data_ML_ON_A_2_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 H1.74 Ca1.98 Cl0.24 Fe1.36 K0.62 Mg3.66 Na0.14 O23.76 Si7.80' _chemical_formula_weight 880.90 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 9.8738(5) _cell_length_b 18.0453(9) _cell_length_c 5.3273(3) _cell_angle_alpha 90 _cell_angle_beta 105.1380(10) _cell_angle_gamma 90 _cell_volume 916.26(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8361 _cell_measurement_theta_min 2.4165 _cell_measurement_theta_max 33.213 _exptl_crystal_description equant _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.193 _exptl_crystal_F_000 874 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.155 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.103 _exptl_absorpt_coefficient_mu 2.601 _shelx_estimated_absorpt_T_min 0.689 _shelx_estimated_absorpt_T_max 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6792 _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 10304 _diffrn_reflns_av_unetI/netI 0.0125 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.257 _diffrn_reflns_theta_max 33.351 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_point_group_measured_fraction_full 0.990 _reflns_number_total 1771 _reflns_number_gt 1727 _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^)+(0.0183P)^2^+0.6350P] 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 0.0076(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1771 _refine_ls_number_parameters 119 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0153 _refine_ls_R_factor_gt 0.0148 _refine_ls_wR_factor_ref 0.0412 _refine_ls_wR_factor_gt 0.0409 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.001 _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 MgM1 Mg 0.000000 0.0902(4) 0.500000 0.00801(14) Uani 0.731(3) 2 d S T P . . FeM1 Fe 0.000000 0.0925(4) 0.500000 0.00801(14) Uani 0.269(3) 2 d S T P . . MgM2 Mg 0.000000 0.17673(2) 0.000000 0.00517(10) Uani 0.773(2) 2 d S T P . . FeM2 Fe 0.000000 0.17673(2) 0.000000 0.00517(10) Uani 0.227(2) 2 d S T P . . MgM3 Mg 0.000000 0.000000 0.000000 0.00734(12) Uani 0.652(3) 4 d S T P . . FeM3 Fe 0.000000 0.000000 0.000000 0.00734(12) Uani 0.348(3) 4 d S T P . . M4 Ca 0.000000 0.28040(2) 0.500000 0.00893(8) Uani 0.9905(19) 2 d S T P . . M4' Fe 0.000000 0.250(3) 0.500000 0.019(7) Uiso 0.0095(19) 2 d S . P . . Si1 Si 0.27944(2) 0.08607(2) 0.30317(4) 0.00670(7) Uani 0.9665(19) 1 d . . P . . Si2 Si 0.29140(2) 0.17387(2) 0.81484(4) 0.00570(7) Uani 0.9833(19) 1 d . . P . . O1 O 0.10434(6) 0.09010(3) 0.21434(11) 0.01052(11) Uani 1 1 d . . . . . O2 O 0.11975(6) 0.17505(3) 0.73674(11) 0.00961(11) Uani 1 1 d . . . . . O3 O 0.10839(13) 0.000000 0.71170(19) 0.00860(16) Uani 0.8819(11) 2 d DS T P . . H3 H 0.017(3) 0.000000 0.66(3) 0.53(11) Uiso 0.88 2 d DS . P . . Cl3 Cl 0.1653(3) 0.000000 0.7392(5) 0.00860(16) Uani 0.1181(11) 2 d S T P . . O4 O 0.36851(6) 0.25123(3) 0.79248(11) 0.01109(11) Uani 1 1 d . . . . . O5 O 0.35075(6) 0.13990(4) 0.11016(11) 0.01144(12) Uani 1 1 d . . . . . O6 O 0.34380(6) 0.11924(4) 0.60788(11) 0.01247(12) Uani 1 1 d . . . . . O7 O 0.33803(10) 0.000000 0.28564(19) 0.01605(17) Uani 1 2 d S T P . . A2M K 0.500000 0.000000 0.000000 0.0887(8) Uani 0.623(7) 4 d S T P . . A2 Na 0.500000 -0.0368(8) 0.000000 0.018(3) Uiso 0.066(5) 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 0.00831(15) 0.0100(3) 0.00627(14) 0.000 0.00282(9) 0.000 FeM1 0.00831(15) 0.0100(3) 0.00627(14) 0.000 0.00282(9) 0.000 MgM2 0.00514(14) 0.00522(14) 0.00535(14) 0.000 0.00172(9) 0.000 FeM2 0.00514(14) 0.00522(14) 0.00535(14) 0.000 0.00172(9) 0.000 MgM3 0.00809(18) 0.00609(17) 0.00709(18) 0.000 0.00062(12) 0.000 FeM3 0.00809(18) 0.00609(17) 0.00709(18) 0.000 0.00062(12) 0.000 M4 0.00986(10) 0.00841(17) 0.01005(10) 0.000 0.00531(7) 0.000 Si1 0.00625(11) 0.00682(11) 0.00686(11) -0.00002(6) 0.00141(7) -0.00068(6) Si2 0.00535(10) 0.00626(10) 0.00570(10) 0.00074(6) 0.00183(7) 0.00001(6) O1 0.0092(2) 0.0139(3) 0.0088(2) -0.00167(18) 0.00287(19) -0.00273(18) O2 0.0067(2) 0.0114(2) 0.0104(2) 0.00145(18) 0.00147(18) 0.00065(18) O3 0.0078(5) 0.0088(3) 0.0086(3) 0.000 0.0013(4) 0.000 Cl3 0.0078(5) 0.0088(3) 0.0086(3) 0.000 0.0013(4) 0.000 O4 0.0133(2) 0.0091(2) 0.0123(2) 0.00074(18) 0.0058(2) -0.00121(19) O5 0.0100(2) 0.0133(3) 0.0101(2) 0.00461(18) 0.00106(19) -0.00008(19) O6 0.0094(2) 0.0151(3) 0.0130(3) -0.00446(19) 0.00310(19) 0.00068(19) O7 0.0130(4) 0.0131(4) 0.0212(4) 0.000 0.0031(3) 0.000 A2M 0.1134(15) 0.0545(17) 0.1457(19) 0.000 0.1185(16) 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 O1 2.0484(6) 2_556 ? MgM1 O1 2.0484(6) . ? MgM1 O3 2.106(6) 5_556 ? MgM1 O3 2.106(6) . ? MgM1 O2 2.134(5) . ? MgM1 O2 2.134(5) 2_556 ? MgM1 Cl3 2.419(5) . ? MgM1 Cl3 2.419(5) 5_556 ? FeM1 O1 2.0489(6) 2_556 ? FeM1 O1 2.0489(6) . ? FeM1 O2 2.104(6) . ? FeM1 O2 2.104(6) 2_556 ? FeM1 O3 2.139(6) 5_556 ? FeM1 O3 2.139(6) . ? FeM1 Cl3 2.447(6) . ? FeM1 Cl3 2.447(6) 5_556 ? MgM2 O4 1.9616(6) 7_556 ? MgM2 O4 1.9616(6) 8_454 ? MgM2 O1 2.0481(6) 2 ? MgM2 O1 2.0481(6) . ? MgM2 O2 2.0572(6) 2_556 ? MgM2 O2 2.0572(6) 1_554 ? MgM3 O3 2.0887(10) 5_556 ? MgM3 O3 2.0887(10) 1_554 ? MgM3 O1 2.0962(6) . ? MgM3 O1 2.0963(6) 5 ? MgM3 O1 2.0963(6) 6 ? MgM3 O1 2.0963(6) 2 ? MgM3 Cl3 2.404(3) 5_556 ? MgM3 Cl3 2.404(3) 1_554 ? FeM3 O3 2.0887(10) 5_556 ? FeM3 O3 2.0887(10) 1_554 ? FeM3 O1 2.0962(6) . ? FeM3 O1 2.0963(6) 5 ? FeM3 O1 2.0963(6) 6 ? FeM3 O1 2.0963(6) 2 ? FeM3 Cl3 2.404(3) 5_556 ? FeM3 Cl3 2.404(3) 1_554 ? M4 M4' 0.54(4) . ? M4 O4 2.3443(6) 8_455 ? M4 O4 2.3443(6) 7_556 ? M4 O2 2.4133(7) 2_556 ? M4 O2 2.4134(7) . ? M4 O6 2.5398(7) 7_556 ? M4 O6 2.5398(7) 8_455 ? M4 O5 2.6371(6) 7_556 ? M4' O2 2.02(3) 2_556 ? M4' O2 2.02(3) . ? M4' O4 2.2740(9) 8_455 ? M4' O4 2.2740(9) 7_556 ? Si1 O7 1.6685(4) . ? Si1 O1 1.6707(6) . ? Si1 O6 1.6907(6) . ? Si1 O5 1.6955(6) . ? Si2 O4 1.6094(6) . ? Si2 O2 1.6363(6) . ? Si2 O5 1.6470(6) 1_556 ? Si2 O6 1.6592(6) . ? O3 Cl3 0.542(2) . ? Cl3 A2M 3.233(3) 1_556 ? Cl3 A2 3.301(4) 5_656 ? Cl3 A2 3.301(4) 1_556 ? O5 A2 2.536(10) 5_655 ? O5 A2M 3.0563(6) . ? O6 A2 2.697(8) 5_656 ? O6 A2M 3.1129(6) 1_556 ? O7 A2M 2.4788(10) . ? O7 A2 2.566(4) . ? O7 A2 2.566(4) 5_655 ? A2M A2 0.663(14) . ? A2M A2 0.663(14) 5_655 ? A2 A2 1.33(3) 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 O1 MgM1 O1 179.9(4) 2_556 . ? O1 MgM1 O3 96.50(18) 2_556 5_556 ? O1 MgM1 O3 83.41(14) . 5_556 ? O1 MgM1 O3 83.41(14) 2_556 . ? O1 MgM1 O3 96.50(18) . . ? O3 MgM1 O3 78.8(3) 5_556 . ? O1 MgM1 O2 82.54(13) 2_556 . ? O1 MgM1 O2 97.54(16) . . ? O3 MgM1 O2 175.2(3) 5_556 . ? O3 MgM1 O2 96.45(3) . . ? O1 MgM1 O2 97.54(16) 2_556 2_556 ? O1 MgM1 O2 82.54(13) . 2_556 ? O3 MgM1 O2 96.45(3) 5_556 2_556 ? O3 MgM1 O2 175.2(3) . 2_556 ? O2 MgM1 O2 88.3(3) . 2_556 ? O1 MgM1 Cl3 90.52(15) 2_556 . ? O1 MgM1 Cl3 89.40(15) . . ? O3 MgM1 Cl3 86.6(3) 5_556 . ? O3 MgM1 Cl3 11.27(5) . . ? O2 MgM1 Cl3 88.74(5) . . ? O2 MgM1 Cl3 170.98(12) 2_556 . ? O1 MgM1 Cl3 89.40(15) 2_556 5_556 ? O1 MgM1 Cl3 90.52(15) . 5_556 ? O3 MgM1 Cl3 11.27(5) 5_556 5_556 ? O3 MgM1 Cl3 86.6(3) . 5_556 ? O2 MgM1 Cl3 170.98(12) . 5_556 ? O2 MgM1 Cl3 88.74(5) 2_556 5_556 ? Cl3 MgM1 Cl3 95.4(3) . 5_556 ? O1 FeM1 O1 177.6(4) 2_556 . ? O1 FeM1 O2 83.26(14) 2_556 . ? O1 FeM1 O2 98.48(18) . . ? O1 FeM1 O2 98.47(18) 2_556 2_556 ? O1 FeM1 O2 83.26(14) . 2_556 ? O2 FeM1 O2 89.9(3) . 2_556 ? O1 FeM1 O3 95.5(2) 2_556 5_556 ? O1 FeM1 O3 82.60(16) . 5_556 ? O2 FeM1 O3 173.7(3) . 5_556 ? O2 FeM1 O3 96.37(3) 2_556 5_556 ? O1 FeM1 O3 82.60(16) 2_556 . ? O1 FeM1 O3 95.5(2) . . ? O2 FeM1 O3 96.37(3) . . ? O2 FeM1 O3 173.7(3) 2_556 . ? O3 FeM1 O3 77.4(3) 5_556 . ? O1 FeM1 Cl3 89.72(17) 2_556 . ? O1 FeM1 Cl3 88.62(16) . . ? O2 FeM1 Cl3 88.67(5) . . ? O2 FeM1 Cl3 171.45(9) 2_556 . ? O3 FeM1 Cl3 85.2(3) 5_556 . ? O3 FeM1 Cl3 11.19(5) . . ? O1 FeM1 Cl3 88.62(16) 2_556 5_556 ? O1 FeM1 Cl3 89.72(17) . 5_556 ? O2 FeM1 Cl3 171.45(9) . 5_556 ? O2 FeM1 Cl3 88.67(5) 2_556 5_556 ? O3 FeM1 Cl3 11.19(5) 5_556 5_556 ? O3 FeM1 Cl3 85.2(3) . 5_556 ? Cl3 FeM1 Cl3 94.0(3) . 5_556 ? O4 MgM2 O4 96.99(4) 7_556 8_454 ? O4 MgM2 O1 169.28(3) 7_556 2 ? O4 MgM2 O1 91.67(2) 8_454 2 ? O4 MgM2 O1 91.67(2) 7_556 . ? O4 MgM2 O1 169.28(2) 8_454 . ? O1 MgM2 O1 80.49(3) 2 . ? O4 MgM2 O2 92.25(2) 7_556 2_556 ? O4 MgM2 O2 88.87(2) 8_454 2_556 ? O1 MgM2 O2 94.23(2) 2 2_556 ? O1 MgM2 O2 84.47(2) . 2_556 ? O4 MgM2 O2 88.87(2) 7_556 1_554 ? O4 MgM2 O2 92.25(2) 8_454 1_554 ? O1 MgM2 O2 84.47(2) 2 1_554 ? O1 MgM2 O2 94.23(2) . 1_554 ? O2 MgM2 O2 178.31(4) 2_556 1_554 ? O3 MgM3 O3 180.00(5) 5_556 1_554 ? O3 MgM3 O1 82.69(3) 5_556 . ? O3 MgM3 O1 97.31(3) 1_554 . ? O3 MgM3 O1 97.31(3) 5_556 5 ? O3 MgM3 O1 82.69(3) 1_554 5 ? O1 MgM3 O1 180.0 . 5 ? O3 MgM3 O1 82.69(3) 5_556 6 ? O3 MgM3 O1 97.31(3) 1_554 6 ? O1 MgM3 O1 101.72(3) . 6 ? O1 MgM3 O1 78.28(3) 5 6 ? O3 MgM3 O1 97.31(3) 5_556 2 ? O3 MgM3 O1 82.69(3) 1_554 2 ? O1 MgM3 O1 78.28(3) . 2 ? O1 MgM3 O1 101.72(3) 5 2 ? O1 MgM3 O1 180.00(4) 6 2 ? O3 MgM3 Cl3 11.30(6) 5_556 5_556 ? O3 MgM3 Cl3 168.70(6) 1_554 5_556 ? O1 MgM3 Cl3 89.79(4) . 5_556 ? O1 MgM3 Cl3 90.21(4) 5 5_556 ? O1 MgM3 Cl3 89.79(4) 6 5_556 ? O1 MgM3 Cl3 90.21(4) 2 5_556 ? O3 MgM3 Cl3 168.70(6) 5_556 1_554 ? O3 MgM3 Cl3 11.30(6) 1_554 1_554 ? O1 MgM3 Cl3 90.21(4) . 1_554 ? O1 MgM3 Cl3 89.79(4) 5 1_554 ? O1 MgM3 Cl3 90.21(4) 6 1_554 ? O1 MgM3 Cl3 89.79(4) 2 1_554 ? Cl3 MgM3 Cl3 180.00(8) 5_556 1_554 ? O3 FeM3 O3 180.00(5) 5_556 1_554 ? O3 FeM3 O1 82.69(3) 5_556 . ? O3 FeM3 O1 97.31(3) 1_554 . ? O3 FeM3 O1 97.31(3) 5_556 5 ? O3 FeM3 O1 82.69(3) 1_554 5 ? O1 FeM3 O1 180.0 . 5 ? O3 FeM3 O1 82.69(3) 5_556 6 ? O3 FeM3 O1 97.31(3) 1_554 6 ? O1 FeM3 O1 101.72(3) . 6 ? O1 FeM3 O1 78.28(3) 5 6 ? O3 FeM3 O1 97.31(3) 5_556 2 ? O3 FeM3 O1 82.69(3) 1_554 2 ? O1 FeM3 O1 78.28(3) . 2 ? O1 FeM3 O1 101.72(3) 5 2 ? O1 FeM3 O1 180.00(4) 6 2 ? O3 FeM3 Cl3 11.30(6) 5_556 5_556 ? O3 FeM3 Cl3 168.70(6) 1_554 5_556 ? O1 FeM3 Cl3 89.79(4) . 5_556 ? O1 FeM3 Cl3 90.21(4) 5 5_556 ? O1 FeM3 Cl3 89.79(4) 6 5_556 ? O1 FeM3 Cl3 90.21(4) 2 5_556 ? O3 FeM3 Cl3 168.70(6) 5_556 1_554 ? O3 FeM3 Cl3 11.30(6) 1_554 1_554 ? O1 FeM3 Cl3 90.21(4) . 1_554 ? O1 FeM3 Cl3 89.79(4) 5 1_554 ? O1 FeM3 Cl3 90.21(4) 6 1_554 ? O1 FeM3 Cl3 89.79(4) 2 1_554 ? Cl3 FeM3 Cl3 180.00(8) 5_556 1_554 ? M4' M4 O4 75.908(16) . 8_455 ? M4' M4 O4 75.91(2) . 7_556 ? O4 M4 O4 151.82(3) 8_455 7_556 ? M4' M4 O2 38.022(15) . 2_556 ? O4 M4 O2 82.80(2) 8_455 2_556 ? O4 M4 O2 75.03(2) 7_556 2_556 ? M4' M4 O2 38.021(17) . . ? O4 M4 O2 75.03(2) 8_455 . ? O4 M4 O2 82.80(2) 7_556 . ? O2 M4 O2 76.04(3) 2_556 . ? M4' M4 O6 135.477(19) . 7_556 ? O4 M4 O6 142.98(2) 8_455 7_556 ? O4 M4 O6 63.18(2) 7_556 7_556 ? O2 M4 O6 133.392(19) 2_556 7_556 ? O2 M4 O6 115.870(19) . 7_556 ? M4' M4 O6 135.477(14) . 8_455 ? O4 M4 O6 63.18(2) 8_455 8_455 ? O4 M4 O6 142.98(2) 7_556 8_455 ? O2 M4 O6 115.869(19) 2_556 8_455 ? O2 M4 O6 133.393(19) . 8_455 ? O6 M4 O6 89.05(3) 7_556 8_455 ? M4' M4 O5 123.048(17) . 7_556 ? O4 M4 O5 84.37(2) 8_455 7_556 ? O4 M4 O5 111.32(2) 7_556 7_556 ? O2 M4 O5 159.70(2) 2_556 7_556 ? O2 M4 O5 85.487(19) . 7_556 ? O6 M4 O5 62.737(19) 7_556 7_556 ? O6 M4 O5 71.36(2) 8_455 7_556 ? M4 M4' O2 132.5(10) . 2_556 ? M4 M4' O2 132.5(9) . . ? O2 M4' O2 95.0(19) 2_556 . ? M4 M4' O4 90.8(11) . 8_455 ? O2 M4' O4 94.2(9) 2_556 8_455 ? O2 M4' O4 84.8(7) . 8_455 ? M4 M4' O4 90.8(11) . 7_556 ? O2 M4' O4 84.8(7) 2_556 7_556 ? O2 M4' O4 94.2(9) . 7_556 ? O4 M4' O4 178(2) 8_455 7_556 ? M4 M4' FeM1 180.0 . . ? O2 M4' FeM1 47.5(10) 2_556 . ? O2 M4' FeM1 47.5(9) . . ? O4 M4' FeM1 89.2(11) 8_455 . ? O4 M4' FeM1 89.2(11) 7_556 . ? M4 M4' MgM1 180.0 . . ? O2 M4' MgM1 47.5(10) 2_556 . ? O2 M4' MgM1 47.5(9) . . ? O4 M4' MgM1 89.2(11) 8_455 . ? O4 M4' MgM1 89.2(11) 7_556 . ? FeM1 M4' MgM1 0.0 . . ? M4 M4' MgM2 116.5(8) . 1_556 ? O2 M4' MgM2 96.9(13) 2_556 1_556 ? O2 M4' MgM2 43.6(4) . 1_556 ? O4 M4' MgM2 41.2(3) 8_455 1_556 ? O4 M4' MgM2 137.8(12) 7_556 1_556 ? FeM1 M4' MgM2 63.5(8) . 1_556 ? MgM1 M4' MgM2 63.5(8) . 1_556 ? M4 M4' MgM2 116.5(8) . . ? O2 M4' MgM2 43.6(4) 2_556 . ? O2 M4' MgM2 96.9(13) . . ? O4 M4' MgM2 137.8(12) 8_455 . ? O4 M4' MgM2 41.2(3) 7_556 . ? FeM1 M4' MgM2 63.5(8) . . ? MgM1 M4' MgM2 63.5(8) . . ? MgM2 M4' MgM2 126.9(16) 1_556 . ? O7 Si1 O1 111.90(4) . . ? O7 Si1 O6 109.54(4) . . ? O1 Si1 O6 110.99(3) . . ? O7 Si1 O5 107.12(4) . . ? O1 Si1 O5 111.48(3) . . ? O6 Si1 O5 105.54(3) . . ? O4 Si2 O2 116.65(3) . . ? O4 Si2 O5 109.65(3) . 1_556 ? O2 Si2 O5 109.53(3) . 1_556 ? O4 Si2 O6 103.32(3) . . ? O2 Si2 O6 108.71(3) . . ? O5 Si2 O6 108.59(3) 1_556 . ? Si1 O1 MgM2 121.59(3) . . ? Si1 O1 MgM1 118.27(3) . . ? MgM2 O1 MgM1 97.82(16) . . ? Si1 O1 FeM1 118.32(3) . . ? MgM2 O1 FeM1 96.93(17) . . ? MgM1 O1 FeM1 1.2(4) . . ? Si1 O1 MgM3 116.46(3) . . ? MgM2 O1 MgM3 100.62(3) . . ? MgM1 O1 MgM3 97.73(16) . . ? FeM1 O1 MgM3 98.64(17) . . ? Si1 O1 FeM3 116.46(3) . . ? MgM2 O1 FeM3 100.62(3) . . ? MgM1 O1 FeM3 97.73(16) . . ? FeM1 O1 FeM3 98.64(17) . . ? MgM3 O1 FeM3 0.0 . . ? Si2 O2 M4' 124.6(6) . . ? Si2 O2 MgM2 124.64(3) . 1_556 ? M4' O2 MgM2 93.95(8) . 1_556 ? Si2 O2 FeM1 121.72(10) . . ? M4' O2 FeM1 87.5(10) . . ? MgM2 O2 FeM1 94.94(3) 1_556 . ? Si2 O2 MgM1 121.21(9) . . ? M4' O2 MgM1 88.3(10) . . ? MgM2 O2 MgM1 94.88(3) 1_556 . ? FeM1 O2 MgM1 0.8(3) . . ? Si2 O2 M4 118.47(3) . . ? M4' O2 M4 9.5(9) . . ? MgM2 O2 M4 93.11(2) 1_556 . ? FeM1 O2 M4 97.03(15) . . ? MgM1 O2 M4 97.82(14) . . ? Cl3 O3 MgM3 119.7(3) . 1_556 ? Cl3 O3 MgM1 119.35(17) . . ? MgM3 O3 MgM1 96.17(4) 1_556 . ? Cl3 O3 MgM1 119.35(17) . 5_556 ? MgM3 O3 MgM1 96.17(4) 1_556 5_556 ? MgM1 O3 MgM1 101.2(2) . 5_556 ? Cl3 O3 FeM1 118.86(17) . . ? MgM3 O3 FeM1 96.07(4) 1_556 . ? MgM1 O3 FeM1 0.7(3) . . ? MgM1 O3 FeM1 101.92(5) 5_556 . ? O3 Cl3 MgM3 49.0(3) . 1_556 ? O3 Cl3 MgM1 49.38(16) . . ? MgM3 Cl3 MgM1 80.67(8) 1_556 . ? O3 Cl3 MgM1 49.38(16) . 5_556 ? MgM3 Cl3 MgM1 80.67(8) 1_556 5_556 ? MgM1 Cl3 MgM1 84.6(3) . 5_556 ? O3 Cl3 FeM1 49.94(17) . . ? MgM3 Cl3 FeM1 80.78(8) 1_556 . ? MgM1 Cl3 FeM1 0.7(3) . . ? MgM1 Cl3 FeM1 85.32(9) 5_556 . ? O3 Cl3 A2M 170.6(3) . 1_556 ? MgM3 Cl3 A2M 121.57(9) 1_556 1_556 ? MgM1 Cl3 A2M 134.40(12) . 1_556 ? MgM1 Cl3 A2M 134.40(12) 5_556 1_556 ? FeM1 Cl3 A2M 133.76(13) . 1_556 ? O3 Cl3 A2 165.1(3) . 5_656 ? MgM3 Cl3 A2 120.86(9) 1_556 5_656 ? MgM1 Cl3 A2 123.4(3) . 5_656 ? MgM1 Cl3 A2 145.2(3) 5_556 5_656 ? FeM1 Cl3 A2 122.7(3) . 5_656 ? A2M Cl3 A2 11.6(2) 1_556 5_656 ? O3 Cl3 A2 165.1(3) . 1_556 ? MgM3 Cl3 A2 120.86(9) 1_556 1_556 ? MgM1 Cl3 A2 145.2(3) . 1_556 ? MgM1 Cl3 A2 123.4(3) 5_556 1_556 ? FeM1 Cl3 A2 144.6(3) . 1_556 ? A2M Cl3 A2 11.6(2) 1_556 1_556 ? A2 Cl3 A2 23.2(5) 5_656 1_556 ? Si2 O4 MgM2 142.13(4) . 7_556 ? Si2 O4 M4' 113.9(11) . 7_556 ? MgM2 O4 M4' 89.0(8) 7_556 7_556 ? Si2 O4 M4 101.12(3) . 7_556 ? MgM2 O4 M4 97.82(2) 7_556 7_556 ? M4' O4 M4 13.3(11) 7_556 7_556 ? Si2 O5 Si1 133.79(4) 1_554 . ? Si2 O5 A2 97.78(9) 1_554 5_655 ? Si1 O5 A2 94.5(2) . 5_655 ? Si2 O5 M4 122.38(3) 1_554 7_556 ? Si1 O5 M4 94.01(3) . 7_556 ? A2 O5 M4 110.09(10) 5_655 7_556 ? Si2 O5 A2M 101.14(3) 1_554 . ? Si1 O5 A2M 86.60(2) . . ? A2 O5 A2M 8.5(2) 5_655 . ? M4 O5 A2M 113.79(2) 7_556 . ? Si2 O6 Si1 138.08(4) . . ? Si2 O6 M4 92.29(3) . 7_556 ? Si1 O6 M4 97.67(3) . 7_556 ? Si2 O6 A2 91.58(18) . 5_656 ? Si1 O6 A2 122.9(2) . 5_656 ? M4 O6 A2 108.09(17) 7_556 5_656 ? Si2 O6 A2M 98.66(3) . 1_556 ? Si1 O6 A2M 113.31(3) . 1_556 ? M4 O6 A2M 114.90(2) 7_556 1_556 ? A2 O6 A2M 10.2(3) 5_656 1_556 ? Si1 O7 Si1 137.14(6) 6 . ? Si1 O7 A2M 108.85(3) 6 . ? Si1 O7 A2M 108.85(3) . . ? Si1 O7 A2 94.1(3) 6 . ? Si1 O7 A2 123.6(3) . . ? A2M O7 A2 15.0(3) . . ? Si1 O7 A2 123.6(3) 6 5_655 ? Si1 O7 A2 94.1(3) . 5_655 ? A2M O7 A2 15.0(3) . 5_655 ? A2 O7 A2 30.0(6) . 5_655 ? A2 A2M A2 180.0 . 5_655 ? A2 A2M O7 90.0 . 5_655 ? A2 A2M O7 90.0 5_655 5_655 ? A2 A2M O7 90.0 . . ? A2 A2M O7 90.0 5_655 . ? O7 A2M O7 180.0 5_655 . ? A2 A2M O5 34.309(11) . 6 ? A2 A2M O5 145.691(11) 5_655 6 ? O7 A2M O5 122.589(12) 5_655 6 ? O7 A2M O5 57.411(12) . 6 ? A2 A2M O5 145.691(11) . 2_655 ? A2 A2M O5 34.309(11) 5_655 2_655 ? O7 A2M O5 57.411(12) 5_655 2_655 ? O7 A2M O5 122.589(12) . 2_655 ? O5 A2M O5 180.000(13) 6 2_655 ? A2 A2M O5 34.309(11) . 5_655 ? A2 A2M O5 145.691(11) 5_655 5_655 ? O7 A2M O5 57.411(12) 5_655 5_655 ? O7 A2M O5 122.589(12) . 5_655 ? O5 A2M O5 68.62(2) 6 5_655 ? O5 A2M O5 111.38(2) 2_655 5_655 ? A2 A2M O5 145.691(11) . . ? A2 A2M O5 34.309(11) 5_655 . ? O7 A2M O5 122.589(12) 5_655 . ? O7 A2M O5 57.411(12) . . ? O5 A2M O5 111.38(2) 6 . ? O5 A2M O5 68.62(2) 2_655 . ? O5 A2M O5 180.0 5_655 . ? A2 A2M O6 46.269(11) . 6_554 ? A2 A2M O6 133.731(11) 5_655 6_554 ? O7 A2M O6 82.765(19) 5_655 6_554 ? O7 A2M O6 97.235(19) . 6_554 ? O5 A2M O6 51.583(14) 6 6_554 ? O5 A2M O6 128.417(14) 2_655 6_554 ? O5 A2M O6 58.626(16) 5_655 6_554 ? O5 A2M O6 121.374(16) . 6_554 ? A2 A2M O6 133.731(11) . 2_656 ? A2 A2M O6 46.269(11) 5_655 2_656 ? O7 A2M O6 97.235(19) 5_655 2_656 ? O7 A2M O6 82.765(19) . 2_656 ? O5 A2M O6 128.417(14) 6 2_656 ? O5 A2M O6 51.583(14) 2_655 2_656 ? O5 A2M O6 121.374(16) 5_655 2_656 ? O5 A2M O6 58.626(16) . 2_656 ? O6 A2M O6 180.00(3) 6_554 2_656 ? A2 A2M O6 46.269(11) . 5_656 ? A2 A2M O6 133.731(11) 5_655 5_656 ? O7 A2M O6 97.235(19) 5_655 5_656 ? O7 A2M O6 82.765(19) . 5_656 ? O5 A2M O6 58.626(16) 6 5_656 ? O5 A2M O6 121.374(16) 2_655 5_656 ? O5 A2M O6 51.583(14) 5_655 5_656 ? O5 A2M O6 128.417(14) . 5_656 ? O6 A2M O6 92.54(2) 6_554 5_656 ? O6 A2M O6 87.46(2) 2_656 5_656 ? A2 A2M O6 133.731(11) . 1_554 ? A2 A2M O6 46.269(11) 5_655 1_554 ? O7 A2M O6 82.765(19) 5_655 1_554 ? O7 A2M O6 97.235(19) . 1_554 ? O5 A2M O6 121.374(16) 6 1_554 ? O5 A2M O6 58.626(16) 2_655 1_554 ? O5 A2M O6 128.417(14) 5_655 1_554 ? O5 A2M O6 51.583(14) . 1_554 ? O6 A2M O6 87.46(2) 6_554 1_554 ? O6 A2M O6 92.54(2) 2_656 1_554 ? O6 A2M O6 180.000(17) 5_656 1_554 ? A2M A2 A2 0.0 . 5_655 ? A2M A2 O5 137.2(2) . 6 ? A2 A2 O5 137.2(2) 5_655 6 ? A2M A2 O5 137.2(2) . 5_655 ? A2 A2 O5 137.2(2) 5_655 5_655 ? O5 A2 O5 85.6(4) 6 5_655 ? A2M A2 O7 75.0(3) . 5_655 ? A2 A2 O7 75.0(3) 5_655 5_655 ? O5 A2 O7 144.8(5) 6 5_655 ? O5 A2 O7 64.07(9) 5_655 5_655 ? A2M A2 O7 75.0(3) . . ? A2 A2 O7 75.0(3) 5_655 . ? O5 A2 O7 64.07(9) 6 . ? O5 A2 O7 144.8(5) 5_655 . ? O7 A2 O7 150.0(6) 5_655 . ? A2M A2 O6 123.5(3) . 6_554 ? A2 A2 O6 123.5(3) 5_655 6_554 ? O5 A2 O6 61.6(2) 6 6_554 ? O5 A2 O6 70.4(3) 5_655 6_554 ? O7 A2 O6 90.13(10) 5_655 6_554 ? O7 A2 O6 106.44(13) . 6_554 ? A2M A2 O6 123.5(3) . 5_656 ? A2 A2 O6 123.5(3) 5_655 5_656 ? O5 A2 O6 70.4(3) 6 5_656 ? O5 A2 O6 61.6(2) 5_655 5_656 ? O7 A2 O6 106.44(13) 5_655 5_656 ? O7 A2 O6 90.13(10) . 5_656 ? O6 A2 O6 113.0(5) 6_554 5_656 ? A2M A2 Si1 106.4(2) . 6 ? A2 A2 Si1 106.4(2) 5_655 6 ? O5 A2 Si1 32.35(4) 6 6 ? O5 A2 Si1 115.6(5) 5_655 6 ? O7 A2 Si1 174.63(15) 5_655 6 ? O7 A2 Si1 31.79(6) . 6 ? O6 A2 Si1 84.8(2) 6_554 6 ? O6 A2 Si1 77.27(18) 5_656 6 ? A2M A2 Si1 106.4(2) . 5_655 ? A2 A2 Si1 106.4(2) 5_655 5_655 ? O5 A2 Si1 115.6(5) 6 5_655 ? O5 A2 Si1 32.35(4) 5_655 5_655 ? O7 A2 Si1 31.79(6) 5_655 5_655 ? O7 A2 Si1 174.63(15) . 5_655 ? O6 A2 Si1 77.27(18) 6_554 5_655 ? O6 A2 Si1 84.8(2) 5_656 5_655 ? Si1 A2 Si1 147.3(5) 6 5_655 ? A2M A2 Si2 140.52(16) . 6_554 ? A2 A2 Si2 140.52(16) 5_655 6_554 ? O5 A2 Si2 30.60(12) 6 6_554 ? O5 A2 Si2 74.2(3) 5_655 6_554 ? O7 A2 Si2 117.8(3) 5_655 6_554 ? O7 A2 Si2 86.11(17) . 6_554 ? O6 A2 Si2 31.16(12) 6_554 6_554 ? O6 A2 Si2 90.2(4) 5_656 6_554 ? Si1 A2 Si2 57.77(15) 6 6_554 ? Si1 A2 Si2 95.7(3) 5_655 6_554 ? A2M A2 Si2 140.52(16) . 5_656 ? A2 A2 Si2 140.52(16) 5_655 5_656 ? O5 A2 Si2 74.2(3) 6 5_656 ? O5 A2 Si2 30.60(12) 5_655 5_656 ? O7 A2 Si2 86.11(17) 5_655 5_656 ? O7 A2 Si2 117.8(3) . 5_656 ? O6 A2 Si2 90.2(4) 6_554 5_656 ? O6 A2 Si2 31.16(12) 5_656 5_656 ? Si1 A2 Si2 95.7(3) 6 5_656 ? Si1 A2 Si2 57.77(15) 5_655 5_656 ? Si2 A2 Si2 79.0(3) 6_554 5_656 ? _refine_diff_density_max 0.379 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.070 _shelx_res_file ; TITL ML_ON_A_2_0m_c.res in C2/m ML_ON_A_2_0m_c.res created by SHELXL-2018/3 at 14:28:02 on 19-Mar-2020 REM Old TITL ML_ON_A_2_0m in C2/m REM SHELXT solution in C2/m REM R1 0.096, Rweak 0.004, Alpha 0.048, Orientation as input REM Flack x = 0.496 ( 0.008 ) from Parsons' quotients REM Formula found by SHELXT: Al3 Ca4 Cl Mg Na2 O23 Si6 CELL 0.71073 9.8738 18.0453 5.3273 90.000 105.138 90.000 ZERR 2.000 0.0005 0.0009 0.0003 0.000 0.001 0.000 LATT 7 SYMM -X, Y, -Z SFAC O H NA MG SI CA FE CL AL K UNIT 47.5277 3.48 0.27728 7.321 15.5952 3.96132 2.71768 0.47232 0 1.23104 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 293 SIZE 0.103 0.127 0.155 EADP MGM1 FEM1 HTAB EXYZ MGM2 FEM2 EADP MGM2 FEM2 EADP MGM3 FEM3 OMIT 0 0 2 OMIT 4 0 0 OMIT -2 0 1 OMIT 0 4 2 OMIT 1 1 2 OMIT 0 8 0 OMIT 2 2 0 OMIT -2 6 1 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 0.018300 0.635000 EXTI 0.007563 FVAR 0.37161 0.73125 0.77288 0.65156 0.99052 0.96645 0.98330 FVAR 0.88187 0.31159 0.06634 MOLE 1 REM MGM1 4 0.000000 0.090209 0.500000 20.50000 0.00831 0.00996 = 0.00627 0.00000 0.00282 0.00000 FEM1 7 0.000000 0.092513 0.500000 -20.50000 0.00831 0.00996 = 0.00627 0.00000 0.00282 0.00000 MGM2 4 0.000000 0.176734 0.000000 30.50000 0.00514 0.00522 = 0.00535 0.00000 0.00172 0.00000 FEM2 7 0.000000 0.176734 0.000000 -30.50000 0.00514 0.00522 = 0.00535 0.00000 0.00172 0.00000 MGM3 4 0.000000 0.000000 0.000000 40.25000 0.00809 0.00609 = 0.00709 0.00000 0.00062 0.00000 FEM3 7 0.000000 0.000000 0.000000 -40.25000 0.00809 0.00609 = 0.00709 0.00000 0.00062 0.00000 REM REM M4 6 0.000000 0.280404 0.500000 50.50000 0.00986 0.00841 = 0.01005 0.00000 0.00531 0.00000 M4' 7 0.000000 0.250473 0.500000 -50.50000 0.01909 REM REM SI1 5 0.279444 0.086068 0.303175 61.00000 0.00625 0.00682 = 0.00686 -0.00002 0.00141 -0.00068 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 0.291395 0.173865 0.814841 71.00000 0.00535 0.00626 = 0.00570 0.00074 0.00183 0.00001 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 0.104339 0.090100 0.214337 11.00000 0.00919 0.01385 = 0.00881 -0.00167 0.00287 -0.00273 O2 1 0.119751 0.175046 0.736739 11.00000 0.00668 0.01139 = 0.01036 0.00145 0.00147 0.00065 REM O3 1 0.108393 0.000000 0.711704 80.50000 0.00784 0.00882 = 0.00864 0.00000 0.00128 0.00000 H3 2 0.016682 0.000000 0.655971 10.44000 0.52816 CL3 8 0.165296 0.000000 0.739157 -80.50000 0.00784 0.00882 = 0.00864 0.00000 0.00128 0.00000 REM O4 1 0.368508 0.251225 0.792484 11.00000 0.01327 0.00911 = 0.01228 0.00074 0.00582 -0.00121 O5 1 0.350750 0.139900 0.110158 11.00000 0.01005 0.01331 = 0.01008 0.00461 0.00106 -0.00008 O6 1 0.343802 0.119244 0.607877 11.00000 0.00943 0.01507 = 0.01301 -0.00446 0.00310 0.00068 O7 1 0.338029 0.000000 0.285639 10.50000 0.01303 0.01314 = 0.02123 0.00000 0.00314 0.00000 A2M 10 0.500000 0.000000 0.000000 90.50000 0.11341 0.05449 = 0.14570 0.00000 0.11854 0.00000 A2 3 0.500000 -0.036763 0.000000 100.50000 0.01774 REM MOLE 2 HKLF 4 REM ML_ON_A_2_0m_c.res in C2/m REM wR2 = 0.041184, GooF = S = 1.13732, Restrained GooF = 1.13718 for all data REM R1 = 0.014806 for 1727 Fo > 4sig(Fo) and 0.015291 for all 1771 data REM 119 parameters refined using 1 restraints END WGHT 0.0183 0.6353 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.379, deepest hole -0.336, 1-sigma level 0.070 Q1 1 0.5210 -0.0382 0.0879 11.00000 0.05 0.38 Q2 1 0.2132 0.0000 0.7929 10.50000 0.05 0.37 Q3 1 0.1058 0.0000 0.7981 10.50000 0.05 0.36 Q4 1 0.3200 0.1432 0.6987 11.00000 0.05 0.35 Q5 1 0.1262 0.0000 0.6523 10.50000 0.05 0.34 Q6 1 0.3152 0.1609 -0.0195 11.00000 0.05 0.34 Q7 1 0.0903 0.0201 0.7500 11.00000 0.05 0.33 Q8 1 0.2990 0.0403 0.3044 11.00000 0.05 0.31 Q9 1 0.3119 0.1132 0.1764 11.00000 0.05 0.28 Q10 1 0.1975 0.1721 0.7974 11.00000 0.05 0.28 Q11 1 0.3032 0.0983 0.4529 11.00000 0.05 0.27 Q12 1 0.3271 0.2215 0.8387 11.00000 0.05 0.26 Q13 1 0.5306 0.0000 0.1899 10.50000 0.05 0.26 Q14 1 0.0718 0.1724 0.8474 11.00000 0.05 0.26 Q15 1 0.0682 0.0000 0.0033 10.50000 0.05 0.24 Q16 1 0.2964 0.0000 0.3694 10.50000 0.05 0.23 Q17 1 0.0678 0.1279 0.1187 11.00000 0.05 0.23 Q18 1 0.5693 0.0000 0.0667 10.50000 0.05 0.22 Q19 1 0.0000 0.1302 0.5000 10.50000 0.05 0.21 Q20 1 0.3392 0.1076 0.0531 11.00000 0.05 0.21 ; _shelx_res_checksum 68532 _shelx_hkl_file ; 2 0 0 100.79 2.30 2 0 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99.69 3.00 -7 9 4 94.69 3.20 7 9 -4 93.99 3.10 7 9 -4 97.49 3.40 5 -9 -4 305.87 7.50 -5 -9 4 303.57 7.30 5 -9 -4 312.27 7.50 -5 9 4 308.27 7.50 -5 9 4 296.27 7.30 5 9 -4 315.47 7.70 5 9 -4 300.87 7.70 3 -9 -4 25.80 1.20 -3 -9 4 24.40 1.20 3 -9 -4 25.10 1.40 -3 9 4 25.10 1.20 3 9 -4 26.40 1.30 3 9 -4 26.40 1.50 3 9 -4 23.80 1.40 -3 9 4 23.80 1.30 -1 -9 4 470.25 10.40 1 -9 -4 471.65 10.80 1 9 -4 458.15 10.70 -1 9 4 445.86 10.00 -1 9 4 458.25 10.60 1 9 -4 451.05 11.00 -1 9 4 455.45 10.50 1 9 -4 468.85 10.80 1 -9 4 4.30 0.70 -1 -9 -4 5.00 0.80 1 -9 4 3.60 0.50 1 9 4 4.30 0.70 -1 9 -4 3.80 0.70 1 9 4 4.50 0.50 1 9 4 4.60 0.70 -1 9 -4 4.10 0.70 3 -9 4 244.68 6.40 -3 -9 -4 256.87 6.70 3 -9 4 249.88 6.20 3 9 4 257.07 6.10 -3 9 -4 245.08 6.60 3 9 4 251.67 6.40 -3 9 -4 253.67 6.80 -5 -9 -4 4.90 0.80 5 -9 4 3.00 0.60 -5 -9 -4 3.90 0.70 -5 9 -4 3.90 0.80 5 9 4 2.80 0.60 5 9 4 3.30 0.70 -5 9 -4 4.00 0.90 -7 -9 -4 26.20 1.70 -7 -9 -4 26.20 1.70 7 -9 4 25.80 1.50 7 9 4 26.00 1.70 7 9 4 24.50 1.50 -7 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1.10 5 -11 4 10.50 1.00 5 11 4 8.40 1.00 -5 11 -4 9.40 1.20 -5 11 -4 12.30 1.30 5 11 4 8.70 0.90 -7 -11 -4 207.38 6.00 -7 -11 -4 212.68 6.10 7 -11 4 208.18 5.60 7 11 4 203.78 6.00 7 11 4 216.78 5.80 -7 11 -4 203.48 6.30 -9 -11 -4 845.52 19.80 9 -11 4 856.21 19.00 -9 11 -4 841.32 20.60 9 11 4 835.32 20.90 9 11 4 868.11 20.40 -12 -12 4 72.09 2.90 12 -12 -4 74.89 3.40 -12 12 4 79.09 3.30 -12 12 4 70.79 3.00 12 12 -4 75.49 3.30 10 -12 -4 199.48 6.10 -10 -12 4 194.68 5.50 -10 12 4 211.78 5.70 10 12 -4 202.58 6.10 -10 12 4 205.18 6.00 8 -12 -4 1701.03 39.00 -8 -12 4 1860.41 38.60 8 -12 -4 1868.01 38.80 8 12 -4 1763.42 38.70 8 12 -4 1868.91 39.30 -8 12 4 1903.31 38.80 -8 12 4 1702.43 38.90 6 -12 -4 5.30 0.80 -6 -12 4 6.20 0.80 6 -12 -4 6.10 0.90 6 12 -4 7.20 0.90 -6 12 4 7.10 0.80 -6 12 4 6.90 0.90 6 12 -4 6.70 1.00 4 -12 -4 286.87 7.30 -4 -12 4 293.77 7.00 4 -12 -4 293.57 7.10 -4 12 4 278.67 7.10 4 12 -4 291.27 7.50 -4 12 4 288.07 7.20 4 12 -4 283.97 7.40 2 -12 -4 253.87 6.70 -2 -12 4 260.17 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13.90 1.10 5 1 5 12.00 1.10 5 1 5 13.70 1.10 -5 1 -5 14.10 1.40 -7 -1 -5 12.80 1.40 7 -1 5 14.60 1.20 -7 1 -5 12.90 1.40 7 1 5 11.50 1.20 7 1 5 11.80 1.20 -9 -1 -5 87.09 3.80 -9 1 -5 92.69 4.40 -12 -2 5 344.77 9.00 12 -2 -5 328.27 9.20 -12 2 5 339.37 9.00 12 2 -5 339.37 9.30 -10 -2 5 52.39 2.30 10 -2 -5 52.29 2.50 -10 -2 5 48.40 1.90 10 2 -5 46.10 2.50 -10 2 5 48.90 2.30 -8 -2 5 0.10 0.40 -8 -2 5 0.80 0.40 8 -2 -5 2.20 0.70 8 2 -5 0.40 0.50 6 -2 -5 138.89 3.70 -6 -2 5 136.09 3.60 6 -2 -5 133.89 4.10 -6 -2 5 138.59 3.80 6 2 -5 138.89 4.20 -6 2 5 134.79 3.90 -6 2 5 137.49 3.50 -4 -2 5 0.20 0.30 4 -2 -5 0.90 0.40 -4 -2 5 0.80 0.30 4 -2 -5 2.30 0.50 -4 2 5 0.20 0.30 4 2 -5 1.00 0.40 4 2 -5 0.70 0.40 -4 2 5 0.80 0.40 -2 -2 5 612.44 13.50 2 -2 -5 637.74 13.60 2 -2 -5 616.14 14.00 2 2 -5 605.24 13.90 -2 2 5 601.24 13.60 -2 2 5 613.44 13.40 2 2 -5 616.24 13.80 0 -2 -5 255.47 6.60 0 -2 5 253.77 6.10 0 2 5 233.88 6.20 0 2 5 257.47 6.00 0 2 5 256.07 6.00 0 2 -5 238.88 6.50 2 -2 5 314.97 7.70 2 -2 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249.68 6.70 7 -9 -5 259.27 6.60 -7 -9 5 254.27 6.40 7 9 -5 253.17 7.00 -7 9 5 252.47 6.70 -7 9 5 254.57 6.40 5 -9 -5 85.49 2.90 5 -9 -5 83.39 2.90 -5 -9 5 84.09 2.70 5 9 -5 84.59 3.20 5 9 -5 84.39 3.10 -5 9 5 88.89 2.80 -5 9 5 91.49 3.00 3 -9 -5 10.50 1.00 -3 -9 5 9.70 0.90 -3 9 5 8.10 0.90 3 9 -5 8.80 0.90 3 9 -5 8.20 1.00 3 9 -5 9.70 1.20 -1 -9 5 21.40 1.20 1 -9 -5 23.80 1.50 1 9 -5 22.60 1.60 -1 9 5 20.80 1.30 1 9 -5 22.00 1.40 -1 9 5 19.30 1.30 1 9 -5 21.90 1.40 1 -9 5 69.39 2.50 -1 -9 -5 73.09 2.90 1 9 5 83.09 2.80 -1 9 -5 75.89 2.70 -1 9 -5 74.29 3.00 1 9 5 75.19 2.30 1 9 5 68.29 2.60 -1 9 -5 75.29 3.00 -3 -9 -5 127.59 4.30 3 -9 5 127.49 3.80 3 9 5 131.69 3.70 3 9 5 124.79 3.90 -3 9 -5 131.69 4.30 -3 9 -5 127.09 4.40 3 9 5 128.79 4.10 5 -9 5 275.97 6.90 -5 -9 -5 264.77 7.40 -5 9 -5 268.97 7.70 5 9 5 257.87 7.20 5 9 5 267.67 7.10 5 9 5 272.87 6.90 7 -9 5 27.10 1.60 -7 -9 -5 25.20 1.90 -7 -9 -5 27.40 1.80 7 9 5 25.90 1.80 -7 9 -5 27.50 2.10 7 9 5 24.20 1.60 -12 -10 5 47.80 2.20 12 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3.80 0.90 3 13 -7 3.70 0.90 -3 13 7 3.40 0.90 -1 13 7 11.90 2.10 4 14 -7 25.80 2.90 2 14 -7 245.58 7.30 -2 0 8 669.73 15.50 2 0 -8 685.53 16.40 -3 -1 8 21.20 1.50 3 -1 -8 23.00 1.80 -1 1 8 42.30 2.10 -4 -2 8 6.10 0.90 -2 -2 8 51.99 2.40 2 -2 -8 55.49 2.80 2 2 -8 55.49 2.80 -5 -3 8 109.89 3.60 -3 -3 8 39.80 2.00 3 -3 -8 38.70 2.30 -6 -4 8 10.00 1.10 -4 -4 8 249.58 6.70 2 4 -8 65.59 3.20 -5 -5 8 85.99 3.70 3 -5 -8 14.60 1.80 4 -6 -8 43.10 2.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 31228