data_hydgug50 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Be2.60 H3 Ca3 F0 Na0 O14 Si3.40' _chemical_formula_weight 466.20 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' 'Be' 'Be' 0.0005 0.0002 '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' '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' _space_group_crystal_system tetragonal _space_group_IT_number 113 _space_group_name_H-M_alt 'P -4 21 m' _space_group_name_Hall 'P -4 2ab' _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' 'x+1/2, -y+1/2, -z' '-y+1/2, -x+1/2, z' 'y+1/2, x+1/2, z' _cell_length_a 7.4151(10) _cell_length_b 7.4151(10) _cell_length_c 4.9652(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 273.01(9) _cell_formula_units_Z 1 _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_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.836 _exptl_crystal_F_000 233 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 1.975 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2540 _diffrn_reflns_av_unetI/netI 0.0180 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.747 _diffrn_reflns_theta_max 27.574 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 355 _reflns_number_gt 342 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.606 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _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-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component twin. ; _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^)+(0.0210P)^2^+0.4299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 128 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.05(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 355 _refine_ls_number_parameters 41 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.305 _refine_ls_restrained_S_all 1.307 _refine_ls_shift/su_max 0.061 _refine_ls_shift/su_mean 0.006 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 Ca1 Ca 0.34079(5) 0.84079(5) 0.51145(12) 0.02025(11) Uani 0.7565(12) 2 d S T . . . Si1 Si 0.0000 0.0000 0.0000 0.01263(18) Uani 0.794(3) 4 d S T P . . Be1 Be 0.0000 0.0000 0.0000 0.01263(18) Uani 0.206(3) 4 d S T P . . Si2 Si 0.35765(9) 0.14235(9) 0.05133(18) 0.0118(2) Uani 0.428(2) 2 d S T P . . Be2 Be 0.35765(9) 0.14235(9) 0.05133(18) 0.0118(2) Uani 0.572(2) 2 d S T P . . O1 O 0.5000 0.0000 0.1811(5) 0.0202(5) Uani 1 4 d S T P . . O2 O 0.35591(15) 0.14409(15) -0.2698(3) 0.0185(3) Uani 1 2 d DS T P . . O3 O 0.16131(15) 0.08519(15) 0.1879(2) 0.0195(3) Uani 1 1 d . . . . . H2A H 0.296(4) 0.204(4) -0.419(7) 0.050 Uiso 0.25 2 d DS U P . . H2B H 0.5000 0.0000 -0.153(9) 0.050 Uiso 1 4 d DS U 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 Ca1 0.02239(14) 0.02239(14) 0.0160(2) 0.00087(17) 0.00087(17) -0.0070(2) Si1 0.0108(2) 0.0108(2) 0.0163(4) 0.000 0.000 0.000 Be1 0.0108(2) 0.0108(2) 0.0163(4) 0.000 0.000 0.000 Si2 0.0115(2) 0.0115(2) 0.0125(4) 0.0000(2) 0.0000(2) -0.0010(4) Be2 0.0115(2) 0.0115(2) 0.0125(4) 0.0000(2) 0.0000(2) -0.0010(4) O1 0.0218(7) 0.0218(7) 0.0170(9) 0.000 0.000 0.0053(10) O2 0.0198(4) 0.0198(4) 0.0159(6) 0.0011(4) -0.0011(4) 0.0011(7) O3 0.0146(4) 0.0227(5) 0.0212(5) -0.0039(4) 0.0012(5) -0.0025(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 Ca1 H2A 1.51(4) 3_565 ? Ca1 O1 2.3403(17) 1_565 ? Ca1 O2 2.3863(17) 3_565 ? Ca1 O3 2.4125(12) 5_556 ? Ca1 O3 2.4125(13) 3_566 ? Ca1 O2 2.5000(13) 2_666 ? Ca1 O2 2.5000(13) 1_566 ? Ca1 O3 2.7633(12) 8 ? Ca1 O3 2.7633(12) 1_565 ? Ca1 Be2 3.0072(11) 3_566 ? Ca1 Si2 3.0072(11) 3_566 ? Ca1 Be2 3.1992(10) 2_665 ? Ca1 Be2 3.1992(10) 1_565 ? Ca1 Si2 3.1992(10) 2_665 ? Ca1 Si2 3.1992(10) 1_565 ? Ca1 Ca1 3.3391(12) 2_675 ? Ca1 Be2 3.4841(12) 3_565 ? Ca1 Si2 3.4841(12) 3_565 ? Si1 O3 1.6433(11) 3 ? Si1 O3 1.6433(11) 2 ? Si1 O3 1.6433(11) 4 ? Si1 O3 1.6433(11) . ? Si1 Ca1 3.6965(6) 4_656 ? Si1 Ca1 3.6965(6) 2_564 ? Si1 Ca1 3.6965(6) 1_544 ? Si1 Ca1 3.6965(6) 3_456 ? Si1 Ca1 3.7720(6) 3_455 ? Si1 Ca1 3.7720(6) 1_545 ? Si1 Ca1 3.7720(6) 4_655 ? Si1 Ca1 3.7720(6) 2_565 ? Si2 O2 1.5946(17) . ? Si2 O1 1.6260(13) . ? Si2 O3 1.6611(13) . ? Si2 O3 1.6612(13) 7 ? Si2 Ca1 3.0072(11) 4_656 ? Si2 Ca1 3.1992(10) 2_665 ? Si2 Ca1 3.1992(10) 1_545 ? Si2 Ca1 3.4840(12) 4_655 ? Si2 Ca1 3.4931(11) 1_544 ? Si2 Ca1 3.4931(11) 2_664 ? O1 Be2 1.6259(13) 2_655 ? O1 Si2 1.6259(13) 2_655 ? O1 H2B 1.66(4) . ? O1 Ca1 2.3404(17) 2_665 ? O1 Ca1 2.3403(17) 1_545 ? O1 Ca1 3.721(2) 1_544 ? O1 Ca1 3.721(2) 2_664 ? O1 Ca1 3.8860(11) 3_556 ? O1 Ca1 3.8860(11) 4_656 ? O2 H2B 1.619(16) . ? O2 Ca1 2.3862(17) 4_655 ? O2 Ca1 2.5000(13) 1_544 ? O2 Ca1 2.5000(13) 2_664 ? O3 Ca1 2.4125(12) 4_656 ? O3 Ca1 2.7633(12) 1_545 ? O3 Ca1 3.9562(14) 4_655 ? O3 Ca1 4.0420(13) 1_544 ? O3 Ca1 4.0635(13) 2_665 ? O3 Ca1 4.0918(13) 2_565 ? 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 H2A Ca1 O1 117.7(15) 3_565 1_565 ? H2A Ca1 O2 12.4(15) 3_565 3_565 ? O1 Ca1 O2 105.33(6) 1_565 3_565 ? H2A Ca1 O3 69.9(12) 3_565 5_556 ? O1 Ca1 O3 146.42(3) 1_565 5_556 ? O2 Ca1 O3 80.03(4) 3_565 5_556 ? H2A Ca1 O3 69.9(12) 3_565 3_566 ? O1 Ca1 O3 146.42(3) 1_565 3_566 ? O2 Ca1 O3 80.03(4) 3_565 3_566 ? O3 Ca1 O3 66.87(6) 5_556 3_566 ? H2A Ca1 O2 140.2(5) 3_565 2_666 ? O1 Ca1 O2 80.10(4) 1_565 2_666 ? O2 Ca1 O2 142.72(3) 3_565 2_666 ? O3 Ca1 O2 76.84(4) 5_556 2_666 ? O3 Ca1 O2 115.99(5) 3_566 2_666 ? H2A Ca1 O2 140.2(5) 3_565 1_566 ? O1 Ca1 O2 80.10(4) 1_565 1_566 ? O2 Ca1 O2 142.72(3) 3_565 1_566 ? O3 Ca1 O2 115.99(5) 5_556 1_566 ? O3 Ca1 O2 76.84(4) 3_566 1_566 ? O2 Ca1 O2 74.37(6) 2_666 1_566 ? H2A Ca1 O3 86.5(9) 3_565 8 ? O1 Ca1 O3 60.32(3) 1_565 8 ? O2 Ca1 O3 79.29(3) 3_565 8 ? O3 Ca1 O3 89.17(5) 5_556 8 ? O3 Ca1 O3 150.66(3) 3_566 8 ? O2 Ca1 O3 71.59(4) 2_666 8 ? O2 Ca1 O3 131.03(4) 1_566 8 ? H2A Ca1 O3 86.5(9) 3_565 1_565 ? O1 Ca1 O3 60.32(3) 1_565 1_565 ? O2 Ca1 O3 79.29(3) 3_565 1_565 ? O3 Ca1 O3 150.66(3) 5_556 1_565 ? O3 Ca1 O3 89.17(5) 3_566 1_565 ? O2 Ca1 O3 131.03(4) 2_666 1_565 ? O2 Ca1 O3 71.59(4) 1_566 1_565 ? O3 Ca1 O3 107.09(5) 8 1_565 ? H2A Ca1 Be2 64.0(15) 3_565 3_566 ? O1 Ca1 Be2 178.28(5) 1_565 3_566 ? O2 Ca1 Be2 76.39(4) 3_565 3_566 ? O3 Ca1 Be2 33.47(3) 5_556 3_566 ? O3 Ca1 Be2 33.47(3) 3_566 3_566 ? O2 Ca1 Be2 98.54(3) 2_666 3_566 ? O2 Ca1 Be2 98.54(3) 1_566 3_566 ? O3 Ca1 Be2 120.32(3) 8 3_566 ? O3 Ca1 Be2 120.32(3) 1_565 3_566 ? H2A Ca1 Si2 64.0(15) 3_565 3_566 ? O1 Ca1 Si2 178.28(5) 1_565 3_566 ? O2 Ca1 Si2 76.39(4) 3_565 3_566 ? O3 Ca1 Si2 33.47(3) 5_556 3_566 ? O3 Ca1 Si2 33.47(3) 3_566 3_566 ? O2 Ca1 Si2 98.54(3) 2_666 3_566 ? O2 Ca1 Si2 98.54(3) 1_566 3_566 ? O3 Ca1 Si2 120.32(3) 8 3_566 ? O3 Ca1 Si2 120.32(3) 1_565 3_566 ? Be2 Ca1 Si2 0.0 3_566 3_566 ? H2A Ca1 Be2 106.2(13) 3_565 2_665 ? O1 Ca1 Be2 29.22(2) 1_565 2_665 ? O2 Ca1 Be2 95.28(4) 3_565 2_665 ? O3 Ca1 Be2 118.49(3) 5_556 2_665 ? O3 Ca1 Be2 172.37(4) 3_566 2_665 ? O2 Ca1 Be2 71.32(4) 2_666 2_665 ? O2 Ca1 Be2 104.11(3) 1_566 2_665 ? O3 Ca1 Be2 31.28(3) 8 2_665 ? O3 Ca1 Be2 84.03(3) 1_565 2_665 ? Be2 Ca1 Be2 151.240(15) 3_566 2_665 ? Si2 Ca1 Be2 151.240(15) 3_566 2_665 ? H2A Ca1 Be2 106.2(13) 3_565 1_565 ? O1 Ca1 Be2 29.22(2) 1_565 1_565 ? O2 Ca1 Be2 95.28(4) 3_565 1_565 ? O3 Ca1 Be2 172.37(4) 5_556 1_565 ? O3 Ca1 Be2 118.49(3) 3_566 1_565 ? O2 Ca1 Be2 104.11(3) 2_666 1_565 ? O2 Ca1 Be2 71.32(4) 1_566 1_565 ? O3 Ca1 Be2 84.03(3) 8 1_565 ? O3 Ca1 Be2 31.28(3) 1_565 1_565 ? Be2 Ca1 Be2 151.240(15) 3_566 1_565 ? Si2 Ca1 Be2 151.240(15) 3_566 1_565 ? Be2 Ca1 Be2 55.63(4) 2_665 1_565 ? H2A Ca1 Si2 106.2(13) 3_565 2_665 ? O1 Ca1 Si2 29.22(2) 1_565 2_665 ? O2 Ca1 Si2 95.28(4) 3_565 2_665 ? O3 Ca1 Si2 118.49(3) 5_556 2_665 ? O3 Ca1 Si2 172.37(4) 3_566 2_665 ? O2 Ca1 Si2 71.32(4) 2_666 2_665 ? O2 Ca1 Si2 104.11(3) 1_566 2_665 ? O3 Ca1 Si2 31.28(3) 8 2_665 ? O3 Ca1 Si2 84.03(3) 1_565 2_665 ? Be2 Ca1 Si2 151.2 3_566 2_665 ? Si2 Ca1 Si2 151.240(15) 3_566 2_665 ? Be2 Ca1 Si2 0.0 2_665 2_665 ? Be2 Ca1 Si2 55.6 1_565 2_665 ? H2A Ca1 Si2 106.2(13) 3_565 1_565 ? O1 Ca1 Si2 29.22(2) 1_565 1_565 ? O2 Ca1 Si2 95.28(4) 3_565 1_565 ? O3 Ca1 Si2 172.37(4) 5_556 1_565 ? O3 Ca1 Si2 118.49(3) 3_566 1_565 ? O2 Ca1 Si2 104.11(3) 2_666 1_565 ? O2 Ca1 Si2 71.32(4) 1_566 1_565 ? O3 Ca1 Si2 84.03(3) 8 1_565 ? O3 Ca1 Si2 31.28(3) 1_565 1_565 ? Be2 Ca1 Si2 151.2 3_566 1_565 ? Si2 Ca1 Si2 151.240(15) 3_566 1_565 ? Be2 Ca1 Si2 55.6 2_665 1_565 ? Be2 Ca1 Si2 0.0 1_565 1_565 ? Si2 Ca1 Si2 55.63(4) 2_665 1_565 ? H2A Ca1 Ca1 162.2(15) 3_565 2_675 ? O1 Ca1 Ca1 44.49(4) 1_565 2_675 ? O2 Ca1 Ca1 149.82(4) 3_565 2_675 ? O3 Ca1 Ca1 124.06(3) 5_556 2_675 ? O3 Ca1 Ca1 124.06(3) 3_566 2_675 ? O2 Ca1 Ca1 48.10(3) 2_666 2_675 ? O2 Ca1 Ca1 48.10(3) 1_566 2_675 ? O3 Ca1 Ca1 82.93(3) 8 2_675 ? O3 Ca1 Ca1 82.93(3) 1_565 2_675 ? Be2 Ca1 Ca1 133.79(2) 3_566 2_675 ? Si2 Ca1 Ca1 133.79(2) 3_566 2_675 ? Be2 Ca1 Ca1 58.543(14) 2_665 2_675 ? Be2 Ca1 Ca1 58.543(14) 1_565 2_675 ? Si2 Ca1 Ca1 58.543(14) 2_665 2_675 ? Si2 Ca1 Ca1 58.543(14) 1_565 2_675 ? H2A Ca1 Be2 35.5(15) 3_565 3_565 ? O1 Ca1 Be2 82.19(5) 1_565 3_565 ? O2 Ca1 Be2 23.14(4) 3_565 3_565 ? O3 Ca1 Be2 99.30(4) 5_556 3_565 ? O3 Ca1 Be2 99.30(4) 3_566 3_565 ? O2 Ca1 Be2 138.36(4) 2_666 3_565 ? O2 Ca1 Be2 138.36(4) 1_566 3_565 ? O3 Ca1 Be2 66.88(3) 8 3_565 ? O3 Ca1 Be2 66.88(3) 1_565 3_565 ? Be2 Ca1 Be2 99.54(3) 3_566 3_565 ? Si2 Ca1 Be2 99.54(3) 3_566 3_565 ? Be2 Ca1 Be2 74.868(19) 2_665 3_565 ? Be2 Ca1 Be2 74.87(2) 1_565 3_565 ? Si2 Ca1 Be2 74.868(19) 2_665 3_565 ? Si2 Ca1 Be2 74.87(2) 1_565 3_565 ? Ca1 Ca1 Be2 126.676(19) 2_675 3_565 ? H2A Ca1 Si2 35.5(15) 3_565 3_565 ? O1 Ca1 Si2 82.19(5) 1_565 3_565 ? O2 Ca1 Si2 23.14(4) 3_565 3_565 ? O3 Ca1 Si2 99.30(4) 5_556 3_565 ? O3 Ca1 Si2 99.30(4) 3_566 3_565 ? O2 Ca1 Si2 138.36(4) 2_666 3_565 ? O2 Ca1 Si2 138.36(4) 1_566 3_565 ? O3 Ca1 Si2 66.88(3) 8 3_565 ? O3 Ca1 Si2 66.88(3) 1_565 3_565 ? Be2 Ca1 Si2 99.5 3_566 3_565 ? Si2 Ca1 Si2 99.54(3) 3_566 3_565 ? Be2 Ca1 Si2 74.9 2_665 3_565 ? Be2 Ca1 Si2 74.9 1_565 3_565 ? Si2 Ca1 Si2 74.868(19) 2_665 3_565 ? Si2 Ca1 Si2 74.87(2) 1_565 3_565 ? Ca1 Ca1 Si2 126.676(19) 2_675 3_565 ? Be2 Ca1 Si2 0.0 3_565 3_565 ? O3 Si1 O3 108.81(4) 3 2 ? O3 Si1 O3 110.80(8) 3 4 ? O3 Si1 O3 108.81(4) 2 4 ? O3 Si1 O3 108.81(4) 3 . ? O3 Si1 O3 110.80(8) 2 . ? O3 Si1 O3 108.81(4) 4 . ? O3 Si1 Ca1 138.37(4) 3 4_656 ? O3 Si1 Ca1 97.04(4) 2 4_656 ? O3 Si1 Ca1 89.88(4) 4 4_656 ? O3 Si1 Ca1 29.78(4) . 4_656 ? O3 Si1 Ca1 97.04(4) 3 2_564 ? O3 Si1 Ca1 89.88(4) 2 2_564 ? O3 Si1 Ca1 29.78(4) 4 2_564 ? O3 Si1 Ca1 138.37(4) . 2_564 ? Ca1 Si1 Ca1 115.509(11) 4_656 2_564 ? O3 Si1 Ca1 29.78(4) 3 1_544 ? O3 Si1 Ca1 138.37(4) 2 1_544 ? O3 Si1 Ca1 97.04(4) 4 1_544 ? O3 Si1 Ca1 89.88(4) . 1_544 ? Ca1 Si1 Ca1 115.509(11) 4_656 1_544 ? Ca1 Si1 Ca1 97.97(2) 2_564 1_544 ? O3 Si1 Ca1 89.88(4) 3 3_456 ? O3 Si1 Ca1 29.78(4) 2 3_456 ? O3 Si1 Ca1 138.37(4) 4 3_456 ? O3 Si1 Ca1 97.04(4) . 3_456 ? Ca1 Si1 Ca1 97.972(19) 4_656 3_456 ? Ca1 Si1 Ca1 115.509(11) 2_564 3_456 ? Ca1 Si1 Ca1 115.509(11) 1_544 3_456 ? O3 Si1 Ca1 41.44(4) 3 3_455 ? O3 Si1 Ca1 84.09(4) 2 3_455 ? O3 Si1 Ca1 89.14(4) 4 3_455 ? O3 Si1 Ca1 150.18(4) . 3_455 ? Ca1 Si1 Ca1 178.697(13) 4_656 3_455 ? Ca1 Si1 Ca1 63.781(8) 2_564 3_455 ? Ca1 Si1 Ca1 63.781(8) 1_544 3_455 ? Ca1 Si1 Ca1 83.331(14) 3_456 3_455 ? O3 Si1 Ca1 84.09(4) 3 1_545 ? O3 Si1 Ca1 89.14(4) 2 1_545 ? O3 Si1 Ca1 150.18(4) 4 1_545 ? O3 Si1 Ca1 41.44(4) . 1_545 ? Ca1 Si1 Ca1 63.781(8) 4_656 1_545 ? Ca1 Si1 Ca1 178.697(13) 2_564 1_545 ? Ca1 Si1 Ca1 83.331(14) 1_544 1_545 ? Ca1 Si1 Ca1 63.781(8) 3_456 1_545 ? Ca1 Si1 Ca1 116.952(11) 3_455 1_545 ? O3 Si1 Ca1 89.14(4) 3 4_655 ? O3 Si1 Ca1 150.18(4) 2 4_655 ? O3 Si1 Ca1 41.44(4) 4 4_655 ? O3 Si1 Ca1 84.09(4) . 4_655 ? Ca1 Si1 Ca1 83.331(14) 4_656 4_655 ? Ca1 Si1 Ca1 63.781(8) 2_564 4_655 ? Ca1 Si1 Ca1 63.781(8) 1_544 4_655 ? Ca1 Si1 Ca1 178.697(13) 3_456 4_655 ? Ca1 Si1 Ca1 95.367(19) 3_455 4_655 ? Ca1 Si1 Ca1 116.952(11) 1_545 4_655 ? O3 Si1 Ca1 150.18(4) 3 2_565 ? O3 Si1 Ca1 41.44(4) 2 2_565 ? O3 Si1 Ca1 84.09(4) 4 2_565 ? O3 Si1 Ca1 89.14(4) . 2_565 ? Ca1 Si1 Ca1 63.781(8) 4_656 2_565 ? Ca1 Si1 Ca1 83.331(14) 2_564 2_565 ? Ca1 Si1 Ca1 178.697(13) 1_544 2_565 ? Ca1 Si1 Ca1 63.781(8) 3_456 2_565 ? Ca1 Si1 Ca1 116.952(11) 3_455 2_565 ? Ca1 Si1 Ca1 95.367(19) 1_545 2_565 ? Ca1 Si1 Ca1 116.952(11) 4_655 2_565 ? O2 Si2 O1 114.01(11) . . ? O2 Si2 O3 113.78(6) . . ? O1 Si2 O3 103.97(7) . . ? O2 Si2 O3 113.78(6) . 7 ? O1 Si2 O3 103.97(7) . 7 ? O3 Si2 O3 106.29(9) . 7 ? O2 Si2 Ca1 135.56(8) . 4_656 ? O1 Si2 Ca1 110.43(8) . 4_656 ? O3 Si2 Ca1 53.22(5) . 4_656 ? O3 Si2 Ca1 53.22(5) 7 4_656 ? O2 Si2 Ca1 136.00(5) . 2_665 ? O1 Si2 Ca1 44.65(5) . 2_665 ? O3 Si2 Ca1 109.33(6) . 2_665 ? O3 Si2 Ca1 59.72(5) 7 2_665 ? Ca1 Si2 Ca1 78.89(2) 4_656 2_665 ? O2 Si2 Ca1 136.00(5) . 1_545 ? O1 Si2 Ca1 44.65(5) . 1_545 ? O3 Si2 Ca1 59.72(5) . 1_545 ? O3 Si2 Ca1 109.33(6) 7 1_545 ? Ca1 Si2 Ca1 78.89(2) 4_656 1_545 ? Ca1 Si2 Ca1 62.91(3) 2_665 1_545 ? O2 Si2 Ca1 36.02(6) . 4_655 ? O1 Si2 Ca1 150.03(9) . 4_655 ? O3 Si2 Ca1 93.73(5) . 4_655 ? O3 Si2 Ca1 93.73(5) 7 4_655 ? Ca1 Si2 Ca1 99.54(3) 4_656 4_655 ? Ca1 Si2 Ca1 148.367(14) 2_665 4_655 ? Ca1 Si2 Ca1 148.367(14) 1_545 4_655 ? O2 Si2 Ca1 40.32(4) . 1_544 ? O1 Si2 Ca1 84.94(7) . 1_544 ? O3 Si2 Ca1 96.82(4) . 1_544 ? O3 Si2 Ca1 152.07(5) 7 1_544 ? Ca1 Si2 Ca1 148.182(17) 4_656 1_544 ? Ca1 Si2 Ca1 126.73(3) 2_665 1_544 ? Ca1 Si2 Ca1 95.69(2) 1_545 1_544 ? Ca1 Si2 Ca1 68.89(2) 4_655 1_544 ? O2 Si2 Ca1 40.32(4) . 2_664 ? O1 Si2 Ca1 84.94(7) . 2_664 ? O3 Si2 Ca1 152.07(5) . 2_664 ? O3 Si2 Ca1 96.81(4) 7 2_664 ? Ca1 Si2 Ca1 148.182(18) 4_656 2_664 ? Ca1 Si2 Ca1 95.69(2) 2_665 2_664 ? Ca1 Si2 Ca1 126.73(3) 1_545 2_664 ? Ca1 Si2 Ca1 68.89(2) 4_655 2_664 ? Ca1 Si2 Ca1 57.11(2) 1_544 2_664 ? Be2 O1 Si2 0.0 2_655 2_655 ? Be2 O1 Si2 133.3 2_655 . ? Si2 O1 Si2 133.29(16) 2_655 . ? Be2 O1 H2B 66.65(8) 2_655 . ? Si2 O1 H2B 66.65(8) 2_655 . ? Si2 O1 H2B 66.65(8) . . ? Be2 O1 Ca1 106.13(4) 2_655 2_665 ? Si2 O1 Ca1 106.13(4) 2_655 2_665 ? Si2 O1 Ca1 106.13(4) . 2_665 ? H2B O1 Ca1 134.49(4) . 2_665 ? Be2 O1 Ca1 106.13(4) 2_655 1_545 ? Si2 O1 Ca1 106.13(4) 2_655 1_545 ? Si2 O1 Ca1 106.13(4) . 1_545 ? H2B O1 Ca1 134.49(4) . 1_545 ? Ca1 O1 Ca1 91.02(8) 2_665 1_545 ? Be2 O1 Ca1 69.25(7) 2_655 1_544 ? Si2 O1 Ca1 69.25(7) 2_655 1_544 ? Si2 O1 Ca1 69.25(7) . 1_544 ? H2B O1 Ca1 26.661(19) . 1_544 ? Ca1 O1 Ca1 161.15(6) 2_665 1_544 ? Ca1 O1 Ca1 107.83(3) 1_545 1_544 ? Be2 O1 Ca1 69.25(7) 2_655 2_664 ? Si2 O1 Ca1 69.25(7) 2_655 2_664 ? Si2 O1 Ca1 69.25(7) . 2_664 ? H2B O1 Ca1 26.661(19) . 2_664 ? Ca1 O1 Ca1 107.83(3) 2_665 2_664 ? Ca1 O1 Ca1 161.15(6) 1_545 2_664 ? Ca1 O1 Ca1 53.32(4) 1_544 2_664 ? Be2 O1 Ca1 46.48(5) 2_655 3_556 ? Si2 O1 Ca1 46.48(5) 2_655 3_556 ? Si2 O1 Ca1 179.78(11) . 3_556 ? H2B O1 Ca1 113.13(3) . 3_556 ? Ca1 O1 Ca1 74.02(3) 2_665 3_556 ? Ca1 O1 Ca1 74.02(3) 1_545 3_556 ? Ca1 O1 Ca1 110.55(3) 1_544 3_556 ? Ca1 O1 Ca1 110.55(3) 2_664 3_556 ? Be2 O1 Ca1 179.78(11) 2_655 4_656 ? Si2 O1 Ca1 179.78(11) 2_655 4_656 ? Si2 O1 Ca1 46.48(5) . 4_656 ? H2B O1 Ca1 113.13(3) . 4_656 ? Ca1 O1 Ca1 74.02(3) 2_665 4_656 ? Ca1 O1 Ca1 74.02(3) 1_545 4_656 ? Ca1 O1 Ca1 110.55(3) 1_544 4_656 ? Ca1 O1 Ca1 110.55(3) 2_664 4_656 ? Ca1 O1 Ca1 133.74(6) 3_556 4_656 ? Si2 O2 H2B 68.3(15) . . ? Si2 O2 Ca1 120.84(9) . 4_655 ? H2B O2 Ca1 170.8(15) . 4_655 ? Si2 O2 Ca1 115.31(6) . 1_544 ? H2B O2 Ca1 65.9(10) . 1_544 ? Ca1 O2 Ca1 107.70(4) 4_655 1_544 ? Si2 O2 Ca1 115.31(6) . 2_664 ? H2B O2 Ca1 65.9(10) . 2_664 ? Ca1 O2 Ca1 107.70(4) 4_655 2_664 ? Ca1 O2 Ca1 83.80(5) 1_544 2_664 ? Si1 O3 Si2 120.27(7) . . ? Si1 O3 Ca1 130.44(6) . 4_656 ? Si2 O3 Ca1 93.32(6) . 4_656 ? Si1 O3 Ca1 115.37(6) . 1_545 ? Si2 O3 Ca1 89.00(6) . 1_545 ? Ca1 O3 Ca1 99.13(4) 4_656 1_545 ? Si1 O3 Ca1 71.51(4) . 4_655 ? Si2 O3 Ca1 61.50(5) . 4_655 ? Ca1 O3 Ca1 99.59(4) 4_656 4_655 ? Ca1 O3 Ca1 145.72(4) 1_545 4_655 ? Si1 O3 Ca1 66.14(4) . 1_544 ? Si2 O3 Ca1 59.10(4) . 1_544 ? Ca1 O3 Ca1 150.28(4) 4_656 1_544 ? Ca1 O3 Ca1 91.74(3) 1_545 1_544 ? Ca1 O3 Ca1 59.113(19) 4_655 1_544 ? Si1 O3 Ca1 159.67(6) . 2_665 ? Si2 O3 Ca1 47.98(4) . 2_665 ? Ca1 O3 Ca1 69.83(3) 4_656 2_665 ? Ca1 O3 Ca1 54.63(3) 1_545 2_665 ? Ca1 O3 Ca1 106.61(3) 4_655 2_665 ? Ca1 O3 Ca1 95.16(3) 1_544 2_665 ? Si1 O3 Ca1 67.18(4) . 2_565 ? Si2 O3 Ca1 157.45(6) . 2_565 ? Ca1 O3 Ca1 69.26(3) 4_656 2_565 ? Ca1 O3 Ca1 107.34(4) 1_545 2_565 ? Ca1 O3 Ca1 106.07(3) 4_655 2_565 ? Ca1 O3 Ca1 133.31(3) 1_544 2_565 ? Ca1 O3 Ca1 130.80(3) 2_665 2_565 ? 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 O2 H2A O1 0.97(4) 3.32(4) 3.7581(17) 110(3) 3_565 O2 H2A O3 0.97(4) 2.36(3) 3.0857(17) 131(2) 1_554 O2 H2A O3 0.97(4) 2.36(3) 3.0857(17) 131(2) 7_554 _refine_diff_density_max 0.562 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.085 _shelx_res_file ; hydgug50.res created by SHELXL-2014/7 TITL HYDROXYLGUGIAITE, Saga I quarry in P-42(1)m (113) out to 50 degrees theta CELL 0.71073 7.4151 7.4151 4.9652 90.000 90.000 90.000 ZERR 1.00 0.0010 0.0010 0.0010 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM Y, -X, -Z SYMM -Y, X, -Z SYMM 0.5-X, 0.5+Y, -Z SYMM 0.5+X, 0.5-Y, -Z SYMM 0.5-Y, 0.5-X, Z SYMM 0.5+Y, 0.5+X, Z SFAC O BE H F NA SI CA UNIT 14 2.6 3 0 0 3.4 3.0 L.S. 8 DAMP 5000 ACTA LIST 6 TWIN 0 1 0 1 0 0 0 0 -1 BOND HTAB 3 EQIV $1 y, -x+1, -z HTAB O2 O1_$1 EQIV $2 x, y, z-1 HTAB O2 O3_$2 EQIV $3 -y+1/2, -x+1/2, z-1 HTAB O2 O3_$3 FMAP 2 PLAN 20 EXYZ SI1 BE1 EADP SI1 BE1 EXYZ SI2 BE2 EADP SI2 BE2 DFIX 0.98 0.05 O2 H2A DFIX 1.8 0.1 O2 H2B BIND O1 H2B BIND O2 H2B CONN 12 2 CA1 H2A CONN 18 3 CA1 H2B BIND CA1 H2A_$1 REM EXTI 0.000000 WGHT 0.021000 0.429900 BASF 0.55771 FVAR 1.89945 0.79421 0.42780 CA1 7 0.340794 0.840794 0.511450 0.37823 0.02239 0.02239 = 0.01597 0.00087 0.00087 -0.00698 REM NA1 5 0.340664 0.840664 0.511664 -40.50000 0.01794 0.0179 SI1 6 0.000000 0.000000 0.000000 20.25000 0.01078 0.01078 = 0.01634 0.00000 0.00000 0.00000 BE1 2 0.000000 0.000000 0.000000 -20.25000 0.01078 0.01078 = 0.01634 0.00000 0.00000 0.00000 SI2 6 0.357649 0.142351 0.051327 30.50000 0.01145 0.01145 = 0.01249 -0.00003 0.00003 -0.00098 BE2 2 0.357649 0.142351 0.051327 -30.50000 0.01145 0.01145 = 0.01249 -0.00003 0.00003 -0.00098 O1 1 0.500000 0.000000 0.181134 10.25000 0.02184 0.02184 = 0.01702 0.00000 0.00000 0.00534 O2 1 0.355909 0.144091 -0.269817 10.50000 0.01976 0.01976 = 0.01585 0.00105 -0.00105 0.00109 O3 1 0.161307 0.085192 0.187942 11.00000 0.01459 0.02268 = 0.02116 -0.00389 0.00117 -0.00247 H2A 3 0.296141 0.203859 -0.418582 10.12500 10.05000 H2B 3 10.500000 10.000000 -0.153001 10.25000 10.05000 HKLF 4 REM HYDROXYLGUGIAITE, Saga I quarry in P-42(1)m (113) out to 50 degrees theta REM R1 = 0.0278 for 342 Fo > 4sig(Fo) and 0.0299 for all 355 data REM 41 parameters refined using 2 restraints END WGHT 0.0207 0.4437 REM Instructions for potential hydrogen bonds HTAB O2 O3_$2 HTAB O2 O3_$3 REM Highest difference peak 0.562, deepest hole -0.427, 1-sigma level 0.085 Q1 1 0.2494 0.9023 0.4985 11.00000 0.05 0.56 Q2 1 0.4211 0.9211 0.4966 10.50000 0.05 0.34 Q3 1 0.3240 0.8240 0.6546 10.50000 0.05 0.28 Q4 1 0.4699 0.8659 0.3730 11.00000 0.05 0.25 Q5 1 0.1023 0.1029 0.4985 11.00000 0.05 0.24 Q6 1 0.1928 -0.0006 0.3682 11.00000 0.05 0.24 Q7 1 0.2773 0.2227 -0.3075 10.50000 0.05 0.22 Q8 1 0.1578 -0.0011 0.3820 11.00000 0.05 0.22 Q9 1 0.5962 0.0962 -0.2840 10.50000 0.05 0.19 Q10 1 0.4860 0.1719 -0.3906 11.00000 0.05 0.19 Q11 1 0.2581 0.0808 -0.3267 11.00000 0.05 0.18 Q12 1 0.3310 0.8310 0.2270 10.50000 0.05 0.18 Q13 1 0.3617 0.2427 0.0423 11.00000 0.05 0.18 Q14 1 0.3132 0.0585 0.0238 11.00000 0.05 0.18 Q15 1 0.1897 0.1401 0.0047 11.00000 0.05 0.18 Q16 1 0.0000 0.0000 0.2566 10.50000 0.05 0.17 Q17 1 0.1230 -0.0112 0.1975 11.00000 0.05 0.16 Q18 1 0.5855 0.0855 0.1629 10.50000 0.05 0.16 Q19 1 0.4133 0.1617 -0.1978 11.00000 0.05 0.16 Q20 1 0.3800 0.1200 -0.0625 10.50000 0.05 0.16 ; _shelx_res_checksum 52717 _shelx_hkl_file ; 0 -1 0 50.18 5.86 -1 0 0 48.04 3.08 1 0 0 44.31 3.79 0 1 0 39.02 2.20 -1 -1 0 125.37 7.23 -1 1 0 100.41 4.72 1 1 0 109.90 5.76 -2 -1 0 340.91 15.26 2 1 0 306.63 10.90 -1 2 0 284.86 7.81 0 -2 0 8.62 4.73 -2 0 0 8.74 5.34 2 0 0 14.30 6.61 0 2 0 9.06 4.07 -1 -2 0 304.24 12.33 2 -1 0 264.20 13.62 -2 1 0 272.83 8.34 1 2 0 292.70 14.58 -2 -2 0 2541.68 63.10 2 -2 0 2391.28 81.88 -2 2 0 2333.21 43.51 2 2 0 2571.79 56.46 -3 -2 0 77.96 6.83 3 2 0 70.75 5.48 -2 3 0 70.26 4.15 -3 -1 0 3776.80 75.13 3 1 0 3692.05 74.91 -1 3 0 3392.88 55.08 0 -3 0 69.87 5.50 -3 0 0 88.14 5.71 3 0 0 75.44 6.12 0 3 0 73.53 4.81 -1 -3 0 3343.65 86.76 3 -1 0 3342.85 87.85 -3 1 0 3436.41 69.41 1 3 0 3481.38 94.33 -2 -3 0 66.11 6.25 3 -2 0 71.29 7.09 -3 2 0 70.54 4.93 2 3 0 77.00 8.06 -3 -3 0 9794.56 236.15 3 -3 0 8915.73 306.98 -3 3 0 8996.88 162.99 3 3 0 9999.00 211.44 3 -4 0 265.70 22.55 -4 -3 0 345.96 14.59 4 3 0 353.60 16.46 -3 4 0 293.39 11.26 -4 -2 0 4709.71 113.73 4 2 0 4785.14 114.97 -2 4 0 4258.79 69.28 1 -4 0 2349.32 76.52 -4 -1 0 2662.05 53.81 4 1 0 2577.91 53.58 -1 4 0 2303.80 52.02 0 -4 0 8209.43 273.15 -4 0 0 8965.66 182.42 4 0 0 8959.32 181.77 0 4 0 8585.81 196.15 -1 -4 0 2327.09 61.76 4 -1 0 2376.77 62.76 -4 1 0 2373.87 58.28 1 4 0 2362.44 67.42 -2 -4 0 4373.16 109.18 4 -2 0 4076.15 110.46 -4 2 0 4231.39 79.66 2 4 0 4458.82 118.63 -3 -4 0 341.02 16.09 4 -3 0 271.59 17.11 -4 3 0 310.94 13.21 3 4 0 345.30 18.38 -4 -4 0 9821.27 207.46 4 -4 0 8774.27 208.94 -4 4 0 9047.63 172.60 4 4 0 9730.78 304.57 4 -5 0 348.51 17.97 -5 -4 0 412.54 16.99 5 4 0 410.86 26.18 -4 5 0 349.13 14.41 3 -5 0 864.48 58.98 -5 -3 0 1034.27 26.70 5 3 0 1000.49 30.59 -3 5 0 918.90 18.90 2 -5 0 877.16 38.32 -5 -2 0 1067.12 30.95 5 2 0 1086.74 31.52 -2 5 0 979.87 20.17 1 -5 0 41.81 7.57 -5 -1 0 56.72 7.04 5 1 0 48.86 6.44 -1 5 0 43.01 7.52 0 -5 0 19.06 6.91 -5 0 0 27.67 7.27 5 0 0 26.97 5.83 0 5 0 24.01 6.69 -1 -5 0 42.97 7.34 5 -1 0 48.95 8.28 -5 1 0 47.56 7.62 1 5 0 30.28 8.96 -2 -5 0 1000.95 38.31 5 -2 0 931.80 30.69 -5 2 0 915.96 28.10 2 5 0 988.61 32.90 -3 -5 0 980.47 29.64 5 -3 0 868.15 31.06 -5 3 0 900.95 28.13 3 5 0 984.97 33.08 -4 -5 0 405.85 21.53 5 -4 0 331.55 20.78 -5 4 0 354.24 18.25 4 5 0 423.55 26.78 -5 -5 0 3.55 10.16 5 -5 0 5.07 11.82 -5 5 0 1.82 8.97 5 5 0 7.09 12.55 5 -6 0 330.19 26.49 -6 -5 0 351.35 24.85 6 5 0 353.49 26.58 -5 6 0 321.73 19.30 4 -6 0 274.94 16.08 -6 -4 0 318.73 18.20 6 4 0 292.35 24.61 -4 6 0 263.50 13.97 3 -6 0 183.36 15.10 -6 -3 0 206.44 16.52 6 3 0 185.72 16.43 -3 6 0 177.92 9.04 2 -6 0 409.62 20.66 -6 -2 0 472.62 20.88 6 2 0 468.12 16.79 -2 6 0 437.75 16.24 1 -6 0 201.38 19.15 -6 -1 0 231.34 21.44 6 1 0 245.90 11.54 -1 6 0 208.39 14.13 0 -6 0 8911.35 291.42 -6 0 0 9692.38 218.79 6 0 0 9356.25 193.61 0 6 0 8910.94 252.59 -1 -6 0 162.56 18.52 6 -1 0 200.38 16.77 -6 1 0 210.61 15.03 1 6 0 216.75 19.30 -2 -6 0 458.43 26.87 6 -2 0 413.15 26.68 -6 2 0 404.75 19.13 2 6 0 442.61 22.99 -3 -6 0 198.54 17.51 6 -3 0 190.01 19.15 -6 3 0 178.74 13.11 3 6 0 217.96 18.81 -4 -6 0 308.95 21.33 6 -4 0 255.03 24.51 -6 4 0 240.85 17.49 4 6 0 289.12 25.26 -5 -6 0 356.73 22.11 6 -5 0 303.55 26.81 -6 5 0 292.64 18.96 5 6 0 356.16 26.90 -6 -6 0 1301.16 49.93 6 -6 0 1204.39 38.61 -6 6 0 1236.13 46.46 6 6 0 1339.17 52.31 6 -7 0 21.63 13.69 -7 -6 0 24.94 20.62 7 6 0 30.27 15.09 -6 7 0 12.35 22.67 5 -7 0 -0.69 10.87 -7 -5 0 26.76 18.58 7 5 0 25.05 14.39 -5 7 0 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