data_13089-77 _audit_creation_method 'SHELXL-2016/6' _chemical_name_mineral 'strassmannite' _chemical_compound_source 'Green Lizard mine, Utah' _chemical_formula_sum 'Al F H32 O26 S2 U' _chemical_formula_weight 796.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.0187(5) _cell_length_b 8.3284(3) _cell_length_c 26.6727(19) _cell_angle_alpha 90 _cell_angle_beta 97.426(7) _cell_angle_gamma 90 _cell_volume 2427.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.179 _exptl_crystal_F_000 1544 _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 7.006 _shelx_estimated_absorpt_T_min 0.640 _shelx_estimated_absorpt_T_max 0.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 19124 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.076 _diffrn_reflns_theta_max 27.461 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 2739 _reflns_number_gt 2220 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+12.6098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2739 _refine_ls_number_parameters 201 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.371 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U U 0.500000 -0.00640(3) 0.250000 0.02151(9) Uani 1 2 d S T P . . Al Al 0.500000 0.500000 0.500000 0.0279(5) Uani 1 2 d S . P . . S S 0.21223(11) 0.15901(15) 0.28046(5) 0.0245(3) Uani 1 1 d . . . . . O1 O 0.2754(4) 0.2476(5) 0.32301(14) 0.0362(9) Uani 1 1 d . . . . . O2 O 0.1450(4) 0.0225(4) 0.29843(15) 0.0379(9) Uani 1 1 d . . . . . O3 O 0.1267(3) 0.2639(5) 0.24835(13) 0.0330(9) Uani 1 1 d . . . . . O4 O 0.2999(3) 0.0974(5) 0.24697(14) 0.0331(9) Uani 1 1 d . . . . . O5 O 0.5191(3) -0.0072(4) 0.31642(13) 0.0307(8) Uani 1 1 d . . . . . F F 0.5462(4) 0.2904(5) 0.49825(14) 0.0428(9) Uani 0.5 1 d . . P . . OW1 O 0.5462(4) 0.2904(5) 0.49825(14) 0.0428(9) Uani 0.5 1 d D . P . . H1A H 0.542(12) 0.223(10) 0.520(3) 0.051 Uiso 0.5 1 d D U P . . H1B H 0.582(11) 0.248(12) 0.477(3) 0.051 Uiso 0.5 1 d D U P . . OW2 O 0.3439(4) 0.4437(5) 0.46821(15) 0.0374(9) Uani 1 1 d D . . . . H2A H 0.293(5) 0.509(5) 0.457(2) 0.045 Uiso 1 1 d D U . . . H2B H 0.327(5) 0.358(4) 0.459(2) 0.045 Uiso 1 1 d D U . . . OW3 O 0.5548(4) 0.5322(6) 0.43668(14) 0.0423(10) Uani 1 1 d D . . . . H3A H 0.619(4) 0.573(8) 0.433(2) 0.051 Uiso 1 1 d D U . . . H3B H 0.513(5) 0.520(7) 0.4099(15) 0.051 Uiso 1 1 d D U . . . OW4 O 0.500000 0.2897(7) 0.250000 0.0422(14) Uani 1 2 d DS T P . . H4A H 0.438(4) 0.343(7) 0.239(2) 0.051 Uiso 1 1 d D U . . . OW5 O 0.6569(4) 0.1248(6) 0.42960(16) 0.0455(11) Uani 1 1 d D . . . . H5A H 0.603(10) 0.060(13) 0.421(3) 0.055 Uiso 0.5 1 d D U P . . H5B H 0.673(6) 0.169(7) 0.4044(16) 0.055 Uiso 1 1 d D U . . . H5C H 0.628(12) 0.195(9) 0.446(3) 0.055 Uiso 0.5 1 d D U P . . OW6 O 0.7739(5) 0.2809(6) 0.35911(16) 0.0508(12) Uani 1 1 d D . . . . H6A H 0.735(6) 0.335(7) 0.3375(19) 0.061 Uiso 1 1 d D U . . . H6B H 0.806(6) 0.211(6) 0.344(2) 0.061 Uiso 1 1 d D U . . . OW7 O 0.4495(5) -0.0715(6) 0.42719(16) 0.0520(12) Uani 1 1 d D . . . . H7A H 0.511(7) -0.030(16) 0.419(4) 0.062 Uiso 0.5 1 d D U P . . H7B H 0.412(6) -0.112(8) 0.4025(17) 0.062 Uiso 1 1 d D U . . . H7C H 0.445(12) -0.132(11) 0.451(2) 0.062 Uiso 0.5 1 d D U P . . OW8 O 0.2724(4) 0.1678(5) 0.42221(15) 0.0419(10) Uani 1 1 d D . . . . H8A H 0.264(5) 0.198(7) 0.3930(13) 0.050 Uiso 1 1 d D U . . . H8B H 0.325(5) 0.100(7) 0.426(2) 0.050 Uiso 1 1 d D U . . . OW9 O 0.4284(4) 0.5120(5) 0.34688(15) 0.0407(10) Uani 1 1 d D . . . . H9A H 0.482(4) 0.517(7) 0.329(2) 0.049 Uiso 1 1 d D U . . . H9B H 0.388(5) 0.433(6) 0.338(2) 0.049 Uiso 1 1 d D 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 U 0.01681(14) 0.02298(16) 0.02484(14) 0.000 0.00302(9) 0.000 Al 0.0285(11) 0.0301(13) 0.0247(10) -0.0002(9) 0.0022(8) -0.0011(10) S 0.0188(6) 0.0222(7) 0.0325(7) -0.0004(5) 0.0030(5) 0.0006(5) O1 0.037(2) 0.036(2) 0.034(2) -0.0040(17) 0.0012(16) -0.0068(18) O2 0.036(2) 0.032(2) 0.047(2) 0.0054(17) 0.0075(17) -0.0082(18) O3 0.025(2) 0.033(2) 0.041(2) 0.0015(16) 0.0028(16) 0.0099(16) O4 0.0204(19) 0.037(2) 0.042(2) -0.0073(17) 0.0058(15) 0.0043(16) O5 0.0282(19) 0.037(2) 0.0270(18) -0.0005(15) 0.0042(14) -0.0024(17) F 0.046(2) 0.044(2) 0.039(2) 0.0001(17) 0.0067(17) 0.0027(19) OW1 0.046(2) 0.044(2) 0.039(2) 0.0001(17) 0.0067(17) 0.0027(19) OW2 0.035(2) 0.035(2) 0.041(2) -0.0035(19) -0.0029(17) -0.0025(19) OW3 0.036(2) 0.063(3) 0.027(2) -0.001(2) 0.0026(17) -0.012(2) OW4 0.029(3) 0.027(3) 0.068(4) 0.000 -0.003(3) 0.000 OW5 0.043(3) 0.048(3) 0.047(3) 0.002(2) 0.011(2) 0.005(2) OW6 0.062(3) 0.049(3) 0.041(3) -0.003(2) 0.007(2) 0.004(2) OW7 0.065(3) 0.048(3) 0.041(3) 0.008(2) 0.000(2) -0.008(2) OW8 0.045(3) 0.042(3) 0.038(2) 0.0011(19) 0.0032(19) -0.003(2) OW9 0.040(2) 0.050(3) 0.032(2) -0.0066(19) 0.0073(17) -0.012(2) _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 U O5 1.757(3) 2_655 ? U O5 1.757(3) . ? U O4 2.360(3) . ? U O4 2.360(3) 2_655 ? U O3 2.372(4) 4_545 ? U O3 2.372(4) 3_545 ? U OW4 2.466(6) . ? Al F 1.820(4) 5_666 ? Al F 1.820(4) . ? Al OW2 1.877(4) 5_666 ? Al OW2 1.877(4) . ? Al OW3 1.885(4) . ? Al OW3 1.885(4) 5_666 ? S O1 1.454(4) . ? S O2 1.471(4) . ? S O3 1.475(4) . ? S O4 1.489(4) . ? F H1A 0.81(3) . ? F H1B 0.81(3) . ? OW2 H2A 0.80(3) . ? OW2 H2B 0.77(3) . ? OW3 H3A 0.80(3) . ? OW3 H3B 0.80(3) . ? OW4 H4A 0.83(3) . ? OW4 H4A 0.83(3) 2_655 ? OW5 H5A 0.82(3) . ? OW5 H5B 0.81(3) . ? OW5 H5C 0.82(3) . ? OW6 H6A 0.81(3) . ? OW6 H6B 0.81(3) . ? OW7 H7A 0.81(3) . ? OW7 H7B 0.80(3) . ? OW7 H7C 0.81(3) . ? OW8 H8A 0.81(3) . ? OW8 H8B 0.81(3) . ? OW9 H9A 0.81(3) . ? OW9 H9B 0.81(3) . ? 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 O5 U O5 179.5(2) 2_655 . ? O5 U O4 88.70(15) 2_655 . ? O5 U O4 91.47(15) . . ? O5 U O4 91.47(15) 2_655 2_655 ? O5 U O4 88.70(15) . 2_655 ? O4 U O4 137.03(19) . 2_655 ? O5 U O3 91.23(14) 2_655 4_545 ? O5 U O3 88.40(14) . 4_545 ? O4 U O3 75.33(13) . 4_545 ? O4 U O3 147.59(13) 2_655 4_545 ? O5 U O3 88.40(14) 2_655 3_545 ? O5 U O3 91.23(14) . 3_545 ? O4 U O3 147.59(14) . 3_545 ? O4 U O3 75.32(13) 2_655 3_545 ? O3 U O3 72.47(18) 4_545 3_545 ? O5 U OW4 90.23(11) 2_655 . ? O5 U OW4 90.23(11) . . ? O4 U OW4 68.51(9) . . ? O4 U OW4 68.51(9) 2_655 . ? O3 U OW4 143.76(9) 4_545 . ? O3 U OW4 143.76(9) 3_545 . ? F Al F 180.0 5_666 . ? F Al OW2 89.54(19) 5_666 5_666 ? F Al OW2 90.46(19) . 5_666 ? F Al OW2 90.46(19) 5_666 . ? F Al OW2 89.54(19) . . ? OW2 Al OW2 180.0(3) 5_666 . ? F Al OW3 90.54(19) 5_666 . ? F Al OW3 89.45(19) . . ? OW2 Al OW3 89.31(19) 5_666 . ? OW2 Al OW3 90.69(19) . . ? F Al OW3 89.46(19) 5_666 5_666 ? F Al OW3 90.55(19) . 5_666 ? OW2 Al OW3 90.69(19) 5_666 5_666 ? OW2 Al OW3 89.32(19) . 5_666 ? OW3 Al OW3 180.0 . 5_666 ? O1 S O2 110.4(2) . . ? O1 S O3 111.0(2) . . ? O2 S O3 109.6(2) . . ? O1 S O4 111.2(2) . . ? O2 S O4 108.8(2) . . ? O3 S O4 105.7(2) . . ? S O3 U 143.1(2) . 3_455 ? S O4 U 141.4(2) . . ? Al F H1A 127(7) . . ? Al F H1B 127(7) . . ? H1A F H1B 106(5) . . ? Al OW2 H2A 123(4) . . ? Al OW2 H2B 123(4) . . ? H2A OW2 H2B 113(5) . . ? Al OW3 H3A 124(4) . . ? Al OW3 H3B 125(4) . . ? H3A OW3 H3B 111(4) . . ? U OW4 H4A 122(5) . . ? U OW4 H4A 122(5) . 2_655 ? H4A OW4 H4A 116(9) . 2_655 ? H5A OW5 H5B 107(5) . . ? H5A OW5 H5C 108(10) . . ? H5B OW5 H5C 105(5) . . ? H6A OW6 H6B 106(4) . . ? H7A OW7 H7B 108(5) . . ? H7A OW7 H7C 128(10) . . ? H7B OW7 H7C 107(5) . . ? H8A OW8 H8B 109(4) . . ? H9A OW9 H9B 107(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 H1A OW7 0.81(3) 1.88(3) 2.694(6) 174(14) 5_656 OW1 H1B OW5 0.81(3) 1.90(4) 2.706(6) 173(12) . OW2 H2A OW5 0.80(3) 1.86(3) 2.651(6) 169(6) 3_455 OW2 H2B OW8 0.77(3) 1.92(3) 2.675(6) 167(6) . OW3 H3A OW8 0.80(3) 1.92(3) 2.722(6) 179(6) 3 OW3 H3B OW9 0.80(3) 1.82(3) 2.616(6) 173(6) . OW4 H4A O2 0.83(3) 1.96(4) 2.729(6) 153(6) 4 OW5 H5A OW7 0.82(3) 2.04(5) 2.804(7) 156(11) . OW5 H5B OW6 0.81(3) 1.98(3) 2.741(6) 158(7) . OW5 H5C F 0.82(3) 1.92(4) 2.706(6) 159(9) . OW6 H6A O2 0.81(3) 2.06(3) 2.845(6) 164(6) 3 OW6 H6B OW9 0.81(3) 2.13(3) 2.857(7) 149(6) 3_545 OW7 H7A OW5 0.81(3) 2.05(5) 2.804(7) 153(10) . OW7 H7B OW6 0.80(3) 2.00(4) 2.765(7) 159(7) 3_445 OW7 H7C F 0.81(3) 1.89(4) 2.694(6) 171(15) 5_656 OW8 H8A O1 0.81(3) 1.93(3) 2.733(5) 168(6) . OW8 H8B OW7 0.81(3) 1.98(3) 2.781(7) 174(6) . OW9 H9A O2 0.81(3) 2.06(3) 2.858(6) 167(7) 3 OW9 H9B O1 0.81(3) 1.99(3) 2.796(6) 173(6) . _refine_diff_density_max 1.522 _refine_diff_density_min -1.291 _refine_diff_density_rms 0.165 _shelx_res_file ; TITL JM-13089 13089-77.res created by SHELXL-2016/6 at 14:04:25 on 13-Aug-2017 CELL 0.71075 11.01870 8.32837 26.67270 90.00000 97.42600 90.00000 ZERR 4 0.00052 0.00032 0.00187 0.00000 0.00690 0.00000 LATT 7 SYMM -X, +Y, 1/2-Z SFAC H O F S Al U UNIT 128 104 4 8 4 4 L.S. 8 omit -1 9 2 omit -1 9 4 omit -1 9 3 omit 0 10 6 omit 1 1 2 omit -2 10 8 omit 0 10 7 omit -2 10 6 omit -2 10 10 EQIV $6 -x+1, -y, -z+1 HTAB OW1 OW7_$6 HTAB OW1 OW5 EQIV $1 x-1/2, y+1/2, z HTAB OW2 OW5_$1 HTAB OW2 OW8 EQIV $7 x+1/2, y+1/2, z HTAB OW3 OW8_$7 HTAB OW3 OW9 EQIV $8 -x+1/2, y+1/2, -z+1/2 HTAB OW4 O2_$8 HTAB OW5 OW7 HTAB OW5 OW6 HTAB OW5 F HTAB OW6 O2_$7 EQIV $2 x+1/2, y-1/2, z HTAB OW6 OW9_$2 HTAB OW7 OW5 EQIV $9 x-1/2, y-1/2, z HTAB OW7 OW6_$9 HTAB OW7 F_$6 HTAB OW8 O1 HTAB OW8 OW7 HTAB OW9 O2_$7 HTAB OW9 O1 EXYZ F OW1 EADP F OW1 FMAP 2 PLAN 120 HTAB BOND $H ACTA DFIX 0.82 0.03 OW1 H1a OW1 H1b OW2 H2a OW2 H2b OW3 H3a OW3 H3b DFIX 0.82 0.03 OW4 H4a OW5 H5a OW5 H5b OW5 H5c OW6 H6a OW6 H6b DFIX 0.82 0.03 OW7 H7a OW7 H7b OW7 H7c OW8 H8a OW8 H8b OW9 H9a OW9 H9b DFIX 1.30 0.03 H1a H1b H2a H2b H3a H3b H4a H4a H5a H5b H5b H5c DFIX 1.30 0.03 H6a H6b H7a H7b H7b H7c H8a H8b H9a H9b SIZE 0.070 0.060 0.030 WGHT 0.024300 12.609800 FVAR 0.19395 0.50031 U 6 0.500000 -0.006397 0.250000 10.50000 0.01681 0.02298 = 0.02484 0.00000 0.00302 0.00000 AL 5 0.500000 0.500000 0.500000 10.50000 0.02847 0.03010 = 0.02467 -0.00018 0.00220 -0.00113 S 4 0.212227 0.159009 0.280459 11.00000 0.01884 0.02224 = 0.03249 -0.00040 0.00305 0.00064 O1 2 0.275425 0.247602 0.323009 11.00000 0.03707 0.03627 = 0.03423 -0.00397 0.00119 -0.00678 O2 2 0.144973 0.022514 0.298432 11.00000 0.03555 0.03221 = 0.04659 0.00537 0.00749 -0.00817 O3 2 0.126668 0.263877 0.248345 11.00000 0.02474 0.03287 = 0.04101 0.00148 0.00284 0.00992 O4 2 0.299883 0.097400 0.246967 11.00000 0.02038 0.03740 = 0.04205 -0.00731 0.00578 0.00431 O5 2 0.519095 -0.007248 0.316424 11.00000 0.02823 0.03708 = 0.02700 -0.00052 0.00421 -0.00236 F 3 0.546194 0.290442 0.498250 10.50000 0.04615 0.04380 = 0.03874 0.00012 0.00670 0.00266 OW1 2 0.546194 0.290442 0.498250 10.50000 0.04615 0.04380 = 0.03874 0.00012 0.00670 0.00266 H1A 1 0.542377 0.223352 0.520122 10.50000 -1.20000 H1B 1 0.582086 0.247973 0.476997 10.50000 -1.20000 OW2 2 0.343856 0.443716 0.468207 11.00000 0.03454 0.03504 = 0.04064 -0.00350 -0.00289 -0.00253 H2A 1 0.293442 0.508895 0.457461 11.00000 -1.20000 H2B 1 0.327086 0.357842 0.458928 11.00000 -1.20000 OW3 2 0.554827 0.532227 0.436678 11.00000 0.03632 0.06309 = 0.02696 -0.00059 0.00257 -0.01210 H3A 1 0.618670 0.572606 0.432929 11.00000 -1.20000 H3B 1 0.513400 0.519813 0.409854 11.00000 -1.20000 OW4 2 0.500000 0.289734 0.250000 10.50000 0.02885 0.02749 = 0.06774 0.00000 -0.00317 0.00000 H4A 1 0.438287 0.342559 0.238756 11.00000 -1.20000 OW5 2 0.656930 0.124773 0.429604 11.00000 0.04269 0.04812 = 0.04708 0.00242 0.01080 0.00481 H5A 1 0.603021 0.059575 0.420736 10.50000 -1.20000 H5B 1 0.672971 0.169180 0.404368 11.00000 -1.20000 H5C 1 0.628083 0.195162 0.446109 10.50000 -1.20000 OW6 2 0.773883 0.280886 0.359113 11.00000 0.06235 0.04935 = 0.04086 -0.00254 0.00727 0.00406 H6A 1 0.735146 0.335185 0.337463 11.00000 -1.20000 H6B 1 0.805891 0.210674 0.344331 11.00000 -1.20000 OW7 2 0.449518 -0.071477 0.427188 11.00000 0.06479 0.04845 = 0.04083 0.00845 -0.00005 -0.00783 H7A 1 0.510675 -0.029948 0.418900 10.50000 -1.20000 H7B 1 0.412063 -0.111678 0.402516 11.00000 -1.20000 H7C 1 0.444605 -0.132122 0.450741 10.50000 -1.20000 OW8 2 0.272366 0.167774 0.422212 11.00000 0.04473 0.04241 = 0.03807 0.00115 0.00316 -0.00328 H8A 1 0.264040 0.197849 0.393012 11.00000 -1.20000 H8B 1 0.325235 0.100261 0.425778 11.00000 -1.20000 OW9 2 0.428371 0.512043 0.346880 11.00000 0.04012 0.05040 = 0.03234 -0.00661 0.00734 -0.01249 H9A 1 0.482228 0.517449 0.329006 11.00000 -1.20000 H9B 1 0.388171 0.433399 0.338490 11.00000 -1.20000 HKLF 4 REM JM-13089 REM R1 = 0.0343 for 2220 Fo > 4sig(Fo) and 0.0456 for all 2739 data REM 201 parameters refined using 30 restraints END WGHT 0.0243 12.6016 REM Instructions for potential hydrogen bonds HTAB F OW7_$6 HTAB OW1 OW7_$6 HTAB F OW5 HTAB OW1 OW5 HTAB OW2 OW5_$1 HTAB OW2 OW8 HTAB OW3 OW8_$7 HTAB OW3 OW9 HTAB OW4 O2_$8 HTAB OW5 OW7 HTAB OW5 OW6 HTAB OW5 F HTAB OW6 O2_$7 HTAB OW6 OW9_$2 HTAB OW7 OW5 HTAB OW7 OW6_$9 HTAB OW7 F_$6 HTAB OW8 S HTAB OW8 O1 HTAB OW8 OW7 HTAB OW9 O2_$7 HTAB OW9 O1 REM Highest difference peak 1.522, deepest hole -1.291, 1-sigma level 0.165 Q1 1 0.4978 -0.0209 0.2783 11.00000 0.05 1.52 Q2 1 0.5444 0.1005 0.2875 11.00000 0.05 0.97 Q3 1 0.4570 -0.0672 0.2459 11.00000 0.05 0.95 Q4 1 0.3942 0.0232 0.2592 11.00000 0.05 0.93 Q5 1 0.0000 0.2993 0.2500 10.50000 0.05 0.87 Q6 1 0.7117 0.3408 0.2811 11.00000 0.05 0.82 Q7 1 0.4476 -0.0022 0.2928 11.00000 0.05 0.79 Q8 1 0.4436 0.1381 0.2657 11.00000 0.05 0.78 Q9 1 0.5000 0.2027 0.2500 10.50000 0.05 0.74 Q10 1 0.5792 0.0070 0.2968 11.00000 0.05 0.70 Q11 1 0.3622 0.1272 0.2385 11.00000 0.05 0.67 Q12 1 0.0460 0.3683 0.2163 11.00000 0.05 0.63 Q13 1 0.3541 0.0793 0.2316 11.00000 0.05 0.62 Q14 1 0.1415 0.4283 0.2691 11.00000 0.05 0.61 Q15 1 0.0749 0.3273 0.2417 11.00000 0.05 0.61 Q16 1 0.5561 -0.1171 0.2891 11.00000 0.05 0.60 Q17 1 0.0570 0.3528 0.2311 11.00000 0.05 0.57 Q18 1 0.3784 0.3436 0.2166 11.00000 0.05 0.57 Q19 1 0.4464 0.4337 0.2112 11.00000 0.05 0.56 Q20 1 0.5209 -0.0034 0.3410 11.00000 0.05 0.56 Q21 1 0.6190 -0.0512 0.2790 11.00000 0.05 0.56 Q22 1 0.7815 0.3587 0.3036 11.00000 0.05 0.55 Q23 1 0.0447 0.3221 0.2772 11.00000 0.05 0.53 Q24 1 0.5429 0.5268 0.4658 11.00000 0.05 0.53 Q25 1 0.0922 0.2190 0.2528 11.00000 0.05 0.53 Q26 1 0.5649 0.5534 0.4999 11.00000 0.05 0.53 Q27 1 0.5312 -0.0916 0.3069 11.00000 0.05 0.51 Q28 1 0.5068 0.5526 0.5268 11.00000 0.05 0.49 Q29 1 0.6237 -0.0088 0.3173 11.00000 0.05 0.49 Q30 1 0.2264 0.1685 0.3177 11.00000 0.05 0.49 Q31 1 0.0636 0.1794 0.2826 11.00000 0.05 0.48 Q32 1 0.4706 0.3149 0.2279 11.00000 0.05 0.47 Q33 1 0.0000 0.2053 0.2500 10.50000 0.05 0.47 Q34 1 0.5975 0.3838 0.3299 11.00000 0.05 0.47 Q35 1 0.2779 0.1388 0.2302 11.00000 0.05 0.47 Q36 1 0.1977 0.3371 0.2381 11.00000 0.05 0.46 Q37 1 0.2723 -0.0059 0.2207 11.00000 0.05 0.46 Q38 1 0.2053 0.1591 0.2445 11.00000 0.05 0.46 Q39 1 0.4155 0.5220 0.4653 11.00000 0.05 0.46 Q40 1 0.5007 0.0424 0.3174 11.00000 0.05 0.46 Q41 1 0.3847 0.0687 0.2998 11.00000 0.05 0.46 Q42 1 0.2017 0.2489 0.4597 11.00000 0.05 0.45 Q43 1 0.1395 0.3447 0.2654 11.00000 0.05 0.44 Q44 1 0.5280 0.0396 0.2518 11.00000 0.05 0.43 Q45 1 0.4178 0.4140 0.4723 11.00000 0.05 0.43 Q46 1 0.1538 0.2499 0.2670 11.00000 0.05 0.42 Q47 1 0.3029 0.1628 0.2582 11.00000 0.05 0.41 Q48 1 0.4412 0.5771 0.4602 11.00000 0.05 0.41 Q49 1 0.5482 0.2989 0.5228 11.00000 0.05 0.41 Q50 1 0.4282 0.5611 0.5000 11.00000 0.05 0.41 Q51 1 0.3218 0.4489 0.5139 11.00000 0.05 0.41 Q52 1 0.3384 0.3975 0.4877 11.00000 0.05 0.41 Q53 1 0.6400 0.2569 0.5004 11.00000 0.05 0.40 Q54 1 0.4743 0.1734 0.4821 11.00000 0.05 0.40 Q55 1 0.3794 0.3689 0.2903 11.00000 0.05 0.40 Q56 1 0.3354 0.4726 0.4147 11.00000 0.05 0.39 Q57 1 0.1626 0.2648 0.2422 11.00000 0.05 0.39 Q58 1 0.5498 0.3280 0.4799 11.00000 0.05 0.39 Q59 1 0.3290 0.2751 0.2861 11.00000 0.05 0.39 Q60 1 0.3860 0.4947 0.4985 11.00000 0.05 0.38 Q61 1 0.4005 0.2069 0.2010 11.00000 0.05 0.38 Q62 1 0.4407 0.2948 0.2504 11.00000 0.05 0.38 Q63 1 0.4462 -0.0680 0.4573 11.00000 0.05 0.38 Q64 1 0.1504 0.0690 0.3210 11.00000 0.05 0.38 Q65 1 0.3168 0.1787 0.3346 11.00000 0.05 0.38 Q66 1 0.0845 0.0685 0.2974 11.00000 0.05 0.38 Q67 1 0.4639 0.0753 0.4233 11.00000 0.05 0.37 Q68 1 0.6391 -0.0220 0.3450 11.00000 0.05 0.37 Q69 1 0.2611 0.3772 0.2875 11.00000 0.05 0.36 Q70 1 0.1986 -0.0439 0.3010 11.00000 0.05 0.36 Q71 1 0.4460 -0.1247 0.4062 11.00000 0.05 0.36 Q72 1 0.5397 -0.0984 0.4691 11.00000 0.05 0.36 Q73 1 0.2613 0.2702 0.2439 11.00000 0.05 0.36 Q74 1 0.5673 -0.1198 0.4204 11.00000 0.05 0.36 Q75 1 0.3359 -0.0218 0.2883 11.00000 0.05 0.36 Q76 1 0.5630 0.1662 0.2678 11.00000 0.05 0.35 Q77 1 0.3423 0.2542 0.2600 11.00000 0.05 0.35 Q78 1 0.4657 -0.0534 0.4872 11.00000 0.05 0.35 Q79 1 0.3747 0.5279 0.3091 11.00000 0.05 0.35 Q80 1 0.1026 0.0198 0.2716 11.00000 0.05 0.35 Q81 1 0.3452 0.5205 0.4708 11.00000 0.05 0.35 Q82 1 0.7745 0.2191 0.2892 11.00000 0.05 0.35 Q83 1 0.6236 0.3794 0.5067 11.00000 0.05 0.34 Q84 1 0.7882 0.3259 0.3353 11.00000 0.05 0.34 Q85 1 0.6801 0.3034 0.3238 11.00000 0.05 0.34 Q86 1 0.5000 0.4934 0.2500 10.50000 0.05 0.34 Q87 1 0.1343 0.2751 0.2960 11.00000 0.05 0.34 Q88 1 0.2800 0.3145 0.3225 11.00000 0.05 0.34 Q89 1 0.3594 0.2029 0.4206 11.00000 0.05 0.34 Q90 1 0.2835 0.2414 0.3557 11.00000 0.05 0.33 Q91 1 0.4208 0.0846 0.4986 11.00000 0.05 0.33 Q92 1 0.3235 -0.0741 0.4691 11.00000 0.05 0.33 Q93 1 0.5568 -0.0832 0.3690 11.00000 0.05 0.33 Q94 1 0.7556 0.2948 0.4245 11.00000 0.05 0.33 Q95 1 0.5174 0.4661 0.3519 11.00000 0.05 0.33 Q96 1 0.6444 -0.0220 0.4304 11.00000 0.05 0.33 Q97 1 0.1722 0.2215 0.3967 11.00000 0.05 0.33 Q98 1 0.2944 0.1070 0.4199 11.00000 0.05 0.33 Q99 1 0.4798 0.4243 0.3572 11.00000 0.05 0.32 Q100 1 0.5006 0.6459 0.3005 11.00000 0.05 0.32 Q101 1 0.4983 0.2850 0.5006 11.00000 0.05 0.32 Q102 1 0.5300 0.1670 0.5166 11.00000 0.05 0.32 Q103 1 0.4016 0.0178 0.3313 11.00000 0.05 0.32 Q104 1 0.2768 0.1433 0.4580 11.00000 0.05 0.32 Q105 1 0.4120 0.5675 0.4328 11.00000 0.05 0.32 Q106 1 0.2420 0.2405 0.2904 11.00000 0.05 0.32 Q107 1 0.5192 0.4325 0.4370 11.00000 0.05 0.32 Q108 1 0.4472 0.5241 0.3370 11.00000 0.05 0.32 Q109 1 0.6005 0.1039 0.4128 11.00000 0.05 0.31 Q110 1 0.1634 0.3892 0.3087 11.00000 0.05 0.31 Q111 1 0.6868 0.2697 0.5514 11.00000 0.05 0.31 Q112 1 0.3677 0.1738 0.5174 11.00000 0.05 0.31 Q113 1 0.1240 -0.0290 0.3038 11.00000 0.05 0.31 Q114 1 0.8348 0.1481 0.2997 11.00000 0.05 0.31 Q115 1 0.1520 0.1174 0.3645 11.00000 0.05 0.30 Q116 1 0.3929 -0.1957 0.4600 11.00000 0.05 0.30 Q117 1 0.4199 0.1007 0.4616 11.00000 0.05 0.30 Q118 1 0.2717 0.0543 0.2618 11.00000 0.05 0.30 Q119 1 0.6670 0.2399 0.3595 11.00000 0.05 0.30 Q120 1 0.3367 0.4259 0.3124 11.00000 0.05 0.30 ; _shelx_res_checksum 99464 _shelx_hkl_file ; 1 -1 0 1537.53 54.67 -1 1 0 1473.47 45.29 -1 -1 0 1560.12 44.02 -1 1 0 1448.75 50.76 1 -1 0 1465.12 44.64 0 0 -413145.78 944.80 0 0 -412688.44 899.02 0 0 412418.87 881.27 0 0 412312.44 890.92 -1 1 1 106.66 4.93 1 -1 -1 107.13 4.55 -1 1 1 105.13 6.26 -1 -1 1 110.27 4.83 1 -1 -1 102.17 4.58 1 1 -1 107.88 4.73 1 -1 1 32.16 3.79 1 -1 1 30.07 4.05 1 1 1 29.15 2.58 -1 1 -1 35.03 3.95 1 1 1 35.07 3.95 -1 -1 -1 31.23 2.45 -1 1 -1 31.66 2.56 -1 1 -1 28.55 3.51 1 -1 1 26.37 2.48 1 -1 -2 4534.54 201.68 -1 1 2 4683.13 204.16 -1 -1 2 4437.35 197.37 1 1 -2 4501.74 198.98 -1 1 2 4196.42 182.74 1 1 2 7460.14 386.73 -1 1 -2 7791.68 413.72 -1 -1 -2 7616.29 394.59 -1 -1 -2 7335.63 396.92 -1 1 -2 6881.07 401.82 -1 -1 -2 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1106.53 49.34 3 3 -6 1082.35 51.27 3 3 -6 1102.79 39.07 -4 0 10 626.22 32.95 -4 0 10 629.20 38.17 4 0 -10 602.37 28.00 4 0 -10 621.53 30.06 -4 0 10 612.49 28.56 -4 0 10 618.91 31.05 4 0 -10 607.05 24.89 0 0 -13 9.16 8.99 0 0 13 -3.48 8.72 0 0 -13 -7.43 6.20 0 0 -13 1.54 3.47 0 0 13 1.16 5.91 0 -4 3 12.68 4.63 0 4 -3 14.96 5.15 2 2 -11 21.64 9.41 -2 -2 11 3.27 3.16 2 -2 -11 2.57 3.17 -2 2 11 11.95 9.72 -2 2 11 8.05 4.86 2 -2 -11 -0.44 9.77 2 -2 -11 6.62 7.76 -2 -2 11 16.08 6.44 -2 2 11 4.78 3.59 -2 -2 11 10.88 6.15 2 2 -11 11.99 6.64 4 -2 5 576.21 40.34 -4 -2 -5 567.03 14.46 -4 -2 -5 578.53 34.63 -4 2 -5 577.95 38.89 -4 -2 -5 579.20 31.40 -4 2 -5 549.00 40.44 4 2 5 577.91 32.74 4 -2 5 493.46 38.90 4 2 5 572.28 23.73 4 -2 5 470.10 39.06 1 3 -9 9.98 5.97 -1 3 9 2.14 3.61 -1 3 9 11.38 5.38 -1 3 9 4.71 5.30 1 -3 -9 2.09 5.82 1 -3 -9 2.69 4.88 -1 -3 9 4.02 8.31 1 3 -9 3.43 8.43 5 1 -6 1420.80 80.53 -5 1 6 1387.14 62.97 5 1 -6 1436.58 52.76 -5 1 6 1443.02 75.64 -5 -1 6 1478.62 82.77 5 1 -6 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