data_fluorapophyllite-(Cs) _publ_section_title 'fluorapophyllite-(Cs)-new mineral' _publ_requested_journal 'Canadian Mineralogist' _publ_contact_author_name 'Elena Sokolova' _publ_contact_author_address 'Dep.of Geological Sciences, University of Manitoba, Winnipeg, Manitoba R3T 2N2,Canada' _publ_contact_author_email elena_sokolova@umanitoba.ca _publ_contact_author_phone '+12044748861' _publ_contact_author_fax '+12044747623' ; _audit_creation_method SHELXL-2014 _chemical_name_systematic ; loop_ _chemical_name_common fluorapophyllite-(Cs) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0.01 H16 Ca3.99 Cs0.75 F0.97 K0.24 Na0.01 O28.03 Si8.01' _chemical_formula_weight 977.52 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' 'F' 'F' 0.0171 0.0103 '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' 'Cs' 'Cs' -0.3680 2.1192 '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' 'Na' 'Na' 0.0362 0.0249 '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' _space_group_crystal_system tetragonal _space_group_IT_number 128 _space_group_name_H-M_alt 'P 4/m n c' _space_group_name_Hall '-P 4 2n' _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' '-y, x, z' 'y, -x, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 9.060(6) _cell_length_b 9.060(6) _cell_length_c 15.741(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1292.1(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5962 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.34 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_density_meas 2.54 _exptl_crystal_density_method floatation _exptl_crystal_density_diffrn 2.513 _exptl_crystal_F_000 974 _exptl_transmission_factor_min 0.897 _exptl_transmission_factor_max 0.930 _exptl_crystal_size_max 0.045 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 2.413 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker D8 QUEST RCO CMOS' _diffrn_measurement_method \\w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7176 _diffrn_reflns_av_unetI/netI 0.0178 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.588 _diffrn_reflns_theta_max 23.977 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.875 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.875 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.875 _reflns_number_total 539 _reflns_number_gt 498 _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 'SMART,version 5.625' _computing_cell_refinement 'SAINT version 6.45' _computing_data_reduction 'SAINT version 6.45' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0322P)^2^+5.9393P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 539 _refine_ls_number_parameters 59 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_restrained_S_all 1.273 _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 F F 0.0000 0.0000 0.0000 0.0141(18) Uani 1 8 d S T P . . Cs Cs 0.0000 0.0000 0.5000 0.0402(6) Uani 0.818(6) 8 d S T P . . Ca Ca 0.10274(14) 0.24597(14) 0.0000 0.0064(4) Uani 1 2 d S T P . . Si Si 0.22099(13) 0.09073(13) 0.19063(7) 0.0053(4) Uani 1 1 d . . . . . O1 O 0.3567(3) 0.1433(3) 0.2500 0.0078(10) Uani 1 2 d S T P . . O2 O 0.0790(3) 0.1897(3) 0.2190(2) 0.0119(8) Uani 1 1 d . . . . . O3 O 0.2578(3) 0.1068(3) 0.09251(19) 0.0103(8) Uani 1 1 d . . . . . O4 O 0.1939(5) 0.4493(4) 0.0907(2) 0.0217(9) Uani 1 1 d D . . . . H1 H 0.219(5) 0.427(5) 0.1498(10) 0.026 Uiso 1 1 d D U . . . H2 H 0.153(5) 0.549(2) 0.085(3) 0.026 Uiso 1 1 d D U . . . 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 F 0.007(2) 0.007(2) 0.028(5) 0.000 0.000 0.000 Cs 0.0196(6) 0.0196(6) 0.0814(13) 0.000 0.000 0.000 Ca 0.0059(7) 0.0071(7) 0.0063(7) 0.000 0.000 0.0013(5) Si 0.0053(7) 0.0046(7) 0.0061(7) -0.0011(5) -0.0016(5) -0.0001(5) O1 0.0071(14) 0.0071(14) 0.009(2) 0.0010(14) 0.0010(14) 0.0011(18) O2 0.0102(18) 0.0109(17) 0.0145(17) -0.0002(14) 0.0010(14) 0.0023(13) O3 0.0101(17) 0.0128(18) 0.0081(16) -0.0027(14) -0.0007(13) 0.0005(13) O4 0.040(2) 0.0115(19) 0.0136(18) -0.0028(15) -0.0022(17) 0.0010(17) _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 F Ca 2.415(2) . ? F Ca 2.415(2) 9 ? F Ca 2.415(2) 11 ? F Ca 2.415(2) 3 ? Cs O4 3.152(4) 15_666 ? Cs O4 3.152(4) 7_445 ? Cs O4 3.152(4) 14_656 ? Cs O4 3.152(4) 6_455 ? Cs O4 3.152(4) 16_556 ? Cs O4 3.152(4) 8 ? Cs O4 3.152(4) 13_566 ? Cs O4 3.152(4) 5_545 ? Cs Ca 4.272(3) 7_445 ? Cs Ca 4.272(3) 15_666 ? Cs Ca 4.272(3) 5_545 ? Cs Ca 4.272(3) 13_566 ? Cs O3 4.430(4) 15_666 ? Cs O3 4.430(4) 7_445 ? Cs O3 4.430(4) 16_556 ? Cs O3 4.430(4) 8 ? Cs O3 4.430(4) 5_545 ? Cs O3 4.430(4) 13_566 ? Cs O3 4.430(4) 6_455 ? Cs O3 4.430(4) 14_656 ? Cs Ca 5.926(4) 5_445 ? Cs Ca 5.926(4) 13_666 ? Cs Ca 5.926(4) 15_656 ? Cs Ca 5.926(4) 7_455 ? Ca O3 2.384(3) . ? Ca O3 2.384(3) 10 ? Ca O3 2.395(3) 12 ? Ca O3 2.395(3) 3 ? Ca O4 2.473(4) 10 ? Ca O4 2.473(4) . ? Ca Ca 3.415(3) 3 ? Ca Ca 3.415(3) 11 ? Ca Si 3.482(2) 12 ? Ca Si 3.482(2) 3 ? Ca Si 3.483(2) 10 ? Si O3 1.587(3) . ? Si O1 1.616(2) . ? Si O2 1.626(3) 4 ? Si O2 1.631(3) . ? Si Ca 3.482(2) 11 ? O1 Si 1.616(2) 8 ? O2 Si 1.626(3) 3 ? O3 Ca 2.395(3) 11 ? O3 Cs 4.430(4) 5 ? O4 Cs 3.152(4) 5 ? O4 H1 0.9799(12) . ? O4 H2 0.9800(12) . ? 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 Ca F Ca 180.0 . 9 ? Ca F Ca 90.0 . 11 ? Ca F Ca 90.0 9 11 ? Ca F Ca 90.0 . 3 ? Ca F Ca 90.0 9 3 ? Ca F Ca 180.00(6) 11 3 ? O4 Cs O4 180.0 15_666 7_445 ? O4 Cs O4 78.17(6) 15_666 14_656 ? O4 Cs O4 101.83(6) 7_445 14_656 ? O4 Cs O4 101.83(6) 15_666 6_455 ? O4 Cs O4 78.17(6) 7_445 6_455 ? O4 Cs O4 180.0 14_656 6_455 ? O4 Cs O4 126.16(14) 15_666 16_556 ? O4 Cs O4 53.84(14) 7_445 16_556 ? O4 Cs O4 78.17(6) 14_656 16_556 ? O4 Cs O4 101.83(6) 6_455 16_556 ? O4 Cs O4 53.84(14) 15_666 8 ? O4 Cs O4 126.16(14) 7_445 8 ? O4 Cs O4 101.83(6) 14_656 8 ? O4 Cs O4 78.17(6) 6_455 8 ? O4 Cs O4 180.0 16_556 8 ? O4 Cs O4 78.17(6) 15_666 13_566 ? O4 Cs O4 101.83(6) 7_445 13_566 ? O4 Cs O4 126.16(14) 14_656 13_566 ? O4 Cs O4 53.84(14) 6_455 13_566 ? O4 Cs O4 78.17(6) 16_556 13_566 ? O4 Cs O4 101.83(6) 8 13_566 ? O4 Cs O4 101.83(6) 15_666 5_545 ? O4 Cs O4 78.17(6) 7_445 5_545 ? O4 Cs O4 53.84(14) 14_656 5_545 ? O4 Cs O4 126.16(14) 6_455 5_545 ? O4 Cs O4 101.83(6) 16_556 5_545 ? O4 Cs O4 78.17(6) 8 5_545 ? O4 Cs O4 180.0 13_566 5_545 ? O4 Cs Ca 145.04(7) 15_666 7_445 ? O4 Cs Ca 34.96(7) 7_445 7_445 ? O4 Cs Ca 110.56(7) 14_656 7_445 ? O4 Cs Ca 69.44(7) 6_455 7_445 ? O4 Cs Ca 34.96(7) 16_556 7_445 ? O4 Cs Ca 145.04(7) 8 7_445 ? O4 Cs Ca 69.44(7) 13_566 7_445 ? O4 Cs Ca 110.56(7) 5_545 7_445 ? O4 Cs Ca 34.96(7) 15_666 15_666 ? O4 Cs Ca 145.04(7) 7_445 15_666 ? O4 Cs Ca 69.44(7) 14_656 15_666 ? O4 Cs Ca 110.56(7) 6_455 15_666 ? O4 Cs Ca 145.04(7) 16_556 15_666 ? O4 Cs Ca 34.96(7) 8 15_666 ? O4 Cs Ca 110.56(7) 13_566 15_666 ? O4 Cs Ca 69.44(7) 5_545 15_666 ? Ca Cs Ca 180.000(18) 7_445 15_666 ? O4 Cs Ca 110.56(7) 15_666 5_545 ? O4 Cs Ca 69.44(7) 7_445 5_545 ? O4 Cs Ca 34.96(7) 14_656 5_545 ? O4 Cs Ca 145.04(7) 6_455 5_545 ? O4 Cs Ca 69.44(7) 16_556 5_545 ? O4 Cs Ca 110.56(7) 8 5_545 ? O4 Cs Ca 145.04(7) 13_566 5_545 ? O4 Cs Ca 34.96(7) 5_545 5_545 ? Ca Cs Ca 90.0 7_445 5_545 ? Ca Cs Ca 90.0 15_666 5_545 ? O4 Cs Ca 69.44(7) 15_666 13_566 ? O4 Cs Ca 110.56(7) 7_445 13_566 ? O4 Cs Ca 145.04(7) 14_656 13_566 ? O4 Cs Ca 34.96(7) 6_455 13_566 ? O4 Cs Ca 110.56(7) 16_556 13_566 ? O4 Cs Ca 69.44(7) 8 13_566 ? O4 Cs Ca 34.96(7) 13_566 13_566 ? O4 Cs Ca 145.04(7) 5_545 13_566 ? Ca Cs Ca 90.0 7_445 13_566 ? Ca Cs Ca 90.0 15_666 13_566 ? Ca Cs Ca 180.0 5_545 13_566 ? O4 Cs O3 45.44(8) 15_666 15_666 ? O4 Cs O3 134.56(8) 7_445 15_666 ? O4 Cs O3 38.37(8) 14_656 15_666 ? O4 Cs O3 141.63(8) 6_455 15_666 ? O4 Cs O3 113.83(8) 16_556 15_666 ? O4 Cs O3 66.17(8) 8 15_666 ? O4 Cs O3 119.11(8) 13_566 15_666 ? O4 Cs O3 60.89(8) 5_545 15_666 ? Ca Cs O3 148.26(4) 7_445 15_666 ? Ca Cs O3 31.74(4) 15_666 15_666 ? Ca Cs O3 65.75(4) 5_545 15_666 ? Ca Cs O3 114.25(4) 13_566 15_666 ? O4 Cs O3 134.56(8) 15_666 7_445 ? O4 Cs O3 45.44(8) 7_445 7_445 ? O4 Cs O3 141.63(8) 14_656 7_445 ? O4 Cs O3 38.37(8) 6_455 7_445 ? O4 Cs O3 66.17(8) 16_556 7_445 ? O4 Cs O3 113.83(8) 8 7_445 ? O4 Cs O3 60.89(8) 13_566 7_445 ? O4 Cs O3 119.11(8) 5_545 7_445 ? Ca Cs O3 31.74(4) 7_445 7_445 ? Ca Cs O3 148.26(4) 15_666 7_445 ? Ca Cs O3 114.25(4) 5_545 7_445 ? Ca Cs O3 65.75(4) 13_566 7_445 ? O3 Cs O3 180.00(5) 15_666 7_445 ? O4 Cs O3 113.83(8) 15_666 16_556 ? O4 Cs O3 66.17(8) 7_445 16_556 ? O4 Cs O3 119.11(8) 14_656 16_556 ? O4 Cs O3 60.89(8) 6_455 16_556 ? O4 Cs O3 45.44(8) 16_556 16_556 ? O4 Cs O3 134.56(8) 8 16_556 ? O4 Cs O3 38.37(8) 13_566 16_556 ? O4 Cs O3 141.63(8) 5_545 16_556 ? Ca Cs O3 31.74(4) 7_445 16_556 ? Ca Cs O3 148.26(4) 15_666 16_556 ? Ca Cs O3 114.25(4) 5_545 16_556 ? Ca Cs O3 65.75(4) 13_566 16_556 ? O3 Cs O3 141.62(8) 15_666 16_556 ? O3 Cs O3 38.38(8) 7_445 16_556 ? O4 Cs O3 66.17(8) 15_666 8 ? O4 Cs O3 113.83(8) 7_445 8 ? O4 Cs O3 60.89(8) 14_656 8 ? O4 Cs O3 119.11(8) 6_455 8 ? O4 Cs O3 134.56(8) 16_556 8 ? O4 Cs O3 45.44(8) 8 8 ? O4 Cs O3 141.63(8) 13_566 8 ? O4 Cs O3 38.37(8) 5_545 8 ? Ca Cs O3 148.26(4) 7_445 8 ? Ca Cs O3 31.74(4) 15_666 8 ? Ca Cs O3 65.75(4) 5_545 8 ? Ca Cs O3 114.25(4) 13_566 8 ? O3 Cs O3 38.38(8) 15_666 8 ? O3 Cs O3 141.62(8) 7_445 8 ? O3 Cs O3 180.0 16_556 8 ? O4 Cs O3 141.63(8) 15_666 5_545 ? O4 Cs O3 38.37(8) 7_445 5_545 ? O4 Cs O3 66.17(8) 14_656 5_545 ? O4 Cs O3 113.83(8) 6_455 5_545 ? O4 Cs O3 60.89(8) 16_556 5_545 ? O4 Cs O3 119.11(8) 8 5_545 ? O4 Cs O3 134.56(8) 13_566 5_545 ? O4 Cs O3 45.44(8) 5_545 5_545 ? Ca Cs O3 65.75(4) 7_445 5_545 ? Ca Cs O3 114.25(4) 15_666 5_545 ? Ca Cs O3 31.74(4) 5_545 5_545 ? Ca Cs O3 148.26(4) 13_566 5_545 ? O3 Cs O3 96.20(3) 15_666 5_545 ? O3 Cs O3 83.80(3) 7_445 5_545 ? O3 Cs O3 96.20(3) 16_556 5_545 ? O3 Cs O3 83.80(3) 8 5_545 ? O4 Cs O3 38.37(8) 15_666 13_566 ? O4 Cs O3 141.63(8) 7_445 13_566 ? O4 Cs O3 113.83(8) 14_656 13_566 ? O4 Cs O3 66.17(8) 6_455 13_566 ? O4 Cs O3 119.11(8) 16_556 13_566 ? O4 Cs O3 60.89(8) 8 13_566 ? O4 Cs O3 45.44(8) 13_566 13_566 ? O4 Cs O3 134.56(8) 5_545 13_566 ? Ca Cs O3 114.25(4) 7_445 13_566 ? Ca Cs O3 65.75(4) 15_666 13_566 ? Ca Cs O3 148.26(4) 5_545 13_566 ? Ca Cs O3 31.74(4) 13_566 13_566 ? O3 Cs O3 83.80(3) 15_666 13_566 ? O3 Cs O3 96.20(3) 7_445 13_566 ? O3 Cs O3 83.80(3) 16_556 13_566 ? O3 Cs O3 96.20(3) 8 13_566 ? O3 Cs O3 180.00(7) 5_545 13_566 ? O4 Cs O3 60.89(8) 15_666 6_455 ? O4 Cs O3 119.11(8) 7_445 6_455 ? O4 Cs O3 134.56(8) 14_656 6_455 ? O4 Cs O3 45.44(8) 6_455 6_455 ? O4 Cs O3 141.63(8) 16_556 6_455 ? O4 Cs O3 38.37(8) 8 6_455 ? O4 Cs O3 66.17(8) 13_566 6_455 ? O4 Cs O3 113.83(8) 5_545 6_455 ? Ca Cs O3 114.25(4) 7_445 6_455 ? Ca Cs O3 65.75(4) 15_666 6_455 ? Ca Cs O3 148.26(4) 5_545 6_455 ? Ca Cs O3 31.74(4) 13_566 6_455 ? O3 Cs O3 96.20(3) 15_666 6_455 ? O3 Cs O3 83.80(3) 7_445 6_455 ? O3 Cs O3 96.20(3) 16_556 6_455 ? O3 Cs O3 83.80(3) 8 6_455 ? O3 Cs O3 141.62(8) 5_545 6_455 ? O3 Cs O3 38.38(8) 13_566 6_455 ? O4 Cs O3 119.11(8) 15_666 14_656 ? O4 Cs O3 60.89(8) 7_445 14_656 ? O4 Cs O3 45.44(8) 14_656 14_656 ? O4 Cs O3 134.56(8) 6_455 14_656 ? O4 Cs O3 38.37(8) 16_556 14_656 ? O4 Cs O3 141.63(8) 8 14_656 ? O4 Cs O3 113.83(8) 13_566 14_656 ? O4 Cs O3 66.17(8) 5_545 14_656 ? Ca Cs O3 65.75(4) 7_445 14_656 ? Ca Cs O3 114.25(4) 15_666 14_656 ? Ca Cs O3 31.74(4) 5_545 14_656 ? Ca Cs O3 148.26(4) 13_566 14_656 ? O3 Cs O3 83.80(3) 15_666 14_656 ? O3 Cs O3 96.20(3) 7_445 14_656 ? O3 Cs O3 83.80(3) 16_556 14_656 ? O3 Cs O3 96.20(3) 8 14_656 ? O3 Cs O3 38.38(8) 5_545 14_656 ? O3 Cs O3 141.62(9) 13_566 14_656 ? O3 Cs O3 180.0 6_455 14_656 ? O4 Cs Ca 118.42(7) 15_666 5_445 ? O4 Cs Ca 61.58(7) 7_445 5_445 ? O4 Cs Ca 138.94(7) 14_656 5_445 ? O4 Cs Ca 41.06(7) 6_455 5_445 ? O4 Cs Ca 61.58(7) 16_556 5_445 ? O4 Cs Ca 118.42(7) 8 5_445 ? O4 Cs Ca 41.06(7) 13_566 5_445 ? O4 Cs Ca 138.94(7) 5_545 5_445 ? Ca Cs Ca 34.55(3) 7_445 5_445 ? Ca Cs Ca 145.45(3) 15_666 5_445 ? Ca Cs Ca 124.55(3) 5_545 5_445 ? Ca Cs Ca 55.45(3) 13_566 5_445 ? O3 Cs Ca 158.97(4) 15_666 5_445 ? O3 Cs Ca 21.03(4) 7_445 5_445 ? O3 Cs Ca 21.03(4) 16_556 5_445 ? O3 Cs Ca 158.97(4) 8 5_445 ? O3 Cs Ca 98.28(4) 5_545 5_445 ? O3 Cs Ca 81.72(4) 13_566 5_445 ? O3 Cs Ca 81.72(4) 6_455 5_445 ? O3 Cs Ca 98.28(4) 14_656 5_445 ? O4 Cs Ca 61.58(7) 15_666 13_666 ? O4 Cs Ca 118.42(7) 7_445 13_666 ? O4 Cs Ca 41.06(7) 14_656 13_666 ? O4 Cs Ca 138.94(7) 6_455 13_666 ? O4 Cs Ca 118.42(7) 16_556 13_666 ? O4 Cs Ca 61.58(7) 8 13_666 ? O4 Cs Ca 138.94(7) 13_566 13_666 ? O4 Cs Ca 41.06(7) 5_545 13_666 ? Ca Cs Ca 145.45(3) 7_445 13_666 ? Ca Cs Ca 34.55(3) 15_666 13_666 ? Ca Cs Ca 55.45(3) 5_545 13_666 ? Ca Cs Ca 124.55(3) 13_566 13_666 ? O3 Cs Ca 21.03(4) 15_666 13_666 ? O3 Cs Ca 158.97(4) 7_445 13_666 ? O3 Cs Ca 158.97(4) 16_556 13_666 ? O3 Cs Ca 21.03(4) 8 13_666 ? O3 Cs Ca 81.72(4) 5_545 13_666 ? O3 Cs Ca 98.28(4) 13_566 13_666 ? O3 Cs Ca 98.28(4) 6_455 13_666 ? O3 Cs Ca 81.72(4) 14_656 13_666 ? Ca Cs Ca 180.0 5_445 13_666 ? O4 Cs Ca 138.94(7) 15_666 15_656 ? O4 Cs Ca 41.06(7) 7_445 15_656 ? O4 Cs Ca 61.58(7) 14_656 15_656 ? O4 Cs Ca 118.42(7) 6_455 15_656 ? O4 Cs Ca 41.06(7) 16_556 15_656 ? O4 Cs Ca 138.94(7) 8 15_656 ? O4 Cs Ca 118.42(7) 13_566 15_656 ? O4 Cs Ca 61.58(7) 5_545 15_656 ? Ca Cs Ca 55.45(3) 7_445 15_656 ? Ca Cs Ca 124.55(3) 15_666 15_656 ? Ca Cs Ca 34.55(3) 5_545 15_656 ? Ca Cs Ca 145.45(3) 13_566 15_656 ? O3 Cs Ca 98.28(4) 15_666 15_656 ? O3 Cs Ca 81.72(4) 7_445 15_656 ? O3 Cs Ca 81.72(4) 16_556 15_656 ? O3 Cs Ca 98.28(4) 8 15_656 ? O3 Cs Ca 21.03(4) 5_545 15_656 ? O3 Cs Ca 158.97(4) 13_566 15_656 ? O3 Cs Ca 158.97(4) 6_455 15_656 ? O3 Cs Ca 21.03(4) 14_656 15_656 ? Ca Cs Ca 90.0 5_445 15_656 ? Ca Cs Ca 90.0 13_666 15_656 ? O4 Cs Ca 41.06(7) 15_666 7_455 ? O4 Cs Ca 138.94(7) 7_445 7_455 ? O4 Cs Ca 118.42(7) 14_656 7_455 ? O4 Cs Ca 61.58(7) 6_455 7_455 ? O4 Cs Ca 138.94(7) 16_556 7_455 ? O4 Cs Ca 41.06(7) 8 7_455 ? O4 Cs Ca 61.58(7) 13_566 7_455 ? O4 Cs Ca 118.42(7) 5_545 7_455 ? Ca Cs Ca 124.55(3) 7_445 7_455 ? Ca Cs Ca 55.45(3) 15_666 7_455 ? Ca Cs Ca 145.45(3) 5_545 7_455 ? Ca Cs Ca 34.55(3) 13_566 7_455 ? O3 Cs Ca 81.72(4) 15_666 7_455 ? O3 Cs Ca 98.28(4) 7_445 7_455 ? O3 Cs Ca 98.28(4) 16_556 7_455 ? O3 Cs Ca 81.72(4) 8 7_455 ? O3 Cs Ca 158.97(4) 5_545 7_455 ? O3 Cs Ca 21.03(4) 13_566 7_455 ? O3 Cs Ca 21.03(4) 6_455 7_455 ? O3 Cs Ca 158.97(4) 14_656 7_455 ? Ca Cs Ca 90.0 5_445 7_455 ? Ca Cs Ca 90.0 13_666 7_455 ? Ca Cs Ca 180.0 15_656 7_455 ? O3 Ca O3 75.29(16) . 10 ? O3 Ca O3 149.55(14) . 12 ? O3 Ca O3 96.85(15) 10 12 ? O3 Ca O3 96.85(15) . 3 ? O3 Ca O3 149.55(14) 10 3 ? O3 Ca O3 74.91(16) 12 3 ? O3 Ca F 74.87(8) . . ? O3 Ca F 74.87(8) 10 . ? O3 Ca F 74.68(8) 12 . ? O3 Ca F 74.68(8) 3 . ? O3 Ca O4 123.35(14) . 10 ? O3 Ca O4 81.07(12) 10 10 ? O3 Ca O4 83.14(13) 12 10 ? O3 Ca O4 125.63(13) 3 10 ? F Ca O4 144.72(9) . 10 ? O3 Ca O4 81.07(12) . . ? O3 Ca O4 123.35(14) 10 . ? O3 Ca O4 125.63(13) 12 . ? O3 Ca O4 83.14(13) 3 . ? F Ca O4 144.72(9) . . ? O4 Ca O4 70.51(18) 10 . ? O3 Ca Ca 110.12(8) . 3 ? O3 Ca Ca 110.12(8) 10 3 ? O3 Ca Ca 44.26(8) 12 3 ? O3 Ca Ca 44.26(8) 3 3 ? F Ca Ca 45.0 . 3 ? O4 Ca Ca 126.32(11) 10 3 ? O4 Ca Ca 126.32(11) . 3 ? O3 Ca Ca 44.51(8) . 11 ? O3 Ca Ca 44.51(8) 10 11 ? O3 Ca Ca 110.03(8) 12 11 ? O3 Ca Ca 110.03(8) 3 11 ? F Ca Ca 45.0 . 11 ? O4 Ca Ca 124.21(10) 10 11 ? O4 Ca Ca 124.21(10) . 11 ? Ca Ca Ca 90.0 3 11 ? O3 Ca Si 142.04(9) . 12 ? O3 Ca Si 74.69(9) 10 12 ? O3 Ca Si 23.07(8) 12 12 ? O3 Ca Si 97.35(10) 3 12 ? F Ca Si 75.29(3) . 12 ? O4 Ca Si 73.70(10) 10 12 ? O4 Ca Si 135.56(10) . 12 ? Ca Ca Si 60.64(4) 3 12 ? Ca Ca Si 97.53(3) 11 12 ? O3 Ca Si 74.69(9) . 3 ? O3 Ca Si 142.04(9) 10 3 ? O3 Ca Si 97.35(10) 12 3 ? O3 Ca Si 23.07(8) 3 3 ? F Ca Si 75.29(3) . 3 ? O4 Ca Si 135.56(10) 10 3 ? O4 Ca Si 73.70(10) . 3 ? Ca Ca Si 60.64(4) 3 3 ? Ca Ca Si 97.53(3) 11 3 ? Si Ca Si 119.01(7) 12 3 ? O3 Ca Si 97.55(10) . 10 ? O3 Ca Si 22.92(8) 10 10 ? O3 Ca Si 74.81(9) 12 10 ? O3 Ca Si 141.80(9) 3 10 ? F Ca Si 75.28(3) . 10 ? O4 Ca Si 72.59(9) 10 10 ? O4 Ca Si 134.06(10) . 10 ? Ca Ca Si 97.53(3) 3 10 ? Ca Ca Si 60.63(4) 11 10 ? Si Ca Si 52.14(5) 12 10 ? Si Ca Si 150.57(6) 3 10 ? O3 Si O1 112.09(15) . . ? O3 Si O2 113.00(17) . 4 ? O1 Si O2 104.63(17) . 4 ? O3 Si O2 112.48(17) . . ? O1 Si O2 106.23(19) . . ? O2 Si O2 107.9(2) 4 . ? O3 Si Ca 36.26(12) . 11 ? O1 Si Ca 126.68(13) . 11 ? O2 Si Ca 76.84(12) 4 11 ? O2 Si Ca 124.35(13) . 11 ? O3 Si Ca 35.82(12) . . ? O1 Si Ca 127.82(8) . . ? O2 Si Ca 124.40(13) 4 . ? O2 Si Ca 76.79(12) . . ? Ca Si Ca 58.73(6) 11 . ? Si O1 Si 141.5(3) . 8 ? Si O2 Si 140.0(2) 3 . ? Si O3 Ca 121.27(18) . . ? Si O3 Ca 120.66(18) . 11 ? Ca O3 Ca 91.23(12) . 11 ? Si O3 Cs 119.85(14) . 5 ? Ca O3 Cs 70.47(8) . 5 ? Ca O3 Cs 117.36(11) 11 5 ? Ca O4 Cs 98.12(12) . 5 ? Ca O4 H1 118(3) . . ? Cs O4 H1 105(3) 5 . ? Ca O4 H2 120(3) . . ? Cs O4 H2 99(3) 5 . ? H1 O4 H2 112(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O2 0.9799(12) 2.225(13) 3.186(5) 167(4) 8 O4 H2 O3 0.9800(12) 1.805(12) 2.769(5) 167(4) 4_565 _refine_diff_density_max 0.421 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.111 _shelxl_version_number 2014-3 _shelx_res_file ; TITL apophyllite 1 in P4/mnc CELL 0.71073 9.06000 9.06000 15.74100 90.0000 90.0000 90.0000 ZERR 2.00 0.006 0.006 0.01100 0.0000 0.0000 0.0000 LATT 1 SYMM -X, -Y, Z SYMM -Y, X, Z SYMM Y, -X, Z SYMM 0.5-X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, 0.5-Z SYMM 0.5+Y, 0.5+X, 0.5-Z SYMM 0.5-Y, 0.5-X, 0.5-Z SFAC O H F SI CA CS K NA AL UNIT 56.06 32 1.94 16.02 7.98 1.50 0.48 0.02 0.02 L.S. 6 ACTA BOND $H OMIT 0 0 11 OMIT -3 48.00 EQIV_$18 -y+1/2,-x+1/2,-z+1/2 EQIV_$21 y,-x+1,z DFIX 0.98 0.001 O4 H1 DFIX 0.98 0.001 O4 H2 HTAB O4 O2_$18 HTAB O4 O3_$21 CONN 30 3.5 CS FMAP 2 PLAN 20 WGHT 0.032200 5.939300 FVAR 0.31825 0.81798 F 3 0.000000 0.000000 0.000000 10.12500 0.00744 0.00744 = 0.02756 0.00000 0.00000 0.00000 CS 6 0.000000 0.000000 0.500000 20.12500 0.01960 0.01960 = 0.08136 0.00000 0.00000 0.00000 CA 5 0.102736 0.245972 0.000000 10.50000 0.00594 0.00710 = 0.00627 0.00000 0.00000 0.00125 SI 4 0.220988 0.090726 0.190628 11.00000 0.00526 0.00459 = 0.00605 -0.00112 -0.00161 -0.00009 O1 1 0.356670 0.143330 0.250000 10.50000 0.00710 0.00710 = 0.00920 0.00100 0.00100 0.00108 O2 1 0.078991 0.189675 0.219025 11.00000 0.01025 0.01088 = 0.01446 -0.00023 0.00098 0.00225 O3 1 0.257804 0.106758 0.092513 11.00000 0.01014 0.01277 = 0.00811 -0.00273 -0.00069 0.00055 O4 1 0.193949 0.449320 0.090667 11.00000 0.03997 0.01145 = 0.01359 -0.00285 -0.00225 0.00098 H1 2 0.219052 0.426622 0.149794 11.00000 -1.20000 H2 2 0.152581 0.548752 0.084860 11.00000 -1.20000 HKLF 4 REM apophyllite 1 in P4/mnc REM R1 = 0.0431 for 498 Fo > 4sig(Fo) and 0.0487 for all 539 data REM 59 parameters refined using 2 restraints END WGHT 0.0301 6.4120 REM Highest difference peak 0.421, deepest hole -0.519, 1-sigma level 0.111 Q1 1 0.4516 0.1151 0.2166 11.00000 0.05 0.42 Q2 1 -0.0037 0.0544 0.4334 11.00000 0.05 0.39 Q3 1 -0.0776 0.0175 0.4537 11.00000 0.05 0.38 Q4 1 0.5000 0.0000 0.2500 10.25000 0.05 0.37 Q5 1 0.2376 0.1121 0.1319 11.00000 0.05 0.37 Q6 1 0.2950 0.6353 0.0000 10.50000 0.05 0.35 Q7 1 0.1116 0.2949 0.1860 11.00000 0.05 0.34 Q8 1 0.0000 0.0000 0.3625 10.25000 0.05 0.33 Q9 1 0.1114 0.1448 0.1924 11.00000 0.05 0.33 Q10 1 0.1849 0.2775 0.0000 10.50000 0.05 0.32 Q11 1 0.2648 0.6598 0.0000 10.50000 0.05 0.32 Q12 1 0.2851 0.1881 0.0000 10.50000 0.05 0.30 Q13 1 0.1590 0.2593 0.1920 11.00000 0.05 0.30 Q14 1 0.2495 0.4787 0.0000 10.50000 0.05 0.30 Q15 1 0.2503 0.1851 0.2283 11.00000 0.05 0.30 Q16 1 0.0262 0.1932 0.1965 11.00000 0.05 0.29 Q17 1 0.3191 0.0570 0.0705 11.00000 0.05 0.28 Q18 1 0.2531 0.5021 0.2063 11.00000 0.05 0.28 Q19 1 0.2107 -0.0210 0.0983 11.00000 0.05 0.28 Q20 1 0.0901 0.0334 0.0000 10.50000 0.05 0.28 ; _shelx_res_checksum 64330 _shelx_hkl_file ; 0 1 0 1.6943 5.0060 -1 -1 0 1022.43 15.39 1 -1 0 1020.74 21.63 -1 1 0 1031.27 18.42 1 1 0 956.55 29.57 0 -2 0 438.86 10.53 -2 0 0 428.28 7.61 2 0 0 438.67 7.53 0 2 0 433.42 9.36 -1 -2 0 120.92 8.15 1 -2 0 127.19 5.34 -2 -1 0 128.14 7.71 2 -1 0 136.18 6.49 2 1 0 125.93 4.44 -1 2 0 126.60 6.66 1 2 0 126.20 8.12 -2 -2 0 2086.50 25.46 2 -2 0 2068.43 18.67 2 2 0 2114.79 20.53 0 -3 0 9.0050 7.4689 -3 0 0 1.6296 4.1765 3 0 0 -3.798 5.644 0 3 0 1.4174 6.3751 -1 -3 0 571.12 11.91 1 -3 0 565.27 11.93 -3 -1 0 565.58 14.06 3 -1 0 572.68 9.26 -3 1 0 571.93 10.90 3 1 0 570.03 18.37 -1 3 0 566.55 12.80 1 3 0 547.51 12.89 -2 -3 0 5.3186 6.3080 2 -3 0 2.1674 5.2807 -3 -2 0 -0.1190 8.4783 3 -2 0 8.1537 5.4037 3 2 0 12.223 3.766 -2 3 0 5.1640 4.9388 2 3 0 11.451 6.389 -3 -3 0 689.08 15.91 3 -3 0 675.65 12.03 3 3 0 685.52 15.21 0 -4 0 355.20 11.82 -4 0 0 359.01 7.68 4 0 0 350.77 13.35 0 4 0 356.21 12.26 -1 -4 0 135.33 9.13 1 -4 0 145.03 11.55 -4 -1 0 130.35 9.64 4 -1 0 124.83 7.05 -4 1 0 119.28 8.41 4 1 0 129.57 8.87 -1 4 0 124.37 8.79 1 4 0 121.81 9.79 -2 -4 0 6381.24 59.33 2 -4 0 6358.20 52.55 -4 -2 0 6474.64 69.45 4 -2 0 6354.01 48.59 -4 2 0 6179.70 73.78 4 2 0 6258.16 61.92 -2 4 0 6297.21 68.04 2 4 0 6420.83 60.68 -3 -4 0 19.571 10.090 3 -4 0 18.197 7.247 -4 -3 0 11.337 9.625 4 -3 0 18.073 6.905 4 3 0 16.226 6.244 -3 4 0 26.406 6.090 3 4 0 27.333 8.489 -4 -4 0 1025.69 22.59 4 -4 0 1030.72 17.49 -4 4 0 1013.82 20.20 4 4 0 1040.33 17.63 0 -5 0 -0.8987 7.7402 -5 0 0 5.5503 4.7701 5 0 0 -0.8663 9.4038 0 5 0 -0.3828 9.7501 -1 -5 0 839.24 18.04 1 -5 0 845.64 20.50 -5 -1 0 849.22 19.42 5 -1 0 869.87 23.39 -5 1 0 849.33 12.52 5 1 0 883.91 18.05 -1 5 0 851.59 17.91 1 5 0 880.51 20.13 -2 -5 0 8.4037 9.8540 2 -5 0 17.194 10.306 -5 -2 0 21.284 11.779 5 -2 0 16.487 7.360 -5 2 0 10.793 6.014 5 2 0 16.991 9.436 -2 5 0 5.7756 7.3470 2 5 0 30.801 14.604 -3 -5 0 745.28 21.82 3 -5 0 741.90 15.18 -5 -3 0 736.17 26.55 5 -3 0 730.94 14.21 5 3 0 748.02 19.63 -3 5 0 760.02 17.82 3 5 0 729.44 17.70 -4 -5 0 307.08 17.19 4 -5 0 314.55 13.00 -5 -4 0 278.48 16.58 5 -4 0 329.15 13.19 5 4 0 312.59 12.39 -4 5 0 308.37 16.71 4 5 0 327.11 14.28 -5 -5 0 418.49 21.35 5 -5 0 407.45 15.65 -5 5 0 395.43 10.95 5 5 0 439.62 16.01 0 -6 0 1845.00 27.79 -6 0 0 1826.00 19.34 6 0 0 1822.17 32.39 0 6 0 1787.02 29.54 -1 -6 0 445.58 16.12 1 -6 0 486.88 20.43 -6 -1 0 466.04 19.37 6 -1 0 479.38 19.02 -6 1 0 486.78 11.77 6 1 0 464.22 19.58 -1 6 0 482.01 21.88 1 6 0 502.28 20.39 -2 -6 0 2669.02 34.91 2 -6 0 2725.11 42.07 -6 -2 0 2733.31 40.78 6 -2 0 2667.56 34.56 -6 2 0 2726.44 29.55 6 2 0 2776.17 36.12 -2 6 0 2821.34 30.37 2 6 0 2687.71 45.46 -3 -6 0 72.432 15.059 3 -6 0 66.558 13.976 -6 -3 0 39.211 17.332 6 -3 0 84.713 10.573 -6 3 0 66.809 7.471 6 3 0 77.289 12.961 -3 6 0 64.704 9.817 3 6 0 65.166 11.048 -4 -6 0 29.257 16.084 4 -6 0 25.793 10.610 -6 -4 0 35.408 12.316 6 -4 0 37.375 9.282 6 4 0 26.338 12.921 -4 6 0 29.153 10.770 4 6 0 32.665 10.758 -5 -6 0 1.739 15.745 5 -6 0 5.903 13.068 -6 -5 0 12.009 13.750 6 -5 0 10.439 11.511 -6 5 0 5.769 57.538 6 5 0 20.587 10.496 -5 6 0 12.467 9.051 5 6 0 -5.207 13.240 -6 -6 0 1633.88 36.24 6 -6 0 1568.03 29.34 -6 6 0 1632.76 32.21 6 6 0 1707.64 27.81 0 -7 0 9.766 13.410 -7 0 0 6.099 11.821 7 0 0 -7.579 13.879 0 7 0 0.609 13.707 -1 -7 0 27.930 13.468 1 -7 0 4.797 14.313 -7 -1 0 57.531 13.577 7 -1 0 23.821 14.671 -7 1 0 40.457 8.393 7 1 0 48.133 14.397 -1 7 0 45.304 13.416 1 7 0 27.823 15.568 -2 -7 0 58.949 13.953 2 -7 0 71.150 18.709 -7 -2 0 75.416 15.561 7 -2 0 68.513 16.006 -7 2 0 64.758 8.854 7 2 0 73.152 17.502 -2 7 0 61.874 13.058 2 7 0 49.097 17.461 -3 -7 0 1006.59 21.01 3 -7 0 940.93 30.08 -7 -3 0 982.43 36.84 7 -3 0 961.55 25.27 -7 3 0 968.88 17.70 7 3 0 976.94 28.26 -3 7 0 1028.09 19.60 3 7 0 931.84 25.46 -4 -7 0 97.549 17.438 4 -7 0 57.407 17.733 -7 -4 0 102.29 20.30 7 -4 0 61.403 14.566 -7 4 0 85.143 7.527 7 4 0 52.651 16.486 -4 7 0 89.481 11.122 4 7 0 72.443 16.823 -5 -7 0 422.63 28.38 5 -7 0 412.76 22.87 -7 -5 0 368.09 20.27 7 -5 0 355.23 19.40 -7 5 0 374.74 34.35 7 5 0 368.22 22.60 -5 7 0 355.70 17.51 5 7 0 370.78 19.83 -6 -7 0 -27.33 19.24 6 -7 0 47.657 18.297 -7 -6 0 13.168 16.530 7 -6 0 -2.781 19.000 -7 6 0 -21.73 31.09 7 6 0 31.816 10.919 -6 7 0 -5.909 9.721 6 7 0 30.811 14.305 -7 -7 0 618.72 31.27 7 -7 0 583.21 32.06 -7 7 0 623.78 37.15 7 7 0 644.46 24.11 0 -8 0 489.85 27.50 -8 0 0 470.61 22.95 8 0 0 503.96 27.14 0 8 0 529.95 26.41 -1 -8 0 15.039 15.227 1 -8 0 -14.32 15.74 -8 -1 0 3.203 15.862 8 -1 0 -1.646 15.477 -8 1 0 12.231 9.423 8 1 0 1.407 17.704 -1 8 0 6.040 15.536 1 8 0 4.013 17.901 -2 -8 0 156.42 22.22 2 -8 0 182.34 21.03 -8 -2 0 185.70 20.14 8 -2 0 179.54 21.89 -8 2 0 171.23 11.51 8 2 0 141.21 18.32 -2 8 0 141.51 17.18 2 8 0 164.57 18.95 -3 -8 0 422.21 27.47 3 -8 0 415.26 25.78 -8 -3 0 485.73 31.05 8 -3 0 440.78 29.25 -8 3 0 445.94 15.65 8 3 0 445.05 24.24 -3 8 0 423.23 16.98 3 8 0 367.90 21.88 -4 -8 0 16.346 12.661 4 -8 0 16.989 18.307 -8 -4 0 -28.95 22.51 8 -4 0 6.920 16.133 -8 4 0 13.602 10.249 8 4 0 28.174 19.670 -4 8 0 17.467 12.381 4 8 0 38.858 19.141 -5 -8 0 3.182 14.474 5 -8 0 40.903 28.188 -8 -5 0 21.918 28.883 8 -5 0 29.137 17.821 -8 5 0 -7.777 31.434 8 5 0 60.670 17.855 -5 8 0 17.205 12.250 5 8 0 4.053 19.418 -6 -8 0 25.284 23.553 6 -8 0 -19.45 23.22 -8 -6 0 14.276 32.585 8 -6 0 -18.10 18.57 -8 6 0 16.160 36.423 8 6 0 -25.08 24.59 -6 8 0 11.100 12.530 6 8 0 29.832 20.136 -7 -8 0 23.175 23.826 7 -8 0 -18.32 28.30 -8 -7 0 36.417 36.566 8 -7 0 70.395 26.060 -8 7 0 47.920 30.759 8 7 0 54.366 29.701 -7 8 0 43.590 27.386 7 8 0 39.078 32.025 -8 -8 0 716.49 57.79 8 -8 0 654.82 50.29 0 -9 0 -32.89 24.63 -9 0 0 34.951 17.580 9 0 0 37.196 20.885 0 9 0 67.002 19.436 -1 -9 0 619.60 28.40 1 -9 0 752.37 42.75 -9 -1 0 733.12 32.13 9 -1 0 658.26 32.37 -9 1 0 612.31 17.25 9 1 0 720.56 33.33 -1 9 0 688.85 29.62 1 9 0 558.84 28.96 -2 -9 0 -6.844 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35.67 -4 2 -18 -62.53 30.00 4 2 -18 75.308 36.972 -2 4 -18 21.159 34.538 2 4 -18 -5.598 28.227 -2 -4 18 58.323 33.854 2 -4 18 -7.270 34.573 -4 -2 18 1.130 37.938 4 -2 18 -91.57 33.04 -4 2 18 -117.78 43.87 4 2 18 65.414 49.404 -2 4 18 39.152 50.272 2 4 18 21.794 31.944 0 0 -19 -0.655 21.477 0 0 19 -4.493 32.199 0 -1 -19 51.731 25.427 -1 0 -19 22.726 23.705 1 0 -19 52.578 24.744 0 1 -19 49.842 28.232 0 -1 19 -85.72 40.66 -1 0 19 1.396 43.899 1 0 19 -8.589 38.795 0 1 19 -25.27 32.80 -1 -1 -19 23.523 22.333 1 -1 -19 32.443 33.134 -1 1 -19 29.999 24.406 1 1 -19 -5.048 21.286 -1 -1 19 -74.38 31.52 1 -1 19 37.139 40.660 -1 1 19 52.079 31.759 1 1 19 -41.67 42.65 0 -2 -19 27.133 32.043 -2 0 -19 59.864 24.821 2 0 -19 17.613 33.934 0 2 -19 2.235 22.630 0 -2 19 101.97 57.58 -2 0 19 -26.51 29.62 2 0 19 -35.58 36.85 0 2 19 46.331 34.574 -1 -2 -19 -9.989 30.179 1 -2 -19 -1.748 37.734 -2 -1 -19 -27.76 22.47 2 -1 -19 9.671 32.758 -2 1 -19 22.421 24.465 2 1 -19 34.906 31.727 -1 2 -19 22.055 23.667 1 2 -19 14.425 21.539 -1 -2 19 -48.05 40.21 1 -2 19 64.994 49.885 -2 -1 19 31.991 36.947 2 -1 19 59.089 45.322 -2 1 19 2.487 40.039 2 1 19 25.412 48.174 -1 2 19 34.638 34.426 1 2 19 137.40 35.00 -2 -2 -19 14.671 23.139 2 -2 -19 2.235 31.225 -2 2 -19 34.630 25.783 2 2 -19 -11.18 32.19 -2 -2 19 -25.24 33.91 2 -2 19 39.434 43.970 -2 2 19 -37.20 35.47 2 2 19 0.873 42.814 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 12416 ==================================================== Validation Reply Form _vrf_THETM01_fluorapophyllite-Cs ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: The crystal does not diffract very well; that is why we cut the data to 48degr 2theta. ; _vrf_PLAT430_fluorapophyllite-Cs ; PROBLEM: Short Inter D...A Contact O1 ..O2 . 2.57 Ang. RESPONSE: This is not a short distance as it has been known from literature. ; # end Validation Reply Form =======================================================