data_MLBECK_3_0m_c _publ_section_references ; Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _diffrn_source_voltage '50 kV' _diffrn_source_current '30 mA' _exptl_crystal_recrystallization_method '?' _publ_contact_author_id_orcid '?' _audit_contact_author_phone '?' _audit_contact_author_name 'Hughes, John M.' _audit_contact_author_email 'jmhughes@uvm.edu' _audit_contact_author_address '?' _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0 H1.30 Ca1.87 Cl0.70 Fe4 K0.68 Mg1.13 Na0.07 O23.30 Si7.72' _chemical_formula_weight 969.65 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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 2/m' _space_group_name_Hall '-C 2y' _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' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.9352(4) _cell_length_b 18.2866(7) _cell_length_c 5.3620(2) _cell_angle_alpha 90 _cell_angle_beta 104.8530(10) _cell_angle_gamma 90 _cell_volume 941.62(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4452 _cell_measurement_theta_min 2.2275 _cell_measurement_theta_max 33.185 _exptl_crystal_description equant _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.420 _exptl_crystal_F_000 953 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.211 _exptl_crystal_size_mid 0.202 _exptl_crystal_size_min 0.176 _exptl_absorpt_coefficient_mu 4.439 _shelx_estimated_absorpt_T_min 0.454 _shelx_estimated_absorpt_T_max 0.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6278 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine focus sealed tube' _diffrn_measurement_device_type 'ApexII CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8930 _diffrn_reflns_av_unetI/netI 0.0102 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.227 _diffrn_reflns_theta_max 33.337 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.952 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.952 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 1791 _reflns_number_gt 1639 _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 'Bruker BIS 2016.5.0.1/14-Jun-2016 && APEX3_2016.5-0' _computing_cell_refinement 'SAINT V8.40A' _computing_data_reduction 'SAINT V8.40A' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material 'FinalCif by Daniel Kratzert, Freiburg 2019' _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^)+(0.0192P)^2^+0.6533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_extinction_coef 0.00007(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1791 _refine_ls_number_parameters 119 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0199 _refine_ls_R_factor_gt 0.0167 _refine_ls_wR_factor_ref 0.0406 _refine_ls_wR_factor_gt 0.0396 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.238 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group MgM1 Mg 0.000000 0.0808(5) 0.500000 0.00967(11) Uani 0.174(4) 2 d S T P . . FeM1 Fe 0.000000 0.09343(3) 0.500000 0.00967(11) Uani 0.826(4) 2 d S T P . . MgM2 Mg 0.000000 0.17880(2) 0.000000 0.00692(8) Uani 0.328(4) 2 d S T P . . FeM2 Fe 0.000000 0.17880(2) 0.000000 0.00692(8) Uani 0.672(4) 2 d S T P . . MgM3 Mg 0.000000 0.000000 0.000000 0.00892(10) Uani 0.126(4) 4 d S T P . . FeM3 Fe 0.000000 0.000000 0.000000 0.00892(10) Uani 0.874(4) 4 d S T P . . M4 Ca 0.000000 0.28079(7) 0.500000 0.01098(11) Uani 0.935(5) 2 d S T P . . M4' Fe 0.000000 0.2653(6) 0.500000 0.0103(16) Uiso 0.065(5) 2 d S . P . . Si1 Si 0.27931(3) 0.08553(2) 0.29998(6) 0.00779(9) Uani 0.955(3) 1 d . . P . . Si2 Si 0.29145(3) 0.17270(2) 0.80951(5) 0.00679(9) Uani 0.974(3) 1 d . . P . . O1 O 0.10521(8) 0.09026(4) 0.21521(14) 0.01175(16) Uani 1 1 d . . . . . O2 O 0.12178(8) 0.17679(4) 0.73158(15) 0.01195(15) Uani 1 1 d . . . . . O3 O 0.1101(3) 0.000000 0.7071(4) 0.0118(3) Uani 0.649(2) 2 d DS T P . . H3 H 0.02(3) 0.000000 0.6(2) 2.0(9) Uiso 0.65 2 d DS . P . . Cl3 Cl 0.16437(15) 0.000000 0.7364(2) 0.0118(3) Uani 0.351(2) 2 d S T P . . O4 O 0.36843(8) 0.24906(4) 0.79268(15) 0.01332(16) Uani 1 1 d . . . . . O5 O 0.34791(8) 0.13672(4) 0.09886(14) 0.01333(16) Uani 1 1 d . . . . . O6 O 0.34389(8) 0.12138(4) 0.59718(14) 0.01432(17) Uani 1 1 d . . . . . O7 O 0.33626(12) 0.000000 0.2949(2) 0.0182(2) Uani 1 2 d S T P . . A2M K 0.500000 0.000000 0.000000 0.0843(8) Uani 0.676(9) 4 d S T P . . A2 Na 0.500000 -0.035(2) 0.000000 0.028(9) Uiso 0.036(7) 2 d S . P . . 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 MgM1 0.01003(12) 0.0120(2) 0.00753(12) 0.000 0.00328(8) 0.000 FeM1 0.01003(12) 0.0120(2) 0.00753(12) 0.000 0.00328(8) 0.000 MgM2 0.00738(12) 0.00595(12) 0.00754(13) 0.000 0.00214(8) 0.000 FeM2 0.00738(12) 0.00595(12) 0.00754(13) 0.000 0.00214(8) 0.000 MgM3 0.01048(16) 0.00622(15) 0.00883(16) 0.000 0.00024(10) 0.000 FeM3 0.01048(16) 0.00622(15) 0.00883(16) 0.000 0.00024(10) 0.000 M4 0.01376(18) 0.0078(3) 0.01389(19) 0.000 0.00808(12) 0.000 Si1 0.00796(14) 0.00719(13) 0.00798(14) -0.00020(9) 0.00160(9) -0.00065(9) Si2 0.00691(13) 0.00675(13) 0.00678(14) 0.00052(9) 0.00188(9) -0.00048(9) O1 0.0116(3) 0.0130(3) 0.0108(3) -0.0011(2) 0.0032(3) -0.0017(2) O2 0.0088(3) 0.0136(3) 0.0129(3) 0.0007(3) 0.0016(2) 0.0008(2) O3 0.0123(6) 0.0118(3) 0.0114(4) 0.000 0.0034(5) 0.000 Cl3 0.0123(6) 0.0118(3) 0.0114(4) 0.000 0.0034(5) 0.000 O4 0.0157(3) 0.0109(3) 0.0140(4) 0.0004(3) 0.0051(3) -0.0026(3) O5 0.0112(3) 0.0157(4) 0.0125(4) 0.0052(3) 0.0020(3) 0.0003(3) O6 0.0121(3) 0.0164(4) 0.0148(4) -0.0046(3) 0.0038(3) 0.0005(3) O7 0.0148(5) 0.0158(5) 0.0233(6) 0.000 0.0040(4) 0.000 A2M 0.1124(16) 0.0397(16) 0.148(2) 0.000 0.1189(18) 0.000 _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 MgM1 O3 1.998(6) 5_556 ? MgM1 O3 1.998(6) . ? MgM1 O1 2.0670(10) 2_556 ? MgM1 O1 2.0670(10) . ? MgM1 O2 2.306(6) . ? MgM1 O2 2.306(6) 2_556 ? MgM1 Cl3 2.323(5) . ? MgM1 Cl3 2.323(5) 5_556 ? FeM1 O1 2.0606(8) 2_556 ? FeM1 O1 2.0606(8) . ? FeM1 O2 2.1353(9) . ? FeM1 O2 2.1354(9) 2_556 ? FeM1 O3 2.1739(16) 5_556 ? FeM1 O3 2.1739(16) . ? FeM1 Cl3 2.4762(11) . ? FeM1 Cl3 2.4762(11) 5_556 ? MgM2 O4 1.9849(8) 7_556 ? MgM2 O4 1.9849(8) 8_454 ? MgM2 O1 2.1040(8) 2 ? MgM2 O1 2.1041(8) . ? MgM2 O2 2.1047(8) 2_556 ? MgM2 O2 2.1047(8) 1_554 ? MgM3 O1 2.1284(7) . ? MgM3 O1 2.1284(7) 5 ? MgM3 O1 2.1284(7) 6 ? MgM3 O1 2.1284(7) 2 ? MgM3 O3 2.132(2) 5_556 ? MgM3 O3 2.132(2) 1_554 ? MgM3 Cl3 2.4182(13) 5_556 ? MgM3 Cl3 2.4182(13) 1_554 ? FeM3 O1 2.1284(7) . ? FeM3 O1 2.1284(7) 5 ? FeM3 O1 2.1284(7) 6 ? FeM3 O1 2.1284(7) 2 ? FeM3 O3 2.132(2) 5_556 ? FeM3 O3 2.132(2) 1_554 ? FeM3 Cl3 2.4182(13) 5_556 ? FeM3 Cl3 2.4182(13) 1_554 ? M4 O4 2.3498(8) 7_556 ? M4 O4 2.3498(8) 8_455 ? M4 O2 2.4191(12) 2_556 ? M4 O2 2.4192(12) . ? M4 O6 2.5083(12) 7_556 ? M4 O6 2.5083(12) 8_455 ? M4 O5 2.7420(10) 7_556 ? M4 O5 2.7420(10) 8_455 ? M4' O2 2.204(8) 2_556 ? M4' O2 2.204(8) . ? M4' O4 2.3006(15) 8_455 ? M4' O4 2.3006(15) 7_556 ? Si1 O7 1.6658(5) . ? Si1 O1 1.6742(8) . ? Si1 O6 1.6902(8) . ? Si1 O5 1.6973(8) . ? Si2 O4 1.6056(8) . ? Si2 O2 1.6312(8) . ? Si2 O5 1.6458(8) 1_556 ? Si2 O6 1.6592(8) . ? O3 Cl3 0.5212(19) . ? Cl3 A2M 3.2711(15) 1_556 ? Cl3 A2 3.331(8) 5_656 ? Cl3 A2 3.331(8) 1_556 ? O5 A2 2.54(3) 5_655 ? O5 A2M 3.0374(8) . ? O6 A2 2.81(2) 5_656 ? O6 A2M 3.2062(8) 1_556 ? O7 A2M 2.5428(12) . ? O7 A2 2.620(11) 5_655 ? O7 A2 2.620(11) . ? A2M A2 0.63(4) 5_655 ? A2M A2 0.63(4) . ? A2 A2 1.26(9) 5_655 ? 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 O3 MgM1 O3 84.6(3) 5_556 . ? O3 MgM1 O1 99.43(19) 5_556 2_556 ? O3 MgM1 O1 87.71(16) . 2_556 ? O3 MgM1 O1 87.70(16) 5_556 . ? O3 MgM1 O1 99.43(19) . . ? O1 MgM1 O1 170.4(5) 2_556 . ? O3 MgM1 O2 178.1(3) 5_556 . ? O3 MgM1 O2 97.28(6) . . ? O1 MgM1 O2 80.41(17) 2_556 . ? O1 MgM1 O2 92.2(2) . . ? O3 MgM1 O2 97.28(6) 5_556 2_556 ? O3 MgM1 O2 178.1(3) . 2_556 ? O1 MgM1 O2 92.2(2) 2_556 2_556 ? O1 MgM1 O2 80.41(17) . 2_556 ? O2 MgM1 O2 80.8(3) . 2_556 ? O3 MgM1 Cl3 92.4(3) 5_556 . ? O3 MgM1 Cl3 10.85(5) . . ? O1 MgM1 Cl3 93.90(14) 2_556 . ? O1 MgM1 Cl3 92.21(14) . . ? O2 MgM1 Cl3 89.54(4) . . ? O2 MgM1 Cl3 167.6(2) 2_556 . ? O3 MgM1 Cl3 10.85(5) 5_556 5_556 ? O3 MgM1 Cl3 92.4(3) . 5_556 ? O1 MgM1 Cl3 92.21(14) 2_556 5_556 ? O1 MgM1 Cl3 93.90(14) . 5_556 ? O2 MgM1 Cl3 167.6(2) . 5_556 ? O2 MgM1 Cl3 89.54(4) 2_556 5_556 ? Cl3 MgM1 Cl3 101.0(3) . 5_556 ? O1 FeM1 O1 176.78(5) 2_556 . ? O1 FeM1 O2 84.75(3) 2_556 . ? O1 FeM1 O2 97.56(3) . . ? O1 FeM1 O2 97.56(3) 2_556 2_556 ? O1 FeM1 O2 84.75(3) . 2_556 ? O2 FeM1 O2 88.89(4) . 2_556 ? O1 FeM1 O3 94.12(7) 2_556 5_556 ? O1 FeM1 O3 83.34(6) . 5_556 ? O2 FeM1 O3 173.75(6) . 5_556 ? O2 FeM1 O3 97.36(6) 2_556 5_556 ? O1 FeM1 O3 83.34(6) 2_556 . ? O1 FeM1 O3 94.12(7) . . ? O2 FeM1 O3 97.36(6) . . ? O2 FeM1 O3 173.75(6) 2_556 . ? O3 FeM1 O3 76.40(10) 5_556 . ? O1 FeM1 Cl3 89.68(4) 2_556 . ? O1 FeM1 Cl3 88.10(4) . . ? O2 FeM1 Cl3 89.65(3) . . ? O2 FeM1 Cl3 172.45(4) 2_556 . ? O3 FeM1 Cl3 84.19(7) 5_556 . ? O3 FeM1 Cl3 10.50(5) . . ? O1 FeM1 Cl3 88.10(4) 2_556 5_556 ? O1 FeM1 Cl3 89.68(4) . 5_556 ? O2 FeM1 Cl3 172.45(4) . 5_556 ? O2 FeM1 Cl3 89.65(3) 2_556 5_556 ? O3 FeM1 Cl3 10.50(5) 5_556 5_556 ? O3 FeM1 Cl3 84.19(7) . 5_556 ? Cl3 FeM1 Cl3 92.75(5) . 5_556 ? O4 MgM2 O4 96.70(5) 7_556 8_454 ? O4 MgM2 O1 169.06(3) 7_556 2 ? O4 MgM2 O1 92.35(3) 8_454 2 ? O4 MgM2 O1 92.35(3) 7_556 . ? O4 MgM2 O1 169.06(3) 8_454 . ? O1 MgM2 O1 79.38(4) 2 . ? O4 MgM2 O2 92.30(3) 7_556 2_556 ? O4 MgM2 O2 89.03(3) 8_454 2_556 ? O1 MgM2 O2 94.00(3) 2 2_556 ? O1 MgM2 O2 84.46(3) . 2_556 ? O4 MgM2 O2 89.03(3) 7_556 1_554 ? O4 MgM2 O2 92.30(3) 8_454 1_554 ? O1 MgM2 O2 84.46(3) 2 1_554 ? O1 MgM2 O2 94.00(3) . 1_554 ? O2 MgM2 O2 178.00(4) 2_556 1_554 ? O1 MgM3 O1 180.0 . 5 ? O1 MgM3 O1 101.70(4) . 6 ? O1 MgM3 O1 78.30(4) 5 6 ? O1 MgM3 O1 78.30(4) . 2 ? O1 MgM3 O1 101.70(4) 5 2 ? O1 MgM3 O1 180.00(5) 6 2 ? O1 MgM3 O3 82.76(5) . 5_556 ? O1 MgM3 O3 97.24(5) 5 5_556 ? O1 MgM3 O3 82.76(5) 6 5_556 ? O1 MgM3 O3 97.24(5) 2 5_556 ? O1 MgM3 O3 97.24(5) . 1_554 ? O1 MgM3 O3 82.76(5) 5 1_554 ? O1 MgM3 O3 97.24(5) 6 1_554 ? O1 MgM3 O3 82.76(5) 2 1_554 ? O3 MgM3 O3 180.00(11) 5_556 1_554 ? O1 MgM3 Cl3 89.69(3) . 5_556 ? O1 MgM3 Cl3 90.32(3) 5 5_556 ? O1 MgM3 Cl3 89.68(3) 6 5_556 ? O1 MgM3 Cl3 90.32(3) 2 5_556 ? O3 MgM3 Cl3 11.01(6) 5_556 5_556 ? O3 MgM3 Cl3 168.99(6) 1_554 5_556 ? O1 MgM3 Cl3 90.31(3) . 1_554 ? O1 MgM3 Cl3 89.68(3) 5 1_554 ? O1 MgM3 Cl3 90.32(3) 6 1_554 ? O1 MgM3 Cl3 89.68(3) 2 1_554 ? O3 MgM3 Cl3 168.99(6) 5_556 1_554 ? O3 MgM3 Cl3 11.01(6) 1_554 1_554 ? Cl3 MgM3 Cl3 180.0 5_556 1_554 ? O1 FeM3 O1 180.0 . 5 ? O1 FeM3 O1 101.70(4) . 6 ? O1 FeM3 O1 78.30(4) 5 6 ? O1 FeM3 O1 78.30(4) . 2 ? O1 FeM3 O1 101.70(4) 5 2 ? O1 FeM3 O1 180.00(5) 6 2 ? O1 FeM3 O3 82.76(5) . 5_556 ? O1 FeM3 O3 97.24(5) 5 5_556 ? O1 FeM3 O3 82.76(5) 6 5_556 ? O1 FeM3 O3 97.24(5) 2 5_556 ? O1 FeM3 O3 97.24(5) . 1_554 ? O1 FeM3 O3 82.76(5) 5 1_554 ? O1 FeM3 O3 97.24(5) 6 1_554 ? O1 FeM3 O3 82.76(5) 2 1_554 ? O3 FeM3 O3 180.00(11) 5_556 1_554 ? O1 FeM3 Cl3 89.69(3) . 5_556 ? O1 FeM3 Cl3 90.32(3) 5 5_556 ? O1 FeM3 Cl3 89.68(3) 6 5_556 ? O1 FeM3 Cl3 90.32(3) 2 5_556 ? O3 FeM3 Cl3 11.01(6) 5_556 5_556 ? O3 FeM3 Cl3 168.99(6) 1_554 5_556 ? O1 FeM3 Cl3 90.31(3) . 1_554 ? O1 FeM3 Cl3 89.68(3) 5 1_554 ? O1 FeM3 Cl3 90.32(3) 6 1_554 ? O1 FeM3 Cl3 89.68(3) 2 1_554 ? O3 FeM3 Cl3 168.99(6) 5_556 1_554 ? O3 FeM3 Cl3 11.01(6) 1_554 1_554 ? Cl3 FeM3 Cl3 180.0 5_556 1_554 ? O4 M4 O4 153.13(7) 7_556 8_455 ? O4 M4 O2 76.42(4) 7_556 2_556 ? O4 M4 O2 82.50(4) 8_455 2_556 ? O4 M4 O2 82.50(4) 7_556 . ? O4 M4 O2 76.42(4) 8_455 . ? O2 M4 O2 76.35(5) 2_556 . ? O4 M4 O6 63.10(3) 7_556 7_556 ? O4 M4 O6 141.62(5) 8_455 7_556 ? O2 M4 O6 135.12(3) 2_556 7_556 ? O2 M4 O6 114.38(3) . 7_556 ? O4 M4 O6 141.62(5) 7_556 8_455 ? O4 M4 O6 63.10(3) 8_455 8_455 ? O2 M4 O6 114.38(3) 2_556 8_455 ? O2 M4 O6 135.12(3) . 8_455 ? O6 M4 O6 89.00(5) 7_556 8_455 ? O4 M4 O5 111.26(3) 7_556 7_556 ? O4 M4 O5 83.86(3) 8_455 7_556 ? O2 M4 O5 159.66(4) 2_556 7_556 ? O2 M4 O5 85.83(2) . 7_556 ? O6 M4 O5 61.63(3) 7_556 7_556 ? O6 M4 O5 71.97(4) 8_455 7_556 ? O4 M4 O5 83.86(3) 7_556 8_455 ? O4 M4 O5 111.26(3) 8_455 8_455 ? O2 M4 O5 85.83(2) 2_556 8_455 ? O2 M4 O5 159.66(4) . 8_455 ? O6 M4 O5 71.97(4) 7_556 8_455 ? O6 M4 O5 61.63(3) 8_455 8_455 ? O5 M4 O5 113.25(5) 7_556 8_455 ? O2 M4' O2 85.4(4) 2_556 . ? O2 M4' O4 88.5(2) 2_556 8_455 ? O2 M4' O4 81.8(2) . 8_455 ? O2 M4' O4 81.8(2) 2_556 7_556 ? O2 M4' O4 88.5(2) . 7_556 ? O4 M4' O4 166.8(5) 8_455 7_556 ? O2 M4' MgM2 89.5(3) 2_556 1_556 ? O2 M4' MgM2 42.48(9) . 1_556 ? O4 M4' MgM2 39.55(9) 8_455 1_556 ? O4 M4' MgM2 130.9(3) 7_556 1_556 ? O2 M4' MgM2 42.48(9) 2_556 . ? O2 M4' MgM2 89.5(3) . . ? O4 M4' MgM2 130.9(3) 8_455 . ? O4 M4' MgM2 39.55(9) 7_556 . ? MgM2 M4' MgM2 118.9(3) 1_556 . ? O7 Si1 O1 112.07(5) . . ? O7 Si1 O6 109.34(5) . . ? O1 Si1 O6 110.61(4) . . ? O7 Si1 O5 108.31(5) . . ? O1 Si1 O5 110.74(4) . . ? O6 Si1 O5 105.54(4) . . ? O4 Si2 O2 114.93(4) . . ? O4 Si2 O5 110.40(4) . 1_556 ? O2 Si2 O5 109.87(4) . 1_556 ? O4 Si2 O6 102.45(4) . . ? O2 Si2 O6 109.62(4) . . ? O5 Si2 O6 109.25(4) 1_556 . ? Si1 O1 FeM1 119.03(4) . . ? Si1 O1 MgM1 118.56(5) . . ? FeM1 O1 MgM1 6.4(2) . . ? Si1 O1 MgM2 121.47(4) . . ? FeM1 O1 MgM2 96.30(3) . . ? MgM1 O1 MgM2 101.27(18) . . ? Si1 O1 MgM3 115.89(4) . . ? FeM1 O1 MgM3 98.72(3) . . ? MgM1 O1 MgM3 93.70(18) . . ? MgM2 O1 MgM3 101.16(3) . . ? Si1 O1 FeM3 115.89(4) . . ? FeM1 O1 FeM3 98.72(3) . . ? MgM1 O1 FeM3 93.70(18) . . ? MgM2 O1 FeM3 101.16(3) . . ? MgM3 O1 FeM3 0.0 . . ? Si2 O2 MgM2 124.27(4) . 1_556 ? Si2 O2 FeM1 120.70(4) . . ? MgM2 O2 FeM1 94.06(3) 1_556 . ? Si2 O2 M4' 124.06(13) . . ? MgM2 O2 M4' 92.50(3) 1_556 . ? FeM1 O2 M4' 92.8(2) . . ? Si2 O2 MgM1 117.92(10) . . ? MgM2 O2 MgM1 93.86(3) 1_556 . ? FeM1 O2 MgM1 4.02(14) . . ? M4' O2 MgM1 96.9(3) . . ? Si2 O2 M4 121.04(4) . . ? MgM2 O2 M4 92.16(3) 1_556 . ? FeM1 O2 M4 97.38(4) . . ? M4' O2 M4 4.54(18) . . ? MgM1 O2 M4 101.40(14) . . ? Cl3 O3 MgM1 123.0(2) . 5_556 ? Cl3 O3 MgM1 123.0(2) . . ? MgM1 O3 MgM1 95.4(3) 5_556 . ? Cl3 O3 MgM3 117.6(3) . 1_556 ? MgM1 O3 MgM3 95.63(9) 5_556 1_556 ? MgM1 O3 MgM3 95.63(9) . 1_556 ? Cl3 O3 FeM1 120.02(15) . 5_556 ? MgM1 O3 FeM1 4.10(16) 5_556 5_556 ? MgM1 O3 FeM1 99.51(18) . 5_556 ? MgM3 O3 FeM1 95.17(8) 1_556 5_556 ? Cl3 O3 FeM1 120.02(16) . . ? MgM1 O3 FeM1 99.51(18) 5_556 . ? MgM1 O3 FeM1 4.10(16) . . ? MgM3 O3 FeM1 95.17(8) 1_556 . ? FeM1 O3 FeM1 103.60(10) 5_556 . ? O3 Cl3 MgM1 46.16(19) . 5_556 ? O3 Cl3 MgM1 46.16(19) . . ? MgM1 Cl3 MgM1 79.0(3) 5_556 . ? O3 Cl3 MgM3 51.4(3) . 1_556 ? MgM1 Cl3 MgM3 80.41(5) 5_556 1_556 ? MgM1 Cl3 MgM3 80.41(5) . 1_556 ? O3 Cl3 FeM1 49.48(13) . 5_556 ? MgM1 Cl3 FeM1 4.12(16) 5_556 5_556 ? MgM1 Cl3 FeM1 83.13(16) . 5_556 ? MgM3 Cl3 FeM1 81.00(4) 1_556 5_556 ? O3 Cl3 FeM1 49.48(13) . . ? MgM1 Cl3 FeM1 83.13(16) 5_556 . ? MgM1 Cl3 FeM1 4.12(16) . . ? MgM3 Cl3 FeM1 81.00(4) 1_556 . ? FeM1 Cl3 FeM1 87.25(5) 5_556 . ? O3 Cl3 A2M 172.3(3) . 1_556 ? MgM1 Cl3 A2M 137.05(14) 5_556 1_556 ? MgM1 Cl3 A2M 137.05(14) . 1_556 ? MgM3 Cl3 A2M 120.92(4) 1_556 1_556 ? FeM1 Cl3 A2M 133.37(3) 5_556 1_556 ? FeM1 Cl3 A2M 133.37(3) . 1_556 ? O3 Cl3 A2 166.7(6) . 5_656 ? MgM1 Cl3 A2 147.1(7) 5_556 5_656 ? MgM1 Cl3 A2 126.7(7) . 5_656 ? MgM3 Cl3 A2 120.30(9) 1_556 5_656 ? FeM1 Cl3 A2 143.6(7) 5_556 5_656 ? FeM1 Cl3 A2 122.9(7) . 5_656 ? A2M Cl3 A2 10.9(7) 1_556 5_656 ? O3 Cl3 A2 166.7(6) . 1_556 ? MgM1 Cl3 A2 126.7(7) 5_556 1_556 ? MgM1 Cl3 A2 147.1(7) . 1_556 ? MgM3 Cl3 A2 120.30(9) 1_556 1_556 ? FeM1 Cl3 A2 122.9(7) 5_556 1_556 ? FeM1 Cl3 A2 143.6(7) . 1_556 ? A2M Cl3 A2 10.9(7) 1_556 1_556 ? A2 Cl3 A2 21.8(15) 5_656 1_556 ? Si2 O4 MgM2 143.25(5) . 7_556 ? Si2 O4 M4' 107.5(3) . 7_556 ? MgM2 O4 M4' 92.89(18) 7_556 7_556 ? Si2 O4 M4 100.95(5) . 7_556 ? MgM2 O4 M4 97.42(4) 7_556 7_556 ? M4' O4 M4 6.9(2) 7_556 7_556 ? Si2 O5 Si1 136.40(5) 1_554 . ? Si2 O5 A2 100.0(3) 1_554 5_655 ? Si1 O5 A2 94.8(6) . 5_655 ? Si2 O5 M4 120.37(4) 1_554 7_556 ? Si1 O5 M4 92.02(3) . 7_556 ? A2 O5 M4 109.3(3) 5_655 7_556 ? Si2 O5 A2M 103.25(4) 1_554 . ? Si1 O5 A2M 87.46(3) . . ? A2 O5 A2M 8.1(7) 5_655 . ? M4 O5 A2M 113.01(3) 7_556 . ? Si2 O6 Si1 139.14(5) . . ? Si2 O6 M4 93.37(4) . 7_556 ? Si1 O6 M4 100.74(4) . 7_556 ? Si2 O6 A2 90.1(5) . 5_656 ? Si1 O6 A2 120.5(7) . 5_656 ? M4 O6 A2 108.3(5) 7_556 5_656 ? Si2 O6 A2M 96.44(3) . 1_556 ? Si1 O6 A2M 111.58(4) . 1_556 ? M4 O6 A2M 114.56(3) 7_556 1_556 ? A2 O6 A2M 9.3(7) 5_656 1_556 ? Si1 O7 Si1 139.73(8) 6 . ? Si1 O7 A2M 106.52(4) 6 . ? Si1 O7 A2M 106.52(4) . . ? Si1 O7 A2 120.1(9) 6 5_655 ? Si1 O7 A2 92.9(9) . 5_655 ? A2M O7 A2 13.9(9) . 5_655 ? Si1 O7 A2 92.9(9) 6 . ? Si1 O7 A2 120.1(9) . . ? A2M O7 A2 13.9(9) . . ? A2 O7 A2 27.9(19) 5_655 . ? A2 A2M A2 180.0 5_655 . ? A2 A2M O7 90.0 5_655 5_655 ? A2 A2M O7 90.0 . 5_655 ? A2 A2M O7 90.0 5_655 . ? A2 A2M O7 90.0 . . ? O7 A2M O7 180.0 5_655 . ? A2 A2M O5 145.399(14) 5_655 6 ? A2 A2M O5 34.601(14) . 6 ? O7 A2M O5 122.326(15) 5_655 6 ? O7 A2M O5 57.674(15) . 6 ? A2 A2M O5 34.601(14) 5_655 2_655 ? A2 A2M O5 145.399(14) . 2_655 ? O7 A2M O5 57.674(15) 5_655 2_655 ? O7 A2M O5 122.326(15) . 2_655 ? O5 A2M O5 180.000(17) 6 2_655 ? A2 A2M O5 145.399(14) 5_655 5_655 ? A2 A2M O5 34.601(14) . 5_655 ? O7 A2M O5 57.674(15) 5_655 5_655 ? O7 A2M O5 122.326(15) . 5_655 ? O5 A2M O5 69.20(3) 6 5_655 ? O5 A2M O5 110.80(3) 2_655 5_655 ? A2 A2M O5 34.601(14) 5_655 . ? A2 A2M O5 145.399(14) . . ? O7 A2M O5 122.326(15) 5_655 . ? O7 A2M O5 57.674(15) . . ? O5 A2M O5 110.80(3) 6 . ? O5 A2M O5 69.20(3) 2_655 . ? O5 A2M O5 180.0 5_655 . ? A2 A2M O6 133.810(14) 5_655 6_554 ? A2 A2M O6 46.190(14) . 6_554 ? O7 A2M O6 81.79(2) 5_655 6_554 ? O7 A2M O6 98.21(2) . 6_554 ? O5 A2M O6 51.051(18) 6 6_554 ? O5 A2M O6 128.949(18) 2_655 6_554 ? O5 A2M O6 59.27(2) 5_655 6_554 ? O5 A2M O6 120.73(2) . 6_554 ? A2 A2M O6 46.190(14) 5_655 2_656 ? A2 A2M O6 133.810(14) . 2_656 ? O7 A2M O6 98.21(2) 5_655 2_656 ? O7 A2M O6 81.79(2) . 2_656 ? O5 A2M O6 128.949(18) 6 2_656 ? O5 A2M O6 51.051(18) 2_655 2_656 ? O5 A2M O6 120.73(2) 5_655 2_656 ? O5 A2M O6 59.27(2) . 2_656 ? O6 A2M O6 180.00(3) 6_554 2_656 ? A2 A2M O6 133.810(14) 5_655 5_656 ? A2 A2M O6 46.190(14) . 5_656 ? O7 A2M O6 98.21(2) 5_655 5_656 ? O7 A2M O6 81.79(2) . 5_656 ? O5 A2M O6 59.27(2) 6 5_656 ? O5 A2M O6 120.73(2) 2_655 5_656 ? O5 A2M O6 51.051(18) 5_655 5_656 ? O5 A2M O6 128.949(18) . 5_656 ? O6 A2M O6 92.38(3) 6_554 5_656 ? O6 A2M O6 87.62(3) 2_656 5_656 ? A2 A2M O6 46.190(14) 5_655 1_554 ? A2 A2M O6 133.810(14) . 1_554 ? O7 A2M O6 81.79(2) 5_655 1_554 ? O7 A2M O6 98.21(2) . 1_554 ? O5 A2M O6 120.73(2) 6 1_554 ? O5 A2M O6 59.27(2) 2_655 1_554 ? O5 A2M O6 128.949(18) 5_655 1_554 ? O5 A2M O6 51.051(18) . 1_554 ? O6 A2M O6 87.62(3) 6_554 1_554 ? O6 A2M O6 92.38(3) 2_656 1_554 ? O6 A2M O6 180.00(2) 5_656 1_554 ? A2M A2 A2 0.0 . 5_655 ? A2M A2 O5 137.3(7) . 6 ? A2 A2 O5 137.3(7) 5_655 6 ? A2M A2 O5 137.3(7) . 5_655 ? A2 A2 O5 137.3(7) 5_655 5_655 ? O5 A2 O5 85.4(13) 6 5_655 ? A2M A2 O7 76.1(9) . 5_655 ? A2 A2 O7 76.1(9) 5_655 5_655 ? O5 A2 O7 142.8(14) 6 5_655 ? O5 A2 O7 63.7(3) 5_655 5_655 ? A2M A2 O7 76.1(9) . . ? A2 A2 O7 76.1(9) 5_655 . ? O5 A2 O7 63.7(3) 6 . ? O5 A2 O7 142.8(14) 5_655 . ? O7 A2 O7 152.1(19) 5_655 . ? A2M A2 O6 124.5(7) . 6_554 ? A2 A2 O6 124.5(7) 5_655 6_554 ? O5 A2 O6 60.3(7) 6 6_554 ? O5 A2 O6 70.4(8) 5_655 6_554 ? O7 A2 O6 88.7(3) 5_655 6_554 ? O7 A2 O6 107.1(4) . 6_554 ? A2M A2 O6 124.5(7) . 5_656 ? A2 A2 O6 124.5(7) 5_655 5_656 ? O5 A2 O6 70.4(8) 6 5_656 ? O5 A2 O6 60.3(7) 5_655 5_656 ? O7 A2 O6 107.1(4) 5_655 5_656 ? O7 A2 O6 88.7(3) . 5_656 ? O6 A2 O6 111.1(15) 6_554 5_656 ? A2M A2 Si1 107.1(8) . 6 ? A2 A2 Si1 107.1(8) 5_655 6 ? O5 A2 Si1 32.20(12) 6 6 ? O5 A2 Si1 114.5(14) 5_655 6 ? O7 A2 Si1 173.3(8) 5_655 6 ? O7 A2 Si1 31.61(17) . 6 ? O6 A2 Si1 84.6(6) 6_554 6 ? O6 A2 Si1 76.2(5) 5_656 6 ? A2M A2 Si1 107.1(8) . 5_655 ? A2 A2 Si1 107.1(8) 5_655 5_655 ? O5 A2 Si1 114.5(14) 6 5_655 ? O5 A2 Si1 32.20(12) 5_655 5_655 ? O7 A2 Si1 31.61(17) 5_655 5_655 ? O7 A2 Si1 173.3(8) . 5_655 ? O6 A2 Si1 76.2(5) 6_554 5_655 ? O6 A2 Si1 84.6(6) 5_656 5_655 ? Si1 A2 Si1 145.8(15) 6 5_655 ? A2M A2 Si2 140.8(5) . 6_554 ? A2 A2 Si2 140.8(5) 5_655 6_554 ? O5 A2 Si2 29.8(4) 6 6_554 ? O5 A2 Si2 74.3(10) 5_655 6_554 ? O7 A2 Si2 116.1(8) 5_655 6_554 ? O7 A2 Si2 86.1(5) . 6_554 ? O6 A2 Si2 30.6(4) 6_554 6_554 ? O6 A2 Si2 89.1(11) 5_656 6_554 ? Si1 A2 Si2 57.7(5) 6 6_554 ? Si1 A2 Si2 94.6(9) 5_655 6_554 ? A2M A2 Si2 140.8(5) . 5_656 ? A2 A2 Si2 140.8(5) 5_655 5_656 ? O5 A2 Si2 74.3(10) 6 5_656 ? O5 A2 Si2 29.8(4) 5_655 5_656 ? O7 A2 Si2 86.1(5) 5_655 5_656 ? O7 A2 Si2 116.1(8) . 5_656 ? O6 A2 Si2 89.1(11) 6_554 5_656 ? O6 A2 Si2 30.6(4) 5_656 5_656 ? Si1 A2 Si2 94.6(9) 6 5_656 ? Si1 A2 Si2 57.7(5) 5_655 5_656 ? Si2 A2 Si2 78.4(10) 6_554 5_656 ? _refine_diff_density_max 0.386 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.070 _shelx_res_file ; TITL MLBECK_3_0m_c.res in C2/m MLBECK_3_0m_c.res created by SHELXL-2018/3 at 14:42:32 on 19-Mar-2020 REM Old TITL MLBECK_3_0m in C2/m REM SHELXT solution in Cm REM R1 0.098, Rweak 0.003, Alpha 0.028, Orientation as input REM Flack x = 0.489 ( 0.010 ) from Parsons' quotients REM Formula found by SHELXT: Ca7 Cl O24 Si8 CELL 0.71073 9.9352 18.2866 5.3620 90.000 104.853 90.000 ZERR 2.000 0.0004 0.0007 0.0002 0.000 0.001 0.000 LATT 7 SYMM -X, Y, -Z SFAC O H NA MG SI CA FE CL AL K UNIT 46.596 2.6 0.146 2.26116 15.4351 3.74048 7.99836 1.40404 0 1.35172 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 293 SIZE 0.176 0.202 0.211 EADP MGM1 FEM1 HTAB EXYZ MGM2 FEM2 EADP MGM2 FEM2 EADP MGM3 FEM3 OMIT 0 0 2 OMIT 1 5 2 OMIT -2 0 1 OMIT -2 6 1 OMIT -8 0 2 OMIT 5 1 0 OMIT 0 8 0 OMIT 5 11 0 OMIT 4 0 0 OMIT 1 3 2 REM EXYZ SI1 AL1 REM EADP SI1 AL1 REM EXYZ SI2 AL2 REM EADP SI2 AL2 DFIX 0.9 0.03 O3 H3 CONN FEM1 8 CONN MGM1 8 CONN FEM2 6 CONN MGM2 6 CONN MGM3 8 CONN FEM3 8 CONN SI1 4 CONN SI2 4 CONN M4 8 L.S. 12 BOND FMAP 2 PLAN 20 HTAB EADP O3 CL3 ACTA WGHT 0.019200 0.653300 EXTI 0.000074 FVAR 0.25902 0.17425 0.32811 0.12588 0.93512 0.95507 0.97432 FVAR 0.64899 0.67586 0.03650 MOLE 1 REM MGM1 4 0.000000 0.080804 0.500000 20.50000 0.01003 0.01201 = 0.00753 0.00000 0.00328 0.00000 FEM1 7 0.000000 0.093425 0.500000 -20.50000 0.01003 0.01201 = 0.00753 0.00000 0.00328 0.00000 MGM2 4 0.000000 0.178800 0.000000 30.50000 0.00738 0.00595 = 0.00754 0.00000 0.00214 0.00000 FEM2 7 0.000000 0.178800 0.000000 -30.50000 0.00738 0.00595 = 0.00754 0.00000 0.00214 0.00000 MGM3 4 0.000000 0.000000 0.000000 40.25000 0.01048 0.00622 = 0.00883 0.00000 0.00024 0.00000 FEM3 7 0.000000 0.000000 0.000000 -40.25000 0.01048 0.00622 = 0.00883 0.00000 0.00024 0.00000 REM REM M4 6 0.000000 0.280793 0.500000 50.50000 0.01376 0.00776 = 0.01389 0.00000 0.00808 0.00000 M4' 7 0.000000 0.265347 0.500000 -50.50000 0.01034 REM REM SI1 5 0.279305 0.085527 0.299976 61.00000 0.00796 0.00719 = 0.00798 -0.00020 0.00160 -0.00065 REM AL1 9 0.278349 0.086007 0.301281 -61.00000 0.00506 0.00522 = REM 0.00552 -0.00009 0.00123 -0.00048 SI2 5 0.291455 0.172704 0.809511 71.00000 0.00691 0.00675 = 0.00678 0.00052 0.00188 -0.00048 REM AL2 9 0.291316 0.173588 0.811951 -71.00000 0.00538 0.00574 = REM 0.00539 0.00062 0.00178 -0.00001 REM REM O1 1 0.105205 0.090262 0.215208 11.00000 0.01164 0.01297 = 0.01083 -0.00113 0.00323 -0.00167 O2 1 0.121781 0.176793 0.731575 11.00000 0.00876 0.01357 = 0.01288 0.00071 0.00162 0.00082 REM O3 1 0.110132 0.000000 0.707063 80.50000 0.01231 0.01177 = 0.01143 0.00000 0.00342 0.00000 H3 2 0.018610 0.000000 0.627854 10.32500 2.00000 CL3 8 0.164374 0.000000 0.736424 -80.50000 0.01231 0.01177 = 0.01143 0.00000 0.00342 0.00000 REM O4 1 0.368426 0.249062 0.792677 11.00000 0.01572 0.01093 = 0.01400 0.00041 0.00506 -0.00261 O5 1 0.347908 0.136720 0.098860 11.00000 0.01125 0.01573 = 0.01247 0.00517 0.00205 0.00027 O6 1 0.343894 0.121377 0.597175 11.00000 0.01205 0.01637 = 0.01476 -0.00460 0.00384 0.00052 O7 1 0.336256 0.000000 0.294907 10.50000 0.01484 0.01582 = 0.02331 0.00000 0.00401 0.00000 A2M 10 0.500000 0.000000 0.000000 90.25000 0.11245 0.03971 = 0.14763 0.00000 0.11893 0.00000 A2 3 0.500000 -0.034504 0.000000 100.50000 0.02767 REM MOLE 2 HKLF 4 REM MLBECK_3_0m_c.res in C2/m REM wR2 = 0.040612, GooF = S = 1.07341, Restrained GooF = 1.07309 for all data REM R1 = 0.016734 for 1639 Fo > 4sig(Fo) and 0.019934 for all 1791 data REM 119 parameters refined using 1 restraints END WGHT 0.0193 0.6461 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.386, deepest hole -0.404, 1-sigma level 0.070 Q1 1 0.5296 0.0000 0.1851 10.50000 0.05 0.39 Q2 1 0.5940 0.0000 0.0953 10.50000 0.05 0.38 Q3 1 0.5204 -0.0375 0.0921 11.00000 0.05 0.36 Q4 1 0.0713 0.0000 0.0421 10.50000 0.05 0.36 Q5 1 0.2000 0.1669 0.7998 11.00000 0.05 0.34 Q6 1 0.3056 0.0994 0.4676 11.00000 0.05 0.31 Q7 1 0.1997 0.0737 0.2559 11.00000 0.05 0.31 Q8 1 0.0771 0.0924 0.5468 11.00000 0.05 0.31 Q9 1 0.3342 0.1148 0.2009 11.00000 0.05 0.28 Q10 1 0.3331 0.2096 0.8193 11.00000 0.05 0.28 Q11 1 0.0212 0.2371 0.5454 11.00000 0.05 0.27 Q12 1 0.3093 0.1555 -0.0155 11.00000 0.05 0.27 Q13 1 0.3213 0.1425 -0.0575 11.00000 0.05 0.27 Q14 1 0.0947 0.0307 0.6905 11.00000 0.05 0.26 Q15 1 0.0249 0.1806 0.1440 11.00000 0.05 0.24 Q16 1 0.3076 0.1399 0.7032 11.00000 0.05 0.24 Q17 1 0.2905 0.0413 0.2971 11.00000 0.05 0.24 Q18 1 0.0914 0.0118 0.8036 11.00000 0.05 0.22 Q19 1 0.4311 0.2356 0.7601 11.00000 0.05 0.22 Q20 1 0.0564 0.2587 0.5895 11.00000 0.05 0.21 ; _shelx_res_checksum 34227 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63.09 2.70 7 13 0 60.89 2.90 -7 13 0 61.89 2.40 -7 13 0 56.69 2.50 -9 -13 0 80.29 3.90 9 -13 0 79.39 4.00 -9 -13 0 80.79 3.60 -9 13 0 83.99 3.20 -9 13 0 79.89 3.10 9 13 0 80.39 3.40 11 -13 0 29.00 3.30 -11 -13 0 28.20 2.80 11 13 0 23.90 2.60 -11 13 0 23.00 2.40 -13 -13 0 5.30 2.00 0 -14 0 57.39 2.40 0 14 0 56.19 2.20 -2 -14 0 21.80 1.80 2 -14 0 26.90 1.90 -2 14 0 21.20 1.60 2 14 0 21.30 1.60 -4 -14 0 2.00 1.00 4 -14 0 4.40 1.20 -4 14 0 1.60 0.80 4 14 0 2.10 0.90 4 14 0 2.20 0.90 -6 -14 0 11.70 1.80 -6 -14 0 15.20 1.70 6 -14 0 14.20 1.90 6 14 0 13.60 1.80 -6 14 0 14.50 1.60 6 14 0 15.80 1.60 8 -14 0 3.50 1.60 -8 -14 0 4.20 1.40 8 14 0 4.00 1.30 -8 14 0 3.20 1.20 -8 14 0 3.20 1.10 10 -14 0 60.99 4.00 -10 -14 0 55.49 3.70 -10 -14 0 64.29 3.60 -10 14 0 59.59 3.00 10 14 0 62.09 3.40 -12 -14 0 104.09 4.70 12 -14 0 89.39 5.20 -12 -14 0 103.89 4.70 12 14 0 104.29 4.60 1 -15 0 73.89 2.80 -1 -15 0 71.09 2.80 -1 15 0 69.69 2.50 1 15 0 71.59 2.50 -3 -15 0 39.10 2.30 3 -15 0 35.70 2.20 -3 15 0 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7.40 -3 -5 -3 447.46 6.70 3 -5 3 443.16 6.60 -3 5 -3 449.86 5.80 3 5 3 445.46 6.30 -3 5 -3 448.16 6.60 -5 -5 -3 1430.56 16.40 -5 -5 -3 1389.46 15.60 5 -5 3 1395.76 15.20 5 5 3 1383.06 14.90 -5 5 -3 1412.66 14.60 -5 5 -3 1405.36 15.30 -7 -5 -3 236.98 5.60 7 -5 3 248.48 5.70 -7 -5 -3 247.18 6.20 -7 -5 -3 238.78 5.90 -7 5 -3 239.08 5.40 -7 5 -3 229.48 5.60 7 5 3 238.58 5.40 -9 -5 -3 1030.00 14.50 9 -5 3 1005.70 12.70 -9 -5 -3 1052.89 14.50 9 -5 3 1035.80 14.30 9 5 3 1035.10 13.70 -9 5 -3 1043.30 14.00 -9 5 -3 1037.10 14.20 -11 -5 -3 21.60 2.80 11 -5 3 30.80 3.30 -11 -5 -3 25.70 3.20 -11 5 -3 27.20 3.20 -11 5 -3 26.50 3.10 11 5 3 27.80 3.00 14 -6 -3 0.40 2.00 -14 -6 3 2.40 1.60 -14 6 3 3.40 1.80 -14 6 3 5.70 1.70 -14 6 3 -0.50 1.60 14 6 -3 2.00 2.00 -12 -6 3 1147.29 14.50 12 -6 -3 1175.08 16.10 -12 6 3 1157.48 15.00 -12 6 3 1179.48 14.60 -12 6 3 1192.68 14.80 12 6 -3 1154.98 15.60 -10 -6 3 136.19 3.90 10 -6 -3 136.39 4.70 -10 6 3 136.89 3.90 -10 6 3 140.49 4.20 10 6 -3 145.89 4.60 -10 6 3 135.29 3.90 10 6 -3 134.09 3.80 8 -6 -3 2174.88 21.90 -8 -6 3 2211.28 20.40 8 -6 -3 2163.78 20.60 -8 -6 3 2174.18 20.40 -8 6 3 2144.89 20.90 -8 6 3 2191.78 20.60 8 6 -3 2206.78 21.10 8 6 -3 2158.88 21.70 -6 -6 3 214.38 3.80 6 -6 -3 211.78 4.40 6 -6 -3 203.78 4.20 6 6 -3 209.78 4.40 -6 6 3 204.58 4.00 6 6 -3 207.28 4.40 -6 6 3 211.28 3.80 -4 -6 3 495.35 6.00 4 -6 -3 515.35 7.10 -4 -6 3 506.35 6.80 4 6 -3 514.15 7.10 -4 6 3 502.55 6.50 -4 6 3 503.95 6.10 -2 -6 3 5631.44 45.40 -2 -6 3 5565.84 44.20 2 -6 -3 5550.54 45.90 2 -6 -3 5448.15 45.60 2 6 -3 5579.04 44.40 -2 6 3 5552.64 44.40 2 6 -3 5608.04 45.80 -2 6 3 5589.14 45.00 0 -6 3 707.43 8.30 0 -6 -3 711.93 9.20 0 -6 -3 708.33 8.50 0 -6 -3 709.93 7.90 0 6 -3 711.93 7.90 0 6 3 705.83 8.00 0 6 -3 721.33 8.40 -2 -6 -3 2004.20 18.60 -2 -6 -3 1961.10 18.90 -2 -6 -3 2021.10 20.30 2 -6 3 2020.00 18.90 -2 6 -3 2007.30 18.70 -2 6 -3 1951.00 18.10 2 6 3 1997.00 18.50 4 -6 3 10.10 1.50 -4 -6 -3 9.50 1.50 -4 -6 -3 12.00 1.80 4 6 3 11.60 1.40 -4 6 -3 10.00 1.40 -4 6 -3 10.30 1.20 6 -6 3 2009.00 20.70 -6 -6 -3 2050.99 22.10 -6 -6 -3 2014.30 21.20 6 6 3 1997.50 20.30 -6 6 -3 2006.70 20.70 -6 6 -3 2022.50 20.00 -8 -6 -3 364.96 7.50 8 -6 3 377.46 7.60 -8 -6 -3 372.46 8.00 -8 -6 -3 361.96 7.70 8 -6 3 364.36 6.40 -8 6 -3 384.36 7.30 -8 6 -3 367.66 7.50 8 6 3 352.46 7.10 -10 -6 -3 152.28 5.60 -10 -6 -3 148.59 5.40 10 -6 3 155.48 5.80 -10 6 -3 147.89 5.30 10 6 3 149.19 5.10 -10 6 -3 152.08 5.30 -13 -7 3 1.20 1.40 13 -7 -3 -2.80 1.60 -13 7 3 1.70 1.50 -13 7 3 3.10 1.60 -13 7 3 -1.10 1.20 -11 -7 3 2.00 1.10 11 -7 -3 2.60 1.60 -11 7 3 2.70 1.30 11 7 -3 3.20 1.60 -11 7 3 2.90 1.20 -9 -7 3 120.29 3.50 -9 -7 3 118.29 3.40 9 -7 -3 123.69 4.30 9 7 -3 122.39 4.00 -9 7 3 120.99 3.50 -9 7 3 117.09 3.60 9 7 -3 126.49 3.70 7 -7 -3 159.88 4.10 7 -7 -3 164.28 3.90 -7 -7 3 169.28 3.60 -7 7 3 164.28 3.60 7 7 -3 165.38 4.10 7 7 -3 159.98 4.10 -7 7 3 166.38 3.90 -5 -7 3 65.39 2.40 -5 -7 3 66.29 2.00 5 -7 -3 66.19 2.50 -5 7 3 66.09 2.10 -5 7 3 66.79 2.30 5 7 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4 208.48 5.10 -9 -1 -4 69.69 3.90 9 -1 4 75.49 3.70 -9 -1 -4 69.99 4.20 -9 1 -4 79.09 4.00 -9 1 -4 67.69 4.20 9 1 4 77.99 3.80 14 -2 -4 96.49 5.10 -14 -2 4 93.29 4.20 -14 -2 4 85.69 4.30 -14 2 4 89.49 4.40 14 2 -4 87.19 5.00 -14 2 4 88.59 4.10 -12 -2 4 2.10 1.50 12 -2 -4 3.40 1.80 -12 -2 4 2.90 1.40 12 2 -4 4.10 1.90 -12 2 4 0.70 1.10 -12 2 4 6.00 1.60 -10 -2 4 0.30 0.90 10 -2 -4 0.20 1.20 10 -2 -4 2.60 1.10 -10 -2 4 0.00 0.90 -10 2 4 0.10 1.00 10 2 -4 -0.40 1.00 10 2 -4 0.90 1.30 -10 2 4 -0.70 0.80 -8 -2 4 30.50 1.90 -8 -2 4 31.90 1.90 8 -2 -4 30.50 2.10 8 -2 -4 29.40 2.50 8 2 -4 35.60 2.50 8 2 -4 25.00 2.10 -8 2 4 22.80 1.90 -8 2 4 31.20 2.10 -6 -2 4 2.80 0.80 6 -2 -4 3.70 1.10 6 -2 -4 3.70 1.10 -6 -2 4 2.90 0.80 6 2 -4 4.80 1.10 -6 2 4 5.30 1.00 -6 2 4 3.30 0.90 6 2 -4 4.20 1.10 -4 -2 4 11.00 1.20 -4 -2 4 11.50 1.30 4 -2 -4 11.40 1.40 -4 2 4 10.00 1.10 4 2 -4 10.20 1.40 -4 2 4 10.30 1.10 -4 2 4 11.00 1.30 -2 -2 4 18.10 1.40 2 -2 -4 14.20 1.50 -2 -2 4 15.60 1.40 -2 2 4 13.00 1.20 2 2 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115.89 2.90 0 4 -4 125.49 3.20 0 4 -4 120.69 2.90 -2 -4 -4 23.50 1.80 2 -4 4 26.20 2.00 -2 -4 -4 25.30 1.90 2 4 4 22.50 1.70 -2 4 -4 25.50 1.90 -4 -4 -4 1.40 1.20 4 -4 4 3.40 1.20 -4 4 -4 3.80 1.00 -4 4 -4 3.10 1.30 4 4 4 3.20 1.10 6 -4 4 4.70 1.50 -6 -4 -4 4.10 1.60 -6 -4 -4 4.90 1.30 6 4 4 4.20 1.30 -6 4 -4 3.60 1.20 -6 4 -4 2.60 1.30 8 -4 4 47.30 3.40 -8 -4 -4 48.30 3.30 -8 -4 -4 52.09 3.70 8 4 4 50.89 3.20 -8 4 -4 50.99 3.30 -8 4 -4 45.40 3.50 -10 -4 -4 57.39 3.90 -10 -4 -4 64.19 4.50 -10 4 -4 69.79 4.40 10 4 4 70.39 4.00 -10 4 -4 69.19 4.20 -13 -5 4 11.50 2.10 -13 -5 4 8.30 1.70 13 -5 -4 11.70 2.40 -13 5 4 10.10 2.00 -13 5 4 11.20 1.90 13 5 -4 8.50 2.20 -11 -5 4 9.90 1.70 11 -5 -4 12.50 2.20 -11 -5 4 12.60 1.70 11 5 -4 9.70 1.80 -11 5 4 9.10 1.90 11 5 -4 8.20 2.00 -11 5 4 12.70 1.80 9 -5 -4 79.59 3.10 9 -5 -4 76.59 3.50 -9 -5 4 75.29 3.00 -9 -5 4 75.59 2.80 -9 5 4 81.99 3.20 9 5 -4 80.59 3.20 9 5 -4 75.59 3.50 -9 5 4 77.59 2.90 -7 -5 4 42.70 2.10 7 -5 -4 39.30 2.40 7 -5 -4 38.60 2.40 -7 5 4 42.10 2.20 -7 5 4 40.00 2.10 7 5 -4 40.60 2.40 5 -5 -4 26.20 2.00 -5 -5 4 26.80 1.90 -5 -5 4 26.40 1.70 -5 5 4 24.50 1.70 5 5 -4 27.80 2.00 -5 5 4 29.70 1.70 -3 -5 4 4.50 1.10 -3 -5 4 3.40 0.90 3 -5 -4 3.70 1.00 -3 5 4 2.70 0.90 -3 5 4 3.50 0.90 3 5 -4 4.80 1.10 -1 -5 4 93.69 3.00 1 -5 -4 100.49 3.10 -1 5 4 96.19 2.70 1 5 -4 101.29 3.10 1 5 -4 97.99 2.50 -1 -5 -4 -0.50 0.80 1 -5 4 0.70 1.00 -1 -5 -4 1.60 0.90 -1 5 -4 0.60 0.80 1 5 4 -0.20 0.70 -1 5 -4 2.40 0.90 -3 -5 -4 39.80 2.40 3 -5 4 34.90 2.40 3 5 4 40.40 2.20 -3 5 -4 32.80 2.20 -5 -5 -4 -1.00 1.10 5 -5 4 2.00 1.30 -5 5 -4 0.70 1.20 5 5 4 1.00 1.00 -5 5 -4 -0.30 0.90 7 -5 4 31.20 2.80 -7 -5 -4 31.20 2.90 -7 -5 -4 30.20 2.70 -7 5 -4 33.00 2.60 7 5 4 35.30 2.70 -7 5 -4 33.40 2.90 -9 -5 -4 36.40 3.60 9 -5 4 39.50 3.30 -9 -5 -4 38.10 3.30 -9 5 -4 43.00 3.30 -9 5 -4 34.00 3.40 9 5 4 37.00 3.00 -14 -6 4 10.50 2.10 -14 -6 4 10.00 2.00 14 6 -4 9.80 2.50 -14 6 4 7.20 2.90 -12 -6 4 4.90 1.50 12 -6 -4 3.80 1.90 -12 -6 4 7.00 1.60 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2.80 -6 6 -4 56.89 3.20 8 -6 4 9.70 2.20 -8 -6 -4 7.00 2.00 -8 -6 -4 6.70 1.80 -8 6 -4 7.30 1.80 -8 6 -4 6.80 2.00 8 6 4 9.00 1.80 -10 -6 -4 12.50 2.70 -10 -6 -4 17.20 2.70 10 -6 4 11.90 2.60 10 6 4 15.00 2.30 -10 6 -4 12.90 2.40 -10 6 -4 13.40 2.70 -13 -7 4 99.59 4.10 -13 -7 4 97.59 4.20 13 -7 -4 105.79 5.10 -13 7 4 102.39 4.60 -13 7 4 104.79 4.30 13 7 -4 103.19 5.00 11 -7 -4 7.40 2.00 -11 -7 4 8.80 1.60 -11 -7 4 9.70 1.70 11 7 -4 9.80 2.00 -11 7 4 8.10 1.80 -11 7 4 8.90 1.70 11 7 -4 5.40 1.50 9 -7 -4 5.70 1.60 -9 -7 4 7.40 1.30 9 -7 -4 3.90 1.20 9 7 -4 3.60 1.30 -9 7 4 1.40 0.90 -9 7 4 3.90 1.40 9 7 -4 3.20 1.40 -7 -7 4 132.59 4.00 -7 -7 4 137.99 3.50 7 -7 -4 140.29 4.00 -7 7 4 134.99 3.50 7 7 -4 138.79 4.10 -7 7 4 135.69 3.70 5 -7 -4 1.30 0.90 -5 -7 4 1.60 0.80 -5 -7 4 1.10 0.70 -5 7 4 1.20 0.80 5 7 -4 -0.30 0.90 -5 7 4 0.60 0.70 -3 -7 4 33.10 1.70 -3 -7 4 34.30 2.10 3 -7 -4 31.40 2.10 -3 7 4 32.60 1.90 3 7 -4 36.50 2.20 -3 7 4 32.60 1.70 -1 -7 4 70.59 2.70 1 -7 -4 75.39 2.90 1 7 -4 77.69 2.80 1 7 -4 74.39 2.40 -1 7 4 75.39 2.50 1 -7 4 129.69 3.70 -1 -7 -4 123.79 3.60 -1 -7 -4 121.59 4.10 -1 -7 -4 126.79 3.50 -1 7 -4 126.69 3.30 -1 7 -4 127.09 3.40 1 7 4 130.49 3.40 3 -7 4 70.49 3.10 -3 -7 -4 64.49 2.90 -3 -7 -4 70.29 3.60 -3 7 -4 57.09 2.70 3 7 4 61.99 2.70 5 -7 4 246.38 5.80 -5 -7 -4 243.38 6.10 -5 -7 -4 234.58 6.60 -5 7 -4 256.37 7.10 -5 7 -4 257.27 5.80 5 7 4 245.18 5.40 -7 -7 -4 10.90 2.20 7 -7 4 10.30 2.10 7 7 4 8.20 1.90 -7 7 -4 6.70 1.60 -7 7 -4 10.60 1.90 -9 -7 -4 1.50 1.60 9 -7 4 3.20 1.90 -9 -7 -4 3.40 2.10 9 7 4 1.10 1.60 -9 7 -4 1.90 1.60 -9 7 -4 1.10 1.80 -12 -8 4 2.50 1.30 12 -8 -4 1.20 1.80 -12 8 4 1.80 1.30 -12 8 4 3.10 1.60 -10 -8 4 45.00 2.60 10 -8 -4 39.90 2.60 10 -8 -4 40.00 3.10 -10 8 4 43.30 2.60 10 8 -4 39.10 2.80 -10 8 4 45.70 2.90 10 8 -4 41.90 3.20 8 -8 -4 422.66 7.40 -8 -8 4 420.46 7.60 -8 -8 4 428.56 6.60 -8 8 4 430.46 7.20 -8 8 4 430.16 6.80 8 8 -4 441.26 7.60 6 -8 -4 230.28 5.20 -6 -8 4 220.28 4.90 -6 -8 4 230.58 4.30 6 8 -4 222.48 5.10 -6 8 4 228.18 4.70 -6 8 4 224.18 4.30 -4 -8 4 23.80 1.60 4 -8 -4 20.50 1.90 -4 -8 4 20.70 1.80 4 8 -4 23.20 2.10 -4 8 4 23.40 1.60 -4 8 4 22.30 1.70 -2 -8 4 15.90 1.30 -2 -8 4 14.30 1.50 2 -8 -4 17.80 1.80 2 -8 -4 17.00 1.80 2 8 -4 19.70 1.40 2 8 -4 19.20 1.80 -2 8 4 18.50 1.60 -2 8 4 17.10 1.40 0 -8 -4 87.29 3.50 0 -8 -4 86.89 3.20 0 -8 4 85.59 3.10 0 8 4 87.99 2.80 0 8 -4 84.69 3.00 0 8 -4 85.79 2.70 -2 -8 -4 5.30 1.20 -2 -8 -4 4.90 1.20 2 -8 4 4.10 1.30 -2 -8 -4 5.50 1.50 -2 8 -4 9.20 1.40 2 8 4 6.00 1.20 -4 -8 -4 15.80 2.30 4 -8 4 13.10 1.90 -4 -8 -4 11.90 1.90 -4 8 -4 13.40 1.80 4 8 4 13.10 1.70 -6 -8 -4 241.08 6.40 -6 -8 -4 233.08 6.80 6 -8 4 240.08 6.10 6 8 4 232.28 5.70 -6 8 -4 230.88 5.90 -8 -8 -4 72.49 3.90 -8 -8 -4 72.49 4.20 8 -8 4 65.49 4.20 -8 8 -4 72.99 4.10 -8 8 -4 76.89 4.80 8 8 4 68.79 3.70 -10 -8 -4 32.60 3.50 -13 -9 4 7.30 1.80 13 -9 -4 9.50 2.40 -13 9 4 6.30 1.90 -13 9 4 6.60 1.70 11 -9 -4 176.78 5.60 -11 -9 4 171.98 4.90 -11 9 4 173.68 4.70 -11 9 4 158.98 5.10 11 9 -4 166.78 5.10 9 -9 -4 1.70 1.10 -9 -9 4 5.00 1.40 -9 -9 4 1.80 1.00 -9 9 4 1.40 1.20 9 9 -4 3.80 1.30 -9 9 4 2.50 1.10 7 -9 -4 42.20 2.60 -7 -9 4 41.20 2.10 -7 -9 4 42.00 2.60 7 9 -4 44.30 2.70 -7 9 4 43.00 2.10 -7 9 4 42.10 2.50 5 -9 -4 100.39 3.50 -5 -9 4 102.19 3.40 -5 9 4 104.69 3.20 -5 9 4 107.09 2.90 5 9 -4 98.59 3.50 3 -9 -4 7.30 1.30 -3 -9 4 6.70 1.20 3 9 -4 8.10 1.40 3 9 -4 7.20 1.00 -3 9 4 6.50 1.00 -3 9 4 5.30 1.10 -1 -9 4 129.19 3.60 1 -9 -4 120.39 4.00 1 -9 -4 125.69 3.80 1 9 -4 134.29 3.80 -1 9 4 122.49 3.40 1 9 -4 121.79 3.10 -1 -9 -4 15.60 1.80 -1 -9 -4 18.00 1.70 -1 -9 -4 11.70 1.90 1 -9 4 12.40 1.60 -1 9 -4 16.70 1.60 1 9 4 12.40 1.50 -1 9 -4 15.70 1.70 -3 -9 -4 160.28 4.20 3 -9 4 161.98 4.50 -3 -9 -4 160.18 5.20 3 9 4 157.08 4.20 -3 9 -4 168.58 4.40 5 -9 4 11.00 1.90 -5 -9 -4 12.60 2.10 -5 -9 -4 11.00 2.20 -5 9 -4 10.40 1.80 5 9 4 10.70 1.80 -7 -9 -4 3.40 1.90 7 -9 4 1.60 1.70 -7 -9 -4 3.30 1.90 7 9 4 4.20 1.60 -7 9 -4 3.50 1.60 -9 -9 -4 118.29 5.40 -9 -9 -4 120.59 5.10 9 -9 4 127.99 5.50 -9 9 -4 123.89 5.20 9 9 4 130.09 5.00 -12 -10 4 165.08 5.10 -12 10 4 180.28 5.50 -12 10 4 172.08 5.00 10 -10 -4 153.28 5.10 10 -10 -4 150.28 4.50 10 10 -4 152.08 4.80 -10 10 4 153.18 4.30 -10 10 4 153.78 4.80 -8 -10 4 508.75 8.60 -8 -10 4 501.65 7.40 8 -10 -4 505.85 8.40 -8 10 4 489.55 8.10 -8 10 4 500.75 7.40 8 10 -4 522.75 8.70 -6 -10 4 205.58 4.90 6 -10 -4 206.28 5.00 -6 10 4 200.88 4.60 6 10 -4 198.48 5.10 -6 10 4 207.48 4.20 -4 -10 4 371.66 6.40 4 -10 -4 364.56 6.80 4 10 -4 365.46 5.60 4 10 -4 366.36 6.80 -4 10 4 377.06 6.20 -4 10 4 367.66 5.50 2 -10 -4 182.08 4.70 -2 -10 4 186.58 4.40 2 -10 -4 179.48 4.70 -2 10 4 184.28 4.10 2 10 -4 180.48 3.80 -2 10 4 176.88 3.60 2 10 -4 177.28 4.50 0 -10 -4 680.33 10.40 0 -10 -4 654.13 8.70 0 -10 4 683.13 9.30 0 -10 -4 673.73 9.70 0 10 4 674.93 8.90 0 10 -4 674.53 8.70 0 10 -4 663.73 9.30 -2 -10 -4 284.47 6.80 -2 -10 -4 280.17 5.80 -2 -10 -4 283.47 5.70 2 -10 4 285.37 5.90 2 10 4 282.97 5.50 -2 10 -4 280.27 5.60 -4 -10 -4 123.49 5.00 -4 -10 -4 122.49 4.30 4 -10 4 124.39 4.40 -4 10 -4 126.79 4.10 4 10 4 119.49 4.00 6 -10 4 285.17 6.90 -6 -10 -4 281.27 7.60 -6 -10 -4 285.87 7.00 6 10 4 276.47 6.30 -6 10 -4 285.67 6.80 -8 -10 -4 35.30 3.70 8 -10 4 35.10 3.50 -8 -10 -4 31.60 3.40 8 10 4 41.50 3.20 -8 10 -4 38.50 3.50 -13 -11 4 2.90 1.50 -13 11 4 1.70 1.40 -11 -11 4 800.62 11.10 -11 11 4 803.32 12.10 11 11 -4 821.42 12.00 -11 11 4 815.62 11.20 9 -11 -4 282.37 6.10 -9 -11 4 268.07 6.30 9 11 -4 267.27 6.40 -9 11 4 272.07 6.10 -9 11 4 267.57 5.50 7 -11 -4 893.71 12.00 -7 -11 4 897.31 11.90 -7 11 4 909.81 10.60 -7 11 4 910.91 11.60 7 11 -4 878.41 12.10 5 -11 -4 993.50 12.80 -5 -11 4 998.90 12.30 -5 11 4 1004.10 10.90 5 11 -4 992.50 12.80 -5 11 4 1004.20 11.90 3 -11 -4 88.09 3.30 3 -11 -4 87.59 3.50 -3 -11 4 83.49 3.20 3 11 -4 82.09 3.30 -3 11 4 84.09 3.00 3 11 -4 85.79 2.70 -3 11 4 85.49 2.50 1 -11 -4 1977.90 21.10 -1 -11 4 1980.40 19.80 1 -11 -4 1956.10 20.60 1 11 -4 1951.50 19.00 1 11 -4 1941.81 20.20 -1 11 4 1965.30 19.40 1 -11 4 330.47 6.30 -1 -11 -4 338.77 6.60 -1 -11 -4 331.87 6.10 -1 -11 -4 335.17 7.40 -1 11 -4 329.97 6.20 -1 11 -4 328.57 6.00 1 11 4 328.57 6.00 3 -11 4 1969.30 20.80 -3 -11 -4 1976.50 20.90 -3 -11 -4 1972.40 23.00 -3 -11 -4 1969.20 20.50 3 11 4 1972.80 20.30 -3 11 -4 2018.50 20.60 -5 -11 -4 26.20 2.60 5 -11 4 29.40 2.80 -5 -11 -4 24.90 3.00 5 11 4 24.30 2.40 -5 11 -4 31.30 2.80 -7 -11 -4 329.87 8.50 -7 -11 -4 338.67 8.00 7 -11 4 336.87 8.00 -7 11 -4 324.87 7.60 7 11 4 331.37 7.40 -9 -11 -4 523.35 12.20 -9 -11 -4 522.85 10.40 9 -11 4 534.95 12.20 9 11 4 532.15 11.30 -9 11 -4 537.95 12.10 -12 12 4 77.49 4.10 10 -12 -4 28.20 2.60 10 12 -4 38.90 3.10 -10 12 4 33.90 2.70 -10 12 4 34.90 3.00 -8 -12 4 1064.19 13.60 8 -12 -4 1078.19 13.70 -8 12 4 1056.69 12.20 8 12 -4 1063.69 14.00 -8 12 4 1081.29 13.40 -6 -12 4 12.80 1.70 6 -12 -4 12.50 1.80 -6 12 4 12.50 1.80 6 12 -4 9.30 1.70 -4 -12 4 332.27 6.30 4 -12 -4 341.57 6.80 4 12 -4 342.77 5.70 -4 12 4 334.07 6.10 4 12 -4 331.27 6.70 2 -12 -4 59.99 3.10 2 -12 -4 56.99 3.00 -2 -12 4 59.89 2.80 2 12 -4 60.39 3.00 -2 12 4 58.69 2.60 2 12 -4 56.09 2.40 0 -12 -4 928.81 12.40 0 -12 -4 948.81 11.40 0 -12 4 944.61 11.90 0 -12 -4 939.81 13.20 0 12 -4 935.31 11.30 0 12 -4 937.61 12.10 0 12 4 949.71 11.50 -2 -12 -4 398.76 8.50 -2 -12 -4 396.36 7.40 -2 -12 -4 399.26 7.20 2 -12 4 396.56 7.30 -2 12 -4 402.06 7.10 2 12 4 390.76 6.90 -2 12 -4 385.66 6.80 -4 -12 -4 51.99 3.70 4 -12 4 56.79 3.40 -4 -12 -4 59.09 3.20 4 12 4 54.89 3.00 -4 12 -4 56.29 3.10 6 -12 4 465.75 9.30 -6 -12 -4 464.05 9.10 -6 -12 -4 449.66 10.10 6 12 4 468.65 8.60 -6 12 -4 462.65 8.80 8 -12 4 10.30 2.40 -8 -12 -4 7.00 2.30 -8 -12 -4 10.70 2.70 8 12 4 7.50 2.00 -8 12 -4 4.60 1.90 -11 13 4 7.10 1.90 11 13 -4 5.90 1.80 9 -13 -4 26.00 2.60 -9 13 4 25.20 2.70 9 13 -4 20.60 2.40 7 -13 -4 3.00 1.40 7 13 -4 5.90 1.60 -7 13 4 5.10 1.40 -5 -13 4 1.60 1.10 5 -13 -4 1.30 1.20 5 13 -4 0.50 0.80 -5 13 4 -0.80 0.90 5 13 -4 0.60 1.10 3 -13 -4 70.39 3.40 3 -13 -4 72.49 3.20 -3 -13 4 77.19 3.20 -3 13 4 76.79 3.00 3 13 -4 76.09 2.80 3 13 -4 71.79 3.30 1 -13 -4 19.00 2.30 1 -13 -4 18.80 2.20 -1 -13 4 22.00 2.10 1 13 -4 20.10 1.80 1 13 -4 15.60 1.90 -1 13 4 19.00 1.80 -1 -13 -4 52.49 3.40 -1 -13 -4 45.40 2.90 -1 -13 -4 44.40 2.60 1 -13 4 44.20 2.80 -1 13 -4 47.10 2.80 -1 13 -4 47.40 2.70 1 13 4 47.70 2.50 -3 -13 -4 64.29 3.30 -3 -13 -4 64.19 3.30 3 -13 4 66.49 3.50 -3 -13 -4 61.79 3.90 -3 13 -4 62.69 3.20 3 13 4 65.29 3.10 -5 -13 -4 44.80 3.30 5 -13 4 48.20 3.50 -5 -13 -4 51.09 4.00 -5 13 -4 50.99 3.30 5 13 4 52.29 3.20 -7 -13 -4 0.20 1.60 -7 -13 -4 2.10 2.00 7 -13 4 4.50 2.00 7 13 4 1.80 1.60 -7 13 -4 1.90 1.50 -10 14 4 31.70 2.90 10 14 -4 33.20 3.10 8 -14 -4 76.09 3.70 8 14 -4 79.89 3.90 -8 14 4 76.49 3.50 -6 -14 4 25.30 2.30 6 -14 -4 26.40 2.70 -6 14 4 27.50 2.40 6 14 -4 24.80 2.60 6 14 -4 25.00 2.00 4 -14 -4 0.70 1.10 -4 -14 4 3.00 1.20 4 -14 -4 1.80 1.20 4 14 -4 -0.10 0.90 4 14 -4 1.90 1.20 -4 14 4 0.70 1.00 2 -14 -4 13.40 1.90 2 -14 -4 13.30 2.00 -2 -14 4 12.60 1.80 2 14 -4 14.60 2.00 -2 14 4 12.70 1.60 2 14 -4 10.80 1.50 0 -14 -4 6.20 1.50 0 -14 -4 9.10 1.90 0 -14 -4 7.60 1.40 0 -14 4 4.80 1.50 0 14 -4 8.20 1.40 0 14 4 10.10 1.50 0 14 -4 7.40 1.50 -2 -14 -4 17.90 2.50 -2 -14 -4 26.90 2.60 2 -14 4 22.70 2.40 -2 -14 -4 25.60 2.30 2 14 4 25.60 2.30 -2 14 -4 25.80 2.30 -2 14 -4 28.30 2.40 4 -14 4 35.40 3.10 -4 -14 -4 39.90 3.00 -4 -14 -4 40.00 3.70 4 14 4 42.00 2.90 -4 14 -4 35.80 2.90 -6 -14 -4 6.50 2.20 -6 -14 -4 5.50 1.90 6 -14 4 5.70 2.10 -6 14 -4 7.20 1.80 6 14 4 6.70 1.70 -8 -14 -4 1.00 1.90 -8 -14 -4 4.70 2.20 8 -14 4 -0.90 2.50 -8 14 -4 1.40 2.00 8 14 4 -0.30 1.80 -11 15 4 124.79 4.90 11 15 -4 112.29 4.90 9 -15 -4 -0.40 1.40 9 15 -4 3.60 1.60 -9 15 4 0.60 1.30 7 -15 -4 10.40 1.90 7 15 -4 14.40 2.20 -7 15 4 8.30 1.70 5 -15 -4 49.40 3.20 5 15 -4 44.40 2.50 5 15 -4 42.90 3.00 -5 15 4 42.70 2.60 3 -15 -4 6.70 1.50 3 -15 -4 4.70 1.50 -3 -15 4 4.40 1.40 3 15 -4 5.10 1.30 3 15 -4 2.80 1.40 -3 15 4 5.80 1.40 1 -15 -4 60.29 3.40 -1 -15 4 65.29 3.20 1 -15 -4 67.49 3.60 -1 15 4 67.49 3.00 1 15 -4 68.39 3.40 1 15 -4 64.69 2.90 -1 -15 -4 19.70 2.10 1 -15 4 15.80 2.10 -1 -15 -4 20.30 2.60 -1 -15 -4 19.30 2.30 -1 15 -4 19.10 2.00 1 15 4 20.10 2.10 -1 15 -4 20.80 2.20 -3 -15 -4 188.18 6.40 -3 -15 -4 202.08 5.50 3 -15 4 191.78 5.60 -3 -15 -4 183.78 5.30 -3 15 -4 198.28 5.30 3 15 4 198.08 5.20 -5 -15 -4 40.50 3.90 5 -15 4 38.70 3.30 -5 -15 -4 46.40 3.40 -5 15 -4 43.00 3.30 5 15 4 40.00 3.00 -7 -15 -4 0.00 1.80 -7 -15 -4 0.70 1.70 7 -15 4 0.30 2.00 -7 15 -4 0.60 1.50 7 15 4 -0.20 1.50 10 16 -4 2.00 1.60 -10 16 4 0.00 1.40 8 -16 -4 146.69 5.10 8 16 -4 150.68 5.20 -8 16 4 143.89 4.70 6 -16 -4 41.30 3.10 -6 16 4 38.60 2.70 6 16 -4 38.90 2.60 6 16 -4 40.60 3.30 4 -16 -4 22.60 2.60 4 16 -4 23.50 2.10 -4 16 4 20.90 2.10 4 16 -4 20.90 2.40 2 -16 -4 51.89 3.20 -2 -16 4 44.60 2.90 2 -16 -4 49.40 3.20 -2 16 4 43.70 2.60 2 16 -4 48.10 2.60 2 16 -4 50.89 3.10 0 -16 4 19.30 2.20 0 -16 -4 17.60 2.00 0 -16 -4 22.20 2.70 0 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5 1630.04 17.10 -7 5 5 1638.24 17.30 -5 -5 5 458.15 6.70 -5 -5 5 459.35 7.60 5 -5 -5 448.46 7.90 5 5 -5 451.95 7.80 -5 5 5 454.75 6.90 -5 5 5 456.25 6.80 -3 -5 5 1074.29 11.70 -3 -5 5 1066.29 12.70 3 -5 -5 1074.79 13.20 -3 5 5 1065.59 11.80 -3 5 5 1044.30 11.90 3 5 -5 1041.20 13.00 -1 -5 5 287.57 5.60 1 -5 -5 279.77 5.90 1 5 -5 285.57 4.90 -1 5 5 283.37 5.20 1 5 -5 281.57 5.80 -1 -5 -5 401.06 7.00 -1 -5 -5 408.86 6.70 1 -5 5 421.46 7.10 1 5 5 413.26 6.60 -1 5 -5 409.96 6.60 -1 5 -5 408.06 6.90 -3 -5 -5 1342.17 15.80 3 -5 5 1365.26 15.80 -3 5 -5 1343.07 15.50 3 5 5 1355.56 15.20 -5 -5 -5 93.19 4.20 5 -5 5 88.79 4.00 -5 5 -5 97.79 4.10 5 5 5 97.59 3.80 -7 -5 -5 641.74 11.40 7 5 5 652.53 10.40 -7 5 -5 632.34 11.30 12 -6 -5 49.40 4.10 -12 -6 5 43.90 3.10 -12 6 5 44.00 3.10 -12 6 5 38.70 3.30 -10 -6 5 663.63 9.90 10 -6 -5 658.43 10.80 -10 -6 5 646.34 10.90 10 -6 -5 662.13 10.40 10 6 -5 660.33 10.50 -10 6 5 651.83 9.80 -10 6 5 672.93 10.20 -8 -6 5 223.08 5.80 8 -6 -5 233.68 5.70 -8 -6 5 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5.70 1.80 11 -9 -5 8.60 2.30 11 9 -5 6.30 1.90 -11 9 5 5.40 1.70 -11 9 5 4.70 1.50 9 -9 -5 108.79 4.20 -9 -9 5 106.19 3.70 -9 -9 5 108.49 4.30 -9 9 5 108.09 4.10 9 9 -5 104.69 4.30 -9 9 5 104.89 3.70 -7 -9 5 219.48 5.60 7 -9 -5 214.08 5.60 -7 -9 5 214.18 4.60 -7 9 5 203.28 4.70 -7 9 5 210.98 5.10 7 9 -5 208.58 5.60 -5 -9 5 50.09 2.90 5 -9 -5 53.29 3.00 -5 9 5 50.69 2.60 5 9 -5 49.20 3.00 -5 9 5 52.49 2.40 3 -9 -5 4.20 1.30 -3 -9 5 5.70 1.40 -3 9 5 6.10 1.30 3 9 -5 6.10 1.50 -3 9 5 3.90 1.10 1 -9 -5 0.60 1.20 -1 -9 5 1.30 1.20 -1 9 5 0.40 1.00 1 9 -5 1.60 0.90 1 9 -5 0.80 1.10 -1 -9 -5 24.10 2.20 1 -9 5 26.60 2.40 -1 -9 -5 25.00 2.40 1 9 5 23.10 2.10 -1 9 -5 28.10 2.40 -1 9 -5 24.30 2.10 -3 -9 -5 72.29 3.60 3 -9 5 74.59 3.60 3 9 5 73.49 3.30 -3 9 -5 72.59 3.50 5 -9 5 55.89 3.70 -5 -9 -5 45.40 3.50 5 9 5 57.59 3.30 -5 9 -5 48.60 3.40 -7 -9 -5 21.20 2.60 -7 -9 -5 20.90 3.00 7 -9 5 17.00 2.70 7 9 5 16.60 2.30 -7 9 -5 13.60 2.50 -12 -10 5 20.60 2.60 -12 -10 5 20.20 2.40 -12 10 5 20.40 2.80 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106.89 4.60 -8 -12 5 24.20 2.50 8 -12 -5 25.60 2.80 8 12 -5 31.10 3.00 -8 12 5 26.90 2.70 -8 12 5 26.80 2.30 6 -12 -5 36.30 3.20 -6 -12 5 31.30 2.70 -6 12 5 32.90 2.20 6 12 -5 35.60 3.00 -6 12 5 26.50 2.50 4 -12 -5 52.09 3.20 -4 -12 5 51.19 3.00 -4 12 5 51.69 2.40 -4 12 5 53.49 2.80 4 12 -5 48.80 3.10 -2 -12 5 46.00 3.00 2 -12 -5 42.30 3.10 2 12 -5 39.30 2.90 2 12 -5 40.60 2.30 -2 12 5 37.40 2.50 0 -12 -5 37.40 3.20 0 -12 5 36.30 2.80 0 -12 -5 39.30 3.00 0 12 -5 39.40 2.50 0 12 5 34.30 2.40 0 12 -5 35.80 2.70 2 -12 5 126.69 4.60 -2 -12 -5 122.19 4.50 -2 -12 -5 124.19 5.30 -2 -12 -5 123.69 4.40 -2 12 -5 120.09 4.20 2 12 5 127.39 4.30 -4 -12 -5 1.40 1.70 -4 -12 -5 0.50 1.50 4 -12 5 1.90 1.70 4 12 5 0.40 1.40 -4 12 -5 1.00 1.40 -6 -12 -5 41.80 3.80 6 -12 5 44.50 3.90 6 12 5 47.30 3.50 -6 12 -5 43.80 3.70 -11 -13 5 2.30 1.70 -11 13 5 4.70 1.60 -11 13 5 3.60 1.70 11 13 -5 2.80 1.80 9 -13 -5 13.60 2.30 -9 -13 5 12.80 2.10 9 13 -5 19.20 2.60 -9 13 5 16.80 2.40 -9 13 5 17.00 2.00 7 -13 -5 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331.67 8.00 -3 -5 7 341.07 7.50 -3 5 7 351.56 6.80 3 5 -7 353.96 8.10 1 -5 -7 274.87 7.10 -1 -5 7 266.57 6.80 1 5 -7 266.77 6.90 -1 5 7 263.77 6.00 1 -5 7 741.23 11.80 -3 5 -7 15.60 2.80 -10 -6 7 316.57 9.40 -10 6 7 311.07 7.30 -8 -6 7 212.08 5.60 8 -6 -7 201.08 6.30 -8 -6 7 211.68 6.50 8 6 -7 192.38 6.30 -8 6 7 207.88 5.60 -8 6 7 197.58 5.60 -6 -6 7 761.92 12.10 -6 -6 7 746.53 10.80 6 -6 -7 728.63 12.50 6 6 -7 722.83 12.40 -6 6 7 758.22 11.00 -6 6 7 746.63 11.00 4 -6 -7 44.00 3.50 -4 -6 7 38.10 3.30 -4 6 7 44.50 2.90 4 6 -7 38.60 3.40 2 -6 -7 1047.20 15.20 -2 -6 7 1063.29 14.50 2 6 -7 1054.99 15.00 -2 6 7 1051.49 13.40 0 -6 -7 230.58 6.50 0 -6 7 226.98 6.40 0 6 7 226.28 5.80 2 -6 7 248.08 6.90 2 6 7 249.78 7.80 -9 -7 7 55.09 3.50 -9 -7 7 56.89 5.20 9 -7 -7 53.09 3.80 -9 7 7 53.09 3.50 -9 7 7 58.59 3.60 9 7 -7 56.09 4.10 7 -7 -7 8.60 2.20 -7 -7 7 5.10 1.60 -7 -7 7 2.00 1.80 -7 7 7 4.80 1.60 7 7 -7 6.10 2.00 -7 7 7 4.70 1.70 5 -7 -7 2.10 1.70 -5 -7 7 -1.20 1.60 -5 7 7 1.70 1.30 5 7 -7 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29.80 3.10 -1 9 7 29.70 2.80 1 -9 7 75.49 4.50 1 9 7 87.59 4.10 -3 9 -7 55.19 5.20 -8 10 7 -1.40 1.20 -8 10 7 -0.30 1.60 -6 -10 7 0.50 1.80 6 -10 -7 1.90 1.80 -6 10 7 4.60 1.60 6 10 -7 3.20 1.90 -6 10 7 4.20 1.70 4 -10 -7 3.20 1.70 -4 -10 7 0.50 1.70 4 10 -7 2.20 1.70 -4 10 7 1.10 1.50 2 -10 -7 97.39 4.80 -2 -10 7 97.49 4.70 -2 10 7 110.49 4.30 2 10 -7 98.69 4.70 0 -10 -7 13.70 2.50 0 -10 7 17.80 2.60 0 10 7 17.80 2.30 2 10 7 9.10 2.20 7 -11 -7 1.40 2.10 -7 -11 7 -0.20 2.60 -7 11 7 -0.20 1.50 -7 11 7 1.50 1.40 -5 -11 7 22.70 2.90 5 -11 -7 19.80 2.80 5 11 -7 25.40 3.20 -5 11 7 21.20 2.50 -3 -11 7 -0.60 1.70 3 -11 -7 0.40 1.60 3 11 -7 1.20 1.80 -3 11 7 2.00 1.50 -1 -11 7 -0.40 1.70 1 -11 -7 0.10 1.60 1 11 -7 0.30 1.60 -1 11 7 -2.40 1.30 1 11 7 9.30 2.00 6 -12 -7 20.90 3.70 -6 -12 7 13.60 3.30 -6 12 7 26.20 2.90 6 12 -7 20.90 3.80 4 -12 -7 25.30 3.10 -4 -12 7 18.70 2.80 -4 12 7 20.60 2.50 4 12 -7 23.40 3.00 2 -12 -7 33.50 3.60 -2 -12 7 31.80 3.30 2 12 -7 29.60 3.40 -2 12 7 27.10 2.80 0 -12 -7 31.40 3.30 0 12 7 25.00 2.80 -7 13 7 16.50 2.30 -5 13 7 2.60 1.80 3 -13 -7 0.30 1.60 -3 -13 7 0.60 2.20 3 13 -7 3.20 1.90 -3 13 7 3.00 1.60 1 -13 -7 3.70 2.00 1 13 -7 5.90 2.20 -1 13 7 6.50 3.10 2 14 -7 99.79 5.10 4 0 -8 118.79 5.30 2 0 -8 437.96 9.60 -5 -1 8 471.85 9.50 3 -1 -8 6.40 2.00 3 1 -8 4.20 1.90 1 -1 -8 79.89 6.00 -6 -2 8 5.50 2.50 4 -2 -8 0.60 1.70 4 2 -8 2.30 1.80 2 -2 -8 16.50 2.50 -2 -2 8 15.20 2.50 2 2 -8 15.10 2.70 -5 -3 8 76.99 4.60 3 -3 -8 21.50 2.80 3 3 -8 25.30 3.10 1 -3 -8 3.40 1.80 4 4 -8 61.99 5.80 2 -4 -8 51.79 4.00 2 4 -8 59.99 4.10 3 5 -8 4.20 2.60 1 -5 -8 2.50 2.00 2 6 -8 4.80 2.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 68083