data_utop21c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H1.25 B0.12 Be2 Ca Fe0.50 Mn0.50 O17 Si5' _chemical_formula_weight 528.56 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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'B' 'B' 0.0013 0.0007 '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 8.7300(5) _cell_length_b 4.9190(3) _cell_length_c 31.283(6) _cell_angle_alpha 90.00 _cell_angle_beta 89.99(3) _cell_angle_gamma 90.00 _cell_volume 1343.4(3) _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 2.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1046 _exptl_absorpt_coefficient_mu 1.982 _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 15660 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0125 _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 30.08 _reflns_number_total 3935 _reflns_number_gt 3911 _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^)+(0.0330P)^2^+10.8561P] 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 3935 _refine_ls_number_parameters 275 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.003 _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 Fe 0.5000 0.5000 0.0000 0.0116(3) Uani 0.960(7) 2 d SP . . MN2 Fe 1.0000 0.5000 0.0000 0.0107(3) Uani 0.930(6) 2 d SP . . Ca1 Ca 0.74969(17) 0.4998(2) -0.08826(2) 0.01307(16) Uani 1 1 d . . . Ca2 Ca 1.740(4) 1.475(6) -0.1988(5) 0.058(7) Uani 0.084(6) 1 d P . . Si1 Si 0.74975(19) 0.0012(3) -0.00131(3) 0.00749(18) Uani 1 1 d . . . Si2 Si 0.41519(17) 0.5933(2) -0.23254(5) 0.0092(4) Uani 0.962(8) 1 d P . . Si22 Si 0.08386(17) 0.3705(3) -0.23219(5) 0.0100(4) Uani 0.962(8) 1 d P . . Si3 Si 0.14237(17) 0.2268(2) -0.13430(5) 0.0086(4) Uani 0.968(8) 1 d P . . Si33 Si 0.35703(18) 0.7185(2) -0.13513(4) 0.0090(4) Uani 0.966(8) 1 d P . . Be4 Be 0.5009(8) 1.0716(13) 0.0574(2) 0.0166(18) Uani 0.973(10) 1 d P . . Si4 Si 0.5009(8) 1.0716(13) 0.0574(2) 0.0166(18) Uani 0.027(10) 1 d P . . Be44 Be 0.0020(8) 0.9171(12) 0.0568(2) 0.0119(14) Uani 0.94(14) 1 d P . . B44 B 0.0020(8) 0.9171(12) 0.0568(2) 0.0119(14) Uani 0.06(14) 1 d P . . O1 O 0.6530(4) -0.2034(7) -0.03294(12) 0.0100(6) Uani 1 1 d . . . O2 O 0.8479(5) 0.2057(7) -0.03221(11) 0.0107(6) Uani 1 1 d . . . O3 O 0.8614(5) -0.1873(7) 0.02803(12) 0.0124(7) Uani 1 1 d . . . O4 O 0.6403(5) 0.1878(7) 0.02822(11) 0.0099(6) Uani 1 1 d . . . O5 O 0.2507(7) 0.4854(10) -0.24810(9) 0.0232(7) Uani 1 1 d . . . O6 O 0.4611(5) 0.8451(8) -0.26370(15) 0.0242(9) Uani 1 1 d . . . O7 O 0.4192(6) 0.6922(10) -0.18336(14) 0.0266(10) Uani 1 1 d . . . O8 O 0.0470(5) 0.1029(9) -0.26092(17) 0.0283(10) Uani 1 1 d . . . O9 O 0.0852(6) 0.2962(10) -0.18191(13) 0.0267(10) Uani 1 1 d . . . O10 O 0.9991(5) 0.7727(7) 0.10255(12) 0.0135(7) Uani 1 1 d . . . O11 O 0.2135(4) 0.9239(9) -0.13426(16) 0.0321(9) Uani 1 1 d . . . O12 O 0.2799(4) 0.4284(8) -0.12070(11) 0.0226(8) Uani 1 1 d . . . O13 O 0.4989(5) 0.7959(8) -0.10560(11) 0.0153(7) Uani 1 1 d . . . OH14 O 0.4880(5) 0.7436(6) 0.05891(11) 0.0085(6) Uani 1 1 d D . . OH15 O 0.0179(6) 0.2456(8) 0.05810(14) 0.0194(9) Uani 1 1 d D . . OW16 O 0.8329(8) 0.7394(10) -0.15048(17) 0.0379(14) Uani 1 1 d D . . OW17 O 0.6557(5) 0.2307(8) -0.14632(14) 0.0196(8) Uani 1 1 d D . . H14 H 0.569(7) 0.667(17) 0.077(2) 0.050 Uiso 1 1 d D . . H15 H -0.043(8) 0.331(17) 0.081(2) 0.050 Uiso 1 1 d D . . H16A H 0.904(8) 0.879(13) -0.140(3) 0.050 Uiso 1 1 d D . . H16B H 0.879(11) 0.676(19) -0.1773(16) 0.050 Uiso 1 1 d D . . H17A H 0.611(11) 0.300(18) -0.1729(17) 0.050 Uiso 1 1 d D . . H17B H 0.709(9) 0.092(12) -0.130(2) 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 0.0140(6) 0.0095(5) 0.0114(5) -0.0005(3) 0.0010(6) -0.0002(4) MN2 0.0134(6) 0.0073(5) 0.0113(6) -0.0015(3) -0.0031(6) -0.0024(4) Ca1 0.0161(3) 0.0112(3) 0.0119(3) -0.0002(3) -0.0006(6) -0.0002(3) Ca2 0.068(14) 0.084(16) 0.022(7) -0.015(10) 0.005(11) -0.019(12) Si1 0.0079(4) 0.0067(4) 0.0079(4) 0.0005(4) -0.0002(9) -0.0013(3) Si2 0.0112(7) 0.0096(6) 0.0069(6) -0.0008(4) 0.0030(5) -0.0018(4) Si22 0.0110(6) 0.0094(6) 0.0096(7) 0.0004(4) -0.0009(6) -0.0012(4) Si3 0.0052(6) 0.0123(6) 0.0083(6) -0.0006(4) 0.0000(5) 0.0019(4) Si33 0.0123(7) 0.0083(6) 0.0063(6) -0.0004(4) 0.0003(6) 0.0016(4) Be4 0.017(3) 0.016(3) 0.016(3) -0.002(2) -0.005(3) -0.003(2) Si4 0.017(3) 0.016(3) 0.016(3) -0.002(2) -0.005(3) -0.003(2) Be44 0.008(3) 0.012(3) 0.015(3) 0.001(2) -0.009(3) -0.001(2) B44 0.008(3) 0.012(3) 0.015(3) 0.001(2) -0.009(3) -0.001(2) O1 0.0063(14) 0.0120(14) 0.0118(15) -0.0005(12) -0.0016(14) -0.0014(12) O2 0.0139(16) 0.0085(13) 0.0098(15) 0.0025(11) -0.0016(15) -0.0017(13) O3 0.0101(15) 0.0129(15) 0.0142(17) 0.0022(13) 0.0005(15) 0.0033(13) O4 0.0114(15) 0.0094(13) 0.0090(15) -0.0013(12) 0.0040(15) -0.0036(13) O5 0.0194(13) 0.0313(18) 0.0190(13) -0.0070(17) -0.003(2) -0.0080(14) O6 0.031(2) 0.0203(18) 0.0217(19) 0.0059(16) -0.0008(17) -0.0059(15) O7 0.027(2) 0.040(2) 0.0124(19) -0.0082(17) 0.0002(17) 0.011(2) O8 0.019(2) 0.029(2) 0.037(3) -0.0094(19) 0.0001(17) -0.0096(16) O9 0.022(2) 0.047(3) 0.0118(19) 0.0059(17) -0.0041(17) -0.019(2) O10 0.0091(15) 0.0180(16) 0.0135(15) 0.0062(12) 0.0045(15) 0.0023(14) O11 0.0168(18) 0.031(2) 0.049(2) -0.009(2) -0.0040(17) 0.0089(15) O12 0.022(2) 0.0238(19) 0.0220(16) 0.0065(14) -0.0059(13) -0.0077(14) O13 0.0186(17) 0.0203(16) 0.0069(14) -0.0039(12) 0.0048(15) -0.0115(16) OH14 0.0093(16) 0.0080(14) 0.0083(15) 0.0028(10) -0.0038(15) 0.0007(11) OH15 0.024(2) 0.0190(18) 0.0155(18) -0.0037(13) 0.0046(19) -0.0012(15) OW16 0.063(4) 0.026(2) 0.024(2) 0.0048(17) 0.007(3) -0.001(2) OW17 0.0149(17) 0.0273(19) 0.0166(17) -0.0025(14) -0.0040(15) -0.0048(15) _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 2.154(4) 3_665 ? MN1 O4 2.154(4) . ? MN1 OH14 2.200(3) 3_665 ? MN1 OH14 2.201(3) . ? MN1 O1 2.230(4) 3_655 ? MN1 O1 2.230(4) 1_565 ? MN1 Be4 2.768(6) 1_545 ? MN1 Si4 2.768(6) 1_545 ? MN1 Si4 2.768(6) 3_675 ? MN1 Be4 2.768(6) 3_675 ? MN1 Ca1 3.5175(15) 3_665 ? MN1 Ca1 3.5175(15) . ? MN2 O3 2.144(4) 3_755 ? MN2 O3 2.144(4) 1_565 ? MN2 O2 2.208(4) . ? MN2 O2 2.208(4) 3_765 ? MN2 OH15 2.212(4) 3_665 ? MN2 OH15 2.212(4) 1_655 ? MN2 Be44 2.714(6) 3_665 ? MN2 Be44 2.714(6) 1_655 ? MN2 Ca1 3.5213(15) 3_765 ? MN2 Ca1 3.5213(15) . ? Ca1 OW16 2.389(5) . ? Ca1 OW17 2.393(4) . ? Ca1 O1 2.416(4) 1_565 ? Ca1 O2 2.429(4) . ? Ca1 OH15 2.564(5) 3_665 ? Ca1 OH14 2.566(4) 3_665 ? Ca1 O10 2.609(4) 3_765 ? Ca1 O13 2.685(5) . ? Ca1 B44 3.142(6) 3_665 ? Ca1 Be44 3.142(6) 3_665 ? Ca1 Be4 3.188(7) 3_675 ? Ca1 Si4 3.188(7) 3_675 ? Ca1 H17B 2.42(8) . ? Ca2 OW16 2.15(2) 1_665 ? Ca2 OW17 2.16(2) 1_665 ? Ca2 O6 2.20(3) 2_754 ? Ca2 O8 2.34(3) 2_764 ? Ca2 O5 2.93(3) 2_754 ? Ca2 O5 3.01(3) 2_764 ? Ca2 O7 3.03(4) 1_665 ? Ca2 Si2 3.08(4) 1_665 ? Ca2 Si2 3.16(2) 2_754 ? Ca2 Si22 3.22(3) 1_765 ? Ca2 Si22 3.29(2) 2_764 ? Ca2 Ca1 3.462(15) 1_665 ? Si1 O4 1.615(4) . ? Si1 O3 1.629(4) . ? Si1 O2 1.637(4) . ? Si1 O1 1.645(4) . ? Si1 Si4 2.828(7) 3_665 ? Si2 O5 1.607(6) . ? Si2 O7 1.614(4) . ? Si2 O6 1.626(4) . ? Si2 O6 1.634(4) 2_644 ? Si2 Ca2 3.08(4) 1_445 ? Si2 Ca2 3.16(2) 2_744 ? Si22 O9 1.615(4) . ? Si22 O8 1.626(5) . ? Si22 O8 1.631(4) 2_554 ? Si22 O5 1.640(6) . ? Si22 Ca2 3.22(3) 1_345 ? Si22 Ca2 3.29(2) 2_734 ? Si3 O10 1.585(4) 3_665 ? Si3 O9 1.607(4) . ? Si3 O11 1.614(4) 1_545 ? Si3 O12 1.614(4) . ? Si33 O13 1.591(5) . ? Si33 O7 1.609(5) . ? Si33 O11 1.610(4) . ? Si33 O12 1.641(4) . ? Be4 OH14 1.618(7) . ? Be4 O4 1.625(8) 1_565 ? Be4 O13 1.643(7) 3_675 ? Be4 O1 1.677(8) 3_665 ? Be4 MN1 2.768(6) 1_565 ? Be4 Ca1 3.188(7) 3_675 ? Be44 O10 1.598(7) 1_455 ? Be44 O3 1.606(7) 1_465 ? Be44 OH15 1.623(7) 1_565 ? Be44 O2 1.636(8) 3_665 ? Be44 MN2 2.714(6) 1_455 ? Be44 Ca1 3.142(6) 3_665 ? O1 Si4 1.677(8) 3_665 ? O1 Be4 1.677(8) 3_665 ? O1 MN1 2.230(4) 1_545 ? O1 Ca1 2.416(4) 1_545 ? O2 B44 1.636(8) 3_665 ? O2 Be44 1.636(8) 3_665 ? O3 B44 1.606(7) 1_645 ? O3 Be44 1.606(7) 1_645 ? O3 MN2 2.145(4) 1_545 ? O4 Si4 1.625(8) 1_545 ? O4 Be4 1.625(8) 1_545 ? O5 Ca2 2.93(3) 2_744 ? O5 Ca2 3.01(3) 2_734 ? O6 Si2 1.634(4) 2_654 ? O6 Ca2 2.20(3) 2_744 ? O7 Ca2 3.03(4) 1_445 ? O8 Si22 1.631(4) 2_544 ? O8 Ca2 2.34(3) 2_734 ? O10 Si3 1.584(4) 3_665 ? O10 B44 1.598(7) 1_655 ? O10 Be44 1.598(7) 1_655 ? O10 Ca1 2.609(4) 3_765 ? O11 Si3 1.614(4) 1_565 ? O13 Si4 1.643(7) 3_675 ? O13 Be4 1.643(7) 3_675 ? OH14 Ca1 2.565(4) 3_665 ? OH14 H14 0.979(2) . ? OH15 B44 1.623(7) 1_545 ? OH15 Be44 1.623(7) 1_545 ? OH15 MN2 2.212(4) 1_455 ? OH15 Ca1 2.564(5) 3_665 ? OH15 H15 0.977(2) . ? OW16 Ca2 2.15(2) 1_445 ? OW16 H16A 0.979(2) . ? OW16 H16B 0.979(2) . ? OW17 Ca2 2.16(2) 1_445 ? OW17 H17A 0.980(2) . ? OW17 H17B 0.978(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 94.13(12) 3_665 3_665 ? O4 MN1 OH14 85.87(12) . 3_665 ? O4 MN1 OH14 85.87(12) 3_665 . ? O4 MN1 OH14 94.13(12) . . ? OH14 MN1 OH14 180.0 3_665 . ? O4 MN1 O1 108.37(12) 3_665 3_655 ? O4 MN1 O1 71.63(12) . 3_655 ? OH14 MN1 O1 93.39(13) 3_665 3_655 ? OH14 MN1 O1 86.61(13) . 3_655 ? O4 MN1 O1 71.63(12) 3_665 1_565 ? O4 MN1 O1 108.37(12) . 1_565 ? OH14 MN1 O1 86.61(13) 3_665 1_565 ? OH14 MN1 O1 93.39(13) . 1_565 ? O1 MN1 O1 180.0(2) 3_655 1_565 ? O4 MN1 Be4 144.13(18) 3_665 1_545 ? O4 MN1 Be4 35.87(18) . 1_545 ? OH14 MN1 Be4 97.38(15) 3_665 1_545 ? OH14 MN1 Be4 82.62(15) . 1_545 ? O1 MN1 Be4 37.27(18) 3_655 1_545 ? O1 MN1 Be4 142.73(18) 1_565 1_545 ? O4 MN1 Si4 144.13(18) 3_665 1_545 ? O4 MN1 Si4 35.87(18) . 1_545 ? OH14 MN1 Si4 97.38(15) 3_665 1_545 ? OH14 MN1 Si4 82.62(15) . 1_545 ? O1 MN1 Si4 37.27(18) 3_655 1_545 ? O1 MN1 Si4 142.73(18) 1_565 1_545 ? Be4 MN1 Si4 0.0(4) 1_545 1_545 ? O4 MN1 Si4 35.87(18) 3_665 3_675 ? O4 MN1 Si4 144.13(18) . 3_675 ? OH14 MN1 Si4 82.62(15) 3_665 3_675 ? OH14 MN1 Si4 97.38(15) . 3_675 ? O1 MN1 Si4 142.73(18) 3_655 3_675 ? O1 MN1 Si4 37.27(18) 1_565 3_675 ? Be4 MN1 Si4 180.00(19) 1_545 3_675 ? Si4 MN1 Si4 180.00(19) 1_545 3_675 ? O4 MN1 Be4 35.87(18) 3_665 3_675 ? O4 MN1 Be4 144.13(18) . 3_675 ? OH14 MN1 Be4 82.62(15) 3_665 3_675 ? OH14 MN1 Be4 97.38(15) . 3_675 ? O1 MN1 Be4 142.73(18) 3_655 3_675 ? O1 MN1 Be4 37.27(18) 1_565 3_675 ? Be4 MN1 Be4 180.00(19) 1_545 3_675 ? Si4 MN1 Be4 180.00(19) 1_545 3_675 ? Si4 MN1 Be4 0.0(4) 3_675 3_675 ? O4 MN1 Ca1 88.23(10) 3_665 3_665 ? O4 MN1 Ca1 91.77(10) . 3_665 ? OH14 MN1 Ca1 133.38(10) 3_665 3_665 ? OH14 MN1 Ca1 46.62(10) . 3_665 ? O1 MN1 Ca1 42.82(9) 3_655 3_665 ? O1 MN1 Ca1 137.18(9) 1_565 3_665 ? Be4 MN1 Ca1 59.54(15) 1_545 3_665 ? Si4 MN1 Ca1 59.54(15) 1_545 3_665 ? Si4 MN1 Ca1 120.46(15) 3_675 3_665 ? Be4 MN1 Ca1 120.46(15) 3_675 3_665 ? O4 MN1 Ca1 91.77(10) 3_665 . ? O4 MN1 Ca1 88.23(10) . . ? OH14 MN1 Ca1 46.62(10) 3_665 . ? OH14 MN1 Ca1 133.38(10) . . ? O1 MN1 Ca1 137.18(9) 3_655 . ? O1 MN1 Ca1 42.82(9) 1_565 . ? Be4 MN1 Ca1 120.46(15) 1_545 . ? Si4 MN1 Ca1 120.46(15) 1_545 . ? Si4 MN1 Ca1 59.54(15) 3_675 . ? Be4 MN1 Ca1 59.54(15) 3_675 . ? Ca1 MN1 Ca1 180.000(14) 3_665 . ? O3 MN2 O3 180.0(3) 3_755 1_565 ? O3 MN2 O2 71.49(13) 3_755 . ? O3 MN2 O2 108.51(13) 1_565 . ? O3 MN2 O2 108.52(13) 3_755 3_765 ? O3 MN2 O2 71.48(13) 1_565 3_765 ? O2 MN2 O2 180.0 . 3_765 ? O3 MN2 OH15 96.30(15) 3_755 3_665 ? O3 MN2 OH15 83.70(15) 1_565 3_665 ? O2 MN2 OH15 87.33(14) . 3_665 ? O2 MN2 OH15 92.67(14) 3_765 3_665 ? O3 MN2 OH15 83.70(15) 3_755 1_655 ? O3 MN2 OH15 96.30(15) 1_565 1_655 ? O2 MN2 OH15 92.67(14) . 1_655 ? O2 MN2 OH15 87.33(14) 3_765 1_655 ? OH15 MN2 OH15 180.0(2) 3_665 1_655 ? O3 MN2 Be44 36.26(18) 3_755 3_665 ? O3 MN2 Be44 143.74(18) 1_565 3_665 ? O2 MN2 Be44 37.05(18) . 3_665 ? O2 MN2 Be44 142.95(18) 3_765 3_665 ? OH15 MN2 Be44 83.63(16) 3_665 3_665 ? OH15 MN2 Be44 96.37(16) 1_655 3_665 ? O3 MN2 Be44 143.74(18) 3_755 1_655 ? O3 MN2 Be44 36.26(18) 1_565 1_655 ? O2 MN2 Be44 142.95(18) . 1_655 ? O2 MN2 Be44 37.05(18) 3_765 1_655 ? OH15 MN2 Be44 96.37(16) 3_665 1_655 ? OH15 MN2 Be44 83.63(16) 1_655 1_655 ? Be44 MN2 Be44 180.0(3) 3_665 1_655 ? O3 MN2 Ca1 88.32(11) 3_755 3_765 ? O3 MN2 Ca1 91.68(11) 1_565 3_765 ? O2 MN2 Ca1 137.00(9) . 3_765 ? O2 MN2 Ca1 42.99(9) 3_765 3_765 ? OH15 MN2 Ca1 133.46(12) 3_665 3_765 ? OH15 MN2 Ca1 46.54(12) 1_655 3_765 ? Be44 MN2 Ca1 121.17(13) 3_665 3_765 ? Be44 MN2 Ca1 58.83(13) 1_655 3_765 ? O3 MN2 Ca1 91.68(11) 3_755 . ? O3 MN2 Ca1 88.32(11) 1_565 . ? O2 MN2 Ca1 43.00(9) . . ? O2 MN2 Ca1 137.01(9) 3_765 . ? OH15 MN2 Ca1 46.54(12) 3_665 . ? OH15 MN2 Ca1 133.46(12) 1_655 . ? Be44 MN2 Ca1 58.83(13) 3_665 . ? Be44 MN2 Ca1 121.17(13) 1_655 . ? Ca1 MN2 Ca1 180.0 3_765 . ? OW16 Ca1 OW17 76.04(15) . . ? OW16 Ca1 O1 113.06(16) . 1_565 ? OW17 Ca1 O1 139.30(16) . 1_565 ? OW16 Ca1 O2 140.8(2) . . ? OW17 Ca1 O2 109.85(14) . . ? O1 Ca1 O2 88.05(9) 1_565 . ? OW16 Ca1 OH15 79.53(19) . 3_665 ? OW17 Ca1 OH15 145.17(16) . 3_665 ? O1 Ca1 OH15 73.61(14) 1_565 3_665 ? O2 Ca1 OH15 75.28(13) . 3_665 ? OW16 Ca1 OH14 140.16(19) . 3_665 ? OW17 Ca1 OH14 74.70(14) . 3_665 ? O1 Ca1 OH14 75.11(12) 1_565 3_665 ? O2 Ca1 OH14 75.48(13) . 3_665 ? OH15 Ca1 OH14 137.41(9) 3_665 3_665 ? OW16 Ca1 O10 81.85(18) . 3_765 ? OW17 Ca1 O10 82.76(14) . 3_765 ? O1 Ca1 O10 136.61(13) 1_565 3_765 ? O2 Ca1 O10 61.38(13) . 3_765 ? OH15 Ca1 O10 69.44(14) 3_665 3_765 ? OH14 Ca1 O10 120.10(11) 3_665 3_765 ? OW16 Ca1 O13 79.38(18) . . ? OW17 Ca1 O13 82.36(14) . . ? O1 Ca1 O13 62.10(12) 1_565 . ? O2 Ca1 O13 139.16(13) . . ? OH15 Ca1 O13 117.04(13) 3_665 . ? OH14 Ca1 O13 70.48(12) 3_665 . ? O10 Ca1 O13 158.37(8) 3_765 . ? OW16 Ca1 B44 111.5(2) . 3_665 ? OW17 Ca1 B44 96.51(16) . 3_665 ? O1 Ca1 B44 114.27(15) 1_565 3_665 ? O2 Ca1 B44 30.90(16) . 3_665 ? OH15 Ca1 B44 69.97(15) 3_665 3_665 ? OH14 Ca1 B44 98.14(15) 3_665 3_665 ? O10 Ca1 B44 30.49(14) 3_765 3_665 ? O13 Ca1 B44 168.49(15) . 3_665 ? OW16 Ca1 Be44 111.5(2) . 3_665 ? OW17 Ca1 Be44 96.51(16) . 3_665 ? O1 Ca1 Be44 114.27(15) 1_565 3_665 ? O2 Ca1 Be44 30.90(16) . 3_665 ? OH15 Ca1 Be44 69.97(15) 3_665 3_665 ? OH14 Ca1 Be44 98.14(15) 3_665 3_665 ? O10 Ca1 Be44 30.49(14) 3_765 3_665 ? O13 Ca1 Be44 168.49(15) . 3_665 ? B44 Ca1 Be44 0.0(3) 3_665 3_665 ? OW16 Ca1 Be4 97.42(19) . 3_675 ? OW17 Ca1 Be4 111.13(16) . 3_675 ? O1 Ca1 Be4 31.11(14) 1_565 3_675 ? O2 Ca1 Be4 114.67(15) . 3_675 ? OH15 Ca1 Be4 96.24(16) 3_665 3_675 ? OH14 Ca1 Be4 69.21(14) 3_665 3_675 ? O10 Ca1 Be4 165.59(15) 3_765 3_675 ? O13 Ca1 Be4 31.00(13) . 3_675 ? B44 Ca1 Be4 144.12(12) 3_665 3_675 ? Be44 Ca1 Be4 144.12(12) 3_665 3_675 ? OW16 Ca1 Si4 97.42(19) . 3_675 ? OW17 Ca1 Si4 111.13(16) . 3_675 ? O1 Ca1 Si4 31.11(14) 1_565 3_675 ? O2 Ca1 Si4 114.67(15) . 3_675 ? OH15 Ca1 Si4 96.24(16) 3_665 3_675 ? OH14 Ca1 Si4 69.21(14) 3_665 3_675 ? O10 Ca1 Si4 165.59(15) 3_765 3_675 ? O13 Ca1 Si4 31.00(13) . 3_675 ? B44 Ca1 Si4 144.12(12) 3_665 3_675 ? Be44 Ca1 Si4 144.12(12) 3_665 3_675 ? Be4 Ca1 Si4 0.0(3) 3_675 3_675 ? OW16 Ca1 H17B 91.0(15) . . ? OW17 Ca1 H17B 23.5(4) . . ? O1 Ca1 H17B 147(2) 1_565 . ? O2 Ca1 H17B 86.8(5) . . ? OH15 Ca1 H17B 136.0(17) 3_665 . ? OH14 Ca1 H17B 72(2) 3_665 . ? O10 Ca1 H17B 66.7(16) 3_765 . ? O13 Ca1 H17B 102.9(11) . . ? B44 Ca1 H17B 74.1(8) 3_665 . ? Be44 Ca1 H17B 74.1(8) 3_665 . ? Be4 Ca1 H17B 127.7(16) 3_675 . ? Si4 Ca1 H17B 127.7(16) 3_675 . ? OW16 Ca2 OW17 86.0(5) 1_665 1_665 ? OW16 Ca2 O6 148.2(18) 1_665 2_754 ? OW17 Ca2 O6 88.5(11) 1_665 2_754 ? OW16 Ca2 O8 85.1(11) 1_665 2_764 ? OW17 Ca2 O8 146.0(18) 1_665 2_764 ? O6 Ca2 O8 115.2(6) 2_754 2_764 ? OW16 Ca2 O5 152.1(17) 1_665 2_754 ? OW17 Ca2 O5 89.0(9) 1_665 2_754 ? O6 Ca2 O5 58.8(5) 2_754 2_754 ? O8 Ca2 O5 83.8(8) 2_764 2_754 ? OW16 Ca2 O5 82.7(9) 1_665 2_764 ? OW17 Ca2 O5 153.1(15) 1_665 2_764 ? O6 Ca2 O5 88.3(9) 2_754 2_764 ? O8 Ca2 O5 57.0(6) 2_764 2_764 ? O5 Ca2 O5 111.9(5) 2_754 2_764 ? OW16 Ca2 O7 91.4(10) 1_665 1_665 ? OW17 Ca2 O7 76.3(9) 1_665 1_665 ? O6 Ca2 O7 56.9(8) 2_754 1_665 ? O8 Ca2 O7 136.7(12) 2_764 1_665 ? O5 Ca2 O7 114.0(10) 2_754 1_665 ? O5 Ca2 O7 79.7(9) 2_764 1_665 ? OW16 Ca2 Si2 118.4(13) 1_665 1_665 ? OW17 Ca2 Si2 93.1(11) 1_665 1_665 ? O6 Ca2 Si2 30.7(5) 2_754 1_665 ? O8 Ca2 Si2 119.9(9) 2_764 1_665 ? O5 Ca2 Si2 89.3(7) 2_754 1_665 ? O5 Ca2 Si2 71.3(7) 2_764 1_665 ? O7 Ca2 Si2 30.6(4) 1_665 1_665 ? OW16 Ca2 Si2 176.9(15) 1_665 2_754 ? OW17 Ca2 Si2 92.3(9) 1_665 2_754 ? O6 Ca2 Si2 28.9(3) 2_754 2_754 ? O8 Ca2 Si2 97.7(6) 2_764 2_754 ? O5 Ca2 Si2 30.3(2) 2_754 2_754 ? O5 Ca2 Si2 97.6(6) 2_764 2_754 ? O7 Ca2 Si2 85.6(8) 1_665 2_754 ? Si2 Ca2 Si2 59.0(5) 1_665 2_754 ? OW16 Ca2 Si22 88.3(11) 1_665 1_765 ? OW17 Ca2 Si22 118.2(14) 1_665 1_765 ? O6 Ca2 Si22 121.5(8) 2_754 1_765 ? O8 Ca2 Si22 28.9(5) 2_764 1_765 ? O5 Ca2 Si22 70.0(7) 2_754 1_765 ? O5 Ca2 Si22 85.9(7) 2_764 1_765 ? O7 Ca2 Si22 165.5(9) 1_665 1_765 ? Si2 Ca2 Si22 141.0(5) 1_665 1_765 ? Si2 Ca2 Si22 94.8(6) 2_754 1_765 ? OW16 Ca2 Si22 85.8(9) 1_665 2_764 ? OW17 Ca2 Si22 170.2(13) 1_665 2_764 ? O6 Ca2 Si22 101.3(7) 2_754 2_764 ? O8 Ca2 Si22 27.5(3) 2_764 2_764 ? O5 Ca2 Si22 95.8(5) 2_754 2_764 ? O5 Ca2 Si22 29.8(3) 2_764 2_764 ? O7 Ca2 Si22 109.2(10) 1_665 2_764 ? Si2 Ca2 Si22 95.4(7) 1_665 2_764 ? Si2 Ca2 Si22 96.1(4) 2_754 2_764 ? Si22 Ca2 Si22 56.3(5) 1_765 2_764 ? OW16 Ca2 Ca1 42.9(3) 1_665 1_665 ? OW17 Ca2 Ca1 43.1(3) 1_665 1_665 ? O6 Ca2 Ca1 124.2(10) 2_754 1_665 ? O8 Ca2 Ca1 120.6(10) 2_764 1_665 ? O5 Ca2 Ca1 126.5(9) 2_754 1_665 ? O5 Ca2 Ca1 121.4(8) 2_764 1_665 ? O7 Ca2 Ca1 81.5(6) 1_665 1_665 ? Si2 Ca2 Ca1 111.1(9) 1_665 1_665 ? Si2 Ca2 Ca1 135.3(8) 2_754 1_665 ? Si22 Ca2 Ca1 107.8(9) 1_765 1_665 ? Si22 Ca2 Ca1 128.5(8) 2_764 1_665 ? O4 Si1 O3 110.82(13) . . ? O4 Si1 O2 107.3(2) . . ? O3 Si1 O2 111.7(2) . . ? O4 Si1 O1 112.8(2) . . ? O3 Si1 O1 107.3(2) . . ? O2 Si1 O1 106.84(13) . . ? O4 Si1 Si4 88.2(2) . 3_665 ? O3 Si1 Si4 137.8(2) . 3_665 ? O2 Si1 Si4 96.7(2) . 3_665 ? O1 Si1 Si4 31.99(19) . 3_665 ? O5 Si2 O7 114.1(2) . . ? O5 Si2 O6 106.9(2) . . ? O7 Si2 O6 109.7(3) . . ? O5 Si2 O6 108.8(3) . 2_644 ? O7 Si2 O6 106.2(2) . 2_644 ? O6 Si2 O6 111.28(11) . 2_644 ? O5 Si2 Ca2 149.8(6) . 1_445 ? O7 Si2 Ca2 73.2(4) . 1_445 ? O6 Si2 Ca2 97.0(5) . 1_445 ? O6 Si2 Ca2 43.6(5) 2_644 1_445 ? O5 Si2 Ca2 66.9(7) . 2_744 ? O7 Si2 Ca2 118.6(5) . 2_744 ? O6 Si2 Ca2 40.9(7) . 2_744 ? O6 Si2 Ca2 132.7(5) 2_644 2_744 ? Ca2 Si2 Ca2 137.7(8) 1_445 2_744 ? O9 Si22 O8 110.9(3) . . ? O9 Si22 O8 107.0(3) . 2_554 ? O8 Si22 O8 110.84(11) . 2_554 ? O9 Si22 O5 111.5(2) . . ? O8 Si22 O5 106.7(2) . . ? O8 Si22 O5 109.9(3) 2_554 . ? O9 Si22 Ca2 74.2(4) . 1_345 ? O8 Si22 Ca2 97.1(5) . 1_345 ? O8 Si22 Ca2 43.7(5) 2_554 1_345 ? O5 Si22 Ca2 150.6(6) . 1_345 ? O9 Si22 Ca2 120.1(4) . 2_734 ? O8 Si22 Ca2 41.5(7) . 2_734 ? O8 Si22 Ca2 131.0(4) 2_554 2_734 ? O5 Si22 Ca2 65.7(7) . 2_734 ? Ca2 Si22 Ca2 138.1(7) 1_345 2_734 ? O10 Si3 O9 109.8(2) 3_665 . ? O10 Si3 O11 107.5(2) 3_665 1_545 ? O9 Si3 O11 108.4(3) . 1_545 ? O10 Si3 O12 114.4(2) 3_665 . ? O9 Si3 O12 110.2(2) . . ? O11 Si3 O12 106.3(2) 1_545 . ? O13 Si33 O7 107.6(3) . . ? O13 Si33 O11 116.5(2) . . ? O7 Si33 O11 109.2(3) . . ? O13 Si33 O12 111.6(2) . . ? O7 Si33 O12 109.0(2) . . ? O11 Si33 O12 102.8(2) . . ? OH14 Be4 O4 114.8(5) . 1_565 ? OH14 Be4 O13 111.6(4) . 3_675 ? O4 Be4 O13 112.0(4) 1_565 3_675 ? OH14 Be4 O1 110.1(4) . 3_665 ? O4 Be4 O1 102.0(4) 1_565 3_665 ? O13 Be4 O1 105.4(4) 3_675 3_665 ? OH14 Be4 MN1 141.1(4) . 1_565 ? O4 Be4 MN1 51.0(2) 1_565 1_565 ? O13 Be4 MN1 107.1(3) 3_675 1_565 ? O1 Be4 MN1 53.7(2) 3_665 1_565 ? OH14 Be4 Ca1 127.1(4) . 3_675 ? O4 Be4 Ca1 116.8(3) 1_565 3_675 ? O13 Be4 Ca1 57.3(3) 3_675 3_675 ? O1 Be4 Ca1 48.1(2) 3_665 3_675 ? MN1 Be4 Ca1 72.00(15) 1_565 3_675 ? O10 Be44 O3 110.4(4) 1_455 1_465 ? O10 Be44 OH15 114.9(4) 1_455 1_565 ? O3 Be44 OH15 113.4(4) 1_465 1_565 ? O10 Be44 O2 105.7(4) 1_455 3_665 ? O3 Be44 O2 103.3(4) 1_465 3_665 ? OH15 Be44 O2 108.1(4) 1_565 3_665 ? O10 Be44 MN2 104.5(3) 1_455 1_455 ? O3 Be44 MN2 52.2(2) 1_465 1_455 ? OH15 Be44 MN2 140.3(4) 1_565 1_455 ? O2 Be44 MN2 54.4(2) 3_665 1_455 ? O10 Be44 Ca1 56.0(2) 1_455 3_665 ? O3 Be44 Ca1 119.6(3) 1_465 3_665 ? OH15 Be44 Ca1 125.7(4) 1_565 3_665 ? O2 Be44 Ca1 49.7(2) 3_665 3_665 ? MN2 Be44 Ca1 73.51(15) 1_455 3_665 ? Si1 O1 Si4 116.7(3) . 3_665 ? Si1 O1 Be4 116.7(3) . 3_665 ? Si4 O1 Be4 0.0(6) 3_665 3_665 ? Si1 O1 MN1 115.47(19) . 1_545 ? Si4 O1 MN1 89.1(3) 3_665 1_545 ? Be4 O1 MN1 89.1(3) 3_665 1_545 ? Si1 O1 Ca1 128.4(2) . 1_545 ? Si4 O1 Ca1 100.8(3) 3_665 1_545 ? Be4 O1 Ca1 100.8(3) 3_665 1_545 ? MN1 O1 Ca1 98.33(14) 1_545 1_545 ? B44 O2 Be44 0.0(5) 3_665 3_665 ? B44 O2 Si1 118.0(3) 3_665 . ? Be44 O2 Si1 118.0(3) 3_665 . ? B44 O2 MN2 88.5(3) 3_665 . ? Be44 O2 MN2 88.5(3) 3_665 . ? Si1 O2 MN2 116.63(19) . . ? B44 O2 Ca1 99.4(3) 3_665 . ? Be44 O2 Ca1 99.4(3) 3_665 . ? Si1 O2 Ca1 127.4(2) . . ? MN2 O2 Ca1 98.70(13) . . ? B44 O3 Be44 0.0(4) 1_645 1_645 ? B44 O3 Si1 126.3(3) 1_645 . ? Be44 O3 Si1 126.3(3) 1_645 . ? B44 O3 MN2 91.6(3) 1_645 1_545 ? Be44 O3 MN2 91.6(3) 1_645 1_545 ? Si1 O3 MN2 121.0(2) . 1_545 ? Si1 O4 Si4 124.3(3) . 1_545 ? Si1 O4 Be4 124.3(3) . 1_545 ? Si4 O4 Be4 0.0(7) 1_545 1_545 ? Si1 O4 MN1 120.49(19) . . ? Si4 O4 MN1 93.2(3) 1_545 . ? Be4 O4 MN1 93.2(3) 1_545 . ? Si2 O5 Si22 144.7(2) . . ? Si2 O5 Ca2 82.8(7) . 2_744 ? Si22 O5 Ca2 118.8(8) . 2_744 ? Si2 O5 Ca2 114.7(8) . 2_734 ? Si22 O5 Ca2 84.6(7) . 2_734 ? Ca2 O5 Ca2 111.9(5) 2_744 2_734 ? Si2 O6 Si2 140.8(3) . 2_654 ? Si2 O6 Ca2 110.1(9) . 2_744 ? Si2 O6 Ca2 105.7(9) 2_654 2_744 ? Si33 O7 Si2 155.7(4) . . ? Si33 O7 Ca2 119.3(4) . 1_445 ? Si2 O7 Ca2 76.2(4) . 1_445 ? Si22 O8 Si22 141.2(3) . 2_544 ? Si22 O8 Ca2 111.0(9) . 2_734 ? Si22 O8 Ca2 107.4(9) 2_544 2_734 ? Si3 O9 Si22 162.4(4) . . ? Si3 O10 B44 125.0(4) 3_665 1_655 ? Si3 O10 Be44 125.0(4) 3_665 1_655 ? B44 O10 Be44 0.0(5) 1_655 1_655 ? Si3 O10 Ca1 139.7(2) 3_665 3_765 ? B44 O10 Ca1 93.5(3) 1_655 3_765 ? Be44 O10 Ca1 93.5(3) 1_655 3_765 ? Si33 O11 Si3 151.5(3) . 1_565 ? Si3 O12 Si33 140.0(2) . . ? Si33 O13 Si4 129.0(4) . 3_675 ? Si33 O13 Be4 129.0(4) . 3_675 ? Si4 O13 Be4 0.0(7) 3_675 3_675 ? Si33 O13 Ca1 128.5(2) . . ? Si4 O13 Ca1 91.7(3) 3_675 . ? Be4 O13 Ca1 91.7(3) 3_675 . ? Be4 OH14 MN1 121.0(3) . . ? Be4 OH14 Ca1 122.2(3) . 3_665 ? MN1 OH14 Ca1 94.82(13) . 3_665 ? Be4 OH14 H14 110(5) . . ? MN1 OH14 H14 104(5) . . ? Ca1 OH14 H14 102(5) 3_665 . ? B44 OH15 Be44 0.0(6) 1_545 1_545 ? B44 OH15 MN2 122.5(3) 1_545 1_455 ? Be44 OH15 MN2 122.5(3) 1_545 1_455 ? B44 OH15 Ca1 124.3(3) 1_545 3_665 ? Be44 OH15 Ca1 124.3(3) 1_545 3_665 ? MN2 OH15 Ca1 94.70(16) 1_455 3_665 ? B44 OH15 H15 113(6) 1_545 . ? Be44 OH15 H15 113(6) 1_545 . ? MN2 OH15 H15 108(6) 1_455 . ? Ca1 OH15 H15 87(5) 3_665 . ? Ca2 OW16 Ca1 99.2(6) 1_445 . ? Ca2 OW16 H16A 154(5) 1_445 . ? Ca1 OW16 H16A 105(5) . . ? Ca2 OW16 H16B 50(6) 1_445 . ? Ca1 OW16 H16B 132(6) . . ? H16A OW16 H16B 105(8) . . ? Ca2 OW17 Ca1 98.8(6) 1_445 . ? Ca2 OW17 H17A 45(6) 1_445 . ? Ca1 OW17 H17A 126(6) . . ? Ca2 OW17 H17B 129(5) 1_445 . ? Ca1 OW17 H17B 80(5) . . ? H17A OW17 H17B 152(7) . . ? 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) 1.959(19) 2.925(5) 169(8) 3_665 OH15 H15 O10 0.977(2) 2.31(8) 2.947(5) 122(7) 1_455 OW16 H16A O10 0.979(2) 2.24(3) 3.187(7) 162(8) 3_775 OW16 H16B O8 0.979(2) 2.07(2) 3.038(8) 169(8) 2_654 OW17 H17B O13 0.978(2) 2.46(9) 2.841(6) 103(6) 1_545 OW17 H17B OW16 0.978(2) 2.14(6) 2.872(6) 130(6) 1_545 OW17 H17A O6 0.980(2) 2.09(3) 3.047(6) 164(8) 2_644 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.882 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.149