data_hanahanite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'hanahanite' _chemical_compound_source 'Redmond mine, North Carolina' _chemical_formula_sum 'H20 O21 S Zn7.82' _chemical_formula_weight 899.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'Zn' 'Zn' 0.2839 1.4301 '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' _space_group_crystal_system hexagonal _space_group_IT_number 173 _space_group_name_H-M_alt 'P 63' _space_group_name_Hall 'P 6c' _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' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 8.312(2) _cell_length_b 8.312(2) _cell_length_c 15.295(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 915.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2587 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 24.7 _exptl_crystal_description 'prism' _exptl_crystal_colour 'blue' _exptl_crystal_density_diffrn 3.263 _exptl_crystal_F_000 877 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 10.276 _shelx_estimated_absorpt_T_min 0.426 _shelx_estimated_absorpt_T_max 0.748 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.286 _exptl_absorpt_process_details 'Higashi2001' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_reflns_number 5789 _diffrn_reflns_av_unetI/netI 0.0650 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.128 _diffrn_reflns_theta_max 24.988 _diffrn_reflns_theta_full 24.988 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 1074 _reflns_number_gt 772 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.923 _reflns_Friedel_fraction_max 0.998 _reflns_Friedel_fraction_full 0.998 _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_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1230P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.27(18) _chemical_absolute_configuration ? _refine_ls_number_reflns 1074 _refine_ls_number_parameters 94 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.2007 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.042 _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 Zn1 Zn 0.000000 0.000000 0.2153(5) 0.0312(19) Uani 1 3 d S T P . . Zn2 Zn 0.000000 0.000000 0.4710(6) 0.0310(18) Uani 1 3 d S T P . . Zn3 Zn 0.4277(2) 0.2888(2) 0.5911(2) 0.0291(10) Uani 0.969(14) 1 d . . P . . Zn4 Zn 0.2821(2) 0.8668(3) 0.5904(3) 0.0307(11) Uani 0.968(15) 1 d . . P . . S S 0.333333 0.666667 0.3913(10) 0.044(2) Uani 1 3 d S T P . . O1 O 0.305(2) 0.492(2) 0.355(2) 0.072(6) Uani 1 1 d . . . . . O2 O 0.333333 0.666667 0.4909(19) 0.031(6) Uani 1 3 d S T P . . OH1 O 0.000000 0.000000 0.337(7) 0.15(2) Uani 1 3 d S T P . . OH2 O 0.1084(17) 0.626(2) 0.6481(15) 0.041(4) Uani 1 1 d . . . . . OH3 O 0.7504(19) 0.941(2) 0.1758(14) 0.045(5) Uani 1 1 d . . . . . OH4 O 0.0530(16) 0.8071(16) 0.5091(16) 0.031(3) Uani 1 1 d . . . . . OH5 O 0.4681(16) 0.0985(14) 0.5240(15) 0.035(4) Uani 1 1 d . . . . . OH6 O 0.666667 0.333333 0.660(2) 0.042(6) Uani 1 3 d S T P . . OW O 0.120(3) 0.684(3) 0.8301(18) 0.089(7) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.034(2) 0.034(2) 0.026(4) 0.000 0.000 0.0169(12) Zn2 0.034(2) 0.034(2) 0.026(4) 0.000 0.000 0.0168(12) Zn3 0.0287(14) 0.0267(13) 0.0337(17) -0.002(2) -0.002(2) 0.0152(9) Zn4 0.0271(14) 0.0280(14) 0.0358(17) 0.0026(19) -0.001(2) 0.0129(9) S 0.051(4) 0.051(4) 0.029(5) 0.000 0.000 0.0255(19) O1 0.088(12) 0.053(10) 0.077(17) 0.007(11) -0.007(12) 0.037(9) O2 0.024(7) 0.024(7) 0.043(15) 0.000 0.000 0.012(4) OH1 0.22(3) 0.22(3) 0.01(2) 0.000 0.000 0.109(17) OH2 0.035(8) 0.052(9) 0.031(8) 0.001(6) -0.005(6) 0.019(7) OH3 0.045(9) 0.056(10) 0.029(9) 0.000(7) -0.007(6) 0.021(7) OH4 0.027(7) 0.028(6) 0.036(7) -0.001(6) 0.000(5) 0.012(5) OH5 0.030(7) 0.023(7) 0.053(12) -0.002(6) -0.003(6) 0.015(6) OH6 0.042(9) 0.042(9) 0.042(13) 0.000 0.000 0.021(4) OW 0.096(14) 0.119(15) 0.013(10) 0.009(11) -0.002(10) 0.023(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 OH1 1.85(11) . ? Zn1 OH3 1.972(15) 1_445 ? Zn1 OH3 1.972(15) 3_565 ? Zn1 OH3 1.972(15) 2_655 ? Zn2 OH4 1.953(13) 2_665 ? Zn2 OH4 1.953(13) 3_455 ? Zn2 OH4 1.953(13) 1_545 ? Zn2 OH1 2.06(11) . ? Zn3 OH5 2.050(15) . ? Zn3 OH2 2.067(15) 2_665 ? Zn3 OH6 2.109(16) . ? Zn3 OH5 2.138(17) 3_665 ? Zn3 OH3 2.165(19) 4_665 ? Zn3 OH4 2.194(18) 2_665 ? Zn3 Zn4 3.087(3) 1_545 ? Zn3 Zn4 3.110(3) 2_665 ? Zn3 Zn4 3.125(2) 3_565 ? Zn4 OH2 1.998(17) . ? Zn4 OH5 2.038(16) 1_565 ? Zn4 OH2 2.058(19) 3_565 ? Zn4 OH4 2.115(18) . ? Zn4 OH3 2.185(19) 4_675 ? Zn4 O2 2.443(19) . ? S O1 1.459(18) 3_565 ? S O1 1.459(18) 2_665 ? S O1 1.459(18) . ? S O2 1.52(3) . ? OH1 OW 3.25(2) 4_564 ? OH2 OW 2.82(3) . ? OH5 OW 2.99(3) 6_654 ? 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 OH1 Zn1 OH3 107.8(6) . 1_445 ? OH1 Zn1 OH3 107.8(6) . 3_565 ? OH3 Zn1 OH3 111.1(6) 1_445 3_565 ? OH1 Zn1 OH3 107.8(6) . 2_655 ? OH3 Zn1 OH3 111.1(6) 1_445 2_655 ? OH3 Zn1 OH3 111.1(6) 3_565 2_655 ? OH4 Zn2 OH4 111.5(7) 2_665 3_455 ? OH4 Zn2 OH4 111.5(7) 2_665 1_545 ? OH4 Zn2 OH4 111.5(7) 3_455 1_545 ? OH4 Zn2 OH1 107.4(7) 2_665 . ? OH4 Zn2 OH1 107.4(7) 3_455 . ? OH4 Zn2 OH1 107.4(7) 1_545 . ? OH5 Zn3 OH2 174.5(11) . 2_665 ? OH5 Zn3 OH6 83.2(5) . . ? OH2 Zn3 OH6 101.8(8) 2_665 . ? OH5 Zn3 OH5 97.7(9) . 3_665 ? OH2 Zn3 OH5 80.8(6) 2_665 3_665 ? OH6 Zn3 OH5 81.1(5) . 3_665 ? OH5 Zn3 OH3 85.6(6) . 4_665 ? OH2 Zn3 OH3 96.7(9) 2_665 4_665 ? OH6 Zn3 OH3 91.5(8) . 4_665 ? OH5 Zn3 OH3 171.4(10) 3_665 4_665 ? OH5 Zn3 OH4 93.7(8) . 2_665 ? OH2 Zn3 OH4 81.3(5) 2_665 2_665 ? OH6 Zn3 OH4 174.9(11) . 2_665 ? OH5 Zn3 OH4 95.5(8) 3_665 2_665 ? OH3 Zn3 OH4 92.2(5) 4_665 2_665 ? OH5 Zn3 Zn4 40.8(5) . 1_545 ? OH2 Zn3 Zn4 140.7(5) 2_665 1_545 ? OH6 Zn3 Zn4 90.04(6) . 1_545 ? OH5 Zn3 Zn4 138.4(4) 3_665 1_545 ? OH3 Zn3 Zn4 45.1(5) 4_665 1_545 ? OH4 Zn3 Zn4 90.1(3) 2_665 1_545 ? OH5 Zn3 Zn4 136.0(5) . 2_665 ? OH2 Zn3 Zn4 39.3(5) 2_665 2_665 ? OH6 Zn3 Zn4 140.7(5) . 2_665 ? OH5 Zn3 Zn4 93.5(3) 3_665 2_665 ? OH3 Zn3 Zn4 89.6(4) 4_665 2_665 ? OH4 Zn3 Zn4 42.8(5) 2_665 2_665 ? Zn4 Zn3 Zn4 117.19(8) 1_545 2_665 ? OH5 Zn3 Zn4 138.0(5) . 3_565 ? OH2 Zn3 Zn4 40.6(5) 2_665 3_565 ? OH6 Zn3 Zn4 88.99(7) . 3_565 ? OH5 Zn3 Zn4 40.3(4) 3_665 3_565 ? OH3 Zn3 Zn4 136.0(5) 4_665 3_565 ? OH4 Zn3 Zn4 90.8(3) 2_665 3_565 ? Zn4 Zn3 Zn4 178.58(8) 1_545 3_565 ? Zn4 Zn3 Zn4 64.16(8) 2_665 3_565 ? OH2 Zn4 OH5 174.3(9) . 1_565 ? OH2 Zn4 OH2 94.9(9) . 3_565 ? OH5 Zn4 OH2 83.4(5) 1_565 3_565 ? OH2 Zn4 OH4 84.8(5) . . ? OH5 Zn4 OH4 95.6(9) 1_565 . ? OH2 Zn4 OH4 166.9(9) 3_565 . ? OH2 Zn4 OH3 100.3(9) . 4_675 ? OH5 Zn4 OH3 85.4(5) 1_565 4_675 ? OH2 Zn4 OH3 97.4(8) 3_565 4_675 ? OH4 Zn4 OH3 95.5(5) . 4_675 ? OH2 Zn4 O2 82.9(6) . . ? OH5 Zn4 O2 91.4(8) 1_565 . ? OH2 Zn4 O2 81.7(5) 3_565 . ? OH4 Zn4 O2 85.3(7) . . ? OH3 Zn4 O2 176.8(6) 4_675 . ? OH2 Zn4 Zn3 144.6(6) . 1_565 ? OH5 Zn4 Zn3 41.1(5) 1_565 1_565 ? OH2 Zn4 Zn3 94.1(4) 3_565 1_565 ? OH4 Zn4 Zn3 93.7(3) . 1_565 ? OH3 Zn4 Zn3 44.5(5) 4_675 1_565 ? O2 Zn4 Zn3 132.3(4) . 1_565 ? OH2 Zn4 Zn3 40.9(5) . 3_565 ? OH5 Zn4 Zn3 140.3(5) 1_565 3_565 ? OH2 Zn4 Zn3 135.7(4) 3_565 3_565 ? OH4 Zn4 Zn3 44.8(5) . 3_565 ? OH3 Zn4 Zn3 94.1(4) 4_675 3_565 ? O2 Zn4 Zn3 88.68(6) . 3_565 ? Zn3 Zn4 Zn3 122.80(8) 1_565 3_565 ? OH2 Zn4 Zn3 135.7(5) . 2_665 ? OH5 Zn4 Zn3 42.8(5) 1_565 2_665 ? OH2 Zn4 Zn3 40.8(5) 3_565 2_665 ? OH4 Zn4 Zn3 137.7(5) . 2_665 ? OH3 Zn4 Zn3 89.0(4) 4_675 2_665 ? O2 Zn4 Zn3 88.32(6) . 2_665 ? Zn3 Zn4 Zn3 61.35(7) 1_565 2_665 ? Zn3 Zn4 Zn3 175.82(8) 3_565 2_665 ? O1 S O1 106.1(12) 3_565 2_665 ? O1 S O1 106.1(12) 3_565 . ? O1 S O1 106.1(12) 2_665 . ? O1 S O2 112.6(11) 3_565 . ? O1 S O2 112.6(11) 2_665 . ? O1 S O2 112.6(11) . . ? S O2 Zn4 128.5(6) . 2_665 ? S O2 Zn4 128.5(6) . 3_565 ? Zn4 O2 Zn4 85.3(8) 2_665 3_565 ? S O2 Zn4 128.5(6) . . ? Zn4 O2 Zn4 85.3(8) 2_665 . ? Zn4 O2 Zn4 85.3(8) 3_565 . ? Zn1 OH1 Zn2 180.0 . . ? Zn1 OH1 OW 88.2(18) . 4_564 ? Zn2 OH1 OW 91.8(18) . 4_564 ? Zn4 OH2 Zn4 109.5(10) . 2_665 ? Zn4 OH2 Zn3 99.8(8) . 3_565 ? Zn4 OH2 Zn3 98.5(8) 2_665 3_565 ? Zn4 OH2 OW 108.6(9) . . ? Zn4 OH2 OW 124.0(9) 2_665 . ? Zn3 OH2 OW 113.5(8) 3_565 . ? Zn1 OH3 Zn3 125.0(8) 1_665 4_664 ? Zn1 OH3 Zn4 120.0(7) 1_665 4_674 ? Zn3 OH3 Zn4 90.4(8) 4_664 4_674 ? Zn1 OH3 O1 103.1(8) 1_665 2_665 ? Zn3 OH3 O1 100.1(7) 4_664 2_665 ? Zn4 OH3 O1 117.4(7) 4_674 2_665 ? Zn2 OH4 Zn4 122.0(7) 1_565 . ? Zn2 OH4 Zn3 122.6(7) 1_565 3_565 ? Zn4 OH4 Zn3 92.4(9) . 3_565 ? Zn2 OH4 O1 107.2(10) 1_565 3_565 ? Zn4 OH4 O1 96.1(7) . 3_565 ? Zn3 OH4 O1 113.5(6) 3_565 3_565 ? Zn4 OH5 Zn3 98.1(9) 1_545 . ? Zn4 OH5 Zn3 96.9(8) 1_545 2_655 ? Zn3 OH5 Zn3 98.4(8) . 2_655 ? Zn4 OH5 OW 120.2(8) 1_545 6_654 ? Zn3 OH5 OW 113.4(8) . 6_654 ? Zn3 OH5 OW 124.8(8) 2_655 6_654 ? Zn3 OH6 Zn3 97.4(10) . 3_665 ? Zn3 OH6 Zn3 97.4(10) . 2_655 ? Zn3 OH6 Zn3 97.4(10) 3_665 2_655 ? Zn3 OH6 O1 112.6(7) . 4_665 ? Zn3 OH6 O1 100.6(7) 3_665 4_665 ? Zn3 OH6 O1 142.3(10) 2_655 4_665 ? OH2 OW O1 90.3(7) . 6 ? OH2 OW O1 96.0(7) . 4_565 ? O1 OW O1 45.5(7) 6 4_565 ? _refine_diff_density_max 2.741 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.229 _shelx_res_file ; TITL User-defined R11.res created by SHELXL-2016/6 at 19:06:46 on 02-Feb-2022 CELL 0.71075 8.31230 8.31230 15.29460 90.00000 90.00000 120.00000 ZERR 2 0.00240 0.00240 0.00240 0.00000 0.00000 0.00000 LATT -1 SYMM -Y, +X-Y, +Z SYMM -X+Y, -X, +Z SYMM -X, -Y, .50+Z SYMM +Y, -X+Y, .50+Z SYMM +X-Y, +X, .50+Z SFAC O S ZN H UNIT 42 2 15.63 40 L.S. 20 FMAP 2 PLAN 20 EQIV $1 -x, -y+1, z-1/2 EQIV $2 -y+1, x-y+1, z EQIV $3 -x+y, -x+1, z EQIV $4 x-y+1, x, z-1/2 EQIV $5 -x+1, -y+1, z+1/2 EQIV $6 x-y, x, z+1/2 EQIV $7 -x, -y+1, z+1/2 BIND OH1 OW_$1 BIND OH2 OW BIND OH3 O1_$2 BIND OH4 O1_$3 BIND OH5 OW_$4 BIND OH6 O1_$5 BIND OW O1_$6 BIND OW O1_$7 ACTA TWIN SIZE 0.100 0.030 0.030 WGHT 0.123000 BASF 0.27283 FVAR 0.28061 0.96851 0.96776 ZN1 3 0.000000 0.000000 0.215341 10.33333 0.03389 0.03389 = 0.02574 0.00000 0.00000 0.01695 ZN2 3 0.000000 0.000000 0.470971 10.33333 0.03357 0.03357 = 0.02581 0.00000 0.00000 0.01678 ZN3 3 0.427663 0.288820 0.591097 21.00000 0.02870 0.02665 = 0.03366 -0.00177 -0.00158 0.01518 ZN4 3 0.282145 0.866767 0.590366 31.00000 0.02709 0.02800 = 0.03583 0.00264 -0.00113 0.01293 S 2 0.333333 0.666667 0.391267 10.33333 0.05103 0.05103 = 0.02885 0.00000 0.00000 0.02552 O1 1 0.304677 0.492201 0.354561 11.00000 0.08770 0.05255 = 0.07690 0.00715 -0.00681 0.03694 O2 1 0.333333 0.666667 0.490886 10.33333 0.02447 0.02447 = 0.04305 0.00000 0.00000 0.01223 OH1 1 0.000000 0.000000 0.336555 10.33333 0.21791 0.21791 = 0.00610 0.00000 0.00000 0.10896 OH2 1 0.108387 0.625530 0.648115 11.00000 0.03521 0.05192 = 0.03071 0.00120 -0.00520 0.01857 OH3 1 0.750412 0.940783 0.175834 11.00000 0.04487 0.05647 = 0.02869 0.00038 -0.00721 0.02145 OH4 1 0.053038 0.807113 0.509124 11.00000 0.02700 0.02754 = 0.03609 -0.00058 -0.00021 0.01213 OH5 1 0.468065 0.098465 0.523999 11.00000 0.03037 0.02350 = 0.05265 -0.00189 -0.00265 0.01540 OH6 1 0.666667 0.333333 0.659637 10.33333 0.04177 0.04177 = 0.04200 0.00000 0.00000 0.02089 OW 1 0.120264 0.683639 0.830060 11.00000 0.09613 0.11897 = 0.01285 0.00948 -0.00248 0.02337 HKLF 4 REM User-defined REM R1 = 0.0650 for 772 Fo > 4sig(Fo) and 0.0854 for all 1074 data REM 94 parameters refined using 1 restraints END WGHT 0.1229 0.0000 REM Highest difference peak 2.741, deepest hole -1.116, 1-sigma level 0.229 Q1 1 0.0000 0.0000 0.5906 10.33333 0.05 2.30 Q2 1 0.1950 0.7035 0.5918 11.00000 0.05 1.12 Q3 1 0.2357 0.9593 0.5903 11.00000 0.05 0.89 Q4 1 0.4922 0.1990 0.5912 11.00000 0.05 0.89 Q5 1 0.0559 0.0789 0.3411 11.00000 0.05 0.86 Q6 1 0.4415 0.2869 0.4715 11.00000 0.05 0.84 Q7 1 0.3333 0.6667 0.5412 10.33333 0.05 0.83 Q8 1 0.1076 0.3965 0.3440 11.00000 0.05 0.82 Q9 1 0.3564 0.7754 0.5872 11.00000 0.05 0.79 Q10 1 0.3333 0.6667 0.2989 10.33333 0.05 0.77 Q11 1 0.4457 0.2941 0.7105 11.00000 0.05 0.77 Q12 1 0.0637 0.8060 0.4395 11.00000 0.05 0.74 Q13 1 0.0664 0.5145 0.5928 11.00000 0.05 0.73 Q14 1 0.2835 0.8424 0.7129 11.00000 0.05 0.71 Q15 1 0.2443 0.0493 0.5304 11.00000 0.05 0.71 Q16 1 0.2858 0.8904 0.8408 11.00000 0.05 0.70 Q17 1 0.4797 0.0956 0.6425 11.00000 0.05 0.69 Q18 1 0.0951 0.6200 0.5368 11.00000 0.05 0.69 Q19 1 0.5142 0.4402 0.5888 11.00000 0.05 0.68 Q20 1 0.2747 0.2358 0.5921 11.00000 0.05 0.68 ; _shelx_res_checksum 7297 _shelx_hkl_file ; 1 -1 -1 92.35 2.54 1 -1 1 95.88 2.68 -1 0 -1 99.49 4.42 0 -1 -1 95.21 3.81 -1 0 1 95.17 4.31 -1 1 1 91.20 3.47 -1 1 -1 89.83 2.83 0 -1 1 91.98 3.03 1 0 1 104.39 4.46 0 1 -1 78.54 2.15 1 0 -1 96.45 3.98 0 1 1 86.08 3.54 -1 1 2 99.87 3.44 -1 0 -2 105.40 4.83 1 0 -2 94.81 4.28 0 -1 2 93.15 2.21 -1 1 -2 91.86 2.33 1 0 2 91.43 4.71 1 -1 2 90.89 3.11 0 1 2 86.99 4.76 -1 1 2 92.21 4.60 0 -1 -2 94.63 3.30 0 1 -2 85.67 2.62 -1 0 2 94.23 4.59 0 0 -3 1.67 1.55 0 0 3 1.71 1.25 0 1 3 110.01 6.20 0 -1 -3 103.18 5.89 -1 0 -3 103.73 5.57 0 -1 3 87.85 2.99 1 0 -3 95.94 4.97 -1 0 3 88.19 5.20 1 -1 -3 92.58 3.92 -1 1 -3 104.80 4.32 1 -1 3 96.78 4.20 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4.19 -6 5 -6 9.41 6.80 5 1 6 24.01 10.73 5 1 -6 16.49 8.12 -6 5 6 7.89 5.34 -6 5 6 16.66 9.64 6 -5 6 17.05 5.95 -5 -1 6 13.98 10.89 -5 -1 -6 27.01 10.55 -1 6 6 15.68 8.01 1 -6 -6 13.78 8.12 -6 1 6 12.30 8.93 -1 -5 6 4.90 4.53 1 5 6 5.41 7.32 -1 -5 -6 3.41 4.91 6 -1 -6 -1.46 6.90 1 5 -6 3.31 3.64 -5 6 6 5.94 5.85 -5 6 6 4.97 4.30 -6 1 -6 12.92 8.11 6 -1 6 -2.98 7.88 3 4 -3 3.71 6.68 -3 -4 -3 3.53 7.85 3 4 3 -1.25 7.83 -3 -4 3 9.11 7.06 -4 7 3 10.67 5.06 -4 7 3 7.81 6.39 -7 3 3 9.39 8.88 7 -3 -3 1.76 7.28 -7 3 -3 5.71 8.13 7 -3 3 -3.49 7.05 -7 4 3 22.46 11.24 7 -4 -3 16.31 8.90 3 -7 -3 14.49 6.82 7 -4 3 25.50 8.46 -7 4 -3 16.64 9.66 -3 7 3 26.73 8.73 4 3 3 30.13 11.32 -4 -3 3 24.70 7.27 -4 -3 -3 6.17 11.23 4 3 -3 20.45 9.02 5 2 0 16.02 9.50 -2 7 0 14.81 6.44 2 -7 0 7.56 6.60 -7 5 0 13.89 8.27 -5 -2 0 17.83 7.00 7 -5 0 18.14 6.92 -5 7 0 257.83 20.32 -5 7 0 262.48 23.53 -7 2 0 253.45 38.37 2 5 0 209.23 29.88 -2 -5 0 205.37 28.31 7 -2 0 255.47 33.26 0 -5 8 25.21 6.33 -5 5 8 49.84 11.71 -5 5 8 36.96 10.95 5 -5 8 34.36 5.03 5 0 8 21.99 12.16 0 5 8 42.42 11.39 -5 0 8 47.72 13.20 -5 5 -8 5.08 5.48 0 -5 -8 47.05 11.68 -5 0 -8 36.86 7.84 5 0 -8 26.81 9.91 2 5 1 8.39 8.27 -7 2 -1 18.60 10.31 -5 7 -1 12.88 3.38 -5 7 -1 8.52 5.57 -5 7 1 14.85 5.89 -5 7 1 14.36 6.96 -7 2 1 5.60 10.71 7 -2 1 5.71 8.84 7 -2 -1 21.52 8.82 -2 -5 -1 7.27 7.81 -2 -5 1 5.68 7.23 2 5 -1 2.25 7.26 -2 7 1 5.13 5.71 5 2 -1 2.80 7.41 5 2 1 30.93 7.60 -7 5 -1 3.16 6.59 -5 -2 1 5.67 8.53 -2 7 -1 2.90 4.51 -5 -2 -1 11.58 8.11 2 -7 1 2.35 4.36 2 -7 -1 -4.04 5.75 -7 5 1 -6.12 6.80 7 -5 1 0.01 5.21 7 -5 -1 -4.23 5.57 6 -6 4 359.61 25.71 -6 6 4 409.75 40.23 -6 6 -4 254.55 31.31 0 -6 4 282.27 29.76 -6 0 -4 393.75 51.56 6 0 -4 355.41 30.07 0 -6 -4 434.30 39.63 6 0 4 384.26 48.54 -6 0 4 388.86 55.20 0 6 -4 260.58 27.97 0 6 4 416.09 42.24 -6 6 4 424.77 37.37 -1 -3 -11 7.51 8.84 4 -1 11 11.92 7.82 -4 1 11 10.91 8.94 3 -4 11 5.45 3.17 -3 4 11 30.26 10.25 -4 1 11 8.63 5.17 3 -4 11 11.75 4.50 -4 1 -11 12.29 7.46 -1 -3 11 14.95 4.75 -1 -3 11 2.07 5.80 1 3 11 24.06 9.23 -3 4 11 16.07 8.28 -3 -1 11 23.46 10.84 1 -4 -11 27.74 12.95 3 1 11 26.13 12.19 1 -4 11 31.45 6.06 -1 4 11 35.69 11.99 -3 -1 11 15.53 9.14 -3 -1 -11 32.42 12.17 4 -3 11 39.45 7.59 -4 3 -11 21.62 6.86 1 -4 11 38.20 5.63 -4 3 11 29.48 11.72 -4 3 11 33.17 7.84 2 -7 -2 137.99 14.74 -2 7 -2 115.54 11.20 -5 -2 2 122.90 25.86 5 2 -2 91.37 14.00 -5 -2 -2 118.35 25.22 5 2 2 130.97 15.46 -7 5 2 114.67 21.48 7 -5 2 92.20 19.80 -7 5 -2 82.31 18.00 2 -7 2 130.82 10.65 7 -5 -2 112.98 17.07 -2 7 2 142.84 14.55 -5 7 2 23.06 5.81 -5 7 -2 13.54 3.68 -5 7 -2 7.15 4.59 7 -2 -2 7.90 8.93 7 -2 2 16.37 8.95 -7 2 -2 19.46 10.57 -7 2 2 17.62 11.25 2 5 2 -2.33 8.02 -2 -5 -2 4.60 8.19 2 5 -2 0.89 6.79 -2 -5 2 4.68 7.00 -5 7 2 16.18 5.11 -2 1 13 -0.72 6.54 1 -2 13 8.11 5.52 -1 -1 13 3.39 5.66 2 -1 13 5.40 5.85 -1 -1 13 1.98 5.56 1 -2 13 2.29 5.02 1 -2 -13 12.96 8.00 -1 -1 -13 2.66 7.57 -2 1 13 10.61 7.15 1 1 13 0.40 7.12 -2 1 -13 6.42 6.16 -1 2 13 16.62 7.47 -3 -4 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-2.58 7.04 0 -1 18 4.82 9.41 0 1 18 17.55 9.59 -1 0 -18 -0.11 6.09 -1 0 18 4.37 9.20 0 -1 18 -7.75 11.65 -1 1 18 1.18 6.08 1 -1 18 -3.67 9.25 1 -1 18 2.30 9.52 -1 1 18 13.39 10.12 1 0 18 10.80 9.18 -1 -8 0 7.76 8.67 -8 9 0 9.61 7.53 -9 1 0 -6.04 9.35 1 -9 0 -1.89 7.10 -1 9 0 -2.56 10.14 -8 -1 0 18.63 14.76 -9 8 0 13.06 7.88 0 -3 17 -1.36 8.48 3 -3 17 -1.02 6.77 -3 0 -17 0.69 8.75 -3 3 17 -3.01 9.30 3 0 17 1.26 8.80 0 3 17 6.86 9.85 -3 0 17 0.45 7.74 0 -3 -17 -2.99 9.87 -8 9 -1 1.47 6.10 -1 -8 -1 3.56 8.13 -1 -8 1 0.12 7.47 -8 9 1 -1.20 7.44 -9 8 -1 22.25 8.33 1 -9 -1 -2.80 8.70 1 -9 1 -0.20 7.36 -9 8 1 24.44 9.27 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 15548