_audit_creation_method SHELXL-2014 _chemical_name_systematic ; Sodium calcium iron magnesium aluminum silicate fluoride hydroxide * ; _chemical_name_common Richterite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca2 F0 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' _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 9.845(5) _cell_length_b 17.940(10) _cell_length_c 5.294(3) _cell_angle_alpha 90 _cell_angle_beta 105.221(7) _cell_angle_gamma 90 _cell_volume 902.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5324 _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 0.11 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_absorpt_coefficient_mu 1.437 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.93 _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 5324 _diffrn_reflns_av_unetI/netI 0.0110 _diffrn_reflns_av_R_equivalents 0.0126 _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 2.270 _diffrn_reflns_theta_max 30.377 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 1379 _reflns_number_gt 1316 _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^)+(0.0457P)^2^+3.6833P] 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 0.0057(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1379 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 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 0.08904(4) 0.5000 0.0074(3) Uani 1.018(5) 2 d S T . . . M2 Mg 0.0000 0.17882(4) 0.0000 0.0077(3) Uani 1.015(5) 2 d S T . . . M3 Mg 0.0000 0.0000 0.0000 0.0070(4) Uani 1.011(7) 4 d S T . . . M4C Ca 0.0000 0.27729(3) 0.5000 0.0125(3) Uani 0.562(8) 2 d S T P . . M4M Na 0.0000 0.27729(3) 0.5000 0.0125(3) Uani 0.438(8) 2 d S T P . . T1 Si 0.27764(4) 0.08494(2) 0.29725(8) 0.00632(13) Uani 1 1 d . . . . . T2 Si 0.28633(4) 0.17175(2) 0.80340(8) 0.00600(13) Uani 1 1 d . . . . . AM Na 0.5361(5) 0.0000 0.0853(11) 0.0171(9) Uiso 0.267(5) 2 d S U . . . A2 Na 0.0000 0.4872(3) 0.0000 0.0171(9) Uiso 0.285(5) 2 d S U . . . O1 O 0.11069(11) 0.08592(6) 0.2180(2) 0.0068(2) Uani 1 1 d . . . . . O2 O 0.11870(11) 0.16987(6) 0.7265(2) 0.0078(2) Uani 1 1 d . . . . . O3 O 0.10657(16) 0.0000 0.7140(3) 0.0088(4) Uani 1.055(8) 2 d S T . . . O4 O 0.36283(12) 0.24841(7) 0.7937(2) 0.0101(2) Uani 1 1 d . . . . . O5 O 0.34638(12) 0.13146(7) 0.0949(2) 0.0104(2) Uani 1 1 d . . . . . O6 O 0.34224(12) 0.11621(7) 0.5940(2) 0.0099(2) Uani 1 1 d . . . . . O7 O 0.33707(17) 0.0000 0.2900(3) 0.0114(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 0.0079(4) 0.0077(4) 0.0066(4) 0.000 0.0019(3) 0.000 M2 0.0071(4) 0.0071(4) 0.0090(4) 0.000 0.0024(3) 0.000 M3 0.0079(5) 0.0063(5) 0.0067(5) 0.000 0.0017(4) 0.000 M4C 0.0151(4) 0.0106(3) 0.0146(4) 0.000 0.0089(2) 0.000 M4M 0.0151(4) 0.0106(3) 0.0146(4) 0.000 0.0089(2) 0.000 T1 0.0062(2) 0.0062(2) 0.0063(2) -0.00026(13) 0.00116(14) -0.00034(13) T2 0.0058(2) 0.0062(2) 0.0059(2) -0.00037(13) 0.00134(14) -0.00082(13) O1 0.0057(5) 0.0077(5) 0.0068(5) -0.0004(4) 0.0012(4) -0.0007(4) O2 0.0057(5) 0.0095(5) 0.0079(5) -0.0007(4) 0.0014(4) -0.0007(4) O3 0.0085(7) 0.0092(7) 0.0088(7) 0.000 0.0024(5) 0.000 O4 0.0116(5) 0.0085(5) 0.0105(5) -0.0007(4) 0.0032(4) -0.0038(4) O5 0.0080(5) 0.0148(6) 0.0084(5) 0.0046(4) 0.0020(4) 0.0005(4) O6 0.0083(5) 0.0126(5) 0.0083(5) -0.0034(4) 0.0015(4) 0.0008(4) O7 0.0095(7) 0.0066(7) 0.0174(8) 0.000 0.0020(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 O2 2.0420(14) . ? M1 O2 2.0421(14) 2_556 ? M1 O1 2.0672(14) . ? M1 O1 2.0672(14) 2_556 ? M1 O3 2.0765(13) . ? M1 O3 2.0765(13) 5_556 ? M1 M3 3.0917(14) . ? M1 M3 3.0917(14) 1_556 ? M1 M2 3.0984(15) 1_556 ? M1 M2 3.0984(15) . ? M1 T1 3.1889(14) 2_556 ? M1 T1 3.1890(14) . ? M2 O4 1.9866(14) 7_556 ? M2 O4 1.9866(14) 8_454 ? M2 O2 2.0921(14) 2_556 ? M2 O2 2.0921(14) 1_554 ? M2 O1 2.1533(15) . ? M2 O1 2.1533(15) 2 ? M2 M1 3.0985(15) 1_554 ? M2 M4C 3.1823(15) 1_554 ? M2 M4M 3.1823(15) 1_554 ? M2 M4C 3.1824(15) . ? M3 O3 2.0561(17) 5_556 ? M3 O3 2.0561(17) 1_554 ? M3 O1 2.0579(13) 5 ? M3 O1 2.0579(13) 6 ? M3 O1 2.0579(13) 2 ? M3 O1 2.0580(13) . ? M3 M1 3.0916(14) 5 ? M3 M1 3.0916(14) 5_556 ? M3 M1 3.0916(14) 1_554 ? M3 T1 3.1640(12) 5 ? M3 T1 3.1640(12) 2 ? M4C O4 2.3572(15) 8_455 ? M4C O4 2.3572(15) 7_556 ? M4C O2 2.4043(15) . ? M4C O2 2.4044(16) 2_556 ? M4C O6 2.5916(16) 7_556 ? M4C O6 2.5916(16) 8_455 ? M4C O5 2.8043(16) 7_556 ? M4C O5 2.8043(16) 8_455 ? M4C T2 3.1009(12) 7_556 ? M4C T2 3.1009(12) 8_455 ? M4C M2 3.1824(15) 1_556 ? T1 O1 1.5861(14) . ? T1 O6 1.6317(14) . ? T1 O7 1.6363(11) . ? T1 O5 1.6381(13) . ? T1 A2 3.279(2) 7 ? T1 M4M 3.2894(14) 7_556 ? T1 M4C 3.2894(14) 7_556 ? T1 AM 3.399(3) . ? T1 AM 3.426(4) 5_655 ? T2 O4 1.5753(14) . ? T2 O2 1.5930(14) . ? T2 O5 1.6655(14) 1_556 ? T2 O6 1.6869(13) . ? T2 M4M 3.1009(12) 7_556 ? T2 M4C 3.1009(12) 7_556 ? T2 M2 3.2536(15) 1_556 ? T2 AM 3.515(3) 5_656 ? AM A2 0.547(5) 3_545 ? AM A2 0.547(5) 7 ? AM AM 0.992(12) 5_655 ? AM O7 2.476(4) . ? AM O7 2.609(4) 5_655 ? AM O6 2.756(4) 2_656 ? AM O6 2.756(4) 5_656 ? AM O5 2.896(3) 2_655 ? AM O5 2.896(3) 5_655 ? AM O5 3.017(3) 6 ? AM O5 3.017(3) . ? A2 AM 0.547(5) 3_455 ? A2 AM 0.547(5) 7 ? A2 O7 2.505(2) 7 ? A2 O7 2.505(2) 3_455 ? A2 O5 2.733(4) 8_455 ? A2 O5 2.733(4) 7 ? A2 O6 2.953(3) 8_454 ? A2 O6 2.953(3) 7_556 ? A2 T1 3.279(2) 8_455 ? A2 T1 3.279(2) 7 ? A2 T1 3.486(3) 4 ? A2 T1 3.486(3) 3_455 ? O2 M2 2.0921(14) 1_556 ? O3 M3 2.0561(17) 1_556 ? O3 M1 2.0765(13) 5_556 ? O4 M2 1.9866(14) 7_556 ? O4 M4M 2.3571(15) 7_556 ? O4 M4C 2.3571(15) 7_556 ? O5 T2 1.6655(14) 1_554 ? O5 A2 2.733(4) 7 ? O5 M4C 2.8043(16) 7_556 ? O5 M4M 2.8043(16) 7_556 ? O5 AM 2.896(3) 5_655 ? O6 M4M 2.5916(16) 7_556 ? O6 M4C 2.5916(16) 7_556 ? O6 AM 2.756(4) 5_656 ? O6 A2 2.953(3) 7_556 ? O7 T1 1.6363(11) 6 ? O7 A2 2.505(2) 3_545 ? O7 A2 2.505(2) 7 ? O7 AM 2.609(4) 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 O2 M1 O2 89.52(8) . 2_556 ? O2 M1 O1 96.56(6) . . ? O2 M1 O1 85.65(6) 2_556 . ? O2 M1 O1 85.65(6) . 2_556 ? O2 M1 O1 96.56(6) 2_556 2_556 ? O1 M1 O1 176.89(7) . 2_556 ? O2 M1 O3 95.55(6) . . ? O2 M1 O3 174.79(5) 2_556 . ? O1 M1 O3 94.96(6) . . ? O1 M1 O3 82.63(6) 2_556 . ? O2 M1 O3 174.79(5) . 5_556 ? O2 M1 O3 95.55(6) 2_556 5_556 ? O1 M1 O3 82.64(6) . 5_556 ? O1 M1 O3 94.96(6) 2_556 5_556 ? O3 M1 O3 79.42(8) . 5_556 ? O2 M1 M3 137.81(4) . . ? O2 M1 M3 89.59(5) 2_556 . ? O1 M1 M3 41.34(4) . . ? O1 M1 M3 136.28(4) 2_556 . ? O3 M1 M3 87.48(6) . . ? O3 M1 M3 41.32(4) 5_556 . ? O2 M1 M3 89.59(5) . 1_556 ? O2 M1 M3 137.81(4) 2_556 1_556 ? O1 M1 M3 136.28(4) . 1_556 ? O1 M1 M3 41.34(4) 2_556 1_556 ? O3 M1 M3 41.32(4) . 1_556 ? O3 M1 M3 87.48(6) 5_556 1_556 ? M3 M1 M3 117.78(5) . 1_556 ? O2 M1 M2 42.07(4) . 1_556 ? O2 M1 M2 90.24(5) 2_556 1_556 ? O1 M1 M2 138.53(4) . 1_556 ? O1 M1 M2 43.86(4) 2_556 1_556 ? O3 M1 M2 92.70(5) . 1_556 ? O3 M1 M2 138.82(5) 5_556 1_556 ? M3 M1 M2 179.79(3) . 1_556 ? M3 M1 M2 62.43(4) 1_556 1_556 ? O2 M1 M2 90.24(5) . . ? O2 M1 M2 42.07(4) 2_556 . ? O1 M1 M2 43.86(4) . . ? O1 M1 M2 138.53(4) 2_556 . ? O3 M1 M2 138.82(5) . . ? O3 M1 M2 92.70(5) 5_556 . ? M3 M1 M2 62.43(4) . . ? M3 M1 M2 179.79(3) 1_556 . ? M2 M1 M2 117.37(5) 1_556 . ? O2 M1 T1 103.16(4) . 2_556 ? O2 M1 T1 78.76(4) 2_556 2_556 ? O1 M1 T1 154.60(3) . 2_556 ? O1 M1 T1 25.23(3) 2_556 2_556 ? O3 M1 T1 98.83(5) . 2_556 ? O3 M1 T1 79.10(5) 5_556 2_556 ? M3 M1 T1 117.96(2) . 2_556 ? M3 M1 T1 60.477(17) 1_556 2_556 ? M2 M1 T1 62.110(18) 1_556 2_556 ? M2 M1 T1 119.46(2) . 2_556 ? O2 M1 T1 78.76(4) . . ? O2 M1 T1 103.17(4) 2_556 . ? O1 M1 T1 25.23(3) . . ? O1 M1 T1 154.60(3) 2_556 . ? O3 M1 T1 79.10(5) . . ? O3 M1 T1 98.83(5) 5_556 . ? M3 M1 T1 60.477(17) . . ? M3 M1 T1 117.96(2) 1_556 . ? M2 M1 T1 119.46(2) 1_556 . ? M2 M1 T1 62.110(18) . . ? T1 M1 T1 177.35(3) 2_556 . ? O4 M2 O4 97.82(9) 7_556 8_454 ? O4 M2 O2 95.31(6) 7_556 2_556 ? O4 M2 O2 90.48(6) 8_454 2_556 ? O4 M2 O2 90.48(6) 7_556 1_554 ? O4 M2 O2 95.31(6) 8_454 1_554 ? O2 M2 O2 171.20(8) 2_556 1_554 ? O4 M2 O1 92.22(6) 7_556 . ? O4 M2 O1 168.14(5) 8_454 . ? O2 M2 O1 82.28(5) 2_556 . ? O2 M2 O1 90.89(5) 1_554 . ? O4 M2 O1 168.13(5) 7_556 2 ? O4 M2 O1 92.22(6) 8_454 2 ? O2 M2 O1 90.89(5) 2_556 2 ? O2 M2 O1 82.28(5) 1_554 2 ? O1 M2 O1 78.58(7) . 2 ? O4 M2 M1 91.40(5) 7_556 . ? O4 M2 M1 131.21(4) 8_454 . ? O2 M2 M1 40.85(4) 2_556 . ? O2 M2 M1 132.59(5) 1_554 . ? O1 M2 M1 41.69(3) . . ? O1 M2 M1 86.68(5) 2 . ? O4 M2 M1 131.21(4) 7_556 1_554 ? O4 M2 M1 91.40(5) 8_454 1_554 ? O2 M2 M1 132.59(5) 2_556 1_554 ? O2 M2 M1 40.85(4) 1_554 1_554 ? O1 M2 M1 86.68(5) . 1_554 ? O1 M2 M1 41.69(3) 2 1_554 ? M1 M2 M1 117.36(5) . 1_554 ? O4 M2 M4C 86.79(5) 7_556 1_554 ? O4 M2 M4C 47.65(4) 8_454 1_554 ? O2 M2 M4C 137.76(4) 2_556 1_554 ? O2 M2 M4C 49.07(4) 1_554 1_554 ? O1 M2 M4C 139.90(3) . 1_554 ? O1 M2 M4C 95.41(5) 2 1_554 ? M1 M2 M4C 177.60(3) . 1_554 ? M1 M2 M4C 65.04(4) 1_554 1_554 ? O4 M2 M4M 86.79(5) 7_556 1_554 ? O4 M2 M4M 47.65(4) 8_454 1_554 ? O2 M2 M4M 137.76(4) 2_556 1_554 ? O2 M2 M4M 49.07(4) 1_554 1_554 ? O1 M2 M4M 139.90(3) . 1_554 ? O1 M2 M4M 95.41(5) 2 1_554 ? M1 M2 M4M 177.60(3) . 1_554 ? M1 M2 M4M 65.04(4) 1_554 1_554 ? M4C M2 M4M 0.000(18) 1_554 1_554 ? O4 M2 M4C 47.65(4) 7_556 . ? O4 M2 M4C 86.79(5) 8_454 . ? O2 M2 M4C 49.07(4) 2_556 . ? O2 M2 M4C 137.76(4) 1_554 . ? O1 M2 M4C 95.41(5) . . ? O1 M2 M4C 139.90(3) 2 . ? M1 M2 M4C 65.04(4) . . ? M1 M2 M4C 177.60(3) 1_554 . ? M4C M2 M4C 112.56(5) 1_554 . ? M4M M2 M4C 112.56(5) 1_554 . ? O3 M3 O3 180.00(6) 5_556 1_554 ? O3 M3 O1 96.64(5) 5_556 5 ? O3 M3 O1 83.36(5) 1_554 5 ? O3 M3 O1 83.36(5) 5_556 6 ? O3 M3 O1 96.64(5) 1_554 6 ? O1 M3 O1 83.00(7) 5 6 ? O3 M3 O1 96.64(5) 5_556 2 ? O3 M3 O1 83.36(5) 1_554 2 ? O1 M3 O1 97.00(7) 5 2 ? O1 M3 O1 180.00(7) 6 2 ? O3 M3 O1 83.36(5) 5_556 . ? O3 M3 O1 96.64(5) 1_554 . ? O1 M3 O1 180.0 5 . ? O1 M3 O1 97.01(7) 6 . ? O1 M3 O1 82.99(7) 2 . ? O3 M3 M1 138.18(3) 5_556 5 ? O3 M3 M1 41.82(3) 1_554 5 ? O1 M3 M1 41.57(4) 5 5 ? O1 M3 M1 88.52(5) 6 5 ? O1 M3 M1 91.48(5) 2 5 ? O1 M3 M1 138.43(4) . 5 ? O3 M3 M1 41.82(3) 5_556 5_556 ? O3 M3 M1 138.18(3) 1_554 5_556 ? O1 M3 M1 88.52(5) 5 5_556 ? O1 M3 M1 41.57(4) 6 5_556 ? O1 M3 M1 138.43(4) 2 5_556 ? O1 M3 M1 91.48(5) . 5_556 ? M1 M3 M1 117.78(5) 5 5_556 ? O3 M3 M1 138.18(3) 5_556 1_554 ? O3 M3 M1 41.82(3) 1_554 1_554 ? O1 M3 M1 91.48(5) 5 1_554 ? O1 M3 M1 138.43(4) 6 1_554 ? O1 M3 M1 41.57(4) 2 1_554 ? O1 M3 M1 88.52(5) . 1_554 ? M1 M3 M1 62.22(5) 5 1_554 ? M1 M3 M1 180.00(2) 5_556 1_554 ? O3 M3 M1 41.83(3) 5_556 . ? O3 M3 M1 138.17(3) 1_554 . ? O1 M3 M1 138.43(4) 5 . ? O1 M3 M1 91.48(5) 6 . ? O1 M3 M1 88.52(5) 2 . ? O1 M3 M1 41.57(4) . . ? M1 M3 M1 180.0 5 . ? M1 M3 M1 62.22(5) 5_556 . ? M1 M3 M1 117.78(5) 1_554 . ? O3 M3 T1 79.92(5) 5_556 5 ? O3 M3 T1 100.08(5) 1_554 5 ? O1 M3 T1 25.74(3) 5 5 ? O1 M3 T1 100.33(5) 6 5 ? O1 M3 T1 79.67(5) 2 5 ? O1 M3 T1 154.26(3) . 5 ? M1 M3 T1 61.28(2) 5 5 ? M1 M3 T1 89.02(3) 5_556 5 ? M1 M3 T1 90.98(3) 1_554 5 ? M1 M3 T1 118.72(2) . 5 ? O3 M3 T1 79.92(5) 5_556 2 ? O3 M3 T1 100.08(5) 1_554 2 ? O1 M3 T1 79.67(5) 5 2 ? O1 M3 T1 154.26(3) 6 2 ? O1 M3 T1 25.74(3) 2 2 ? O1 M3 T1 100.33(5) . 2 ? M1 M3 T1 90.98(3) 5 2 ? M1 M3 T1 118.72(2) 5_556 2 ? M1 M3 T1 61.28(2) 1_554 2 ? M1 M3 T1 89.02(3) . 2 ? T1 M3 T1 57.58(4) 5 2 ? O4 M4C O4 157.45(7) 8_455 7_556 ? O4 M4C O2 78.58(5) 8_455 . ? O4 M4C O2 83.37(5) 7_556 . ? O4 M4C O2 83.37(5) 8_455 2_556 ? O4 M4C O2 78.58(5) 7_556 2_556 ? O2 M4C O2 73.46(7) . 2_556 ? O4 M4C O6 138.32(4) 8_455 7_556 ? O4 M4C O6 62.71(5) 7_556 7_556 ? O2 M4C O6 116.70(5) . 7_556 ? O2 M4C O6 137.10(4) 2_556 7_556 ? O4 M4C O6 62.71(5) 8_455 8_455 ? O4 M4C O6 138.32(4) 7_556 8_455 ? O2 M4C O6 137.10(4) . 8_455 ? O2 M4C O6 116.70(5) 2_556 8_455 ? O6 M4C O6 85.00(7) 7_556 8_455 ? O4 M4C O5 84.09(5) 8_455 7_556 ? O4 M4C O5 109.35(5) 7_556 7_556 ? O2 M4C O5 89.58(5) . 7_556 ? O2 M4C O5 160.59(4) 2_556 7_556 ? O6 M4C O5 59.10(5) 7_556 7_556 ? O6 M4C O5 69.68(5) 8_455 7_556 ? O4 M4C O5 109.35(5) 8_455 8_455 ? O4 M4C O5 84.09(5) 7_556 8_455 ? O2 M4C O5 160.59(4) . 8_455 ? O2 M4C O5 89.58(5) 2_556 8_455 ? O6 M4C O5 69.68(5) 7_556 8_455 ? O6 M4C O5 59.10(5) 8_455 8_455 ? O5 M4C O5 108.57(6) 7_556 8_455 ? O4 M4C T2 169.54(3) 8_455 7_556 ? O4 M4C T2 29.76(3) 7_556 7_556 ? O2 M4C T2 100.81(4) . 7_556 ? O2 M4C T2 106.56(4) 2_556 7_556 ? O6 M4C T2 32.95(3) 7_556 7_556 ? O6 M4C T2 113.85(4) 8_455 7_556 ? O5 M4C T2 85.47(4) 7_556 7_556 ? O5 M4C T2 74.61(4) 8_455 7_556 ? O4 M4C T2 29.76(3) 8_455 8_455 ? O4 M4C T2 169.54(3) 7_556 8_455 ? O2 M4C T2 106.56(4) . 8_455 ? O2 M4C T2 100.81(4) 2_556 8_455 ? O6 M4C T2 113.85(4) 7_556 8_455 ? O6 M4C T2 32.95(3) 8_455 8_455 ? O5 M4C T2 74.61(4) 7_556 8_455 ? O5 M4C T2 85.47(4) 8_455 8_455 ? T2 M4C T2 145.70(3) 7_556 8_455 ? O4 M4C M2 124.42(4) 8_455 . ? O4 M4C M2 38.53(3) 7_556 . ? O2 M4C M2 82.17(5) . . ? O2 M4C M2 41.10(3) 2_556 . ? O6 M4C M2 96.82(4) 7_556 . ? O6 M4C M2 134.41(3) 8_455 . ? O5 M4C M2 147.40(3) 7_556 . ? O5 M4C M2 78.79(5) 8_455 . ? T2 M4C M2 65.46(3) 7_556 . ? T2 M4C M2 137.960(19) 8_455 . ? O4 M4C M2 38.53(3) 8_455 1_556 ? O4 M4C M2 124.42(4) 7_556 1_556 ? O2 M4C M2 41.10(3) . 1_556 ? O2 M4C M2 82.17(5) 2_556 1_556 ? O6 M4C M2 134.41(3) 7_556 1_556 ? O6 M4C M2 96.82(4) 8_455 1_556 ? O5 M4C M2 78.80(5) 7_556 1_556 ? O5 M4C M2 147.40(3) 8_455 1_556 ? T2 M4C M2 137.96(2) 7_556 1_556 ? T2 M4C M2 65.46(3) 8_455 1_556 ? M2 M4C M2 112.56(5) . 1_556 ? O1 T1 O6 111.45(6) . . ? O1 T1 O7 110.87(7) . . ? O6 T1 O7 106.94(8) . . ? O1 T1 O5 113.50(6) . . ? O6 T1 O5 109.33(7) . . ? O7 T1 O5 104.33(8) . . ? O1 T1 M3 34.30(4) . . ? O6 T1 M3 135.39(5) . . ? O7 T1 M3 78.89(6) . . ? O5 T1 M3 111.80(5) . . ? O1 T1 M1 33.74(5) . . ? O6 T1 M1 79.62(5) . . ? O7 T1 M1 111.89(6) . . ? O5 T1 M1 138.26(5) . . ? M3 T1 M1 58.24(3) . . ? O1 T1 M2 35.25(4) . . ? O6 T1 M2 110.75(5) . . ? O7 T1 M2 137.13(6) . . ? O5 T1 M2 81.86(5) . . ? M3 T1 M2 60.06(4) . . ? M1 T1 M2 57.58(3) . . ? O1 T1 A2 130.81(6) . 7 ? O6 T1 A2 117.20(5) . 7 ? O7 T1 A2 48.20(10) . 7 ? O5 T1 A2 56.26(9) . 7 ? M3 T1 A2 99.77(6) . 7 ? M1 T1 A2 155.50(7) . 7 ? M2 T1 A2 123.75(5) . 7 ? O1 T1 M4M 129.24(5) . 7_556 ? O6 T1 M4M 50.93(4) . 7_556 ? O7 T1 M4M 119.74(7) . 7_556 ? O5 T1 M4M 58.45(5) . 7_556 ? M3 T1 M4M 159.750(17) . 7_556 ? M1 T1 M4M 115.38(3) . 7_556 ? M2 T1 M4M 99.90(4) . 7_556 ? A2 T1 M4M 88.97(7) 7 7_556 ? O1 T1 M4C 129.24(5) . 7_556 ? O6 T1 M4C 50.93(4) . 7_556 ? O7 T1 M4C 119.74(7) . 7_556 ? O5 T1 M4C 58.45(5) . 7_556 ? M3 T1 M4C 159.750(17) . 7_556 ? M1 T1 M4C 115.38(3) . 7_556 ? M2 T1 M4C 99.90(4) . 7_556 ? A2 T1 M4C 88.97(7) 7 7_556 ? M4M T1 M4C 0.000(14) 7_556 7_556 ? O1 T1 AM 136.99(10) . . ? O6 T1 AM 109.61(11) . . ? O7 T1 AM 43.25(7) . . ? O5 T1 AM 62.54(7) . . ? M3 T1 AM 104.11(9) . . ? M1 T1 AM 154.63(4) . . ? M2 T1 AM 132.92(10) . . ? A2 T1 AM 9.16(8) 7 . ? M4M T1 AM 87.29(7) 7_556 . ? M4C T1 AM 87.29(7) 7_556 . ? O1 T1 AM 121.80(10) . 5_655 ? O6 T1 AM 126.04(11) . 5_655 ? O7 T1 AM 47.29(8) . 5_655 ? O5 T1 AM 57.51(6) . 5_655 ? M3 T1 AM 91.05(9) . 5_655 ? M1 T1 AM 148.03(7) . 5_655 ? M2 T1 AM 117.24(10) . 5_655 ? A2 T1 AM 9.02(8) 7 5_655 ? M4M T1 AM 96.52(7) 7_556 5_655 ? M4C T1 AM 96.52(7) 7_556 5_655 ? AM T1 AM 16.71(19) . 5_655 ? O4 T2 O2 118.83(7) . . ? O4 T2 O5 110.65(7) . 1_556 ? O2 T2 O5 108.64(6) . 1_556 ? O4 T2 O6 104.65(7) . . ? O2 T2 O6 108.33(6) . . ? O5 T2 O6 104.76(7) 1_556 . ? O4 T2 M4M 47.97(5) . 7_556 ? O2 T2 M4M 132.22(5) . 7_556 ? O5 T2 M4M 118.93(5) 1_556 7_556 ? O6 T2 M4M 56.70(5) . 7_556 ? O4 T2 M4C 47.97(5) . 7_556 ? O2 T2 M4C 132.22(5) . 7_556 ? O5 T2 M4C 118.93(5) 1_556 7_556 ? O6 T2 M4C 56.70(5) . 7_556 ? M4M T2 M4C 0.0 7_556 7_556 ? O4 T2 M1 138.60(5) . . ? O2 T2 M1 31.73(5) . . ? O5 T2 M1 108.29(5) 1_556 . ? O6 T2 M1 78.10(5) . . ? M4M T2 M1 120.13(4) 7_556 . ? M4C T2 M1 120.13(4) 7_556 . ? O4 T2 M2 115.99(5) . 1_556 ? O2 T2 M2 32.46(5) . 1_556 ? O5 T2 M2 81.21(5) 1_556 1_556 ? O6 T2 M2 133.86(5) . 1_556 ? M4M T2 M2 156.46(2) 7_556 1_556 ? M4C T2 M2 156.46(2) 7_556 1_556 ? M1 T2 M2 57.22(3) . 1_556 ? O4 T2 M4C 81.01(6) . . ? O2 T2 M4C 38.92(5) . . ? O5 T2 M4C 136.27(4) 1_556 . ? O6 T2 M4C 112.87(5) . . ? M4M T2 M4C 100.42(4) 7_556 . ? M4C T2 M4C 100.42(4) 7_556 . ? M1 T2 M4C 61.02(4) . . ? M2 T2 M4C 56.84(3) 1_556 . ? O4 T2 AM 123.35(9) . 5_656 ? O2 T2 AM 117.42(8) . 5_656 ? O5 T2 AM 54.85(9) 1_556 5_656 ? O6 T2 AM 50.11(9) . 5_656 ? M4M T2 AM 88.29(6) 7_556 5_656 ? M4C T2 AM 88.29(6) 7_556 5_656 ? M1 T2 AM 90.65(9) . 5_656 ? M2 T2 AM 114.52(6) 1_556 5_656 ? M4C T2 AM 151.04(9) . 5_656 ? A2 AM A2 49.8(12) 3_545 7 ? A2 AM AM 24.9(6) 3_545 5_655 ? A2 AM AM 24.9(6) 7 5_655 ? A2 AM O7 86.8(4) 3_545 . ? A2 AM O7 86.8(4) 7 . ? AM AM O7 86.4(4) 5_655 . ? A2 AM O7 73.1(4) 3_545 5_655 ? A2 AM O7 73.1(4) 7 5_655 ? AM AM O7 71.3(4) 5_655 5_655 ? O7 AM O7 157.7(3) . 5_655 ? A2 AM O6 155.6(7) 3_545 2_656 ? A2 AM O6 105.9(5) 7 2_656 ? AM AM O6 130.73(10) 5_655 2_656 ? O7 AM O6 89.78(12) . 2_656 ? O7 AM O6 104.58(11) 5_655 2_656 ? A2 AM O6 105.9(5) 3_545 5_656 ? A2 AM O6 155.6(7) 7 5_656 ? AM AM O6 130.73(10) 5_655 5_656 ? O7 AM O6 89.78(12) . 5_656 ? O7 AM O6 104.58(11) 5_655 5_656 ? O6 AM O6 98.31(19) 2_656 5_656 ? A2 AM O5 107.5(6) 3_545 2_655 ? A2 AM O5 67.3(5) 7 2_655 ? AM AM O5 87.3(3) 5_655 2_655 ? O7 AM O5 125.07(7) . 2_655 ? O7 AM O5 55.73(7) 5_655 2_655 ? O6 AM O5 55.97(6) 2_656 2_655 ? O6 AM O5 132.25(19) 5_656 2_655 ? A2 AM O5 67.3(5) 3_545 5_655 ? A2 AM O5 107.5(6) 7 5_655 ? AM AM O5 87.3(3) 5_655 5_655 ? O7 AM O5 125.07(7) . 5_655 ? O7 AM O5 55.73(7) 5_655 5_655 ? O6 AM O5 132.25(19) 2_656 5_655 ? O6 AM O5 55.97(6) 5_656 5_655 ? O5 AM O5 109.03(13) 2_655 5_655 ? A2 AM O5 54.1(4) 3_545 6 ? A2 AM O5 94.1(6) 7 6 ? AM AM O5 73.5(3) 5_655 6 ? O7 AM O5 55.11(7) . 6 ? O7 AM O5 115.78(13) 5_655 6 ? O6 AM O5 138.74(16) 2_656 6 ? O6 AM O5 64.48(6) 5_656 6 ? O5 AM O5 160.8(2) 2_655 6 ? O5 AM O5 70.83(6) 5_655 6 ? A2 AM O5 94.1(6) 3_545 . ? A2 AM O5 54.1(4) 7 . ? AM AM O5 73.5(3) 5_655 . ? O7 AM O5 55.11(7) . . ? O7 AM O5 115.78(13) 5_655 . ? O6 AM O5 64.48(6) 2_656 . ? O6 AM O5 138.74(16) 5_656 . ? O5 AM O5 70.83(6) 2_655 . ? O5 AM O5 160.8(2) 5_655 . ? O5 AM O5 102.82(14) 6 . ? A2 AM T1 94.6(5) 3_545 . ? A2 AM T1 72.7(4) 7 . ? AM AM T1 83.1(4) 5_655 . ? O7 AM T1 26.92(3) . . ? O7 AM T1 143.19(15) 5_655 . ? O6 AM T1 72.51(7) 2_656 . ? O6 AM T1 112.18(13) 5_656 . ? O5 AM T1 98.16(6) 2_655 . ? O5 AM T1 150.69(11) 5_655 . ? O5 AM T1 79.89(10) 6 . ? O5 AM T1 28.80(4) . . ? AM A2 AM 130.2(12) 3_455 7 ? AM A2 O7 94.9(4) 3_455 7 ? AM A2 O7 80.6(4) 7 7 ? AM A2 O7 80.6(4) 3_455 3_455 ? AM A2 O7 94.9(4) 7 3_455 ? O7 A2 O7 169.5(2) 7 3_455 ? AM A2 O5 116.6(5) 3_455 8_455 ? AM A2 O5 102.0(5) 7 8_455 ? O7 A2 O5 131.19(16) 7 8_455 ? O7 A2 O5 58.98(6) 3_455 8_455 ? AM A2 O5 102.0(5) 3_455 7 ? AM A2 O5 116.6(5) 7 7 ? O7 A2 O5 58.98(6) 7 7 ? O7 A2 O5 131.19(16) 3_455 7 ? O5 A2 O5 77.70(14) 8_455 7 ? AM A2 O6 165.8(7) 3_455 8_454 ? AM A2 O6 63.9(5) 7 8_454 ? O7 A2 O6 84.88(8) 7 8_454 ? O7 A2 O6 101.82(9) 3_455 8_454 ? O5 A2 O6 55.52(8) 8_455 8_454 ? O5 A2 O6 65.66(10) 7 8_454 ? AM A2 O6 63.9(5) 3_455 7_556 ? AM A2 O6 165.8(7) 7 7_556 ? O7 A2 O6 101.82(9) 7 7_556 ? O7 A2 O6 84.88(8) 3_455 7_556 ? O5 A2 O6 65.66(10) 8_455 7_556 ? O5 A2 O6 55.52(8) 7 7_556 ? O6 A2 O6 102.18(16) 8_454 7_556 ? AM A2 T1 98.1(4) 3_455 8_455 ? AM A2 T1 101.0(4) 7 8_455 ? O7 A2 T1 161.08(18) 7 8_455 ? O7 A2 T1 29.14(4) 3_455 8_455 ? O5 A2 T1 29.90(3) 8_455 8_455 ? O5 A2 T1 104.62(14) 7 8_455 ? O6 A2 T1 79.15(9) 8_454 8_455 ? O6 A2 T1 72.10(8) 7_556 8_455 ? AM A2 T1 101.0(4) 3_455 7 ? AM A2 T1 98.1(4) 7 7 ? O7 A2 T1 29.14(4) 7 7 ? O7 A2 T1 161.08(18) 3_455 7 ? O5 A2 T1 104.62(14) 8_455 7 ? O5 A2 T1 29.90(3) 7 7 ? O6 A2 T1 72.10(8) 8_454 7 ? O6 A2 T1 79.15(9) 7_556 7 ? T1 A2 T1 133.53(16) 8_455 7 ? AM A2 T1 79.1(5) 3_455 4 ? AM A2 T1 76.4(5) 7 4 ? O7 A2 T1 25.60(4) 7 4 ? O7 A2 T1 144.03(18) 3_455 4 ? O5 A2 T1 156.66(12) 8_455 4 ? O5 A2 T1 82.27(4) 7 4 ? O6 A2 T1 105.07(4) 8_454 4 ? O6 A2 T1 111.84(4) 7_556 4 ? T1 A2 T1 173.03(15) 8_455 4 ? T1 A2 T1 53.44(3) 7 4 ? AM A2 T1 76.4(5) 3_455 3_455 ? AM A2 T1 79.1(5) 7 3_455 ? O7 A2 T1 144.03(18) 7 3_455 ? O7 A2 T1 25.60(4) 3_455 3_455 ? O5 A2 T1 82.27(4) 8_455 3_455 ? O5 A2 T1 156.66(12) 7 3_455 ? O6 A2 T1 111.84(4) 8_454 3_455 ? O6 A2 T1 105.07(4) 7_556 3_455 ? T1 A2 T1 53.44(4) 8_455 3_455 ? T1 A2 T1 173.03(15) 7 3_455 ? T1 A2 T1 119.59(14) 4 3_455 ? T1 O1 M3 119.96(6) . . ? T1 O1 M1 121.03(7) . . ? M3 O1 M1 97.09(6) . . ? T1 O1 M2 119.59(6) . . ? M3 O1 M2 99.21(6) . . ? M1 O1 M2 94.45(5) . . ? T2 O2 M1 124.05(7) . . ? T2 O2 M2 123.42(7) . 1_556 ? M1 O2 M2 97.08(6) . 1_556 ? T2 O2 M4C 116.48(6) . . ? M1 O2 M4C 98.52(6) . . ? M2 O2 M4C 89.83(5) 1_556 . ? M3 O3 M1 96.85(6) 1_556 5_556 ? M3 O3 M1 96.85(6) 1_556 . ? M1 O3 M1 100.58(8) 5_556 . ? T2 O4 M2 144.85(8) . 7_556 ? T2 O4 M4M 102.26(6) . 7_556 ? M2 O4 M4M 93.82(6) 7_556 7_556 ? T2 O4 M4C 102.26(6) . 7_556 ? M2 O4 M4C 93.82(6) 7_556 7_556 ? M4M O4 M4C 0.00(3) 7_556 7_556 ? T1 O5 T2 136.05(8) . 1_554 ? T1 O5 A2 93.84(8) . 7 ? T2 O5 A2 104.28(7) 1_554 7 ? T1 O5 M4C 91.70(6) . 7_556 ? T2 O5 M4C 116.37(7) 1_554 7_556 ? A2 O5 M4C 112.45(6) 7 7_556 ? T1 O5 M4M 91.70(6) . 7_556 ? T2 O5 M4M 116.37(7) 1_554 7_556 ? A2 O5 M4M 112.45(6) 7 7_556 ? M4C O5 M4M 0.00(2) 7_556 7_556 ? T1 O5 AM 94.00(9) . 5_655 ? T2 O5 AM 97.10(12) 1_554 5_655 ? A2 O5 AM 10.64(10) 7 5_655 ? M4C O5 AM 123.05(12) 7_556 5_655 ? M4M O5 AM 123.05(12) 7_556 5_655 ? T1 O5 AM 88.66(9) . . ? T2 O5 AM 113.23(11) 1_554 . ? A2 O5 AM 9.33(10) 7 . ? M4C O5 AM 104.91(11) 7_556 . ? M4M O5 AM 104.91(11) 7_556 . ? AM O5 AM 19.2(2) 5_655 . ? T1 O6 T2 136.37(8) . . ? T1 O6 M4M 99.81(6) . 7_556 ? T2 O6 M4M 90.35(6) . 7_556 ? T1 O6 M4C 99.81(6) . 7_556 ? T2 O6 M4C 90.35(6) . 7_556 ? M4M O6 M4C 0.000(18) 7_556 7_556 ? T1 O6 AM 109.24(11) . 5_656 ? T2 O6 AM 101.88(10) . 5_656 ? M4M O6 AM 119.38(10) 7_556 5_656 ? M4C O6 AM 119.38(10) 7_556 5_656 ? T1 O6 A2 118.85(10) . 7_556 ? T2 O6 A2 95.31(8) . 7_556 ? M4M O6 A2 112.06(7) 7_556 7_556 ? M4C O6 A2 112.06(7) 7_556 7_556 ? AM O6 A2 10.26(9) 5_656 7_556 ? T1 O7 T1 137.26(12) . 6 ? T1 O7 AM 109.83(6) . . ? T1 O7 AM 109.83(6) 6 . ? T1 O7 A2 112.98(13) . 3_545 ? T1 O7 A2 102.66(12) 6 3_545 ? AM O7 A2 12.59(11) . 3_545 ? T1 O7 A2 102.66(12) . 7 ? T1 O7 A2 112.98(13) 6 7 ? AM O7 A2 12.59(11) . 7 ? A2 O7 A2 10.5(2) 3_545 7 ? T1 O7 AM 105.27(7) . 5_655 ? T1 O7 AM 105.27(7) 6 5_655 ? AM O7 AM 22.3(3) . 5_655 ? A2 O7 AM 12.05(10) 3_545 5_655 ? A2 O7 AM 12.05(10) 7 5_655 ? _refine_diff_density_max 1.374 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.099 _shelxl_version_number 2014-3 _shelx_res_file ; TITL Am4 in C2/m CELL 0.71073 9.845 17.940 5.294 90.000 105.221 90.000 ZERR 2.00 0.005 0.010 0.003 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 UNIT 4 1 1 8 12 46 2 L.S. 1 BOND ACTA FMAP 2 PLAN 20 WGHT 0.045700 3.683300 EXTI 0.005688 FVAR 0.40113 0.56204 0.01706 M1 4 0.000000 0.089043 0.500000 0.50907 0.00787 0.00769 = 0.00656 0.00000 0.00194 0.00000 M2 4 0.000000 0.178816 0.000000 0.50753 0.00714 0.00712 = 0.00898 0.00000 0.00241 0.00000 M3 4 0.000000 0.000000 0.000000 0.25286 0.00791 0.00632 = 0.00665 0.00000 0.00172 0.00000 M4C 1 0.000000 0.277287 0.500000 20.50000 0.01507 0.01056 = 0.01463 0.00000 0.00890 0.00000 M4M 2 0.000000 0.277287 0.500000 -20.50000 0.01507 0.01056 = 0.01463 0.00000 0.00890 0.00000 T1 5 0.277643 0.084936 0.297254 11.00000 0.00622 0.00617 = 0.00630 -0.00026 0.00116 -0.00034 T2 5 0.286327 0.171748 0.803403 11.00000 0.00577 0.00625 = 0.00586 -0.00037 0.00134 -0.00082 AM 2 0.536125 0.000000 0.085299 0.13370 31.00000 A2 2 0.000000 0.487166 0.000000 0.14230 31.00000 O1 6 0.110690 0.085920 0.218023 11.00000 0.00572 0.00771 = 0.00678 -0.00039 0.00119 -0.00071 O2 6 0.118698 0.169871 0.726466 11.00000 0.00573 0.00954 = 0.00788 -0.00074 0.00145 -0.00066 O3 6 0.106575 0.000000 0.713993 0.52775 0.00849 0.00920 = 0.00882 0.00000 0.00242 0.00000 O4 6 0.362833 0.248408 0.793699 11.00000 0.01161 0.00848 = 0.01046 -0.00072 0.00324 -0.00379 O5 6 0.346385 0.131459 0.094874 11.00000 0.00801 0.01476 = 0.00845 0.00457 0.00196 0.00053 O6 6 0.342244 0.116206 0.593986 11.00000 0.00827 0.01263 = 0.00829 -0.00338 0.00146 0.00079 O7 6 0.337067 0.000000 0.289994 10.50000 0.00947 0.00655 = 0.01745 0.00000 0.00198 0.00000 EXYZ M4C M4M EADP M4C M4M HKLF 4 REM Am4 in C2/m REM R1 = 0.0253 for 1316 Fo > 4sig(Fo) and 0.0262 for all 1379 data REM 107 parameters refined using 0 restraints END WGHT 0.0328 2.7283 REM Highest difference peak 1.374, deepest hole -0.802, 1-sigma level 0.099 Q1 1 0.0238 0.4586 0.0711 11.00000 0.05 1.37 Q2 1 0.0000 0.4519 0.0000 10.50000 0.05 1.34 Q3 1 0.5887 0.0000 0.1915 10.50000 0.05 0.79 Q4 1 0.1949 0.0000 0.7490 10.50000 0.05 0.72 Q5 1 0.4436 0.0000 0.1207 10.50000 0.05 0.48 Q6 1 0.1828 0.0855 0.2583 11.00000 0.05 0.37 Q7 1 0.5969 -0.0200 -0.0064 11.00000 0.05 0.36 Q8 1 0.0000 0.2406 0.5000 10.50000 0.05 0.34 Q9 1 0.1882 0.1752 0.7731 11.00000 0.05 0.34 Q10 1 0.3097 0.0980 0.4764 11.00000 0.05 0.27 Q11 1 0.3304 0.2134 0.7949 11.00000 0.05 0.27 Q12 1 0.3122 0.0000 0.3538 10.50000 0.05 0.25 Q13 1 0.3112 0.1139 0.1588 11.00000 0.05 0.24 Q14 1 0.0259 0.2864 0.5864 11.00000 0.05 0.24 Q15 1 0.0306 0.2601 0.3635 11.00000 0.05 0.23 Q16 1 0.3119 0.1544 -0.0374 11.00000 0.05 0.23 Q17 1 0.3136 0.1368 0.5495 11.00000 0.05 0.21 Q18 1 0.4963 -0.0636 0.2477 11.00000 0.05 0.20 Q19 1 0.0678 0.2783 0.5563 11.00000 0.05 0.20 Q20 1 0.3123 0.1397 0.7139 11.00000 0.05 0.19 ; _shelx_res_checksum 73524 _shelx_hkl_file ; -2 0 0 254.15 3.18 2 0 0 260.78 3.59 -4 0 0 55.890 0.963 4 0 0 55.899 1.154 -6 0 0 2250.13 27.03 6 0 0 2284.47 24.69 -8 0 0 2651.55 32.08 8 0 0 2643.99 31.92 -10 0 0 1087.99 15.60 10 0 0 1100.95 18.33 -12 0 0 6.7109 0.7319 12 0 0 5.7972 1.1012 -1 -1 0 296.70 5.91 1 -1 0 300.29 4.84 -1 1 0 294.32 4.36 1 1 0 304.54 4.71 -3 -1 0 3364.32 62.77 3 -1 0 3235.24 37.26 -3 1 0 3258.88 41.75 3 1 0 3274.94 38.13 -5 -1 0 2162.80 25.57 5 -1 0 2153.68 24.38 -5 1 0 2164.92 24.22 5 1 0 2147.46 25.71 -7 -1 0 982.21 12.14 7 -1 0 989.88 11.13 -7 1 0 968.85 12.32 7 1 0 994.34 11.18 -9 -1 0 115.49 2.17 9 -1 0 120.29 2.56 -9 1 0 119.24 2.45 9 1 0 119.26 2.33 -11 -1 0 783.25 11.52 11 -1 0 778.12 13.57 -11 1 0 759.52 11.47 11 1 0 761.75 16.63 -13 -1 0 275.51 11.64 13 -1 0 292.08 7.87 -13 1 0 285.57 8.10 13 1 0 281.15 7.86 0 -2 0 111.25 2.28 0 2 0 115.79 3.31 -2 -2 0 19.437 0.392 2 -2 0 19.064 0.466 -2 2 0 19.254 0.412 2 2 0 19.886 0.562 -4 -2 0 1.1303 0.1933 4 -2 0 1.5721 0.2115 -4 2 0 1.5813 0.1900 4 2 0 1.1205 0.2062 -6 -2 0 182.32 2.85 6 -2 0 188.28 2.76 -6 2 0 188.11 2.76 6 2 0 189.07 2.80 -8 -2 0 51.681 1.376 8 -2 0 50.237 1.203 -8 2 0 51.839 1.212 8 2 0 52.048 1.266 -10 -2 0 9.7985 0.7545 10 -2 0 10.928 0.977 -10 2 0 12.154 0.850 10 2 0 12.350 0.897 -12 -2 0 36.478 1.486 12 -2 0 38.127 1.936 -12 2 0 35.931 2.571 12 2 0 33.798 2.406 -1 -3 0 26.714 0.511 1 -3 0 28.074 0.526 -1 3 0 28.128 0.498 1 3 0 26.576 0.482 -3 -3 0 1299.83 17.52 3 -3 0 1277.80 15.18 -3 3 0 1274.63 15.45 3 3 0 1284.29 18.48 -5 -3 0 730.41 10.40 5 -3 0 738.57 9.06 -5 3 0 729.88 9.44 5 3 0 735.21 10.53 -7 -3 0 498.55 6.49 7 -3 0 505.15 6.55 -7 3 0 495.36 6.59 7 3 0 499.38 6.62 -9 -3 0 76.812 1.854 9 -3 0 78.239 2.415 -9 3 0 76.848 1.843 9 3 0 78.040 1.707 -11 -3 0 95.980 2.305 11 -3 0 93.840 2.807 -11 3 0 90.447 2.500 11 3 0 90.516 3.456 -13 -3 0 75.684 5.100 13 -3 0 77.921 3.393 -13 3 0 70.983 3.453 13 3 0 77.176 3.438 0 -4 0 1224.30 16.06 0 4 0 1199.85 23.58 -2 -4 0 2843.21 31.74 2 -4 0 2678.48 32.32 -2 4 0 2756.39 37.87 2 4 0 2807.48 37.28 -4 -4 0 38.238 0.916 4 -4 0 37.522 0.805 -4 4 0 37.402 0.784 4 4 0 37.595 0.870 -6 -4 0 64.514 1.456 6 -4 0 66.708 1.306 -6 4 0 64.118 1.264 6 4 0 66.825 1.452 -8 -4 0 45.393 1.295 8 -4 0 45.310 1.153 -8 4 0 45.118 1.118 8 4 0 46.827 1.218 -10 -4 0 4.1535 0.5534 10 -4 0 4.3797 0.6556 -10 4 0 5.8091 0.5873 10 4 0 5.2637 0.7531 -12 -4 0 63.153 1.919 12 -4 0 60.332 2.836 -12 4 0 62.408 3.065 12 4 0 63.610 2.962 -1 -5 0 14.440 0.350 1 -5 0 15.012 0.426 -1 5 0 14.230 0.463 1 5 0 14.653 0.359 -3 -5 0 1165.51 18.25 3 -5 0 1142.23 13.74 -3 5 0 1144.35 16.10 3 5 0 1160.52 14.12 -5 -5 0 52.045 1.403 5 -5 0 58.655 1.132 -5 5 0 56.471 1.316 5 5 0 55.923 1.218 -7 -5 0 8.2523 0.5822 7 -5 0 9.7103 0.5679 -7 5 0 8.3449 0.4995 7 5 0 8.2113 0.5765 -9 -5 0 6.4816 0.6081 9 -5 0 4.4018 0.6423 -9 5 0 6.6285 0.5807 9 5 0 4.7199 0.5506 -11 -5 0 156.75 3.22 11 -5 0 150.63 4.74 -11 5 0 142.11 4.89 11 5 0 156.18 4.83 -13 -5 0 68.902 2.366 13 -5 0 61.884 3.089 -13 5 0 68.048 3.342 13 5 0 63.555 3.113 0 -6 0 3.3448 0.2023 0 6 0 3.3782 0.2609 -2 -6 0 12.076 0.317 2 -6 0 11.173 0.505 -2 6 0 11.551 0.428 2 6 0 11.964 0.413 -4 -6 0 0.4846 0.1515 4 -6 0 0.4862 0.1599 -4 6 0 0.3767 0.1790 4 6 0 0.3798 0.1416 -6 -6 0 43.152 1.158 6 -6 0 43.572 1.074 -6 6 0 42.361 1.195 6 6 0 46.581 1.128 -8 -6 0 134.03 3.28 8 -6 0 133.96 2.63 -8 6 0 139.20 3.34 8 6 0 133.85 2.72 -10 -6 0 98.578 2.313 10 -6 0 101.56 3.53 -10 6 0 99.261 2.949 10 6 0 98.895 3.458 -12 -6 0 23.510 1.480 12 -6 0 23.036 2.044 -12 6 0 22.448 2.085 12 6 0 24.040 2.077 -1 -7 0 32.271 0.749 1 -7 0 32.636 0.746 -1 7 0 29.409 0.741 1 7 0 32.716 0.808 -3 -7 0 697.61 8.33 3 -7 0 677.13 9.56 -3 7 0 696.82 9.98 3 7 0 691.88 9.75 -5 -7 0 101.02 1.70 5 -7 0 104.40 1.76 -5 7 0 101.97 2.06 5 7 0 105.05 1.89 -7 -7 0 214.79 3.80 7 -7 0 223.38 3.36 -7 7 0 223.04 3.92 7 7 0 220.71 4.44 -9 -7 0 598.18 9.00 9 -7 0 590.88 13.06 -9 7 0 596.79 10.94 9 7 0 597.35 9.08 -11 -7 0 16.420 1.068 11 -7 0 16.863 1.663 -11 7 0 18.366 1.792 11 7 0 17.359 1.677 -13 -7 0 15.366 1.297 13 -7 0 16.368 1.829 -13 7 0 15.870 1.933 13 7 0 16.002 1.876 0 -8 0 282.13 3.65 0 8 0 280.25 4.28 -2 -8 0 139.89 1.80 2 -8 0 137.02 2.38 -2 8 0 132.20 2.45 2 8 0 138.93 2.04 -4 -8 0 1983.68 26.09 4 -8 0 1972.95 26.73 -4 8 0 1973.76 27.69 4 8 0 2008.31 24.86 -6 -8 0 883.81 12.66 6 -8 0 895.02 10.99 -6 8 0 871.79 12.84 6 8 0 859.19 14.50 -8 -8 0 0.8105 0.4206 8 -8 0 0.5166 0.3520 -8 8 0 0.2025 0.3681 8 8 0 0.5930 0.3894 -10 -8 0 628.24 10.96 10 -8 0 641.34 13.96 -10 8 0 626.60 14.42 10 8 0 619.16 11.09 -12 -8 0 296.64 6.07 12 -8 0 282.19 7.84 -12 8 0 277.77 8.08 12 8 0 289.16 7.85 -1 -9 0 1126.70 13.36 1 -9 0 1153.25 13.73 -1 9 0 1133.10 15.93 1 9 0 1141.19 15.98 -3 -9 0 13.668 0.424 3 -9 0 13.379 0.705 -3 9 0 13.953 0.826 3 9 0 14.411 0.569 -5 -9 0 5.3158 0.3939 5 -9 0 5.2844 0.4243 -5 9 0 4.8204 0.4713 5 9 0 5.6099 0.4702 -7 -9 0 1789.65 29.18 7 -9 0 1786.63 27.93 -7 9 0 1779.55 25.13 7 9 0 1731.41 28.41 -9 -9 0 152.79 3.85 9 -9 0 166.53 4.78 -9 9 0 153.18 4.85 9 9 0 156.89 3.72 -11 -9 0 72.766 2.355 11 -9 0 72.952 3.160 -11 9 0 74.193 4.619 11 9 0 66.518 4.589 0 -10 0 1729.95 20.45 0 10 0 1700.68 23.81 -2 -10 0 200.47 2.53 2 -10 0 199.76 3.20 -2 10 0 196.26 3.25 2 10 0 196.07 3.34 -4 -10 0 650.03 8.10 4 -10 0 647.03 10.75 -4 10 0 657.47 9.72 4 10 0 658.23 9.47 -6 -10 0 51.146 1.181 6 -10 0 53.317 1.647 -6 10 0 50.305 1.445 6 10 0 52.244 1.585 -8 -10 0 151.42 3.66 8 -10 0 150.65 3.68 -8 10 0 140.60 3.59 8 10 0 143.23 3.42 -10 -10 0 210.54 4.93 10 -10 0 208.66 5.95 -10 10 0 199.27 6.10 10 10 0 199.89 4.77 -12 -10 0 111.75 3.17 12 -10 0 108.25 4.22 -12 10 0 105.93 4.37 12 10 0 115.24 6.50 -1 -11 0 2900.46 33.24 1 -11 0 2912.41 34.06 -1 11 0 2870.61 39.56 1 11 0 2829.97 39.60 -3 -11 0 1491.39 15.96 3 -11 0 1467.45 20.18 -3 11 0 1467.12 20.83 3 11 0 1451.11 20.32 -5 -11 0 266.94 3.83 5 -11 0 269.79 5.07 -5 11 0 268.71 4.57 5 11 0 264.11 4.38 -7 -11 0 4010.20 63.82 7 -11 0 3995.96 64.42 -7 11 0 3995.51 63.84 7 11 0 3904.45 77.54 -9 -11 0 37.749 1.710 9 -11 0 37.343 1.632 -9 11 0 33.780 2.225 9 11 0 37.804 2.244 -11 -11 0 1033.76 17.47 11 -11 0 1015.18 22.06 -11 11 0 1057.37 22.92 11 11 0 1055.50 32.41 0 -12 0 7659.76 92.58 0 12 0 7270.35 111.67 -2 -12 0 327.59 3.98 2 -12 0 331.82 5.02 -2 12 0 323.90 5.11 2 12 0 321.16 5.22 -4 -12 0 532.97 7.68 4 -12 0 538.09 7.94 -4 12 0 533.83 8.23 4 12 0 532.74 9.50 -6 -12 0 149.24 2.52 6 -12 0 150.53 3.38 -6 12 0 148.31 3.44 6 12 0 147.23 3.53 -8 -12 0 552.19 10.27 8 -12 0 552.29 9.78 -8 12 0 539.21 12.72 8 12 0 540.47 12.52 -10 -12 0 802.65 17.85 10 -12 0 779.38 17.20 -10 12 0 790.00 17.84 10 12 0 777.32 17.55 -1 -13 0 25.010 0.771 1 -13 0 25.434 0.799 -1 13 0 23.580 0.854 1 13 0 21.892 0.881 -3 -13 0 47.677 1.217 3 -13 0 47.435 1.266 -3 13 0 48.727 1.605 3 13 0 46.772 1.557 -5 -13 0 721.25 12.40 5 -13 0 727.76 10.60 -5 13 0 723.09 10.94 5 13 0 722.77 12.63 -7 -13 0 285.66 6.00 7 -13 0 285.69 5.69 -7 13 0 281.06 5.99 7 13 0 296.33 7.42 -9 -13 0 106.67 3.98 9 -13 0 111.52 3.05 -9 13 0 116.34 4.22 9 13 0 105.10 3.96 -11 -13 0 71.871 2.599 11 -13 0 61.532 3.103 -11 13 0 73.373 3.531 11 13 0 71.379 4.929 0 -14 0 79.375 2.025 0 14 0 76.509 1.758 -2 -14 0 226.11 3.69 2 -14 0 225.64 4.49 -2 14 0 222.96 4.64 2 14 0 221.48 3.93 -4 -14 0 23.916 0.945 4 -14 0 22.017 0.958 -4 14 0 21.363 1.202 4 14 0 23.179 1.190 -6 -14 0 0.5587 0.2705 6 -14 0 0.3146 0.3248 -6 14 0 0.4857 0.3500 6 14 0 0.7166 0.4413 -8 -14 0 2.4747 0.6657 8 -14 0 1.7738 0.5623 -8 14 0 2.9070 0.8812 8 14 0 3.6850 0.8750 -10 -14 0 1.4522 0.9003 10 -14 0 1.1094 0.7460 -10 14 0 0.7112 0.7615 10 14 0 0.6757 0.7927 -1 -15 0 19.663 0.928 1 -15 0 17.132 1.034 -1 15 0 16.404 1.092 1 15 0 16.631 0.891 -3 -15 0 1.4211 0.3089 3 -15 0 0.2352 0.3170 -3 15 0 0.6636 0.3810 3 15 0 0.5722 0.3725 -5 -15 0 349.16 5.50 5 -15 0 351.68 5.71 -5 15 0 340.20 6.84 5 15 0 341.91 6.83 -7 -15 0 552.85 8.50 7 -15 0 560.72 9.96 -7 15 0 556.25 13.01 7 15 0 547.45 12.78 -9 -15 0 270.51 7.65 9 -15 0 279.95 5.88 -9 15 0 272.35 7.79 9 15 0 259.86 7.56 0 -16 0 0.8182 0.2823 0 16 0 1.3796 0.4470 -2 -16 0 0.0713 0.2275 2 -16 0 0.6126 0.3458 -2 16 0 0.1438 0.3692 2 16 0 0.0826 0.2691 -4 -16 0 642.65 9.35 4 -16 0 655.04 11.32 -4 16 0 631.97 11.60 4 16 0 644.36 11.54 -6 -16 0 161.00 2.83 6 -16 0 163.85 3.86 -6 16 0 156.96 3.93 6 16 0 155.15 3.93 -8 -16 0 19.999 1.883 8 -16 0 19.715 1.405 -8 16 0 20.381 1.952 8 16 0 20.888 1.886 -10 -16 0 216.64 6.80 10 -16 0 222.60 6.58 -10 16 0 220.72 6.95 10 16 0 217.24 6.79 -1 -17 0 28.035 1.169 1 -17 0 28.086 1.257 -1 17 0 26.140 1.416 1 17 0 26.261 1.426 -3 -17 0 112.42 2.36 3 -17 0 112.79 2.92 -3 17 0 111.53 3.05 3 17 0 110.38 2.95 -5 -17 0 10.484 0.792 5 -17 0 10.620 0.996 -5 17 0 9.9400 0.9926 5 17 0 9.2101 0.9615 -7 -17 0 17.363 1.113 7 -17 0 20.583 1.779 -7 17 0 15.408 1.724 7 17 0 18.430 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12.208 1.722 -3 -3 7 13.366 1.437 -3 3 7 12.375 2.400 1 -3 -7 -0.0020 0.7469 1 3 -7 -0.0863 0.8583 -1 -3 7 -0.4459 0.8040 -1 3 7 0.4881 0.8802 6 -4 -7 1.4179 0.9559 6 4 -7 2.1578 0.7816 -6 -4 7 1.9194 1.0145 -6 4 7 0.8744 1.3034 4 -4 -7 3.1632 0.8878 4 4 -7 5.3320 1.2536 -4 -4 7 3.7925 1.1560 -4 4 7 7.1086 1.3008 2 -4 -7 8.8017 1.2258 2 4 -7 9.6230 1.2955 -2 -4 7 9.5474 1.6176 -2 4 7 8.4904 1.4909 0 -4 -7 2.5758 1.1498 0 4 -7 1.6850 0.9982 0 -4 7 2.4456 0.6226 0 4 7 0.8716 1.3761 5 -5 -7 165.15 4.47 5 5 -7 160.27 5.73 -5 -5 7 159.47 5.65 -5 5 7 175.37 7.77 3 -5 -7 161.12 4.42 3 5 -7 148.19 5.53 -3 -5 7 154.00 5.40 -3 5 7 162.64 7.65 1 -5 -7 142.97 4.29 1 5 -7 146.79 5.43 -1 -5 7 143.39 3.63 -1 5 7 152.34 7.27 6 -6 -7 817.31 14.60 6 6 -7 783.61 18.35 -6 -6 7 800.72 18.30 -6 6 7 813.32 24.93 4 -6 -7 547.86 10.49 4 6 -7 536.58 13.48 -4 -6 7 540.77 13.27 -4 6 7 560.83 17.84 2 -6 -7 1557.02 32.15 2 6 -7 1513.86 26.71 -2 -6 7 1583.41 25.26 5 -7 -7 1.3773 0.7599 5 7 -7 1.2991 1.0201 -5 -7 7 2.6764 1.0963 -5 7 7 1.9826 1.3443 3 7 -7 0.7088 0.7638 -3 -7 7 0.6257 0.7362 1 -7 -7 -1.435 1.146 1 7 -7 0.5378 0.9471 -1 -7 7 0.2174 0.5724 4 -8 -7 9.0036 1.4561 4 8 -7 11.745 1.701 -4 -8 7 10.465 1.324 2 8 -7 13.237 1.516 -2 -8 7 15.000 1.359 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 13636 # start CheckCIF/PLATON Validation Reply Form _vrf_PLAT041_I PROBLEM: Calc. and Reported SumFormula Strings Differ Please 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_ABSMU01_I PROBLEM: The ratio of given/expected absorption coefficient lies _vrf_PLAT051_I PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 10.82 % RESPONSE: The ratio of Mu(calc) to Mu(CIF) lies within the range 0.95 <> 1.05 as indicated by alert ABSMU01_ALERT_1_C, an acceptable result for an amphibole with significant short-range disorder such as AM4. _vrf_PLAT075_I PROBLEM: Occupancy 1.018 Greater Than 1.0 for ...... M1 _vrf_PLAT068_I PROBLEM: Reported F000 Differs from Calcd (or Missing)... Please Check _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 and discrepancies between the reported and calculated F000. # end Validation Reply Form