data_shelxl _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_mineral chabazite _chemical_compound_source 'Monte Somma, Vesuvius, Italy' _chemical_formula_sum 'Al0 K3 O24 Si12' _chemical_formula_weight 838.38 _publ_section_title 'Structural intergrowth of merlinoite/phillipsite and its temperature dehydration behavior' loop_ _publ_author_name 'Danisi, R.M.' 'Armbruster, T.' 'Nagashima, M.' _publ_contact_author_name 'Danisi, R.M.' _publ_contact_author_address 'University of Bern, Freiestr. 3, CH-3012 Bern' _publ_contact_author_email 'rosa.danisi@krist.unibe.ch' _publ_requested_journal 'Mineralogical Magazine' 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' 'Al' 'Al' 0.0645 0.0514 '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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 166 _space_group_name_H-M_alt 'R -3 m :H' _space_group_name_Hall '-R 3 2"' _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' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 13.4275(19) _cell_length_b 13.4275(19) _cell_length_c 15.510(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2421.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 523(2) _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.725 _exptl_crystal_F_000 1251 _exptl_absorpt_coefficient_mu 0.948 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 523(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'two circle diffractometer' _diffrn_measurement_device_type 'Apex II SMART' _diffrn_reflns_number 32393 _diffrn_reflns_av_unetI/netI 0.1211 _diffrn_reflns_av_R_equivalents 0.6641 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.189 _diffrn_reflns_theta_max 28.656 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 787 _reflns_number_gt 429 _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. Chabazite represents a very minor inclusion within a merlinoite-phillipsite intergrowth. The chemical composition of this chabazite is unknown. Some of the chabazite reflections were overlapping with those of merlinoite/phillipsite explaining the very poor internal R values. The poor data only allowed to resolve the framework sites and major channel occupants. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 787 _refine_ls_number_parameters 44 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2700 _refine_ls_R_factor_gt 0.1892 _refine_ls_wR_factor_ref 0.4209 _refine_ls_wR_factor_gt 0.3902 _refine_ls_goodness_of_fit_ref 2.243 _refine_ls_restrained_S_all 2.243 _refine_ls_shift/su_max 0.000 _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 K1 K 0.6667 0.3333 0.8333 0.037(5) Uiso 0.70(4) 12 d S . . . . K2 K 0.6667 0.3333 1.165(6) 0.092(13) Uiso 0.15(3) 6 d S U . . . K3 K 0.6667 -0.1667 0.8333 0.092(13) Uiso 0.32(3) 4 d S U . . . K4 K 0.765(7) -0.011(6) 0.933(5) 0.092(13) Uiso 0.069(12) 1 d . U . . . K5 K 0.6667 0.3333 0.982(8) 0.092(13) Uiso 0.12(3) 6 d S U . . . Si1 Si 0.6665(3) 0.1017(3) 0.9298(2) 0.0231(10) Uani 1 1 d . . . . . O1 O 0.6255(12) 0.0000 1.0000 0.049(4) Uani 1 2 d S T P . . O2 O 0.5771(6) 0.1542(12) 0.9237(10) 0.044(4) Uani 1 2 d S T P . . O3 O 0.7906(7) 0.2094(7) 0.9555(10) 0.045(4) Uani 1 2 d S T P . . O4 O 0.6667 0.0478(11) 0.8333 0.043(4) 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 Si1 0.0251(18) 0.0236(19) 0.0217(15) 0.0060(15) -0.0002(13) 0.0128(16) O1 0.059(7) 0.028(8) 0.048(9) 0.021(6) 0.010(3) 0.014(4) O2 0.029(5) 0.040(8) 0.067(11) 0.006(8) 0.003(4) 0.020(4) O3 0.033(5) 0.033(5) 0.053(10) 0.006(4) -0.006(4) 0.005(6) O4 0.059(10) 0.044(6) 0.031(7) 0.002(3) 0.003(7) 0.029(5) _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 K1 K5 2.31(12) . ? K1 K5 2.31(12) 31_656 ? K1 O2 2.511(14) 32_556 ? K1 O2 2.511(14) 2_655 ? K1 O2 2.511(14) 31_656 ? K1 O2 2.511(14) . ? K1 O2 2.511(14) 3_665 ? K1 O2 2.511(14) 33_546 ? K1 Si1 3.450(3) 16_546 ? K1 Si1 3.450(3) 31_656 ? K1 Si1 3.450(3) 22_665 ? K1 Si1 3.450(3) 2_655 ? K2 K5 2.84(15) . ? K2 K4 3.47(9) 29_655 ? K2 K4 3.47(9) 8_545 ? K2 K4 3.47(9) 9_665 ? K2 K4 3.47(9) 30_445 ? K2 K4 3.47(9) 28_565 ? K2 K4 3.47(9) 7_455 ? K2 K3 3.8762(9) 8_545 ? K2 K3 3.8763(8) 7_455 ? K2 K3 3.8763(8) 9_665 ? K2 K4 4.78(12) 25_657 ? K2 K4 4.78(12) 10_547 ? K3 K4 2.40(7) 18_656 ? K3 K4 2.40(8) . ? K3 K4 2.40(7) 24_545 ? K3 K4 2.40(8) 31_646 ? K3 O4 2.880(15) . ? K3 O4 2.880(15) 31_646 ? K3 O3 3.423(15) 21_547 ? K3 O3 3.423(15) 15_654 ? K3 K2 3.8762(11) 19_657 ? K3 K2 3.8763(12) 13_544 ? K3 Si1 3.903(3) 18_656 ? K3 Si1 3.903(3) 24_545 ? K4 K4 2.09(16) 5_557 ? K4 O1 2.20(8) . ? K4 O4 2.40(8) . ? K4 Si1 2.45(8) . ? K4 O3 2.82(7) . ? K4 K4 2.88(15) 24_545 ? K4 O3 3.10(8) 21_547 ? K4 Si1 3.15(9) 5_557 ? K4 K4 3.30(16) 22_665 ? K4 K2 3.47(9) 13_544 ? K4 K4 3.73(12) 20_667 ? K5 O2 2.27(5) 2_655 ? K5 O2 2.27(5) . ? K5 O2 2.27(5) 3_665 ? K5 O3 2.91(2) . ? K5 O3 2.91(2) 3_665 ? K5 O3 2.91(2) 2_655 ? K5 Si1 3.21(3) . ? K5 Si1 3.21(3) 22_665 ? K5 Si1 3.21(3) 23_655 ? K5 Si1 3.21(3) 2_655 ? Si1 O1 1.613(3) . ? Si1 O3 1.618(6) . ? Si1 O4 1.663(7) . ? Si1 O2 1.671(6) . ? Si1 K4 3.15(9) 5_557 ? Si1 K4 3.90(8) 18_656 ? O1 Si1 1.613(3) 5_557 ? O1 K4 2.20(9) 5_557 ? O2 Si1 1.671(6) 23_655 ? O3 Si1 1.618(6) 22_665 ? O3 K4 2.82(7) 22_665 ? O3 K4 3.10(8) 20_667 ? O3 K4 3.10(8) 5_557 ? O3 K3 3.423(15) 8_545 ? O4 Si1 1.663(7) 18_656 ? O4 K4 2.40(8) 18_656 ? 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 K5 K1 K5 180.0 . 31_656 ? K5 K1 O2 123.9(4) . 32_556 ? K5 K1 O2 56.1(4) 31_656 32_556 ? K5 K1 O2 56.1(4) . 2_655 ? K5 K1 O2 123.9(4) 31_656 2_655 ? O2 K1 O2 180.0 32_556 2_655 ? K5 K1 O2 123.9(4) . 31_656 ? K5 K1 O2 56.1(4) 31_656 31_656 ? O2 K1 O2 91.9(5) 32_556 31_656 ? O2 K1 O2 88.1(5) 2_655 31_656 ? K5 K1 O2 56.1(4) . . ? K5 K1 O2 123.9(4) 31_656 . ? O2 K1 O2 88.1(5) 32_556 . ? O2 K1 O2 91.9(5) 2_655 . ? O2 K1 O2 180.0 31_656 . ? K5 K1 O2 56.1(4) . 3_665 ? K5 K1 O2 123.9(4) 31_656 3_665 ? O2 K1 O2 88.1(5) 32_556 3_665 ? O2 K1 O2 91.9(5) 2_655 3_665 ? O2 K1 O2 88.1(5) 31_656 3_665 ? O2 K1 O2 91.9(5) . 3_665 ? K5 K1 O2 123.9(4) . 33_546 ? K5 K1 O2 56.1(4) 31_656 33_546 ? O2 K1 O2 91.9(5) 32_556 33_546 ? O2 K1 O2 88.1(5) 2_655 33_546 ? O2 K1 O2 91.9(5) 31_656 33_546 ? O2 K1 O2 88.1(5) . 33_546 ? O2 K1 O2 180.0(6) 3_665 33_546 ? K5 K1 Si1 115.71(6) . 16_546 ? K5 K1 Si1 64.30(6) 31_656 16_546 ? O2 K1 Si1 27.15(8) 32_556 16_546 ? O2 K1 Si1 152.85(8) 2_655 16_546 ? O2 K1 Si1 76.02(15) 31_656 16_546 ? O2 K1 Si1 103.98(15) . 16_546 ? O2 K1 Si1 66.1(3) 3_665 16_546 ? O2 K1 Si1 113.9(3) 33_546 16_546 ? K5 K1 Si1 115.71(6) . 31_656 ? K5 K1 Si1 64.30(5) 31_656 31_656 ? O2 K1 Si1 76.02(15) 32_556 31_656 ? O2 K1 Si1 103.98(15) 2_655 31_656 ? O2 K1 Si1 27.15(8) 31_656 31_656 ? O2 K1 Si1 152.85(8) . 31_656 ? O2 K1 Si1 66.1(3) 3_665 31_656 ? O2 K1 Si1 113.9(3) 33_546 31_656 ? Si1 K1 Si1 53.62(12) 16_546 31_656 ? K5 K1 Si1 64.30(6) . 22_665 ? K5 K1 Si1 115.70(6) 31_656 22_665 ? O2 K1 Si1 152.85(8) 32_556 22_665 ? O2 K1 Si1 27.15(8) 2_655 22_665 ? O2 K1 Si1 103.98(15) 31_656 22_665 ? O2 K1 Si1 76.02(15) . 22_665 ? O2 K1 Si1 113.9(3) 3_665 22_665 ? O2 K1 Si1 66.1(3) 33_546 22_665 ? Si1 K1 Si1 180.0 16_546 22_665 ? Si1 K1 Si1 126.38(12) 31_656 22_665 ? K5 K1 Si1 64.30(6) . 2_655 ? K5 K1 Si1 115.70(6) 31_656 2_655 ? O2 K1 Si1 152.85(8) 32_556 2_655 ? O2 K1 Si1 27.15(8) 2_655 2_655 ? O2 K1 Si1 66.1(3) 31_656 2_655 ? O2 K1 Si1 113.9(3) . 2_655 ? O2 K1 Si1 76.02(15) 3_665 2_655 ? O2 K1 Si1 103.98(15) 33_546 2_655 ? Si1 K1 Si1 126.52(12) 16_546 2_655 ? Si1 K1 Si1 77.42(7) 31_656 2_655 ? Si1 K1 Si1 53.48(12) 22_665 2_655 ? K5 K2 K4 116.9(19) . 29_655 ? K5 K2 K4 116.9(19) . 8_545 ? K4 K2 K4 49(3) 29_655 8_545 ? K5 K2 K4 116.9(19) . 9_665 ? K4 K2 K4 57(2) 29_655 9_665 ? K4 K2 K4 101(2) 8_545 9_665 ? K5 K2 K4 116.9(19) . 30_445 ? K4 K2 K4 101(2) 29_655 30_445 ? K4 K2 K4 57(2) 8_545 30_445 ? K4 K2 K4 126(4) 9_665 30_445 ? K5 K2 K4 116.9(19) . 28_565 ? K4 K2 K4 101(2) 29_655 28_565 ? K4 K2 K4 126(4) 8_545 28_565 ? K4 K2 K4 49(3) 9_665 28_565 ? K4 K2 K4 101(2) 30_445 28_565 ? K5 K2 K4 116.9(19) . 7_455 ? K4 K2 K4 126(4) 29_655 7_455 ? K4 K2 K4 101(2) 8_545 7_455 ? K4 K2 K4 101(2) 9_665 7_455 ? K4 K2 K4 49(3) 30_445 7_455 ? K4 K2 K4 57(2) 28_565 7_455 ? K5 K2 K3 90.4(14) . 8_545 ? K4 K2 K3 37.6(13) 29_655 8_545 ? K4 K2 K3 37.6(13) 8_545 8_545 ? K4 K2 K3 91.9(14) 9_665 8_545 ? K4 K2 K3 91.9(13) 30_445 8_545 ? K4 K2 K3 139(2) 28_565 8_545 ? K4 K2 K3 139(2) 7_455 8_545 ? K5 K2 K3 90.4(14) . 7_455 ? K4 K2 K3 139(2) 29_655 7_455 ? K4 K2 K3 91.9(14) 8_545 7_455 ? K4 K2 K3 139(2) 9_665 7_455 ? K4 K2 K3 37.6(13) 30_445 7_455 ? K4 K2 K3 91.9(14) 28_565 7_455 ? K4 K2 K3 37.6(13) 7_455 7_455 ? K3 K2 K3 120.00(3) 8_545 7_455 ? K5 K2 K3 90.4(14) . 9_665 ? K4 K2 K3 91.9(14) 29_655 9_665 ? K4 K2 K3 139(2) 8_545 9_665 ? K4 K2 K3 37.6(13) 9_665 9_665 ? K4 K2 K3 139(2) 30_445 9_665 ? K4 K2 K3 37.6(13) 28_565 9_665 ? K4 K2 K3 91.9(14) 7_455 9_665 ? K3 K2 K3 120.00(3) 8_545 9_665 ? K3 K2 K3 119.99(3) 7_455 9_665 ? K5 K2 K4 139.7(13) . 25_657 ? K4 K2 K4 23.1(19) 29_655 25_657 ? K4 K2 K4 50.7(13) 8_545 25_657 ? K4 K2 K4 50.7(13) 9_665 25_657 ? K4 K2 K4 89(2) 30_445 25_657 ? K4 K2 K4 84(2) 28_565 25_657 ? K4 K2 K4 103(3) 7_455 25_657 ? K3 K2 K4 56.5(11) 8_545 25_657 ? K3 K2 K4 125(2) 7_455 25_657 ? K3 K2 K4 88.2(14) 9_665 25_657 ? K5 K2 K4 139.7(13) . 10_547 ? K4 K2 K4 50.7(13) 29_655 10_547 ? K4 K2 K4 23.1(19) 8_545 10_547 ? K4 K2 K4 89(2) 9_665 10_547 ? K4 K2 K4 50.7(13) 30_445 10_547 ? K4 K2 K4 103(3) 28_565 10_547 ? K4 K2 K4 84(2) 7_455 10_547 ? K3 K2 K4 56.5(11) 8_545 10_547 ? K3 K2 K4 88.2(14) 7_455 10_547 ? K3 K2 K4 125(2) 9_665 10_547 ? K4 K2 K4 40(2) 25_657 10_547 ? K4 K3 K4 106(4) 18_656 . ? K4 K3 K4 179.998(18) 18_656 24_545 ? K4 K3 K4 74(4) . 24_545 ? K4 K3 K4 74(4) 18_656 31_646 ? K4 K3 K4 180.0 . 31_646 ? K4 K3 K4 106(4) 24_545 31_646 ? K4 K3 O4 53.1(19) 18_656 . ? K4 K3 O4 53.1(19) . . ? K4 K3 O4 126.9(19) 24_545 . ? K4 K3 O4 126.9(19) 31_646 . ? K4 K3 O4 126.9(19) 18_656 31_646 ? K4 K3 O4 126.9(19) . 31_646 ? K4 K3 O4 53.1(19) 24_545 31_646 ? K4 K3 O4 53.1(19) 31_646 31_646 ? O4 K3 O4 180.0 . 31_646 ? K4 K3 O3 119(2) 18_656 21_547 ? K4 K3 O3 61(2) . 21_547 ? K4 K3 O3 61(2) 24_545 21_547 ? K4 K3 O3 119(2) 31_646 21_547 ? O4 K3 O3 90.000(1) . 21_547 ? O4 K3 O3 90.002(2) 31_646 21_547 ? K4 K3 O3 61(2) 18_656 15_654 ? K4 K3 O3 119(2) . 15_654 ? K4 K3 O3 119(2) 24_545 15_654 ? K4 K3 O3 61(2) 31_646 15_654 ? O4 K3 O3 90.001(1) . 15_654 ? O4 K3 O3 90.0 31_646 15_654 ? O3 K3 O3 180.0 21_547 15_654 ? K4 K3 K2 62(2) 18_656 19_657 ? K4 K3 K2 118(2) . 19_657 ? K4 K3 K2 118(2) 24_545 19_657 ? K4 K3 K2 62(2) 31_646 19_657 ? O4 K3 K2 90.001(5) . 19_657 ? O4 K3 K2 90.000(12) 31_646 19_657 ? O3 K3 K2 72.8(14) 21_547 19_657 ? O3 K3 K2 107.2(14) 15_654 19_657 ? K4 K3 K2 118(2) 18_656 13_544 ? K4 K3 K2 62(2) . 13_544 ? K4 K3 K2 62(2) 24_545 13_544 ? K4 K3 K2 118(2) 31_646 13_544 ? O4 K3 K2 90.000(12) . 13_544 ? O4 K3 K2 89.999(6) 31_646 13_544 ? O3 K3 K2 107.2(14) 21_547 13_544 ? O3 K3 K2 72.8(14) 15_654 13_544 ? K2 K3 K2 180.0 19_657 13_544 ? K4 K3 Si1 37(2) 18_656 18_656 ? K4 K3 Si1 72.1(19) . 18_656 ? K4 K3 Si1 143(2) 24_545 18_656 ? K4 K3 Si1 107.9(19) 31_646 18_656 ? O4 K3 Si1 22.54(4) . 18_656 ? O4 K3 Si1 157.45(4) 31_646 18_656 ? O3 K3 Si1 111.53(6) 21_547 18_656 ? O3 K3 Si1 68.47(6) 15_654 18_656 ? K2 K3 Si1 90.2(5) 19_657 18_656 ? K2 K3 Si1 89.8(5) 13_544 18_656 ? K4 K3 Si1 143(2) 18_656 24_545 ? K4 K3 Si1 107.9(19) . 24_545 ? K4 K3 Si1 37(2) 24_545 24_545 ? K4 K3 Si1 72.1(19) 31_646 24_545 ? O4 K3 Si1 157.46(4) . 24_545 ? O4 K3 Si1 22.54(4) 31_646 24_545 ? O3 K3 Si1 68.47(6) 21_547 24_545 ? O3 K3 Si1 111.53(6) 15_654 24_545 ? K2 K3 Si1 89.8(5) 19_657 24_545 ? K2 K3 Si1 90.2(5) 13_544 24_545 ? Si1 K3 Si1 180.0 18_656 24_545 ? K4 K4 O1 62(2) 5_557 . ? K4 K4 K3 137(6) 5_557 . ? O1 K4 K3 104(3) . . ? K4 K4 O4 127(3) 5_557 . ? O1 K4 O4 70(2) . . ? K3 K4 O4 74(2) . . ? K4 K4 Si1 88(3) 5_557 . ? O1 K4 Si1 40.1(14) . . ? K3 K4 Si1 107(3) . . ? O4 K4 Si1 40.1(13) . . ? K4 K4 O3 77(4) 5_557 . ? O1 K4 O3 62.5(19) . . ? K3 K4 O3 136(3) . . ? O4 K4 O3 62.5(18) . . ? Si1 K4 O3 34.9(10) . . ? K4 K4 K4 96(4) 5_557 24_545 ? O1 K4 K4 119(2) . 24_545 ? K3 K4 K4 53.1(19) . 24_545 ? O4 K4 K4 126.9(18) . 24_545 ? Si1 K4 K4 152.2(18) . 24_545 ? O3 K4 K4 170.5(17) . 24_545 ? K4 K4 O3 62(4) 5_557 21_547 ? O1 K4 O3 57.2(19) . 21_547 ? K3 K4 O3 76(2) . 21_547 ? O4 K4 O3 108(3) . 21_547 ? Si1 K4 O3 96(3) . 21_547 ? O3 K4 O3 118(3) . 21_547 ? K4 K4 O3 62.3(15) 24_545 21_547 ? K4 K4 Si1 51(2) 5_557 5_557 ? O1 K4 Si1 28.6(11) . 5_557 ? K3 K4 Si1 96(3) . 5_557 ? O4 K4 Si1 94(3) . 5_557 ? Si1 K4 Si1 69(2) . 5_557 ? O3 K4 Si1 88(2) . 5_557 ? K4 K4 Si1 92.1(13) 24_545 5_557 ? O3 K4 Si1 30.0(8) 21_547 5_557 ? K4 K4 K4 84(4) 5_557 22_665 ? O1 K4 K4 113.1(19) . 22_665 ? K3 K4 K4 135(2) . 22_665 ? O4 K4 K4 96.3(19) . 22_665 ? Si1 K4 K4 87.8(18) . 22_665 ? O3 K4 K4 54.1(18) . 22_665 ? K4 K4 K4 120.00(4) 24_545 22_665 ? O3 K4 K4 145.9(15) 21_547 22_665 ? Si1 K4 K4 128.3(13) 5_557 22_665 ? K4 K4 K2 116.4(19) 5_557 13_544 ? O1 K4 K2 175(3) . 13_544 ? K3 K4 K2 80(2) . 13_544 ? O4 K4 K2 109(3) . 13_544 ? Si1 K4 K2 137(3) . 13_544 ? O3 K4 K2 112(2) . 13_544 ? K4 K4 K2 65.5(13) 24_545 13_544 ? O3 K4 K2 127(2) 21_547 13_544 ? Si1 K4 K2 154(3) 5_557 13_544 ? K4 K4 K2 61.6(12) 22_665 13_544 ? K4 K4 K4 50(4) 5_557 20_667 ? O1 K4 K4 92(3) . 20_667 ? K3 K4 K4 163(3) . 20_667 ? O4 K4 K4 115(3) . 20_667 ? Si1 K4 K4 87(3) . 20_667 ? O3 K4 K4 54(2) . 20_667 ? K4 K4 K4 116.3(14) 24_545 20_667 ? O3 K4 K4 112(3) 21_547 20_667 ? Si1 K4 K4 97(3) 5_557 20_667 ? K4 K4 K4 34(2) 22_665 20_667 ? K2 K4 K4 83.3(15) 13_544 20_667 ? O2 K5 O2 105(3) 2_655 . ? O2 K5 O2 105(3) 2_655 3_665 ? O2 K5 O2 105(3) . 3_665 ? O2 K5 K1 67(3) 2_655 . ? O2 K5 K1 67(3) . . ? O2 K5 K1 67(3) 3_665 . ? O2 K5 K2 113(3) 2_655 . ? O2 K5 K2 113(3) . . ? O2 K5 K2 113(3) 3_665 . ? K1 K5 K2 180.00(3) . . ? O2 K5 O3 59.3(7) 2_655 . ? O2 K5 O3 59.3(7) . . ? O2 K5 O3 148(5) 3_665 . ? K1 K5 O3 82(2) . . ? K2 K5 O3 98(2) . . ? O2 K5 O3 148(5) 2_655 3_665 ? O2 K5 O3 59.3(7) . 3_665 ? O2 K5 O3 59.3(7) 3_665 3_665 ? K1 K5 O3 82(2) . 3_665 ? K2 K5 O3 98(2) . 3_665 ? O3 K5 O3 118.0(11) . 3_665 ? O2 K5 O3 59.3(7) 2_655 2_655 ? O2 K5 O3 148(5) . 2_655 ? O2 K5 O3 59.3(7) 3_665 2_655 ? K1 K5 O3 82(2) . 2_655 ? K2 K5 O3 98(2) . 2_655 ? O3 K5 O3 118.0(11) . 2_655 ? O3 K5 O3 118.0(11) 3_665 2_655 ? O2 K5 Si1 84.3(14) 2_655 . ? O2 K5 Si1 29.6(2) . . ? O2 K5 Si1 132(4) 3_665 . ? K1 K5 Si1 75(2) . . ? K2 K5 Si1 105(2) . . ? O3 K5 Si1 30.1(3) . . ? O3 K5 Si1 87.9(9) 3_665 . ? O3 K5 Si1 143(3) 2_655 . ? O2 K5 Si1 29.6(2) 2_655 22_665 ? O2 K5 Si1 84.3(14) . 22_665 ? O2 K5 Si1 132(4) 3_665 22_665 ? K1 K5 Si1 75(2) . 22_665 ? K2 K5 Si1 105(2) . 22_665 ? O3 K5 Si1 30.1(3) . 22_665 ? O3 K5 Si1 143(3) 3_665 22_665 ? O3 K5 Si1 87.9(9) 2_655 22_665 ? Si1 K5 Si1 58.0(6) . 22_665 ? O2 K5 Si1 132(4) 2_655 23_655 ? O2 K5 Si1 29.6(2) . 23_655 ? O2 K5 Si1 84.3(14) 3_665 23_655 ? K1 K5 Si1 75(2) . 23_655 ? K2 K5 Si1 105(2) . 23_655 ? O3 K5 Si1 87.9(9) . 23_655 ? O3 K5 Si1 30.1(3) 3_665 23_655 ? O3 K5 Si1 143(3) 2_655 23_655 ? Si1 K5 Si1 57.8(6) . 23_655 ? Si1 K5 Si1 113.9(16) 22_665 23_655 ? O2 K5 Si1 29.6(2) 2_655 2_655 ? O2 K5 Si1 132(4) . 2_655 ? O2 K5 Si1 84.3(14) 3_665 2_655 ? K1 K5 Si1 75(2) . 2_655 ? K2 K5 Si1 105(2) . 2_655 ? O3 K5 Si1 87.9(9) . 2_655 ? O3 K5 Si1 143(3) 3_665 2_655 ? O3 K5 Si1 30.1(3) 2_655 2_655 ? Si1 K5 Si1 113.9(16) . 2_655 ? Si1 K5 Si1 57.8(6) 22_665 2_655 ? Si1 K5 Si1 151(4) 23_655 2_655 ? O1 Si1 O3 110.7(7) . . ? O1 Si1 O4 108.2(5) . . ? O3 Si1 O4 112.7(6) . . ? O1 Si1 O2 112.5(7) . . ? O3 Si1 O2 105.9(7) . . ? O4 Si1 O2 106.9(6) . . ? O1 Si1 K4 62(2) . . ? O3 Si1 K4 85.1(19) . . ? O4 Si1 K4 68.4(19) . . ? O2 Si1 K4 169.0(19) . . ? O1 Si1 K4 40.9(15) . 5_557 ? O3 Si1 K4 73.2(15) . 5_557 ? O4 Si1 K4 109.7(15) . 5_557 ? O2 Si1 K4 140.5(16) . 5_557 ? K4 Si1 K4 42(3) . 5_557 ? O1 Si1 K5 119.0(19) . . ? O3 Si1 K5 64.6(7) . . ? O4 Si1 K5 130(2) . . ? O2 Si1 K5 42.2(9) . . ? K4 Si1 K5 148(2) . . ? K4 Si1 K5 115(2) 5_557 . ? O1 Si1 K1 154.5(5) . . ? O3 Si1 K1 76.4(5) . . ? O4 Si1 K1 90.1(5) . . ? O2 Si1 K1 43.3(5) . . ? K4 Si1 K1 144(2) . . ? K4 Si1 K1 148.3(13) 5_557 . ? K5 Si1 K1 40(2) . . ? O1 Si1 K4 93.7(12) . 18_656 ? O3 Si1 K4 131.4(14) . 18_656 ? O4 Si1 K4 19.5(13) . 18_656 ? O2 Si1 K4 102.0(12) . 18_656 ? K4 Si1 K4 70(3) . 18_656 ? K4 Si1 K4 107.4(6) 5_557 18_656 ? K5 Si1 K4 137(2) . 18_656 ? K1 Si1 K4 99.3(11) . 18_656 ? O1 Si1 K3 68.5(3) . . ? O3 Si1 K3 116.3(6) . . ? O4 Si1 K3 41.6(5) . . ? O2 Si1 K3 134.4(5) . . ? K4 Si1 K3 35.9(18) . . ? K4 Si1 K3 71.7(14) 5_557 . ? K5 Si1 K3 172(2) . . ? K1 Si1 K3 131.75(9) . . ? K4 Si1 K3 35.8(11) 18_656 . ? Si1 O1 Si1 170.5(11) . 5_557 ? Si1 O1 K4 78(2) . . ? Si1 O1 K4 111(2) 5_557 . ? Si1 O1 K4 111(2) . 5_557 ? Si1 O1 K4 78(2) 5_557 5_557 ? K4 O1 K4 57(4) . 5_557 ? Si1 O2 Si1 136.6(9) 23_655 . ? Si1 O2 K5 108.2(8) 23_655 . ? Si1 O2 K5 108.2(8) . . ? Si1 O2 K1 109.5(5) 23_655 . ? Si1 O2 K1 109.5(5) . . ? K5 O2 K1 57(3) . . ? Si1 O3 Si1 148.3(11) . 22_665 ? Si1 O3 K4 60.0(18) . . ? Si1 O3 K4 129(2) 22_665 . ? Si1 O3 K4 129(2) . 22_665 ? Si1 O3 K4 60.0(18) 22_665 22_665 ? K4 O3 K4 72(4) . 22_665 ? Si1 O3 K5 85.3(8) . . ? Si1 O3 K5 85.3(8) 22_665 . ? K4 O3 K5 144.1(18) . . ? K4 O3 K5 144.1(18) 22_665 . ? Si1 O3 K4 131.7(16) . 20_667 ? Si1 O3 K4 76.8(15) 22_665 20_667 ? K4 O3 K4 78(3) . 20_667 ? K4 O3 K4 41(3) 22_665 20_667 ? K5 O3 K4 127(3) . 20_667 ? Si1 O3 K4 76.8(15) . 5_557 ? Si1 O3 K4 131.7(16) 22_665 5_557 ? K4 O3 K4 41(3) . 5_557 ? K4 O3 K4 78(3) 22_665 5_557 ? K5 O3 K4 127(3) . 5_557 ? K4 O3 K4 55(3) 20_667 5_557 ? Si1 O3 K3 105.7(5) . 8_545 ? Si1 O3 K3 105.7(5) 22_665 8_545 ? K4 O3 K3 83.5(17) . 8_545 ? K4 O3 K3 83.5(17) 22_665 8_545 ? K5 O3 K3 99(2) . 8_545 ? K4 O3 K3 42.8(14) 20_667 8_545 ? K4 O3 K3 42.8(14) 5_557 8_545 ? Si1 O4 Si1 128.3(9) 18_656 . ? Si1 O4 K4 147(2) 18_656 . ? Si1 O4 K4 71.5(19) . . ? Si1 O4 K4 71.5(19) 18_656 18_656 ? Si1 O4 K4 147(2) . 18_656 ? K4 O4 K4 106(4) . 18_656 ? Si1 O4 K3 115.9(5) 18_656 . ? Si1 O4 K3 115.9(5) . . ? K4 O4 K3 53.1(18) . . ? K4 O4 K3 53.1(18) 18_656 . ? _refine_diff_density_max 2.729 _refine_diff_density_min -1.639 _refine_diff_density_rms 0.325 _shelxl_version_number 2012-9 _shelx_res_file ; TITL Chaba250 in R-3m CELL 0.71073 13.4275 13.4275 15.5098 90.000 90.000 120.000 ZERR 3.00 0.0019 0.0019 0.0031 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM Y, X, -Z SYMM X-Y, -Y, -Z SYMM -X, -X+Y, -Z SFAC O AL SI K UNIT 72 0 36 9 TEMP 23.000 L.S. 10 ACTA BOND FMAP 2 PLAN 20 WGHT 0.100000 FVAR 0.13399 0.09184 K1 4 0.666667 0.333333 0.833333 0.05801 0.03707 K2 4 0.666667 0.333333 1.165071 0.02453 21.00000 K3 4 0.666667 -0.166667 0.833333 0.08059 21.00000 K4 4 0.764556 -0.010564 0.932936 0.06891 21.00000 K5 4 0.666667 0.333333 0.981979 0.02068 21.00000 SI1 3 0.666482 0.101723 0.929820 11.00000 0.02508 0.02356 = 0.02166 0.00605 -0.00016 0.01280 O1 1 0.625545 0.000000 1.000000 10.50000 0.05886 0.02835 = 0.04842 0.02069 0.01034 0.01417 O2 1 0.577090 0.154180 0.923717 10.50000 0.02918 0.03969 = 0.06740 0.00580 0.00290 0.01985 O3 1 0.790619 0.209381 0.955501 10.50000 0.03318 0.03318 = 0.05315 0.00604 -0.00604 0.00534 O4 1 0.666667 0.047808 0.833333 10.50000 0.05896 0.04365 = 0.03115 0.00175 0.00349 0.02948 HKLF 4 REM Chaba250 in R-3m REM R1 = 0.1892 for 429 Fo > 4sig(Fo) and 0.2700 for all 787 data REM 44 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 2.729, deepest hole -1.639, 1-sigma level 0.325 Q1 1 0.5632 -0.0983 0.9324 11.00000 0.05 2.73 Q2 1 0.6535 -0.1732 0.7942 10.50000 0.05 1.41 Q3 1 0.4786 -0.0427 0.8959 10.50000 0.05 1.35 Q4 1 0.7983 0.2017 1.0368 10.50000 0.05 1.15 Q5 1 0.7060 0.0422 1.0010 11.00000 0.05 1.12 Q6 1 0.7933 0.2067 0.8797 10.50000 0.05 0.98 Q7 1 0.7079 0.4158 1.0432 10.50000 0.05 0.97 Q8 1 0.7521 -0.0886 0.8987 11.00000 0.05 0.96 Q9 1 0.7169 0.0023 0.8388 11.00000 0.05 0.96 Q10 1 0.8575 0.1425 0.9541 10.50000 0.05 0.93 Q11 1 0.6667 0.3333 0.9318 10.16667 0.05 0.86 Q12 1 0.9039 0.0961 0.9383 10.50000 0.05 0.86 Q13 1 0.7983 -0.1009 0.9710 10.50000 0.05 0.78 Q14 1 0.6667 0.3333 1.3333 10.08333 0.05 0.76 Q15 1 0.6667 0.1066 0.8333 10.50000 0.05 0.69 Q16 1 0.7671 -0.0553 0.8374 11.00000 0.05 0.68 Q17 1 0.7199 0.4397 1.1230 10.50000 0.05 0.66 Q18 1 0.5866 0.1733 1.0001 10.50000 0.05 0.65 Q19 1 0.9097 0.0903 0.9892 10.50000 0.05 0.64 Q20 1 0.5881 0.1761 0.8230 10.50000 0.05 0.63 ; _shelx_res_checksum 57183 _shelx_hkl_file ; 0 0 -3 655.96 22.69 0 0 -3 702.79 17.75 0 0 -3 443.69 21.66 0 0 -3 299.98 18.25 0 0 -3 373.99 20.32 0 0 3 626.49 23.17 0 0 3 593.29 16.02 0 0 3 239.56 17.00 0 0 3 670.91 23.13 0 0 3 288.79 17.82 0 0 3 353.96 20.41 0 0 -6 505.04 21.63 0 0 -6 398.61 29.82 0 0 -6 593.40 29.26 0 0 -6 238.33 25.28 0 0 -6 319.75 28.04 0 0 6 537.36 31.79 0 0 6 396.86 19.40 0 0 6 394.70 29.72 0 0 6 217.62 24.53 0 0 6 562.54 31.66 0 0 6 237.57 24.75 0 0 6 260.31 25.88 0 0 -9 1891.00 46.10 0 0 -9 2214.70 82.60 0 0 -9 1842.20 73.10 0 0 -9 2540.50 69.30 0 0 -9 1128.30 58.60 0 0 -9 1429.10 65.80 0 0 9 2203.60 75.60 0 0 9 1371.70 39.80 0 0 9 2744.40 79.00 0 0 9 1488.60 66.40 0 0 9 2202.40 63.10 0 0 9 1036.90 56.50 0 0 9 2533.50 78.70 0 0 9 985.90 55.83 0 0 9 1327.90 64.90 0 0 -12 975.83 70.97 0 0 -12 758.56 64.46 0 0 -12 958.33 69.52 0 0 -12 771.61 62.42 0 0 12 865.92 62.48 0 0 12 1022.00 69.70 0 0 12 1047.60 63.80 0 0 12 640.22 60.68 0 0 12 997.76 57.47 0 0 12 933.41 63.45 0 0 12 492.18 55.78 0 0 -15 531.91 63.22 0 0 -15 479.13 60.09 0 0 -15 226.70 46.31 0 0 -15 488.64 62.18 0 0 -15 453.43 58.68 0 0 15 505.65 57.45 0 0 15 543.52 61.35 0 0 15 625.17 58.75 0 0 15 316.26 54.72 0 0 15 544.93 51.54 0 0 15 555.36 56.62 0 0 15 300.87 53.52 0 0 -18 13.72 39.26 0 0 -18 -1.32 35.37 0 0 -18 20.65 47.91 0 0 -18 -10.51 39.34 0 0 -18 -16.35 40.99 0 0 -18 21.86 43.19 0 0 18 17.00 38.90 0 0 18 15.15 42.10 0 0 18 45.98 46.22 0 0 18 4.99 31.62 0 0 18 38.17 36.43 -1 0 20 11.69 49.84 -1 0 20 29.77 40.14 -1 0 20 7.21 43.50 -1 1 -20 -12.49 43.64 -1 1 -20 -42.33 52.80 -1 1 -20 -23.11 49.34 -1 1 -20 66.62 54.11 0 -1 -20 32.11 48.01 0 -1 -20 -11.40 37.57 0 -1 -20 -37.38 50.44 0 -1 -20 -42.46 44.42 0 -1 -20 -8.28 47.82 0 -1 -20 19.74 44.46 0 1 20 13.54 45.57 0 1 20 23.48 49.45 0 1 20 -0.60 47.41 0 1 20 45.92 42.39 0 1 20 13.24 41.61 1 -1 20 59.99 54.15 1 -1 20 39.41 39.54 1 0 -20 31.79 47.56 1 0 -20 15.89 41.05 1 0 -20 36.89 57.06 1 0 -20 4.99 48.61 -1 0 17 41.50 37.31 -1 0 17 10.45 40.95 -1 0 17 12.62 41.63 -1 0 17 -3.74 29.86 -1 0 17 27.24 35.25 -1 1 -17 -10.70 33.94 -1 1 -17 -5.23 31.41 -1 1 -17 -18.12 40.68 -1 1 -17 14.88 44.94 -1 1 -17 6.36 38.95 0 -1 -17 41.70 39.99 0 -1 -17 123.17 54.15 0 -1 -17 123.76 50.05 0 -1 -17 51.75 45.24 0 -1 -17 48.41 41.27 0 1 17 76.55 41.89 0 1 17 55.86 43.28 0 1 17 59.47 44.75 0 1 17 75.13 35.90 0 1 17 31.19 36.70 1 -1 17 10.84 35.48 1 -1 17 43.42 40.36 1 -1 17 -4.95 39.19 1 -1 17 -11.48 28.30 1 -1 17 27.44 34.72 1 0 -17 1.02 31.62 1 0 -17 4.41 31.70 1 0 -17 19.83 45.41 1 0 -17 6.05 37.28 1 0 -17 -26.18 41.84 1 0 -17 27.97 38.17 -1 0 14 -7.07 30.91 -1 0 14 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