763 -0.0483 15 5 6 -6.2648 -1.4524 15 5 7 -4.2253 2.2147 15 5 8 -0.2304 0.2196 15 5 9 -8.7232 -0.6971 15 5 10 1.0341 -1.0644 15 5 11 4.0991 -1.0069 15 5 12 -0.9550 4.9341 15 5 13 7.1373 0.1192 15 5 14 -0.6118 -2.9071 15 5 15 -1.0849 4.3776 15 5 16 3.5927 -2.4582 15 6 0 -4.7752 0.0000 15 6 1 1.8451 -3.2728 15 6 5 -1.1786 -4.7392 15 6 6 7.0686 -2.5599 15 6 7 -2.3326 4.1565 15 6 8 -5.4148 -0.2322 15 6 9 -4.2585 -1.6397 15 6 10 -4.9084 4.8983 15 6 11 3.8644 -7.2406 15 6 12 -1.6600 -6.0104 15 6 13 3.9536 1.9710 15 6 14 -0.9438 0.2445 15 6 15 2.3299 -3.4115 15 7 0 1.3581 -0.0000 15 7 1 5.8467 3.4495 15 7 2 -4.8132 -6.9663 15 7 3 4.5010 -3.0273 15 7 5 -3.9743 4.8083 15 7 6 0.8954 -2.5026 15 7 7 4.6066 3.5489 15 7 8 4.9538 1.0971 15 7 9 -1.8037 -1.0236 15 7 10 -5.4585 -7.2222 15 7 11 9.1473 3.4451 15 7 12 2.2899 -6.2182 15 7 13 -0.8055 0.7328 15 8 0 -6.5310 0.0000 15 8 1 2.1644 -0.1269 15 8 2 2.3438 -6.7570 15 8 3 4.3700 -4.9540 15 8 4 0.8893 1.1291 15 8 5 -3.1133 1.4943 15 8 6 3.4890 3.7940 15 8 7 -3.3621 3.4944 15 8 8 0.2915 5.4757 15 8 9 0.5851 -2.7389 15 8 10 6.2739 0.9255 15 8 11 0.2680 1.3107 15 9 0 -1.8976 -0.0000 15 9 1 -1.4596 3.3923 15 9 2 -3.2959 -3.3163 15 9 3 0.6154 2.4740 15 9 4 -3.8196 0.7137 15 9 5 5.0929 -5.6750 15 9 6 -1.8953 -1.6951 15 9 7 -1.3862 -2.8786 15 9 8 -7.0020 -1.3524 16 0 4 14.0896 -0.0000 16 0 5 -0.0000 -7.7382 16 0 6 -0.5024 0.0000 16 0 7 0.0000 0.5370 16 0 8 1.0093 0.0000 16 0 9 0.0000 12.0454 16 0 10 7.7381 -0.0000 16 0 11 -0.0000 0.1199 16 0 12 -0.3106 0.0000 16 0 13 -0.0000 -3.2174 16 0 14 -3.0546 -0.0000 16 0 15 0.0000 3.2947 16 0 16 6.2714 0.0000 16 1 4 -7.5086 3.0033 16 1 5 -3.9232 12.7676 16 1 6 -5.4220 -5.8377 16 1 7 -5.4260 9.9525 16 1 8 -6.3600 10.5533 16 1 9 -2.5763 0.1729 16 1 10 1.4177 11.6309 16 1 11 -3.6403 -2.9923 16 1 12 -5.1413 5.7558 16 1 13 5.6023 0.2664 16 1 14 5.9731 -1.3302 16 1 15 -1.4662 -6.7598 16 1 16 2.6590 0.6403 16 2 5 -2.8702 -2.6333 16 2 6 -1.1867 2.1864 16 2 7 2.8288 0.4825 16 2 8 -3.3375 7.2704 16 2 9 -4.0717 -8.9900 16 2 10 2.3709 -4.7980 16 2 11 3.1651 3.3009 16 2 12 -2.3681 -0.9239 16 2 13 4.1369 -3.4669 16 2 14 -4.0913 4.1520 16 2 15 2.0624 -3.5573 16 3 5 9.1215 2.5416 16 3 6 3.6624 3.1576 16 3 7 -4.3749 2.9495 16 3 8 2.5751 -1.3682 16 3 9 3.9810 2.3782 16 3 10 1.2902 -5.7104 16 3 11 -4.0245 -0.4106 16 3 12 3.1930 0.4754 16 3 13 3.1737 -1.1796 16 3 14 -0.0702 0.2172 16 3 15 3.8706 0.4749 16 4 0 4.9833 -0.0000 16 4 1 -0.9438 -1.1612 16 4 2 6.0010 1.5373 16 4 5 -2.7061 4.9872 16 4 6 -2.6185 6.4510 16 4 7 -0.0321 -4.5271 16 4 8 3.9407 -3.0196 16 4 9 4.2962 1.0424 16 4 10 5.4260 2.7432 16 4 11 1.0665 -4.4558 16 4 12 -0.8858 -0.7836 16 4 13 5.8130 -2.5329 16 4 14 -6.7476 -2.8125 16 5 0 0.0095 0.0000 16 5 1 2.5512 7.7796 16 5 5 -6.1925 -0.9212 16 5 6 1.1863 -5.0765 16 5 7 1.8288 -7.9066 16 5 8 1.3634 1.8224 16 5 9 3.3640 1.0804 16 5 10 -1.7945 -0.4836 16 5 11 -0.0630 -4.4866 16 5 12 -6.0555 4.5323 16 6 0 -1.1641 0.0000 16 6 1 4.7641 -1.0688 16 6 5 1.8252 -3.2698 16 6 6 3.7977 0.8841 16 6 7 -2.5286 -2.4038 16 6 8 -5.1652 -0.6649 16 6 9 4.2371 -2.3350 16 6 10 1.0133 0.1985 16 6 11 -0.1183 -0.7522 16 7 0 0.9824 -0.0000 16 7 1 -0.1869 2.9542 16 7 6 2.1317 2.5593 16 7 7 -2.1057 0.1762 16 7 8 5.1032 -2.4137 16 8 0 2.3770 -0.0000 16 8 1 7.8201 0.2017 16 8 2 3.8907 4.8709 16 8 3 5.5421 1.1175 16 8 4 -1.5531 4.4026 17 0 5 9.0099 -0.0000 17 0 6 -0.0000 -8.7828 17 0 7 -2.6129 0.0000 17 0 8 -0.0000 -16.1415 17 0 9 -2.2485 0.0000 17 0 10 -0.0000 -3.0998 17 0 11 -6.8747 0.0000 17 1 5 3.7449 0.6524 17 1 6 0.4279 2.6736 17 1 7 1.3947 3.0139 17 1 8 -3.5274 5.8787 17 1 9 3.2463 0.3699 17 1 10 3.4338 6.2334 17 1 11 -3.2644 -0.7332 17 2 5 -2.0355 -8.5956 17 2 6 -8.7601 0.0563 17 2 7 5.2571 -4.2147 17 2 8 -4.2136 4.1098 17 2 9 -4.0082 -1.5130 17 2 10 1.5982 -5.1693 17 2 11 -1.7554 2.0139 17 3 3 -3.2537 -5.1192 17 3 6 -0.3759 0.9901 17 3 7 0.9767 -4.3308 17 3 8 0.0230 4.5283 17 3 9 3.1071 -1.2977 17 3 10 -3.7307 2.4492 17 4 2 5.5288 3.7577 17 4 6 6.5876 6.0719 17 4 7 -3.8739 -0.6201 17 4 8 -1.0362 6.9749 17 5 0 1.4276 -0.0000 17 5 2 -4.8170 -2.7346 17 5 6 0.0180 1.7272 0 0 0 0.0 0.0 ; _shelx_fab_checksum 91315 _olex2_submission_special_instructions 'No special instructions were received' #END data_MOF520_0.15GPa _chemical_name_common 'MOF-520_0.15GPa' _chemical_name_systematic ? _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0310 0.0240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 94 _space_group_name_H-M_alt 'P 42 21 2' _space_group_name_Hall 'P 4n 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 19.070(3) _cell_length_b 19.070(3) _cell_length_c 36.930(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13430(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3242 _cell_measurement_theta_max 13.01 _cell_measurement_theta_min 2.19 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.563 _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 0.029 _shelx_estimated_absorpt_T_max 0.7437 _shelx_estimated_absorpt_T_min 0.4700 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_correction_T_min 0.4700 _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1657 before and 0.0791 after correction. The Ratio of minimum to maximum transmission is 0.6320. The \l/2 correction factor is Not present. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Perkin Elmer CMOS' _diffrn_measurement_method '\w 80 degrees scan' _diffrn_detector_area_resol_mean ? _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 0.15 GPa was measured via ruby method. The sample was collected by rotating 80 degrees. The data sets were merged in XPREP to produce the final data set. ; _diffrn_reflns_number 10435 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_unetI/netI 0.1517 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_theta_full 13.025 _diffrn_reflns_theta_max 13.025 _diffrn_reflns_theta_min 0.839 _diffrn_measured_fraction_theta_full 0.892 _diffrn_measured_fraction_theta_max 0.892 _diffrn_reflns_Laue_measured_fraction_full 0.892 _diffrn_reflns_Laue_measured_fraction_max 0.892 _diffrn_reflns_point_group_measured_fraction_full 0.875 _diffrn_reflns_point_group_measured_fraction_max 0.875 _reflns_number_total 4641 _reflns_number_gt 1888 _diffrn_standards_number 0 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.686 _reflns_Friedel_fraction_full 0.852 _reflns_Friedel_fraction_max 0.852 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_diff_density_max 0.153 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Flack x determined using 563 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.6(7) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 4641 _refine_ls_number_restraints 303 _refine_ls_R_factor_all 0.1582 _refine_ls_R_factor_gt 0.0628 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1060P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1628 _refine_ls_wR_factor_ref 0.2101 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, H1 of O1, H2 of O2 At 1.5 times of: H3 of O3 2. Restrained distances O3-H3 0.85 with sigma of 0.01 C1-H3 1.988823 with sigma of 0.02 Al2-H3 2.384167 with sigma of 0.02 3. Rigid body (RIGU) restrains C6, Al1, O1, O10, Al2, H1, C28, O3, O2, O9, H28, C1, Al3, H2, C2, O4, C3, C4, C5, C8, C13, C9, C12, C10, C21, C11, C14, C26, C22, C19, C15, C25, C23, C1AA, C24, C0AA, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O3, Al2, O2, Al2, O9, O9, C28, C28, H28, O3, C1, Al3, O2, O2, H2, O4, C1, C2, C1, Al3, O4, C6, C2, C3, C2, C6, C4, C3, C5, C4, C5, C4, C8, C5, C8, C13, C9, C8, C13, C12, C9, C10, C21, C12, C12, C11, C14, C10, C11, C10, C26, C21, C22, C21, C19, C14, C15, C14, C26, C25, C23, C22, C22, C19, C1AA, C15, C25, C23, C25, C24, C24, C23, C1AA, C0AA, C27, C24, C20, C0AA, O8, C27, O7, C27, O5, C20, O6, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C23(H23), C22(H22), C26(H26), C25(H25), C6(H6), C44(H44), C4(H4), C3(H3A), C13(H13), C9(H9), C28(H28), C11(H11), C17(H17), C19(H19), C15(H15), C1AA(H1AA) 4.b Fitted hexagon refined as free rotating group: C23(C22,C21,C26,C25,C24), C6(C44,C5,C4,C3,C2), C17(C19,C14,C15,C1AA,C0AA) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.6635(3) 0.3365(3) 0.5000 0.110(3) Uani 1 2 d S TU P . . Al2 Al 0.6182(3) 0.3913(3) 0.41600(19) 0.119(2) Uani 1 1 d D U . . . Al3 Al 0.5000 0.5000 0.3815(2) 0.082(2) Uani 1 2 d S TU P . . O2 O 0.5628(3) 0.4716(3) 0.4195(2) 0.068(3) Uani 1 1 d . U . . . H2 H 0.5656 0.4988 0.4403 0.082 Uiso 1 1 calc R U . . . O3 O 0.6506(5) 0.4069(6) 0.3704(4) 0.132(4) Uani 1 1 d D U . . . H3 H 0.693(3) 0.397(8) 0.3648(15) 0.198 Uiso 1 1 d DR . . . . O1 O 0.5970(6) 0.3530(5) 0.4676(3) 0.139(4) Uani 1 1 d . U . . . H1 H 0.5506 0.3442 0.4740 0.167 Uiso 1 1 calc R U . . . O4 O 0.5527(4) 0.4793(4) 0.3442(3) 0.081(3) Uani 1 1 d . U . . . C1 C 0.6128(7) 0.4384(7) 0.3377(5) 0.085(4) Uani 1 1 d D U . . . C23 C 0.7895(6) 0.6334(7) 0.0666(3) 0.187(9) Uani 1 1 d . U . . . H23 H 0.7967 0.6358 0.0417 0.224 Uiso 1 1 calc R . . . . C22 C 0.7805(6) 0.5687(5) 0.0833(4) 0.148(7) Uani 1 1 d G U . . . H22 H 0.7818 0.5278 0.0696 0.178 Uiso 1 1 calc R . . . . C21 C 0.7697(5) 0.5651(4) 0.1204(4) 0.123(6) Uani 1 1 d G U . . . C26 C 0.7678(5) 0.6262(7) 0.1409(3) 0.134(6) Uani 1 1 d G U . . . H26 H 0.7605 0.6238 0.1658 0.161 Uiso 1 1 calc R . . . . C25 C 0.7767(5) 0.6909(5) 0.1242(4) 0.163(8) Uani 1 1 d G U . . . H25 H 0.7754 0.7318 0.1379 0.196 Uiso 1 1 calc R . . . . C24 C 0.7875(5) 0.6945(4) 0.0870(4) 0.104(5) Uani 1 1 d G U . . . C20 C 0.9827(10) 0.1537(9) 0.1203(6) 0.129(7) Uani 1 1 d . U . . . C27 C 0.8162(11) 0.7665(12) 0.0593(6) 0.088(6) Uani 1 1 d . U . . . C6 C 0.6175(5) 0.4833(6) 0.2783(4) 0.162(8) Uani 1 1 d . U . . . H6 H 0.5805 0.5135 0.2835 0.194 Uiso 1 1 calc R . . . . C44 C 0.6461(7) 0.4818(6) 0.2437(4) 0.35(2) Uani 1 1 d G . . . . H44 H 0.6282 0.5109 0.2257 0.421 Uiso 1 1 calc R . . . . C5 C 0.7013(6) 0.4366(7) 0.2359(3) 0.101(5) Uani 1 1 d G U . . . C4 C 0.7279(4) 0.3931(5) 0.2628(4) 0.107(5) Uani 1 1 d G U . . . H4 H 0.7649 0.3629 0.2576 0.128 Uiso 1 1 calc R . . . . C3 C 0.6993(6) 0.3946(5) 0.2974(3) 0.146(7) Uani 1 1 d G U . . . H3A H 0.7172 0.3654 0.3154 0.175 Uiso 1 1 calc R . . . . C2 C 0.6441(6) 0.4397(6) 0.3052(3) 0.086(4) Uani 1 1 d G U . . . C13 C 0.7292(8) 0.4905(9) 0.1721(5) 0.114(6) Uani 1 1 d . U . . . H13 H 0.6957 0.5250 0.1762 0.137 Uiso 1 1 calc R . . . . C10 C 0.8089(8) 0.3882(8) 0.1489(6) 0.093(5) Uani 1 1 d . U . . . C12 C 0.7621(9) 0.4953(10) 0.1394(6) 0.133(6) Uani 1 1 d . U . . . C9 C 0.7690(8) 0.3784(7) 0.1827(5) 0.110(5) Uani 1 1 d . U . . . H9 H 0.7633 0.3340 0.1926 0.131 Uiso 1 1 calc R . . . . O8 O 0.8286(4) 0.8088(4) 0.0847(3) 0.084(3) Uani 1 1 d . U . . . O10 O 0.7312(5) 0.3991(5) 0.4813(3) 0.107(4) Uani 1 1 d . U . . . O5 O 1.0328(5) 0.1705(5) 0.0935(3) 0.100(4) Uani 1 1 d . U . . . O6 O 0.9559(4) 0.0912(4) 0.1203(3) 0.081(3) Uani 1 1 d . U . . . O7 O 0.7999(8) 0.7668(9) 0.0376(4) 0.130(6) Uani 1 1 d . U . . . O9 O 0.6983(6) 0.4448(5) 0.4272(4) 0.120(4) Uani 1 1 d . U . . . C28 C 0.7354(7) 0.4442(8) 0.4532(6) 0.085(5) Uani 1 1 d . U . . . H28 H 0.7704 0.4781 0.4542 0.102 Uiso 1 1 calc R U . . . C8 C 0.7373(9) 0.4419(10) 0.2009(7) 0.143(6) Uani 1 1 d . U . . . C11 C 0.8020(8) 0.4332(9) 0.1277(5) 0.117(6) Uani 1 1 d . U . . . H11 H 0.8208 0.4299 0.1045 0.141 Uiso 1 1 calc R . . . . C17 C 0.9552(5) 0.2797(8) 0.1092(3) 0.220(12) Uani 1 1 d . . . . . H17 H 0.9961 0.2862 0.0959 0.264 Uiso 1 1 calc R . . . . C19 C 0.9122(7) 0.3366(6) 0.1169(3) 0.168(9) Uani 1 1 d G U . . . H19 H 0.9243 0.3811 0.1088 0.201 Uiso 1 1 calc R . . . . C14 C 0.8510(6) 0.3269(5) 0.1368(3) 0.124(6) Uani 1 1 d G U . . . C15 C 0.8330(4) 0.2603(6) 0.1490(3) 0.113(6) Uani 1 1 d G U . . . H15 H 0.7920 0.2539 0.1622 0.135 Uiso 1 1 calc R . . . . C1AA C 0.8760(6) 0.2035(5) 0.1413(4) 0.132(7) Uani 1 1 d G U . . . H1AA H 0.8639 0.1589 0.1494 0.158 Uiso 1 1 calc R . . . . C0AA C 0.9372(6) 0.2131(6) 0.1214(4) 0.147(7) Uani 1 1 d G 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 0.085(3) 0.085(3) 0.159(9) 0.009(3) 0.009(3) 0.001(4) Al2 0.090(4) 0.090(4) 0.175(6) 0.004(4) -0.003(4) 0.002(3) Al3 0.057(4) 0.069(4) 0.121(7) 0.000 0.000 0.001(3) O2 0.044(5) 0.065(5) 0.097(8) 0.009(4) 0.018(4) -0.009(4) O3 0.081(7) 0.133(9) 0.182(9) 0.019(7) 0.010(6) 0.009(7) O1 0.124(8) 0.118(8) 0.176(11) 0.008(7) 0.003(7) -0.014(7) O4 0.063(6) 0.076(6) 0.105(8) 0.007(5) -0.011(5) 0.007(5) C1 0.044(8) 0.056(8) 0.155(10) 0.008(7) 0.001(6) -0.008(6) C23 0.25(2) 0.115(10) 0.197(16) -0.003(9) 0.031(13) -0.021(11) C22 0.152(16) 0.101(10) 0.191(15) -0.003(8) 0.021(11) -0.003(10) C21 0.099(12) 0.091(8) 0.178(14) -0.001(8) 0.016(11) 0.000(8) C26 0.117(13) 0.110(9) 0.174(14) -0.004(8) 0.015(10) -0.004(10) C25 0.193(19) 0.114(11) 0.182(15) 0.000(9) 0.014(12) -0.022(11) C24 0.071(10) 0.081(8) 0.160(13) 0.000(7) -0.011(9) -0.017(7) C20 0.114(11) 0.093(9) 0.181(17) 0.005(9) 0.012(10) 0.001(7) C27 0.060(12) 0.053(9) 0.151(13) 0.000(8) -0.003(9) 0.013(8) C6 0.131(15) 0.155(16) 0.198(17) 0.045(13) 0.011(12) 0.020(12) C44 0.28(4) 0.39(5) 0.38(6) 0.05(4) 0.08(4) 0.07(4) C5 0.067(10) 0.076(11) 0.159(12) -0.010(8) -0.008(8) -0.003(8) C4 0.069(10) 0.088(11) 0.164(13) -0.007(9) 0.022(8) 0.015(8) C3 0.122(12) 0.136(13) 0.179(14) 0.009(10) 0.022(9) 0.025(10) C2 0.050(8) 0.057(9) 0.153(11) -0.007(7) 0.007(7) -0.025(6) C13 0.084(11) 0.091(10) 0.168(13) -0.005(8) 0.003(9) 0.005(8) C10 0.071(9) 0.075(8) 0.132(13) -0.002(7) -0.011(8) -0.024(7) C12 0.119(14) 0.103(9) 0.176(14) -0.004(8) 0.012(10) -0.005(8) C9 0.098(11) 0.081(9) 0.150(13) 0.021(8) -0.007(8) -0.001(8) O8 0.062(6) 0.061(6) 0.130(11) 0.012(6) 0.004(6) -0.005(5) O10 0.086(7) 0.072(7) 0.163(11) -0.013(6) 0.011(6) 0.003(5) O5 0.082(7) 0.079(7) 0.138(12) 0.010(6) -0.019(6) -0.003(5) O6 0.067(6) 0.067(6) 0.111(10) 0.011(5) 0.005(5) 0.013(5) O7 0.115(11) 0.110(9) 0.165(13) 0.006(8) -0.013(9) -0.014(8) O9 0.086(7) 0.096(7) 0.177(11) -0.003(7) 0.009(6) -0.005(6) C28 0.040(9) 0.053(9) 0.162(12) -0.013(8) 0.017(7) 0.012(7) C8 0.139(15) 0.109(11) 0.179(12) 0.005(9) 0.021(9) 0.004(10) C11 0.113(12) 0.094(9) 0.144(14) 0.005(8) 0.015(10) 0.000(9) C17 0.26(3) 0.14(2) 0.26(4) 0.03(2) 0.01(2) -0.03(2) C19 0.144(14) 0.136(15) 0.22(2) 0.003(14) 0.047(14) -0.026(11) C14 0.106(11) 0.102(9) 0.163(17) 0.010(8) 0.013(10) -0.007(8) C15 0.107(11) 0.103(9) 0.129(16) 0.009(9) 0.007(9) -0.011(8) C1AA 0.112(12) 0.107(10) 0.177(19) 0.012(10) 0.004(10) -0.011(8) C0AA 0.130(12) 0.096(10) 0.21(2) -0.001(10) 0.019(12) -0.005(9) _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 O1 1.771(11) 8_666 ? Al1 O1 1.771(11) . ? Al1 O10 1.890(10) . ? Al1 O10 1.890(10) 8_666 ? Al1 O7 2.045(18) 2_645 ? Al1 O7 2.045(18) 6_645 ? Al2 O2 1.865(8) . ? Al2 O3 1.818(13) . ? Al2 O1 2.080(12) . ? Al2 O8 1.871(9) 6_645 ? Al2 O5 2.039(10) 5_455 ? Al2 O9 1.883(12) . ? Al3 O2 1.923(10) 3_665 ? Al3 O2 1.923(10) . ? Al3 O4 1.751(11) . ? Al3 O4 1.751(11) 3_665 ? Al3 O6 1.933(8) 6_655 ? Al3 O6 1.933(8) 5_455 ? O3 C1 1.530(18) . ? O4 C1 1.407(14) . ? C1 C2 1.341(18) . ? C23 C22 1.3900 . ? C23 C24 1.3900 . ? C22 C21 1.3900 . ? C21 C26 1.3900 . ? C21 C12 1.511(19) . ? C26 C25 1.3900 . ? C25 C24 1.3900 . ? C24 C27 1.80(2) . ? C20 O5 1.413(19) . ? C20 O6 1.296(17) . ? C20 C0AA 1.429(17) . ? C27 O8 1.26(2) . ? C27 O7 0.86(3) . ? C6 C44 1.3900 . ? C6 C2 1.3900 . ? C44 C5 1.3900 . ? C5 C4 1.3900 . ? C5 C8 1.47(2) . ? C4 C3 1.3900 . ? C3 C2 1.3900 . ? C13 C12 1.36(2) . ? C13 C8 1.42(2) . ? C10 C9 1.47(2) . ? C10 C11 1.169(18) . ? C10 C14 1.487(17) . ? C12 C11 1.47(2) . ? C9 C8 1.51(2) . ? O8 Al2 1.871(9) 6_655 ? O10 C28 1.351(18) . ? O5 Al2 2.039(10) 5 ? O6 Al3 1.933(8) 5 ? O7 Al1 2.045(18) 4_564 ? O9 C28 1.193(18) . ? C17 C19 1.3900 . ? C17 C0AA 1.3900 . ? C19 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C1AA 1.3900 . ? C1AA C0AA 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 101.6(8) 8_666 . ? O1 Al1 O10 97.5(5) . . ? O1 Al1 O10 85.2(5) . 8_666 ? O1 Al1 O10 85.2(5) 8_666 . ? O1 Al1 O10 97.5(5) 8_666 8_666 ? O1 Al1 O7 84.3(5) 8_666 2_645 ? O1 Al1 O7 84.3(5) . 6_645 ? O1 Al1 O7 169.9(6) 8_666 6_645 ? O1 Al1 O7 169.9(6) . 2_645 ? O10 Al1 O10 175.8(7) . 8_666 ? O10 Al1 O7 85.9(6) . 6_645 ? O10 Al1 O7 85.9(6) 8_666 2_645 ? O10 Al1 O7 91.1(6) 8_666 6_645 ? O10 Al1 O7 91.1(6) . 2_645 ? O7 Al1 O7 91.0(8) 2_645 6_645 ? O2 Al2 O1 96.6(5) . . ? O2 Al2 O8 176.4(6) . 6_645 ? O2 Al2 O5 92.0(4) . 5_455 ? O2 Al2 O9 90.0(4) . . ? O3 Al2 O2 97.0(5) . . ? O3 Al2 O1 166.4(5) . . ? O3 Al2 O8 86.5(6) . 6_645 ? O3 Al2 O5 101.9(6) . 5_455 ? O3 Al2 O9 80.7(6) . . ? O8 Al2 O1 79.9(5) 6_645 . ? O8 Al2 O5 86.8(4) 6_645 5_455 ? O8 Al2 O9 91.1(5) 6_645 . ? O5 Al2 O1 78.5(5) 5_455 . ? O9 Al2 O1 98.4(6) . . ? O9 Al2 O5 176.5(6) . 5_455 ? O2 Al3 O2 86.2(6) . 3_665 ? O2 Al3 O6 90.4(4) . 6_655 ? O2 Al3 O6 92.4(4) 3_665 6_655 ? O2 Al3 O6 90.4(4) 3_665 5_455 ? O2 Al3 O6 92.4(4) . 5_455 ? O4 Al3 O2 174.6(5) . 3_665 ? O4 Al3 O2 98.8(4) 3_665 3_665 ? O4 Al3 O2 98.8(4) . . ? O4 Al3 O2 174.6(5) 3_665 . ? O4 Al3 O4 76.2(7) . 3_665 ? O4 Al3 O6 85.8(4) . 6_655 ? O4 Al3 O6 85.8(4) 3_665 5_455 ? O4 Al3 O6 91.2(4) 3_665 6_655 ? O4 Al3 O6 91.2(4) . 5_455 ? O6 Al3 O6 176.2(7) 5_455 6_655 ? Al2 O2 Al3 122.3(5) . . ? C1 O3 Al2 129.5(9) . . ? Al1 O1 Al2 122.8(6) . . ? C1 O4 Al3 136.6(10) . . ? O4 C1 O3 117.8(14) . . ? C2 C1 O3 120.4(13) . . ? C2 C1 O4 120.3(14) . . ? C22 C23 C24 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 C12 121.0(14) . . ? C26 C21 C12 119.0(14) . . ? C21 C26 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C23 C24 C27 108.9(12) . . ? C25 C24 C23 120.0 . . ? C25 C24 C27 130.2(12) . . ? O5 C20 C0AA 104.5(14) . . ? O6 C20 O5 118.3(16) . . ? O6 C20 C0AA 119.3(16) . . ? O8 C27 C24 97.0(16) . . ? O7 C27 C24 115(3) . . ? O7 C27 O8 139(3) . . ? C44 C6 C2 120.0 . . ? C5 C44 C6 120.0 . . ? C44 C5 C4 120.0 . . ? C44 C5 C8 119.6(14) . . ? C4 C5 C8 119.9(14) . . ? C5 C4 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C1 C2 C6 119.2(13) . . ? C1 C2 C3 120.7(13) . . ? C3 C2 C6 120.0 . . ? C12 C13 C8 131(2) . . ? C9 C10 C14 115.8(15) . . ? C11 C10 C9 127(2) . . ? C11 C10 C14 116(2) . . ? C13 C12 C21 120.8(18) . . ? C13 C12 C11 116.3(18) . . ? C11 C12 C21 121.6(18) . . ? C10 C9 C8 118.9(15) . . ? C27 O8 Al2 129.0(15) . 6_655 ? C28 O10 Al1 136.3(10) . . ? C20 O5 Al2 121.9(10) . 5 ? C20 O6 Al3 130.9(10) . 5 ? C27 O7 Al1 121(3) . 4_564 ? C28 O9 Al2 130.7(14) . . ? O9 C28 O10 126.2(17) . . ? C5 C8 C9 121.7(17) . . ? C13 C8 C5 130.9(19) . . ? C13 C8 C9 103(2) . . ? C10 C11 C12 117(2) . . ? C19 C17 C0AA 120.0 . . ? C17 C19 C14 120.0 . . ? C19 C14 C10 120.5(11) . . ? C15 C14 C10 119.1(12) . . ? C15 C14 C19 120.0 . . ? C14 C15 C1AA 120.0 . . ? C0AA C1AA C15 120.0 . . ? C17 C0AA C20 124.4(13) . . ? C1AA C0AA C20 114.8(13) . . ? C1AA C0AA C17 120.0 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.761 -0.155 -0.040 9653.7 15064.2 ? _shelx_res_file ; p2_25kev_0m.res created by SHELXL-2014/7 TITL P2_25keV_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.07 19.07 36.93 90 90 90 ZERR 222 0.0027 0.0027 0.00739 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.031 0.024 81.761 DISP C 0.001 0.001 6.243 DISP H -0 0 0.608 DISP O 0.004 0.003 13.948 UNIT 222 222 222 222 DFIX 0.85 0.01 O3 H3 DANG 1.988823 0.02 C1 H3 DANG 2.384167 0.02 Al2 H3 RIGU C6 Al1 O1 O10 Al2 H1 C28 O3 O2 O9 H28 C1 Al3 H2 C2 O4 C3 C4 C5 C8 C13 = C9 C12 C10 C21 C11 C14 C26 C22 C19 C15 C25 C23 C1AA C24 C0AA C27 C20 O8 O7 = O5 O6 AL1 O1 AL1 O10 AL2 O1 O1 H1 O10 C28 AL2 O3 AL2 O2 AL2 O9 O9 C28 C28 = H28 O3 C1 AL3 O2 O2 H2 O4 C1 C2 C1 AL3 O4 C6 C2 C3 C2 C6 C4 C3 C5 C4 C5 C4 = C8 C5 C8 C13 C9 C8 C13 C12 C9 C10 C21 C12 C12 C11 C14 C10 C11 C10 C26 C21 = C22 C21 C19 C14 C15 C14 C26 C25 C23 C22 C22 C19 C1AA C15 C25 C23 C25 C24 C24 = C23 C1AA C0AA C27 C24 C20 C0AA O8 C27 O7 C27 O5 C20 O6 C20 L.S. 24 PLAN 120 TEMP 23 BOND ABIN ACTA fmap 2 REM REM REM WGHT 0.106000 FVAR 0.12322 AL1 4 0.663493 0.336507 0.500000 10.50000 0.08543 0.08543 = 0.15907 0.00890 0.00890 0.00122 AL2 4 0.618172 0.391257 0.415996 11.00000 0.09028 0.08993 = 0.17535 0.00417 -0.00263 0.00206 AL3 4 0.500000 0.500000 0.381488 10.50000 0.05653 0.06893 = 0.12050 0.00000 0.00000 0.00081 O2 3 0.562779 0.471566 0.419496 11.00000 0.04367 0.06493 = 0.09681 0.00932 0.01809 -0.00866 AFIX 43 H2 2 0.565616 0.498793 0.440337 11.00000 -1.20000 AFIX 0 O3 3 0.650602 0.406861 0.370423 11.00000 0.08136 0.13343 = 0.18204 0.01950 0.01000 0.00897 H3 2 0.692855 0.397394 0.364751 11.00000 -1.50000 O1 3 0.597016 0.353008 0.467613 11.00000 0.12400 0.11780 = 0.17614 0.00825 0.00291 -0.01371 AFIX 43 H1 2 0.550650 0.344194 0.473953 11.00000 -1.20000 AFIX 0 O4 3 0.552730 0.479319 0.344183 11.00000 0.06267 0.07560 = 0.10457 0.00681 -0.01133 0.00664 C1 1 0.612826 0.438365 0.337683 11.00000 0.04405 0.05627 = 0.15502 0.00827 0.00143 -0.00842 AFIX 66 C23 1 0.789454 0.633380 0.066568 11.00000 0.24771 0.11457 = 0.19748 -0.00273 0.03062 -0.02115 AFIX 43 H23 2 0.796714 0.635778 0.041697 11.00000 -1.20000 AFIX 65 C22 1 0.780543 0.568666 0.083266 11.00000 0.15244 0.10117 = 0.19116 -0.00273 0.02076 -0.00324 AFIX 43 H22 2 0.781841 0.527767 0.069566 11.00000 -1.20000 AFIX 65 C21 1 0.769692 0.565081 0.120439 11.00000 0.09912 0.09109 = 0.17755 -0.00124 0.01560 -0.00028 C26 1 0.767752 0.626210 0.140915 11.00000 0.11722 0.11037 = 0.17390 -0.00365 0.01488 -0.00434 AFIX 43 H26 2 0.760492 0.623811 0.165786 11.00000 -1.20000 AFIX 65 C25 1 0.776663 0.690924 0.124218 11.00000 0.19344 0.11383 = 0.18214 0.00033 0.01430 -0.02169 AFIX 43 H25 2 0.775365 0.731823 0.137918 11.00000 -1.20000 AFIX 65 C24 1 0.787513 0.694510 0.087045 11.00000 0.07142 0.08061 = 0.16046 0.00019 -0.01136 -0.01656 AFIX 0 C20 1 0.982731 0.153669 0.120309 11.00000 0.11435 0.09269 = 0.18135 0.00489 0.01180 0.00137 C27 1 0.816173 0.766550 0.059338 11.00000 0.05997 0.05298 = 0.15128 -0.00050 -0.00331 0.01314 AFIX 66 C6 1 0.617465 0.483305 0.278320 11.00000 0.13127 0.15496 = 0.19841 0.04512 0.01143 0.01993 AFIX 43 H6 2 0.580513 0.513498 0.283516 11.00000 -1.20000 AFIX 65 C44 1 0.646057 0.481771 0.243707 11.00000 0.27976 0.39441 = 0.37933 0.04913 0.07820 0.06971 AFIX 43 H44 2 0.628236 0.510937 0.225745 11.00000 -1.20000 AFIX 65 C5 1 0.701285 0.436644 0.235941 11.00000 0.06709 0.07623 = 0.15940 -0.01031 -0.00761 -0.00253 C4 1 0.727922 0.393051 0.262788 11.00000 0.06886 0.08781 = 0.16446 -0.00708 0.02225 0.01491 AFIX 43 H4 2 0.764873 0.362858 0.257592 11.00000 -1.20000 AFIX 65 C3 1 0.699330 0.394584 0.297401 11.00000 0.12203 0.13625 = 0.17860 0.00875 0.02199 0.02494 AFIX 43 H3A 2 0.717152 0.365417 0.315363 11.00000 -1.20000 AFIX 65 C2 1 0.644102 0.439711 0.305167 11.00000 0.04954 0.05663 = 0.15261 -0.00667 0.00692 -0.02530 AFIX 0 C13 1 0.729230 0.490474 0.172064 11.00000 0.08384 0.09107 = 0.16823 -0.00481 0.00302 0.00499 AFIX 43 H13 2 0.695686 0.524966 0.176174 11.00000 -1.20000 AFIX 0 C10 1 0.808926 0.388189 0.148900 11.00000 0.07102 0.07487 = 0.13201 -0.00243 -0.01069 -0.02391 C12 1 0.762127 0.495261 0.139371 11.00000 0.11927 0.10252 = 0.17600 -0.00354 0.01221 -0.00531 C9 1 0.768983 0.378446 0.182665 11.00000 0.09793 0.08071 = 0.15009 0.02072 -0.00650 -0.00139 AFIX 43 H9 2 0.763329 0.333975 0.192580 11.00000 -1.20000 AFIX 0 O8 3 0.828646 0.808816 0.084740 11.00000 0.06243 0.06069 = 0.13031 0.01190 0.00403 -0.00532 O10 3 0.731241 0.399089 0.481274 11.00000 0.08564 0.07214 = 0.16292 -0.01343 0.01130 0.00273 O5 3 1.032839 0.170505 0.093489 11.00000 0.08180 0.07910 = 0.13834 0.01003 -0.01909 -0.00251 O6 3 0.955899 0.091215 0.120262 11.00000 0.06663 0.06655 = 0.11098 0.01091 0.00509 0.01281 O7 3 0.799889 0.766800 0.037589 11.00000 0.11459 0.11042 = 0.16473 0.00626 -0.01273 -0.01412 O9 3 0.698320 0.444772 0.427151 11.00000 0.08567 0.09596 = 0.17746 -0.00298 0.00936 -0.00548 C28 1 0.735367 0.444239 0.453167 11.00000 0.03983 0.05269 = 0.16186 -0.01289 0.01716 0.01164 AFIX 43 H28 2 0.770404 0.478101 0.454202 11.00000 -1.20000 AFIX 0 C8 1 0.737342 0.441908 0.200928 11.00000 0.13938 0.10904 = 0.17915 0.00524 0.02066 0.00448 C11 1 0.801993 0.433192 0.127707 11.00000 0.11263 0.09441 = 0.14439 0.00467 0.01502 0.00013 AFIX 43 H11 2 0.820814 0.429910 0.104538 11.00000 -1.20000 AFIX 66 C17 1 0.955237 0.279701 0.109206 11.00000 0.26433 0.13866 = 0.25745 0.02798 0.01304 -0.03488 AFIX 43 H17 2 0.996144 0.286176 0.095910 11.00000 -1.20000 AFIX 65 C19 1 0.912169 0.336584 0.116904 11.00000 0.14364 0.13550 = 0.22447 0.00300 0.04700 -0.02598 AFIX 43 H19 2 0.924260 0.381117 0.108759 11.00000 -1.20000 AFIX 65 C14 1 0.851029 0.326906 0.136777 11.00000 0.10610 0.10229 = 0.16255 0.00995 0.01309 -0.00669 C15 1 0.832957 0.260345 0.148952 11.00000 0.10705 0.10266 = 0.12891 0.00919 0.00721 -0.01112 AFIX 43 H15 2 0.792050 0.253870 0.162248 11.00000 -1.20000 AFIX 65 C1AA 1 0.876024 0.203461 0.141254 11.00000 0.11153 0.10651 = 0.17654 0.01237 0.00372 -0.01079 AFIX 43 H1AA 2 0.863933 0.158928 0.149399 11.00000 -1.20000 AFIX 65 C0AA 1 0.937165 0.213138 0.121381 11.00000 0.12996 0.09567 = 0.21452 -0.00070 0.01894 -0.00515 AFIX 0 HKLF 4 REM P2_25keV_0m in P42212 #94 REM R1 = 0.0628 for 1888 Fo > 4sig(Fo) and 0.1582 for all 4641 data REM 329 parameters refined using 303 restraints END WGHT 0.1052 0.0000 REM Highest difference peak 0.153, deepest hole -0.351, 1-sigma level 0.035 Q1 1 0.6436 0.5145 0.3810 11.00000 0.05 0.15 Q2 1 0.5003 0.4817 0.3698 11.00000 0.05 0.15 Q3 1 0.6898 0.3221 0.5176 11.00000 0.05 0.14 Q4 1 0.6902 0.4006 0.5001 11.00000 0.05 0.13 Q5 1 0.9426 0.1265 0.1469 11.00000 0.05 0.13 Q6 1 0.7579 0.4258 0.4332 11.00000 0.05 0.12 Q7 1 0.6238 0.4779 0.4709 11.00000 0.05 0.12 Q8 1 0.6025 0.3175 0.3666 11.00000 0.05 0.12 Q9 1 0.8371 0.7583 0.0487 11.00000 0.05 0.12 Q10 1 0.6901 0.3997 0.2333 11.00000 0.05 0.11 Q11 1 0.6215 0.3157 0.5002 11.00000 0.05 0.11 Q12 1 0.7592 0.3653 0.4991 11.00000 0.05 0.11 Q13 1 0.8331 0.7125 0.0056 11.00000 0.05 0.11 Q14 1 0.6986 0.4027 0.4562 11.00000 0.05 0.11 Q15 1 1.0265 0.2250 0.0657 11.00000 0.05 0.11 Q16 1 0.6558 0.5280 0.4121 11.00000 0.05 0.11 Q17 1 1.0377 0.2090 0.0724 11.00000 0.05 0.11 Q18 1 0.6460 0.4025 0.2998 11.00000 0.05 0.11 Q19 1 0.5120 0.4815 0.3980 11.00000 0.05 0.10 Q20 1 0.7030 0.5200 0.3115 11.00000 0.05 0.10 Q21 1 0.8361 0.3163 0.1976 11.00000 0.05 0.10 Q22 1 0.8139 0.3833 0.1597 11.00000 0.05 0.10 Q23 1 0.9785 0.2695 0.2405 11.00000 0.05 0.10 Q24 1 0.7790 0.2723 0.1133 11.00000 0.05 0.10 Q25 1 0.7301 0.6969 0.0505 11.00000 0.05 0.10 Q26 1 0.9069 0.0967 0.1004 11.00000 0.05 0.10 Q27 1 0.7185 0.4272 0.4548 11.00000 0.05 0.10 Q28 1 0.6411 0.3324 0.5123 11.00000 0.05 0.10 Q29 1 0.7268 0.6990 0.0915 11.00000 0.05 0.10 Q30 1 0.7531 0.3811 0.4969 11.00000 0.05 0.10 Q31 1 1.0016 0.1853 0.1228 11.00000 0.05 0.10 Q32 1 0.7022 0.6340 -0.0079 11.00000 0.05 0.10 Q33 1 1.0146 0.2570 0.1537 11.00000 0.05 0.10 Q34 1 1.0484 0.1497 0.1140 11.00000 0.05 0.10 Q35 1 0.5545 0.4776 0.4094 11.00000 0.05 0.09 Q36 1 0.8368 0.4312 0.3251 11.00000 0.05 0.09 Q37 1 0.8043 0.6714 0.0745 11.00000 0.05 0.09 Q38 1 0.5941 0.2517 0.1559 11.00000 0.05 0.09 Q39 1 0.8055 0.4190 0.4019 11.00000 0.05 0.09 Q40 1 0.6553 0.3528 0.3895 11.00000 0.05 0.09 Q41 1 0.8569 0.5604 0.1139 11.00000 0.05 0.09 Q42 1 0.7892 0.7342 0.0181 11.00000 0.05 0.09 Q43 1 0.6834 0.4922 0.3983 11.00000 0.05 0.09 Q44 1 0.5585 0.2004 0.1124 11.00000 0.05 0.09 Q45 1 0.9101 0.0657 0.1104 11.00000 0.05 0.09 Q46 1 0.6183 0.3968 0.3496 11.00000 0.05 0.09 Q47 1 0.8185 0.7112 0.0964 11.00000 0.05 0.09 Q48 1 0.7901 0.2336 0.1398 11.00000 0.05 0.09 Q49 1 0.9469 0.3122 0.0913 11.00000 0.05 0.09 Q50 1 0.7183 0.2165 0.1176 11.00000 0.05 0.09 Q51 1 0.5797 0.5528 0.3385 11.00000 0.05 0.09 Q52 1 0.5024 0.3234 0.5002 11.00000 0.05 0.09 Q53 1 0.8552 0.0955 0.1377 11.00000 0.05 0.09 Q54 1 0.8238 0.4991 0.4575 11.00000 0.05 0.09 Q55 1 0.8626 0.4789 0.4029 11.00000 0.05 0.08 Q56 1 0.8635 0.2914 0.1022 11.00000 0.05 0.08 Q57 1 0.5892 0.6277 0.4436 11.00000 0.05 0.08 Q58 1 0.7416 0.5493 0.0515 11.00000 0.05 0.08 Q59 1 1.0248 0.1332 0.0761 11.00000 0.05 0.08 Q60 1 0.5589 0.4138 0.3810 11.00000 0.05 0.08 Q61 1 0.7826 0.3801 0.1398 11.00000 0.05 0.08 Q62 1 0.9762 0.3008 0.1198 11.00000 0.05 0.08 Q63 1 0.9062 0.5881 0.4370 11.00000 0.05 0.08 Q64 1 0.5364 0.3057 0.1154 11.00000 0.05 0.08 Q65 1 0.7816 0.5493 0.1832 11.00000 0.05 0.08 Q66 1 0.6569 0.3320 0.2586 11.00000 0.05 0.08 Q67 1 0.6664 0.4399 0.3155 11.00000 0.05 0.08 Q68 1 0.9632 0.2821 0.1227 11.00000 0.05 0.08 Q69 1 0.8583 0.6725 0.1086 11.00000 0.05 0.08 Q70 1 0.7481 0.2859 0.3242 11.00000 0.05 0.08 Q71 1 0.5431 0.3875 0.4631 11.00000 0.05 0.08 Q72 1 0.8605 0.2511 0.1304 11.00000 0.05 0.08 Q73 1 0.5447 0.4553 0.5000 10.50000 0.05 0.08 Q74 1 0.7196 0.6415 0.4540 11.00000 0.05 0.08 Q75 1 0.6749 0.3022 0.2146 11.00000 0.05 0.08 Q76 1 0.5069 0.4298 0.4655 11.00000 0.05 0.08 Q77 1 0.6765 0.4334 0.4106 11.00000 0.05 0.08 Q78 1 0.7422 0.3353 0.4569 11.00000 0.05 0.08 Q79 1 0.8507 0.3507 0.2307 11.00000 0.05 0.08 Q80 1 0.6369 0.5737 0.3163 11.00000 0.05 0.08 Q81 1 0.6757 0.3488 0.1406 11.00000 0.05 0.08 Q82 1 1.0411 0.3274 0.2116 11.00000 0.05 0.08 Q83 1 0.9829 0.5229 0.3349 11.00000 0.05 0.08 Q84 1 0.5302 0.4745 0.1085 11.00000 0.05 0.08 Q85 1 0.5193 0.3463 0.1380 11.00000 0.05 0.08 Q86 1 0.8245 0.5673 0.1380 11.00000 0.05 0.08 Q87 1 0.8141 0.7983 0.1028 11.00000 0.05 0.08 Q88 1 0.6184 0.5634 0.0257 11.00000 0.05 0.08 Q89 1 0.5563 0.1902 0.1779 11.00000 0.05 0.08 Q90 1 0.6424 0.6821 0.1669 11.00000 0.05 0.08 Q91 1 0.5609 0.3789 0.4478 11.00000 0.05 0.08 Q92 1 0.8003 0.3733 0.3104 11.00000 0.05 0.08 Q93 1 0.8531 0.7677 0.0860 11.00000 0.05 0.08 Q94 1 0.6827 0.7193 0.1853 11.00000 0.05 0.08 Q95 1 0.5572 0.4612 0.4941 11.00000 0.05 0.08 Q96 1 0.5984 0.5325 0.1602 11.00000 0.05 0.08 Q97 1 1.0000 0.5000 0.3440 10.50000 0.05 0.07 Q98 1 0.6710 0.4741 0.2433 11.00000 0.05 0.07 Q99 1 0.5570 0.2534 0.2174 11.00000 0.05 0.07 Q100 1 0.8822 0.4270 0.4713 11.00000 0.05 0.07 Q101 1 0.6318 0.7859 0.1229 11.00000 0.05 0.07 Q102 1 0.5992 0.3170 0.4535 11.00000 0.05 0.07 Q103 1 0.9078 0.3068 0.0596 11.00000 0.05 0.07 Q104 1 0.7059 0.5879 0.0317 11.00000 0.05 0.07 Q105 1 0.8920 0.3775 0.3048 11.00000 0.05 0.07 Q106 1 0.6070 0.4079 0.3427 11.00000 0.05 0.07 Q107 1 0.6369 0.4360 0.1290 11.00000 0.05 0.07 Q108 1 0.5413 0.2559 0.4745 11.00000 0.05 0.07 Q109 1 0.8779 0.3193 0.1439 11.00000 0.05 0.07 Q110 1 0.9226 0.5507 0.3912 11.00000 0.05 0.07 Q111 1 0.7807 0.5000 0.2033 11.00000 0.05 0.07 Q112 1 1.0042 0.3801 0.3239 11.00000 0.05 0.07 Q113 1 0.6577 0.4801 0.2755 11.00000 0.05 0.07 Q114 1 0.7877 0.3511 0.4219 11.00000 0.05 0.07 Q115 1 0.8987 0.1436 0.1775 11.00000 0.05 0.07 Q116 1 0.6657 0.2892 0.3060 11.00000 0.05 0.07 Q117 1 0.7829 0.4294 0.3092 11.00000 0.05 0.07 Q118 1 0.8236 0.3692 0.4452 11.00000 0.05 0.07 Q119 1 0.7075 0.5207 0.4797 11.00000 0.05 0.07 Q120 1 0.5128 0.5854 0.0815 11.00000 0.05 0.07 ; _shelx_res_checksum 85078 _shelx_hkl_file ; 1 -1 0 286.11 20.76 -1 1 0 349.01 20.79 0 2 0 11.41 0.91 0 -2 0 12.98 0.92 -1 2 0 302.08 17.47 1 -2 0 229.77 17.43 2 -2 0 1.59 0.36 -2 2 0 1.83 0.37 0 -3 0 -0.05 0.31 0 3 0 -0.08 0.34 1 -3 0 17.50 1.33 -1 3 0 17.24 1.36 -3 2 0 241.96 18.35 2 -3 0 296.56 18.33 -2 3 0 296.16 18.37 3 -3 0 8.98 0.85 -3 3 0 8.67 0.93 0 -4 0 66.52 4.55 1 -4 0 14.32 1.20 -1 4 0 13.82 1.24 -2 4 0 84.39 5.80 -4 3 0 60.13 4.31 3 -4 0 62.56 4.23 -3 4 0 59.73 4.33 4 -4 0 126.37 8.55 -4 4 0 126.84 8.66 0 -5 0 -0.14 0.45 1 -5 0 56.36 4.09 -1 5 0 61.12 4.25 2 -5 0 3.32 0.71 -2 5 0 3.49 0.89 -5 4 0 -0.58 0.82 -4 5 0 0.32 0.88 -5 5 0 148.44 10.19 0 -6 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52.47 4.17 -2 7 9 28.66 3.27 7 -2 -9 23.80 2.59 -7 -2 9 25.91 2.87 7 2 -9 30.16 2.52 -7 2 9 32.42 3.10 2 -7 -9 26.41 3.00 -7 -3 9 36.84 3.41 7 -3 -9 32.78 3.29 3 7 -9 34.34 2.59 -3 7 9 37.02 3.90 3 -7 -9 35.79 3.65 -7 3 9 41.22 3.79 7 3 -9 38.95 3.08 -4 7 9 98.23 7.99 -7 -4 9 95.52 7.50 7 -4 -9 104.05 7.66 4 -7 -9 104.19 7.79 -7 4 9 104.18 8.03 7 4 -9 108.92 7.24 -7 -5 9 49.62 4.18 -5 7 9 52.12 5.00 7 -5 -9 53.64 4.48 -7 5 9 50.92 4.83 5 -7 -9 48.35 4.42 -7 -6 9 57.10 4.77 -6 7 9 66.85 5.58 7 -6 -9 63.90 5.18 -7 6 9 60.44 5.53 -6 -7 9 51.49 4.55 6 -7 -9 65.90 5.19 -7 7 9 17.26 3.09 -7 -7 9 14.94 1.95 7 -7 -9 16.09 2.47 -8 0 9 2.01 2.52 8 0 -9 0.56 1.38 0 -8 -9 0.14 2.02 -8 -1 9 42.71 3.90 8 -1 -9 43.52 3.68 -8 1 9 42.31 4.19 8 1 -9 42.56 3.47 1 -8 -9 39.88 3.95 -8 -2 9 96.82 7.16 -2 8 9 96.23 7.49 8 -2 -9 80.18 6.82 -8 2 9 99.30 7.42 2 -8 -9 94.24 7.24 8 2 -9 93.78 6.73 -3 8 9 112.57 8.48 -8 -3 9 109.09 7.92 8 -3 -9 98.67 7.80 8 3 -9 116.82 7.65 -8 3 9 94.37 8.12 3 -8 -9 108.77 8.15 -8 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1.49 6 -9 -9 0.99 2.23 -9 6 9 7.16 3.22 -7 9 9 1.76 3.16 9 -7 -9 0.78 1.49 -9 -7 9 2.73 1.88 7 -9 -9 2.17 2.72 -9 7 9 1.34 3.63 -7 -9 9 1.92 1.51 9 -8 -9 40.80 4.13 -9 -8 9 42.63 3.75 -8 9 9 42.69 5.34 -9 8 9 42.15 5.31 -8 -9 9 44.28 3.71 8 -9 -9 44.51 4.12 -9 9 9 -1.12 3.66 9 -9 -9 -0.76 1.85 -9 -9 9 2.28 2.02 10 0 -9 12.37 2.02 -10 0 9 13.05 2.93 10 -1 -9 8.62 1.90 -10 -1 9 15.75 2.94 -10 1 9 14.00 3.16 1 -10 -9 18.70 3.78 10 1 -9 8.05 1.81 -10 -2 9 26.97 3.00 10 -2 -9 24.35 2.63 2 -10 -9 25.05 3.49 -10 2 9 28.73 3.51 -2 10 -9 21.06 1.88 -10 -3 9 11.56 2.45 10 -3 -9 8.08 1.97 -3 10 9 9.96 3.54 -10 3 9 13.23 3.01 3 -10 -9 12.08 2.79 10 -4 -9 8.27 2.40 -10 -4 9 13.50 2.63 -4 10 9 2.69 3.22 -10 4 9 10.56 3.17 4 -10 -9 6.26 2.83 10 -5 -9 23.80 2.81 -5 10 9 23.76 4.14 -10 -5 9 27.85 2.94 -10 5 9 24.53 3.85 5 -10 -9 23.30 3.17 10 -6 -9 5.33 2.27 -6 10 9 16.13 4.72 -10 -6 9 8.94 1.94 -6 -10 9 6.23 1.75 -10 6 9 17.62 4.18 6 -10 -9 10.42 3.15 -10 -7 9 9.93 2.09 10 -7 -9 4.82 2.34 -7 10 9 17.63 4.97 -7 -10 9 8.90 1.78 -10 7 9 13.41 4.27 7 -10 -9 13.57 3.61 10 -8 -9 12.09 2.38 -8 10 9 20.69 4.93 -10 8 9 18.24 4.19 -8 -10 9 17.43 2.16 8 -10 -9 14.90 2.90 10 -9 -9 21.25 3.50 -9 10 9 26.85 4.72 9 -10 -9 30.52 3.76 -10 9 9 30.20 4.78 -9 -10 9 32.78 2.93 -10 10 9 24.52 4.68 10 -10 -9 26.07 3.29 -11 0 9 13.69 3.11 11 0 -9 11.20 2.46 -11 -1 9 5.10 2.66 11 -1 -9 2.62 1.68 1 -11 -9 3.30 2.46 -11 1 9 -0.28 3.33 -11 -2 9 9.31 2.26 11 -2 -9 8.67 1.96 -11 2 9 17.55 3.60 2 -11 -9 14.78 3.49 11 -3 -9 26.61 3.16 -11 -3 9 31.39 3.67 3 -11 -9 29.39 3.70 -11 3 9 32.52 4.06 -11 -4 9 19.47 2.72 11 -4 -9 16.77 2.54 4 -11 -9 15.22 2.94 -11 4 9 17.54 3.86 -11 -5 9 1.93 2.01 -5 11 9 3.88 3.59 11 -5 -9 0.53 1.69 -11 5 9 1.50 3.34 -5 -11 9 0.22 1.30 5 -11 -9 2.12 2.44 -6 11 9 33.55 4.71 11 -6 -9 29.06 3.47 6 -11 -9 32.81 3.82 -11 6 9 39.78 5.20 11 -7 -9 9.67 3.06 -7 11 9 13.34 5.23 -11 7 9 10.28 4.40 7 -11 -9 11.74 4.08 -7 -11 9 8.36 1.55 -8 11 9 1.54 4.90 11 -8 -9 1.19 2.30 -11 8 9 4.08 3.81 8 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30.82 2.17 8 -3 -10 25.99 3.05 3 -8 -10 29.05 3.50 -8 3 10 33.67 3.75 8 3 -10 29.76 2.67 -4 8 10 1.27 2.52 -8 -4 10 0.28 1.99 8 -4 -10 0.33 1.37 8 4 -10 -0.30 1.27 -8 4 10 -0.47 2.65 4 -8 -10 -0.87 2.26 -4 -8 10 0.43 1.44 -8 -5 10 9.18 2.17 -5 8 10 10.89 3.01 8 -5 -10 10.89 2.53 5 -8 -10 10.05 3.27 -8 5 10 8.05 3.15 -6 8 10 32.17 4.23 8 -6 -10 29.09 3.20 -8 -6 10 25.46 2.88 -8 6 10 28.91 4.37 6 -8 -10 28.67 3.44 -8 -7 10 15.82 2.34 8 -7 -10 16.72 2.89 -7 8 10 17.82 3.35 7 -8 -10 15.29 2.81 -7 -8 10 18.04 2.38 -8 7 10 20.59 3.47 -8 8 10 64.69 6.63 -8 -8 10 65.13 5.33 8 -8 -10 70.78 5.94 -9 0 10 55.31 4.96 9 0 -10 49.77 4.25 -9 -1 10 10.54 2.53 9 -1 -10 7.97 1.79 9 1 -10 8.46 1.66 1 -9 -10 10.90 2.46 -9 1 10 17.41 3.52 -9 -2 10 80.52 6.25 9 -2 -10 67.33 5.91 2 -9 -10 75.64 6.47 9 2 -10 77.80 5.74 -9 2 10 81.56 6.75 -3 9 10 29.92 4.15 -9 -3 10 34.46 3.44 9 -3 -10 28.38 3.22 -9 3 10 33.56 3.92 3 -9 -10 31.98 3.89 9 3 -10 34.23 2.91 9 -4 -10 12.05 2.52 -9 -4 10 15.06 3.26 -4 9 10 11.67 3.30 4 -9 -10 7.83 2.70 -9 4 10 13.46 3.17 -5 9 10 48.66 5.19 9 -5 -10 46.65 4.25 -9 -5 10 44.09 4.12 -9 5 10 51.25 5.26 5 -9 -10 45.92 4.59 -9 -6 10 20.82 2.62 -6 9 10 25.09 3.80 9 -6 -10 20.54 2.93 -9 6 10 25.91 3.87 6 -9 -10 19.76 3.20 -6 -9 10 18.37 2.29 9 -7 -10 1.42 1.55 -9 -7 10 0.93 1.62 -7 9 10 3.86 4.03 -7 -9 10 0.42 1.38 7 -9 -10 3.51 2.83 -9 7 10 0.35 3.60 9 -8 -10 10.37 2.50 -9 -8 10 12.84 2.17 -8 9 10 16.70 4.42 -9 8 10 26.19 6.05 8 -9 -10 16.36 3.56 -8 -9 10 9.52 2.02 -9 -9 10 140.59 9.93 -9 9 10 139.99 11.24 9 -9 -10 134.25 10.32 10 0 -10 0.18 1.53 -10 0 10 0.34 2.47 0 -10 -10 -0.35 1.35 -10 -1 10 14.04 2.88 10 -1 -10 14.47 2.22 1 -10 -10 19.04 3.30 -10 1 10 19.81 3.46 10 1 -10 15.44 2.16 -10 -2 10 6.18 2.87 10 -2 -10 4.22 1.99 2 -10 -10 4.71 2.75 -10 2 10 4.87 3.00 10 -3 -10 9.17 2.61 -10 -3 10 15.63 2.65 -3 10 10 17.13 3.71 3 -10 -10 13.58 2.83 -10 3 10 18.79 3.45 -4 10 10 12.96 4.11 -10 -4 10 19.75 2.75 10 -4 -10 17.55 2.32 4 -10 -10 20.84 3.29 -10 4 10 20.14 3.58 -5 10 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1 18.6695 -10.0570 16 1 2 20.0572 14.7123 16 1 3 -8.5081 27.0509 16 1 4 -11.7077 9.0618 16 1 5 13.7763 6.8448 16 1 6 -19.2862 7.3455 16 1 7 1.8903 -10.6412 16 1 8 3.5026 21.9598 16 1 9 -4.5859 -3.0058 16 1 10 -15.7345 11.3283 16 2 1 33.4996 50.7960 16 2 5 1.2238 4.0801 16 2 6 14.8353 5.5005 16 3 0 5.5404 -0.0000 16 3 1 4.6108 6.0918 16 3 3 -11.9444 0.8040 16 4 1 12.3347 -0.7169 16 4 2 5.2263 -6.7771 16 4 3 -0.9686 8.5385 16 4 4 7.9461 -3.1986 16 4 6 5.1037 -8.1524 16 4 7 0.2719 -1.0085 16 5 0 0.1912 -0.0000 16 5 2 -0.7149 -2.9507 16 5 3 -3.9821 -4.5364 16 5 4 -0.5240 2.7647 16 5 5 12.8952 10.0809 16 5 6 -6.4292 -3.9908 16 5 7 5.8575 9.5966 16 5 8 0.2828 3.8830 16 6 0 5.3287 -0.0000 16 6 1 -3.5957 0.9277 16 6 2 5.5346 1.1501 16 6 3 -1.7803 1.8312 16 6 4 -4.7628 -7.3635 16 6 5 -2.2033 2.0673 17 0 1 7.2607 0.0000 17 0 2 0.0000 34.3502 17 0 3 21.9872 0.0000 17 0 4 -0.0000 -13.6407 17 0 5 -3.1028 0.0000 17 0 6 -0.0000 -29.8576 17 1 0 -32.5581 -0.0000 17 1 1 -17.8101 -34.4993 17 1 2 17.2067 -4.5593 17 1 3 -29.8640 -22.5320 17 1 4 -18.7755 -15.0888 17 1 5 13.3955 17.5737 17 1 6 7.1616 15.3863 17 2 0 -0.4206 0.0000 17 2 1 -13.3506 9.1608 17 2 2 -0.0252 9.5004 17 2 5 5.1753 -1.7376 17 3 0 -0.3350 -0.0000 17 3 1 -7.5963 8.7856 17 3 2 8.5459 9.2153 17 3 3 5.9868 -7.3618 0 0 0 0.0 0.0 ; _shelx_fab_checksum 48350 _olex2_submission_special_instructions 'No special instructions were received' #END data_MOF520_0.86GPa _chemical_name_common 'MOF-520_0.86GPa' _chemical_name_systematic ? _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0090 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.1200 0.1100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 94 _space_group_name_H-M_alt 'P 42 21 2' _space_group_name_Hall 'P 4n 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 19.196(3) _cell_length_b 19.196(3) _cell_length_c 36.569(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13475(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3798 _cell_measurement_theta_max 13.02 _cell_measurement_theta_min 2.21 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.560 _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 0.029 _shelx_estimated_absorpt_T_max 0.7437 _shelx_estimated_absorpt_T_min 0.2828 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 0.7437 _exptl_absorpt_correction_T_min 0.2828 _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1433 before and 0.0736 after correction. The Ratio of minimum to maximum transmission is 0.3803. The \l/2 correction factor is Not present. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Perkin Elmer CMOS' _diffrn_measurement_method '\w 80 degrees scan' _diffrn_detector_area_resol_mean ? _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 0.86 GPa was measured via ruby method. The sample was collected by rotating 80 degrees. The data sets were merged in XPREP to produce the final data set. ; _diffrn_reflns_number 12386 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_unetI/netI 0.0942 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_theta_full 13.027 _diffrn_reflns_theta_max 13.027 _diffrn_reflns_theta_min 0.836 _diffrn_measured_fraction_theta_full 0.930 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_Laue_measured_fraction_full 0.930 _diffrn_reflns_Laue_measured_fraction_max 0.930 _diffrn_reflns_point_group_measured_fraction_full 0.891 _diffrn_reflns_point_group_measured_fraction_max 0.890 _reflns_number_total 4730 _reflns_number_gt 3219 _diffrn_standards_number 0 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.645 _reflns_Friedel_fraction_full 0.835 _reflns_Friedel_fraction_max 0.836 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_diff_density_max 0.097 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.019 _refine_ls_abs_structure_details ; Flack x determined using 991 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.50(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 4730 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0396 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.0885 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All O(H) groups 2. Rigid body (RIGU) restrains C13, Al1, O1, O10, Al2, H1, C28, O2, O3, O9, H28, Al3, H2, C1, O4, C2, C7, C3, H7, C6, H3, C4, C5, H6, H4, C8, C9, H13, C12, C10, H9, C21, C11, C14, C26, C22, H11, C19, C15, H26, C25, C23, H22, C18, H19, C16, H15, H25, C24, H23, C17, H18, H16, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, H28, Al3, O2, O2, H2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C3, C2, C7, H7, C7, C6, C3, H3, C4, C3, C6, C5, C6, H6, C5, C4, C4, H4, C8, C5, C8, C13, C9, C8, C13, H13, C13, C12, C9, C10, C9, H9, C21, C12, C12, C11, C14, C10, C11, C10, C26, C21, C22, C21, C11, H11, C19, C14, C15, C14, C26, H26, C26, C25, C23, C22, C22, H22, C19, C18, C19, H19, C16, C15, C15, H15, C25, H25, C25, C24, C23, H23, C24, C23, C18, C17, C18, H18, C17, C16, C16, H16, C27, C24, C20, C17, O8, C27, O7, C27, O5, C20, O6, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C10, Al1, O1, O10, Al2, H1, C28, O2, O3, O9, H28, Al3, H2, C1, O4, C2, C7, C3, H7, C6, H3, C4, C5, H6, H4, C8, C13, C9, H13, C12, H9, C21, C11, C14, C26, C22, H11, C19, C15, H26, C25, C23, H22, C18, H19, C16, H15, H25, C24, H23, C17, H18, H16, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, H28, Al3, O2, O2, H2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C3, C2, C7, H7, C7, C6, C3, H3, C4, C3, C6, C5, C6, H6, C5, C4, C4, H4, C8, C5, C8, C13, C9, C8, C13, H13, C13, C12, C9, C10, C9, H9, C21, C12, C12, C11, C14, C10, C11, C10, C26, C21, C22, C21, C11, H11, C19, C14, C15, C14, C26, H26, C26, C25, C23, C22, C22, H22, C19, C18, C19, H19, C16, C15, C15, H15, C25, H25, C25, C24, C23, H23, C24, C23, C18, C17, C18, H18, C17, C16, C16, H16, C27, C24, C20, C17, O8, C27, O7, C27, O5, C20, O6, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C26(H26), C23(H23), C25(H25), C22(H22), C7(H7), C16(H16), C18(H18), C3(H3), C4(H4), C6(H6), C13(H13), C19(H19), C15(H15), C11(H11), C9(H9), C28(H28) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.66300(8) 0.33700(8) 0.5000 0.0604(7) Uani 1 2 d S TU P . . Al2 Al 0.61770(9) 0.39045(8) 0.41629(5) 0.0676(6) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38282(7) 0.0586(7) Uani 1 2 d S TU P . . O2 O 0.56562(15) 0.47217(15) 0.41761(10) 0.0603(11) Uani 1 1 d . U . . . H2 H 0.5729 0.5018 0.4374 0.072 Uiso 1 1 calc R U . . . O3 O 0.64215(18) 0.40276(19) 0.36632(12) 0.0770(13) Uani 1 1 d . U . . . O1 O 0.60095(16) 0.36676(16) 0.46549(10) 0.0691(12) Uani 1 1 d . U . . . H1 H 0.5550 0.3707 0.4732 0.083 Uiso 1 1 calc R U . . . O4 O 0.5593(2) 0.47554(18) 0.34352(10) 0.0695(13) Uani 1 1 d . U . . . C1 C 0.6110(4) 0.4383(3) 0.3393(2) 0.0714(19) Uani 1 1 d . U . . . C26 C 0.7726(3) 0.6281(4) 0.1435(2) 0.111(3) Uani 1 1 d . U . . . H26 H 0.7688 0.6258 0.1688 0.134 Uiso 1 1 calc R U . . . C23 C 0.7803(3) 0.6363(4) 0.0644(2) 0.105(2) Uani 1 1 d . U . . . H23 H 0.7754 0.6389 0.0392 0.126 Uiso 1 1 calc R U . . . C20 C 0.9819(4) 0.1497(3) 0.11246(18) 0.076(2) Uani 1 1 d . U . . . C25 C 0.7801(4) 0.6946(4) 0.1207(2) 0.126(3) Uani 1 1 d . U . . . H25 H 0.7772 0.7370 0.1329 0.151 Uiso 1 1 calc R U . . . C22 C 0.7784(4) 0.5703(4) 0.0839(3) 0.126(3) Uani 1 1 d . U . . . H22 H 0.7817 0.5288 0.0709 0.152 Uiso 1 1 calc R U . . . C24 C 0.7899(4) 0.6961(4) 0.0862(3) 0.096(2) Uani 1 1 d . U . . . C27 C 0.8061(4) 0.7614(4) 0.0656(3) 0.086(3) Uani 1 1 d . U . . . C17 C 0.9352(3) 0.2116(3) 0.12120(18) 0.086(2) Uani 1 1 d . U . . . C7 C 0.6141(4) 0.4771(4) 0.2737(2) 0.134(3) Uani 1 1 d . U . . . H7 H 0.5716 0.5000 0.2759 0.160 Uiso 1 1 calc R U . . . C21 C 0.7723(4) 0.5688(4) 0.1182(3) 0.112(3) Uani 1 1 d . U . . . C5 C 0.6975(4) 0.4344(3) 0.2310(2) 0.100(2) Uani 1 1 d . U . . . C16 C 0.8715(4) 0.1992(3) 0.13891(19) 0.105(3) Uani 1 1 d . U . . . H16 H 0.8579 0.1541 0.1448 0.126 Uiso 1 1 calc R U . . . C8 C 0.7342(4) 0.4356(4) 0.1962(2) 0.119(3) Uani 1 1 d . U . . . C2 C 0.6473(4) 0.4381(3) 0.3069(2) 0.097(2) Uani 1 1 d . U . . . C18 C 0.9539(3) 0.2762(3) 0.1103(2) 0.125(3) Uani 1 1 d . U . . . H18 H 0.9936 0.2841 0.0963 0.149 Uiso 1 1 calc R U . . . C3 C 0.7020(4) 0.3954(4) 0.2982(2) 0.134(3) Uani 1 1 d . U . . . H3 H 0.7191 0.3651 0.3159 0.161 Uiso 1 1 calc R U . . . C4 C 0.7328(4) 0.3958(3) 0.2639(2) 0.108(2) Uani 1 1 d . U . . . H4 H 0.7749 0.3728 0.2604 0.130 Uiso 1 1 calc R U . . . C14 C 0.8483(4) 0.3229(4) 0.13633(19) 0.096(2) Uani 1 1 d . U . . . C6 C 0.6479(4) 0.4764(4) 0.2431(2) 0.126(3) Uani 1 1 d . U . . . H6 H 0.6352 0.5114 0.2268 0.151 Uiso 1 1 calc R U . . . C13 C 0.7360(4) 0.4956(4) 0.1742(2) 0.126(3) Uani 1 1 d . U . . . H13 H 0.7137 0.5354 0.1828 0.152 Uiso 1 1 calc R U . . . C19 C 0.9115(4) 0.3287(3) 0.12092(19) 0.101(2) Uani 1 1 d . U . . . H19 H 0.9279 0.3737 0.1171 0.121 Uiso 1 1 calc R U . . . C10 C 0.8082(3) 0.3817(4) 0.1512(2) 0.101(2) Uani 1 1 d . U . . . C15 C 0.8311(3) 0.2532(3) 0.14704(17) 0.092(2) Uani 1 1 d . U . . . H15 H 0.7902 0.2455 0.1601 0.110 Uiso 1 1 calc R U . . . C12 C 0.7676(4) 0.4987(4) 0.1421(2) 0.108(3) Uani 1 1 d . U . . . C11 C 0.8045(3) 0.4446(4) 0.12983(19) 0.106(3) Uani 1 1 d . U . . . H11 H 0.8278 0.4475 0.1076 0.127 Uiso 1 1 calc R U . . . C9 C 0.7728(3) 0.3778(3) 0.1849(2) 0.108(3) Uani 1 1 d . U . . . H9 H 0.7750 0.3378 0.1992 0.129 Uiso 1 1 calc R U . . . O8 O 0.82800(18) 0.80747(19) 0.08938(11) 0.0748(13) Uani 1 1 d . U . . . O10 O 0.73403(18) 0.3991(2) 0.48207(13) 0.0785(14) Uani 1 1 d . U . . . O5 O 1.0390(2) 0.16520(17) 0.09834(11) 0.0789(14) Uani 1 1 d . U . . . O6 O 0.96020(17) 0.08936(19) 0.12008(11) 0.0693(12) Uani 1 1 d . U . . . O9 O 0.6991(2) 0.4407(2) 0.42790(14) 0.0830(14) Uani 1 1 d . U . . . O7 O 0.8027(2) 0.7655(2) 0.03397(14) 0.0850(16) Uani 1 1 d . U . . . C28 C 0.7390(4) 0.4409(4) 0.4559(2) 0.094(3) Uani 1 1 d . U . . . H28 H 0.7740 0.4744 0.4569 0.113 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 0.0605(10) 0.0605(10) 0.060(2) 0.0012(11) 0.0012(11) 0.0009(12) Al2 0.0674(13) 0.0572(12) 0.0781(18) 0.0017(11) -0.0035(11) 0.0100(10) Al3 0.0661(17) 0.0537(16) 0.056(2) 0.000 0.000 0.0146(12) O2 0.072(2) 0.065(2) 0.044(3) -0.0052(17) 0.0026(19) 0.0138(19) O3 0.073(3) 0.077(3) 0.081(4) 0.011(2) 0.026(2) 0.020(2) O1 0.055(2) 0.076(3) 0.076(4) 0.021(2) -0.001(2) -0.0053(19) O4 0.080(3) 0.068(3) 0.060(4) -0.005(2) -0.001(2) 0.015(2) C1 0.085(5) 0.060(4) 0.070(6) 0.006(4) 0.024(4) 0.012(4) C26 0.181(7) 0.076(5) 0.076(7) 0.010(4) 0.028(5) 0.017(5) C23 0.150(7) 0.089(5) 0.075(7) 0.002(4) 0.023(4) -0.020(4) C20 0.088(5) 0.062(4) 0.079(6) -0.009(4) 0.026(4) -0.005(4) C25 0.219(8) 0.090(5) 0.069(7) 0.004(5) 0.022(6) -0.014(5) C22 0.192(8) 0.083(5) 0.103(8) 0.005(5) 0.064(6) -0.002(5) C24 0.126(6) 0.085(5) 0.078(7) 0.005(5) 0.017(5) -0.011(4) C27 0.102(5) 0.081(5) 0.076(7) 0.010(5) 0.004(5) 0.004(4) C17 0.100(5) 0.066(4) 0.092(7) -0.012(4) 0.032(4) 0.006(4) C7 0.143(7) 0.168(7) 0.090(7) 0.051(5) 0.053(5) 0.100(6) C21 0.153(6) 0.076(5) 0.106(7) 0.009(5) 0.059(6) 0.014(4) C5 0.120(6) 0.079(5) 0.101(7) 0.025(4) 0.042(5) 0.024(4) C16 0.112(5) 0.072(5) 0.132(8) -0.012(4) 0.054(5) 0.002(4) C8 0.152(7) 0.083(5) 0.122(7) 0.021(5) 0.056(5) 0.038(5) C2 0.109(5) 0.088(5) 0.096(6) 0.026(4) 0.040(4) 0.054(4) C18 0.122(6) 0.062(4) 0.190(9) 0.003(5) 0.077(5) 0.005(4) C3 0.142(6) 0.145(7) 0.116(8) 0.040(5) 0.067(5) 0.075(6) C4 0.127(6) 0.077(5) 0.121(7) 0.007(5) 0.044(5) 0.040(4) C14 0.109(5) 0.077(5) 0.102(7) -0.012(4) 0.030(4) 0.001(4) C6 0.148(7) 0.125(6) 0.104(8) 0.035(5) 0.050(5) 0.073(5) C13 0.181(8) 0.079(5) 0.118(7) 0.019(5) 0.086(6) 0.044(5) C19 0.116(6) 0.079(5) 0.106(7) 0.000(4) 0.043(5) 0.006(4) C10 0.107(5) 0.078(5) 0.117(7) 0.002(4) 0.044(4) -0.004(4) C15 0.111(5) 0.072(5) 0.093(7) -0.013(4) 0.045(4) 0.000(4) C12 0.128(6) 0.083(5) 0.115(7) 0.004(5) 0.056(5) 0.021(4) C11 0.133(6) 0.086(5) 0.100(7) 0.009(4) 0.067(5) 0.022(4) C9 0.135(6) 0.071(5) 0.117(7) 0.020(4) 0.071(5) 0.016(4) O8 0.088(3) 0.073(3) 0.064(4) 0.002(2) 0.013(2) -0.017(2) O10 0.064(3) 0.074(3) 0.098(5) -0.001(2) 0.001(2) 0.002(2) O5 0.092(3) 0.050(3) 0.095(4) -0.003(2) 0.029(3) 0.000(2) O6 0.076(3) 0.059(3) 0.073(4) -0.011(2) 0.018(2) 0.000(2) O9 0.067(3) 0.084(3) 0.098(5) 0.013(3) 0.007(2) -0.001(2) O7 0.089(3) 0.093(3) 0.073(4) 0.008(3) -0.005(3) -0.012(2) C28 0.079(5) 0.101(6) 0.101(7) 0.012(5) 0.004(4) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.827(4) 8_666 ? Al1 O1 1.827(4) . ? Al1 O10 1.926(4) . ? Al1 O10 1.926(4) 8_666 ? Al1 O7 1.965(5) 6_645 ? Al1 O7 1.965(5) 2_645 ? Al2 O2 1.861(3) . ? Al2 O3 1.901(5) . ? Al2 O1 1.883(4) . ? Al2 O8 1.915(4) 6_645 ? Al2 O5 1.926(4) 5_455 ? Al2 O9 1.885(4) . ? Al3 O2 1.868(4) 3_665 ? Al3 O2 1.868(4) . ? Al3 O4 1.892(4) 3_665 ? Al3 O4 1.892(4) . ? Al3 O6 1.881(3) 6_655 ? Al3 O6 1.881(3) 5_455 ? O3 C1 1.341(7) . ? O4 C1 1.232(7) . ? C1 C2 1.375(8) . ? C26 C25 1.531(9) . ? C26 C21 1.467(9) . ? C23 C22 1.453(8) . ? C23 C24 1.410(9) . ? C20 C17 1.522(8) . ? C20 O5 1.248(6) . ? C20 O6 1.262(6) . ? C25 C24 1.275(8) . ? C22 C21 1.260(9) . ? C24 C27 1.496(10) . ? C27 O8 1.310(8) . ? C27 O7 1.161(8) . ? C17 C16 1.405(7) . ? C17 C18 1.350(7) . ? C7 C2 1.563(9) . ? C7 C6 1.293(8) . ? C21 C12 1.608(9) . ? C5 C8 1.455(9) . ? C5 C4 1.566(9) . ? C5 C6 1.326(8) . ? C16 C15 1.328(7) . ? C8 C13 1.404(8) . ? C8 C9 1.396(8) . ? C2 C3 1.370(8) . ? C18 C19 1.351(7) . ? C3 C4 1.387(8) . ? C14 C19 1.342(7) . ? C14 C10 1.469(8) . ? C14 C15 1.434(8) . ? C13 C12 1.325(8) . ? C10 C11 1.439(8) . ? C10 C9 1.411(8) . ? C12 C11 1.335(7) . ? O8 Al2 1.915(4) 6_655 ? O10 C28 1.252(7) . ? O5 Al2 1.926(4) 5 ? O6 Al3 1.881(3) 5 ? O9 C28 1.279(8) . ? O7 Al1 1.965(5) 4_564 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 94.0(2) 8_666 . ? O1 Al1 O10 93.03(16) . 8_666 ? O1 Al1 O10 91.88(16) . . ? O1 Al1 O10 91.89(16) 8_666 8_666 ? O1 Al1 O10 93.03(16) 8_666 . ? O1 Al1 O7 175.5(2) 8_666 6_645 ? O1 Al1 O7 90.01(17) 8_666 2_645 ? O1 Al1 O7 90.01(17) . 6_645 ? O1 Al1 O7 175.5(2) . 2_645 ? O10 Al1 O10 172.8(2) 8_666 . ? O10 Al1 O7 85.88(18) . 2_645 ? O10 Al1 O7 88.85(18) . 6_645 ? O10 Al1 O7 85.88(18) 8_666 6_645 ? O10 Al1 O7 88.85(18) 8_666 2_645 ? O7 Al1 O7 86.1(3) 6_645 2_645 ? O2 Al2 O3 93.03(16) . . ? O2 Al2 O1 94.99(16) . . ? O2 Al2 O8 175.2(2) . 6_645 ? O2 Al2 O5 93.06(16) . 5_455 ? O2 Al2 O9 90.48(16) . . ? O3 Al2 O8 82.24(18) . 6_645 ? O3 Al2 O5 89.73(18) . 5_455 ? O1 Al2 O3 171.98(16) . . ? O1 Al2 O8 89.74(17) . 6_645 ? O1 Al2 O5 89.87(17) . 5_455 ? O1 Al2 O9 92.87(19) . . ? O8 Al2 O5 86.30(17) 6_645 5_455 ? O9 Al2 O3 87.0(2) . . ? O9 Al2 O8 89.92(17) . 6_645 ? O9 Al2 O5 175.3(2) . 5_455 ? O2 Al3 O2 94.2(2) 3_665 . ? O2 Al3 O4 173.48(19) . 3_665 ? O2 Al3 O4 92.34(15) . . ? O2 Al3 O4 173.48(19) 3_665 . ? O2 Al3 O4 92.34(15) 3_665 3_665 ? O2 Al3 O6 92.96(15) 3_665 6_655 ? O2 Al3 O6 91.45(15) 3_665 5_455 ? O2 Al3 O6 92.96(15) . 5_455 ? O2 Al3 O6 91.45(15) . 6_655 ? O4 Al3 O4 81.1(3) . 3_665 ? O6 Al3 O4 88.57(16) 6_655 3_665 ? O6 Al3 O4 86.52(16) 6_655 . ? O6 Al3 O4 86.52(16) 5_455 3_665 ? O6 Al3 O4 88.57(16) 5_455 . ? O6 Al3 O6 173.5(3) 5_455 6_655 ? Al2 O2 Al3 125.8(2) . . ? C1 O3 Al2 131.3(4) . . ? Al1 O1 Al2 128.61(18) . . ? C1 O4 Al3 136.3(4) . . ? O3 C1 C2 114.0(7) . . ? O4 C1 O3 124.3(7) . . ? O4 C1 C2 121.1(7) . . ? C21 C26 C25 107.7(7) . . ? C24 C23 C22 115.9(8) . . ? O5 C20 C17 114.7(6) . . ? O5 C20 O6 126.8(6) . . ? O6 C20 C17 118.5(6) . . ? C24 C25 C26 124.8(8) . . ? C21 C22 C23 120.6(8) . . ? C23 C24 C27 115.1(8) . . ? C25 C24 C23 121.4(8) . . ? C25 C24 C27 123.3(9) . . ? O8 C27 C24 107.3(8) . . ? O7 C27 C24 123.3(9) . . ? O7 C27 O8 129.3(9) . . ? C16 C17 C20 118.4(6) . . ? C18 C17 C20 119.9(7) . . ? C18 C17 C16 121.6(6) . . ? C6 C7 C2 117.6(7) . . ? C26 C21 C12 107.9(8) . . ? C22 C21 C26 127.6(8) . . ? C22 C21 C12 124.4(8) . . ? C8 C5 C4 118.1(7) . . ? C6 C5 C8 129.1(8) . . ? C6 C5 C4 110.0(7) . . ? C15 C16 C17 118.6(6) . . ? C13 C8 C5 121.7(7) . . ? C9 C8 C5 120.2(7) . . ? C9 C8 C13 118.0(7) . . ? C1 C2 C7 117.5(7) . . ? C3 C2 C1 126.3(7) . . ? C3 C2 C7 114.7(7) . . ? C17 C18 C19 116.1(6) . . ? C2 C3 C4 122.3(8) . . ? C3 C4 C5 120.9(7) . . ? C19 C14 C10 124.4(7) . . ? C19 C14 C15 113.6(6) . . ? C15 C14 C10 119.7(7) . . ? C7 C6 C5 131.0(8) . . ? C12 C13 C8 123.7(7) . . ? C14 C19 C18 127.1(7) . . ? C11 C10 C14 118.0(7) . . ? C9 C10 C14 122.3(7) . . ? C9 C10 C11 119.6(6) . . ? C16 C15 C14 122.2(6) . . ? C13 C12 C21 123.1(7) . . ? C13 C12 C11 120.4(7) . . ? C11 C12 C21 116.1(7) . . ? C12 C11 C10 119.8(7) . . ? C8 C9 C10 118.2(7) . . ? C27 O8 Al2 131.6(5) . 6_655 ? C28 O10 Al1 135.3(5) . . ? C20 O5 Al2 132.3(4) . 5 ? C20 O6 Al3 133.7(4) . 5 ? C28 O9 Al2 132.7(5) . . ? C27 O7 Al1 131.2(6) . 4_564 ? O10 C28 O9 124.4(8) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.259 -0.456 -0.833 9629.5 10558.6 ? _shelx_res_file ; p3_25kev_0m.res created by SHELXL-2014/7 TITL P3_25kev_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.196 19.196 36.569 90 90 90 ZERR 222 0.00271 0.00271 0.00731 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.12 0.11 744.346 DISP C 0.009 0.004 30.879 DISP H -0 0 0.639 DISP O 0.025 0.014 100.516 UNIT 224 144 80 16 RIGU C13 Al1 O1 O10 Al2 H1 C28 O2 O3 O9 H28 Al3 H2 C1 O4 C2 C7 C3 H7 C6 H3 = C4 C5 H6 H4 C8 C9 H13 C12 C10 H9 C21 C11 C14 C26 C22 H11 C19 C15 H26 C25 C23 = H22 C18 H19 C16 H15 H25 C24 H23 C17 H18 H16 C27 C20 O8 O7 O5 O6 AL1 O1 AL1 = O10 AL2 O1 O1 H1 O10 C28 AL2 O2 AL2 O3 AL2 O9 O9 C28 C28 H28 AL3 O2 O2 H2 O3 = C1 AL3 O4 O4 C1 C2 C1 C7 C2 C3 C2 C7 H7 C7 C6 C3 H3 C4 C3 C6 C5 C6 H6 C5 C4 = C4 H4 C8 C5 C8 C13 C9 C8 C13 H13 C13 C12 C9 C10 C9 H9 C21 C12 C12 C11 C14 = C10 C11 C10 C26 C21 C22 C21 C11 H11 C19 C14 C15 C14 C26 H26 C26 C25 C23 C22 = C22 H22 C19 C18 C19 H19 C16 C15 C15 H15 C25 H25 C25 C24 C23 H23 C24 C23 C18 = C17 C18 H18 C17 C16 C16 H16 C27 C24 C20 C17 O8 C27 O7 C27 O5 C20 O6 C20 RIGU C10 Al1 O1 O10 Al2 H1 C28 O2 O3 O9 H28 Al3 H2 C1 O4 C2 C7 C3 H7 C6 H3 = C4 C5 H6 H4 C8 C13 C9 H13 C12 H9 C21 C11 C14 C26 C22 H11 C19 C15 H26 C25 C23 = H22 C18 H19 C16 H15 H25 C24 H23 C17 H18 H16 C27 C20 O8 O7 O5 O6 AL1 O1 AL1 = O10 AL2 O1 O1 H1 O10 C28 AL2 O2 AL2 O3 AL2 O9 O9 C28 C28 H28 AL3 O2 O2 H2 O3 = C1 AL3 O4 O4 C1 C2 C1 C7 C2 C3 C2 C7 H7 C7 C6 C3 H3 C4 C3 C6 C5 C6 H6 C5 C4 = C4 H4 C8 C5 C8 C13 C9 C8 C13 H13 C13 C12 C9 C10 C9 H9 C21 C12 C12 C11 C14 = C10 C11 C10 C26 C21 C22 C21 C11 H11 C19 C14 C15 C14 C26 H26 C26 C25 C23 C22 = C22 H22 C19 C18 C19 H19 C16 C15 C15 H15 C25 H25 C25 C24 C23 H23 C24 C23 C18 = C17 C18 H18 C17 C16 C16 H16 C27 C24 C20 C17 O8 C27 O7 C27 O5 C20 O6 C20 L.S. 24 PLAN 20 TEMP 23 BOND ABIN ACTA fmap 2 REM REM REM WGHT 0.026000 FVAR 0.11317 AL1 4 0.662996 0.337004 0.500000 10.50000 0.06046 0.06046 = 0.06041 0.00119 0.00119 0.00091 AL2 4 0.617703 0.390452 0.416292 11.00000 0.06737 0.05720 = 0.07811 0.00169 -0.00354 0.00999 AL3 4 0.500000 0.500000 0.382822 10.50000 0.06609 0.05369 = 0.05616 0.00000 0.00000 0.01465 O2 3 0.565625 0.472174 0.417615 11.00000 0.07174 0.06540 = 0.04364 -0.00519 0.00265 0.01380 AFIX 43 H2 2 0.572913 0.501821 0.437361 11.00000 -1.20000 AFIX 0 O3 3 0.642146 0.402755 0.366320 11.00000 0.07286 0.07687 = 0.08135 0.01061 0.02602 0.02031 O1 3 0.600947 0.366763 0.465490 11.00000 0.05538 0.07634 = 0.07551 0.02065 -0.00074 -0.00529 AFIX 43 H1 2 0.554980 0.370743 0.473246 11.00000 -1.20000 AFIX 0 O4 3 0.559259 0.475536 0.343525 11.00000 0.08047 0.06809 = 0.05997 -0.00535 -0.00085 0.01481 C1 1 0.610966 0.438321 0.339333 11.00000 0.08504 0.05955 = 0.06969 0.00586 0.02419 0.01193 C26 1 0.772550 0.628122 0.143471 11.00000 0.18139 0.07606 = 0.07643 0.00971 0.02784 0.01735 AFIX 43 H26 2 0.768829 0.625755 0.168796 11.00000 -1.20000 AFIX 0 C23 1 0.780259 0.636284 0.064447 11.00000 0.15007 0.08911 = 0.07490 0.00200 0.02334 -0.02019 AFIX 43 H23 2 0.775386 0.638912 0.039182 11.00000 -1.20000 AFIX 0 C20 1 0.981856 0.149735 0.112458 11.00000 0.08800 0.06221 = 0.07861 -0.00907 0.02641 -0.00488 C25 1 0.780063 0.694593 0.120697 11.00000 0.21896 0.08987 = 0.06924 0.00361 0.02236 -0.01382 AFIX 43 H25 2 0.777223 0.737000 0.132903 11.00000 -1.20000 AFIX 0 C22 1 0.778377 0.570272 0.083870 11.00000 0.19236 0.08311 = 0.10348 0.00454 0.06394 -0.00227 AFIX 43 H22 2 0.781706 0.528759 0.070876 11.00000 -1.20000 AFIX 0 C24 1 0.789925 0.696120 0.086237 11.00000 0.12598 0.08467 = 0.07801 0.00541 0.01728 -0.01084 C27 1 0.806135 0.761392 0.065585 11.00000 0.10228 0.08071 = 0.07574 0.00961 0.00411 0.00376 C17 1 0.935237 0.211649 0.121196 11.00000 0.09964 0.06650 = 0.09172 -0.01229 0.03207 0.00634 C7 1 0.614095 0.477135 0.273702 11.00000 0.14328 0.16789 = 0.08973 0.05144 0.05275 0.09999 AFIX 43 H7 2 0.571587 0.500015 0.275852 11.00000 -1.20000 AFIX 0 C21 1 0.772274 0.568797 0.118163 11.00000 0.15297 0.07629 = 0.10633 0.00870 0.05934 0.01438 C5 1 0.697533 0.434356 0.230989 11.00000 0.12021 0.07881 = 0.10143 0.02462 0.04182 0.02409 C16 1 0.871495 0.199169 0.138909 11.00000 0.11153 0.07152 = 0.13200 -0.01192 0.05352 0.00159 AFIX 43 H16 2 0.857887 0.154055 0.144819 11.00000 -1.20000 AFIX 0 C8 1 0.734198 0.435581 0.196172 11.00000 0.15193 0.08337 = 0.12169 0.02106 0.05611 0.03837 C2 1 0.647282 0.438137 0.306938 11.00000 0.10866 0.08758 = 0.09616 0.02550 0.03962 0.05438 C18 1 0.953903 0.276222 0.110313 11.00000 0.12204 0.06187 = 0.18965 0.00306 0.07663 0.00501 AFIX 43 H18 2 0.993600 0.284134 0.096338 11.00000 -1.20000 AFIX 0 C3 1 0.701986 0.395406 0.298180 11.00000 0.14153 0.14527 = 0.11588 0.03982 0.06683 0.07508 AFIX 43 H3 2 0.719063 0.365077 0.315870 11.00000 -1.20000 AFIX 0 C4 1 0.732777 0.395783 0.263881 11.00000 0.12737 0.07660 = 0.12131 0.00669 0.04418 0.04016 AFIX 43 H4 2 0.774911 0.372828 0.260362 11.00000 -1.20000 AFIX 0 C14 1 0.848324 0.322930 0.136325 11.00000 0.10870 0.07669 = 0.10152 -0.01214 0.02963 0.00086 C6 1 0.647881 0.476435 0.243107 11.00000 0.14790 0.12523 = 0.10387 0.03508 0.05002 0.07254 AFIX 43 H6 2 0.635174 0.511423 0.226830 11.00000 -1.20000 AFIX 0 C13 1 0.735962 0.495570 0.174239 11.00000 0.18148 0.07895 = 0.11841 0.01947 0.08641 0.04397 AFIX 43 H13 2 0.713668 0.535395 0.182769 11.00000 -1.20000 AFIX 0 C19 1 0.911517 0.328676 0.120917 11.00000 0.11647 0.07910 = 0.10635 0.00024 0.04252 0.00588 AFIX 43 H19 2 0.927934 0.373680 0.117121 11.00000 -1.20000 AFIX 0 C10 1 0.808248 0.381687 0.151161 11.00000 0.10687 0.07818 = 0.11731 0.00183 0.04403 -0.00429 C15 1 0.831079 0.253164 0.147036 11.00000 0.11112 0.07226 = 0.09285 -0.01314 0.04467 0.00049 AFIX 43 H15 2 0.790238 0.245466 0.160106 11.00000 -1.20000 AFIX 0 C12 1 0.767578 0.498679 0.142079 11.00000 0.12765 0.08275 = 0.11495 0.00392 0.05606 0.02064 C11 1 0.804521 0.444556 0.129831 11.00000 0.13252 0.08574 = 0.09996 0.00914 0.06725 0.02243 AFIX 43 H11 2 0.827779 0.447490 0.107575 11.00000 -1.20000 AFIX 0 C9 1 0.772782 0.377781 0.184886 11.00000 0.13545 0.07112 = 0.11714 0.01974 0.07109 0.01645 AFIX 43 H9 2 0.775036 0.337811 0.199209 11.00000 -1.20000 AFIX 0 O8 3 0.827998 0.807472 0.089379 11.00000 0.08776 0.07275 = 0.06385 0.00236 0.01265 -0.01652 O10 3 0.734035 0.399118 0.482072 11.00000 0.06417 0.07361 = 0.09772 -0.00130 0.00095 0.00222 O5 3 1.039016 0.165196 0.098344 11.00000 0.09151 0.04992 = 0.09541 -0.00299 0.02885 -0.00001 O6 3 0.960198 0.089360 0.120083 11.00000 0.07567 0.05893 = 0.07323 -0.01064 0.01788 -0.00007 O9 3 0.699135 0.440685 0.427898 11.00000 0.06734 0.08391 = 0.09783 0.01302 0.00748 -0.00051 O7 3 0.802704 0.765523 0.033972 11.00000 0.08870 0.09340 = 0.07289 0.00772 -0.00468 -0.01232 C28 1 0.738991 0.440910 0.455925 11.00000 0.07919 0.10126 = 0.10134 0.01168 0.00426 -0.00731 AFIX 43 H28 2 0.773988 0.474355 0.456946 11.00000 -1.20000 AFIX 0 HKLF 4 REM P3_25kev_0m in P42212 #94 REM R1 = 0.0396 for 3219 Fo > 4sig(Fo) and 0.0658 for all 4730 data REM 362 parameters refined using 336 restraints END WGHT 0.0267 0.0000 REM Highest difference peak 0.097, deepest hole -0.219, 1-sigma level 0.019 Q1 1 0.6410 0.3565 0.5187 11.00000 0.05 0.10 Q2 1 0.5406 0.3574 0.5009 11.00000 0.05 0.09 Q3 1 0.5399 0.4809 0.3625 11.00000 0.05 0.09 Q4 1 0.6898 0.3231 0.5189 11.00000 0.05 0.09 Q5 1 0.6373 0.3543 0.3947 11.00000 0.05 0.08 Q6 1 0.6084 0.5264 0.2593 11.00000 0.05 0.08 Q7 1 0.8431 0.5578 0.1128 11.00000 0.05 0.08 Q8 1 0.8038 0.1992 0.1724 11.00000 0.05 0.08 Q9 1 0.5000 0.5000 0.4551 10.50000 0.05 0.08 Q10 1 0.5652 0.4492 0.2475 11.00000 0.05 0.08 Q11 1 0.8579 0.6887 0.1116 11.00000 0.05 0.08 Q12 1 0.5000 0.5000 0.4026 10.50000 0.05 0.07 Q13 1 0.7632 0.6524 0.1286 11.00000 0.05 0.07 Q14 1 0.7791 0.5119 0.4549 11.00000 0.05 0.07 Q15 1 0.7210 0.6303 0.0391 11.00000 0.05 0.07 Q16 1 0.6354 0.5058 0.3817 11.00000 0.05 0.07 Q17 1 1.0206 0.1191 0.1590 11.00000 0.05 0.07 Q18 1 0.7360 0.2942 0.3316 11.00000 0.05 0.07 Q19 1 0.6063 0.3945 0.4751 11.00000 0.05 0.07 Q20 1 0.7369 0.7463 0.0446 11.00000 0.05 0.07 ; _shelx_res_checksum 75070 _shelx_hkl_file ; 0 -3 0 0.02 0.08 0 -4 0 53.78 3.48 0 -5 0 -0.01 0.14 -1 -5 0 42.31 2.79 0 -6 0 190.29 12.26 -1 -6 0 21.77 1.49 -2 -6 0 27.41 1.88 0 -7 0 -0.18 0.22 -1 -7 0 69.16 4.52 -2 -7 0 16.33 1.19 0 -8 0 3.43 0.45 -1 -8 0 85.21 5.56 -2 -8 0 97.19 6.35 -3 -8 0 12.13 0.99 -4 8 0 17.60 1.19 0 -9 0 -0.05 0.33 -1 -9 0 20.04 1.62 1 -9 0 26.43 1.62 -2 -9 0 0.59 0.39 -3 -9 0 0.61 0.42 -5 9 0 93.45 6.06 -6 9 0 3.34 0.42 0 -10 0 5.25 0.64 1 -10 0 7.16 0.75 -1 -10 0 8.04 0.78 -2 -10 0 0.05 0.36 -3 -10 0 84.12 5.57 -4 -10 0 -0.02 0.39 -5 10 0 10.35 0.76 -6 10 0 6.19 0.57 -7 10 0 25.86 1.81 0 -11 0 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1.55 0.61 -5 0 9 1.39 0.71 0 5 -9 1.35 0.88 1 5 -9 236.71 14.39 5 -1 -9 225.71 14.28 -5 -1 9 220.53 14.34 -5 1 9 225.83 14.35 -1 -5 9 202.07 14.26 5 1 -9 199.59 14.29 2 5 -9 27.94 2.29 5 -2 -9 29.07 2.19 -5 -2 9 28.68 2.29 2 -5 -9 31.84 2.26 5 2 -9 27.51 2.29 -5 2 9 29.37 2.37 -2 -5 9 27.16 2.41 3 5 -9 4.80 0.94 -5 -3 9 6.35 1.08 5 -3 -9 4.95 0.83 3 -5 -9 6.82 1.29 -5 3 9 6.38 1.16 -3 -5 9 6.32 1.38 5 3 -9 5.31 0.96 -5 -4 9 7.06 1.24 4 5 -9 6.10 1.07 -4 5 9 6.31 1.05 5 -4 -9 6.26 0.92 5 4 -9 8.40 1.07 4 -5 -9 7.34 1.03 -5 4 9 8.87 1.42 -4 -5 9 7.36 1.27 -5 -5 9 0.52 0.79 -5 5 9 1.80 1.32 5 -5 -9 1.07 0.59 5 5 -9 0.38 0.62 -6 0 9 0.90 0.69 6 0 -9 1.78 0.72 0 6 -9 1.48 1.23 1 6 -9 154.92 9.72 6 -1 -9 143.82 9.59 -6 -1 9 145.24 9.65 -6 1 9 142.04 9.61 -1 -6 9 128.88 9.56 6 1 -9 146.28 9.61 -1 6 -9 153.04 9.67 2 6 -9 34.53 2.58 6 -2 -9 35.48 2.56 -6 -2 9 35.57 2.62 -6 2 9 33.60 2.58 6 2 -9 31.26 2.54 2 -6 -9 33.20 2.52 -2 -6 9 32.77 2.73 3 6 -9 13.64 1.31 -6 -3 9 12.84 1.44 6 -3 -9 15.00 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13 7 16 -4.5501 -4.8444 13 7 17 1.3361 0.4799 13 8 0 8.6501 -0.0000 13 8 1 -2.0835 -3.1448 13 8 2 1.1876 4.1250 13 8 3 7.0585 -3.9544 13 8 4 -3.2039 -1.4846 13 8 5 -2.0219 -8.4005 13 8 6 1.1549 -0.9041 13 8 7 0.6476 -0.5117 13 8 8 1.1234 0.7195 13 8 9 -2.4207 2.6646 13 8 10 -4.1433 4.7448 13 8 11 -1.5040 -0.0535 13 8 12 -0.2141 5.8105 13 8 13 0.9538 1.6939 13 8 14 -1.5390 4.6557 13 8 15 1.2025 -0.6910 13 8 16 1.2846 3.1968 13 9 0 5.7080 -0.0000 13 9 1 -1.0290 2.9069 13 9 2 3.7099 -1.7877 13 9 3 4.3477 -0.2893 13 9 4 0.4771 -0.2293 13 9 5 -1.1146 1.0172 13 9 6 1.0068 -0.7700 13 9 7 -0.8954 0.8034 13 9 8 -0.0338 -0.0808 13 9 9 1.6880 0.5098 13 9 10 -2.1807 4.4341 13 9 11 -0.9901 -2.0747 13 9 12 0.8928 -0.2863 13 9 13 -0.2002 1.2321 13 9 14 -3.9802 1.8792 13 10 0 5.1985 -0.0000 13 10 1 -2.8325 2.8253 13 10 2 3.5579 -0.4271 13 10 3 3.0746 -1.6501 13 10 4 -1.6959 0.0691 13 10 5 1.0734 -1.5033 13 10 6 3.4501 4.2061 13 10 7 0.3464 1.8543 13 10 8 2.4883 -0.4423 13 10 9 5.2738 -3.9474 13 10 10 -2.0995 3.4562 13 10 11 3.3578 1.5195 13 11 0 -3.6216 0.0000 13 11 1 0.2685 -2.1177 13 11 2 -2.2613 4.0153 13 11 3 -1.9117 -2.9911 13 11 4 -0.5765 -2.6476 13 11 5 -2.9122 1.5766 13 11 6 1.7554 2.1424 13 11 7 0.5272 -2.4931 14 0 0 -5.8987 0.0000 14 0 1 -0.0000 -2.0013 14 0 2 -6.1727 -0.0000 14 0 3 0.0000 3.4423 14 0 4 2.3773 0.0000 14 0 5 -0.0000 -8.6195 14 0 6 -8.0636 -0.0000 14 0 7 0.0000 1.7081 14 0 8 4.4854 -0.0000 14 0 9 -0.0000 -4.1113 14 0 10 1.2188 -0.0000 14 0 11 -0.0000 -7.0716 14 0 12 -4.1136 0.0000 14 0 13 -0.0000 -2.4575 14 0 14 0.0899 -0.0000 14 0 15 0.0000 0.8833 14 0 16 0.1831 0.0000 14 0 17 0.0000 2.4872 14 0 18 2.7430 0.0000 14 0 19 0.0000 1.9059 14 1 0 2.5801 -0.0000 14 1 1 3.3964 0.5162 14 1 2 2.2299 1.6141 14 1 6 -0.0784 -3.7879 14 1 7 1.1472 -3.3613 14 1 8 -2.1373 -1.6948 14 1 9 -7.5617 7.5075 14 1 10 2.1790 -2.5998 14 1 11 -0.3877 2.1965 14 1 12 -3.8882 2.6748 14 1 13 -4.6112 -5.3833 14 1 14 -0.2196 -3.6720 14 1 15 3.6621 -1.5804 14 1 16 -0.9229 5.1767 14 1 17 1.4173 5.8945 14 1 18 1.4184 -2.4876 14 1 19 6.5725 1.7230 14 2 0 1.1172 0.0000 14 2 1 -5.7109 -5.7700 14 2 2 -6.1910 -0.9063 14 2 7 -2.7377 5.5125 14 2 9 0.1772 5.4794 14 2 10 -10.1222 -3.2025 14 2 11 -5.0505 0.8707 14 2 12 5.6278 2.0637 14 2 13 -0.7123 4.2166 14 2 14 1.1403 3.0691 14 2 15 -0.2528 0.3008 14 2 16 -1.3081 3.9985 14 2 17 -2.3298 2.2129 14 2 18 -6.9928 -2.4954 14 2 19 -2.6406 2.4007 14 3 0 0.4843 -0.0000 14 3 1 5.0994 -1.0178 14 3 2 6.2953 -0.4584 14 3 7 -1.9313 -6.3295 14 3 8 3.5548 -0.7817 14 3 9 -1.9328 -4.7093 14 3 10 2.2585 8.3953 14 3 11 -1.0429 -4.1839 14 3 12 0.4159 2.2861 14 3 13 1.4855 4.4582 14 3 14 -1.9971 1.8879 14 3 15 2.5656 -1.8466 14 3 16 2.7871 4.4701 14 3 17 7.1717 1.9142 14 3 18 4.9944 1.4034 14 3 19 4.3779 1.9055 14 4 0 5.9064 -0.0000 14 4 1 7.3285 6.7094 14 4 8 3.9033 -2.2919 14 4 9 0.1688 0.2808 14 4 10 1.1031 -2.1007 14 4 11 -7.6300 1.6517 14 4 12 -1.0118 -2.0295 14 4 13 -3.8365 2.4310 14 4 14 6.2860 -3.3327 14 4 15 0.0522 -0.3097 14 4 16 1.3411 1.7284 14 4 17 1.7006 5.1034 14 4 18 1.2681 0.8622 14 5 0 2.6840 -0.0000 14 5 9 2.8501 2.3472 14 5 10 9.5744 3.2438 14 5 11 7.1214 3.8010 14 5 12 1.7396 -0.1292 14 5 13 4.2139 -3.9994 14 5 14 6.1478 -2.6639 14 5 15 -1.5545 0.5136 14 5 16 3.6679 1.4606 14 5 17 -3.5307 -0.4853 14 6 9 -0.7394 -0.9222 14 6 10 2.4178 -1.1893 14 6 11 2.5810 -1.5687 14 6 12 -4.4707 -1.9516 14 6 13 -0.1836 1.6252 14 6 14 -1.1491 -4.7206 14 6 15 -1.9242 1.0648 14 6 16 2.1791 -1.8460 14 7 10 3.4800 -1.2033 14 7 11 4.2937 -1.5980 14 7 12 -0.3563 0.4043 14 7 13 2.8610 1.8403 14 7 14 1.7227 -2.9757 14 8 0 3.2019 -0.0000 14 8 1 1.5597 -2.2486 14 8 2 1.1356 2.5579 14 8 3 -1.3658 -3.2180 14 8 4 3.0857 3.4106 14 8 5 2.8538 1.1733 14 8 10 -1.6828 -0.2348 14 8 11 0.5579 -1.8968 14 8 12 1.4728 -2.7746 14 9 0 4.1290 -0.0000 14 9 1 4.3831 -0.9189 14 9 2 -1.9284 -3.8959 14 9 3 10.9381 -3.2076 14 9 4 4.2265 0.2838 14 9 5 1.4684 2.4291 14 9 6 -0.8311 -3.6099 14 9 8 -3.5109 1.8866 14 9 9 1.3112 1.0544 14 10 0 -2.2714 0.0000 14 10 1 -0.5142 -1.5694 14 10 2 -1.1958 -3.5510 14 10 3 7.7410 -3.3519 14 10 4 0.2780 -2.8485 14 10 5 2.0563 -1.4016 15 0 1 -2.2564 0.0000 15 0 2 0.0000 5.4702 15 0 3 4.9084 0.0000 15 0 4 0.0000 0.8315 15 0 5 7.9526 0.0000 15 0 6 -0.0000 -3.7263 15 0 7 -1.9778 -0.0000 15 0 8 -0.0000 -2.5018 15 0 9 1.6765 -0.0000 15 0 10 -0.0000 -8.5189 15 0 11 -1.6002 -0.0000 15 0 12 -0.0000 -0.1742 15 0 13 -5.0082 -0.0000 15 0 14 0.0000 5.3917 15 0 15 0.8777 0.0000 15 0 16 0.0000 5.9752 15 1 0 9.3095 -0.0000 15 1 1 -3.7997 -1.3288 15 1 3 -3.4806 3.4825 15 1 7 -9.0120 1.0592 15 1 8 9.0605 -12.3373 15 1 9 -0.4023 -2.6679 15 1 10 -0.1448 4.0316 15 1 11 -1.5190 -3.2137 15 1 12 -2.2881 -1.4003 15 1 13 -6.0400 -3.7485 15 1 14 5.2348 -3.5297 15 1 15 -1.0591 -2.9624 15 1 16 -3.3105 -0.7772 15 2 0 -1.5546 0.0000 15 2 1 5.2059 7.6049 15 2 2 1.6185 -5.3043 15 2 3 -1.0525 -4.9908 15 2 9 0.2463 -10.9129 15 2 10 5.6568 0.2244 15 2 11 2.4503 6.9236 15 2 12 0.7882 1.1988 15 2 13 2.6184 -2.1822 15 2 14 2.7055 0.2416 15 2 15 -2.6233 3.4838 15 2 16 1.4637 -5.2587 15 3 0 5.7191 -0.0000 15 3 1 3.4088 -5.8020 15 3 2 2.6098 -9.0228 15 3 8 2.6089 4.6505 15 3 10 -0.8525 -2.5033 15 3 11 -5.2014 -0.6952 15 3 12 0.5814 6.8941 15 3 13 0.8118 3.9092 15 3 14 0.3601 -1.7135 15 3 15 -2.1747 4.5952 15 4 0 0.6760 -0.0000 15 4 1 -6.7963 -2.2243 15 4 9 4.5204 -0.8718 15 4 10 -0.9669 1.7361 15 4 11 0.1414 -1.7281 15 4 12 2.7234 -0.6120 15 4 13 1.9780 2.8463 15 4 14 0.2278 0.6456 15 4 15 -2.7309 2.0118 15 5 0 5.1985 -0.0000 15 5 1 2.4169 -0.9969 15 5 10 0.3595 -1.2066 15 5 11 1.6105 -0.4810 15 5 12 -1.8755 3.0507 15 5 13 3.8103 -4.5106 15 5 14 -1.8023 -3.3547 15 6 0 -8.1822 0.0000 15 6 11 -0.7511 1.1561 15 6 12 2.8292 1.4966 16 0 0 -11.6434 0.0000 16 0 1 0.0000 0.8212 16 0 2 -2.8415 0.0000 16 0 3 0.0000 1.5557 16 0 4 -2.7344 0.0000 16 0 5 -0.0000 -2.1045 16 0 6 2.1292 0.0000 16 0 7 -0.0000 -3.2777 16 0 8 -1.9454 0.0000 16 0 9 0.0000 3.4806 16 0 10 -2.1294 0.0000 16 0 11 -0.0000 -4.7956 16 0 12 -0.0704 0.0000 16 0 13 -0.0000 -3.3571 16 1 0 10.2759 -0.0000 16 1 1 -1.0193 3.8949 16 1 4 -1.3373 1.7354 16 1 5 -2.5431 -0.2673 16 1 8 4.9844 5.1240 16 1 9 -1.6364 -2.2684 16 1 10 0.4016 2.2032 16 1 11 2.4303 -2.4907 16 1 12 0.3740 3.6894 16 1 13 0.9040 -3.8318 16 2 0 -6.9479 0.0000 16 2 1 6.9208 8.2440 16 2 2 -3.6220 -5.3222 16 2 3 3.7705 4.3641 16 2 4 -9.2632 -9.6370 16 2 8 -3.0634 2.9475 16 2 9 -10.4035 2.0965 16 2 10 -2.0323 -6.4388 16 2 11 -3.7911 -1.9523 16 2 12 1.5720 -5.5606 16 3 0 3.8693 -0.0000 16 3 1 -0.7267 -2.7335 16 3 2 -3.5113 6.3566 16 3 3 -6.0930 0.1060 16 3 9 -0.8620 1.0971 16 3 10 -4.2294 3.4704 16 3 11 -1.7568 -0.5376 16 4 0 5.3473 -0.0000 16 4 1 -0.0204 2.5677 16 4 2 -1.3581 -2.4147 16 4 10 4.2421 2.4681 16 5 0 -4.2986 0.0000 16 5 1 -7.1162 0.9737 16 6 0 -4.4985 0.0000 17 0 1 1.8064 0.0000 17 0 2 -0.0000 -5.0538 17 0 3 4.7510 -0.0000 17 0 4 0.0000 1.3520 17 0 5 2.2632 0.0000 17 0 6 -0.0000 -8.1761 17 1 0 -2.9968 0.0000 17 1 1 -3.5892 -2.8479 17 1 2 3.9092 -0.5117 17 1 3 2.4223 0.2291 17 1 4 -3.2587 -2.9901 17 1 5 2.4256 6.0123 17 2 0 -1.0609 0.0000 17 2 1 -0.9122 0.9303 17 2 2 -2.1614 -0.8319 17 2 3 0.8836 -2.5659 17 2 5 4.2167 4.2154 17 3 0 -0.0203 0.0000 17 3 1 2.5257 -3.6113 17 3 2 0.2851 4.6257 17 3 3 3.7460 2.6287 17 3 4 5.2492 1.6165 0 0 0 0.0 0.0 ; _shelx_fab_checksum 13769 _olex2_submission_special_instructions 'No special instructions were received' #END data_MOF520_1.47GPa _chemical_name_common 'MOF-520_1.47 GPa' _chemical_name_systematic ? _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0310 0.0240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 94 _space_group_name_H-M_alt 'P 42 21 2' _space_group_name_Hall 'P 4n 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 19.182(3) _cell_length_b 19.182(3) _cell_length_c 36.534(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13443(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4625 _cell_measurement_theta_max 11.91 _cell_measurement_theta_min 2.21 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.562 _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 0.029 _shelx_estimated_absorpt_T_max 0.7436 _shelx_estimated_absorpt_T_min 0.6380 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 0.7436 _exptl_absorpt_correction_T_min 0.6380 _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1253 before and 0.0622 after correction. The Ratio of minimum to maximum transmission is 0.8580. The \l/2 correction factor is Not present. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Perkin Elmer CMOS' _diffrn_measurement_method '\w 80 degrees scan' _diffrn_detector_area_resol_mean ? _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 1.47 GPa was measured via ruby method. The sample was collected by rotating 80 degrees. The data sets were merged in XPREP to produce the final data set. ; _diffrn_reflns_number 9518 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_unetI/netI 0.0568 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_theta_full 17.311 _diffrn_reflns_theta_max 11.925 _diffrn_reflns_theta_min 0.837 _diffrn_measured_fraction_theta_full 0.332 _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_Laue_measured_fraction_full 0.332 _diffrn_reflns_Laue_measured_fraction_max 0.945 _diffrn_reflns_point_group_measured_fraction_full 0.316 _diffrn_reflns_point_group_measured_fraction_max 0.944 _reflns_number_total 3850 _reflns_number_gt 3381 _diffrn_standards_number 0 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.695 _reflns_Friedel_fraction_full 0.297 _reflns_Friedel_fraction_max 0.942 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_diff_density_max 0.115 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.023 _refine_ls_abs_structure_details ; Flack x determined using 1289 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.1(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 3850 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0361 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1009 _refine_ls_wR_factor_ref 0.1045 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All O(H) groups 2. Rigid body (RIGU) restrains C5, Al1, O1, O10, Al2, C28, O2, O3, O9, H28, Al3, C1, O4, C2, C7, C3, H7, C6, H3, C4, H6, H4, C8, C13, C9, H13, C12, C10, H9, C21, C11, C14, C26, C22, H11, C19, C15, H26, C25, C23, H22, C18, H19, C16, H15, H25, C24, H23, C17, H18, H16, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, H28, Al3, O2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C2, C3, C7, H7, C7, C6, C3, H3, C4, C3, C6, H6, C5, C6, C5, C4, C4, H4, C5, C8, C8, C13, C9, C8, C13, H13, C13, C12, C9, C10, C9, H9, C21, C12, C11, C12, C14, C10, C11, C10, C26, C21, C22, C21, C11, H11, C19, C14, C15, C14, C26, H26, C26, C25, C23, C22, C22, H22, C19, C18, C19, H19, C16, C15, C15, H15, C25, H25, C25, C24, C23, H23, C24, C23, C18, C17, C18, H18, C17, C16, C16, H16, C27, C24, C20, C17, O8, C27, O7, C27, O5, C20, O6, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C26(H26), C23(H23), C25(H25), C22(H22), C7(H7), C16(H16), C18(H18), C6(H6), C13(H13), C19(H19), C15(H15), C9(H9), C28(H28), C3(H3), C4(H4), C11(H11) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.66349(8) 0.33651(8) 0.5000 0.0507(8) Uani 1 2 d S TU P . . Al2 Al 0.61670(9) 0.38957(9) 0.41625(5) 0.0536(6) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38334(7) 0.0516(8) Uani 1 2 d S TU P . . O2 O 0.56495(16) 0.47062(16) 0.41844(11) 0.0515(11) Uani 1 1 d . U . . . H2 H 0.5717 0.4993 0.4387 0.062 Uiso 1 1 calc R . . . . O3 O 0.6395(2) 0.4010(2) 0.36565(13) 0.0620(13) Uani 1 1 d . U . . . O1 O 0.60065(17) 0.36668(17) 0.46646(10) 0.0555(12) Uani 1 1 d . U . . . H1 H 0.5550 0.3716 0.4747 0.067 Uiso 1 1 calc R . . . . O4 O 0.5590(2) 0.47333(19) 0.34441(11) 0.0608(13) Uani 1 1 d . U . . . C1 C 0.6117(4) 0.4354(3) 0.3402(2) 0.0550(19) Uani 1 1 d . U . . . C26 C 0.7689(4) 0.6312(4) 0.1400(2) 0.091(2) Uani 1 1 d . U . . . H26 H 0.7643 0.6290 0.1653 0.109 Uiso 1 1 calc R U . . . C23 C 0.7793(4) 0.6300(4) 0.0677(2) 0.094(2) Uani 1 1 d . U . . . H23 H 0.7790 0.6305 0.0423 0.113 Uiso 1 1 calc R U . . . C20 C 0.9755(4) 0.1505(4) 0.11125(18) 0.060(2) Uani 1 1 d . U . . . C25 C 0.7798(4) 0.6924(4) 0.1252(2) 0.092(2) Uani 1 1 d . U . . . H25 H 0.7823 0.7331 0.1389 0.110 Uiso 1 1 calc R U . . . C22 C 0.7712(4) 0.5676(4) 0.0850(2) 0.088(3) Uani 1 1 d . U . . . H22 H 0.7717 0.5268 0.0713 0.105 Uiso 1 1 calc R U . . . C24 C 0.7876(3) 0.6917(4) 0.0857(2) 0.077(2) Uani 1 1 d . U . . . C27 C 0.8039(3) 0.7570(4) 0.0627(2) 0.057(2) Uani 1 1 d . U . . . C17 C 0.9330(4) 0.2084(3) 0.12017(18) 0.066(2) Uani 1 1 d . U . . . C7 C 0.6120(4) 0.4752(4) 0.2758(2) 0.110(3) Uani 1 1 d . U . . . H7 H 0.5706 0.4999 0.2786 0.132 Uiso 1 1 calc R U . . . C21 C 0.7633(3) 0.5638(3) 0.1185(2) 0.062(2) Uani 1 1 d . U . . . C16 C 0.8693(4) 0.1966(3) 0.1387(2) 0.090(3) Uani 1 1 d . U . . . H16 H 0.8541 0.1520 0.1448 0.108 Uiso 1 1 calc R U . . . C2 C 0.6439(4) 0.4353(3) 0.3069(2) 0.068(2) Uani 1 1 d . U . . . C18 C 0.9578(4) 0.2762(3) 0.1085(2) 0.107(3) Uani 1 1 d . U . . . H18 H 0.9996 0.2839 0.0962 0.128 Uiso 1 1 calc R U . . . C14 C 0.8429(4) 0.3215(4) 0.13833(19) 0.070(2) Uani 1 1 d . U . . . C6 C 0.6454(4) 0.4737(4) 0.2442(2) 0.109(3) Uani 1 1 d . U . . . H6 H 0.6285 0.5063 0.2275 0.130 Uiso 1 1 calc R U . . . C13 C 0.7303(4) 0.4934(4) 0.1741(2) 0.103(3) Uani 1 1 d . U . . . H13 H 0.7076 0.5332 0.1824 0.123 Uiso 1 1 calc R U . . . C19 C 0.9068(4) 0.3325(4) 0.1189(2) 0.088(2) Uani 1 1 d . U . . . H19 H 0.9176 0.3780 0.1121 0.105 Uiso 1 1 calc R U . . . C10 C 0.8031(4) 0.3816(4) 0.1482(2) 0.088(2) Uani 1 1 d . U . . . C15 C 0.8321(4) 0.2540(4) 0.14696(19) 0.081(2) Uani 1 1 d . U . . . H15 H 0.7924 0.2458 0.1609 0.097 Uiso 1 1 calc R U . . . C12 C 0.7627(4) 0.4950(4) 0.1370(2) 0.088(2) Uani 1 1 d . U . . . C9 C 0.7681(4) 0.3786(3) 0.1826(2) 0.090(2) Uani 1 1 d . U . . . H9 H 0.7691 0.3376 0.1962 0.108 Uiso 1 1 calc R U . . . O8 O 0.82701(19) 0.8037(2) 0.08835(12) 0.0687(13) Uani 1 1 d . U . . . O10 O 0.73317(18) 0.3990(2) 0.48188(12) 0.0625(13) Uani 1 1 d . U . . . O5 O 1.0379(2) 0.16650(18) 0.09799(11) 0.0577(13) Uani 1 1 d . U . . . O6 O 0.95740(18) 0.0894(2) 0.11988(11) 0.0554(12) Uani 1 1 d . U . . . O7 O 0.8013(2) 0.7646(2) 0.03226(16) 0.0735(17) Uani 1 1 d . U . . . O9 O 0.6971(2) 0.4398(2) 0.42654(14) 0.0720(14) Uani 1 1 d . U . . . C28 C 0.7395(4) 0.4454(4) 0.4531(2) 0.080(2) Uani 1 1 d . U . . . H28 H 0.7738 0.4797 0.4532 0.095 Uiso 1 1 calc R U . . . C5 C 0.6987(4) 0.4353(4) 0.2307(2) 0.088(2) Uani 1 1 d . U . . . C8 C 0.7322(4) 0.4372(4) 0.1964(3) 0.094(3) Uani 1 1 d . U . . . C3 C 0.7000(4) 0.3965(4) 0.2976(2) 0.111(3) Uani 1 1 d . U . . . H3 H 0.7192 0.3681 0.3156 0.133 Uiso 1 1 calc R U . . . C4 C 0.7315(4) 0.3955(4) 0.2633(2) 0.100(3) Uani 1 1 d . U . . . H4 H 0.7726 0.3706 0.2599 0.121 Uiso 1 1 calc R U . . . C11 C 0.7987(3) 0.4415(3) 0.1263(2) 0.081(2) Uani 1 1 d . U . . . H11 H 0.8218 0.4428 0.1040 0.097 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 0.0519(11) 0.0519(11) 0.048(2) -0.0022(11) -0.0022(11) 0.0072(13) Al2 0.0656(14) 0.0455(13) 0.0497(17) -0.0054(10) -0.0061(10) 0.0174(10) Al3 0.0626(19) 0.0497(19) 0.042(2) 0.000 0.000 0.0120(13) O2 0.048(2) 0.059(3) 0.048(3) -0.0053(19) -0.0016(18) 0.0069(19) O3 0.079(3) 0.056(3) 0.051(4) 0.000(2) 0.019(2) 0.020(2) O1 0.051(2) 0.066(3) 0.049(3) 0.017(2) -0.0053(19) 0.018(2) O4 0.083(3) 0.058(3) 0.041(3) -0.001(2) 0.006(2) 0.019(3) C1 0.081(5) 0.044(4) 0.039(5) -0.001(4) 0.019(4) 0.020(4) C26 0.156(7) 0.073(5) 0.044(6) 0.023(4) 0.031(4) -0.001(4) C23 0.124(7) 0.091(5) 0.067(6) 0.001(4) 0.017(4) -0.031(5) C20 0.084(5) 0.044(5) 0.053(6) -0.001(4) 0.028(4) 0.017(4) C25 0.158(7) 0.072(5) 0.046(6) 0.019(4) 0.004(5) -0.023(5) C22 0.140(7) 0.068(5) 0.055(6) 0.016(4) 0.057(5) -0.019(4) C24 0.103(5) 0.072(5) 0.057(6) 0.021(4) 0.024(4) -0.026(4) C27 0.075(5) 0.052(5) 0.045(6) 0.007(4) -0.008(4) -0.013(3) C17 0.095(5) 0.052(5) 0.052(6) -0.009(3) 0.032(4) 0.022(4) C7 0.134(7) 0.119(7) 0.076(7) 0.048(5) 0.032(5) 0.071(5) C21 0.073(4) 0.049(4) 0.062(6) 0.011(4) 0.049(4) 0.000(3) C16 0.109(5) 0.039(4) 0.121(7) -0.018(4) 0.066(5) 0.005(4) C2 0.087(5) 0.054(4) 0.063(6) 0.008(4) 0.028(4) 0.039(4) C18 0.127(6) 0.046(5) 0.147(8) 0.008(4) 0.041(5) 0.012(4) C14 0.087(5) 0.059(5) 0.064(6) -0.006(4) 0.009(4) -0.001(4) C6 0.155(7) 0.102(6) 0.069(7) 0.050(5) 0.033(5) 0.093(6) C13 0.157(7) 0.042(4) 0.109(7) 0.010(4) 0.070(5) 0.016(5) C19 0.108(5) 0.077(5) 0.078(6) -0.007(4) 0.015(4) -0.001(4) C10 0.107(6) 0.067(5) 0.089(7) 0.000(4) 0.036(4) 0.007(4) C15 0.108(6) 0.055(5) 0.079(6) -0.011(4) 0.043(4) 0.006(4) C12 0.098(6) 0.060(5) 0.107(7) 0.006(4) 0.038(4) 0.006(4) C9 0.123(6) 0.044(4) 0.103(7) 0.020(4) 0.045(5) 0.015(4) O8 0.071(3) 0.070(3) 0.064(4) 0.026(2) 0.013(2) -0.017(2) O10 0.048(3) 0.062(3) 0.078(4) -0.020(2) 0.000(2) 0.002(2) O5 0.085(3) 0.042(3) 0.046(3) -0.015(2) 0.023(2) 0.010(2) O6 0.073(3) 0.046(3) 0.047(3) -0.002(2) 0.018(2) 0.010(2) O7 0.103(4) 0.070(3) 0.048(4) 0.025(3) -0.013(3) -0.014(2) O9 0.060(3) 0.074(3) 0.082(4) 0.000(3) 0.012(3) -0.010(2) C28 0.069(5) 0.097(6) 0.072(7) 0.000(5) 0.010(4) -0.005(4) C5 0.103(6) 0.071(5) 0.090(6) 0.028(4) 0.025(5) 0.034(4) C8 0.131(6) 0.041(5) 0.111(7) 0.010(4) 0.049(5) 0.034(4) C3 0.135(7) 0.110(6) 0.087(7) 0.037(5) 0.045(5) 0.077(5) C4 0.102(6) 0.114(6) 0.086(7) 0.016(5) 0.033(5) 0.056(5) C11 0.103(5) 0.045(4) 0.094(6) 0.015(4) 0.061(4) 0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.814(4) . ? Al1 O1 1.814(4) 8_666 ? Al1 O10 1.913(4) . ? Al1 O10 1.913(4) 8_666 ? Al1 O7 1.936(5) 2_645 ? Al1 O7 1.936(5) 6_645 ? Al2 O2 1.846(4) . ? Al2 O3 1.913(5) . ? Al2 O1 1.911(4) . ? Al2 O8 1.976(4) 6_645 ? Al2 O5 1.926(4) 5_455 ? Al2 O9 1.857(5) . ? Al3 O2 1.875(4) . ? Al3 O2 1.875(4) 3_665 ? Al3 O4 1.889(5) 3_665 ? Al3 O4 1.888(5) . ? Al3 O6 1.904(4) 5_455 ? Al3 O6 1.904(4) 6_655 ? O3 C1 1.259(8) . ? O4 C1 1.255(7) . ? C1 C2 1.365(9) . ? C26 C25 1.308(8) . ? C26 C21 1.516(9) . ? C23 C22 1.362(9) . ? C23 C24 1.364(9) . ? C20 C17 1.417(8) . ? C20 O5 1.327(7) . ? C20 O6 1.262(7) . ? C25 C24 1.451(9) . ? C22 C21 1.235(8) . ? C24 C27 1.540(10) . ? C27 O8 1.371(8) . ? C27 O7 1.122(7) . ? C17 C16 1.415(8) . ? C17 C18 1.450(8) . ? C7 C2 1.500(9) . ? C7 C6 1.319(9) . ? C21 C12 1.484(9) . ? C16 C15 1.347(8) . ? C2 C3 1.353(8) . ? C18 C19 1.506(9) . ? C14 C19 1.432(9) . ? C14 C10 1.429(9) . ? C14 C15 1.348(8) . ? C6 C5 1.354(9) . ? C13 C12 1.492(9) . ? C13 C8 1.350(9) . ? C10 C9 1.426(9) . ? C10 C11 1.402(9) . ? C12 C11 1.296(8) . ? C9 C8 1.411(8) . ? O8 Al2 1.976(4) 6_655 ? O10 C28 1.384(8) . ? O5 Al2 1.926(4) 5 ? O6 Al3 1.904(4) 5 ? O7 Al1 1.936(5) 4_564 ? O9 C28 1.271(8) . ? C5 C8 1.409(9) . ? C5 C4 1.548(10) . ? C3 C4 1.391(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 91.9(3) . 8_666 ? O1 Al1 O10 91.76(17) 8_666 8_666 ? O1 Al1 O10 92.33(16) 8_666 . ? O1 Al1 O10 92.33(16) . 8_666 ? O1 Al1 O10 91.76(17) . . ? O1 Al1 O7 92.73(18) 8_666 2_645 ? O1 Al1 O7 175.0(2) 8_666 6_645 ? O1 Al1 O7 92.73(19) . 6_645 ? O1 Al1 O7 175.0(2) . 2_645 ? O10 Al1 O10 174.1(3) 8_666 . ? O10 Al1 O7 86.02(19) . 2_645 ? O10 Al1 O7 89.57(18) 8_666 2_645 ? O10 Al1 O7 86.02(19) 8_666 6_645 ? O10 Al1 O7 89.57(18) . 6_645 ? O7 Al1 O7 82.8(3) 2_645 6_645 ? O2 Al2 O3 93.89(18) . . ? O2 Al2 O1 93.75(17) . . ? O2 Al2 O8 177.5(2) . 6_645 ? O2 Al2 O5 93.44(17) . 5_455 ? O2 Al2 O9 90.03(17) . . ? O3 Al2 O8 83.61(18) . 6_645 ? O3 Al2 O5 89.00(18) . 5_455 ? O1 Al2 O3 172.35(17) . . ? O1 Al2 O8 88.75(18) . 6_645 ? O1 Al2 O5 90.27(18) . 5_455 ? O5 Al2 O8 86.58(17) 5_455 6_645 ? O9 Al2 O3 86.9(2) . . ? O9 Al2 O1 93.4(2) . . ? O9 Al2 O8 89.78(18) . 6_645 ? O9 Al2 O5 174.8(2) . 5_455 ? O2 Al3 O2 93.7(3) . 3_665 ? O2 Al3 O4 92.03(16) 3_665 3_665 ? O2 Al3 O4 174.3(2) 3_665 . ? O2 Al3 O4 92.03(16) . . ? O2 Al3 O4 174.3(2) . 3_665 ? O2 Al3 O6 93.24(16) . 5_455 ? O2 Al3 O6 93.24(16) 3_665 6_655 ? O2 Al3 O6 91.60(16) 3_665 5_455 ? O2 Al3 O6 91.60(16) . 6_655 ? O4 Al3 O4 82.3(3) . 3_665 ? O4 Al3 O6 88.09(17) 3_665 6_655 ? O4 Al3 O6 86.57(17) 3_665 5_455 ? O4 Al3 O6 88.09(17) . 5_455 ? O4 Al3 O6 86.57(17) . 6_655 ? O6 Al3 O6 172.9(3) 5_455 6_655 ? Al2 O2 Al3 125.5(2) . . ? C1 O3 Al2 132.7(5) . . ? Al1 O1 Al2 127.9(2) . . ? C1 O4 Al3 137.1(4) . . ? O3 C1 C2 117.9(7) . . ? O4 C1 O3 123.6(7) . . ? O4 C1 C2 118.3(7) . . ? C25 C26 C21 124.2(7) . . ? C22 C23 C24 123.6(8) . . ? O5 C20 C17 115.0(6) . . ? O6 C20 C17 120.8(7) . . ? O6 C20 O5 123.6(6) . . ? C26 C25 C24 114.8(7) . . ? C21 C22 C23 121.7(8) . . ? C23 C24 C25 118.3(6) . . ? C23 C24 C27 117.8(8) . . ? C25 C24 C27 123.9(7) . . ? O8 C27 C24 102.9(7) . . ? O7 C27 C24 129.6(8) . . ? O7 C27 O8 127.4(7) . . ? C20 C17 C18 116.5(6) . . ? C16 C17 C20 118.8(6) . . ? C16 C17 C18 124.7(6) . . ? C6 C7 C2 117.0(7) . . ? C22 C21 C26 117.0(7) . . ? C22 C21 C12 120.2(7) . . ? C12 C21 C26 121.6(7) . . ? C15 C16 C17 115.6(6) . . ? C1 C2 C7 119.4(7) . . ? C3 C2 C1 125.8(7) . . ? C3 C2 C7 114.5(7) . . ? C17 C18 C19 110.8(6) . . ? C10 C14 C19 117.7(7) . . ? C15 C14 C19 112.8(7) . . ? C15 C14 C10 129.3(7) . . ? C7 C6 C5 134.2(7) . . ? C8 C13 C12 123.5(7) . . ? C14 C19 C18 125.2(7) . . ? C9 C10 C14 116.2(7) . . ? C11 C10 C14 123.3(7) . . ? C11 C10 C9 120.5(7) . . ? C16 C15 C14 130.7(7) . . ? C21 C12 C13 115.8(6) . . ? C11 C12 C21 124.3(7) . . ? C11 C12 C13 118.6(7) . . ? C8 C9 C10 120.8(7) . . ? C27 O8 Al2 131.5(5) . 6_655 ? C28 O10 Al1 136.7(5) . . ? C20 O5 Al2 132.6(4) . 5 ? C20 O6 Al3 134.7(4) . 5 ? C27 O7 Al1 132.8(5) . 4_564 ? C28 O9 Al2 136.9(6) . . ? O9 C28 O10 118.0(7) . . ? C6 C5 C8 130.9(7) . . ? C6 C5 C4 107.1(7) . . ? C8 C5 C4 120.8(7) . . ? C13 C8 C9 115.8(8) . . ? C13 C8 C5 122.9(7) . . ? C5 C8 C9 121.2(7) . . ? C2 C3 C4 125.4(7) . . ? C3 C4 C5 120.7(7) . . ? C12 C11 C10 120.6(7) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.437 -0.834 -0.615 9495.8 13890.3 ? _shelx_res_file ; TITL P4_25kev_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.182 19.182 36.534 90 90 90 ZERR 222 0.00271 0.00271 0.00731 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.031 0.024 81.761 DISP C 0.001 0.001 6.243 DISP H -0 0 0.608 DISP O 0.004 0.003 13.948 UNIT 222 222 222 222 RIGU C5 Al1 O1 O10 Al2 C28 O2 O3 O9 H28 Al3 C1 O4 C2 C7 C3 H7 C6 H3 C4 H6 H4 = C8 C13 C9 H13 C12 C10 H9 C21 C11 C14 C26 C22 H11 C19 C15 H26 C25 C23 H22 C18 = H19 C16 H15 H25 C24 H23 C17 H18 H16 C27 C20 O8 O7 O5 O6 AL1 O1 AL1 O10 AL2 = O1 O10 C28 AL2 O2 AL2 O3 AL2 O9 O9 C28 C28 H28 AL3 O2 O3 C1 AL3 O4 O4 C1 C2 = C1 C7 C2 C2 C3 C7 H7 C7 C6 C3 H3 C4 C3 C6 H6 C5 C6 C5 C4 C4 H4 C5 C8 C8 C13 = C9 C8 C13 H13 C13 C12 C9 C10 C9 H9 C21 C12 C11 C12 C14 C10 C11 C10 C26 C21 = C22 C21 C11 H11 C19 C14 C15 C14 C26 H26 C26 C25 C23 C22 C22 H22 C19 C18 C19 = H19 C16 C15 C15 H15 C25 H25 C25 C24 C23 H23 C24 C23 C18 C17 C18 H18 C17 C16 = C16 H16 C27 C24 C20 C17 O8 C27 O7 C27 O5 C20 O6 C20 L.S. 14 PLAN 20 TEMP 23 BOND ABIN ACTA fmap 2 REM REM REM WGHT 0.063000 FVAR 0.11387 AL1 4 0.663494 0.336506 0.500000 10.50000 0.05187 0.05187 = 0.04832 -0.00215 -0.00215 0.00723 AL2 4 0.616702 0.389572 0.416255 11.00000 0.06557 0.04549 = 0.04971 -0.00538 -0.00607 0.01741 AL3 4 0.500000 0.500000 0.383338 10.50000 0.06258 0.04972 = 0.04243 0.00000 0.00000 0.01204 O2 3 0.564946 0.470615 0.418441 11.00000 0.04811 0.05900 = 0.04750 -0.00529 -0.00161 0.00689 AFIX 43 H2 2 0.571662 0.499283 0.438664 11.00000 -1.20000 AFIX 0 O3 3 0.639516 0.401049 0.365653 11.00000 0.07891 0.05648 = 0.05065 0.00043 0.01929 0.01978 O1 3 0.600654 0.366676 0.466456 11.00000 0.05102 0.06601 = 0.04939 0.01667 -0.00530 0.01757 AFIX 43 H1 2 0.555047 0.371604 0.474696 11.00000 -1.20000 AFIX 0 O4 3 0.559020 0.473333 0.344410 11.00000 0.08321 0.05802 = 0.04112 -0.00114 0.00634 0.01885 C1 1 0.611701 0.435383 0.340172 11.00000 0.08142 0.04431 = 0.03916 -0.00142 0.01865 0.02016 C26 1 0.768878 0.631226 0.139997 11.00000 0.15553 0.07262 = 0.04443 0.02273 0.03068 -0.00055 AFIX 43 H26 2 0.764251 0.628952 0.165308 11.00000 -1.20000 AFIX 0 C23 1 0.779254 0.629961 0.067722 11.00000 0.12437 0.09110 = 0.06726 0.00096 0.01685 -0.03139 AFIX 43 H23 2 0.779037 0.630464 0.042268 11.00000 -1.20000 AFIX 0 C20 1 0.975513 0.150520 0.111251 11.00000 0.08430 0.04384 = 0.05330 -0.00058 0.02814 0.01662 C25 1 0.779763 0.692356 0.125204 11.00000 0.15798 0.07204 = 0.04574 0.01890 0.00388 -0.02259 AFIX 43 H25 2 0.782297 0.733087 0.138948 11.00000 -1.20000 AFIX 0 C22 1 0.771240 0.567587 0.085026 11.00000 0.13991 0.06781 = 0.05502 0.01551 0.05729 -0.01944 AFIX 43 H22 2 0.771742 0.526789 0.071275 11.00000 -1.20000 AFIX 0 C24 1 0.787583 0.691739 0.085693 11.00000 0.10306 0.07194 = 0.05694 0.02111 0.02400 -0.02647 C27 1 0.803934 0.756993 0.062676 11.00000 0.07504 0.05213 = 0.04525 0.00710 -0.00806 -0.01275 C17 1 0.932951 0.208441 0.120168 11.00000 0.09495 0.05183 = 0.05193 -0.00895 0.03245 0.02220 C7 1 0.611994 0.475224 0.275759 11.00000 0.13411 0.11897 = 0.07589 0.04796 0.03173 0.07146 AFIX 43 H7 2 0.570614 0.499899 0.278606 11.00000 -1.20000 AFIX 0 C21 1 0.763323 0.563832 0.118507 11.00000 0.07302 0.04946 = 0.06241 0.01060 0.04882 -0.00029 C16 1 0.869294 0.196578 0.138709 11.00000 0.10855 0.03940 = 0.12082 -0.01812 0.06615 0.00495 AFIX 43 H16 2 0.854110 0.152020 0.144801 11.00000 -1.20000 AFIX 0 C2 1 0.643854 0.435294 0.306855 11.00000 0.08656 0.05445 = 0.06332 0.00808 0.02762 0.03874 C18 1 0.957838 0.276242 0.108485 11.00000 0.12709 0.04595 = 0.14706 0.00780 0.04051 0.01216 AFIX 43 H18 2 0.999646 0.283949 0.096248 11.00000 -1.20000 AFIX 0 C14 1 0.842896 0.321519 0.138329 11.00000 0.08720 0.05885 = 0.06370 -0.00641 0.00921 -0.00116 C6 1 0.645363 0.473734 0.244187 11.00000 0.15469 0.10241 = 0.06880 0.04986 0.03329 0.09313 AFIX 43 H6 2 0.628504 0.506277 0.227523 11.00000 -1.20000 AFIX 0 C13 1 0.730345 0.493367 0.174115 11.00000 0.15705 0.04220 = 0.10893 0.01028 0.07015 0.01636 AFIX 43 H13 2 0.707631 0.533209 0.182370 11.00000 -1.20000 AFIX 0 C19 1 0.906775 0.332486 0.118863 11.00000 0.10758 0.07696 = 0.07824 -0.00736 0.01500 -0.00100 AFIX 43 H19 2 0.917571 0.377960 0.112096 11.00000 -1.20000 AFIX 0 C10 1 0.803054 0.381566 0.148207 11.00000 0.10728 0.06671 = 0.08927 0.00011 0.03574 0.00700 C15 1 0.832128 0.254028 0.146959 11.00000 0.10800 0.05458 = 0.07914 -0.01112 0.04323 0.00608 AFIX 43 H15 2 0.792445 0.245783 0.160929 11.00000 -1.20000 AFIX 0 C12 1 0.762728 0.494951 0.136984 11.00000 0.09796 0.05959 = 0.10709 0.00602 0.03847 0.00630 C9 1 0.768147 0.378624 0.182627 11.00000 0.12271 0.04357 = 0.10338 0.01966 0.04473 0.01498 AFIX 43 H9 2 0.769058 0.337595 0.196181 11.00000 -1.20000 AFIX 0 O8 3 0.827009 0.803736 0.088348 11.00000 0.07149 0.07045 = 0.06412 0.02617 0.01295 -0.01740 O10 3 0.733168 0.398954 0.481881 11.00000 0.04823 0.06156 = 0.07765 -0.02050 0.00018 0.00226 O5 3 1.037929 0.166501 0.097995 11.00000 0.08508 0.04225 = 0.04590 -0.01497 0.02316 0.00980 O6 3 0.957400 0.089434 0.119882 11.00000 0.07317 0.04568 = 0.04730 -0.00227 0.01801 0.00966 O7 3 0.801348 0.764550 0.032263 11.00000 0.10289 0.06958 = 0.04790 0.02507 -0.01261 -0.01351 O9 3 0.697090 0.439838 0.426543 11.00000 0.06038 0.07383 = 0.08187 0.00017 0.01199 -0.00968 C28 1 0.739546 0.445434 0.453097 11.00000 0.06950 0.09704 = 0.07218 -0.00016 0.01015 -0.00546 AFIX 43 H28 2 0.773839 0.479706 0.453182 11.00000 -1.20000 AFIX 0 C5 1 0.698712 0.435335 0.230663 11.00000 0.10253 0.07089 = 0.08965 0.02797 0.02538 0.03423 C8 1 0.732247 0.437232 0.196358 11.00000 0.13071 0.04094 = 0.11137 0.00973 0.04901 0.03442 C3 1 0.700048 0.396471 0.297560 11.00000 0.13525 0.10962 = 0.08727 0.03744 0.04527 0.07674 AFIX 43 H3 2 0.719231 0.368136 0.315594 11.00000 -1.20000 AFIX 0 C4 1 0.731460 0.395468 0.263256 11.00000 0.10180 0.11395 = 0.08564 0.01581 0.03330 0.05617 AFIX 43 H4 2 0.772567 0.370591 0.259857 11.00000 -1.20000 AFIX 0 C11 1 0.798698 0.441473 0.126318 11.00000 0.10345 0.04482 = 0.09422 0.01483 0.06057 0.03542 AFIX 43 H11 2 0.821819 0.442840 0.103955 11.00000 -1.20000 AFIX 0 HKLF 4 REM P4_25kev_0m in P42212 #94 REM R1 = 0.0361 for 3381 Fo > 4sig(Fo) and 0.0422 for all 3850 data REM 362 parameters refined using 336 restraints END WGHT 0.0628 0.0000 REM Highest difference peak 0.115, deepest hole -0.185, 1-sigma level 0.023 Q1 1 0.7810 0.4900 0.0687 11.00000 0.05 0.11 Q2 1 0.8008 0.4837 0.4426 11.00000 0.05 0.10 Q3 1 0.7859 0.5158 0.4562 11.00000 0.05 0.10 Q4 1 1.0557 0.2651 0.0810 11.00000 0.05 0.10 Q5 1 0.7180 0.4923 0.4082 11.00000 0.05 0.09 Q6 1 0.9758 0.2680 0.0706 11.00000 0.05 0.09 Q7 1 1.0205 0.2903 0.1277 11.00000 0.05 0.09 Q8 1 1.0445 0.2922 0.0886 11.00000 0.05 0.09 Q9 1 1.0418 0.2827 0.1219 11.00000 0.05 0.09 Q10 1 0.7846 0.2612 0.1413 11.00000 0.05 0.09 Q11 1 0.8349 0.5381 0.1126 11.00000 0.05 0.09 Q12 1 0.9025 0.0789 0.1522 11.00000 0.05 0.09 Q13 1 0.8215 0.5130 0.1098 11.00000 0.05 0.09 Q14 1 0.4990 0.4667 0.3068 11.00000 0.05 0.08 Q15 1 0.8189 0.5806 0.1303 11.00000 0.05 0.08 Q16 1 0.7378 0.7295 0.0520 11.00000 0.05 0.08 Q17 1 0.9590 0.3524 0.0858 11.00000 0.05 0.08 Q18 1 0.8579 0.1081 0.1536 11.00000 0.05 0.08 Q19 1 0.6589 0.5367 0.2314 11.00000 0.05 0.08 Q20 1 0.7240 0.5814 0.0392 11.00000 0.05 0.07 ; _shelx_res_checksum 16205 _shelx_hkl_file ; 1 1 0 360.95 18.33 -1 -1 0 339.13 18.33 1 2 0 354.66 19.02 -1 -2 0 371.30 19.02 -2 -2 0 4.10 0.29 2 2 0 3.90 0.29 0 -3 0 0.01 0.08 -1 -3 0 18.61 1.05 1 3 0 19.15 1.07 -2 -3 0 243.22 14.02 3 2 0 266.02 14.05 2 3 0 291.63 14.05 3 3 0 3.47 0.33 0 -4 0 76.60 4.08 1 4 0 8.10 0.56 -1 -4 0 9.30 0.55 -2 -4 0 162.04 8.44 2 4 0 157.39 8.46 3 4 0 31.76 1.82 -3 -4 0 33.85 1.80 4 3 0 30.71 1.82 4 4 0 103.99 5.59 0 -5 0 0.02 0.14 -1 -5 0 45.30 2.39 1 5 0 42.12 2.40 -2 -5 0 8.96 0.57 2 5 0 7.80 0.59 5 3 0 331.59 18.21 3 5 0 361.21 18.21 -3 -5 0 343.35 18.17 4 5 0 0.61 0.26 5 4 0 0.42 0.22 5 5 0 137.99 7.41 0 -6 0 360.15 18.93 -1 -6 0 26.52 1.47 1 6 0 24.92 1.49 2 6 0 20.41 1.26 -2 -6 0 21.39 1.22 -3 -6 0 12.35 0.77 3 6 0 10.84 0.81 4 6 0 40.16 2.37 -4 -6 0 42.90 2.32 6 4 0 41.00 2.39 6 5 0 29.90 1.84 5 6 0 31.06 1.84 6 6 0 8.20 0.74 0 -7 0 -0.03 0.21 1 7 0 65.78 3.73 -1 -7 0 71.23 3.71 2 7 0 30.78 1.74 -2 -7 0 28.42 1.68 -3 -7 0 30.74 1.67 3 7 0 26.96 1.72 -4 -7 0 11.94 0.89 4 7 0 16.31 1.03 7 5 0 9.83 0.80 5 7 0 9.51 0.83 6 7 0 328.78 17.53 7 6 0 331.57 17.53 7 7 0 48.96 2.87 0 -8 0 14.09 0.90 1 -8 0 100.20 5.14 -1 -8 0 96.24 5.15 1 8 0 91.05 5.16 2 8 0 114.05 6.12 -2 -8 0 111.75 6.04 -3 -8 0 19.41 1.11 3 8 0 16.40 1.20 4 8 0 33.01 1.88 -4 -8 0 27.89 1.74 5 8 0 5.07 0.69 6 8 0 10.50 0.99 8 6 0 10.44 0.94 8 7 0 53.65 3.15 7 8 0 53.43 3.17 8 8 0 10.90 1.06 0 -9 0 -0.23 0.23 1 -9 0 31.07 1.71 1 9 0 28.75 1.74 -1 -9 0 28.55 1.71 -2 -9 0 -0.08 0.20 2 9 0 0.25 0.39 3 9 0 -0.07 0.29 -3 -9 0 1.23 0.26 4 9 0 55.87 3.40 -4 -9 0 63.57 3.31 5 9 0 107.12 5.73 -5 -9 0 99.50 5.58 6 9 0 7.70 0.90 9 7 0 0.37 0.47 7 9 0 -0.05 0.46 8 9 0 -0.11 0.41 9 8 0 0.51 0.42 9 9 0 86.72 5.01 0 -10 0 5.49 0.58 1 -10 0 12.79 0.90 -1 -10 0 13.36 0.91 -2 -10 0 1.41 0.29 2 10 0 1.35 0.36 -3 -10 0 96.52 5.08 3 10 0 91.25 5.19 -4 -10 0 0.56 0.29 4 10 0 0.45 0.42 5 10 0 11.51 1.16 -5 -10 0 17.63 1.05 6 10 0 6.52 0.88 7 10 0 37.87 2.45 8 10 0 91.58 5.30 10 8 0 93.68 5.30 10 9 0 3.38 0.76 9 10 0 3.79 0.87 10 10 0 4.82 0.93 0 -11 0 0.03 0.28 -1 -11 0 0.77 0.27 1 -11 0 0.80 0.40 -2 -11 0 18.82 1.16 2 11 0 17.62 1.29 3 11 0 1.53 0.48 -3 -11 0 1.43 0.31 -4 -11 0 37.55 2.07 4 11 0 33.03 2.25 -5 -11 0 51.33 2.85 5 11 0 48.72 3.01 6 11 0 27.92 1.94 7 11 0 27.25 1.95 8 11 0 20.62 1.71 9 11 0 0.74 0.77 10 11 0 8.20 1.34 11 10 0 12.12 1.40 11 11 0 11.01 1.44 0 -12 0 5.84 0.61 -1 -12 0 1.70 0.37 1 -12 0 1.92 0.41 2 12 0 0.77 0.43 -2 -12 0 0.62 0.29 2 -12 0 0.38 0.41 3 12 0 5.63 0.83 -3 -12 0 7.93 0.65 -4 -12 0 44.76 2.44 4 12 0 39.81 2.64 -5 -12 0 0.86 0.36 5 12 0 0.82 0.46 6 12 0 90.98 5.19 7 12 0 23.89 1.83 8 12 0 0.93 0.61 9 12 0 10.92 1.45 10 12 0 4.11 1.01 0 -13 0 -0.34 0.32 1 -13 0 3.20 0.52 -1 -13 0 3.21 0.46 2 -13 0 6.54 0.76 -2 -13 0 5.10 0.58 3 13 0 30.28 2.07 -3 -13 0 32.87 1.87 -4 -13 0 12.08 0.87 4 13 0 9.38 1.12 5 13 0 94.39 5.37 6 13 0 -0.47 0.60 7 13 0 1.74 0.64 8 13 0 0.85 0.84 9 13 0 0.44 0.83 0 -14 0 3.28 0.53 1 -14 0 2.17 0.44 -1 -14 0 1.90 0.38 2 -14 0 6.38 0.85 -2 -14 0 5.59 0.58 3 -14 0 -0.93 0.42 -3 -14 0 0.19 0.27 3 14 0 -0.67 0.55 -4 -14 0 75.22 4.06 4 14 0 71.70 4.32 5 14 0 0.23 0.79 6 14 0 -0.16 0.63 7 14 0 -0.43 0.55 0 -15 0 0.20 0.35 1 -15 0 0.06 0.37 -1 -15 0 -0.18 0.31 -2 -15 0 8.64 0.74 2 -15 0 9.61 0.93 3 -15 0 34.12 2.03 -3 -15 0 33.86 1.96 3 15 0 31.42 2.21 4 15 0 0.85 0.66 -4 -15 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12 2 10 0.6919 -2.7122 12 2 11 4.5734 -3.9587 12 2 12 0.0572 -1.3264 12 2 13 0.9376 0.2318 12 2 14 5.8108 0.0013 12 2 15 6.5523 -2.0339 12 2 16 -0.3195 3.2412 12 2 17 1.7963 4.5782 12 2 18 -3.0156 0.5573 12 2 19 5.0719 2.4100 12 3 0 4.0229 -0.0000 12 3 1 7.4308 11.0200 12 3 2 -7.6853 1.4037 12 3 3 -0.8975 7.0174 12 3 4 2.2208 -1.3802 12 3 5 8.6674 -4.5540 12 3 6 -7.0789 0.9357 12 3 8 -5.8234 1.0703 12 3 9 12.7388 -0.2515 12 3 10 -3.1183 0.6559 12 3 11 0.8958 11.9527 12 3 12 5.1138 -7.3584 12 3 13 4.5328 2.2682 12 3 14 -0.7410 -2.3022 12 3 15 -0.0806 4.5120 12 3 16 -0.1537 -0.6612 12 3 17 2.7247 -0.7158 12 3 18 2.3184 0.6273 12 3 19 -1.1098 -0.8705 12 4 0 7.3228 -0.0000 12 4 1 0.7478 1.4144 12 4 2 -1.0331 -3.8144 12 4 3 -2.4758 4.6505 12 4 4 -0.1362 -3.9839 12 4 5 -1.4209 4.6467 12 4 6 3.8511 -4.6593 12 4 7 1.6106 -2.2068 12 4 8 9.9398 -5.4457 12 4 9 3.5897 7.5357 12 4 10 3.9844 1.0337 12 4 11 0.8605 0.4061 12 4 12 4.9546 1.5208 12 4 13 -2.7118 -5.0893 12 4 14 6.5496 4.6080 12 4 15 -2.0009 -4.6596 12 4 16 -0.7412 -0.1050 12 4 17 0.8716 -2.2664 12 4 18 2.4007 4.4418 12 5 0 -2.2317 0.0000 12 5 1 -5.7204 8.6545 12 5 2 -2.4195 7.0290 12 5 3 7.8728 4.2012 12 5 4 -9.1873 6.7882 12 5 5 -1.3258 -3.7708 12 5 6 1.1738 6.3409 12 5 7 5.0127 1.2206 12 5 8 1.5280 -1.1467 12 5 9 4.1736 -5.3025 12 5 10 -4.8662 -2.5271 12 5 11 2.5152 3.6493 12 5 12 4.2181 -9.0347 12 5 13 -0.3397 -5.7938 12 5 14 0.0115 -5.0588 12 5 15 3.1886 1.2983 12 5 16 -0.6697 1.6404 12 5 17 0.7619 1.2017 12 6 0 -0.1766 0.0000 12 6 1 -4.8482 -4.0518 12 6 2 3.9413 5.1726 12 6 3 -3.2233 10.9372 12 6 4 2.7026 -8.8409 12 6 5 -3.5198 -2.2056 12 6 6 6.6645 -7.8707 12 6 7 -1.9308 6.2401 12 6 8 -0.8906 -1.1594 12 6 9 -3.3064 3.2157 12 6 10 -10.5079 -5.1199 12 6 11 4.3128 -1.7464 12 6 12 0.3833 2.5405 12 6 13 0.3489 6.4051 12 6 14 -6.3663 1.4741 12 6 15 -0.4256 -2.0757 12 6 16 -1.4217 4.6801 12 7 0 -0.4505 -0.0000 12 7 1 8.3114 -4.6163 12 7 2 -3.4332 -10.4955 12 7 3 6.5457 3.7002 12 7 4 4.1046 -0.7245 12 7 5 0.8786 7.8186 12 7 6 -4.7186 3.2789 12 7 7 -1.6190 1.0383 12 7 8 -0.9936 2.1420 12 7 9 -7.7953 -0.1154 12 7 10 0.6668 5.3733 12 7 11 -1.5964 -0.1733 12 7 12 -0.4135 -4.3995 12 7 13 -3.4599 3.1436 12 7 14 -1.2173 4.5022 12 7 15 -4.2641 1.5581 12 8 0 3.3286 -0.0000 12 8 1 -8.3037 -1.6610 12 8 2 3.9717 -2.9565 12 8 3 -0.4280 3.5604 12 8 4 2.4892 -1.5842 12 8 5 -0.4629 3.5113 12 8 6 -5.0305 4.6896 12 8 7 -0.7744 -3.4775 12 8 8 -3.7319 0.6739 12 8 9 1.6650 2.6227 12 8 10 -4.6570 3.7464 12 8 11 0.7694 -3.0509 12 8 12 -3.3045 -0.3324 12 8 13 0.0824 3.0911 12 9 0 -6.3713 0.0000 12 9 1 3.3827 -5.0597 12 9 2 -6.9664 -4.6994 12 9 3 5.1050 0.8141 12 9 4 -2.4073 -3.3999 12 9 5 3.3886 -6.8539 12 9 6 -2.5608 0.9452 12 9 7 -0.5021 3.2415 12 9 8 -3.0514 -2.0978 12 9 9 -3.4007 -2.6174 12 9 10 -1.9507 -2.8246 12 10 0 -1.1849 -0.0000 12 10 1 0.0915 -3.8309 12 10 2 -2.1682 2.3851 12 10 3 -3.5115 5.6709 12 10 4 -0.9215 0.8036 12 10 5 -3.2455 0.6271 12 10 6 -0.7396 0.0980 13 0 1 -2.3172 0.0000 13 0 2 0.0000 0.2028 13 0 3 -1.7791 0.0000 13 0 4 -0.0000 -13.1919 13 0 5 -5.7678 0.0000 13 0 6 -0.0000 -11.6009 13 0 7 5.0137 0.0000 13 0 8 -0.0000 -13.4834 13 0 9 6.2935 -0.0000 13 0 10 -0.0000 -7.9873 13 0 11 8.8830 -0.0000 13 0 12 -0.0000 -8.5333 13 0 13 -3.2472 -0.0000 13 0 14 -0.0000 -3.2256 13 0 15 -5.8721 0.0000 13 0 16 -0.0000 -0.8479 13 0 17 9.1650 0.0000 13 1 0 0.5983 0.0000 13 1 1 3.2869 -1.4839 13 1 2 -2.6643 0.1659 13 1 3 0.0297 2.3884 13 1 4 3.6018 -3.0819 13 1 5 3.1544 -11.1592 13 1 6 3.7150 5.0961 13 1 7 10.8358 -12.1148 13 1 8 5.6472 3.6986 13 1 9 2.4974 1.5053 13 1 10 -0.3338 7.3025 13 1 11 -0.2786 2.5845 13 1 12 -1.3350 3.4663 13 1 13 0.4395 -0.0514 13 1 14 -2.7720 6.5388 13 1 15 -5.6368 -1.0118 13 1 16 2.6877 2.4226 13 1 17 0.9161 -1.6190 13 2 0 0.1371 -0.0000 13 2 1 5.5806 11.6868 13 2 2 1.7902 2.9248 13 2 3 8.6879 -5.4797 13 2 9 2.6885 10.9543 13 2 10 4.5304 5.7876 13 2 11 4.4296 -3.9060 13 2 12 1.8775 -0.3939 13 2 13 5.5769 -0.7090 13 2 14 3.3455 2.1977 13 2 15 -2.9751 -2.8114 13 2 16 4.4662 -0.3808 13 2 17 -3.2974 0.5606 13 3 0 10.7638 -0.0000 13 3 1 -9.4275 -2.1880 13 3 2 -0.5154 -1.0858 13 3 3 -2.4312 4.1940 13 3 4 4.0242 -14.1607 13 3 9 -5.6706 -1.7087 13 3 10 7.6928 -4.3293 13 3 11 -4.6538 -1.3965 13 3 12 1.7271 2.2474 13 3 13 -0.2369 3.0924 13 3 14 4.4869 4.1026 13 3 15 1.0343 4.0869 13 3 16 10.0997 -1.2040 13 4 0 0.1590 -0.0000 13 4 1 5.9591 -4.2258 13 4 2 0.6893 7.7890 13 4 3 6.9837 -5.7360 13 4 4 4.5103 0.5744 13 4 5 0.9536 -10.6029 13 4 6 0.9586 -2.5057 13 4 7 2.3311 -3.2436 13 4 8 0.9625 9.4546 13 4 9 1.2710 -8.3771 13 4 10 11.4027 0.1816 13 4 11 4.3597 -7.5434 13 4 12 2.2381 -4.8822 13 4 13 5.6590 -0.8736 13 4 14 -0.3676 3.1963 13 4 15 1.3857 -5.5745 13 5 0 1.8625 0.0000 13 5 1 -0.6324 1.3443 13 5 2 -3.7905 0.9571 13 5 3 4.1064 -4.2892 13 5 4 0.8548 -5.0873 13 5 5 3.3510 3.9911 13 5 6 5.0531 3.7818 13 5 7 4.7317 -1.8228 13 5 8 -2.2647 -2.6492 13 5 9 1.5579 -0.1531 13 5 10 2.0551 1.0563 13 5 11 0.5020 6.0736 13 5 12 0.2533 2.6277 13 5 13 0.6891 3.3060 13 5 14 3.7678 -6.1951 13 6 0 -2.1811 0.0000 13 6 1 2.8788 -3.0936 13 6 2 1.5865 7.3235 13 6 3 -0.2224 3.2982 13 6 4 5.5784 9.5455 13 6 5 0.0859 3.2309 13 6 6 3.2845 -2.2360 13 6 7 -6.8335 -2.1076 13 6 8 8.4332 1.7890 13 6 9 2.3538 -4.1650 13 6 10 3.7217 -3.1939 13 6 11 -2.7864 -1.6339 13 6 12 1.7707 -2.5718 13 6 13 -2.5616 -6.3743 13 7 0 3.6919 -0.0000 13 7 1 8.0982 -3.6053 13 7 2 -1.5903 5.4331 13 7 3 2.4115 -4.0999 13 7 4 -6.8403 -0.4700 13 7 5 2.0485 -6.0474 13 7 6 2.5230 4.8339 13 7 7 4.1152 -0.4869 13 7 8 -0.3918 3.3548 13 7 9 1.1450 0.5994 13 7 10 -1.3066 -0.0781 13 7 11 -6.7583 0.5823 13 8 0 6.3851 -0.0000 13 8 1 2.8095 -1.3414 13 8 2 2.1394 4.0853 13 8 3 5.1732 6.0851 13 8 4 -5.6364 0.1454 13 8 5 -3.8749 1.3520 13 8 6 0.1703 0.3783 13 8 7 1.9371 3.3587 13 8 8 -1.6752 1.1189 13 8 9 -4.5453 4.5182 13 9 0 2.1489 -0.0000 13 9 1 0.9915 0.0537 13 9 2 2.7283 -1.5802 13 9 3 4.4423 -0.3894 13 9 4 1.0058 2.7251 14 0 0 0.7488 -0.0000 14 0 1 -0.0000 -0.9739 14 0 2 3.2213 0.0000 14 0 3 0.0000 3.5508 14 0 4 1.3666 0.0000 14 0 5 0.0000 1.4706 14 0 6 -1.0872 -0.0000 14 0 7 0.0000 3.8364 14 0 8 -7.8459 0.0000 14 0 9 0.0000 1.5329 14 0 10 -4.2793 0.0000 14 0 13 0.0000 2.3617 14 0 14 0.2989 0.0000 14 1 0 3.8052 -0.0000 14 1 1 0.4551 -6.0822 14 1 2 5.3225 -4.6019 14 1 3 5.2943 -0.2659 14 1 4 5.0064 5.0474 14 1 5 0.9921 -0.8703 14 1 6 -1.1495 2.9114 14 1 9 -3.6004 -0.3396 14 1 10 1.8188 -3.2464 14 1 11 -0.9175 -0.9725 14 1 12 2.2680 3.6429 14 1 13 0.2561 -5.7290 14 1 14 -0.6726 -4.4220 14 2 0 1.9108 -0.0000 14 2 1 -6.6029 -11.1071 14 2 2 -3.1443 -8.3704 14 2 3 -3.2390 -2.6028 14 2 4 7.7282 -1.7146 14 2 10 6.5703 -1.0059 14 2 11 -2.8385 2.1271 14 2 12 3.2035 4.9706 14 2 13 -2.4238 2.8790 14 2 14 3.9070 -0.2993 14 3 0 3.3255 -0.0000 14 3 1 3.1356 4.7300 14 3 2 1.9824 -1.9372 14 3 3 -1.5574 2.2883 14 3 10 -1.6312 6.5103 14 3 11 -4.9881 -0.5969 14 3 12 1.9049 2.3710 14 3 13 -2.2394 3.1003 14 4 0 2.8296 0.0000 14 4 1 -0.9310 5.3458 14 4 2 -5.3811 -2.1676 14 4 3 -0.0927 -6.9223 14 4 4 1.1235 1.2746 14 4 5 0.0584 3.2542 14 4 6 0.2431 4.2053 14 4 7 -3.4919 0.6288 14 4 10 3.3917 -0.2130 14 4 11 -1.0699 3.6121 14 4 12 -2.2796 -5.9242 14 5 0 0.9539 -0.0000 14 5 1 -1.6521 0.4743 14 5 2 0.9313 -2.2173 14 5 3 -5.9645 -4.6829 14 5 4 -1.2035 -1.0661 14 5 5 1.2739 -0.7995 14 5 6 3.9577 -0.8581 14 5 7 0.7369 -3.4683 14 5 8 -4.3753 3.3564 14 5 9 -0.7099 -0.9666 14 5 10 6.4244 -0.0339 14 5 11 4.5327 -0.3357 14 6 0 -0.4759 0.0000 14 6 1 -4.1184 -5.8627 14 6 2 -1.0335 2.6976 14 6 3 0.6423 -1.3216 14 6 4 3.4146 0.6821 14 6 5 -2.4546 0.0574 14 6 6 0.5760 1.4980 14 6 7 9.9280 -4.6678 14 6 8 2.5726 -2.6224 14 6 9 -1.4038 -4.2767 14 7 0 2.6753 -0.0000 14 7 1 -2.1491 1.5380 14 7 2 2.6412 -2.0411 14 7 3 -3.4251 -4.9761 14 7 4 3.1878 -3.0464 14 7 5 2.2626 0.5283 14 7 6 -4.3927 -1.1385 15 0 1 0.5297 0.0000 15 0 2 0.0000 7.1458 15 0 3 -5.0086 -0.0000 15 0 4 0.0000 1.0517 15 0 5 0.7239 -0.0000 15 0 6 -0.0000 -3.5860 15 0 7 -0.9420 -0.0000 15 0 8 -0.0000 -1.9686 15 0 9 6.3568 0.0000 15 0 10 -0.0000 -6.0036 15 1 0 -2.7584 -0.0000 15 1 1 -3.4002 -0.7217 15 1 2 -1.2306 0.2741 15 1 3 -4.5870 1.6391 15 1 4 0.1962 5.3316 15 1 5 2.3987 -5.2104 15 1 6 0.8866 4.5010 15 1 7 -7.3989 5.3135 15 1 8 0.5530 -1.8551 15 1 10 -1.2291 6.5880 15 2 0 -0.8254 0.0000 15 2 1 5.1565 -1.9136 15 2 2 3.2346 4.4634 15 2 3 0.8413 -3.2744 15 2 4 6.6312 6.8230 15 2 5 4.1373 -1.4505 15 3 0 8.5462 -0.0000 15 4 0 -4.6029 0.0000 15 4 1 -9.9662 -2.5885 15 4 2 -0.5266 1.3786 15 4 3 -0.8724 -0.3187 15 4 4 1.0886 -0.7128 15 4 5 -7.6517 -4.1520 15 5 0 -3.4598 -0.0000 15 5 1 1.5571 -3.7991 15 5 2 -5.0914 2.8000 15 5 3 -3.3238 3.6839 15 5 4 1.0145 0.1704 0 0 0 0.0 0.0 ; _shelx_fab_checksum 31049 _olex2_submission_special_instructions 'No special instructions were received' #END data_MOF520_2.24GPa _chemical_name_common 'MOF-520_2.24GPa' _chemical_name_systematic ? _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0310 0.0240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 94 _space_group_name_H-M_alt 'P 42 21 2' _space_group_name_Hall 'P 4n 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 19.130(3) _cell_length_b 19.130(3) _cell_length_c 36.480(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13350(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4198 _cell_measurement_theta_max 12.42 _cell_measurement_theta_min 2.21 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.566 _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 0.029 _shelx_estimated_absorpt_T_max 0.7436 _shelx_estimated_absorpt_T_min 0.5946 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 0.7436 _exptl_absorpt_correction_T_min 0.5946 _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1180 before and 0.0640 after correction. The Ratio of minimum to maximum transmission is 0.7996. The \l/2 correction factor is Not present. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Perkin Elmer CMOS' _diffrn_measurement_method '\w 80 degrees scan' _diffrn_detector_area_resol_mean ? _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 2.24 GPa was measured via ruby method. The sample was collected by rotating 80 degrees. The data sets were merged in XPREP to produce the final data set. ; _diffrn_reflns_number 11629 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_unetI/netI 0.0652 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_theta_full 17.311 _diffrn_reflns_theta_max 12.449 _diffrn_reflns_theta_min 0.839 _diffrn_measured_fraction_theta_full 0.378 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_Laue_measured_fraction_full 0.378 _diffrn_reflns_Laue_measured_fraction_max 0.952 _diffrn_reflns_point_group_measured_fraction_full 0.361 _diffrn_reflns_point_group_measured_fraction_max 0.946 _reflns_number_total 4366 _reflns_number_gt 3499 _diffrn_standards_number 0 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.698 _reflns_Friedel_fraction_full 0.339 _reflns_Friedel_fraction_max 0.938 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_diff_density_max 0.146 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.028 _refine_ls_abs_structure_details ; Flack x determined using 1264 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.2(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 4366 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0465 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1261 _refine_ls_wR_factor_ref 0.1332 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All O(H) groups 2. Rigid body (RIGU) restrains O3, Al1, O1, O10, Al2, H1, C28, O2, O9, H28, Al3, H2, C1, O4, C2, C7, C3, H7, C6, H3, C4, H6, C5, H4, C8, C13, C9, H13, C12, C10, H9, C21, C11, C14, C26, C22, H11, C19, C15, H26, C25, C23, H22, C18, H19, C16, H15, H25, C24, H23, C17, H18, H16, C27, C20, O8, O7, O5, O6, Al1, O1, Al1, O10, Al2, O1, O1, H1, O10, C28, Al2, O2, Al2, O3, Al2, O9, O9, C28, C28, H28, Al3, O2, O2, H2, O3, C1, Al3, O4, O4, C1, C2, C1, C7, C2, C3, C2, C7, H7, C7, C6, C3, H3, C4, C3, C6, H6, C6, C5, C5, C4, C4, H4, C8, C5, C8, C13, C9, C8, C13, H13, C13, C12, C9, C10, C9, H9, C21, C12, C12, C11, C14, C10, C11, C10, C26, C21, C22, C21, C11, H11, C19, C14, C15, C14, C26, H26, C26, C25, C23, C22, C22, H22, C19, C18, C19, H19, C16, C15, C15, H15, C25, H25, C25, C24, C23, H23, C24, C23, C18, C17, C18, H18, C17, C16, C16, H16, C27, C24, C20, C17, O8, C27, O7, C27, O5, C20, O6, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C26(H26), C23(H23), C25(H25), C22(H22), C7(H7), C16(H16), C18(H18), C6(H6), C13(H13), C19(H19), C15(H15), C9(H9), C28(H28), C3(H3), C4(H4), C11(H11) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.66374(10) 0.33626(10) 0.5000 0.0525(9) Uani 1 2 d S TU P . . Al2 Al 0.61615(11) 0.38886(10) 0.41646(6) 0.0555(7) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38307(9) 0.0483(9) Uani 1 2 d S TU P . . O2 O 0.5649(2) 0.4716(2) 0.41875(13) 0.0537(13) Uani 1 1 d . U . . . H2 H 0.5720 0.5007 0.4388 0.064 Uiso 1 1 calc R U . . . O3 O 0.6397(2) 0.3999(2) 0.36570(15) 0.0652(15) Uani 1 1 d . U . . . O1 O 0.6001(2) 0.3673(2) 0.46521(12) 0.0559(14) Uani 1 1 d . U . . . H1 H 0.5543 0.3728 0.4733 0.067 Uiso 1 1 calc R U . . . O4 O 0.5591(2) 0.4747(2) 0.34412(13) 0.0581(15) Uani 1 1 d . U . . . C1 C 0.6095(4) 0.4367(4) 0.3393(3) 0.057(2) Uani 1 1 d . U . . . C26 C 0.7667(4) 0.6287(4) 0.1404(2) 0.090(3) Uani 1 1 d . U . . . H26 H 0.7636 0.6262 0.1658 0.108 Uiso 1 1 calc R U . . . C23 C 0.7765(4) 0.6346(4) 0.0651(3) 0.092(3) Uani 1 1 d . U . . . H23 H 0.7728 0.6375 0.0397 0.110 Uiso 1 1 calc R U . . . C20 C 0.9745(4) 0.1476(4) 0.1120(2) 0.072(3) Uani 1 1 d . U . . . C25 C 0.7763(5) 0.6944(4) 0.1222(3) 0.104(3) Uani 1 1 d . U . . . H25 H 0.7767 0.7368 0.1347 0.125 Uiso 1 1 calc R U . . . C22 C 0.7732(5) 0.5680(4) 0.0841(3) 0.104(3) Uani 1 1 d . U . . . H22 H 0.7796 0.5267 0.0710 0.125 Uiso 1 1 calc R U . . . C24 C 0.7848(4) 0.6897(4) 0.0851(3) 0.083(3) Uani 1 1 d . U . . . C27 C 0.8050(4) 0.7612(4) 0.0626(3) 0.061(3) Uani 1 1 d . U . . . C17 C 0.9317(4) 0.2085(4) 0.1205(2) 0.072(3) Uani 1 1 d . U . . . C7 C 0.6159(5) 0.4767(5) 0.2752(3) 0.117(4) Uani 1 1 d . U . . . H7 H 0.5794 0.5078 0.2793 0.141 Uiso 1 1 calc R U . . . C21 C 0.7618(4) 0.5658(4) 0.1177(3) 0.072(2) Uani 1 1 d . U . . . C16 C 0.8721(4) 0.2007(4) 0.1374(2) 0.075(3) Uani 1 1 d . U . . . H16 H 0.8584 0.1558 0.1441 0.090 Uiso 1 1 calc R U . . . C2 C 0.6429(5) 0.4336(4) 0.3063(3) 0.078(3) Uani 1 1 d . U . . . C18 C 0.9471(5) 0.2768(4) 0.1050(3) 0.117(4) Uani 1 1 d . U . . . H18 H 0.9828 0.2852 0.0883 0.141 Uiso 1 1 calc R U . . . C14 C 0.8400(5) 0.3198(4) 0.1359(2) 0.082(3) Uani 1 1 d . U . . . C6 C 0.6429(5) 0.4717(4) 0.2417(3) 0.104(3) Uani 1 1 d . U . . . H6 H 0.6223 0.4995 0.2237 0.125 Uiso 1 1 calc R U . . . C13 C 0.7267(4) 0.4947(4) 0.1725(3) 0.091(3) Uani 1 1 d . U . . . H13 H 0.7032 0.5338 0.1813 0.109 Uiso 1 1 calc R U . . . C19 C 0.9004(5) 0.3297(4) 0.1186(3) 0.097(3) Uani 1 1 d . U . . . H19 H 0.9139 0.3759 0.1149 0.116 Uiso 1 1 calc R U . . . C10 C 0.8034(5) 0.3785(4) 0.1512(3) 0.091(3) Uani 1 1 d . U . . . C15 C 0.8288(4) 0.2553(4) 0.1458(2) 0.078(3) Uani 1 1 d . U . . . H15 H 0.7888 0.2459 0.1594 0.094 Uiso 1 1 calc R U . . . C12 C 0.7579(5) 0.4965(5) 0.1390(3) 0.105(3) Uani 1 1 d . U . . . C9 C 0.7678(5) 0.3778(4) 0.1828(3) 0.094(3) Uani 1 1 d . U . . . H9 H 0.7689 0.3381 0.1975 0.113 Uiso 1 1 calc R U . . . O8 O 0.8273(2) 0.8040(2) 0.08941(14) 0.0662(15) Uani 1 1 d . U . . . O10 O 0.7337(2) 0.3978(3) 0.48275(15) 0.0695(16) Uani 1 1 d . U . . . O5 O 1.0391(3) 0.1671(2) 0.09762(14) 0.0664(16) Uani 1 1 d . U . . . O6 O 0.9568(2) 0.0894(2) 0.12021(13) 0.0536(14) Uani 1 1 d . U . . . O7 O 0.8015(3) 0.7660(2) 0.03245(17) 0.0680(18) Uani 1 1 d . U . . . O9 O 0.6985(3) 0.4397(3) 0.42709(17) 0.0742(17) Uani 1 1 d . U . . . C28 C 0.7375(5) 0.4394(5) 0.4545(3) 0.087(3) Uani 1 1 d . U . . . H28 H 0.7731 0.4725 0.4548 0.105 Uiso 1 1 calc R U . . . C5 C 0.6939(5) 0.4330(4) 0.2312(3) 0.093(3) Uani 1 1 d . U . . . C8 C 0.7301(5) 0.4340(5) 0.1936(3) 0.111(4) Uani 1 1 d . U . . . C3 C 0.6978(5) 0.3946(5) 0.2965(3) 0.115(4) Uani 1 1 d . U . . . H3 H 0.7168 0.3656 0.3143 0.138 Uiso 1 1 calc R U . . . C4 C 0.7276(5) 0.3933(4) 0.2640(3) 0.106(3) Uani 1 1 d . U . . . H4 H 0.7690 0.3686 0.2606 0.127 Uiso 1 1 calc R U . . . C11 C 0.7941(5) 0.4412(4) 0.1280(3) 0.113(4) Uani 1 1 d . U . . . H11 H 0.8144 0.4419 0.1049 0.136 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 0.0558(13) 0.0558(13) 0.046(3) -0.0048(12) -0.0048(12) 0.0098(15) Al2 0.0569(15) 0.0482(14) 0.061(2) -0.0004(12) -0.0022(12) 0.0142(11) Al3 0.060(2) 0.0474(19) 0.038(3) 0.000 0.000 0.0117(14) O2 0.054(3) 0.057(3) 0.050(4) -0.003(2) 0.002(2) 0.009(2) O3 0.075(3) 0.055(3) 0.065(4) 0.007(3) 0.013(3) 0.017(3) O1 0.048(3) 0.061(3) 0.059(4) 0.013(2) -0.002(2) 0.010(2) O4 0.076(4) 0.051(3) 0.048(4) 0.004(2) 0.008(3) 0.022(3) C1 0.077(5) 0.042(5) 0.051(6) 0.000(4) 0.016(4) 0.017(4) C26 0.135(8) 0.067(5) 0.066(7) 0.016(4) 0.023(5) 0.008(5) C23 0.135(8) 0.071(5) 0.070(7) -0.003(5) 0.018(5) -0.033(5) C20 0.089(6) 0.050(5) 0.077(8) -0.006(4) 0.035(5) 0.005(4) C25 0.179(9) 0.071(5) 0.062(7) 0.008(5) 0.007(6) -0.012(5) C22 0.165(9) 0.066(5) 0.081(7) 0.008(5) 0.053(6) -0.013(5) C24 0.111(7) 0.066(5) 0.072(6) 0.013(4) 0.010(5) -0.020(5) C27 0.071(5) 0.057(5) 0.057(6) 0.007(5) -0.007(5) -0.005(4) C17 0.093(5) 0.052(5) 0.072(7) -0.003(4) 0.038(5) 0.008(4) C7 0.142(8) 0.135(8) 0.075(7) 0.033(6) 0.039(6) 0.088(7) C21 0.084(6) 0.057(5) 0.075(7) 0.008(4) 0.036(5) 0.006(4) C16 0.098(6) 0.046(5) 0.079(7) 0.008(4) 0.040(5) 0.003(4) C2 0.094(6) 0.072(6) 0.068(6) 0.011(4) 0.025(5) 0.046(5) C18 0.144(8) 0.060(5) 0.148(10) 0.015(5) 0.078(7) 0.005(5) C14 0.112(6) 0.048(5) 0.087(8) -0.003(4) 0.034(5) 0.009(5) C6 0.137(8) 0.106(7) 0.068(7) 0.029(5) 0.030(6) 0.070(6) C13 0.128(7) 0.055(5) 0.090(7) 0.005(5) 0.056(6) 0.026(5) C19 0.126(7) 0.058(5) 0.105(8) 0.005(5) 0.049(6) 0.007(5) C10 0.122(7) 0.054(5) 0.097(7) 0.008(5) 0.055(5) 0.008(4) C15 0.101(6) 0.049(5) 0.084(8) -0.001(4) 0.048(5) 0.007(4) C12 0.141(8) 0.070(5) 0.103(8) 0.003(5) 0.055(6) 0.018(5) C9 0.127(7) 0.055(5) 0.099(8) 0.016(5) 0.057(6) 0.021(5) O8 0.072(3) 0.068(4) 0.058(5) 0.011(3) 0.008(3) -0.017(3) O10 0.051(3) 0.074(4) 0.084(5) -0.002(3) -0.004(3) -0.001(3) O5 0.087(4) 0.046(3) 0.067(5) -0.009(3) 0.025(3) 0.003(3) O6 0.075(3) 0.042(3) 0.045(4) -0.005(3) 0.022(2) -0.005(3) O7 0.091(4) 0.069(3) 0.044(5) 0.007(3) -0.012(4) -0.010(3) O9 0.062(4) 0.079(4) 0.081(5) 0.001(3) 0.001(3) 0.003(3) C28 0.074(6) 0.101(7) 0.087(8) 0.016(5) -0.002(5) -0.012(5) C5 0.118(7) 0.079(6) 0.081(7) 0.022(5) 0.035(5) 0.032(5) C8 0.158(9) 0.070(6) 0.105(7) 0.020(5) 0.060(6) 0.046(6) C3 0.133(8) 0.124(8) 0.089(8) 0.034(6) 0.044(6) 0.074(6) C4 0.122(7) 0.100(7) 0.096(8) 0.021(6) 0.030(6) 0.055(6) C11 0.174(9) 0.060(5) 0.105(8) 0.019(5) 0.084(7) 0.045(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.856(5) 8_666 ? Al1 O1 1.857(5) . ? Al1 O10 1.890(5) 8_666 ? Al1 O10 1.890(5) . ? Al1 O7 1.911(6) 6_645 ? Al1 O7 1.911(6) 2_645 ? Al2 O2 1.864(4) . ? Al2 O3 1.917(6) . ? Al2 O1 1.851(5) . ? Al2 O8 1.962(5) 6_645 ? Al2 O5 1.894(5) 5_455 ? Al2 O9 1.892(6) . ? Al3 O2 1.879(5) . ? Al3 O2 1.879(5) 3_665 ? Al3 O4 1.879(5) 3_665 ? Al3 O4 1.879(5) . ? Al3 O6 1.903(4) 6_655 ? Al3 O6 1.903(4) 5_455 ? O3 C1 1.326(9) . ? O4 C1 1.221(8) . ? C1 C2 1.364(11) . ? C26 C25 1.433(11) . ? C26 C21 1.466(11) . ? C23 C22 1.451(11) . ? C23 C24 1.293(11) . ? C20 C17 1.458(10) . ? C20 O5 1.393(8) . ? C20 O6 1.202(8) . ? C25 C24 1.367(11) . ? C22 C21 1.246(10) . ? C24 C27 1.642(12) . ? C27 O8 1.345(10) . ? C27 O7 1.106(9) . ? C17 C16 1.304(9) . ? C17 C18 1.453(10) . ? C7 C2 1.495(11) . ? C7 C6 1.329(11) . ? C21 C12 1.539(12) . ? C16 C15 1.369(9) . ? C2 C3 1.337(11) . ? C18 C19 1.437(10) . ? C14 C19 1.329(10) . ? C14 C10 1.437(11) . ? C14 C15 1.303(10) . ? C6 C5 1.284(10) . ? C13 C12 1.361(10) . ? C13 C8 1.394(11) . ? C10 C9 1.339(10) . ? C10 C11 1.479(11) . ? C12 C11 1.325(10) . ? C9 C8 1.352(10) . ? O8 Al2 1.962(5) 6_655 ? O10 C28 1.306(10) . ? O5 Al2 1.894(5) 5 ? O6 Al3 1.903(4) 5 ? O7 Al1 1.911(6) 4_564 ? O9 C28 1.247(10) . ? C5 C8 1.537(12) . ? C5 C4 1.558(12) . ? C3 C4 1.314(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 92.7(3) 8_666 . ? O1 Al1 O10 92.6(2) . 8_666 ? O1 Al1 O10 92.2(2) . . ? O1 Al1 O10 92.2(2) 8_666 8_666 ? O1 Al1 O10 92.6(2) 8_666 . ? O1 Al1 O7 175.2(2) 8_666 6_645 ? O1 Al1 O7 175.2(2) . 2_645 ? O1 Al1 O7 91.7(2) 8_666 2_645 ? O1 Al1 O7 91.7(2) . 6_645 ? O10 Al1 O10 173.0(3) 8_666 . ? O10 Al1 O7 85.7(2) . 2_645 ? O10 Al1 O7 89.2(2) . 6_645 ? O10 Al1 O7 85.7(2) 8_666 6_645 ? O10 Al1 O7 89.2(2) 8_666 2_645 ? O7 Al1 O7 83.9(4) 6_645 2_645 ? O2 Al2 O3 94.2(2) . . ? O2 Al2 O8 175.8(3) . 6_645 ? O2 Al2 O5 94.8(2) . 5_455 ? O2 Al2 O9 89.5(2) . . ? O3 Al2 O8 81.7(2) . 6_645 ? O1 Al2 O2 93.4(2) . . ? O1 Al2 O3 172.4(2) . . ? O1 Al2 O8 90.7(2) . 6_645 ? O1 Al2 O5 90.3(2) . 5_455 ? O1 Al2 O9 93.2(2) . . ? O5 Al2 O3 89.0(2) 5_455 . ? O5 Al2 O8 86.1(2) 5_455 6_645 ? O9 Al2 O3 86.9(2) . . ? O9 Al2 O8 89.3(2) . 6_645 ? O9 Al2 O5 174.3(3) . 5_455 ? O2 Al3 O2 92.3(3) 3_665 . ? O2 Al3 O6 94.09(19) 3_665 6_655 ? O2 Al3 O6 90.92(19) 3_665 5_455 ? O2 Al3 O6 94.08(19) . 5_455 ? O2 Al3 O6 90.92(19) . 6_655 ? O4 Al3 O2 174.7(2) 3_665 . ? O4 Al3 O2 92.96(19) 3_665 3_665 ? O4 Al3 O2 174.7(2) . 3_665 ? O4 Al3 O2 92.96(19) . . ? O4 Al3 O4 81.8(3) 3_665 . ? O4 Al3 O6 89.0(2) 3_665 6_655 ? O4 Al3 O6 89.0(2) . 5_455 ? O4 Al3 O6 85.6(2) . 6_655 ? O4 Al3 O6 85.6(2) 3_665 5_455 ? O6 Al3 O6 172.8(3) 5_455 6_655 ? Al2 O2 Al3 124.2(3) . . ? C1 O3 Al2 131.2(5) . . ? Al2 O1 Al1 128.2(2) . . ? C1 O4 Al3 137.6(5) . . ? O3 C1 C2 114.5(8) . . ? O4 C1 O3 123.7(8) . . ? O4 C1 C2 121.6(8) . . ? C25 C26 C21 117.8(9) . . ? C24 C23 C22 116.9(10) . . ? O5 C20 C17 111.4(7) . . ? O6 C20 C17 121.9(7) . . ? O6 C20 O5 126.3(7) . . ? C24 C25 C26 114.6(8) . . ? C21 C22 C23 120.4(9) . . ? C23 C24 C25 126.8(9) . . ? C23 C24 C27 115.2(10) . . ? C25 C24 C27 117.9(8) . . ? O8 C27 C24 102.6(8) . . ? O7 C27 C24 123.5(9) . . ? O7 C27 O8 133.8(9) . . ? C16 C17 C20 120.0(8) . . ? C16 C17 C18 117.6(7) . . ? C18 C17 C20 121.4(8) . . ? C6 C7 C2 121.6(8) . . ? C26 C21 C12 115.1(9) . . ? C22 C21 C26 121.2(8) . . ? C22 C21 C12 122.3(8) . . ? C17 C16 C15 123.2(7) . . ? C1 C2 C7 119.0(8) . . ? C3 C2 C1 129.0(9) . . ? C3 C2 C7 112.0(9) . . ? C19 C18 C17 111.9(7) . . ? C19 C14 C10 119.8(8) . . ? C15 C14 C19 114.2(8) . . ? C15 C14 C10 123.4(8) . . ? C5 C6 C7 127.7(9) . . ? C12 C13 C8 119.7(8) . . ? C14 C19 C18 127.0(8) . . ? C14 C10 C11 118.0(9) . . ? C9 C10 C14 125.1(8) . . ? C9 C10 C11 116.0(8) . . ? C14 C15 C16 124.1(8) . . ? C13 C12 C21 119.8(8) . . ? C11 C12 C21 120.7(9) . . ? C11 C12 C13 118.7(9) . . ? C10 C9 C8 120.9(8) . . ? C27 O8 Al2 126.8(5) . 6_655 ? C28 O10 Al1 133.0(6) . . ? C20 O5 Al2 129.9(4) . 5 ? C20 O6 Al3 134.0(5) . 5 ? C27 O7 Al1 130.8(6) . 4_564 ? C28 O9 Al2 131.3(6) . . ? O9 C28 O10 127.1(9) . . ? C6 C5 C8 127.1(9) . . ? C6 C5 C4 111.4(9) . . ? C8 C5 C4 120.4(8) . . ? C13 C8 C5 118.7(8) . . ? C9 C8 C13 121.8(9) . . ? C9 C8 C5 119.3(8) . . ? C4 C3 C2 126.4(10) . . ? C3 C4 C5 120.3(9) . . ? C12 C11 C10 122.5(9) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.854 -0.839 -0.644 9528.4 12753.2 ? _shelx_res_file ; TITL P5_25kev_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.13 19.13 36.48 90 90 90 ZERR 220 0.00271 0.00271 0.0073 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.031 0.024 81.761 DISP C 0.001 0.001 6.243 DISP H -0 0 0.608 DISP O 0.004 0.003 13.948 UNIT 220 220 220 220 RIGU O3 Al1 O1 O10 Al2 H1 C28 O2 O9 H28 Al3 H2 C1 O4 C2 C7 C3 H7 C6 H3 C4 H6 = C5 H4 C8 C13 C9 H13 C12 C10 H9 C21 C11 C14 C26 C22 H11 C19 C15 H26 C25 C23 = H22 C18 H19 C16 H15 H25 C24 H23 C17 H18 H16 C27 C20 O8 O7 O5 O6 AL1 O1 AL1 = O10 AL2 O1 O1 H1 O10 C28 AL2 O2 AL2 O3 AL2 O9 O9 C28 C28 H28 AL3 O2 O2 H2 O3 = C1 AL3 O4 O4 C1 C2 C1 C7 C2 C3 C2 C7 H7 C7 C6 C3 H3 C4 C3 C6 H6 C6 C5 C5 C4 = C4 H4 C8 C5 C8 C13 C9 C8 C13 H13 C13 C12 C9 C10 C9 H9 C21 C12 C12 C11 C14 = C10 C11 C10 C26 C21 C22 C21 C11 H11 C19 C14 C15 C14 C26 H26 C26 C25 C23 C22 = C22 H22 C19 C18 C19 H19 C16 C15 C15 H15 C25 H25 C25 C24 C23 H23 C24 C23 C18 = C17 C18 H18 C17 C16 C16 H16 C27 C24 C20 C17 O8 C27 O7 C27 O5 C20 O6 C20 L.S. 24 PLAN 20 TEMP 23 BOND ABIN acta fmap 2 REM REM REM WGHT 0.085000 FVAR 0.10389 AL1 4 0.663738 0.336262 0.500000 10.50000 0.05581 0.05581 = 0.04580 -0.00483 -0.00483 0.00976 AL2 4 0.616148 0.388864 0.416457 11.00000 0.05694 0.04823 = 0.06122 -0.00036 -0.00218 0.01418 AL3 4 0.500000 0.500000 0.383072 10.50000 0.05983 0.04737 = 0.03761 0.00000 0.00000 0.01166 O2 3 0.564937 0.471629 0.418746 11.00000 0.05436 0.05658 = 0.05029 -0.00330 0.00217 0.00936 AFIX 43 H2 2 0.571969 0.500747 0.438825 11.00000 -1.20000 AFIX 0 O3 3 0.639668 0.399855 0.365699 11.00000 0.07540 0.05535 = 0.06472 0.00708 0.01344 0.01656 O1 3 0.600085 0.367339 0.465212 11.00000 0.04791 0.06066 = 0.05927 0.01309 -0.00174 0.01043 AFIX 43 H1 2 0.554309 0.372787 0.473307 11.00000 -1.20000 AFIX 0 O4 3 0.559084 0.474664 0.344121 11.00000 0.07578 0.05112 = 0.04750 0.00414 0.00826 0.02211 C1 1 0.609545 0.436720 0.339271 11.00000 0.07689 0.04214 = 0.05060 0.00018 0.01627 0.01698 C26 1 0.766664 0.628747 0.140423 11.00000 0.13528 0.06746 = 0.06636 0.01560 0.02340 0.00822 AFIX 43 H26 2 0.763622 0.626153 0.165830 11.00000 -1.20000 AFIX 0 C23 1 0.776463 0.634575 0.065076 11.00000 0.13486 0.07091 = 0.07035 -0.00348 0.01791 -0.03332 AFIX 43 H23 2 0.772764 0.637460 0.039701 11.00000 -1.20000 AFIX 0 C20 1 0.974520 0.147608 0.112008 11.00000 0.08938 0.04993 = 0.07737 -0.00630 0.03545 0.00454 C25 1 0.776293 0.694401 0.122219 11.00000 0.17917 0.07051 = 0.06227 0.00833 0.00738 -0.01162 AFIX 43 H25 2 0.776725 0.736829 0.134663 11.00000 -1.20000 AFIX 0 C22 1 0.773157 0.567979 0.084055 11.00000 0.16519 0.06637 = 0.08104 0.00850 0.05276 -0.01304 AFIX 43 H22 2 0.779585 0.526667 0.071046 11.00000 -1.20000 AFIX 0 C24 1 0.784792 0.689693 0.085107 11.00000 0.11052 0.06564 = 0.07175 0.01289 0.01019 -0.01962 C27 1 0.805024 0.761194 0.062599 11.00000 0.07087 0.05675 = 0.05677 0.00724 -0.00652 -0.00480 C17 1 0.931656 0.208484 0.120507 11.00000 0.09340 0.05205 = 0.07191 -0.00337 0.03848 0.00803 C7 1 0.615910 0.476719 0.275156 11.00000 0.14175 0.13519 = 0.07518 0.03297 0.03880 0.08814 AFIX 43 H7 2 0.579394 0.507811 0.279326 11.00000 -1.20000 AFIX 0 C21 1 0.761768 0.565792 0.117654 11.00000 0.08395 0.05704 = 0.07525 0.00808 0.03575 0.00552 C16 1 0.872117 0.200695 0.137422 11.00000 0.09827 0.04615 = 0.07936 0.00758 0.03972 0.00342 AFIX 43 H16 2 0.858441 0.155828 0.144123 11.00000 -1.20000 AFIX 0 C2 1 0.642879 0.433570 0.306274 11.00000 0.09380 0.07182 = 0.06840 0.01135 0.02473 0.04636 C18 1 0.947050 0.276780 0.105030 11.00000 0.14447 0.05952 = 0.14763 0.01477 0.07787 0.00505 AFIX 43 H18 2 0.982821 0.285238 0.088346 11.00000 -1.20000 AFIX 0 C14 1 0.840034 0.319789 0.135880 11.00000 0.11152 0.04833 = 0.08663 -0.00275 0.03442 0.00859 C6 1 0.642878 0.471701 0.241672 11.00000 0.13654 0.10632 = 0.06839 0.02940 0.02981 0.06976 AFIX 43 H6 2 0.622331 0.499492 0.223744 11.00000 -1.20000 AFIX 0 C13 1 0.726684 0.494666 0.172486 11.00000 0.12772 0.05450 = 0.08951 0.00468 0.05551 0.02560 AFIX 43 H13 2 0.703156 0.533757 0.181288 11.00000 -1.20000 AFIX 0 C19 1 0.900382 0.329691 0.118592 11.00000 0.12631 0.05788 = 0.10544 0.00491 0.04883 0.00718 AFIX 43 H19 2 0.913879 0.375851 0.114866 11.00000 -1.20000 AFIX 0 C10 1 0.803412 0.378468 0.151212 11.00000 0.12180 0.05421 = 0.09669 0.00812 0.05496 0.00755 C15 1 0.828750 0.255345 0.145799 11.00000 0.10128 0.04901 = 0.08361 -0.00141 0.04759 0.00652 AFIX 43 H15 2 0.788756 0.245875 0.159415 11.00000 -1.20000 AFIX 0 C12 1 0.757923 0.496465 0.138977 11.00000 0.14125 0.06962 = 0.10289 0.00259 0.05471 0.01849 C9 1 0.767783 0.377764 0.182790 11.00000 0.12732 0.05514 = 0.09910 0.01624 0.05747 0.02074 AFIX 43 H9 2 0.768945 0.338106 0.197522 11.00000 -1.20000 AFIX 0 O8 3 0.827281 0.804046 0.089410 11.00000 0.07182 0.06846 = 0.05824 0.01050 0.00759 -0.01712 O10 3 0.733731 0.397763 0.482748 11.00000 0.05101 0.07381 = 0.08366 -0.00196 -0.00435 -0.00132 O5 3 1.039061 0.167132 0.097616 11.00000 0.08664 0.04598 = 0.06654 -0.00905 0.02533 0.00330 O6 3 0.956808 0.089373 0.120212 11.00000 0.07454 0.04177 = 0.04460 -0.00495 0.02193 -0.00495 O7 3 0.801504 0.765982 0.032446 11.00000 0.09081 0.06892 = 0.04422 0.00701 -0.01220 -0.00976 O9 3 0.698497 0.439712 0.427086 11.00000 0.06243 0.07906 = 0.08101 0.00130 0.00089 0.00280 C28 1 0.737492 0.439426 0.454469 11.00000 0.07407 0.10078 = 0.08698 0.01636 -0.00151 -0.01186 AFIX 43 H28 2 0.773132 0.472484 0.454786 11.00000 -1.20000 AFIX 0 C5 1 0.693942 0.433020 0.231158 11.00000 0.11789 0.07872 = 0.08115 0.02189 0.03478 0.03157 C8 1 0.730117 0.433961 0.193554 11.00000 0.15836 0.06971 = 0.10467 0.02021 0.06041 0.04616 C3 1 0.697826 0.394620 0.296454 11.00000 0.13320 0.12406 = 0.08872 0.03395 0.04389 0.07353 AFIX 43 H3 2 0.716811 0.365635 0.314335 11.00000 -1.20000 AFIX 0 C4 1 0.727600 0.393310 0.264009 11.00000 0.12202 0.10015 = 0.09584 0.02148 0.03031 0.05495 AFIX 43 H4 2 0.768951 0.368570 0.260634 11.00000 -1.20000 AFIX 0 C11 1 0.794103 0.441218 0.128026 11.00000 0.17441 0.05998 = 0.10497 0.01910 0.08440 0.04462 AFIX 43 H11 2 0.814428 0.441919 0.104871 11.00000 -1.20000 AFIX 0 HKLF 4 REM P5_25kev_0m in P42212 #94 REM R1 = 0.0465 for 3499 Fo > 4sig(Fo) and 0.0590 for all 4366 data REM 362 parameters refined using 336 restraints END WGHT 0.0844 0.0000 REM Highest difference peak 0.146, deepest hole -0.254, 1-sigma level 0.028 Q1 1 0.7710 0.4966 0.0671 11.00000 0.05 0.15 Q2 1 0.8631 0.4474 0.1027 11.00000 0.05 0.13 Q3 1 1.0435 0.2842 0.1162 11.00000 0.05 0.11 Q4 1 0.7572 0.5628 0.0451 11.00000 0.05 0.11 Q5 1 1.0067 0.2726 0.0608 11.00000 0.05 0.11 Q6 1 1.0518 0.2215 0.1167 11.00000 0.05 0.10 Q7 1 0.9161 0.4017 0.1052 11.00000 0.05 0.09 Q8 1 0.5167 0.3323 0.5040 11.00000 0.05 0.09 Q9 1 0.7907 0.4991 0.4457 11.00000 0.05 0.09 Q10 1 0.8207 0.7364 0.1396 11.00000 0.05 0.09 Q11 1 0.8392 0.5684 0.1149 11.00000 0.05 0.09 Q12 1 0.7343 0.4217 0.4608 11.00000 0.05 0.09 Q13 1 0.8248 0.7822 0.1195 11.00000 0.05 0.09 Q14 1 0.5362 0.4710 0.3640 11.00000 0.05 0.09 Q15 1 0.8959 0.3921 0.0988 11.00000 0.05 0.09 Q16 1 0.5585 0.4672 0.3264 11.00000 0.05 0.09 Q17 1 0.8288 0.5004 0.1543 11.00000 0.05 0.09 Q18 1 0.7642 0.6217 0.1545 11.00000 0.05 0.09 Q19 1 0.7165 0.4909 0.4165 11.00000 0.05 0.09 Q20 1 0.9535 0.1083 0.0977 11.00000 0.05 0.08 ; _shelx_res_checksum 5670 _shelx_hkl_file ; 1 1 0 372.48 19.62 -1 -1 0 375.90 19.62 -2 -1 0 386.52 19.96 2 1 0 374.30 19.95 -2 -2 0 3.93 0.32 2 2 0 4.72 0.32 -3 -1 0 20.50 1.17 3 1 0 21.71 1.17 -2 -3 0 259.47 13.48 3 2 0 249.21 13.44 -3 -2 0 257.82 13.46 3 3 0 3.44 0.31 -3 -3 0 3.04 0.34 4 0 0 76.35 4.04 4 1 0 7.11 0.45 -4 -1 0 6.44 0.45 4 2 0 132.41 7.06 -4 -2 0 134.54 7.09 -4 -3 0 23.62 1.39 -3 -4 0 23.37 1.41 4 3 0 24.78 1.37 -4 -4 0 88.33 4.79 5 0 0 0.15 0.17 5 1 0 38.31 1.99 -5 -1 0 34.11 1.98 -5 -2 0 9.44 0.68 5 2 0 10.86 0.66 5 3 0 343.93 18.73 -5 -3 0 367.98 18.78 -4 -5 0 0.37 0.28 5 4 0 0.25 0.23 -5 -4 0 0.75 0.28 -5 -5 0 124.82 6.73 6 0 0 322.79 16.97 -6 -1 0 22.79 1.36 6 1 0 24.88 1.35 6 2 0 19.29 1.16 -6 -2 0 20.93 1.21 6 3 0 10.91 0.72 -6 -3 0 10.71 0.77 -6 -4 0 34.91 2.02 6 4 0 34.10 1.96 -5 -6 0 24.58 1.56 -6 -5 0 25.28 1.55 -6 -6 0 8.65 0.80 7 0 0 0.19 0.25 -7 -1 0 48.75 2.78 7 1 0 53.49 2.79 -7 -2 0 32.59 1.71 7 2 0 25.67 1.62 -7 -3 0 24.69 1.49 7 3 0 23.75 1.41 7 4 0 14.09 0.92 -7 -4 0 14.14 1.04 7 5 0 7.59 0.62 -7 -5 0 5.75 0.71 -7 -6 0 315.49 16.71 -6 -7 0 312.91 16.73 -7 -7 0 42.83 2.58 8 0 0 14.79 0.93 8 1 0 75.80 4.11 -8 -1 0 77.20 4.12 8 2 0 92.46 4.99 -8 -2 0 93.76 5.04 8 3 0 16.39 0.99 -8 -3 0 13.79 1.08 -8 -4 0 34.40 1.91 8 4 0 27.06 1.75 8 5 0 4.11 0.53 -8 -5 0 6.53 0.78 -8 -6 0 10.36 1.00 -8 -7 0 46.27 2.78 -7 -8 0 44.63 2.75 -8 -8 0 9.42 1.11 9 0 0 -0.28 0.30 9 -1 0 9.73 0.71 9 2 0 0.08 0.24 -9 -2 0 0.25 0.41 9 3 0 0.61 0.28 -9 -3 0 0.50 0.46 -9 -4 0 47.83 2.98 9 4 0 54.34 2.86 9 5 0 80.67 4.57 -9 -5 0 87.53 4.71 -9 -6 0 7.07 0.94 -9 -7 0 -0.70 0.56 -9 -8 0 -0.13 0.67 -8 -9 0 -0.11 0.62 -9 -9 0 60.15 3.65 10 0 0 7.62 0.65 10 -1 0 12.14 0.82 10 1 0 10.83 0.79 10 2 0 2.53 0.38 -10 -2 0 2.29 0.50 -10 -3 0 73.68 4.10 10 3 0 73.53 4.00 10 4 0 0.49 0.30 -10 -4 0 0.53 0.54 10 5 0 13.78 0.92 -10 -5 0 11.50 1.14 -10 -6 0 5.18 0.79 -10 -7 0 34.16 2.30 -10 -8 0 67.70 4.04 -9 -10 0 3.69 0.94 -10 -9 0 4.06 0.96 -10 -10 0 4.88 1.19 11 0 0 0.18 0.35 11 -1 0 0.49 0.40 11 1 0 0.40 0.29 11 2 0 18.78 1.13 -11 -2 0 17.09 1.23 -11 -3 0 1.38 0.57 11 3 0 1.48 0.36 11 4 0 29.70 1.61 -11 -4 0 23.32 1.78 -11 -5 0 37.77 2.52 11 5 0 42.89 2.32 -11 -6 0 23.96 1.78 -11 -7 0 23.48 1.83 -11 -8 0 16.18 1.58 -11 -9 0 0.24 0.84 -10 -11 0 9.85 1.73 -11 -10 0 12.97 1.64 -11 -11 0 9.66 1.56 12 0 0 3.13 0.46 12 1 0 1.90 0.37 12 -1 0 1.87 0.48 12 2 0 0.52 0.35 -12 -3 0 2.66 0.69 12 3 0 5.40 0.54 -12 -4 0 34.06 2.30 12 4 0 39.20 2.15 -12 -5 0 0.09 0.72 -12 -6 0 66.47 3.90 -12 -7 0 19.95 1.70 -12 -8 0 0.94 0.78 -12 -9 0 8.60 1.37 -12 -10 0 2.21 1.17 -12 -11 0 3.95 1.33 13 0 0 -0.17 0.34 13 -1 0 1.94 0.49 13 1 0 3.17 0.47 13 2 0 3.76 0.49 13 -2 0 3.79 0.60 13 3 0 28.09 1.58 -13 -3 0 24.05 1.71 13 4 0 9.67 0.73 -13 -4 0 6.92 1.06 -13 -5 0 70.98 4.12 -13 -6 0 0.69 0.77 -13 -7 0 1.59 0.90 -13 -8 0 0.18 0.87 -13 -9 0 0.67 0.95 -13 -10 0 4.49 1.30 14 0 0 1.59 0.38 14 -1 0 2.07 0.51 14 1 0 1.60 0.38 14 2 0 4.15 0.53 14 -2 0 4.80 0.75 14 3 0 -0.18 0.30 -14 -3 0 -0.21 0.63 14 4 0 56.57 3.11 -14 -4 0 55.18 3.34 -14 -5 0 1.07 0.79 -14 -6 0 -0.39 0.90 -14 -7 0 -0.97 0.88 -14 -8 0 0.70 1.01 15 0 0 -0.31 0.32 15 -1 0 0.09 0.40 15 1 0 -0.29 0.32 15 2 0 7.90 0.66 15 -2 0 7.50 0.87 15 3 0 24.75 1.48 -15 -4 0 1.84 0.76 -15 -5 0 0.05 0.81 -15 -6 0 0.81 0.86 -15 -7 0 2.36 1.06 16 0 0 28.96 1.64 16 1 0 34.70 1.95 16 -2 0 11.73 1.00 16 2 0 12.50 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2.47 0.40 -2 1 -5 100.23 5.14 -2 -1 5 92.35 5.17 1 2 -5 86.00 5.18 1 -2 5 95.47 5.18 2 -1 5 89.57 5.12 -1 2 -5 100.82 5.18 2 1 -5 98.84 5.19 -1 -2 5 104.75 5.22 2 2 -5 0.40 0.34 -2 2 -5 0.12 0.22 -2 -2 5 0.45 0.31 2 -2 5 0.35 0.24 0 -3 5 8.55 0.70 0 3 -5 7.91 0.65 -3 1 -5 53.98 2.82 1 -3 5 53.06 2.90 1 3 -5 47.36 2.91 -3 -1 5 52.04 2.89 -1 3 -5 54.73 2.90 3 -1 5 48.42 2.81 -1 -3 5 47.40 2.93 3 1 -5 57.79 2.91 2 3 -5 2.66 0.46 -3 -2 5 2.64 0.50 2 -3 5 2.87 0.44 -3 2 -5 2.06 0.34 -2 -3 5 2.33 0.50 3 -2 5 2.43 0.36 -2 3 -5 1.90 0.33 3 2 -5 2.58 0.44 -3 -3 5 2.66 0.50 -3 3 -5 1.83 0.32 3 3 -5 2.86 0.50 3 -3 5 2.60 0.38 0 -4 5 2.06 0.46 0 4 -5 2.04 0.41 -4 -1 5 121.40 6.72 1 -4 5 129.98 6.76 -4 1 -5 130.57 6.64 1 4 -5 117.74 6.75 4 1 -5 138.28 6.75 4 -1 5 119.01 6.63 -1 4 -5 120.21 6.72 -1 -4 5 123.19 6.78 -4 2 -5 122.97 6.26 2 4 -5 115.89 6.38 2 -4 5 121.54 6.36 -4 -2 5 112.95 6.36 -2 -4 5 114.21 6.41 -2 4 -5 115.79 6.31 4 2 -5 124.66 6.39 4 -2 5 112.41 6.27 -4 -3 5 28.26 1.75 -4 3 -5 25.45 1.56 3 -4 5 29.38 1.69 3 4 -5 28.82 1.75 -3 -4 5 28.43 1.75 -3 4 -5 24.71 1.59 4 3 -5 29.02 1.73 4 -3 5 29.10 1.63 4 -4 5 260.87 13.93 4 4 -5 265.35 14.01 -4 4 -5 263.92 13.88 -4 -4 5 261.04 14.03 0 -5 5 167.28 8.77 0 5 -5 157.56 8.69 -5 -1 5 189.80 9.80 1 5 -5 167.77 9.80 1 -5 5 186.80 9.85 -5 1 -5 196.87 9.68 5 1 -5 196.49 9.82 -1 5 -5 186.75 9.79 5 -1 5 161.05 9.67 -1 -5 5 183.07 9.87 2 5 -5 108.93 6.13 2 -5 5 114.44 6.12 -5 2 -5 115.07 5.98 -5 -2 5 108.43 6.11 5 -2 5 112.28 6.01 5 2 -5 112.84 6.13 -2 5 -5 119.70 6.07 -2 -5 5 108.94 6.18 -5 -3 5 20.76 1.43 3 -5 5 21.31 1.40 3 5 -5 24.14 1.46 -5 3 -5 22.96 1.25 -3 5 -5 20.21 1.31 5 3 -5 22.70 1.46 5 -3 5 19.66 1.29 -3 -5 5 22.54 1.50 -5 -4 5 402.44 20.83 -5 4 -5 387.01 20.66 4 5 -5 399.97 20.81 4 -5 5 398.59 20.75 5 4 -5 393.07 20.81 5 -4 5 393.09 20.71 -4 -5 5 415.45 20.87 -4 5 -5 352.57 20.69 5 -5 5 9.31 0.79 5 5 -5 10.93 0.96 -5 -5 5 12.25 1.02 -6 0 -5 14.53 0.78 0 -6 5 13.38 1.06 0 6 -5 10.87 0.95 -6 1 -5 26.61 1.42 1 -6 5 25.15 1.67 1 6 -5 25.08 1.61 -1 6 -5 25.74 1.60 6 1 -5 26.82 1.65 -1 -6 5 26.12 1.73 2 -6 5 100.49 5.62 2 6 -5 97.76 5.61 -6 -2 5 99.67 5.60 -6 2 -5 116.24 5.44 6 2 -5 110.74 5.65 6 -2 5 100.74 5.48 -2 6 -5 92.91 5.55 -2 -6 5 102.15 5.71 3 -6 5 27.37 1.71 -6 -3 5 28.72 1.77 3 6 -5 29.05 1.77 6 3 -5 30.41 1.80 -3 -6 5 28.14 1.87 6 -3 5 29.25 1.62 -3 6 -5 23.01 1.65 -6 -4 5 89.59 4.97 4 6 -5 90.05 4.92 4 -6 5 88.42 4.88 6 -4 5 87.19 4.80 6 4 -5 90.72 4.94 -4 -6 5 86.60 5.01 5 6 -5 55.85 3.04 5 -6 5 53.81 2.98 -6 -5 5 50.42 3.08 -5 -6 5 49.61 3.10 6 -5 5 53.09 2.93 6 5 -5 51.04 3.05 6 -6 5 127.29 6.92 -6 -6 5 124.34 7.11 6 6 -5 133.64 7.02 0 -7 5 5.57 0.83 0 7 -5 4.42 0.58 1 -7 5 58.52 3.35 1 7 -5 53.14 3.29 -1 7 -5 54.69 3.28 -1 -7 5 59.99 3.42 7 1 -5 64.59 3.33 2 7 -5 49.84 2.60 -7 -2 5 42.54 2.54 2 -7 5 36.09 2.55 -2 -7 5 43.69 2.68 7 -2 5 42.11 2.39 7 2 -5 43.24 2.61 -2 7 -5 50.02 2.55 -7 -3 5 44.27 2.71 3 7 -5 50.55 2.75 3 -7 5 43.55 2.70 -3 -7 5 46.60 2.85 7 -3 5 44.10 2.54 7 3 -5 48.10 2.74 -7 -4 5 1.78 0.54 4 7 -5 2.12 0.59 4 -7 5 2.33 0.50 -4 -7 5 1.93 0.64 7 -4 5 1.38 0.36 7 4 -5 1.67 0.57 5 -7 5 188.17 9.85 5 7 -5 178.31 9.87 -7 -5 5 192.66 9.98 -5 -7 5 182.40 10.01 7 5 -5 195.32 9.93 7 -5 5 165.53 9.76 6 -7 5 55.76 3.07 6 7 -5 53.97 3.11 -7 -6 5 52.14 3.21 -6 -7 5 50.63 3.23 7 6 -5 53.58 3.13 7 -6 5 53.04 3.00 -7 -7 5 79.21 4.66 7 -7 5 82.96 4.47 7 7 -5 78.66 4.51 0 8 -5 0.52 0.37 8 0 -5 0.69 0.50 0 -8 5 0.71 0.54 1 8 -5 5.06 0.72 1 -8 5 6.19 0.82 -8 -1 -5 5.89 0.39 -1 -8 5 6.59 0.88 -1 8 -5 5.41 0.65 8 1 -5 6.61 0.85 2 -8 5 5.68 0.82 -8 -2 5 4.88 0.77 2 8 -5 5.28 0.70 8 2 -5 5.40 0.81 8 -2 5 4.62 0.45 -2 -8 5 5.62 0.89 3 8 -5 43.46 2.70 -8 -3 5 43.81 2.74 3 -8 5 46.75 2.73 8 -3 5 45.07 2.52 -3 -8 5 46.82 2.85 8 3 -5 48.49 2.73 -8 -4 5 11.16 1.15 4 -8 5 10.36 1.02 4 8 -5 10.64 1.00 -4 -8 5 11.47 1.21 8 4 -5 10.48 1.01 8 -4 5 10.54 0.77 5 8 -5 46.06 2.80 -8 -5 5 46.91 2.92 8 5 -5 45.86 2.78 -5 -8 5 48.33 2.95 8 -5 5 46.10 2.62 -8 -6 5 55.37 3.25 6 8 -5 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15 -5 8 0.76 0.57 16 0 -8 6.61 1.27 16 -1 -8 -0.13 1.05 16 1 -8 2.77 1.12 0 1 -9 179.84 9.65 -1 1 -9 3.71 0.60 1 1 -9 3.64 0.62 0 -2 9 0.02 0.41 0 2 -9 0.49 0.45 1 -2 9 238.61 12.39 1 2 -9 220.32 12.41 -2 1 -9 234.72 12.37 -1 -2 9 225.44 12.40 2 1 -9 231.67 12.42 -1 2 -9 243.30 12.42 -2 -2 9 1.69 0.52 2 -2 9 1.51 0.41 2 2 -9 1.38 0.55 -2 2 -9 2.76 0.52 0 3 -9 10.82 0.99 0 -3 9 10.89 1.00 -3 1 -9 40.25 2.24 1 3 -9 37.28 2.35 1 -3 9 38.02 2.34 -1 -3 9 39.17 2.37 -1 3 -9 38.09 2.32 -3 -2 9 39.62 2.39 2 3 -9 38.66 2.43 2 -3 9 36.20 2.39 -3 2 -9 39.58 2.33 3 -2 9 38.46 2.31 -2 3 -9 43.81 2.40 -2 -3 9 42.27 2.46 3 -3 9 24.19 1.65 -3 3 -9 24.62 1.62 3 3 -9 26.52 1.75 -3 -3 9 26.02 1.78 0 -4 9 2.20 0.69 0 4 -9 2.04 0.61 1 -4 9 65.62 3.75 -4 1 -9 69.08 3.62 1 4 -9 56.70 3.74 -1 -4 9 64.35 3.76 -1 4 -9 66.16 3.72 4 1 -9 69.12 3.74 -4 -2 9 110.78 6.29 2 -4 9 115.46 6.29 2 4 -9 110.50 6.32 -4 2 -9 119.58 6.21 -2 4 -9 113.68 6.27 4 -2 9 107.12 6.17 -2 -4 9 117.81 6.35 4 2 -9 120.39 6.32 3 4 -9 25.16 1.77 3 -4 9 24.15 1.64 -4 -3 9 25.75 1.79 -4 3 -9 23.97 1.57 4 3 -9 26.71 1.75 -3 4 -9 26.68 1.63 -3 -4 9 24.34 1.77 4 -3 9 23.11 1.62 -4 -4 9 49.09 3.08 4 -4 9 49.00 2.97 4 4 -9 53.22 3.09 -4 4 -9 52.67 2.94 0 -5 9 4.86 0.81 0 5 -9 3.38 0.64 1 5 -9 198.99 11.27 1 -5 9 218.63 11.31 -5 1 -9 209.05 11.13 -1 -5 9 207.69 11.32 5 1 -9 210.19 11.24 -1 5 -9 211.43 11.26 -5 -2 9 24.83 1.68 2 -5 9 24.98 1.72 -5 2 -9 27.49 1.59 2 5 -9 24.74 1.75 5 2 -9 25.07 1.74 5 -2 9 24.50 1.55 -2 5 -9 24.90 1.67 -2 -5 9 24.70 1.83 3 -5 9 7.76 0.92 -5 3 -9 7.66 0.73 -5 -3 9 6.93 0.84 3 5 -9 6.60 1.02 5 -3 9 7.21 0.80 -3 5 -9 7.33 0.79 5 3 -9 7.78 1.01 -3 -5 9 7.88 1.13 -5 -4 9 7.40 0.98 4 -5 9 5.88 0.86 -5 4 -9 5.51 0.66 4 5 -9 6.47 1.05 5 -4 9 5.97 0.78 5 4 -9 5.78 0.95 -4 5 -9 6.42 0.73 -4 -5 9 7.02 1.03 5 -5 9 0.14 0.51 5 5 -9 0.42 0.75 -5 5 -9 0.68 0.39 -5 -5 9 0.65 0.57 0 6 -9 3.54 0.74 0 -6 9 3.55 0.77 1 -6 9 142.24 7.69 -6 1 -9 142.23 7.50 1 6 -9 129.38 7.66 -1 -6 9 139.71 7.73 -1 6 -9 144.79 7.65 6 1 -9 140.44 7.63 -6 -2 9 30.35 1.94 -6 2 -9 30.67 1.81 2 6 -9 27.99 2.01 2 -6 9 29.98 2.00 -2 -6 9 30.43 2.12 -2 6 -9 29.50 1.91 6 -2 9 28.77 1.79 6 2 -9 32.75 2.05 -6 -3 9 15.93 1.25 -6 3 -9 17.47 1.12 3 -6 9 16.37 1.38 3 6 -9 15.93 1.37 6 -3 9 16.64 1.20 -3 -6 9 16.38 1.50 6 3 -9 16.37 1.43 -3 6 -9 16.44 1.24 -6 -4 9 19.87 1.56 4 6 -9 19.34 1.56 4 -6 9 20.51 1.55 -6 4 -9 20.55 1.31 6 4 -9 21.84 1.70 -4 -6 9 19.89 1.68 -4 6 -9 18.23 1.35 6 -4 9 20.14 1.40 -6 5 -9 37.22 2.15 5 6 -9 38.72 2.43 -6 -5 9 36.13 2.40 5 -6 9 36.42 2.33 6 5 -9 38.41 2.47 6 -5 9 34.75 2.25 -5 6 -9 37.38 2.18 -5 -6 9 35.68 2.46 -6 6 -9 12.77 1.00 -6 -6 9 13.06 1.38 6 -6 9 12.88 1.21 6 6 -9 13.69 1.35 0 -7 9 260.62 13.79 0 7 -9 250.05 13.69 1 7 -9 24.66 1.83 -7 1 -9 27.68 1.62 1 -7 9 27.36 1.93 -1 7 -9 27.24 1.81 7 1 -9 27.64 1.86 -1 -7 9 27.37 2.01 2 7 -9 15.09 1.34 -7 -2 9 17.62 1.25 -7 2 -9 14.74 1.04 2 -7 9 13.75 1.34 -2 7 -9 17.30 1.22 7 -2 9 14.32 1.06 -2 -7 9 15.36 1.49 7 2 -9 15.71 1.34 3 -7 9 26.60 1.89 -7 -3 9 23.36 1.81 3 7 -9 26.85 1.90 -7 3 -9 27.36 1.61 -3 -7 9 28.62 2.08 7 -3 9 26.62 1.68 -3 7 -9 27.20 1.73 7 3 -9 28.44 1.99 -7 4 -9 61.87 3.45 4 7 -9 62.38 3.73 4 -7 9 61.87 3.70 -7 -4 9 61.10 3.71 7 -4 9 61.58 3.55 -4 -7 9 63.77 3.86 -4 7 -9 64.96 3.57 7 4 -9 63.19 3.77 -7 5 -9 25.88 1.58 -7 -5 9 26.23 1.93 5 -7 9 26.28 1.85 5 7 -9 24.71 1.91 7 -5 9 24.48 1.72 -5 7 -9 26.86 1.66 7 5 -9 24.11 1.95 -5 -7 9 26.98 1.99 -7 -6 9 41.32 2.90 6 -7 9 45.79 2.80 6 7 -9 45.51 2.90 -7 6 -9 41.82 2.54 7 6 -9 45.72 2.89 -6 7 -9 43.78 2.58 7 -6 9 48.96 2.74 -6 -7 9 45.14 2.91 -7 7 -9 10.35 0.86 7 -7 9 9.22 1.13 -7 -7 9 9.23 1.30 7 7 -9 11.48 1.34 0 -8 9 0.47 0.72 -8 0 -9 0.30 0.31 0 8 -9 0.31 0.53 1 -8 9 31.43 2.10 1 8 -9 25.66 1.91 -8 1 -9 29.59 1.71 -1 8 -9 26.32 1.90 8 1 -9 32.30 2.00 -1 -8 9 29.35 2.12 2 -8 9 64.82 3.78 -8 2 -9 63.81 3.42 2 8 -9 54.87 3.63 -2 -8 9 66.67 3.87 8 2 -9 63.71 3.75 -2 8 -9 61.67 3.59 3 8 -9 60.19 3.61 -8 3 -9 57.85 3.32 -8 -3 9 58.00 3.60 3 -8 9 61.13 3.66 -3 8 -9 63.03 3.52 -3 -8 9 64.42 3.82 8 -3 9 59.02 3.40 8 3 -9 63.69 3.70 4 -8 9 21.52 1.72 -8 -4 9 20.20 1.74 4 8 -9 20.05 1.70 -8 4 -9 22.91 1.32 8 -4 9 20.60 1.46 -4 -8 9 22.87 1.95 -4 8 -9 21.07 1.49 8 4 -9 22.99 1.81 -8 5 -9 22.05 1.29 -8 -5 9 18.33 1.65 5 -8 9 20.68 1.66 5 8 -9 18.87 1.66 8 5 -9 20.72 1.82 -5 -8 9 21.73 1.83 8 -5 9 19.49 1.46 -5 8 -9 21.53 1.41 6 8 -9 5.58 0.99 -8 6 -9 6.80 0.61 -8 -6 9 5.52 1.08 6 -8 9 7.98 1.07 8 -6 9 5.46 0.83 8 6 -9 6.88 1.13 -6 -8 9 4.81 1.13 -6 8 -9 5.05 0.70 -8 -7 9 24.11 1.98 7 -8 9 25.22 1.80 7 8 -9 23.53 1.87 -7 -8 9 23.81 2.01 8 7 -9 22.37 1.90 8 -7 9 22.04 1.71 8 -8 9 0.44 0.61 -8 -8 9 0.24 0.92 8 8 -9 -0.49 0.78 0 -9 9 15.56 1.53 -9 0 -9 14.28 0.96 0 9 -9 15.24 1.29 1 9 -9 1.30 0.65 1 -9 9 1.46 0.95 -9 1 -9 0.62 0.32 -1 -9 9 1.73 0.97 9 1 -9 1.93 0.74 -1 9 -9 2.08 0.69 2 9 -9 36.94 2.53 2 -9 9 40.82 2.71 -9 2 -9 40.28 2.22 -2 -9 9 38.84 2.79 9 2 -9 42.43 2.64 -2 9 -9 41.39 2.48 3 9 -9 3.63 0.81 3 -9 9 3.15 0.94 -9 -3 9 2.98 0.88 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16.14 2.45 -15 -5 -9 16.94 1.29 15 5 -9 15.31 1.83 0 1 -10 135.08 7.32 0 2 -10 68.22 3.81 0 -2 10 65.26 3.78 1 2 -10 83.49 4.59 -2 1 -10 79.57 4.52 1 -2 10 78.15 4.52 -1 2 -10 86.14 4.56 -1 -2 10 79.54 4.56 -2 2 -10 1.70 0.51 2 2 -10 1.60 0.58 2 -2 10 1.43 0.55 -2 -2 10 1.15 0.63 0 3 -10 204.95 10.73 0 -3 10 193.04 10.72 -3 1 -10 248.08 13.39 1 3 -10 236.40 13.47 1 -3 10 247.84 13.46 -1 -3 10 256.07 13.49 -1 3 -10 269.78 13.48 -3 -2 10 22.20 1.49 -3 2 -10 21.49 1.40 2 -3 10 20.30 1.43 2 3 -10 15.94 1.48 3 2 -10 20.24 1.49 -2 -3 10 20.08 1.49 3 -2 10 22.29 1.41 -2 3 -10 19.86 1.44 3 -3 10 17.34 1.32 -3 3 -10 18.20 1.32 3 3 -10 18.31 1.44 -3 -3 10 19.62 1.44 0 -4 10 11.10 1.07 0 4 -10 11.15 1.12 1 -4 10 268.33 15.27 -4 1 -10 308.55 15.18 1 4 -10 262.93 15.28 -1 4 -10 284.56 15.28 -1 -4 10 304.67 15.33 -4 2 -10 5.00 0.70 2 4 -10 2.72 0.71 -4 -2 10 5.34 0.84 2 -4 10 4.16 0.77 -2 4 -10 3.29 0.65 -2 -4 10 4.07 0.87 4 2 -10 5.09 0.80 4 -2 10 4.14 0.62 3 4 -10 36.20 2.20 -4 3 -10 29.07 1.95 -4 -3 10 30.36 2.05 3 -4 10 33.28 2.05 4 -3 10 31.18 1.99 -3 -4 10 27.09 2.16 4 3 -10 34.52 2.16 -3 4 -10 32.01 1.97 4 4 -10 3.63 0.81 4 -4 10 2.48 0.64 -4 -4 10 4.06 0.89 -4 4 -10 3.64 0.66 0 5 -10 58.13 3.54 0 -5 10 61.82 3.56 1 -5 10 77.62 4.35 1 5 -10 72.52 4.34 -5 1 -10 73.75 4.16 -1 -5 10 79.02 4.39 -1 5 -10 75.31 4.31 2 -5 10 12.80 1.18 -5 2 -10 13.49 1.02 -5 -2 10 12.97 1.08 2 5 -10 11.09 1.17 -2 -5 10 11.96 1.29 5 -2 10 11.26 0.98 5 2 -10 14.50 1.24 -2 5 -10 12.33 1.09 -5 3 -10 2.98 0.58 -5 -3 10 3.47 0.66 3 -5 10 3.34 0.67 3 5 -10 4.43 0.86 5 -3 10 2.87 0.62 5 3 -10 5.09 0.89 -3 -5 10 4.58 0.94 -3 5 -10 3.24 0.61 4 -5 10 25.27 1.80 4 5 -10 28.85 1.98 -5 -4 10 26.52 1.88 -5 4 -10 27.43 1.73 -4 -5 10 26.41 2.04 5 -4 10 25.94 1.80 -4 5 -10 28.15 1.77 5 4 -10 28.19 2.01 5 -5 10 0.26 0.55 -5 -5 10 0.15 0.67 -5 5 -10 0.65 0.48 5 5 -10 0.14 0.74 0 6 -10 123.38 7.15 0 -6 10 136.17 7.22 -6 1 -10 89.03 4.52 1 6 -10 75.41 4.68 1 -6 10 82.20 4.74 -1 -6 10 83.07 4.76 -1 6 -10 85.38 4.67 6 1 -10 76.31 4.63 -6 2 -10 16.94 1.15 2 -6 10 17.02 1.42 -6 -2 10 17.07 1.29 2 6 -10 15.08 1.33 -2 -6 10 18.20 1.57 -2 6 -10 15.47 1.29 6 2 -10 16.38 1.42 6 -2 10 13.95 1.13 -6 3 -10 21.56 1.41 -6 -3 10 18.80 1.53 3 6 -10 24.21 1.69 3 -6 10 19.35 1.63 -3 6 -10 22.62 1.54 6 3 -10 22.63 1.67 6 -3 10 21.44 1.47 -3 -6 10 21.13 1.81 4 -6 10 2.14 0.77 4 6 -10 1.20 0.75 -6 -4 10 1.89 0.69 -6 4 -10 1.70 0.43 6 -4 10 2.05 0.63 -4 -6 10 1.47 0.76 -4 6 -10 2.19 0.66 6 4 -10 1.74 0.84 5 6 -10 23.04 1.81 -6 5 -10 22.68 1.49 5 -6 10 22.07 1.68 -6 -5 10 21.00 1.71 -5 -6 10 22.11 1.74 6 5 -10 23.80 1.84 -5 6 -10 23.53 1.50 6 -5 10 22.32 1.61 -6 -6 10 126.36 7.05 6 6 -10 124.13 7.01 6 -6 10 124.08 6.89 -6 6 -10 125.38 6.78 0 7 -10 24.47 1.76 0 -7 10 23.99 1.82 1 7 -10 19.78 1.70 -7 1 -10 25.80 1.52 1 -7 10 24.88 1.82 7 1 -10 25.56 1.77 -1 -7 10 24.00 1.85 -1 7 -10 23.02 1.69 -7 2 -10 62.94 3.30 2 -7 10 58.67 3.57 2 7 -10 50.30 3.48 -2 -7 10 58.31 3.61 7 2 -10 61.65 3.54 -2 7 -10 59.01 3.44 3 -7 10 25.98 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14 1 17 -4.0987 4.9706 14 2 0 2.3175 -0.0000 14 2 1 2.4643 1.1917 14 2 2 -5.6118 -8.3604 14 2 3 6.9471 -3.4490 14 2 9 4.3920 1.1539 14 2 10 1.9659 -4.2722 14 2 11 -5.9295 1.4628 14 2 12 3.3224 6.2065 14 2 13 -2.3678 4.1341 14 2 14 2.5441 2.0449 14 2 15 -0.5756 -2.8722 14 2 16 2.0530 1.1388 14 3 0 -3.8022 0.0000 14 3 1 5.0812 -1.6178 14 3 9 2.7336 -2.0470 14 3 10 0.9040 7.3501 14 3 11 -1.5584 -2.5174 14 3 12 4.9248 6.4002 14 3 13 0.7337 0.4069 14 3 14 -3.9896 2.4607 14 3 15 -0.0402 -2.9552 14 3 16 0.8445 1.9685 14 4 0 -1.2652 0.0000 14 4 1 2.8299 -0.3493 14 4 2 -8.0721 0.5397 14 4 3 2.4940 -3.1659 14 4 4 2.5849 -5.6336 14 4 5 -1.5665 4.2012 14 4 6 5.1989 0.5869 14 4 7 -3.0556 3.4707 14 4 8 4.6636 1.3605 14 4 9 0.6447 0.9402 14 4 10 0.6404 -3.9519 14 4 11 -5.7632 2.3300 14 4 12 -2.7588 -4.0998 14 4 13 -4.7108 4.4269 14 4 14 0.5493 -3.1176 14 4 15 -2.6508 -1.3502 14 5 0 1.8249 -0.0000 14 5 1 -6.3785 2.5173 14 5 2 -5.4870 -1.3445 14 5 3 -8.4144 -4.2702 14 5 4 -3.6755 -7.6148 14 5 5 1.9691 -6.1749 14 5 6 7.6054 -1.2087 14 5 7 0.4298 -3.5844 14 5 8 1.5466 1.9185 14 5 9 3.7018 1.7162 14 5 10 4.4033 4.0196 14 5 11 3.3050 1.3133 14 5 12 5.3277 -0.1932 14 5 13 2.8056 -4.2664 14 5 14 3.8702 0.7032 14 6 0 -0.1475 0.0000 14 6 1 -1.0478 -4.2861 14 6 2 2.5300 7.2759 14 6 3 -2.2273 -0.8832 14 6 4 2.2763 -1.5182 14 6 5 -0.3009 1.5967 14 6 6 0.7041 -0.3426 14 6 7 7.4387 5.5094 14 6 8 -4.7798 0.3977 14 6 9 -1.1208 -2.3056 14 6 10 -2.3556 -0.8552 14 6 11 6.0750 -0.4417 14 6 12 -1.5680 -5.0524 14 7 0 6.4647 -0.0000 14 7 1 -1.7858 -1.2187 14 7 2 5.7026 -2.9219 14 7 3 -2.9656 -1.3498 14 7 4 1.1588 1.8711 14 7 5 -0.9305 3.9756 14 7 6 1.8102 -4.3751 14 7 7 0.6765 0.1381 14 7 8 0.7343 -2.1716 14 7 9 -2.9790 2.5612 14 7 10 2.0769 -4.5847 14 8 0 -4.4228 0.0000 14 8 1 -3.6333 -0.6118 14 8 2 6.5687 3.7908 14 8 3 -0.7949 -0.4252 14 8 4 4.5700 1.0717 14 8 5 1.4695 -1.9092 14 8 6 0.6212 4.6945 14 8 7 3.4771 -1.4875 15 0 1 -1.3056 0.0000 15 0 2 0.0000 4.4026 15 0 3 -8.9235 -0.0000 15 0 4 -0.0000 -7.4676 15 0 5 -1.2536 -0.0000 15 0 6 -0.0000 -8.8553 15 0 7 -0.8542 0.0000 15 0 8 -0.0000 -6.7468 15 0 9 2.7186 0.0000 15 0 10 -0.0000 -7.3082 15 0 11 2.4014 -0.0000 15 0 12 -0.0000 -1.4900 15 0 13 -6.1359 -0.0000 15 1 0 -5.8003 -0.0000 15 1 1 -0.2842 -1.0971 15 1 2 0.8207 0.9446 15 1 3 -8.0857 1.5831 15 1 4 -2.3017 8.3271 15 1 5 -0.8013 -3.6213 15 1 6 -1.6758 3.8096 15 1 8 -0.7488 -5.1820 15 1 9 -1.2731 6.3589 15 1 10 -2.1534 2.9636 15 1 11 -2.1554 -2.8014 15 1 12 -0.1373 -5.0147 15 1 13 -6.3912 3.5716 15 2 0 -1.9490 -0.0000 15 2 1 1.1596 4.3581 15 2 2 1.2683 -3.0063 15 2 3 9.0427 -1.4453 15 2 4 7.2814 0.1657 15 2 10 0.2007 2.9345 15 2 11 0.1113 6.3344 15 2 12 0.0568 -4.4733 15 2 13 1.3605 -3.7798 15 3 0 6.1470 -0.0000 15 3 10 -2.4372 -1.2574 15 3 11 -3.4409 4.1921 15 3 12 -2.3440 1.8296 15 4 0 -2.0225 -0.0000 15 4 1 -3.3751 4.1237 15 4 2 1.5429 0.3686 15 4 3 -1.1736 -3.9941 15 4 4 3.1792 1.2851 15 4 5 -6.9853 -2.7653 15 4 10 -3.4432 -0.4341 15 4 11 3.3241 3.1503 15 5 0 -1.3829 0.0000 15 5 1 2.6982 -1.4207 15 5 2 2.5322 -5.0612 15 5 3 -7.1040 0.9713 15 5 4 1.9194 0.6650 15 5 5 0.1021 -2.3874 15 5 6 -6.4117 -4.7444 15 5 7 -4.7373 -4.5445 15 5 8 -2.1322 -1.0800 15 5 9 6.8251 -2.2539 15 6 0 -7.6532 0.0000 15 6 1 2.5887 4.3911 15 6 2 0.6137 -2.7996 15 6 3 0.1579 0.5809 15 6 4 1.5879 0.9910 15 6 5 -0.7109 2.5585 15 6 6 3.8223 -2.7967 15 6 7 6.6785 1.0417 15 7 0 2.7895 0.0000 15 7 1 -0.5615 3.2361 15 7 2 -3.1614 -0.8080 15 7 3 -4.5520 3.2329 16 0 0 5.8694 0.0000 16 0 1 -0.0000 -0.9596 16 0 2 2.9296 0.0000 16 0 3 0.0000 2.7310 16 0 4 1.6743 0.0000 16 0 5 0.0000 2.0123 16 0 6 10.1226 0.0000 16 0 7 -0.0000 -3.2280 16 0 8 -1.6484 0.0000 16 1 0 0.7458 -0.0000 16 1 1 -1.5479 0.6856 16 1 2 -2.7989 -3.0414 16 1 3 1.4027 6.5082 16 1 4 -2.7887 -2.3908 16 1 5 3.2877 0.3963 16 1 6 -0.8723 4.5070 16 1 7 0.3056 3.3613 16 1 8 -5.3490 7.0684 16 2 0 -3.1444 0.0000 16 2 1 1.9033 1.1032 16 2 2 -8.3216 -2.0733 16 2 3 -1.8811 2.2037 16 2 5 8.6597 4.0018 16 3 0 -17.1410 0.0000 16 3 1 -0.4071 -2.5919 16 4 0 3.6543 -0.0000 16 4 1 -0.8322 3.8275 16 4 2 0.9770 -0.3315 0 0 0 0.0 0.0 ; _shelx_fab_checksum 80264 _olex2_submission_special_instructions 'No special instructions were received' #END data_MOF520_2.82GPa _chemical_name_common 'MOF-520_2.82 GPa' _chemical_name_systematic ? _chemical_formula_moiety 'C28 H18 Al2 O10' _chemical_formula_sum 'C28 H18 Al2 O10' _chemical_formula_weight 568.38 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0310 0.0240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 94 _space_group_name_H-M_alt 'P 42 21 2' _space_group_name_Hall 'P 4n 2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/2' '-x, -y, z' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 19.070(3) _cell_length_b 19.070(3) _cell_length_c 36.409(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13241(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4008 _cell_measurement_theta_max 15.03 _cell_measurement_theta_min 2.16 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.566 _exptl_crystal_F_000 2336 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_absorpt_coefficient_mu 0.029 _shelx_estimated_absorpt_T_max 0.7439 _shelx_estimated_absorpt_T_min 0.5539 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 0.7439 _exptl_absorpt_correction_T_min 0.5539 _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1229 before and 0.0720 after correction. The Ratio of minimum to maximum transmission is 0.7446. The \l/2 correction factor is Not present. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.49594 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 12.2.2 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Perkin Elmer CMOS' _diffrn_measurement_method '\w 80 degrees scan' _diffrn_detector_area_resol_mean ? _exptl_absorpt_special_details ; Data was collected in a Merril Bassett DAC. DAC opening angle of 40 degrees. The pressure of 2.82 GPa was measured via ruby method. The sample was collected by rotating 80 degrees. The data sets were merged in XPREP to produce the final data set. ; _diffrn_reflns_number 19178 _diffrn_reflns_av_R_equivalents 0.1082 _diffrn_reflns_av_unetI/netI 0.1327 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_theta_full 15.130 _diffrn_reflns_theta_max 15.130 _diffrn_reflns_theta_min 0.841 _diffrn_measured_fraction_theta_full 0.908 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_Laue_measured_fraction_full 0.908 _diffrn_reflns_Laue_measured_fraction_max 0.908 _diffrn_reflns_point_group_measured_fraction_full 0.870 _diffrn_reflns_point_group_measured_fraction_max 0.870 _reflns_number_total 7050 _reflns_number_gt 3723 _diffrn_standards_number 0 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.677 _reflns_Friedel_fraction_full 0.820 _reflns_Friedel_fraction_max 0.820 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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_cell_refinement 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_data_collection 'Bruker APEX2 Bruker-AXS, Madison WI' _computing_data_reduction 'SAINT V8.34A Bruker-AXS, Madison WI' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015)' _refine_diff_density_max 0.155 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.029 _refine_ls_abs_structure_details ; Flack x determined using 1092 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.4(5) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 7050 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0495 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.1272 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All O(H) groups 2. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Aromatic/amide H refined with riding coordinates: O2(H2), O1(H1), C26(H26), C23(H23), C25(H25), C22(H22), C7(H7), C16(H16), C18(H18), C6(H6), C13(H13), C19(H19), C15(H15), C9(H9), C28(H28), C3(H3), C4(H4), C11(H11) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.66529(9) 0.33471(9) 0.5000 0.0506(7) Uani 1 2 d S TU P . . Al2 Al 0.61778(10) 0.38823(9) 0.41744(5) 0.0562(5) Uani 1 1 d . U . . . Al3 Al 0.5000 0.5000 0.38505(7) 0.0531(7) Uani 1 2 d S TU P . . O2 O 0.56717(17) 0.47078(17) 0.41908(10) 0.0507(11) Uani 1 1 d . U . . . H2 H 0.5760 0.5006 0.4387 0.061 Uiso 1 1 calc R . . . . O3 O 0.6421(2) 0.39961(19) 0.36619(11) 0.0629(12) Uani 1 1 d . U . . . O1 O 0.60090(18) 0.36373(17) 0.46566(9) 0.0504(11) Uani 1 1 d . U . . . H1 H 0.5545 0.3664 0.4735 0.060 Uiso 1 1 calc R . . . . O4 O 0.5574(2) 0.4736(2) 0.34612(11) 0.0684(13) Uani 1 1 d . U . . . C1 C 0.6107(4) 0.4354(3) 0.3403(2) 0.0601(18) Uani 1 1 d . U . . . C26 C 0.7639(4) 0.6311(4) 0.1416(2) 0.093(2) Uani 1 1 d . U . . . H26 H 0.7652 0.6291 0.1671 0.111 Uiso 1 1 calc R . . . . C23 C 0.7729(3) 0.6332(4) 0.0641(2) 0.080(2) Uani 1 1 d . U . . . H23 H 0.7729 0.6373 0.0387 0.096 Uiso 1 1 calc R . . . . C20 C 0.9763(4) 0.1486(4) 0.10999(17) 0.0634(19) Uani 1 1 d . U . . . C25 C 0.7683(4) 0.6926(4) 0.1227(2) 0.101(3) Uani 1 1 d . U . . . H25 H 0.7648 0.7353 0.1350 0.121 Uiso 1 1 calc R . . . . C22 C 0.7677(4) 0.5629(4) 0.0826(2) 0.103(3) Uani 1 1 d . U . . . H22 H 0.7720 0.5207 0.0700 0.123 Uiso 1 1 calc R . . . . C24 C 0.7779(4) 0.6909(4) 0.0863(2) 0.079(2) Uani 1 1 d . U . . . C27 C 0.7990(3) 0.7622(3) 0.0642(2) 0.062(2) Uani 1 1 d . U . . . C17 C 0.9296(4) 0.2077(3) 0.11955(19) 0.071(2) Uani 1 1 d . U . . . C7 C 0.6052(4) 0.4702(4) 0.2767(2) 0.124(3) Uani 1 1 d . U . . . H7 H 0.5633 0.4944 0.2798 0.148 Uiso 1 1 calc R . . . . C21 C 0.7566(3) 0.5660(4) 0.1177(2) 0.080(2) Uani 1 1 d . U . . . C16 C 0.8683(4) 0.1977(3) 0.1373(2) 0.092(3) Uani 1 1 d . U . . . H16 H 0.8555 0.1525 0.1442 0.110 Uiso 1 1 calc R . . . . C2 C 0.6419(4) 0.4317(4) 0.3087(2) 0.094(3) Uani 1 1 d . U . . . C18 C 0.9461(4) 0.2772(4) 0.1075(2) 0.118(3) Uani 1 1 d . U . . . H18 H 0.9858 0.2860 0.0934 0.142 Uiso 1 1 calc R . . . . C14 C 0.8369(4) 0.3193(4) 0.13381(19) 0.077(2) Uani 1 1 d . U . . . C6 C 0.6387(4) 0.4664(4) 0.2433(2) 0.115(3) Uani 1 1 d . U . . . H6 H 0.6191 0.4944 0.2250 0.138 Uiso 1 1 calc R . . . . C13 C 0.7189(4) 0.4942(4) 0.17253(19) 0.080(2) Uani 1 1 d . U . . . H13 H 0.6918 0.5318 0.1805 0.095 Uiso 1 1 calc R . . . . C19 C 0.8986(4) 0.3336(4) 0.1178(2) 0.084(2) Uani 1 1 d . U . . . H19 H 0.9112 0.3800 0.1133 0.100 Uiso 1 1 calc R . . . . C10 C 0.7983(3) 0.3798(4) 0.1518(2) 0.074(2) Uani 1 1 d . U . . . C15 C 0.8245(4) 0.2520(4) 0.14526(18) 0.084(2) Uani 1 1 d . U . . . H15 H 0.7845 0.2431 0.1591 0.101 Uiso 1 1 calc R . . . . C12 C 0.7513(4) 0.4960(4) 0.1414(2) 0.089(2) Uani 1 1 d . U . . . C9 C 0.7650(4) 0.3761(3) 0.1835(2) 0.078(2) Uani 1 1 d . U . . . H9 H 0.7680 0.3360 0.1979 0.094 Uiso 1 1 calc R . . . . O8 O 0.8243(2) 0.8060(2) 0.08836(11) 0.0643(12) Uani 1 1 d . U . . . O10 O 0.73470(19) 0.3971(2) 0.48285(12) 0.0596(12) Uani 1 1 d . U . . . O5 O 1.0411(2) 0.16666(19) 0.09772(11) 0.0693(14) Uani 1 1 d . U . . . O6 O 0.95687(19) 0.08848(19) 0.11815(11) 0.0546(12) Uani 1 1 d . U . . . O7 O 0.8006(2) 0.76400(19) 0.03269(13) 0.0585(13) Uani 1 1 d . U . . . O9 O 0.6987(2) 0.4404(2) 0.42826(12) 0.0680(13) Uani 1 1 d . U . . . C28 C 0.7430(4) 0.4415(4) 0.4567(2) 0.081(2) Uani 1 1 d . U . . . H28 H 0.7793 0.4740 0.4575 0.097 Uiso 1 1 calc R . . . . C5 C 0.6910(4) 0.4317(4) 0.2332(2) 0.088(2) Uani 1 1 d . U . . . C8 C 0.7265(4) 0.4316(4) 0.1945(2) 0.092(3) Uani 1 1 d . U . . . C3 C 0.7012(4) 0.3952(4) 0.3003(2) 0.119(3) Uani 1 1 d . U . . . H3 H 0.7261 0.3722 0.3187 0.142 Uiso 1 1 calc R . . . . C4 C 0.7261(4) 0.3924(4) 0.2615(2) 0.129(4) Uani 1 1 d . U . . . H4 H 0.7648 0.3649 0.2555 0.155 Uiso 1 1 calc R . . . . C11 C 0.7922(3) 0.4407(3) 0.13010(19) 0.081(2) Uani 1 1 d . U . . . H11 H 0.8160 0.4435 0.1079 0.097 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0586(10) 0.0586(10) 0.035(2) -0.0052(10) -0.0052(10) 0.0031(13) Al2 0.0682(14) 0.0563(13) 0.0443(14) -0.0006(10) -0.0003(10) 0.0089(10) Al3 0.0632(19) 0.0599(18) 0.036(2) 0.000 0.000 0.0096(13) O2 0.060(3) 0.060(3) 0.032(3) -0.0049(18) -0.0016(18) 0.0064(19) O3 0.094(3) 0.056(3) 0.039(3) 0.002(2) 0.009(2) 0.009(2) O1 0.050(2) 0.069(3) 0.032(3) 0.0083(18) -0.0075(17) -0.0037(19) O4 0.095(3) 0.072(3) 0.038(3) 0.016(2) 0.007(2) 0.020(3) C1 0.088(5) 0.054(4) 0.038(5) 0.008(3) 0.015(3) 0.004(4) C26 0.149(7) 0.080(5) 0.049(6) 0.025(4) 0.016(4) 0.004(4) C23 0.101(6) 0.084(5) 0.056(5) 0.008(4) 0.014(4) -0.021(4) C20 0.100(5) 0.059(4) 0.032(5) -0.008(3) 0.011(4) 0.016(4) C25 0.162(8) 0.083(5) 0.058(6) 0.013(4) 0.012(5) -0.010(5) C22 0.147(7) 0.082(5) 0.079(6) 0.024(4) 0.034(5) -0.015(4) C24 0.098(5) 0.080(5) 0.060(5) 0.016(4) 0.003(4) -0.014(4) C27 0.079(5) 0.061(4) 0.045(5) 0.016(4) 0.000(4) -0.010(3) C17 0.096(5) 0.050(4) 0.066(6) 0.004(3) 0.031(4) 0.005(3) C7 0.142(7) 0.176(8) 0.052(6) 0.048(5) 0.031(5) 0.095(6) C21 0.090(5) 0.071(5) 0.079(6) 0.022(4) 0.022(4) 0.002(4) C16 0.114(6) 0.053(5) 0.109(7) 0.000(4) 0.047(5) 0.002(4) C2 0.124(6) 0.102(6) 0.058(5) 0.028(4) 0.021(4) 0.062(5) C18 0.131(6) 0.066(5) 0.157(9) 0.020(5) 0.073(6) 0.012(4) C14 0.102(5) 0.064(4) 0.065(6) -0.003(4) 0.016(4) 0.006(4) C6 0.144(7) 0.143(7) 0.059(6) 0.039(5) 0.027(5) 0.085(6) C13 0.097(6) 0.078(5) 0.064(6) 0.008(4) 0.031(4) 0.006(4) C19 0.101(5) 0.064(4) 0.085(6) 0.003(4) 0.031(4) 0.007(4) C10 0.084(5) 0.068(4) 0.070(6) 0.012(4) 0.025(4) 0.000(3) C15 0.106(6) 0.064(5) 0.083(7) 0.008(4) 0.039(4) 0.001(4) C12 0.112(6) 0.077(5) 0.077(6) 0.009(4) 0.031(4) 0.011(4) C9 0.104(6) 0.062(5) 0.070(6) 0.013(4) 0.032(4) 0.007(4) O8 0.081(3) 0.074(3) 0.038(3) 0.017(2) 0.000(2) -0.020(2) O10 0.055(3) 0.065(3) 0.058(4) -0.007(2) -0.002(2) -0.006(2) O5 0.098(3) 0.041(3) 0.069(4) -0.007(2) 0.035(3) 0.009(2) O6 0.077(3) 0.042(3) 0.045(3) -0.004(2) 0.018(2) 0.012(2) O7 0.084(3) 0.052(3) 0.039(3) 0.010(2) -0.009(2) -0.012(2) O9 0.076(3) 0.066(3) 0.063(4) -0.003(2) 0.002(2) -0.003(2) C28 0.078(5) 0.093(6) 0.071(6) 0.010(4) -0.004(4) -0.017(4) C5 0.118(6) 0.078(5) 0.067(6) 0.016(4) 0.023(4) 0.033(4) C8 0.126(6) 0.072(5) 0.078(6) 0.017(4) 0.032(4) 0.022(4) C3 0.143(7) 0.125(7) 0.088(7) 0.036(5) 0.037(5) 0.069(6) C4 0.142(7) 0.157(8) 0.088(7) 0.046(5) 0.040(5) 0.090(6) C11 0.098(5) 0.069(5) 0.076(6) 0.013(4) 0.038(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.838(4) . ? Al1 O1 1.838(4) 8_666 ? Al1 O10 1.886(4) . ? Al1 O10 1.886(4) 8_666 ? Al1 O7 1.913(4) 6_645 ? Al1 O7 1.913(4) 2_645 ? Al2 O2 1.847(4) . ? Al2 O3 1.935(4) . ? Al2 O1 1.845(4) . ? Al2 O8 1.931(4) 6_645 ? Al2 O5 1.881(4) 5_455 ? Al2 O9 1.879(5) . ? Al3 O2 1.867(4) 3_665 ? Al3 O2 1.867(4) . ? Al3 O4 1.861(4) . ? Al3 O4 1.861(4) 3_665 ? Al3 O6 1.881(3) 6_655 ? Al3 O6 1.881(3) 5_455 ? O3 C1 1.308(7) . ? O4 C1 1.267(7) . ? C1 C2 1.299(9) . ? C26 C25 1.362(8) . ? C26 C21 1.521(10) . ? C23 C22 1.504(9) . ? C23 C24 1.369(9) . ? C20 C17 1.478(8) . ? C20 O5 1.358(7) . ? C20 O6 1.241(7) . ? C25 C24 1.337(9) . ? C22 C21 1.297(9) . ? C24 C27 1.631(9) . ? C27 O8 1.304(8) . ? C27 O7 1.149(7) . ? C17 C16 1.350(8) . ? C17 C18 1.431(8) . ? C7 C2 1.544(9) . ? C7 C6 1.377(9) . ? C21 C12 1.593(9) . ? C16 C15 1.362(8) . ? C2 C3 1.363(9) . ? C18 C19 1.456(9) . ? C14 C19 1.342(8) . ? C14 C10 1.517(9) . ? C14 C15 1.370(8) . ? C6 C5 1.252(8) . ? C13 C12 1.292(8) . ? C13 C8 1.445(9) . ? C10 C9 1.318(8) . ? C10 C11 1.409(8) . ? C12 C11 1.373(8) . ? C9 C8 1.349(8) . ? O8 Al2 1.931(4) 6_655 ? O10 C28 1.285(7) . ? O5 Al2 1.881(4) 5 ? O6 Al3 1.881(3) 5 ? O7 Al1 1.913(4) 4_564 ? O9 C28 1.335(7) . ? C5 C8 1.563(9) . ? C5 C4 1.440(10) . ? C3 C4 1.491(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O1 93.5(2) . 8_666 ? O1 Al1 O10 90.86(17) 8_666 . ? O1 Al1 O10 93.08(17) 8_666 8_666 ? O1 Al1 O10 93.08(17) . . ? O1 Al1 O10 90.86(17) . 8_666 ? O1 Al1 O7 90.94(17) . 6_645 ? O1 Al1 O7 90.94(17) 8_666 2_645 ? O1 Al1 O7 175.5(2) . 2_645 ? O1 Al1 O7 175.5(2) 8_666 6_645 ? O10 Al1 O10 174.2(3) . 8_666 ? O10 Al1 O7 85.75(18) . 2_645 ? O10 Al1 O7 85.75(18) 8_666 6_645 ? O10 Al1 O7 90.00(18) 8_666 2_645 ? O10 Al1 O7 90.00(18) . 6_645 ? O7 Al1 O7 84.7(3) 6_645 2_645 ? O2 Al2 O3 93.49(18) . . ? O2 Al2 O8 174.3(2) . 6_645 ? O2 Al2 O5 94.44(18) . 5_455 ? O2 Al2 O9 88.34(17) . . ? O1 Al2 O2 95.38(17) . . ? O1 Al2 O3 171.06(17) . . ? O1 Al2 O8 89.90(18) . 6_645 ? O1 Al2 O5 90.15(18) . 5_455 ? O1 Al2 O9 94.48(19) . . ? O8 Al2 O3 81.28(18) 6_645 . ? O5 Al2 O3 88.04(19) 5_455 . ? O5 Al2 O8 87.76(19) 5_455 6_645 ? O9 Al2 O3 86.90(19) . . ? O9 Al2 O8 89.03(19) . 6_645 ? O9 Al2 O5 174.4(2) . 5_455 ? O2 Al3 O2 96.9(3) . 3_665 ? O2 Al3 O6 94.21(16) . 5_455 ? O2 Al3 O6 90.50(16) 3_665 5_455 ? O2 Al3 O6 90.50(16) . 6_655 ? O2 Al3 O6 94.20(16) 3_665 6_655 ? O4 Al3 O2 171.9(2) . 3_665 ? O4 Al3 O2 91.20(17) 3_665 3_665 ? O4 Al3 O2 91.19(17) . . ? O4 Al3 O2 171.9(2) 3_665 . ? O4 Al3 O4 80.8(3) . 3_665 ? O4 Al3 O6 86.45(18) . 6_655 ? O4 Al3 O6 86.45(18) 3_665 5_455 ? O4 Al3 O6 88.15(18) 3_665 6_655 ? O4 Al3 O6 88.15(18) . 5_455 ? O6 Al3 O6 172.9(3) 5_455 6_655 ? Al2 O2 Al3 126.2(2) . . ? C1 O3 Al2 130.0(4) . . ? Al1 O1 Al2 127.4(2) . . ? C1 O4 Al3 138.9(4) . . ? O4 C1 O3 123.2(6) . . ? O4 C1 C2 123.1(7) . . ? C2 C1 O3 113.6(7) . . ? C25 C26 C21 114.8(7) . . ? C24 C23 C22 117.2(7) . . ? O5 C20 C17 115.6(6) . . ? O6 C20 C17 117.9(6) . . ? O6 C20 O5 125.8(6) . . ? C24 C25 C26 119.2(8) . . ? C21 C22 C23 114.2(7) . . ? C23 C24 C27 113.3(8) . . ? C25 C24 C23 126.5(7) . . ? C25 C24 C27 120.2(7) . . ? O8 C27 C24 106.9(7) . . ? O7 C27 C24 121.6(7) . . ? O7 C27 O8 130.2(6) . . ? C16 C17 C20 121.8(6) . . ? C16 C17 C18 118.0(6) . . ? C18 C17 C20 120.1(6) . . ? C6 C7 C2 115.6(7) . . ? C26 C21 C12 112.5(7) . . ? C22 C21 C26 125.9(7) . . ? C22 C21 C12 120.2(7) . . ? C17 C16 C15 121.7(7) . . ? C1 C2 C7 115.8(7) . . ? C1 C2 C3 127.3(8) . . ? C3 C2 C7 116.8(7) . . ? C17 C18 C19 118.0(6) . . ? C19 C14 C10 117.3(6) . . ? C19 C14 C15 118.3(7) . . ? C15 C14 C10 119.8(7) . . ? C5 C6 C7 131.0(8) . . ? C12 C13 C8 117.3(7) . . ? C14 C19 C18 120.5(7) . . ? C9 C10 C14 124.7(7) . . ? C9 C10 C11 119.7(7) . . ? C11 C10 C14 115.1(7) . . ? C16 C15 C14 122.8(7) . . ? C13 C12 C21 121.7(7) . . ? C13 C12 C11 120.9(7) . . ? C11 C12 C21 116.5(7) . . ? C10 C9 C8 118.7(7) . . ? C27 O8 Al2 131.1(4) . 6_655 ? C28 O10 Al1 138.4(5) . . ? C20 O5 Al2 131.5(4) . 5 ? C20 O6 Al3 133.1(4) . 5 ? C27 O7 Al1 130.6(4) . 4_564 ? C28 O9 Al2 133.7(5) . . ? O10 C28 O9 119.1(7) . . ? C6 C5 C8 127.6(7) . . ? C6 C5 C4 115.8(8) . . ? C4 C5 C8 116.4(7) . . ? C13 C8 C5 117.0(6) . . ? C9 C8 C13 122.6(7) . . ? C9 C8 C5 120.3(7) . . ? C2 C3 C4 119.6(7) . . ? C5 C4 C3 120.8(7) . . ? C12 C11 C10 120.8(7) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.085 -0.806 -0.999 9441.1 11252.0 ? _shelx_res_file ; p6_25kev_0m.res created by SHELXL-2014/7 TITL P6_25kev_0m in P42212 #94 REM reset to P42212 #94 CELL 0.49594 19.07 19.07 36.4087 90 90 90 ZERR 218 0.0027 0.0027 0.00728 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.5+Z SYMM -X,-Y,+Z SYMM 0.5+Y,0.5-X,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC C H O Al DISP Al 0.031 0.024 81.761 DISP C 0.001 0.001 6.243 DISP H -0 0 0.608 DISP O 0.004 0.003 13.948 UNIT 218 218 218 218 RIGU L.S. 14 PLAN 20 TEMP 23 BOND acta ABIN fmap 2 REM REM REM WGHT 0.049000 FVAR 0.10016 AL1 4 0.665287 0.334713 0.500000 10.50000 0.05864 0.05864 = 0.03452 -0.00518 -0.00518 0.00313 AL2 4 0.617782 0.388230 0.417438 11.00000 0.06817 0.05628 = 0.04426 -0.00064 -0.00033 0.00891 AL3 4 0.500000 0.500000 0.385051 10.50000 0.06323 0.05989 = 0.03604 0.00000 0.00000 0.00960 O2 3 0.567171 0.470776 0.419081 11.00000 0.06001 0.05972 = 0.03231 -0.00494 -0.00159 0.00643 AFIX 43 H2 2 0.575995 0.500635 0.438741 11.00000 -1.20000 AFIX 0 O3 3 0.642096 0.399610 0.366186 11.00000 0.09404 0.05587 = 0.03885 0.00204 0.00905 0.00858 O1 3 0.600897 0.363731 0.465656 11.00000 0.04963 0.06930 = 0.03229 0.00826 -0.00748 -0.00367 AFIX 43 H1 2 0.554542 0.366364 0.473469 11.00000 -1.20000 AFIX 0 O4 3 0.557440 0.473605 0.346123 11.00000 0.09527 0.07152 = 0.03841 0.01595 0.00719 0.02047 C1 1 0.610679 0.435442 0.340342 11.00000 0.08850 0.05441 = 0.03754 0.00795 0.01518 0.00381 C26 1 0.763861 0.631128 0.141599 11.00000 0.14893 0.07990 = 0.04882 0.02479 0.01600 0.00393 AFIX 43 H26 2 0.765173 0.629087 0.167111 11.00000 -1.20000 AFIX 0 C23 1 0.772942 0.633198 0.064147 11.00000 0.10059 0.08351 = 0.05594 0.00795 0.01434 -0.02096 AFIX 43 H23 2 0.772860 0.637280 0.038693 11.00000 -1.20000 AFIX 0 C20 1 0.976331 0.148593 0.109990 11.00000 0.09964 0.05905 = 0.03155 -0.00770 0.01061 0.01555 C25 1 0.768322 0.692642 0.122709 11.00000 0.16223 0.08311 = 0.05787 0.01321 0.01199 -0.00964 AFIX 43 H25 2 0.764774 0.735285 0.134962 11.00000 -1.20000 AFIX 0 C22 1 0.767671 0.562869 0.082647 11.00000 0.14687 0.08188 = 0.07928 0.02358 0.03422 -0.01509 AFIX 43 H22 2 0.772000 0.520722 0.069998 11.00000 -1.20000 AFIX 0 C24 1 0.777865 0.690944 0.086332 11.00000 0.09834 0.08006 = 0.05965 0.01578 0.00257 -0.01357 C27 1 0.798968 0.762244 0.064208 11.00000 0.07876 0.06132 = 0.04514 0.01571 0.00029 -0.01036 C17 1 0.929625 0.207723 0.119547 11.00000 0.09608 0.05046 = 0.06607 0.00441 0.03064 0.00536 C7 1 0.605240 0.470203 0.276706 11.00000 0.14209 0.17616 = 0.05232 0.04786 0.03110 0.09464 AFIX 43 H7 2 0.563310 0.494381 0.279832 11.00000 -1.20000 AFIX 0 C21 1 0.756571 0.566048 0.117748 11.00000 0.08965 0.07128 = 0.07869 0.02151 0.02224 0.00197 C16 1 0.868256 0.197655 0.137250 11.00000 0.11378 0.05334 = 0.10871 -0.00045 0.04709 0.00157 AFIX 43 H16 2 0.855519 0.152463 0.144154 11.00000 -1.20000 AFIX 0 C2 1 0.641866 0.431675 0.308676 11.00000 0.12413 0.10176 = 0.05758 0.02762 0.02056 0.06223 C18 1 0.946073 0.277178 0.107459 11.00000 0.13128 0.06615 = 0.15695 0.02044 0.07283 0.01195 AFIX 43 H18 2 0.985837 0.285996 0.093411 11.00000 -1.20000 AFIX 0 C14 1 0.836897 0.319335 0.133810 11.00000 0.10235 0.06391 = 0.06538 -0.00314 0.01610 0.00587 C6 1 0.638706 0.466432 0.243261 11.00000 0.14377 0.14274 = 0.05895 0.03909 0.02653 0.08496 AFIX 43 H6 2 0.619105 0.494439 0.225044 11.00000 -1.20000 AFIX 0 C13 1 0.718924 0.494228 0.172529 11.00000 0.09725 0.07765 = 0.06362 0.00828 0.03075 0.00571 AFIX 43 H13 2 0.691821 0.531805 0.180503 11.00000 -1.20000 AFIX 0 C19 1 0.898645 0.333636 0.117826 11.00000 0.10106 0.06438 = 0.08522 0.00289 0.03060 0.00704 AFIX 43 H19 2 0.911250 0.379960 0.113334 11.00000 -1.20000 AFIX 0 C10 1 0.798300 0.379845 0.151797 11.00000 0.08421 0.06802 = 0.07032 0.01229 0.02485 -0.00027 C15 1 0.824498 0.252017 0.145262 11.00000 0.10590 0.06368 = 0.08341 0.00786 0.03910 0.00060 AFIX 43 H15 2 0.784495 0.243053 0.159097 11.00000 -1.20000 AFIX 0 C12 1 0.751320 0.495966 0.141375 11.00000 0.11192 0.07663 = 0.07723 0.00948 0.03122 0.01126 C9 1 0.765019 0.376098 0.183456 11.00000 0.10357 0.06170 = 0.06951 0.01277 0.03168 0.00742 AFIX 43 H9 2 0.768031 0.336008 0.197914 11.00000 -1.20000 AFIX 0 O8 3 0.824267 0.805963 0.088362 11.00000 0.08072 0.07390 = 0.03825 0.01713 -0.00036 -0.02018 O10 3 0.734704 0.397114 0.482853 11.00000 0.05480 0.06546 = 0.05849 -0.00744 -0.00198 -0.00556 O5 3 1.041083 0.166658 0.097723 11.00000 0.09774 0.04140 = 0.06868 -0.00694 0.03450 0.00853 O6 3 0.956866 0.088482 0.118147 11.00000 0.07694 0.04170 = 0.04510 -0.00393 0.01797 0.01191 O7 3 0.800569 0.764000 0.032688 11.00000 0.08393 0.05225 = 0.03933 0.00988 -0.00867 -0.01181 O9 3 0.698746 0.440427 0.428260 11.00000 0.07595 0.06555 = 0.06256 -0.00280 0.00206 -0.00267 C28 1 0.742996 0.441533 0.456664 11.00000 0.07840 0.09330 = 0.07085 0.01042 -0.00368 -0.01747 AFIX 43 H28 2 0.779339 0.474014 0.457491 11.00000 -1.20000 AFIX 0 C5 1 0.691034 0.431735 0.233172 11.00000 0.11772 0.07843 = 0.06674 0.01609 0.02297 0.03341 C8 1 0.726487 0.431581 0.194479 11.00000 0.12614 0.07173 = 0.07808 0.01665 0.03224 0.02226 C3 1 0.701234 0.395222 0.300318 11.00000 0.14296 0.12536 = 0.08777 0.03650 0.03657 0.06881 AFIX 43 H3 2 0.726081 0.372231 0.318705 11.00000 -1.20000 AFIX 0 C4 1 0.726108 0.392422 0.261518 11.00000 0.14237 0.15654 = 0.08845 0.04561 0.03972 0.09050 AFIX 43 H4 2 0.764754 0.364948 0.255547 11.00000 -1.20000 AFIX 0 C11 1 0.792160 0.440711 0.130100 11.00000 0.09824 0.06922 = 0.07566 0.01325 0.03845 0.01502 AFIX 43 H11 2 0.816049 0.443496 0.107879 11.00000 -1.20000 AFIX 0 HKLF 4 REM P6_25kev_0m in P42212 #94 REM R1 = 0.0495 for 3723 Fo > 4sig(Fo) and 0.1022 for all 7050 data REM 362 parameters refined using 336 restraints END WGHT 0.0487 0.0000 REM Highest difference peak 0.155, deepest hole -0.232, 1-sigma level 0.029 Q1 1 0.5000 0.5000 0.4010 10.50000 0.05 0.15 Q2 1 0.6070 0.3767 0.3638 11.00000 0.05 0.14 Q3 1 1.0493 0.1878 0.1109 11.00000 0.05 0.13 Q4 1 0.6572 0.3404 0.5160 11.00000 0.05 0.13 Q5 1 0.6330 0.3350 0.4961 11.00000 0.05 0.13 Q6 1 0.9561 0.1029 0.1050 11.00000 0.05 0.12 Q7 1 0.5618 0.4445 0.3562 11.00000 0.05 0.12 Q8 1 0.9947 0.0919 0.1195 11.00000 0.05 0.12 Q9 1 0.4969 0.4617 0.3814 11.00000 0.05 0.12 Q10 1 0.7980 0.5009 0.4418 11.00000 0.05 0.11 Q11 1 0.8699 0.0408 0.1222 11.00000 0.05 0.11 Q12 1 0.6142 0.3601 0.4108 11.00000 0.05 0.11 Q13 1 0.4976 0.4145 0.4531 11.00000 0.05 0.11 Q14 1 0.5176 0.4799 0.3717 11.00000 0.05 0.11 Q15 1 0.6390 0.4003 0.3866 11.00000 0.05 0.11 Q16 1 0.6842 0.3784 0.3548 11.00000 0.05 0.11 Q17 1 0.7374 0.4207 0.4177 11.00000 0.05 0.10 Q18 1 0.9551 0.0886 0.1368 11.00000 0.05 0.10 Q19 1 0.6072 0.3956 0.4701 11.00000 0.05 0.10 Q20 1 0.8383 0.1230 0.1108 11.00000 0.05 0.10 ; 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6.31 6 -1 10 80.01 6.21 -1 -6 10 79.63 6.32 -1 6 -10 73.79 6.30 2 -6 10 18.43 1.79 -6 2 -10 18.53 1.70 2 6 -10 16.61 1.81 -2 6 -10 19.03 1.84 6 2 -10 19.01 1.70 6 -2 10 18.02 1.63 -2 -6 10 15.67 1.79 -6 -3 10 27.04 2.32 3 -6 10 25.42 2.42 -6 3 -10 28.45 2.28 3 6 -10 26.34 2.45 6 -3 10 24.79 2.39 -3 -6 10 26.52 2.43 -3 6 -10 29.59 2.52 6 3 -10 25.73 2.43 -6 -4 10 -0.80 0.67 4 6 -10 -0.22 0.87 -6 4 -10 0.30 0.70 4 -6 10 0.35 0.87 6 -4 10 -0.97 1.14 -4 6 -10 -0.21 0.74 6 4 -10 -0.57 0.83 -4 -6 10 -0.63 1.02 5 -6 10 24.90 2.31 5 6 -10 25.43 2.34 -6 5 -10 23.08 2.24 -6 -5 10 25.39 2.38 6 5 -10 26.85 2.24 -5 -6 10 26.28 2.60 -5 6 -10 25.30 2.24 6 -5 10 24.96 2.33 6 6 -10 124.68 9.62 -6 -6 10 124.94 9.67 6 -6 10 121.31 9.58 -6 6 -10 117.89 9.52 0 7 -10 23.11 2.46 0 -7 10 31.47 2.66 -7 0 -10 30.54 2.39 1 -7 10 24.07 2.20 -7 1 -10 22.06 1.88 -1 7 -10 17.39 1.86 -1 -7 10 16.94 1.90 7 -1 10 18.41 1.74 2 -7 10 48.73 4.20 -7 2 -10 50.36 4.04 2 7 -10 52.24 4.26 -2 -7 10 48.29 4.17 7 -2 10 50.47 4.04 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5 2 -14 51.55 4.28 3 5 -14 8.24 1.38 3 -5 14 7.73 1.43 -5 3 -14 10.72 1.81 -5 -3 14 9.62 1.55 5 -3 14 7.81 1.72 5 3 -14 10.75 1.75 -3 -5 14 12.37 1.63 -3 5 -14 8.76 1.47 -5 4 -14 44.15 3.83 4 5 -14 47.15 3.87 4 -5 14 52.89 4.20 -5 -4 14 45.64 3.78 5 -4 14 42.85 3.81 5 4 -14 43.46 3.89 -4 5 -14 42.87 3.77 5 5 -14 15.04 1.95 5 -5 14 17.98 2.06 -5 5 -14 18.29 1.82 -5 -5 14 16.02 1.78 0 -6 14 3.44 1.63 -6 0 -14 -0.28 0.78 0 6 -14 2.32 1.00 -6 1 -14 128.18 10.83 1 6 -14 143.99 10.89 -1 -6 14 150.55 11.00 -1 6 -14 133.68 10.90 2 -6 14 51.23 4.46 2 6 -14 56.28 4.39 -6 2 -14 51.11 4.31 6 -2 14 51.89 4.26 -2 6 -14 49.69 4.28 6 2 -14 53.30 4.29 -2 -6 14 48.88 4.41 3 6 -14 9.34 1.47 -6 3 -14 10.27 1.66 -6 -3 14 11.75 1.48 3 -6 14 11.88 1.96 6 -3 14 9.01 1.42 -3 -6 14 10.63 1.78 6 3 -14 11.37 1.59 -3 6 -14 10.11 1.44 -6 4 -14 38.51 3.20 4 -6 14 39.03 3.54 4 6 -14 33.13 3.24 -6 -4 14 37.57 3.24 6 4 -14 37.78 3.35 6 -4 14 36.79 3.28 -4 6 -14 38.56 3.29 -4 -6 14 36.56 3.36 -6 5 -14 22.36 2.25 5 -6 14 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