data_chivn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H0.38 Be2 Ca Mn O17 Si5' _chemical_formula_weight 525.87 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 8.7603(7) _cell_length_b 4.8727(2) _cell_length_c 31.2860(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.250(6) _cell_angle_gamma 90.00 _cell_volume 1335.47(13) _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 2.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1038 _exptl_absorpt_coefficient_mu 1.923 _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 15529 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0311 _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 1.95 _diffrn_reflns_theta_max 30.06 _reflns_number_total 3913 _reflns_number_gt 3528 _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^)+(0.0456P)^2^+9.8907P] 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 3913 _refine_ls_number_parameters 259 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.081 _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_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 0.0094(4) Uani 0.983(6) 2 d SP . . Mn2 Mn 1.0000 0.5000 0.0000 0.0104(4) Uani 0.982(7) 2 d SP . . Ca3 Ca 0.75315(18) 0.5031(2) -0.08999(3) 0.01517(18) Uani 1 1 d . . . Si1 Si 0.7502(2) 0.0026(3) -0.00246(3) 0.0090(2) Uani 1 1 d . . . Si2 Si 0.41480(18) 0.6004(3) -0.23286(5) 0.0117(3) Uani 1 1 d . . . Si22 Si 0.08571(18) 0.3648(3) -0.23248(5) 0.0121(3) Uani 1 1 d . . . Si3 Si 0.14155(17) 0.2140(3) -0.13453(4) 0.0087(3) Uani 1 1 d . . . Si33 Si 0.35391(18) 0.7099(3) -0.13543(4) 0.0097(3) Uani 1 1 d . . . Be1 Be 0.5028(8) 0.0746(13) 0.0576(2) 0.0106(11) Uani 1 1 d . . . Be11 Be 0.9996(9) 0.9172(13) 0.0571(2) 0.0106(11) Uani 1 1 d . . . O1 O 0.6511(4) -0.2030(8) -0.03349(11) 0.0102(7) Uani 1 1 d . . . O2 O 0.8458(4) 0.2106(8) -0.03294(12) 0.0103(7) Uani 1 1 d . . . O3 O 0.8606(5) -0.1900(9) 0.02681(12) 0.0153(8) Uani 1 1 d . . . O4 O 0.6393(5) 0.1944(9) 0.02659(12) 0.0157(8) Uani 1 1 d . . . O5 O 0.2482(7) 0.4858(10) -0.24854(11) 0.0244(8) Uani 1 1 d . . . O6 O 0.4590(5) 0.8501(9) -0.26566(15) 0.0236(9) Uani 1 1 d . . . O7 O 0.4135(6) 0.7127(9) -0.18376(13) 0.0213(9) Uani 1 1 d . . . O8 O 0.0485(5) 0.0987(9) -0.26258(16) 0.0257(10) Uani 1 1 d . . . O9 O 0.0866(6) 0.2800(10) -0.18225(14) 0.0263(10) Uani 1 1 d . . . O10 O 0.9986(5) 0.7613(7) 0.10251(12) 0.0126(7) Uani 1 1 d . . . O11 O 0.2063(5) 0.9018(8) -0.13132(15) 0.0230(8) Uani 1 1 d . . . O12 O 0.2883(4) 0.4092(8) -0.12185(12) 0.0170(8) Uani 1 1 d . . . O13 O 0.4925(5) 0.7990(8) -0.10485(12) 0.0162(8) Uani 1 1 d . . . OH14 O 0.4945(6) 0.7357(7) 0.05609(13) 0.0164(8) Uani 1 1 d D . . OH15 O 0.0154(5) 0.2540(8) 0.05759(14) 0.0168(8) Uani 1 1 d D . . OW16 O 0.8338(7) 0.7381(9) -0.15211(16) 0.0294(12) Uani 1 1 d D . . OW17 O 0.6501(6) 0.2233(9) -0.14605(15) 0.0232(9) Uani 1 1 d D . . H14 H 0.561(9) 0.662(18) 0.079(2) 0.050 Uiso 1 1 d D . . H15 H -0.056(8) 0.28(2) 0.081(2) 0.050 Uiso 1 1 d D . . H16A H 0.852(11) 0.935(4) -0.149(3) 0.050 Uiso 1 1 d D . . H16B H 0.884(9) 0.688(19) -0.1789(15) 0.050 Uiso 1 1 d D . . H17A H 0.695(10) 0.309(18) -0.1714(18) 0.050 Uiso 1 1 d D . . H17B H 0.560(6) 0.110(17) -0.141(3) 0.050 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 0.0160(6) 0.0049(5) 0.0074(5) 0.0000(3) 0.0006(5) -0.0006(4) Mn2 0.0166(7) 0.0050(5) 0.0095(6) -0.0013(3) -0.0035(5) -0.0006(4) Ca3 0.0233(4) 0.0101(4) 0.0122(3) -0.0013(4) -0.0015(5) 0.0018(4) Si1 0.0110(4) 0.0087(5) 0.0074(4) -0.0004(5) -0.0005(7) -0.0031(5) Si2 0.0152(7) 0.0093(6) 0.0106(6) -0.0007(5) 0.0026(6) -0.0010(5) Si22 0.0175(7) 0.0094(6) 0.0094(6) 0.0012(5) -0.0022(6) -0.0017(5) Si3 0.0105(6) 0.0088(5) 0.0069(6) 0.0003(4) -0.0002(5) 0.0002(5) Si33 0.0152(7) 0.0068(5) 0.0073(6) -0.0007(4) -0.0008(5) -0.0020(5) Be1 0.015(3) 0.007(2) 0.009(3) -0.001(2) -0.002(2) -0.004(2) Be11 0.015(3) 0.007(2) 0.009(3) -0.001(2) -0.002(2) -0.004(2) O1 0.0140(18) 0.0101(14) 0.0066(15) -0.0017(12) -0.0007(14) -0.0005(14) O2 0.0119(17) 0.0084(14) 0.0105(16) 0.0004(12) 0.0020(14) -0.0001(14) O3 0.0168(19) 0.0161(17) 0.0131(17) 0.0055(14) -0.0039(16) -0.0054(16) O4 0.0186(19) 0.0166(17) 0.0119(17) -0.0062(14) 0.0056(16) -0.0082(16) O5 0.0241(17) 0.028(2) 0.0212(16) -0.0012(18) 0.001(2) -0.0079(16) O6 0.032(2) 0.0156(18) 0.023(2) -0.0001(16) 0.0020(18) -0.0078(17) O7 0.026(2) 0.029(2) 0.0093(18) -0.0026(15) 0.0023(17) -0.0052(19) O8 0.027(2) 0.019(2) 0.031(2) -0.0042(18) -0.0003(19) -0.0088(17) O9 0.030(3) 0.039(3) 0.0093(19) 0.0092(17) -0.0020(18) -0.005(2) O10 0.0116(17) 0.0156(17) 0.0105(17) 0.0028(13) 0.0002(14) 0.0047(14) O11 0.0160(18) 0.0147(17) 0.038(2) -0.0029(17) 0.0035(17) 0.0038(14) O12 0.0172(19) 0.0123(17) 0.0215(18) 0.0024(14) -0.0040(14) -0.0054(14) O13 0.023(2) 0.0183(17) 0.0070(16) -0.0021(13) -0.0015(15) -0.0081(17) OH14 0.022(2) 0.0098(17) 0.017(2) 0.0066(13) -0.0091(17) -0.0035(15) OH15 0.018(2) 0.0118(17) 0.020(2) -0.0057(14) 0.0066(17) -0.0018(14) OW16 0.049(3) 0.020(2) 0.020(2) 0.0047(16) 0.005(2) 0.002(2) OW17 0.023(2) 0.021(2) 0.026(2) -0.0014(16) -0.0022(18) -0.0099(18) _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 2.095(5) 3_665 ? Mn1 O4 2.095(5) . ? Mn1 OH14 2.098(4) . ? Mn1 OH14 2.098(4) 3_665 ? Mn1 O1 2.226(4) 3_655 ? Mn1 O1 2.226(4) 1_565 ? Mn1 Be1 2.746(6) . ? Mn1 Be1 2.746(6) 3_665 ? Mn1 Ca3 3.5917(12) . ? Mn1 Ca3 3.5917(12) 3_665 ? Mn2 O3 2.118(4) 3_755 ? Mn2 O3 2.118(4) 1_565 ? Mn2 OH15 2.168(4) 3_665 ? Mn2 OH15 2.168(4) 1_655 ? Mn2 O2 2.205(4) 3_765 ? Mn2 O2 2.206(4) . ? Mn2 Be11 2.706(6) 3_765 ? Mn2 Be11 2.706(6) . ? Mn2 Ca3 3.5427(11) . ? Mn2 Ca3 3.5428(11) 3_765 ? Ca3 OW16 2.366(5) . ? Ca3 OW17 2.395(5) . ? Ca3 O2 2.421(4) . ? Ca3 O1 2.447(4) 1_565 ? Ca3 OH15 2.554(5) 3_665 ? Ca3 O10 2.559(4) 3_765 ? Ca3 OH14 2.685(5) 3_665 ? Ca3 O13 2.738(5) . ? Ca3 Be11 3.150(7) 3_765 ? Ca3 Be1 3.211(7) 3_665 ? Ca3 H17A 2.76(8) . ? Si1 O2 1.626(4) . ? Si1 O3 1.627(4) . ? Si1 O4 1.628(4) . ? Si1 O1 1.641(4) . ? Si2 O7 1.631(4) . ? Si2 O5 1.636(6) . ? Si2 O6 1.639(5) . ? Si2 O6 1.647(4) 2_644 ? Si22 O5 1.623(6) . ? Si22 O9 1.625(4) . ? Si22 O8 1.634(5) . ? Si22 O8 1.645(5) 2_554 ? Si3 O10 1.593(4) 3_665 ? Si3 O9 1.599(5) . ? Si3 O11 1.627(4) 1_545 ? Si3 O12 1.646(4) . ? Si33 O11 1.601(4) . ? Si33 O7 1.602(4) . ? Si33 O13 1.603(4) . ? Si33 O12 1.631(4) . ? Be1 O13 1.603(7) 3_665 ? Be1 O4 1.649(8) . ? Be1 OH14 1.653(7) 1_545 ? Be1 O1 1.663(8) 3_655 ? Be1 Ca3 3.211(7) 3_665 ? Be11 O10 1.611(7) . ? Be11 O3 1.626(8) 1_565 ? Be11 OH15 1.647(7) 1_665 ? Be11 O2 1.674(8) 3_765 ? Be11 Ca3 3.150(7) 3_765 ? O1 Be1 1.663(8) 3_655 ? O1 Mn1 2.226(4) 1_545 ? O1 Ca3 2.447(4) 1_545 ? O2 Be11 1.674(8) 3_765 ? O3 Be11 1.626(8) 1_545 ? O3 Mn2 2.118(4) 1_545 ? O6 Si2 1.647(4) 2_654 ? O8 Si22 1.645(5) 2_544 ? O10 Si3 1.593(4) 3_665 ? O10 Ca3 2.559(4) 3_765 ? O11 Si3 1.627(4) 1_565 ? O13 Be1 1.603(7) 3_665 ? OH14 Be1 1.653(7) 1_565 ? OH14 Ca3 2.685(5) 3_665 ? OH14 H14 0.9800(10) . ? OH15 Be11 1.647(7) 1_445 ? OH15 Mn2 2.168(4) 1_455 ? OH15 Ca3 2.554(5) 3_665 ? OH15 H15 0.9800(10) . ? OW16 H16A 0.9802(11) . ? OW16 H16B 0.9800(10) . ? OW17 H17A 0.9800(10) . ? OW17 H17B 0.9800(11) . ? 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 85.85(15) 3_665 . ? O4 Mn1 OH14 94.15(15) . . ? O4 Mn1 OH14 94.15(15) 3_665 3_665 ? O4 Mn1 OH14 85.85(15) . 3_665 ? OH14 Mn1 OH14 180.00(12) . 3_665 ? O4 Mn1 O1 107.62(14) 3_665 3_655 ? O4 Mn1 O1 72.38(14) . 3_655 ? OH14 Mn1 O1 86.93(14) . 3_655 ? OH14 Mn1 O1 93.07(14) 3_665 3_655 ? O4 Mn1 O1 72.38(14) 3_665 1_565 ? O4 Mn1 O1 107.62(14) . 1_565 ? OH14 Mn1 O1 93.07(14) . 1_565 ? OH14 Mn1 O1 86.93(14) 3_665 1_565 ? O1 Mn1 O1 180.0(2) 3_655 1_565 ? O4 Mn1 Be1 143.17(19) 3_665 . ? O4 Mn1 Be1 36.83(19) . . ? OH14 Mn1 Be1 82.24(16) . . ? OH14 Mn1 Be1 97.76(16) 3_665 . ? O1 Mn1 Be1 37.26(18) 3_655 . ? O1 Mn1 Be1 142.74(18) 1_565 . ? O4 Mn1 Be1 36.83(19) 3_665 3_665 ? O4 Mn1 Be1 143.17(19) . 3_665 ? OH14 Mn1 Be1 97.76(16) . 3_665 ? OH14 Mn1 Be1 82.24(16) 3_665 3_665 ? O1 Mn1 Be1 142.74(18) 3_655 3_665 ? O1 Mn1 Be1 37.26(18) 1_565 3_665 ? Be1 Mn1 Be1 179.998(1) . 3_665 ? O4 Mn1 Ca3 92.65(11) 3_665 . ? O4 Mn1 Ca3 87.35(11) . . ? OH14 Mn1 Ca3 132.05(13) . . ? OH14 Mn1 Ca3 47.95(13) 3_665 . ? O1 Mn1 Ca3 137.91(10) 3_655 . ? O1 Mn1 Ca3 42.09(10) 1_565 . ? Be1 Mn1 Ca3 120.90(15) . . ? Be1 Mn1 Ca3 59.09(15) 3_665 . ? O4 Mn1 Ca3 87.35(11) 3_665 3_665 ? O4 Mn1 Ca3 92.65(11) . 3_665 ? OH14 Mn1 Ca3 47.95(13) . 3_665 ? OH14 Mn1 Ca3 132.05(13) 3_665 3_665 ? O1 Mn1 Ca3 42.09(10) 3_655 3_665 ? O1 Mn1 Ca3 137.91(10) 1_565 3_665 ? Be1 Mn1 Ca3 59.10(15) . 3_665 ? Be1 Mn1 Ca3 120.91(15) 3_665 3_665 ? Ca3 Mn1 Ca3 180.0 . 3_665 ? O3 Mn2 O3 180.0(3) 3_755 1_565 ? O3 Mn2 OH15 95.70(15) 3_755 3_665 ? O3 Mn2 OH15 84.30(15) 1_565 3_665 ? O3 Mn2 OH15 84.30(15) 3_755 1_655 ? O3 Mn2 OH15 95.70(15) 1_565 1_655 ? OH15 Mn2 OH15 180.0(2) 3_665 1_655 ? O3 Mn2 O2 106.73(14) 3_755 3_765 ? O3 Mn2 O2 73.27(14) 1_565 3_765 ? OH15 Mn2 O2 94.05(14) 3_665 3_765 ? OH15 Mn2 O2 85.95(14) 1_655 3_765 ? O3 Mn2 O2 73.27(14) 3_755 . ? O3 Mn2 O2 106.73(14) 1_565 . ? OH15 Mn2 O2 85.95(14) 3_665 . ? OH15 Mn2 O2 94.05(14) 1_655 . ? O2 Mn2 O2 180.0(2) 3_765 . ? O3 Mn2 Be11 36.92(19) 3_755 3_765 ? O3 Mn2 Be11 143.08(19) 1_565 3_765 ? OH15 Mn2 Be11 82.36(16) 3_665 3_765 ? OH15 Mn2 Be11 97.64(16) 1_655 3_765 ? O2 Mn2 Be11 141.84(19) 3_765 3_765 ? O2 Mn2 Be11 38.16(19) . 3_765 ? O3 Mn2 Be11 143.08(19) 3_755 . ? O3 Mn2 Be11 36.92(19) 1_565 . ? OH15 Mn2 Be11 97.64(16) 3_665 . ? OH15 Mn2 Be11 82.36(16) 1_655 . ? O2 Mn2 Be11 38.16(19) 3_765 . ? O2 Mn2 Be11 141.84(19) . . ? Be11 Mn2 Be11 180.0(3) 3_765 . ? O3 Mn2 Ca3 92.26(11) 3_755 . ? O3 Mn2 Ca3 87.74(11) 1_565 . ? OH15 Mn2 Ca3 45.69(12) 3_665 . ? OH15 Mn2 Ca3 134.31(12) 1_655 . ? O2 Mn2 Ca3 137.66(10) 3_765 . ? O2 Mn2 Ca3 42.34(10) . . ? Be11 Mn2 Ca3 58.74(15) 3_765 . ? Be11 Mn2 Ca3 121.26(15) . . ? O3 Mn2 Ca3 87.74(11) 3_755 3_765 ? O3 Mn2 Ca3 92.26(11) 1_565 3_765 ? OH15 Mn2 Ca3 134.31(12) 3_665 3_765 ? OH15 Mn2 Ca3 45.69(12) 1_655 3_765 ? O2 Mn2 Ca3 42.34(10) 3_765 3_765 ? O2 Mn2 Ca3 137.66(10) . 3_765 ? Be11 Mn2 Ca3 121.26(15) 3_765 3_765 ? Be11 Mn2 Ca3 58.74(15) . 3_765 ? Ca3 Mn2 Ca3 180.0 . 3_765 ? OW16 Ca3 OW17 77.69(17) . . ? OW16 Ca3 O2 142.19(19) . . ? OW17 Ca3 O2 109.19(15) . . ? OW16 Ca3 O1 114.92(15) . 1_565 ? OW17 Ca3 O1 136.42(17) . 1_565 ? O2 Ca3 O1 86.24(10) . 1_565 ? OW16 Ca3 OH15 82.10(18) . 3_665 ? OW17 Ca3 OH15 148.28(17) . 3_665 ? O2 Ca3 OH15 73.58(14) . 3_665 ? O1 Ca3 OH15 74.57(13) 1_565 3_665 ? OW16 Ca3 O10 82.02(17) . 3_765 ? OW17 Ca3 O10 85.36(16) . 3_765 ? O2 Ca3 O10 62.24(13) . 3_765 ? O1 Ca3 O10 135.93(13) 1_565 3_765 ? OH15 Ca3 O10 67.69(14) 3_665 3_765 ? OW16 Ca3 OH14 141.16(18) . 3_665 ? OW17 Ca3 OH14 74.93(15) . 3_665 ? O2 Ca3 OH14 73.88(13) . 3_665 ? O1 Ca3 OH14 70.72(13) 1_565 3_665 ? OH15 Ca3 OH14 133.29(10) 3_665 3_665 ? O10 Ca3 OH14 122.07(13) 3_765 3_665 ? OW16 Ca3 O13 81.80(17) . . ? OW17 Ca3 O13 82.20(15) . . ? O2 Ca3 O13 135.36(13) . . ? O1 Ca3 O13 60.49(12) 1_565 . ? OH15 Ca3 O13 118.89(13) 3_665 . ? O10 Ca3 O13 161.35(10) 3_765 . ? OH14 Ca3 O13 67.71(13) 3_665 . ? OW16 Ca3 Be11 112.1(2) . 3_765 ? OW17 Ca3 Be11 97.20(17) . 3_765 ? O2 Ca3 Be11 31.66(15) . 3_765 ? O1 Ca3 Be11 113.41(15) 1_565 3_765 ? OH15 Ca3 Be11 68.17(15) 3_665 3_765 ? O10 Ca3 Be11 30.61(15) 3_765 3_765 ? OH14 Ca3 Be11 98.32(16) 3_665 3_765 ? O13 Ca3 Be11 165.75(16) . 3_765 ? OW16 Ca3 Be1 99.24(18) . 3_665 ? OW17 Ca3 Be1 109.57(18) . 3_665 ? O2 Ca3 Be1 112.12(15) . 3_665 ? O1 Ca3 Be1 30.56(14) 1_565 3_665 ? OH15 Ca3 Be1 97.56(15) 3_665 3_665 ? O10 Ca3 Be1 164.99(15) 3_765 3_665 ? OH14 Ca3 Be1 65.57(15) 3_665 3_665 ? O13 Ca3 Be1 29.93(14) . 3_665 ? Be11 Ca3 Be1 142.50(13) 3_765 3_665 ? OW16 Ca3 Mn2 118.13(16) . . ? OW17 Ca3 Mn2 143.74(12) . . ? O2 Ca3 Mn2 37.84(9) . . ? O1 Ca3 Mn2 69.65(9) 1_565 . ? OH15 Ca3 Mn2 37.41(10) 3_665 . ? O10 Ca3 Mn2 66.63(9) 3_765 . ? OH14 Ca3 Mn2 100.12(9) 3_665 . ? O13 Ca3 Mn2 130.00(8) . . ? Be11 Ca3 Mn2 47.25(11) 3_765 . ? Be1 Ca3 Mn2 100.15(12) 3_665 . ? OW16 Ca3 Mn1 146.45(14) . . ? OW17 Ca3 Mn1 109.86(13) . . ? O2 Ca3 Mn1 68.02(9) . . ? O1 Ca3 Mn1 37.57(9) 1_565 . ? OH15 Ca3 Mn1 100.52(10) 3_665 . ? O10 Ca3 Mn1 130.22(9) 3_765 . ? OH14 Ca3 Mn1 35.47(9) 3_665 . ? O13 Ca3 Mn1 67.55(9) . . ? Be11 Ca3 Mn1 99.62(13) 3_765 . ? Be1 Ca3 Mn1 47.21(12) 3_665 . ? Mn2 Ca3 Mn1 75.748(17) . . ? OW16 Ca3 H17A 57.5(11) . . ? OW17 Ca3 H17A 20.3(10) . . ? O2 Ca3 H17A 122.5(17) . . ? O1 Ca3 H17A 143(2) 1_565 . ? OH15 Ca3 H17A 131.9(13) 3_665 . ? O10 Ca3 H17A 80.8(19) 3_765 . ? OH14 Ca3 H17A 94.0(12) 3_665 . ? O13 Ca3 H17A 83(2) . . ? Be11 Ca3 H17A 102(2) 3_765 . ? Be1 Ca3 H17A 113(2) 3_665 . ? Mn2 Ca3 H17A 147(2) . . ? Mn1 Ca3 H17A 127.5(14) . . ? O2 Si1 O3 112.5(2) . . ? O2 Si1 O4 106.2(2) . . ? O3 Si1 O4 111.81(17) . . ? O2 Si1 O1 107.81(15) . . ? O3 Si1 O1 107.0(2) . . ? O4 Si1 O1 111.4(2) . . ? O7 Si2 O5 112.8(2) . . ? O7 Si2 O6 110.1(2) . . ? O5 Si2 O6 106.2(2) . . ? O7 Si2 O6 106.4(3) . 2_644 ? O5 Si2 O6 109.7(3) . 2_644 ? O6 Si2 O6 111.81(12) . 2_644 ? O5 Si22 O9 113.0(3) . . ? O5 Si22 O8 106.4(2) . . ? O9 Si22 O8 110.8(3) . . ? O5 Si22 O8 110.3(3) . 2_554 ? O9 Si22 O8 105.5(3) . 2_554 ? O8 Si22 O8 110.80(12) . 2_554 ? O10 Si3 O9 110.0(3) 3_665 . ? O10 Si3 O11 107.6(2) 3_665 1_545 ? O9 Si3 O11 110.4(3) . 1_545 ? O10 Si3 O12 114.1(2) 3_665 . ? O9 Si3 O12 109.9(2) . . ? O11 Si3 O12 104.7(2) 1_545 . ? O11 Si33 O7 109.7(3) . . ? O11 Si33 O13 113.8(2) . . ? O7 Si33 O13 108.2(2) . . ? O11 Si33 O12 102.6(2) . . ? O7 Si33 O12 111.7(2) . . ? O13 Si33 O12 110.8(2) . . ? O13 Be1 O4 113.0(4) 3_665 . ? O13 Be1 OH14 114.2(4) 3_665 1_545 ? O4 Be1 OH14 111.6(5) . 1_545 ? O13 Be1 O1 106.9(5) 3_665 3_655 ? O4 Be1 O1 100.9(4) . 3_655 ? OH14 Be1 O1 109.1(4) 1_545 3_655 ? O13 Be1 Mn1 108.4(3) 3_665 . ? O4 Be1 Mn1 49.6(2) . . ? OH14 Be1 Mn1 137.3(4) 1_545 . ? O1 Be1 Mn1 54.1(2) 3_655 . ? O13 Be1 Ca3 58.5(3) 3_665 3_665 ? O4 Be1 Ca3 117.9(3) . 3_665 ? OH14 Be1 Ca3 128.2(4) 1_545 3_665 ? O1 Be1 Ca3 48.4(2) 3_655 3_665 ? Mn1 Be1 Ca3 73.70(16) . 3_665 ? O10 Be11 O3 110.8(4) . 1_565 ? O10 Be11 OH15 117.6(4) . 1_665 ? O3 Be11 OH15 112.8(5) 1_565 1_665 ? O10 Be11 O2 103.3(4) . 3_765 ? O3 Be11 O2 102.9(4) 1_565 3_765 ? OH15 Be11 O2 107.9(4) 1_665 3_765 ? O10 Be11 Mn2 103.2(3) . . ? O3 Be11 Mn2 51.5(2) 1_565 . ? OH15 Be11 Mn2 139.0(4) 1_665 . ? O2 Be11 Mn2 54.5(2) 3_765 . ? O10 Be11 Ca3 54.0(3) . 3_765 ? O3 Be11 Ca3 119.6(3) 1_565 3_765 ? OH15 Be11 Ca3 126.0(4) 1_665 3_765 ? O2 Be11 Ca3 49.4(2) 3_765 3_765 ? Mn2 Be11 Ca3 74.01(16) . 3_765 ? Si1 O1 Be1 117.6(3) . 3_655 ? Si1 O1 Mn1 115.62(19) . 1_545 ? Be1 O1 Mn1 88.6(3) 3_655 1_545 ? Si1 O1 Ca3 126.2(2) . 1_545 ? Be1 O1 Ca3 101.0(3) 3_655 1_545 ? Mn1 O1 Ca3 100.33(14) 1_545 1_545 ? Si1 O2 Be11 116.9(3) . 3_765 ? Si1 O2 Mn2 116.13(19) . . ? Be11 O2 Mn2 87.3(3) 3_765 . ? Si1 O2 Ca3 128.9(2) . . ? Be11 O2 Ca3 98.9(3) 3_765 . ? Mn2 O2 Ca3 99.83(14) . . ? Be11 O3 Si1 125.8(3) 1_545 . ? Be11 O3 Mn2 91.6(3) 1_545 1_545 ? Si1 O3 Mn2 122.1(2) . 1_545 ? Si1 O4 Be1 124.1(3) . . ? Si1 O4 Mn1 122.3(2) . . ? Be1 O4 Mn1 93.6(3) . . ? Si22 O5 Si2 144.5(2) . . ? Si2 O6 Si2 136.7(3) . 2_654 ? Si33 O7 Si2 152.8(3) . . ? Si22 O8 Si22 138.1(3) . 2_544 ? Si3 O9 Si22 162.6(4) . . ? Si3 O10 Be11 121.7(4) 3_665 . ? Si3 O10 Ca3 142.4(2) 3_665 3_765 ? Be11 O10 Ca3 95.4(3) . 3_765 ? Si33 O11 Si3 145.4(3) . 1_565 ? Si33 O12 Si3 137.1(3) . . ? Be1 O13 Si33 132.2(4) 3_665 . ? Be1 O13 Ca3 91.6(3) 3_665 . ? Si33 O13 Ca3 126.0(2) . . ? Be1 OH14 Mn1 124.7(3) 1_565 . ? Be1 OH14 Ca3 117.2(4) 1_565 3_665 ? Mn1 OH14 Ca3 96.58(15) . 3_665 ? Be1 OH14 H14 109(6) 1_565 . ? Mn1 OH14 H14 113(6) . . ? Ca3 OH14 H14 92(6) 3_665 . ? Be11 OH15 Mn2 122.6(3) 1_445 1_455 ? Be11 OH15 Ca3 122.1(4) 1_445 3_665 ? Mn2 OH15 Ca3 96.91(15) 1_455 3_665 ? Be11 OH15 H15 95(6) 1_445 . ? Mn2 OH15 H15 121(6) 1_455 . ? Ca3 OH15 H15 98(6) 3_665 . ? Ca3 OW16 H16A 116(6) . . ? Ca3 OW16 H16B 136(6) . . ? H16A OW16 H16B 105(8) . . ? Ca3 OW17 H17A 102(6) . . ? Ca3 OW17 H17B 120(5) . . ? H17A OW17 H17B 134(8) . . ? 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 0.9800(10) 1.92(2) 2.884(5) 168(8) 3_665 OH15 H15 O10 0.9800(10) 2.47(10) 2.848(5) 102(6) 1_455 OW16 H16A O10 0.9802(11) 2.44(6) 3.240(7) 138(7) 3_775 OW16 H16B O8 0.9800(10) 1.974(17) 2.945(7) 170(8) 2_654 OW17 H17B O13 0.9800(11) 1.98(6) 2.803(6) 140(7) 1_545 OW17 H17A OW16 0.9800(10) 2.49(9) 2.986(6) 111(6) . OW17 H17A O6 0.9800(10) 2.39(8) 2.984(7) 119(7) 2_644 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.355 _refine_diff_density_min -1.027 _refine_diff_density_rms 0.158