_audit_creation_method SHELXL-2014 _chemical_name_systematic ; Sodium calcium iron magnesium aluminum silicate fluoride hydroxide * ; _chemical_name_common Pargasite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca2 F0 Fe0 K0 Mg5 Na1 O24 Si8' _chemical_formula_weight 833.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 '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' 'K' 'K' 0.2009 0.2494 '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' 'O' 'O2-' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 9.885(6) _cell_length_b 17.978(12) _cell_length_c 5.283(4) _cell_angle_alpha 90 _cell_angle_beta 105.193(7) _cell_angle_gamma 90 _cell_volume 906.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5310 _cell_measurement_theta_min 4 _cell_measurement_theta_max 60 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.07 _exptl_crystal_F_000 836 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_absorpt_coefficient_mu 1.508 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details Sheldrick2008 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source Rotating-anode _diffrn_measurement_device_type BrukerD8three-circle _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5310 _diffrn_reflns_av_unetI/netI 0.0112 _diffrn_reflns_av_R_equivalents 0.0119 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.266 _diffrn_reflns_theta_max 30.083 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 1376 _reflns_number_gt 1364 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+3.6000P] 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 SHELXL _refine_ls_extinction_coef 0.0451(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1376 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.003 _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 M1 Mg 0.0000 0.08896(4) 0.5000 0.0077(2) Uani 1.014(5) 2 d S T . . . M2 Mg 0.0000 0.17628(4) 0.0000 0.0071(2) Uani 1.026(5) 2 d S T . . . M3 Mg 0.0000 0.0000 0.0000 0.0072(3) Uani 1.016(7) 4 d S T . . . M4 Ca 0.0000 0.27899(2) 0.5000 0.01205(16) Uani 0.968(3) 2 d S T . . . T1 Si 0.28004(4) 0.08506(2) 0.30208(8) 0.00817(14) Uani 1 1 d . . . . . T2 Si 0.28950(4) 0.17281(2) 0.81057(7) 0.00700(14) Uani 1 1 d . . . . . AM Na 0.5382(10) 0.0000 0.086(2) 0.032(2) Uiso 0.234(14) 2 d S . . . . A2 Na 0.0000 0.4764(4) 0.0000 0.032(2) Uiso 0.305(14) 2 d S . . . . O1 O 0.10771(11) 0.08616(6) 0.2179(2) 0.0099(2) Uani 1 1 d . . . . . O2 O 0.11933(11) 0.17190(6) 0.7295(2) 0.0089(2) Uani 1 1 d . . . . . O3 O 0.10702(15) 0.0000 0.7162(3) 0.0100(4) Uani 1.056(7) 2 d S T . . . O4 O 0.36546(12) 0.24983(6) 0.7887(2) 0.0114(2) Uani 1 1 d . . . . . O5 O 0.34947(11) 0.13886(7) 0.1095(2) 0.0124(2) Uani 1 1 d . . . . . O6 O 0.34461(11) 0.11554(7) 0.6093(2) 0.0122(2) Uani 1 1 d . . . . . O7 O 0.34175(17) 0.0000 0.2774(3) 0.0137(3) Uani 1 2 d S T 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 M1 0.0086(4) 0.0080(4) 0.0068(4) 0.000 0.0026(2) 0.000 M2 0.0074(4) 0.0072(4) 0.0071(4) 0.000 0.0025(2) 0.000 M3 0.0077(5) 0.0079(5) 0.0062(5) 0.000 0.0019(3) 0.000 M4 0.0141(2) 0.0115(2) 0.0124(2) 0.000 0.00664(16) 0.000 T1 0.0079(2) 0.0082(2) 0.0081(2) -0.00019(12) 0.00163(14) -0.00052(12) T2 0.0070(2) 0.0075(2) 0.0065(2) 0.00028(12) 0.00183(14) -0.00039(12) O1 0.0083(5) 0.0129(5) 0.0084(5) -0.0007(4) 0.0019(4) -0.0017(4) O2 0.0067(4) 0.0106(5) 0.0093(5) 0.0005(4) 0.0018(4) 0.0001(3) O3 0.0092(7) 0.0097(7) 0.0110(7) 0.000 0.0025(5) 0.000 O4 0.0133(5) 0.0096(5) 0.0120(5) -0.0002(4) 0.0046(4) -0.0031(4) O5 0.0104(5) 0.0163(6) 0.0097(5) 0.0047(4) 0.0011(4) -0.0002(4) O6 0.0101(5) 0.0139(5) 0.0129(5) -0.0043(4) 0.0032(4) 0.0006(4) O7 0.0109(7) 0.0124(7) 0.0176(7) 0.000 0.0034(6) 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 M1 O1 2.0467(15) 2_556 ? M1 O1 2.0467(15) . ? M1 O2 2.0822(14) 2_556 ? M1 O2 2.0822(14) . ? M1 O3 2.0854(14) 5_556 ? M1 O3 2.0854(14) . ? M1 M2 3.0727(19) 1_556 ? M1 M2 3.0727(19) . ? M1 M3 3.0879(18) . ? M1 M3 3.0879(18) 1_556 ? M1 M1 3.199(3) 5_556 ? M1 T1 3.2059(17) . ? M2 O4 2.0004(14) 7_556 ? M2 O4 2.0004(14) 8_454 ? M2 O2 2.0791(15) 1_554 ? M2 O2 2.0791(15) 2_556 ? M2 O1 2.1074(15) . ? M2 O1 2.1075(15) 2 ? M2 M1 3.0727(19) 1_554 ? M2 M3 3.169(2) . ? M2 M4 3.2230(18) . ? M2 M4 3.2230(18) 1_554 ? M2 T1 3.2532(15) . ? M3 O3 2.0488(18) 5_556 ? M3 O3 2.0488(18) 1_554 ? M3 O1 2.0532(14) 5 ? M3 O1 2.0532(14) 6 ? M3 O1 2.0532(14) 2 ? M3 O1 2.0532(14) . ? M3 M1 3.0879(18) 5 ? M3 M1 3.0879(18) 5_556 ? M3 M1 3.0879(18) 1_554 ? M3 M2 3.169(2) 5 ? M4 O4 2.3294(16) 7_556 ? M4 O4 2.3294(16) 8_455 ? M4 O2 2.4122(16) . ? M4 O2 2.4122(16) 2_556 ? M4 O6 2.5987(17) 7_556 ? M4 O6 2.5987(17) 8_455 ? M4 O5 2.6536(17) 7_556 ? M4 O5 2.6536(17) 8_455 ? M4 T2 3.0922(14) 7_556 ? M4 T2 3.0922(14) 8_455 ? M4 M2 3.2230(18) 1_556 ? T1 O1 1.6440(15) . ? T1 O7 1.6641(12) . ? T1 O6 1.6729(16) . ? T1 O5 1.6755(14) . ? T1 A2 3.212(3) 7 ? T1 M4 3.2563(15) 7_556 ? T1 AM 3.419(6) 5_655 ? T1 AM 3.419(6) . ? T2 O4 1.5937(14) . ? T2 O2 1.6235(15) . ? T2 O5 1.6516(15) 1_556 ? T2 O6 1.6708(14) . ? T2 M4 3.0922(14) 7_556 ? T2 A2 3.382(6) 7_556 ? T2 AM 3.516(5) 5_656 ? AM A2 0.661(6) 3_545 ? AM A2 0.661(6) 7 ? AM AM 1.01(2) 5_655 ? AM O7 2.414(6) . ? AM O7 2.506(7) 5_655 ? AM O6 2.698(8) 2_656 ? AM O6 2.698(8) 5_656 ? AM O5 3.021(4) 2_655 ? AM O5 3.021(4) 5_655 ? AM T1 3.419(6) 5_655 ? AM T1 3.419(6) 2_655 ? AM T1 3.419(6) 6 ? A2 AM 0.661(6) 3_455 ? A2 AM 0.661(6) 7 ? A2 A2 0.847(15) 5_565 ? A2 O7 2.445(2) 7 ? A2 O7 2.445(2) 3_455 ? A2 O5 2.701(6) 8_455 ? A2 O5 2.701(6) 7 ? A2 O6 2.773(5) 8_454 ? A2 O6 2.773(5) 7_556 ? A2 T1 3.212(3) 8_455 ? A2 T1 3.212(3) 7 ? A2 T2 3.382(6) 8_454 ? O2 M2 2.0791(15) 1_556 ? O3 M3 2.0488(18) 1_556 ? O3 M1 2.0853(14) 5_556 ? O4 M2 2.0004(14) 7_556 ? O4 M4 2.3294(15) 7_556 ? O5 T2 1.6516(15) 1_554 ? O5 M4 2.6536(16) 7_556 ? O5 A2 2.701(6) 7 ? O5 AM 3.021(4) 5_655 ? O6 M4 2.5987(16) 7_556 ? O6 AM 2.698(8) 5_656 ? O6 A2 2.773(5) 7_556 ? O7 T1 1.6641(12) 6 ? O7 A2 2.445(2) 7 ? O7 A2 2.445(2) 3_545 ? O7 AM 2.506(7) 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 M1 O1 177.18(7) 2_556 . ? O1 M1 O2 96.79(6) 2_556 2_556 ? O1 M1 O2 85.24(6) . 2_556 ? O1 M1 O2 85.24(6) 2_556 . ? O1 M1 O2 96.79(6) . . ? O2 M1 O2 88.53(8) 2_556 . ? O1 M1 O3 95.39(6) 2_556 5_556 ? O1 M1 O3 82.43(6) . 5_556 ? O2 M1 O3 95.83(6) 2_556 5_556 ? O2 M1 O3 175.49(5) . 5_556 ? O1 M1 O3 82.43(6) 2_556 . ? O1 M1 O3 95.39(7) . . ? O2 M1 O3 175.49(5) 2_556 . ? O2 M1 O3 95.83(6) . . ? O3 M1 O3 79.84(8) 5_556 . ? O1 M1 M2 43.06(4) 2_556 1_556 ? O1 M1 M2 139.09(5) . 1_556 ? O2 M1 M2 90.41(6) 2_556 1_556 ? O2 M1 M2 42.37(4) . 1_556 ? O3 M1 M2 138.46(5) 5_556 1_556 ? O3 M1 M2 92.01(6) . 1_556 ? O1 M1 M2 139.09(5) 2_556 . ? O1 M1 M2 43.06(4) . . ? O2 M1 M2 42.37(4) 2_556 . ? O2 M1 M2 90.41(6) . . ? O3 M1 M2 92.01(6) 5_556 . ? O3 M1 M2 138.46(4) . . ? M2 M1 M2 118.56(6) 1_556 . ? O1 M1 M3 136.62(5) 2_556 . ? O1 M1 M3 41.21(4) . . ? O2 M1 M3 89.98(6) 2_556 . ? O2 M1 M3 137.91(4) . . ? O3 M1 M3 41.23(4) 5_556 . ? O3 M1 M3 87.58(6) . . ? M2 M1 M3 179.53(2) 1_556 . ? M2 M1 M3 61.91(5) . . ? O1 M1 M3 41.21(4) 2_556 1_556 ? O1 M1 M3 136.62(5) . 1_556 ? O2 M1 M3 137.91(4) 2_556 1_556 ? O2 M1 M3 89.99(6) . 1_556 ? O3 M1 M3 87.58(6) 5_556 1_556 ? O3 M1 M3 41.23(4) . 1_556 ? M2 M1 M3 61.91(5) 1_556 1_556 ? M2 M1 M3 179.53(2) . 1_556 ? M3 M1 M3 117.61(6) . 1_556 ? O1 M1 M1 88.59(4) 2_556 5_556 ? O1 M1 M1 88.59(4) . 5_556 ? O2 M1 M1 135.74(4) 2_556 5_556 ? O2 M1 M1 135.74(4) . 5_556 ? O3 M1 M1 39.92(4) 5_556 5_556 ? O3 M1 M1 39.92(4) . 5_556 ? M2 M1 M1 120.72(3) 1_556 5_556 ? M2 M1 M1 120.72(3) . 5_556 ? M3 M1 M1 58.81(3) . 5_556 ? M3 M1 M1 58.81(3) 1_556 5_556 ? O1 M1 T1 153.56(3) 2_556 . ? O1 M1 T1 26.31(3) . . ? O2 M1 T1 103.39(5) 2_556 . ? O2 M1 T1 78.45(5) . . ? O3 M1 T1 99.32(5) 5_556 . ? O3 M1 T1 78.72(5) . . ? M2 M1 T1 119.08(2) 1_556 . ? M2 M1 T1 62.37(2) . . ? M3 M1 T1 61.06(2) . . ? M3 M1 T1 117.47(2) 1_556 . ? M1 M1 T1 88.747(14) 5_556 . ? O4 M2 O4 96.77(9) 7_556 8_454 ? O4 M2 O2 89.70(6) 7_556 1_554 ? O4 M2 O2 93.18(6) 8_454 1_554 ? O4 M2 O2 93.18(6) 7_556 2_556 ? O4 M2 O2 89.70(6) 8_454 2_556 ? O2 M2 O2 175.66(7) 1_554 2_556 ? O4 M2 O1 92.23(6) 7_556 . ? O4 M2 O1 169.18(5) 8_454 . ? O2 M2 O1 92.86(6) 1_554 . ? O2 M2 O1 83.80(6) 2_556 . ? O4 M2 O1 169.18(5) 7_556 2 ? O4 M2 O1 92.23(6) 8_454 2 ? O2 M2 O1 83.80(6) 1_554 2 ? O2 M2 O1 92.86(6) 2_556 2 ? O1 M2 O1 79.51(8) . 2 ? O4 M2 M1 90.53(5) 7_556 . ? O4 M2 M1 132.01(4) 8_454 . ? O2 M2 M1 134.37(5) 1_554 . ? O2 M2 M1 42.44(4) 2_556 . ? O1 M2 M1 41.54(4) . . ? O1 M2 M1 87.88(6) 2 . ? O4 M2 M1 132.01(4) 7_556 1_554 ? O4 M2 M1 90.53(5) 8_454 1_554 ? O2 M2 M1 42.44(4) 1_554 1_554 ? O2 M2 M1 134.37(5) 2_556 1_554 ? O1 M2 M1 87.88(6) . 1_554 ? O1 M2 M1 41.54(3) 2 1_554 ? M1 M2 M1 118.56(6) . 1_554 ? O4 M2 M3 131.61(4) 7_556 . ? O4 M2 M3 131.61(4) 8_454 . ? O2 M2 M3 87.83(4) 1_554 . ? O2 M2 M3 87.83(4) 2_556 . ? O1 M2 M3 39.76(4) . . ? O1 M2 M3 39.76(4) 2 . ? M1 M2 M3 59.28(3) . . ? M1 M2 M3 59.28(3) 1_554 . ? O4 M2 M4 45.96(4) 7_556 . ? O4 M2 M4 86.22(6) 8_454 . ? O2 M2 M4 134.98(4) 1_554 . ? O2 M2 M4 48.44(4) 2_556 . ? O1 M2 M4 95.81(6) . . ? O1 M2 M4 141.23(4) 2 . ? M1 M2 M4 65.68(5) . . ? M1 M2 M4 175.77(2) 1_554 . ? M3 M2 M4 124.96(3) . . ? O4 M2 M4 86.22(6) 7_556 1_554 ? O4 M2 M4 45.96(4) 8_454 1_554 ? O2 M2 M4 48.44(4) 1_554 1_554 ? O2 M2 M4 134.98(4) 2_556 1_554 ? O1 M2 M4 141.23(4) . 1_554 ? O1 M2 M4 95.81(6) 2 1_554 ? M1 M2 M4 175.77(2) . 1_554 ? M1 M2 M4 65.68(5) 1_554 1_554 ? M3 M2 M4 124.96(3) . 1_554 ? M4 M2 M4 110.09(6) . 1_554 ? O4 M2 T1 72.86(6) 7_556 . ? O4 M2 T1 164.65(4) 8_454 . ? O2 M2 T1 75.82(5) 1_554 . ? O2 M2 T1 101.94(5) 2_556 . ? O1 M2 T1 26.02(3) . . ? O1 M2 T1 97.10(5) 2 . ? M1 M2 T1 60.82(3) . . ? M1 M2 T1 88.42(4) 1_554 . ? M3 M2 T1 59.73(2) . . ? M4 M2 T1 93.99(4) . . ? M4 M2 T1 120.54(3) 1_554 . ? O3 M3 O3 180.00(6) 5_556 1_554 ? O3 M3 O1 96.83(5) 5_556 5 ? O3 M3 O1 83.17(5) 1_554 5 ? O3 M3 O1 83.17(5) 5_556 6 ? O3 M3 O1 96.83(5) 1_554 6 ? O1 M3 O1 82.05(8) 5 6 ? O3 M3 O1 96.83(5) 5_556 2 ? O3 M3 O1 83.17(5) 1_554 2 ? O1 M3 O1 97.95(8) 5 2 ? O1 M3 O1 180.00(7) 6 2 ? O3 M3 O1 83.17(5) 5_556 . ? O3 M3 O1 96.83(5) 1_554 . ? O1 M3 O1 180.0 5 . ? O1 M3 O1 97.95(8) 6 . ? O1 M3 O1 82.05(8) 2 . ? O3 M3 M1 137.87(4) 5_556 5 ? O3 M3 M1 42.13(4) 1_554 5 ? O1 M3 M1 41.06(4) 5 5 ? O1 M3 M1 88.43(6) 6 5 ? O1 M3 M1 91.57(6) 2 5 ? O1 M3 M1 138.94(4) . 5 ? O3 M3 M1 42.13(4) 5_556 5_556 ? O3 M3 M1 137.87(4) 1_554 5_556 ? O1 M3 M1 88.43(6) 5 5_556 ? O1 M3 M1 41.06(4) 6 5_556 ? O1 M3 M1 138.94(4) 2 5_556 ? O1 M3 M1 91.57(6) . 5_556 ? M1 M3 M1 117.61(6) 5 5_556 ? O3 M3 M1 137.87(4) 5_556 1_554 ? O3 M3 M1 42.13(4) 1_554 1_554 ? O1 M3 M1 91.57(6) 5 1_554 ? O1 M3 M1 138.94(4) 6 1_554 ? O1 M3 M1 41.06(4) 2 1_554 ? O1 M3 M1 88.43(6) . 1_554 ? M1 M3 M1 62.39(6) 5 1_554 ? M1 M3 M1 180.00(2) 5_556 1_554 ? O3 M3 M1 42.13(4) 5_556 . ? O3 M3 M1 137.87(4) 1_554 . ? O1 M3 M1 138.94(4) 5 . ? O1 M3 M1 91.57(6) 6 . ? O1 M3 M1 88.43(6) 2 . ? O1 M3 M1 41.06(4) . . ? M1 M3 M1 180.0 5 . ? M1 M3 M1 62.39(6) 5_556 . ? M1 M3 M1 117.61(6) 1_554 . ? O3 M3 M2 90.0 5_556 5 ? O3 M3 M2 90.0 1_554 5 ? O1 M3 M2 41.03(4) 5 5 ? O1 M3 M2 41.03(4) 6 5 ? O1 M3 M2 138.97(4) 2 5 ? O1 M3 M2 138.97(4) . 5 ? M1 M3 M2 58.81(3) 5 5 ? M1 M3 M2 58.81(3) 5_556 5 ? M1 M3 M2 121.19(3) 1_554 5 ? M1 M3 M2 121.19(3) . 5 ? O3 M3 M2 90.0 5_556 . ? O3 M3 M2 90.0 1_554 . ? O1 M3 M2 138.97(4) 5 . ? O1 M3 M2 138.97(4) 6 . ? O1 M3 M2 41.03(4) 2 . ? O1 M3 M2 41.03(4) . . ? M1 M3 M2 121.19(3) 5 . ? M1 M3 M2 121.19(3) 5_556 . ? M1 M3 M2 58.81(3) 1_554 . ? M1 M3 M2 58.81(3) . . ? M2 M3 M2 180.0 5 . ? O4 M4 O4 154.30(6) 7_556 8_455 ? O4 M4 O2 82.17(5) 7_556 . ? O4 M4 O2 77.36(5) 8_455 . ? O4 M4 O2 77.36(5) 7_556 2_556 ? O4 M4 O2 82.17(5) 8_455 2_556 ? O2 M4 O2 74.09(7) . 2_556 ? O4 M4 O6 62.92(5) 7_556 7_556 ? O4 M4 O6 141.25(4) 8_455 7_556 ? O2 M4 O6 117.03(5) . 7_556 ? O2 M4 O6 135.27(5) 2_556 7_556 ? O4 M4 O6 141.25(4) 7_556 8_455 ? O4 M4 O6 62.92(5) 8_455 8_455 ? O2 M4 O6 135.26(5) . 8_455 ? O2 M4 O6 117.03(5) 2_556 8_455 ? O6 M4 O6 86.28(7) 7_556 8_455 ? O4 M4 O5 109.43(6) 7_556 7_556 ? O4 M4 O5 85.12(6) 8_455 7_556 ? O2 M4 O5 87.29(6) . 7_556 ? O2 M4 O5 159.34(4) 2_556 7_556 ? O6 M4 O5 61.50(5) 7_556 7_556 ? O6 M4 O5 70.42(5) 8_455 7_556 ? O4 M4 O5 85.12(6) 7_556 8_455 ? O4 M4 O5 109.43(6) 8_455 8_455 ? O2 M4 O5 159.34(4) . 8_455 ? O2 M4 O5 87.29(6) 2_556 8_455 ? O6 M4 O5 70.42(5) 7_556 8_455 ? O6 M4 O5 61.50(5) 8_455 8_455 ? O5 M4 O5 112.37(7) 7_556 8_455 ? O4 M4 T2 30.22(4) 7_556 7_556 ? O4 M4 T2 171.40(3) 8_455 7_556 ? O2 M4 T2 100.48(4) . 7_556 ? O2 M4 T2 105.39(5) 2_556 7_556 ? O6 M4 T2 32.71(3) 7_556 7_556 ? O6 M4 T2 115.63(5) 8_455 7_556 ? O5 M4 T2 86.46(5) 7_556 7_556 ? O5 M4 T2 75.51(5) 8_455 7_556 ? O4 M4 T2 171.40(3) 7_556 8_455 ? O4 M4 T2 30.22(4) 8_455 8_455 ? O2 M4 T2 105.39(5) . 8_455 ? O2 M4 T2 100.48(4) 2_556 8_455 ? O6 M4 T2 115.63(5) 7_556 8_455 ? O6 M4 T2 32.71(3) 8_455 8_455 ? O5 M4 T2 75.51(5) 7_556 8_455 ? O5 M4 T2 86.46(5) 8_455 8_455 ? T2 M4 T2 147.46(3) 7_556 8_455 ? O4 M4 M2 38.13(4) 7_556 . ? O4 M4 M2 122.13(5) 8_455 . ? O2 M4 M2 81.35(6) . . ? O2 M4 M2 40.16(3) 2_556 . ? O6 M4 M2 96.26(5) 7_556 . ? O6 M4 M2 136.64(3) 8_455 . ? O5 M4 M2 146.67(3) 7_556 . ? O5 M4 M2 78.59(6) 8_455 . ? T2 M4 M2 65.24(4) 7_556 . ? T2 M4 M2 137.73(2) 8_455 . ? O4 M4 M2 122.13(5) 7_556 1_556 ? O4 M4 M2 38.13(3) 8_455 1_556 ? O2 M4 M2 40.16(3) . 1_556 ? O2 M4 M2 81.35(6) 2_556 1_556 ? O6 M4 M2 136.64(3) 7_556 1_556 ? O6 M4 M2 96.26(5) 8_455 1_556 ? O5 M4 M2 78.59(6) 7_556 1_556 ? O5 M4 M2 146.67(3) 8_455 1_556 ? T2 M4 M2 137.73(2) 7_556 1_556 ? T2 M4 M2 65.24(4) 8_455 1_556 ? M2 M4 M2 110.09(6) . 1_556 ? O1 T1 O7 111.41(7) . . ? O1 T1 O6 111.31(6) . . ? O7 T1 O6 108.81(7) . . ? O1 T1 O5 112.90(6) . . ? O7 T1 O5 105.43(8) . . ? O6 T1 O5 106.68(7) . . ? O1 T1 M3 34.00(4) . . ? O7 T1 M3 78.97(7) . . ? O6 T1 M3 134.50(4) . . ? O5 T1 M3 114.31(6) . . ? O1 T1 M1 33.48(5) . . ? O7 T1 M1 114.28(6) . . ? O6 T1 M1 79.57(5) . . ? O5 T1 M1 135.35(5) . . ? M3 T1 M1 57.65(4) . . ? O1 T1 A2 131.16(7) . 7 ? O7 T1 A2 48.32(14) . 7 ? O6 T1 A2 117.32(6) . 7 ? O5 T1 A2 57.23(14) . 7 ? M3 T1 A2 101.40(9) . 7 ? M1 T1 A2 157.58(11) . 7 ? O1 T1 M2 34.22(4) . . ? O7 T1 M2 135.00(6) . . ? O6 T1 M2 111.72(5) . . ? O5 T1 M2 80.93(6) . . ? M3 T1 M2 58.83(4) . . ? M1 T1 M2 56.81(4) . . ? A2 T1 M2 121.98(7) 7 . ? O1 T1 M4 129.43(5) . 7_556 ? O7 T1 M4 119.16(7) . 7_556 ? O6 T1 M4 52.39(4) . 7_556 ? O5 T1 M4 54.29(5) . 7_556 ? M3 T1 M4 159.511(16) . 7_556 ? M1 T1 M4 116.09(3) . 7_556 ? A2 T1 M4 86.32(11) 7 7_556 ? M2 T1 M4 100.95(5) . 7_556 ? O1 T1 AM 120.9(2) . 5_655 ? O7 T1 AM 44.04(10) . 5_655 ? O6 T1 AM 126.9(2) . 5_655 ? O5 T1 AM 62.06(8) . 5_655 ? M3 T1 AM 90.53(17) . 5_655 ? M1 T1 AM 147.08(14) . 5_655 ? A2 T1 AM 10.87(11) 7 5_655 ? M2 T1 AM 116.4(2) . 5_655 ? M4 T1 AM 96.69(13) 7_556 5_655 ? O1 T1 AM 136.56(19) . . ? O7 T1 AM 40.69(7) . . ? O6 T1 AM 110.0(2) . . ? O5 T1 AM 66.09(10) . . ? M3 T1 AM 104.09(17) . . ? M1 T1 AM 154.54(6) . . ? A2 T1 AM 10.87(11) 7 . ? M2 T1 AM 132.46(19) . . ? M4 T1 AM 87.08(13) 7_556 . ? AM T1 AM 17.1(4) 5_655 . ? O4 T2 O2 117.71(6) . . ? O4 T2 O5 109.43(6) . 1_556 ? O2 T2 O5 109.62(6) . 1_556 ? O4 T2 O6 104.53(7) . . ? O2 T2 O6 108.30(6) . . ? O5 T2 O6 106.60(8) 1_556 . ? O4 T2 M4 47.37(4) . 7_556 ? O2 T2 M4 131.12(5) . 7_556 ? O5 T2 M4 119.22(6) 1_556 7_556 ? O6 T2 M4 57.18(5) . 7_556 ? O4 T2 A2 116.47(10) . 7_556 ? O2 T2 A2 125.77(9) . 7_556 ? O5 T2 A2 52.05(5) 1_556 7_556 ? O6 T2 A2 54.65(6) . 7_556 ? M4 T2 A2 86.10(6) 7_556 7_556 ? O4 T2 M4 80.43(6) . . ? O2 T2 M4 38.05(4) . . ? O5 T2 M4 134.39(4) 1_556 . ? O6 T2 M4 113.81(6) . . ? M4 T2 M4 100.43(5) 7_556 . ? A2 T2 M4 160.49(8) 7_556 . ? O4 T2 AM 124.11(13) . 5_656 ? O2 T2 AM 117.28(15) . 5_656 ? O5 T2 AM 59.10(17) 1_556 5_656 ? O6 T2 AM 47.89(16) . 5_656 ? M4 T2 AM 87.97(10) 7_556 5_656 ? A2 T2 AM 10.77(13) 7_556 5_656 ? M4 T2 AM 149.85(18) . 5_656 ? A2 AM A2 80(2) 3_545 7 ? A2 AM AM 39.9(11) 3_545 5_655 ? A2 AM AM 39.9(11) 7 5_655 ? A2 AM O7 84.8(6) 3_545 . ? A2 AM O7 84.8(6) 7 . ? AM AM O7 83.2(7) 5_655 . ? A2 AM O7 77.1(6) 3_545 5_655 ? A2 AM O7 77.1(6) 7 5_655 ? AM AM O7 73.1(7) 5_655 5_655 ? O7 AM O7 156.3(6) . 5_655 ? A2 AM O6 168.9(13) 3_545 2_656 ? A2 AM O6 89.6(10) 7 2_656 ? AM AM O6 129.4(2) 5_655 2_656 ? O7 AM O6 90.9(2) . 2_656 ? O7 AM O6 104.0(2) 5_655 2_656 ? A2 AM O6 89.6(10) 3_545 5_656 ? A2 AM O6 168.9(13) 7 5_656 ? AM AM O6 129.4(2) 5_655 5_656 ? O7 AM O6 90.9(2) . 5_656 ? O7 AM O6 104.0(2) 5_655 5_656 ? O6 AM O6 100.7(4) 2_656 5_656 ? A2 AM O5 119.4(11) 3_545 2_655 ? A2 AM O5 55.4(7) 7 2_655 ? AM AM O5 87.2(4) 5_655 2_655 ? O7 AM O5 123.45(12) . 2_655 ? O7 AM O5 56.55(10) 5_655 2_655 ? O6 AM O5 55.18(9) 2_656 2_655 ? O6 AM O5 134.5(4) 5_656 2_655 ? A2 AM O5 55.4(7) 3_545 5_655 ? A2 AM O5 119.4(11) 7 5_655 ? AM AM O5 87.2(4) 5_655 5_655 ? O7 AM O5 123.45(12) . 5_655 ? O7 AM O5 56.55(10) 5_655 5_655 ? O6 AM O5 134.5(4) 2_656 5_655 ? O6 AM O5 55.18(9) 5_656 5_655 ? O5 AM O5 111.44(19) 2_655 5_655 ? A2 AM T1 66.4(5) 3_545 5_655 ? A2 AM T1 100.0(8) 7 5_655 ? AM AM T1 81.5(6) 5_655 5_655 ? O7 AM T1 149.1(2) . 5_655 ? O7 AM T1 27.49(5) 5_655 5_655 ? O6 AM T1 119.4(2) 2_656 5_655 ? O6 AM T1 78.63(12) 5_656 5_655 ? O5 AM T1 82.38(15) 2_655 5_655 ? O5 AM T1 29.34(5) 5_655 5_655 ? A2 AM T1 100.0(8) 3_545 2_655 ? A2 AM T1 66.4(5) 7 2_655 ? AM AM T1 81.5(6) 5_655 2_655 ? O7 AM T1 149.1(2) . 2_655 ? O7 AM T1 27.49(5) 5_655 2_655 ? O6 AM T1 78.63(12) 2_656 2_655 ? O6 AM T1 119.4(2) 5_656 2_655 ? O5 AM T1 29.34(5) 2_655 2_655 ? O5 AM T1 82.38(15) 5_655 2_655 ? T1 AM T1 53.14(10) 5_655 2_655 ? A2 AM T1 66.4(5) 3_545 6 ? A2 AM T1 100.0(8) 7 6 ? AM AM T1 81.5(6) 5_655 6 ? O7 AM T1 26.70(5) . 6 ? O7 AM T1 143.2(3) 5_655 6 ? O6 AM T1 112.7(2) 2_656 6 ? O6 AM T1 72.36(11) 5_656 6 ? O5 AM T1 149.0(2) 2_655 6 ? O5 AM T1 96.77(8) 5_655 6 ? T1 AM T1 123.77(12) 5_655 6 ? T1 AM T1 162.9(4) 2_655 6 ? AM A2 AM 100(2) 3_455 7 ? AM A2 A2 50.1(11) 3_455 5_565 ? AM A2 A2 50.1(11) 7 5_565 ? AM A2 O7 87.6(6) 3_455 7 ? AM A2 O7 79.6(5) 7 7 ? A2 A2 O7 80.02(18) 5_565 7 ? AM A2 O7 79.6(5) 3_455 3_455 ? AM A2 O7 87.6(6) 7 3_455 ? A2 A2 O7 80.02(18) 5_565 3_455 ? O7 A2 O7 160.0(4) 7 3_455 ? AM A2 O5 126.4(8) 3_455 8_455 ? AM A2 O5 113.0(9) 7 8_455 ? A2 A2 O5 140.12(11) 5_565 8_455 ? O7 A2 O5 137.4(3) 7 8_455 ? O7 A2 O5 61.94(8) 3_455 8_455 ? AM A2 O5 113.0(9) 3_455 7 ? AM A2 O5 126.4(8) 7 7 ? A2 A2 O5 140.12(11) 5_565 7 ? O7 A2 O5 61.94(8) 7 7 ? O7 A2 O5 137.4(3) 3_455 7 ? O5 A2 O5 79.8(2) 8_455 7 ? AM A2 O6 175.4(10) 3_455 8_454 ? AM A2 O6 76.6(10) 7 8_454 ? A2 A2 O6 126.59(13) 5_565 8_454 ? O7 A2 O6 88.49(10) 7 8_454 ? O7 A2 O6 103.47(11) 3_455 8_454 ? O5 A2 O6 58.22(13) 8_455 8_454 ? O5 A2 O6 67.16(15) 7 8_454 ? AM A2 O6 76.6(10) 3_455 7_556 ? AM A2 O6 175.4(9) 7 7_556 ? A2 A2 O6 126.59(13) 5_565 7_556 ? O7 A2 O6 103.47(11) 7 7_556 ? O7 A2 O6 88.49(10) 3_455 7_556 ? O5 A2 O6 67.16(15) 8_455 7_556 ? O5 A2 O6 58.22(13) 7 7_556 ? O6 A2 O6 106.8(3) 8_454 7_556 ? AM A2 T1 102.7(5) 3_455 8_455 ? AM A2 T1 102.8(5) 7 8_455 ? A2 A2 T1 110.13(13) 5_565 8_455 ? O7 A2 T1 168.7(3) 7 8_455 ? O7 A2 T1 30.56(5) 3_455 8_455 ? O5 A2 T1 31.44(4) 8_455 8_455 ? O5 A2 T1 109.0(2) 7 8_455 ? O6 A2 T1 81.35(13) 8_454 8_455 ? O6 A2 T1 74.93(11) 7_556 8_455 ? AM A2 T1 102.8(5) 3_455 7 ? AM A2 T1 102.7(5) 7 7 ? A2 A2 T1 110.13(13) 5_565 7 ? O7 A2 T1 30.56(5) 7 7 ? O7 A2 T1 168.7(3) 3_455 7 ? O5 A2 T1 109.0(2) 8_455 7 ? O5 A2 T1 31.44(4) 7 7 ? O6 A2 T1 74.93(11) 8_454 7 ? O6 A2 T1 81.35(13) 7_556 7 ? T1 A2 T1 139.7(3) 8_455 7 ? AM A2 T2 155.2(9) 3_455 8_454 ? AM A2 T2 96.3(10) 7 8_454 ? A2 A2 T2 142.50(8) 5_565 8_454 ? O7 A2 T2 113.63(17) 7 8_454 ? O7 A2 T2 82.77(12) 3_455 8_454 ? O5 A2 T2 28.83(7) 8_455 8_454 ? O5 A2 T2 70.04(17) 7 8_454 ? O6 A2 T2 29.43(7) 8_454 8_454 ? O6 A2 T2 85.7(2) 7_556 8_454 ? T1 A2 T2 55.24(9) 8_455 8_454 ? T1 A2 T2 91.38(16) 7 8_454 ? T1 O1 M1 120.21(7) . . ? T1 O1 M3 119.40(6) . . ? M1 O1 M3 97.73(6) . . ? T1 O1 M2 119.76(6) . . ? M1 O1 M2 95.40(6) . . ? M3 O1 M2 99.22(7) . . ? T2 O2 M2 123.62(7) . 1_556 ? T2 O2 M1 123.40(6) . . ? M2 O2 M1 95.19(6) 1_556 . ? T2 O2 M4 117.44(6) . . ? M2 O2 M4 91.41(5) 1_556 . ? M1 O2 M4 98.69(6) . . ? M3 O3 M1 96.65(6) 1_556 5_556 ? M3 O3 M1 96.65(6) 1_556 . ? M1 O3 M1 100.16(8) 5_556 . ? T2 O4 M2 142.51(7) . 7_556 ? T2 O4 M4 102.41(6) . 7_556 ? M2 O4 M4 95.91(6) 7_556 7_556 ? T2 O5 T1 133.83(8) 1_554 . ? T2 O5 M4 121.69(7) 1_554 7_556 ? T1 O5 M4 94.87(7) . 7_556 ? T2 O5 A2 99.12(7) 1_554 7 ? T1 O5 A2 91.34(12) . 7 ? M4 O5 A2 111.43(7) 7_556 7 ? T2 O5 AM 92.9(2) 1_554 5_655 ? T1 O5 AM 88.61(12) . 5_655 ? M4 O5 AM 122.9(2) 7_556 5_655 ? A2 O5 AM 11.62(17) 7 5_655 ? T2 O6 T1 135.58(8) . . ? T2 O6 M4 90.11(7) . 7_556 ? T1 O6 M4 96.95(6) . 7_556 ? T2 O6 AM 104.76(17) . 5_656 ? T1 O6 AM 108.8(2) . 5_656 ? M4 O6 AM 120.55(18) 7_556 5_656 ? T2 O6 A2 95.91(11) . 7_556 ? T1 O6 A2 121.53(14) . 7_556 ? M4 O6 A2 110.86(10) 7_556 7_556 ? AM O6 A2 13.79(12) 5_656 7_556 ? T1 O7 T1 133.54(11) 6 . ? T1 O7 AM 112.61(6) 6 . ? T1 O7 AM 112.61(6) . . ? T1 O7 A2 120.76(19) 6 7 ? T1 O7 A2 101.13(18) . 7 ? AM O7 A2 15.62(15) . 7 ? T1 O7 A2 101.13(18) 6 3_545 ? T1 O7 A2 120.76(19) . 3_545 ? AM O7 A2 15.62(15) . 3_545 ? A2 O7 A2 20.0(4) 7 3_545 ? T1 O7 AM 108.47(9) 6 5_655 ? T1 O7 AM 108.47(9) . 5_655 ? AM O7 AM 23.7(6) . 5_655 ? A2 O7 AM 15.28(13) 7 5_655 ? A2 O7 AM 15.28(13) 3_545 5_655 ? _refine_diff_density_max 1.237 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.172 _shelxl_version_number 2014-3 _shelx_res_file ; TITL Am5 in C2/m CELL 0.71073 9.885 17.978 5.283 90.000 105.193 90.000 ZERR 2.00 0.006 0.012 0.004 0.000 0.007 0.000 LATT 7 SYMM -X, Y, -Z SFAC CA NA K MG SI SFAC O2- 3.04484 7.98437 0.50181 3.73146 1.55609 0.32297 4.20924 = 23.9207 0.23641 0.0106 0.006 32.5 0.66 15.9994 SFAC F FE UNIT 4 1 1 8 12 46 2 0.2 L.S. 10 BOND ACTA FMAP 2 PLAN 20 WGHT 0.053100 3.600000 EXTI 0.045107 FVAR 0.50395 M1 4 0.000000 0.088959 0.500000 0.50720 0.00858 0.00804 = 0.00677 0.00000 0.00256 0.00000 M2 4 0.000000 0.176275 0.000000 0.51297 0.00739 0.00717 = 0.00706 0.00000 0.00249 0.00000 M3 4 0.000000 0.000000 0.000000 0.25406 0.00766 0.00786 = 0.00620 0.00000 0.00195 0.00000 M4 1 0.000000 0.278990 0.500000 0.48407 0.01409 0.01146 = 0.01239 0.00000 0.00664 0.00000 T1 5 0.280036 0.085059 0.302076 11.00000 0.00792 0.00823 = 0.00809 -0.00019 0.00163 -0.00052 T2 5 0.289503 0.172814 0.810566 11.00000 0.00700 0.00750 = 0.00655 0.00028 0.00183 -0.00039 AM 2 0.538179 0.000000 0.085536 0.11676 0.03230 A2 2 0.000000 0.476432 0.000000 0.15246 0.03264 O1 6 0.107712 0.086158 0.217894 11.00000 0.00828 0.01288 = 0.00838 -0.00069 0.00190 -0.00165 O2 6 0.119328 0.171902 0.729525 11.00000 0.00670 0.01057 = 0.00927 0.00048 0.00175 0.00006 O3 6 0.107024 0.000000 0.716247 0.52812 0.00925 0.00967 = 0.01099 0.00000 0.00245 0.00000 O4 6 0.365460 0.249831 0.788682 11.00000 0.01332 0.00963 = 0.01200 -0.00017 0.00463 -0.00312 O5 6 0.349467 0.138863 0.109540 11.00000 0.01042 0.01627 = 0.00968 0.00467 0.00110 -0.00019 O6 6 0.344609 0.115535 0.609267 11.00000 0.01008 0.01386 = 0.01287 -0.00428 0.00317 0.00064 O7 6 0.341754 0.000000 0.277424 10.50000 0.01088 0.01236 = 0.01763 0.00000 0.00344 0.00000 HKLF 4 REM Am5 in C2/m REM R1 = 0.0322 for 1364 Fo > 4sig(Fo) and 0.0323 for all 1376 data REM 108 parameters refined using 0 restraints END WGHT 0.0424 1.4703 REM Highest difference peak 1.237, deepest hole -1.064, 1-sigma level 0.172 Q1 1 0.0000 0.5000 0.0000 10.25000 0.05 1.24 Q2 1 0.0000 0.4502 0.0000 10.50000 0.05 1.21 Q3 1 0.5000 0.2159 1.0000 10.50000 0.05 0.60 Q4 1 0.1120 0.2081 0.5354 11.00000 0.05 0.55 Q5 1 0.5907 0.0000 0.1878 10.50000 0.05 0.55 Q6 1 0.5000 -0.0458 0.5000 10.50000 0.05 0.54 Q7 1 0.4828 0.0000 0.4002 10.50000 0.05 0.54 Q8 1 0.1095 0.1252 0.0264 11.00000 0.05 0.51 Q9 1 0.2809 0.0000 0.8023 10.50000 0.05 0.50 Q10 1 0.0000 0.1915 0.5000 10.50000 0.05 0.47 Q11 1 0.1160 0.0402 0.5117 11.00000 0.05 0.47 Q12 1 0.2149 0.2290 0.6957 11.00000 0.05 0.44 Q13 1 0.4217 0.2783 0.8670 11.00000 0.05 0.43 Q14 1 0.1392 0.0116 0.2504 11.00000 0.05 0.43 Q15 1 0.5379 0.0000 0.3260 10.50000 0.05 0.42 Q16 1 0.2288 0.0571 0.7141 11.00000 0.05 0.41 Q17 1 0.0527 0.4104 0.1176 11.00000 0.05 0.41 Q18 1 0.1179 0.0443 0.0056 11.00000 0.05 0.40 Q19 1 0.0170 0.4172 -0.1620 11.00000 0.05 0.40 Q20 1 0.1749 0.0000 0.7655 10.50000 0.05 0.39 ; _shelx_res_checksum 68371 _shelx_hkl_file ; -2 0 0 77.033 1.655 2 0 0 76.798 1.132 -4 0 0 38.148 0.845 4 0 0 36.406 0.531 -6 0 0 3541.90 92.47 6 0 0 3603.51 47.50 -8 0 0 3869.82 62.64 8 0 0 3883.80 62.63 -10 0 0 2207.66 45.50 10 0 0 2330.56 37.18 -12 0 0 24.911 1.211 12 0 0 26.202 1.261 -1 -1 0 451.96 6.20 1 -1 0 447.12 4.41 -1 1 0 425.56 12.61 1 1 0 451.21 6.21 -3 -1 0 3269.27 64.93 3 -1 0 3221.05 38.83 -3 1 0 3307.49 66.44 3 1 0 3217.79 43.30 -5 -1 0 2869.12 52.60 5 -1 0 2774.19 41.50 -5 1 0 2675.75 54.68 5 1 0 2815.77 39.74 -7 -1 0 1261.60 20.66 7 -1 0 1266.97 17.77 -7 1 0 1261.23 20.66 7 1 0 1262.02 20.66 -9 -1 0 149.61 2.42 9 -1 0 150.40 2.92 -9 1 0 151.16 2.91 9 1 0 149.41 2.93 -11 -1 0 1077.43 17.39 11 -1 0 1054.97 22.06 -11 1 0 1041.34 21.77 11 1 0 1070.77 17.76 -13 -1 0 254.31 4.20 13 -1 0 258.28 6.27 -13 1 0 253.44 5.06 13 1 0 258.64 6.26 0 -2 0 541.59 7.55 0 2 0 516.98 14.75 -2 -2 0 93.298 1.111 2 -2 0 93.726 0.916 -2 2 0 93.071 1.993 2 2 0 92.465 1.588 -4 -2 0 15.866 0.340 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0.513 0 6 0 36.430 0.729 -2 -6 0 0.8472 0.0829 2 -6 0 0.3185 0.0456 -2 6 0 0.3024 0.0916 2 6 0 0.4225 0.0846 -4 -6 0 50.644 0.723 4 -6 0 50.578 0.641 -4 6 0 53.888 1.844 4 6 0 51.741 0.896 -6 -6 0 155.98 2.45 6 -6 0 159.74 2.22 -6 6 0 156.68 3.02 6 6 0 158.35 2.45 -8 -6 0 167.05 2.69 8 -6 0 169.43 2.76 -8 6 0 172.10 3.19 8 6 0 168.61 3.19 -10 -6 0 58.277 1.210 10 -6 0 57.766 1.882 -10 6 0 57.629 1.852 10 6 0 57.483 1.463 -12 -6 0 34.527 0.953 12 -6 0 34.315 1.063 -12 6 0 33.286 1.189 12 6 0 33.442 1.141 -1 -7 0 2.6270 0.1198 1 -7 0 2.7549 0.1069 -1 7 0 3.0053 0.1377 1 7 0 2.7867 0.2303 -3 -7 0 1558.98 19.71 3 -7 0 1587.69 15.67 -3 7 0 1586.75 43.52 3 7 0 1601.88 22.28 -5 -7 0 601.82 6.90 5 -7 0 596.41 6.06 -5 7 0 599.50 9.96 5 7 0 598.59 8.57 -7 -7 0 248.81 3.80 7 -7 0 252.79 3.43 -7 7 0 253.38 3.41 7 7 0 249.44 4.46 -9 -7 0 1110.44 15.72 9 -7 0 1123.69 15.85 -9 7 0 1109.06 18.41 9 7 0 1100.97 18.39 -11 -7 0 1.2078 0.2324 11 -7 0 1.8278 0.4137 -11 7 0 0.6452 0.3067 11 7 0 0.7949 0.2573 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-7 2327.03 47.96 -2 -6 7 2374.87 48.01 -2 6 7 2470.67 48.68 5 -7 -7 9.6166 0.8719 5 7 -7 10.363 0.877 -5 -7 7 10.927 0.958 -5 7 7 10.832 0.954 3 -7 -7 2.2509 0.5025 3 7 -7 0.8850 0.3511 -3 -7 7 1.1741 0.4283 -3 7 7 0.6910 0.3945 1 -7 -7 51.141 2.669 1 7 -7 50.038 1.816 -1 -7 7 51.279 1.946 -1 7 7 50.369 1.909 4 -8 -7 25.908 1.273 4 8 -7 24.755 1.228 -4 -8 7 26.691 1.328 -4 8 7 24.957 1.291 2 -8 -7 23.400 1.200 2 8 -7 24.486 1.209 -2 -8 7 24.434 1.267 -2 8 7 23.165 1.243 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 22856 # start CheckCIF/PLATON Validation Reply Form _vrf_PLAT041_I PROBLEM: Calc. and Reported SumFormula Strings Differ Please Check _vrf_PLAT043_I PROBLEM: Calculated and Reported Mol. Weight Differ by .. 6.71 Check RESPONSE: The site-occupancies of the M(1,2,3) sites in AM1 were refined using only Mg. However, the refinement results clearly indicate there may be minor occupancy of the M(1,2,3) sites by 6Al, Fe2+, Ti4+, V3+ and Cr3+. Although such species were not incorporated into the refinement, the occupancies of these sites were not fixed so as to reflect the minor amounts of these heavier scattering species. Inclusion of these additional species during refinement would provide no additional information as the identity and fractional abundance of such species was unknown. For this reason all of the alerts below are to be expected. Discrepancies in the ratio of the given/expected molecular weights and between the calculated and reported “sumformula” are expected as the M(1,2,3) sites contained minor amounts of heavier species not included in the site-occupancy refinement. _vrf_PLAT075_I PROBLEM: Occupancy 1.014 Greater Than 1.0 for ...... M1 _vrf_PLAT077_I PROBLEM: Unitcell Contains Non-integer Number of Atoms .. Please Check RESPONSE: The occupancy of the M(1,2,3) and O(3) sites were refined using Mg and O2-, respectively. However, the M(1,2,3) sites contain minor amounts of certain species (as listed above) all with a relatively higher scattering than Mg and the O(3) sites contains (OH)- and F-. This resulted in an occupancy slightly higher than 1.0 at certain sites as the site-occupancy was refined rather than fixed. This difference in scattering factors between particularly Mg and the other species that occupy the M(1,2,3) sites (in minor amounts) also resulted in a unit-cell that contains non-integer numbers. # end Validation Reply Form