data_Hogarthite _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ca Na2 O34 Si10 Ti2' _chemical_formula_weight 1006.76 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' 'Na' 'Na' 0.0362 0.0249 '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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_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 10.1839(5) _cell_length_b 15.8244(6) _cell_length_c 9.1327(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.463(2) _cell_angle_gamma 90.00 _cell_volume 1425.13(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.326 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6739 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2144 _reflns_number_gt 1335 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2144 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.091 _refine_ls_shift/su_mean 0.005 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.5000 0.39364(19) 0.0000 0.0219(6) Uani 0.50 2 d SP . . Na Na 0.0954(4) 0.5000 -0.1168(6) 0.0834(16) Uani 1 2 d S . . Ti1 Ti 0.2500 0.2500 0.0000 0.0097(2) Uani 1 2 d S . . Si1 Si -0.04961(10) 0.29075(7) -0.22198(13) 0.0110(2) Uani 1 1 d . . . Si2 Si 0.28484(10) 0.40010(7) 0.24989(13) 0.0101(2) Uani 1 1 d . . . Si3 Si 0.5000 0.30722(10) 0.5000 0.0121(3) Uani 1 2 d S . . O1 O -0.1292(3) 0.38175(17) -0.2551(3) 0.0150(6) Uani 1 1 d . . . O2 O 0.3800(3) 0.3662(2) 0.4067(3) 0.0239(7) Uani 1 1 d . . . O3 O -0.0593(3) 0.2506(2) -0.3878(3) 0.0210(7) Uani 1 1 d . . . O4 O 0.3055(4) 0.5000 0.2415(5) 0.0194(9) Uani 1 2 d S . . O5 O -0.1316(3) 0.23038(17) -0.1346(3) 0.0148(6) Uani 1 1 d . . . O6 O 0.1043(2) 0.31173(18) -0.1352(3) 0.0174(6) Uani 1 1 d . . . O7 O 0.3188(3) 0.35555(18) 0.1057(3) 0.0157(6) Uani 1 1 d . . . OW8 O 0.2655(10) 0.4163(6) -0.1594(12) 0.010(2) Uani 0.25 1 d P . . OW9 O 0.3515(12) 0.4401(8) -0.2398(13) 0.101(4) Uani 0.50 1 d P . . OW10 O 0.5000 0.4516(8) 0.0000 0.049(3) Uani 0.50 2 d SP . . OW11 O 0.1950(13) 0.4058(6) -0.3754(12) 0.168(6) Uani 0.75 1 d P . . OW12 O 0.000(3) 0.5000 -0.394(6) 0.30(3) Uani 0.50 2 d SP . . 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 Ca 0.0213(13) 0.0206(14) 0.0269(16) 0.000 0.0121(11) 0.000 Na 0.045(2) 0.040(2) 0.155(5) 0.000 0.008(3) 0.000 Ti1 0.0080(4) 0.0130(5) 0.0078(5) -0.0032(4) 0.0013(4) 0.0014(4) Si1 0.0102(5) 0.0132(5) 0.0102(6) 0.0001(4) 0.0037(4) 0.0013(4) Si2 0.0100(5) 0.0087(5) 0.0116(6) 0.0001(4) 0.0027(4) 0.0000(4) Si3 0.0127(7) 0.0139(8) 0.0086(8) 0.000 0.0005(6) 0.000 O1 0.0124(13) 0.0163(14) 0.0176(16) 0.0038(12) 0.0065(12) 0.0029(11) O2 0.0231(15) 0.0291(18) 0.0163(17) 0.0034(14) -0.0008(13) 0.0076(14) O3 0.0238(15) 0.0262(17) 0.0142(16) -0.0026(14) 0.0068(12) 0.0055(14) O4 0.017(2) 0.011(2) 0.032(3) 0.000 0.0101(19) 0.000 O5 0.0138(13) 0.0153(15) 0.0183(16) 0.0026(12) 0.0096(12) 0.0004(11) O6 0.0106(13) 0.0198(16) 0.0208(17) 0.0052(13) 0.0017(12) -0.0002(12) O7 0.0155(14) 0.0175(15) 0.0161(16) -0.0066(12) 0.0074(12) -0.0049(12) OW8 0.016(5) 0.003(5) 0.013(6) -0.003(4) 0.008(5) -0.004(4) OW9 0.137(10) 0.084(8) 0.067(8) -0.002(7) -0.002(8) 0.043(8) OW10 0.076(8) 0.030(6) 0.059(8) 0.000 0.053(7) 0.000 OW11 0.335(17) 0.082(7) 0.157(10) -0.013(7) 0.194(12) -0.013(9) OW12 0.130(18) 0.16(3) 0.68(11) 0.000 0.22(5) 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 Ca OW10 0.917(11) . ? Ca O7 2.364(3) 2_655 ? Ca O7 2.364(3) . ? Ca OW9 2.444(11) . ? Ca OW9 2.444(11) 2_655 ? Ca OW10 2.449(13) 5_665 ? Ca OW8 2.492(11) 2_655 ? Ca OW8 2.492(10) . ? Ca O5 2.517(4) 8 ? Ca O5 2.517(4) 7 ? Ca Ca 3.366(6) 5_665 ? Ca Ti1 3.413(2) . ? Na OW8 2.290(11) 6_565 ? Na OW8 2.290(11) . ? Na OW12 2.47(6) . ? Na O1 2.981(4) . ? Na O1 2.981(4) 6_565 ? Na O6 2.987(3) . ? Na O6 2.987(3) 6_565 ? Na Na 3.225(10) 5_565 ? Ti1 O6 1.940(3) . ? Ti1 O6 1.940(3) 7 ? Ti1 O5 1.950(3) 8 ? Ti1 O5 1.950(3) 2 ? Ti1 O7 1.969(3) 7 ? Ti1 O7 1.969(3) . ? Ti1 Ca 3.413(2) 7 ? Si1 O6 1.605(3) . ? Si1 O5 1.606(3) . ? Si1 O3 1.623(3) . ? Si1 O1 1.643(3) . ? Si1 Ca 3.517(3) 7 ? Si2 O4 1.5991(12) . ? Si2 O7 1.606(3) . ? Si2 O2 1.608(3) . ? Si2 O1 1.623(3) 2 ? Si3 O3 1.600(3) 7 ? Si3 O3 1.600(3) 8_556 ? Si3 O2 1.603(3) . ? Si3 O2 1.603(3) 2_656 ? O1 Si2 1.623(3) 2 ? O3 Si3 1.600(3) 7 ? O4 Si2 1.5991(12) 6_565 ? O5 Ti1 1.950(3) 2 ? O5 Ca 2.517(4) 7 ? OW8 OW9 1.330(15) . ? OW10 OW10 1.53(2) 5_665 ? OW10 Ca 2.449(13) 5_665 ? 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 OW10 Ca O7 104.77(10) . 2_655 ? OW10 Ca O7 104.77(10) . . ? O7 Ca O7 150.5(2) 2_655 . ? OW10 Ca OW9 72.5(3) . . ? O7 Ca OW9 94.7(3) 2_655 . ? O7 Ca OW9 94.1(3) . . ? OW10 Ca OW9 72.5(3) . 2_655 ? O7 Ca OW9 94.1(3) 2_655 2_655 ? O7 Ca OW9 94.7(3) . 2_655 ? OW9 Ca OW9 145.0(6) . 2_655 ? OW10 Ca OW10 0.000(2) . 5_665 ? O7 Ca OW10 104.77(10) 2_655 5_665 ? O7 Ca OW10 104.77(10) . 5_665 ? OW9 Ca OW10 72.5(3) . 5_665 ? OW9 Ca OW10 72.5(3) 2_655 5_665 ? OW10 Ca OW8 81.7(2) . 2_655 ? O7 Ca OW8 62.8(3) 2_655 2_655 ? O7 Ca OW8 122.0(3) . 2_655 ? OW9 Ca OW8 140.2(4) . 2_655 ? OW9 Ca OW8 31.2(4) 2_655 2_655 ? OW10 Ca OW8 81.7(2) 5_665 2_655 ? OW10 Ca OW8 81.7(2) . . ? O7 Ca OW8 122.0(3) 2_655 . ? O7 Ca OW8 62.8(3) . . ? OW9 Ca OW8 31.2(4) . . ? OW9 Ca OW8 140.2(4) 2_655 . ? OW10 Ca OW8 81.7(2) 5_665 . ? OW8 Ca OW8 163.5(5) 2_655 . ? OW10 Ca O5 141.23(8) . 8 ? O7 Ca O5 88.64(12) 2_655 8 ? O7 Ca O5 68.04(10) . 8 ? OW9 Ca O5 70.2(3) . 8 ? OW9 Ca O5 143.8(3) 2_655 8 ? OW10 Ca O5 141.23(8) 5_665 8 ? OW8 Ca O5 135.5(3) 2_655 8 ? OW8 Ca O5 60.7(2) . 8 ? OW10 Ca O5 141.23(8) . 7 ? O7 Ca O5 68.04(10) 2_655 7 ? O7 Ca O5 88.64(12) . 7 ? OW9 Ca O5 143.8(3) . 7 ? OW9 Ca O5 70.2(3) 2_655 7 ? OW10 Ca O5 141.23(8) 5_665 7 ? OW8 Ca O5 60.7(2) 2_655 7 ? OW8 Ca O5 135.5(3) . 7 ? O5 Ca O5 77.55(15) 8 7 ? OW10 Ca Ca 0.000(1) . 5_665 ? O7 Ca Ca 104.77(10) 2_655 5_665 ? O7 Ca Ca 104.77(10) . 5_665 ? OW9 Ca Ca 72.5(3) . 5_665 ? OW9 Ca Ca 72.5(3) 2_655 5_665 ? OW10 Ca Ca 0.000(1) 5_665 5_665 ? OW8 Ca Ca 81.7(2) 2_655 5_665 ? OW8 Ca Ca 81.7(2) . 5_665 ? O5 Ca Ca 141.23(8) 8 5_665 ? O5 Ca Ca 141.23(8) 7 5_665 ? OW10 Ca Ti1 131.76(4) . . ? O7 Ca Ti1 119.24(12) 2_655 . ? O7 Ca Ti1 34.10(7) . . ? OW9 Ca Ti1 84.6(3) . . ? OW9 Ca Ti1 119.7(3) 2_655 . ? OW10 Ca Ti1 131.76(4) 5_665 . ? OW8 Ca Ti1 134.5(2) 2_655 . ? OW8 Ca Ti1 59.3(2) . . ? O5 Ca Ti1 34.37(6) 8 . ? O5 Ca Ti1 77.70(9) 7 . ? Ca Ca Ti1 131.76(4) 5_665 . ? OW8 Na OW8 70.7(5) 6_565 . ? OW8 Na OW12 86.9(5) 6_565 . ? OW8 Na OW12 86.9(5) . . ? OW8 Na O1 145.5(4) 6_565 . ? OW8 Na O1 95.6(3) . . ? OW12 Na O1 60.2(4) . . ? OW8 Na O1 95.6(3) 6_565 6_565 ? OW8 Na O1 145.5(4) . 6_565 ? OW12 Na O1 60.2(4) . 6_565 ? O1 Na O1 77.76(14) . 6_565 ? OW8 Na O6 122.2(3) 6_565 . ? OW8 Na O6 51.6(3) . . ? OW12 Na O6 87.25(13) . . ? O1 Na O6 51.74(7) . . ? O1 Na O6 129.28(15) 6_565 . ? OW8 Na O6 51.6(3) 6_565 6_565 ? OW8 Na O6 122.2(3) . 6_565 ? OW12 Na O6 87.25(13) . 6_565 ? O1 Na O6 129.28(15) . 6_565 ? O1 Na O6 51.74(8) 6_565 6_565 ? O6 Na O6 171.9(2) . 6_565 ? OW8 Na Na 136.0(3) 6_565 5_565 ? OW8 Na Na 136.0(3) . 5_565 ? OW12 Na Na 122.0(6) . 5_565 ? O1 Na Na 75.80(12) . 5_565 ? O1 Na Na 75.80(12) 6_565 5_565 ? O6 Na Na 93.96(11) . 5_565 ? O6 Na Na 93.96(11) 6_565 5_565 ? O6 Ti1 O6 180.0(2) . 7 ? O6 Ti1 O5 90.77(12) . 8 ? O6 Ti1 O5 89.23(12) 7 8 ? O6 Ti1 O5 89.23(12) . 2 ? O6 Ti1 O5 90.77(12) 7 2 ? O5 Ti1 O5 180.0 8 2 ? O6 Ti1 O7 89.60(12) . 7 ? O6 Ti1 O7 90.40(12) 7 7 ? O5 Ti1 O7 91.52(11) 8 7 ? O5 Ti1 O7 88.48(11) 2 7 ? O6 Ti1 O7 90.40(12) . . ? O6 Ti1 O7 89.60(12) 7 . ? O5 Ti1 O7 88.48(11) 8 . ? O5 Ti1 O7 91.52(11) 2 . ? O7 Ti1 O7 180.00(18) 7 . ? O6 Ti1 Ca 83.31(8) . 7 ? O6 Ti1 Ca 96.69(8) 7 7 ? O5 Ti1 Ca 133.22(8) 8 7 ? O5 Ti1 Ca 46.78(8) 2 7 ? O7 Ti1 Ca 42.32(8) 7 7 ? O7 Ti1 Ca 137.68(8) . 7 ? O6 Ti1 Ca 96.69(8) . . ? O6 Ti1 Ca 83.31(8) 7 . ? O5 Ti1 Ca 46.78(8) 8 . ? O5 Ti1 Ca 133.22(8) 2 . ? O7 Ti1 Ca 137.68(8) 7 . ? O7 Ti1 Ca 42.32(8) . . ? Ca Ti1 Ca 180.00(8) 7 . ? O6 Si1 O5 116.28(16) . . ? O6 Si1 O3 111.48(16) . . ? O5 Si1 O3 108.21(16) . . ? O6 Si1 O1 106.61(15) . . ? O5 Si1 O1 108.59(14) . . ? O3 Si1 O1 105.05(16) . . ? O6 Si1 Ca 84.55(11) . 7 ? O5 Si1 Ca 40.34(10) . 7 ? O3 Si1 Ca 100.33(13) . 7 ? O1 Si1 Ca 145.73(11) . 7 ? O4 Si2 O7 109.7(2) . . ? O4 Si2 O2 108.4(2) . . ? O7 Si2 O2 112.23(16) . . ? O4 Si2 O1 108.61(18) . 2 ? O7 Si2 O1 110.94(15) . 2 ? O2 Si2 O1 106.84(16) . 2 ? O4 Si2 Ca 83.55(16) . . ? O7 Si2 Ca 33.20(10) . . ? O2 Si2 Ca 103.44(12) . . ? O1 Si2 Ca 141.26(12) 2 . ? O3 Si3 O3 110.3(2) 7 8_556 ? O3 Si3 O2 110.59(15) 7 . ? O3 Si3 O2 108.25(16) 8_556 . ? O3 Si3 O2 108.25(16) 7 2_656 ? O3 Si3 O2 110.59(16) 8_556 2_656 ? O2 Si3 O2 108.9(2) . 2_656 ? Si2 O1 Si1 126.29(17) 2 . ? Si2 O1 Na 121.79(16) 2 . ? Si1 O1 Na 100.43(13) . . ? Si3 O2 Si2 151.4(2) . . ? Si3 O3 Si1 151.3(2) 7 . ? Si2 O4 Si2 162.7(3) . 6_565 ? Si1 O5 Ti1 134.31(17) . 2 ? Si1 O5 Ca 115.28(13) . 7 ? Ti1 O5 Ca 98.85(11) 2 7 ? Si1 O6 Ti1 135.03(18) . . ? Si1 O6 Na 101.22(15) . . ? Ti1 O6 Na 119.70(15) . . ? Si2 O7 Ti1 130.64(16) . . ? Si2 O7 Ca 124.97(16) . . ? Ti1 O7 Ca 103.58(13) . . ? OW9 OW8 Na 124.0(8) . . ? OW9 OW8 Ca 72.4(7) . . ? Na OW8 Ca 129.7(5) . . ? OW8 OW9 Ca 76.4(7) . . ? Ca OW10 OW10 180.000(2) . 5_665 ? Ca OW10 Ca 180.0 . 5_665 ? OW10 OW10 Ca 0.000(1) 5_665 5_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.121 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.153