data_chiavmad _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H1.50 Be2 Ca Mn O17 Si5' _chemical_formula_weight 527.00 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' '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' 'Mn' 'Mn' 0.3368 0.7283 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7597(17) _cell_length_b 4.8933(10) _cell_length_c 31.245(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.46(3) _cell_angle_gamma 90.00 _cell_volume 1339.2(5) _cell_formula_units_Z 4 _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 2.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 1.918 _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 15651 _diffrn_reflns_av_R_equivalents 0.0122 _diffrn_reflns_av_sigmaI/netI 0.0109 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 30.08 _reflns_number_total 3932 _reflns_number_gt 3813 _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^)+(0.0350P)^2^+0.9556P] 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 SHELXL _refine_ls_extinction_coef 0.0001(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3932 _refine_ls_number_parameters 268 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0665 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.007 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.5000 0.0000 0.00976(11) Uani 0.968(2) 2 d SP . . Mn2 Mn 1.0000 0.5000 0.0000 0.01231(12) Uani 0.951(2) 2 d SP . . Ca Ca 0.75169(4) 0.50390(6) -0.089778(9) 0.01610(8) Uani 1 1 d . . . Si1 Si 0.74954(4) 0.00264(8) -0.002053(11) 0.00954(9) Uani 1 1 d . . . Si2 Si 0.41513(4) 0.59846(8) -0.232824(12) 0.01118(9) Uani 1 1 d . . . Si22 Si 0.08496(4) 0.37443(8) -0.232419(12) 0.01145(8) Uani 1 1 d . . . Si3 Si 0.14250(4) 0.21647(8) -0.134619(12) 0.01053(8) Uani 1 1 d . . . Si33 Si 0.35512(4) 0.71149(8) -0.135372(12) 0.01007(8) Uani 1 1 d . . . Be4 Be 0.5019(2) 0.0738(4) 0.05735(6) 0.0167(5) Uani 0.963(3) 1 d P . . Si4 Si 0.5019(2) 0.0738(4) 0.05735(6) 0.0167(5) Uani 0.037(3) 1 d P . . Be44 Be 1.00209(18) 0.9206(4) 0.05733(5) 0.0144(5) Uani 0.942(3) 1 d P . . Si44 Si 1.00209(18) 0.9206(4) 0.05733(5) 0.0144(5) Uani 0.058(3) 1 d P . . O1 O 0.65135(11) -0.2031(2) -0.03328(3) 0.01127(18) Uani 1 1 d . . . O2 O 0.84665(11) 0.2094(2) -0.03297(3) 0.01134(18) Uani 1 1 d . . . O3 O 0.86115(12) -0.1858(2) 0.02723(3) 0.0155(2) Uani 1 1 d . . . O4 O 0.63977(12) 0.1925(2) 0.02731(3) 0.0154(2) Uani 1 1 d . . . O5 O 0.24879(14) 0.4911(3) -0.24838(4) 0.0224(3) Uani 1 1 d . . . O6 O 0.46271(14) 0.8455(2) -0.26519(4) 0.0205(2) Uani 1 1 d . . . O7 O 0.41567(15) 0.7089(3) -0.18386(4) 0.0232(3) Uani 1 1 d . . . O8 O 0.04463(15) 0.1134(3) -0.26298(4) 0.0231(2) Uani 1 1 d . . . O9 O 0.08696(15) 0.2857(3) -0.18246(4) 0.0265(3) Uani 1 1 d . . . O10 O 0.99914(12) 0.7641(2) 0.10273(3) 0.0156(2) Uani 1 1 d . . . O11 O 0.20918(14) 0.9086(3) -0.13204(5) 0.0257(3) Uani 1 1 d . . . O12 O 0.28786(13) 0.4126(2) -0.12193(4) 0.0193(2) Uani 1 1 d . . . O13 O 0.49540(12) 0.7972(2) -0.10492(3) 0.0154(2) Uani 1 1 d . . . OH14 O 0.49151(13) 0.7391(2) 0.05677(4) 0.0179(2) Uani 1 1 d D . . OH15 O 0.01611(13) 0.2502(2) 0.05846(4) 0.0177(2) Uani 1 1 d D . . OW16 O 0.83368(17) 0.7389(3) -0.15162(4) 0.0286(3) Uani 1 1 d D . . OW17 O 0.65242(15) 0.2242(3) -0.14642(4) 0.0236(2) Uani 1 1 d D . . H14 H 0.560(3) 0.662(6) 0.0785(7) 0.052(9) Uiso 1 1 d D . . H15 H -0.041(4) 0.339(8) 0.0814(9) 0.087(13) Uiso 1 1 d D . . H16A H 0.791(5) 0.895(7) -0.1673(15) 0.121(18) Uiso 1 1 d D . . H16B H 0.864(5) 0.650(8) -0.1783(8) 0.095(14) Uiso 1 1 d D . . H17A H 0.625(5) 0.307(9) -0.1740(7) 0.101(15) Uiso 1 1 d D . . H17B H 0.587(3) 0.081(5) -0.1344(10) 0.060(10) Uiso 1 1 d D . . 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 Mn1 0.01263(16) 0.00760(16) 0.00906(16) 0.00008(9) 0.00139(10) 0.00017(10) Mn2 0.01453(18) 0.00952(17) 0.01282(17) -0.00140(10) -0.00357(11) -0.00026(10) Ca 0.02173(15) 0.01461(15) 0.01194(13) -0.00095(10) -0.00106(11) 0.00163(10) Si1 0.00803(17) 0.01187(19) 0.00871(17) -0.00074(12) 0.00013(13) -0.00158(12) Si2 0.01189(17) 0.01173(18) 0.00993(17) -0.00052(13) 0.00139(13) -0.00109(13) Si22 0.01207(17) 0.01218(17) 0.01008(17) 0.00050(13) -0.00113(13) -0.00093(13) Si3 0.01077(16) 0.01127(17) 0.00955(16) 0.00020(12) -0.00014(12) -0.00011(13) Si33 0.01065(16) 0.01074(17) 0.00881(16) -0.00089(12) -0.00019(12) -0.00093(12) Be4 0.0184(9) 0.0165(9) 0.0151(9) -0.0008(6) -0.0009(6) -0.0018(6) Si4 0.0184(9) 0.0165(9) 0.0151(9) -0.0008(6) -0.0009(6) -0.0018(6) Be44 0.0138(8) 0.0165(8) 0.0130(8) -0.0001(5) 0.0006(5) -0.0011(5) Si44 0.0138(8) 0.0165(8) 0.0130(8) -0.0001(5) 0.0006(5) -0.0011(5) O1 0.0108(4) 0.0123(4) 0.0108(4) -0.0015(3) -0.0010(3) -0.0017(3) O2 0.0105(4) 0.0129(4) 0.0106(4) 0.0003(3) 0.0009(3) -0.0019(3) O3 0.0136(5) 0.0199(5) 0.0129(5) 0.0043(4) -0.0037(4) -0.0041(4) O4 0.0139(5) 0.0189(5) 0.0136(5) -0.0051(4) 0.0043(4) -0.0049(4) O5 0.0173(5) 0.0286(7) 0.0213(6) -0.0008(5) 0.0000(4) -0.0079(4) O6 0.0233(6) 0.0172(5) 0.0211(5) 0.0017(4) -0.0001(4) -0.0050(4) O7 0.0255(6) 0.0342(7) 0.0099(5) -0.0036(4) 0.0019(4) -0.0063(5) O8 0.0229(6) 0.0203(6) 0.0260(6) -0.0046(5) 0.0016(5) -0.0057(5) O9 0.0268(6) 0.0419(8) 0.0107(5) 0.0057(5) -0.0025(4) -0.0037(6) O10 0.0142(5) 0.0204(5) 0.0122(5) 0.0017(4) 0.0024(4) 0.0034(4) O11 0.0178(5) 0.0153(5) 0.0439(8) -0.0033(5) 0.0017(5) 0.0037(4) O12 0.0193(5) 0.0146(5) 0.0239(6) 0.0046(4) -0.0058(4) -0.0058(4) O13 0.0154(5) 0.0210(5) 0.0098(4) -0.0025(4) -0.0011(4) -0.0055(4) OH14 0.0201(5) 0.0143(5) 0.0192(5) 0.0050(4) -0.0089(4) -0.0022(4) OH15 0.0186(5) 0.0163(5) 0.0184(5) -0.0058(4) 0.0056(4) -0.0009(4) OW16 0.0374(7) 0.0244(6) 0.0242(6) 0.0058(5) 0.0105(5) 0.0040(6) OW17 0.0268(6) 0.0232(6) 0.0209(6) -0.0009(5) -0.0031(5) -0.0061(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 Mn1 O4 2.1152(12) . ? Mn1 O4 2.1153(12) 3_665 ? Mn1 OH14 2.1267(12) . ? Mn1 OH14 2.1268(12) 3_665 ? Mn1 O1 2.2296(11) 3_655 ? Mn1 O1 2.2296(11) 1_565 ? Mn1 Si4 2.7494(19) 3_665 ? Mn1 Be4 2.7494(19) 3_665 ? Mn1 Be4 2.7495(19) . ? Mn1 Ca 3.5816(11) 3_665 ? Mn1 Ca 3.5817(11) . ? Mn2 O3 2.1410(12) 3_755 ? Mn2 O3 2.1410(12) 1_565 ? Mn2 OH15 2.2014(13) 3_665 ? Mn2 OH15 2.2014(12) 1_655 ? Mn2 O2 2.2057(11) . ? Mn2 O2 2.2057(11) 3_765 ? Mn2 Be44 2.7285(17) . ? Mn2 Si44 2.7285(17) 3_765 ? Mn2 Be44 2.7285(17) 3_765 ? Mn2 Ca 3.5359(11) 3_765 ? Mn2 Ca 3.5360(11) . ? Ca OW16 2.3650(14) . ? Ca OW17 2.3952(14) . ? Ca O2 2.4281(12) . ? Ca O1 2.4430(12) 1_565 ? Ca OH15 2.5518(13) 3_665 ? Ca O10 2.5810(12) 3_765 ? Ca OH14 2.6552(13) 3_665 ? Ca O13 2.7031(13) . ? Ca Si44 3.1559(18) 3_765 ? Ca Be44 3.1559(18) 3_765 ? Ca Be4 3.204(2) 3_665 ? Ca Si4 3.204(2) 3_665 ? Si1 O3 1.6214(12) . ? Si1 O4 1.6259(12) . ? Si1 O1 1.6408(11) . ? Si1 O2 1.6412(11) . ? Si1 Si4 2.813(2) 3_655 ? Si1 Si44 2.8139(18) 3_765 ? Si2 O5 1.6198(13) . ? Si2 O7 1.6224(12) . ? Si2 O6 1.6322(13) . ? Si2 O6 1.6378(13) 2_644 ? Si22 O9 1.6203(13) . ? Si22 O5 1.6265(13) . ? Si22 O8 1.6320(13) . ? Si22 O8 1.6351(13) 2_554 ? Si3 O10 1.6003(12) 3_665 ? Si3 O9 1.6044(13) . ? Si3 O11 1.6176(13) 1_545 ? Si3 O12 1.6405(12) . ? Si3 Si44 2.8167(17) 3_665 ? Si33 O13 1.6039(12) . ? Si33 O11 1.6054(13) . ? Si33 O7 1.6093(13) . ? Si33 O12 1.6330(12) . ? Be4 O13 1.615(2) 3_665 ? Be4 OH14 1.641(2) 1_545 ? Be4 O4 1.642(2) . ? Be4 O1 1.659(2) 3_655 ? Be4 Ca 3.204(2) 3_665 ? Be44 O10 1.6124(19) . ? Be44 OH15 1.618(2) 1_665 ? Be44 O3 1.6314(19) 1_565 ? Be44 O2 1.6601(19) 3_765 ? Be44 Ca 3.1558(18) 3_765 ? O1 Si4 1.659(2) 3_655 ? O1 Be4 1.659(2) 3_655 ? O1 Mn1 2.2295(11) 1_545 ? O1 Ca 2.4430(12) 1_545 ? O2 Si44 1.6601(19) 3_765 ? O2 Be44 1.6601(19) 3_765 ? O3 Si44 1.6313(19) 1_545 ? O3 Be44 1.6313(19) 1_545 ? O3 Mn2 2.1410(12) 1_545 ? O6 Si2 1.6378(13) 2_654 ? O8 Si22 1.6351(13) 2_544 ? O10 Si3 1.6002(12) 3_665 ? O10 Ca 2.5810(12) 3_765 ? O11 Si3 1.6176(13) 1_565 ? O13 Si4 1.615(2) 3_665 ? O13 Be4 1.615(2) 3_665 ? OH14 Si4 1.641(2) 1_565 ? OH14 Be4 1.641(2) 1_565 ? OH14 Ca 2.6552(13) 3_665 ? OH14 H14 0.979(2) . ? OH15 Si44 1.618(2) 1_445 ? OH15 Be44 1.618(2) 1_445 ? OH15 Mn2 2.2014(13) 1_455 ? OH15 Ca 2.5517(13) 3_665 ? OH15 H15 0.980(2) . ? OW16 H16A 0.979(2) . ? OW16 H16B 0.979(2) . ? OW17 H17A 0.979(2) . ? OW17 H17B 0.979(2) . ? 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 O4 Mn1 O4 180.0 . 3_665 ? O4 Mn1 OH14 94.52(4) . . ? O4 Mn1 OH14 85.48(4) 3_665 . ? O4 Mn1 OH14 85.48(4) . 3_665 ? O4 Mn1 OH14 94.51(4) 3_665 3_665 ? OH14 Mn1 OH14 180.0 . 3_665 ? O4 Mn1 O1 72.11(4) . 3_655 ? O4 Mn1 O1 107.89(4) 3_665 3_655 ? OH14 Mn1 O1 86.82(4) . 3_655 ? OH14 Mn1 O1 93.18(4) 3_665 3_655 ? O4 Mn1 O1 107.89(4) . 1_565 ? O4 Mn1 O1 72.11(4) 3_665 1_565 ? OH14 Mn1 O1 93.18(4) . 1_565 ? OH14 Mn1 O1 86.82(4) 3_665 1_565 ? O1 Mn1 O1 180.00(6) 3_655 1_565 ? O4 Mn1 Si4 143.40(5) . 3_665 ? O4 Mn1 Si4 36.60(5) 3_665 3_665 ? OH14 Mn1 Si4 97.25(5) . 3_665 ? OH14 Mn1 Si4 82.75(5) 3_665 3_665 ? O1 Mn1 Si4 142.91(5) 3_655 3_665 ? O1 Mn1 Si4 37.09(5) 1_565 3_665 ? O4 Mn1 Be4 143.40(5) . 3_665 ? O4 Mn1 Be4 36.60(5) 3_665 3_665 ? OH14 Mn1 Be4 97.25(5) . 3_665 ? OH14 Mn1 Be4 82.75(5) 3_665 3_665 ? O1 Mn1 Be4 142.91(5) 3_655 3_665 ? O1 Mn1 Be4 37.09(5) 1_565 3_665 ? Si4 Mn1 Be4 0.00(9) 3_665 3_665 ? O4 Mn1 Be4 36.60(5) . . ? O4 Mn1 Be4 143.40(5) 3_665 . ? OH14 Mn1 Be4 82.75(5) . . ? OH14 Mn1 Be4 97.26(5) 3_665 . ? O1 Mn1 Be4 37.09(5) 3_655 . ? O1 Mn1 Be4 142.91(5) 1_565 . ? Si4 Mn1 Be4 180.0 3_665 . ? Be4 Mn1 Be4 180.0 3_665 . ? O4 Mn1 Ca 92.19(3) . 3_665 ? O4 Mn1 Ca 87.81(3) 3_665 3_665 ? OH14 Mn1 Ca 47.46(3) . 3_665 ? OH14 Mn1 Ca 132.54(3) 3_665 3_665 ? O1 Mn1 Ca 42.20(3) 3_655 3_665 ? O1 Mn1 Ca 137.80(3) 1_565 3_665 ? Si4 Mn1 Ca 120.93(4) 3_665 3_665 ? Be4 Mn1 Ca 120.93(4) 3_665 3_665 ? Be4 Mn1 Ca 59.07(4) . 3_665 ? O4 Mn1 Ca 87.81(3) . . ? O4 Mn1 Ca 92.19(3) 3_665 . ? OH14 Mn1 Ca 132.55(3) . . ? OH14 Mn1 Ca 47.45(3) 3_665 . ? O1 Mn1 Ca 137.80(3) 3_655 . ? O1 Mn1 Ca 42.20(3) 1_565 . ? Si4 Mn1 Ca 59.07(4) 3_665 . ? Be4 Mn1 Ca 59.07(4) 3_665 . ? Be4 Mn1 Ca 120.93(4) . . ? Ca Mn1 Ca 180.0 3_665 . ? O3 Mn2 O3 180.00(7) 3_755 1_565 ? O3 Mn2 OH15 95.85(4) 3_755 3_665 ? O3 Mn2 OH15 84.15(4) 1_565 3_665 ? O3 Mn2 OH15 84.15(4) 3_755 1_655 ? O3 Mn2 OH15 95.85(4) 1_565 1_655 ? OH15 Mn2 OH15 180.00(6) 3_665 1_655 ? O3 Mn2 O2 72.38(4) 3_755 . ? O3 Mn2 O2 107.62(4) 1_565 . ? OH15 Mn2 O2 86.32(4) 3_665 . ? OH15 Mn2 O2 93.68(4) 1_655 . ? O3 Mn2 O2 107.62(4) 3_755 3_765 ? O3 Mn2 O2 72.38(4) 1_565 3_765 ? OH15 Mn2 O2 93.68(4) 3_665 3_765 ? OH15 Mn2 O2 86.32(4) 1_655 3_765 ? O2 Mn2 O2 180.0 . 3_765 ? O3 Mn2 Be44 143.30(4) 3_755 . ? O3 Mn2 Be44 36.70(4) 1_565 . ? OH15 Mn2 Be44 97.23(5) 3_665 . ? OH15 Mn2 Be44 82.77(5) 1_655 . ? O2 Mn2 Be44 142.54(4) . . ? O2 Mn2 Be44 37.46(4) 3_765 . ? O3 Mn2 Si44 36.70(4) 3_755 3_765 ? O3 Mn2 Si44 143.30(4) 1_565 3_765 ? OH15 Mn2 Si44 82.77(5) 3_665 3_765 ? OH15 Mn2 Si44 97.23(5) 1_655 3_765 ? O2 Mn2 Si44 37.46(4) . 3_765 ? O2 Mn2 Si44 142.54(4) 3_765 3_765 ? Be44 Mn2 Si44 179.999(1) . 3_765 ? O3 Mn2 Be44 36.70(4) 3_755 3_765 ? O3 Mn2 Be44 143.30(4) 1_565 3_765 ? OH15 Mn2 Be44 82.77(5) 3_665 3_765 ? OH15 Mn2 Be44 97.23(5) 1_655 3_765 ? O2 Mn2 Be44 37.46(4) . 3_765 ? O2 Mn2 Be44 142.54(4) 3_765 3_765 ? Be44 Mn2 Be44 179.999(1) . 3_765 ? Si44 Mn2 Be44 0.00(8) 3_765 3_765 ? O3 Mn2 Ca 87.91(3) 3_755 3_765 ? O3 Mn2 Ca 92.09(3) 1_565 3_765 ? OH15 Mn2 Ca 134.12(3) 3_665 3_765 ? OH15 Mn2 Ca 45.88(3) 1_655 3_765 ? O2 Mn2 Ca 137.35(3) . 3_765 ? O2 Mn2 Ca 42.65(3) 3_765 3_765 ? Be44 Mn2 Ca 58.83(4) . 3_765 ? Si44 Mn2 Ca 121.17(4) 3_765 3_765 ? Be44 Mn2 Ca 121.17(4) 3_765 3_765 ? O3 Mn2 Ca 92.09(3) 3_755 . ? O3 Mn2 Ca 87.91(3) 1_565 . ? OH15 Mn2 Ca 45.88(3) 3_665 . ? OH15 Mn2 Ca 134.12(3) 1_655 . ? O2 Mn2 Ca 42.65(3) . . ? O2 Mn2 Ca 137.35(3) 3_765 . ? Be44 Mn2 Ca 121.17(4) . . ? Si44 Mn2 Ca 58.83(4) 3_765 . ? Be44 Mn2 Ca 58.83(4) 3_765 . ? Ca Mn2 Ca 180.0 3_765 . ? OW16 Ca OW17 77.58(5) . . ? OW16 Ca O2 141.38(5) . . ? OW17 Ca O2 108.74(5) . . ? OW16 Ca O1 114.73(5) . 1_565 ? OW17 Ca O1 137.61(4) . 1_565 ? O2 Ca O1 86.74(4) . 1_565 ? OW16 Ca OH15 80.66(5) . 3_665 ? OW17 Ca OH15 146.76(4) . 3_665 ? O2 Ca OH15 74.46(4) . 3_665 ? O1 Ca OH15 74.72(4) 1_565 3_665 ? OW16 Ca O10 81.73(5) . 3_765 ? OW17 Ca O10 84.05(5) . 3_765 ? O2 Ca O10 61.83(4) . 3_765 ? O1 Ca O10 136.13(4) 1_565 3_765 ? OH15 Ca O10 68.11(4) 3_665 3_765 ? OW16 Ca OH14 141.70(5) . 3_665 ? OW17 Ca OH14 75.13(5) . 3_665 ? O2 Ca OH14 73.84(4) . 3_665 ? O1 Ca OH14 71.81(4) 1_565 3_665 ? OH15 Ca OH14 134.57(4) 3_665 3_665 ? O10 Ca OH14 121.03(4) 3_765 3_665 ? OW16 Ca O13 81.72(5) . . ? OW17 Ca O13 82.99(5) . . ? O2 Ca O13 136.24(4) . . ? O1 Ca O13 60.78(4) 1_565 . ? OH15 Ca O13 118.37(4) 3_665 . ? O10 Ca O13 160.83(4) 3_765 . ? OH14 Ca O13 68.77(4) 3_665 . ? OW16 Ca Si44 111.79(5) . 3_765 ? OW17 Ca Si44 95.99(5) . 3_765 ? O2 Ca Si44 31.27(4) . 3_765 ? O1 Ca Si44 113.77(4) 1_565 3_765 ? OH15 Ca Si44 69.30(4) 3_665 3_765 ? O10 Ca Si44 30.60(4) 3_765 3_765 ? OH14 Ca Si44 97.41(4) 3_665 3_765 ? O13 Ca Si44 165.98(4) . 3_765 ? OW16 Ca Be44 111.79(5) . 3_765 ? OW17 Ca Be44 95.99(5) . 3_765 ? O2 Ca Be44 31.27(4) . 3_765 ? O1 Ca Be44 113.77(4) 1_565 3_765 ? OH15 Ca Be44 69.30(4) 3_665 3_765 ? O10 Ca Be44 30.60(4) 3_765 3_765 ? OH14 Ca Be44 97.41(4) 3_665 3_765 ? O13 Ca Be44 165.98(4) . 3_765 ? Si44 Ca Be44 0.00(7) 3_765 3_765 ? OW16 Ca Be4 99.24(5) . 3_665 ? OW17 Ca Be4 110.72(5) . 3_665 ? O2 Ca Be4 112.70(4) . 3_665 ? O1 Ca Be4 30.54(4) 1_565 3_665 ? OH15 Ca Be4 97.30(4) 3_665 3_665 ? O10 Ca Be4 165.12(4) 3_765 3_665 ? OH14 Ca Be4 66.77(4) 3_665 3_665 ? O13 Ca Be4 30.24(4) . 3_665 ? Si44 Ca Be4 142.81(5) 3_765 3_665 ? Be44 Ca Be4 142.81(5) 3_765 3_665 ? OW16 Ca Si4 99.24(5) . 3_665 ? OW17 Ca Si4 110.72(5) . 3_665 ? O2 Ca Si4 112.70(4) . 3_665 ? O1 Ca Si4 30.54(4) 1_565 3_665 ? OH15 Ca Si4 97.30(4) 3_665 3_665 ? O10 Ca Si4 165.12(4) 3_765 3_665 ? OH14 Ca Si4 66.77(4) 3_665 3_665 ? O13 Ca Si4 30.24(4) . 3_665 ? Si44 Ca Si4 142.81(5) 3_765 3_665 ? Be44 Ca Si4 142.81(5) 3_765 3_665 ? Be4 Ca Si4 0.00(9) 3_665 3_665 ? O3 Si1 O4 111.29(6) . . ? O3 Si1 O1 107.31(6) . . ? O4 Si1 O1 112.12(6) . . ? O3 Si1 O2 111.70(6) . . ? O4 Si1 O2 106.94(6) . . ? O1 Si1 O2 107.46(6) . . ? O3 Si1 Si4 137.44(6) . 3_655 ? O4 Si1 Si4 87.65(6) . 3_655 ? O1 Si1 Si4 31.69(5) . 3_655 ? O2 Si1 Si4 97.32(5) . 3_655 ? O3 Si1 Si44 87.51(5) . 3_765 ? O4 Si1 Si44 137.20(6) . 3_765 ? O1 Si1 Si44 96.96(5) . 3_765 ? O2 Si1 Si44 31.73(5) . 3_765 ? Si4 Si1 Si44 104.25(5) 3_655 3_765 ? O5 Si2 O7 112.75(7) . . ? O5 Si2 O6 106.73(7) . . ? O7 Si2 O6 109.80(7) . . ? O5 Si2 O6 109.27(7) . 2_644 ? O7 Si2 O6 106.89(7) . 2_644 ? O6 Si2 O6 111.48(4) . 2_644 ? O9 Si22 O5 112.74(7) . . ? O9 Si22 O8 110.76(8) . . ? O5 Si22 O8 106.43(7) . . ? O9 Si22 O8 106.18(7) . 2_554 ? O5 Si22 O8 109.61(7) . 2_554 ? O8 Si22 O8 111.18(4) . 2_554 ? O10 Si3 O9 109.68(7) 3_665 . ? O10 Si3 O11 107.81(7) 3_665 1_545 ? O9 Si3 O11 110.46(8) . 1_545 ? O10 Si3 O12 114.76(7) 3_665 . ? O9 Si3 O12 109.31(7) . . ? O11 Si3 O12 104.68(7) 1_545 . ? O10 Si3 Si44 28.86(5) 3_665 3_665 ? O9 Si3 Si44 135.55(6) . 3_665 ? O11 Si3 Si44 84.27(6) 1_545 3_665 ? O12 Si3 Si44 106.59(6) . 3_665 ? O13 Si33 O11 114.28(7) . . ? O13 Si33 O7 107.69(7) . . ? O11 Si33 O7 109.53(8) . . ? O13 Si33 O12 110.97(6) . . ? O11 Si33 O12 103.43(7) . . ? O7 Si33 O12 110.93(7) . . ? O13 Be4 OH14 113.62(12) 3_665 1_545 ? O13 Be4 O4 112.47(12) 3_665 . ? OH14 Be4 O4 112.82(12) 1_545 . ? O13 Be4 O1 105.92(12) 3_665 3_655 ? OH14 Be4 O1 109.37(12) 1_545 3_655 ? O4 Be4 O1 101.67(11) . 3_655 ? O13 Be4 Mn1 107.66(10) 3_665 . ? OH14 Be4 Mn1 138.61(10) 1_545 . ? O4 Be4 Mn1 50.18(7) . . ? O1 Be4 Mn1 54.17(6) 3_655 . ? O13 Be4 Ca 57.46(7) 3_665 3_665 ? OH14 Be4 Ca 127.52(10) 1_545 3_665 ? O4 Be4 Ca 117.88(10) . 3_665 ? O1 Be4 Ca 48.46(6) 3_655 3_665 ? Mn1 Be4 Ca 73.52(5) . 3_665 ? O10 Be44 OH15 117.14(11) . 1_665 ? O10 Be44 O3 109.77(11) . 1_565 ? OH15 Be44 O3 112.80(11) 1_665 1_565 ? O10 Be44 O2 103.88(11) . 3_765 ? OH15 Be44 O2 109.35(11) 1_665 3_765 ? O3 Be44 O2 102.50(10) 1_565 3_765 ? O10 Be44 Mn2 102.66(9) . . ? OH15 Be44 Mn2 140.02(9) 1_665 . ? O3 Be44 Mn2 51.66(6) 1_565 . ? O2 Be44 Mn2 53.92(6) 3_765 . ? O10 Be44 Ca 54.59(6) . 3_765 ? OH15 Be44 Ca 126.70(9) 1_665 3_765 ? O3 Be44 Ca 119.16(9) 1_565 3_765 ? O2 Be44 Ca 49.39(6) 3_765 3_765 ? Mn2 Be44 Ca 73.46(4) . 3_765 ? Si1 O1 Si4 116.99(9) . 3_655 ? Si1 O1 Be4 116.99(9) . 3_655 ? Si4 O1 Be4 0.00(16) 3_655 3_655 ? Si1 O1 Mn1 115.68(5) . 1_545 ? Si4 O1 Mn1 88.74(8) 3_655 1_545 ? Be4 O1 Mn1 88.74(8) 3_655 1_545 ? Si1 O1 Ca 126.86(6) . 1_545 ? Si4 O1 Ca 101.00(8) 3_655 1_545 ? Be4 O1 Ca 101.00(8) 3_655 1_545 ? Mn1 O1 Ca 99.98(4) 1_545 1_545 ? Si1 O2 Si44 116.93(9) . 3_765 ? Si1 O2 Be44 116.93(9) . 3_765 ? Si44 O2 Be44 0.00(11) 3_765 3_765 ? Si1 O2 Mn2 116.05(5) . . ? Si44 O2 Mn2 88.62(7) 3_765 . ? Be44 O2 Mn2 88.62(7) 3_765 . ? Si1 O2 Ca 128.31(6) . . ? Si44 O2 Ca 99.34(7) 3_765 . ? Be44 O2 Ca 99.34(7) 3_765 . ? Mn2 O2 Ca 99.36(4) . . ? Si1 O3 Si44 126.45(10) . 1_545 ? Si1 O3 Be44 126.45(10) . 1_545 ? Si44 O3 Be44 0.00(12) 1_545 1_545 ? Si1 O3 Mn2 121.74(6) . 1_545 ? Si44 O3 Mn2 91.64(8) 1_545 1_545 ? Be44 O3 Mn2 91.64(8) 1_545 1_545 ? Si1 O4 Be4 124.16(10) . . ? Si1 O4 Mn1 121.46(6) . . ? Be4 O4 Mn1 93.22(8) . . ? Si2 O5 Si22 144.65(9) . . ? Si2 O6 Si2 138.88(8) . 2_654 ? Si33 O7 Si2 153.11(9) . . ? Si22 O8 Si22 139.29(9) . 2_544 ? Si3 O9 Si22 162.75(10) . . ? Si3 O10 Be44 122.51(9) 3_665 . ? Si3 O10 Ca 142.06(6) 3_665 3_765 ? Be44 O10 Ca 94.81(8) . 3_765 ? Si33 O11 Si3 147.53(9) . 1_565 ? Si33 O12 Si3 137.96(8) . . ? Si33 O13 Si4 130.84(10) . 3_665 ? Si33 O13 Be4 130.84(10) . 3_665 ? Si4 O13 Be4 0.00(19) 3_665 3_665 ? Si33 O13 Ca 126.61(6) . . ? Si4 O13 Ca 92.30(8) 3_665 . ? Be4 O13 Ca 92.30(8) 3_665 . ? Si4 OH14 Be4 0.00(12) 1_565 1_565 ? Si4 OH14 Mn1 123.78(9) 1_565 . ? Be4 OH14 Mn1 123.78(9) 1_565 . ? Si4 OH14 Ca 119.16(9) 1_565 3_665 ? Be4 OH14 Ca 119.16(9) 1_565 3_665 ? Mn1 OH14 Ca 96.38(5) . 3_665 ? Si4 OH14 H14 110.1(19) 1_565 . ? Be4 OH14 H14 110.1(19) 1_565 . ? Mn1 OH14 H14 109.9(19) . . ? Ca OH14 H14 92.8(19) 3_665 . ? Si44 OH15 Be44 0.00(16) 1_445 1_445 ? Si44 OH15 Mn2 122.09(8) 1_445 1_455 ? Be44 OH15 Mn2 122.09(8) 1_445 1_455 ? Si44 OH15 Ca 122.58(9) 1_445 3_665 ? Be44 OH15 Ca 122.58(9) 1_445 3_665 ? Mn2 OH15 Ca 95.85(5) 1_455 3_665 ? Si44 OH15 H15 115(2) 1_445 . ? Be44 OH15 H15 115(2) 1_445 . ? Mn2 OH15 H15 109(2) 1_455 . ? Ca OH15 H15 86(2) 3_665 . ? Ca OW16 H16A 132(3) . . ? Ca OW16 H16B 124(3) . . ? H16A OW16 H16B 91(4) . . ? Ca OW17 H17A 120(3) . . ? Ca OW17 H17B 109(2) . . ? H17A OW17 H17B 120(3) . . ? 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 OH14 H14 O12 0.979(2) 1.928(7) 2.8928(17) 168(3) 3_665 OH15 H15 O10 0.980(2) 2.21(3) 2.8744(17) 124(3) 1_455 OW16 H16A OW17 0.979(2) 2.12(4) 2.862(2) 131(4) 1_565 OW16 H16B O8 0.979(2) 2.016(17) 2.946(2) 158(4) 2_654 OW17 H17B O13 0.979(2) 1.855(7) 2.8227(18) 169(3) 1_545 OW17 H17A O6 0.979(2) 2.054(16) 2.9920(19) 160(4) 2_644 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.506 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.114