data_chiavit _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 8.749(3) _cell_length_b 4.9090(15) _cell_length_c 31.338(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.236(9) _cell_angle_gamma 90.00 _cell_volume 1345.9(7) _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 2.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 1.908 _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 15707 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0313 _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 30.10 _reflns_number_total 3951 _reflns_number_gt 3658 _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^)+(0.0422P)^2^+11.4009P] 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 3951 _refine_ls_number_parameters 261 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.001 _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 0.0112(4) Uani 1.019(7) 2 d SP . . Mn2 Mn 1.0000 0.5000 0.0000 0.0112(3) Uani 1 2 d S . . Ca Ca 0.75065(19) 0.4999(3) -0.08849(3) 0.0146(2) Uani 1 1 d . . . Si1 Si 0.7497(2) 0.0015(4) -0.00148(4) 0.0083(2) Uani 1 1 d . . . Si2 Si 0.41566(19) 0.5896(3) -0.23239(5) 0.0105(3) Uani 1 1 d . . . Si22 Si 0.0836(2) 0.3748(3) -0.23212(5) 0.0104(3) Uani 1 1 d . . . Si3 Si 0.14024(19) 0.2297(3) -0.13471(5) 0.0106(3) Uani 1 1 d . . . Si33 Si 0.3549(2) 0.7200(3) -0.13548(5) 0.0105(3) Uani 1 1 d . . . Be4 Be 0.5020(9) 0.0709(14) 0.0574(2) 0.014(2) Uani 0.961(12) 1 d P . . Si4 Si 0.5020(9) 0.0709(14) 0.0574(2) 0.014(2) Uani 0.039(12) 1 d P . . Be44 Be 1.0024(9) 0.9238(14) 0.0571(2) 0.012(2) Uani 0.965(12) 1 d P . . Si44 Si 1.0024(9) 0.9238(14) 0.0571(2) 0.012(2) Uani 0.035(12) 1 d P . . O1 O 0.6512(5) -0.2030(9) -0.03296(13) 0.0097(7) Uani 1 1 d . . . O2 O 0.8465(5) 0.2067(8) -0.03221(13) 0.0096(7) Uani 1 1 d . . . O3 O 0.8611(5) -0.1884(9) 0.02776(13) 0.0119(8) Uani 1 1 d . . . O4 O 0.6410(5) 0.1889(9) 0.02807(13) 0.0112(8) Uani 1 1 d . . . O5 O 0.2486(7) 0.4861(12) -0.24786(12) 0.0231(8) Uani 1 1 d . . . O6 O 0.4617(6) 0.8403(10) -0.26371(17) 0.0247(11) Uani 1 1 d . . . O7 O 0.4190(6) 0.6888(12) -0.18331(16) 0.0285(12) Uani 1 1 d . . . O8 O 0.0462(6) 0.1064(11) -0.2599(2) 0.0304(13) Uani 1 1 d . . . O9 O 0.0815(7) 0.3087(13) -0.18194(15) 0.0311(13) Uani 1 1 d . . . O10 O 0.0021(6) 0.7763(9) 0.10340(14) 0.0149(9) Uani 1 1 d . . . O11 O 0.2149(6) 0.9276(12) -0.1357(2) 0.0384(14) Uani 1 1 d . . . O12 O 0.2774(5) 0.4336(10) -0.11992(15) 0.0258(11) Uani 1 1 d . . . O13 O 0.4962(5) 0.7984(9) -0.10530(13) 0.0139(8) Uani 1 1 d . . . OH14 O 0.4911(6) 0.7392(8) 0.05793(14) 0.0146(9) Uani 1 1 d D . . OH15 O 0.0159(6) 0.2550(8) 0.05790(15) 0.0144(9) Uani 1 1 d D . . OW16 O 0.8343(8) 0.7418(11) -0.15052(19) 0.0313(13) Uani 1 1 d D . . OW17 O 0.6537(7) 0.2253(11) -0.14604(17) 0.0244(11) Uani 1 1 d D . . H14 H 0.573(8) 0.71(2) 0.079(3) 0.050 Uiso 1 1 d D . . H15 H -0.040(10) 0.353(19) 0.080(2) 0.050 Uiso 1 1 d D . . H16A H 0.916(9) 0.853(19) -0.138(3) 0.050 Uiso 1 1 d D . . H16B H 0.869(11) 0.73(2) -0.1801(11) 0.050 Uiso 1 1 d D . . H17A H 0.567(8) 0.25(2) -0.165(3) 0.050 Uiso 1 1 d D . . H17B H 0.633(12) 0.081(15) -0.126(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 0.0165(7) 0.0083(6) 0.0089(6) -0.0006(4) 0.0052(5) -0.0009(4) Mn2 0.0160(6) 0.0073(5) 0.0102(6) -0.0013(4) 0.0009(5) -0.0030(4) Ca 0.0206(4) 0.0121(4) 0.0113(4) -0.0010(4) 0.0032(6) -0.0005(4) Si1 0.0095(5) 0.0084(5) 0.0070(5) -0.0003(5) 0.0046(7) -0.0024(5) Si2 0.0117(7) 0.0113(7) 0.0084(7) -0.0012(5) 0.0047(6) -0.0014(5) Si22 0.0127(7) 0.0102(6) 0.0083(7) 0.0015(5) 0.0022(6) -0.0012(5) Si3 0.0098(7) 0.0137(7) 0.0083(7) -0.0002(5) 0.0020(6) 0.0010(5) Si33 0.0127(7) 0.0110(6) 0.0076(6) -0.0017(5) 0.0018(6) -0.0006(5) Be4 0.015(4) 0.013(3) 0.015(4) -0.002(2) 0.002(3) -0.005(3) Si4 0.015(4) 0.013(3) 0.015(4) -0.002(2) 0.002(3) -0.005(3) Be44 0.014(3) 0.013(3) 0.010(3) 0.002(2) 0.001(2) 0.000(2) Si44 0.014(3) 0.013(3) 0.010(3) 0.002(2) 0.001(2) 0.000(2) O1 0.0096(18) 0.0112(17) 0.0082(17) -0.0010(14) 0.0018(15) -0.0014(15) O2 0.0111(19) 0.0089(16) 0.0089(18) 0.0032(14) 0.0037(15) -0.0011(15) O3 0.0107(19) 0.0138(18) 0.0112(19) 0.0026(15) 0.0019(15) -0.0019(16) O4 0.014(2) 0.0110(17) 0.0083(18) -0.0033(14) 0.0085(16) -0.0026(16) O5 0.0203(18) 0.031(2) 0.0184(17) -0.007(2) 0.006(2) -0.0105(17) O6 0.034(3) 0.019(2) 0.022(2) 0.0037(19) 0.000(2) -0.006(2) O7 0.024(3) 0.047(3) 0.014(2) -0.008(2) 0.006(2) -0.007(3) O8 0.021(3) 0.025(3) 0.045(3) -0.014(2) 0.002(2) -0.010(2) O9 0.027(3) 0.057(4) 0.009(2) 0.010(2) 0.002(2) -0.013(3) O10 0.014(2) 0.022(2) 0.0088(18) 0.0068(16) 0.0050(16) 0.0014(18) O11 0.023(3) 0.037(3) 0.056(3) -0.015(3) -0.011(2) 0.017(2) O12 0.023(3) 0.030(3) 0.024(2) 0.0106(19) -0.0108(18) -0.013(2) O13 0.015(2) 0.020(2) 0.0067(17) -0.0024(15) 0.0049(16) -0.0082(18) OH14 0.023(2) 0.0092(19) 0.011(2) 0.0049(14) 0.0002(18) -0.0041(16) OH15 0.015(2) 0.013(2) 0.016(2) -0.0036(15) 0.0097(17) 0.0003(16) OW16 0.041(3) 0.026(3) 0.027(3) 0.007(2) 0.014(2) 0.003(2) OW17 0.028(3) 0.027(2) 0.019(2) -0.0031(19) -0.004(2) -0.006(2) _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 2.149(5) 3_665 ? Mn1 O4 2.149(5) . ? Mn1 OH14 2.164(4) 3_665 ? Mn1 OH14 2.164(4) . ? Mn1 O1 2.226(4) 3_655 ? Mn1 O1 2.226(4) 1_565 ? Mn1 Be4 2.771(7) . ? Mn1 Be4 2.771(7) 3_665 ? Mn1 Si4 2.771(7) 3_665 ? Mn1 Ca 3.5425(14) . ? Mn1 Ca 3.5426(14) 3_665 ? Mn2 O3 2.141(4) 3_755 ? Mn2 O3 2.141(4) 1_565 ? Mn2 OH15 2.181(5) 3_665 ? Mn2 OH15 2.181(5) 1_655 ? Mn2 O2 2.210(4) 3_765 ? Mn2 O2 2.210(4) . ? Mn2 Be44 2.744(7) . ? Mn2 Si44 2.744(7) 3_765 ? Mn2 Be44 2.744(7) 3_765 ? Mn2 Ca 3.5213(15) . ? Mn2 Ca 3.5213(15) 3_765 ? Ca OW16 2.395(6) . ? Ca OW17 2.404(5) . ? Ca O2 2.424(4) . ? Ca O1 2.434(4) 1_565 ? Ca OH15 2.554(5) 3_665 ? Ca O10 2.597(5) 3_665 ? Ca OH14 2.605(5) 3_665 ? Ca O13 2.715(5) . ? Ca Si44 3.154(7) 3_765 ? Ca Be44 3.154(7) 3_765 ? Ca Be4 3.208(8) 3_665 ? Ca Si4 3.208(8) 3_665 ? Ca H16A 2.74(9) . ? Ca H17B 2.58(10) . ? Si1 O4 1.618(4) . ? Si1 O3 1.628(5) . ? Si1 O2 1.633(4) . ? Si1 O1 1.649(4) . ? Si1 Si44 2.812(7) 3_765 ? Si1 Si4 2.832(8) 3_655 ? Si2 O7 1.614(5) . ? Si2 O5 1.620(6) . ? Si2 O6 1.626(5) . ? Si2 O6 1.632(5) 2_644 ? Si22 O9 1.606(5) . ? Si22 O8 1.612(5) . ? Si22 O5 1.623(6) . ? Si22 O8 1.625(5) 2_554 ? Si3 O10 1.589(5) 3_565 ? Si3 O9 1.612(5) . ? Si3 O11 1.621(6) 1_545 ? Si3 O12 1.628(5) . ? Si3 Si44 2.840(7) 3_665 ? Si33 O11 1.593(5) . ? Si33 O13 1.600(5) . ? Si33 O7 1.610(5) . ? Si33 O12 1.636(5) . ? Be4 OH14 1.631(8) 1_545 ? Be4 O13 1.632(8) 3_665 ? Be4 O4 1.634(8) . ? Be4 O1 1.672(9) 3_655 ? Be4 Ca 3.208(8) 3_665 ? Be44 O10 1.622(8) 1_655 ? Be44 OH15 1.630(8) 1_665 ? Be44 O3 1.633(9) 1_565 ? Be44 O2 1.666(8) 3_765 ? Be44 Ca 3.154(7) 3_765 ? O1 Si4 1.672(9) 3_655 ? O1 Be4 1.672(9) 3_655 ? O1 Mn1 2.226(4) 1_545 ? O1 Ca 2.434(4) 1_545 ? O2 Si44 1.666(8) 3_765 ? O2 Be44 1.666(8) 3_765 ? O3 Si44 1.633(9) 1_545 ? O3 Be44 1.633(9) 1_545 ? O3 Mn2 2.141(4) 1_545 ? O6 Si2 1.632(5) 2_654 ? O8 Si22 1.625(5) 2_544 ? O10 Si3 1.589(5) 3_565 ? O10 Si44 1.621(8) 1_455 ? O10 Be44 1.621(8) 1_455 ? O10 Ca 2.597(5) 3_665 ? O11 Si3 1.621(6) 1_565 ? O13 Si4 1.632(8) 3_665 ? O13 Be4 1.632(8) 3_665 ? OH14 Si4 1.631(8) 1_565 ? OH14 Be4 1.631(8) 1_565 ? OH14 Ca 2.605(5) 3_665 ? OH14 H14 0.980(2) . ? OH15 Si44 1.630(8) 1_445 ? OH15 Be44 1.630(8) 1_445 ? OH15 Mn2 2.181(5) 1_455 ? OH15 Ca 2.553(5) 3_665 ? OH15 H15 0.980(2) . ? OW16 H16A 0.980(2) . ? OW16 H16B 0.980(2) . ? OW17 H17A 0.969(2) . ? OW17 H17B 0.960(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 93.71(16) 3_665 3_665 ? O4 Mn1 OH14 86.29(16) . 3_665 ? O4 Mn1 OH14 86.29(16) 3_665 . ? O4 Mn1 OH14 93.71(16) . . ? OH14 Mn1 OH14 180.0(3) 3_665 . ? O4 Mn1 O1 108.32(15) 3_665 3_655 ? O4 Mn1 O1 71.68(15) . 3_655 ? OH14 Mn1 O1 93.29(15) 3_665 3_655 ? OH14 Mn1 O1 86.71(15) . 3_655 ? O4 Mn1 O1 71.68(15) 3_665 1_565 ? O4 Mn1 O1 108.32(15) . 1_565 ? OH14 Mn1 O1 86.71(15) 3_665 1_565 ? OH14 Mn1 O1 93.29(15) . 1_565 ? O1 Mn1 O1 180.0(2) 3_655 1_565 ? O4 Mn1 Be4 143.92(19) 3_665 . ? O4 Mn1 Be4 36.08(19) . . ? OH14 Mn1 Be4 97.60(18) 3_665 . ? OH14 Mn1 Be4 82.40(18) . . ? O1 Mn1 Be4 37.11(19) 3_655 . ? O1 Mn1 Be4 142.89(19) 1_565 . ? O4 Mn1 Be4 36.08(19) 3_665 3_665 ? O4 Mn1 Be4 143.92(19) . 3_665 ? OH14 Mn1 Be4 82.39(18) 3_665 3_665 ? OH14 Mn1 Be4 97.61(18) . 3_665 ? O1 Mn1 Be4 142.89(19) 3_655 3_665 ? O1 Mn1 Be4 37.11(19) 1_565 3_665 ? Be4 Mn1 Be4 180.0 . 3_665 ? O4 Mn1 Si4 36.08(19) 3_665 3_665 ? O4 Mn1 Si4 143.92(19) . 3_665 ? OH14 Mn1 Si4 82.39(18) 3_665 3_665 ? OH14 Mn1 Si4 97.61(18) . 3_665 ? O1 Mn1 Si4 142.89(19) 3_655 3_665 ? O1 Mn1 Si4 37.11(19) 1_565 3_665 ? Be4 Mn1 Si4 180.0 . 3_665 ? Be4 Mn1 Si4 0.0(4) 3_665 3_665 ? O4 Mn1 Ca 92.05(11) 3_665 . ? O4 Mn1 Ca 87.95(11) . . ? OH14 Mn1 Ca 47.06(13) 3_665 . ? OH14 Mn1 Ca 132.94(13) . . ? O1 Mn1 Ca 137.24(11) 3_655 . ? O1 Mn1 Ca 42.76(11) 1_565 . ? Be4 Mn1 Ca 120.41(15) . . ? Be4 Mn1 Ca 59.59(15) 3_665 . ? Si4 Mn1 Ca 59.59(15) 3_665 . ? O4 Mn1 Ca 87.95(11) 3_665 3_665 ? O4 Mn1 Ca 92.05(11) . 3_665 ? OH14 Mn1 Ca 132.94(13) 3_665 3_665 ? OH14 Mn1 Ca 47.06(13) . 3_665 ? O1 Mn1 Ca 42.76(11) 3_655 3_665 ? O1 Mn1 Ca 137.24(11) 1_565 3_665 ? Be4 Mn1 Ca 59.59(15) . 3_665 ? Be4 Mn1 Ca 120.42(15) 3_665 3_665 ? Si4 Mn1 Ca 120.42(15) 3_665 3_665 ? Ca Mn1 Ca 180.0 . 3_665 ? O3 Mn2 O3 180.0(3) 3_755 1_565 ? O3 Mn2 OH15 95.19(16) 3_755 3_665 ? O3 Mn2 OH15 84.81(16) 1_565 3_665 ? O3 Mn2 OH15 84.81(16) 3_755 1_655 ? O3 Mn2 OH15 95.19(16) 1_565 1_655 ? OH15 Mn2 OH15 180.0(2) 3_665 1_655 ? O3 Mn2 O2 107.84(15) 3_755 3_765 ? O3 Mn2 O2 72.16(15) 1_565 3_765 ? OH15 Mn2 O2 93.29(16) 3_665 3_765 ? OH15 Mn2 O2 86.71(16) 1_655 3_765 ? O3 Mn2 O2 72.16(15) 3_755 . ? O3 Mn2 O2 107.84(15) 1_565 . ? OH15 Mn2 O2 86.71(16) 3_665 . ? OH15 Mn2 O2 93.29(16) 1_655 . ? O2 Mn2 O2 180.0 3_765 . ? O3 Mn2 Be44 143.5(2) 3_755 . ? O3 Mn2 Be44 36.5(2) 1_565 . ? OH15 Mn2 Be44 97.16(18) 3_665 . ? OH15 Mn2 Be44 82.84(18) 1_655 . ? O2 Mn2 Be44 37.36(19) 3_765 . ? O2 Mn2 Be44 142.64(19) . . ? O3 Mn2 Si44 36.5(2) 3_755 3_765 ? O3 Mn2 Si44 143.5(2) 1_565 3_765 ? OH15 Mn2 Si44 82.84(18) 3_665 3_765 ? OH15 Mn2 Si44 97.16(18) 1_655 3_765 ? O2 Mn2 Si44 142.64(19) 3_765 3_765 ? O2 Mn2 Si44 37.36(19) . 3_765 ? Be44 Mn2 Si44 179.999(1) . 3_765 ? O3 Mn2 Be44 36.5(2) 3_755 3_765 ? O3 Mn2 Be44 143.5(2) 1_565 3_765 ? OH15 Mn2 Be44 82.84(18) 3_665 3_765 ? OH15 Mn2 Be44 97.16(18) 1_655 3_765 ? O2 Mn2 Be44 142.64(19) 3_765 3_765 ? O2 Mn2 Be44 37.36(19) . 3_765 ? Be44 Mn2 Be44 179.999(1) . 3_765 ? Si44 Mn2 Be44 0.0(4) 3_765 3_765 ? O3 Mn2 Ca 91.77(12) 3_755 . ? O3 Mn2 Ca 88.23(12) 1_565 . ? OH15 Mn2 Ca 46.18(13) 3_665 . ? OH15 Mn2 Ca 133.82(13) 1_655 . ? O2 Mn2 Ca 137.14(11) 3_765 . ? O2 Mn2 Ca 42.86(11) . . ? Be44 Mn2 Ca 121.11(15) . . ? Si44 Mn2 Ca 58.89(15) 3_765 . ? Be44 Mn2 Ca 58.89(15) 3_765 . ? O3 Mn2 Ca 88.23(12) 3_755 3_765 ? O3 Mn2 Ca 91.77(12) 1_565 3_765 ? OH15 Mn2 Ca 133.82(13) 3_665 3_765 ? OH15 Mn2 Ca 46.18(13) 1_655 3_765 ? O2 Mn2 Ca 42.86(11) 3_765 3_765 ? O2 Mn2 Ca 137.14(11) . 3_765 ? Be44 Mn2 Ca 58.89(15) . 3_765 ? Si44 Mn2 Ca 121.11(15) 3_765 3_765 ? Be44 Mn2 Ca 121.11(15) 3_765 3_765 ? Ca Mn2 Ca 180.0 . 3_765 ? OW16 Ca OW17 77.13(19) . . ? OW16 Ca O2 141.2(2) . . ? OW17 Ca O2 109.44(17) . . ? OW16 Ca O1 113.24(17) . 1_565 ? OW17 Ca O1 138.28(19) . 1_565 ? O2 Ca O1 87.67(11) . 1_565 ? OW16 Ca OH15 79.9(2) . 3_665 ? OW17 Ca OH15 145.61(18) . 3_665 ? O2 Ca OH15 74.50(15) . 3_665 ? O1 Ca OH15 74.75(14) 1_565 3_665 ? OW16 Ca O10 81.68(18) . 3_665 ? OW17 Ca O10 82.17(18) . 3_665 ? O2 Ca O10 62.27(14) . 3_665 ? O1 Ca O10 137.90(15) 1_565 3_665 ? OH15 Ca O10 69.40(15) 3_665 3_665 ? OW16 Ca OH14 140.6(2) . 3_665 ? OW17 Ca OH14 74.84(17) . 3_665 ? O2 Ca OH14 75.17(15) . 3_665 ? O1 Ca OH14 73.37(14) 1_565 3_665 ? OH15 Ca OH14 136.36(11) 3_665 3_665 ? O10 Ca OH14 120.60(15) 3_665 3_665 ? OW16 Ca O13 80.10(18) . . ? OW17 Ca O13 82.56(17) . . ? O2 Ca O13 137.97(14) . . ? O1 Ca O13 61.32(14) 1_565 . ? OH15 Ca O13 118.19(14) 3_665 . ? O10 Ca O13 158.41(11) 3_665 . ? OH14 Ca O13 69.39(14) 3_665 . ? OW16 Ca Si44 111.6(2) . 3_765 ? OW17 Ca Si44 95.92(19) . 3_765 ? O2 Ca Si44 31.42(16) . 3_765 ? O1 Ca Si44 114.76(16) 1_565 3_765 ? OH15 Ca Si44 69.39(17) 3_665 3_765 ? O10 Ca Si44 30.86(15) 3_665 3_765 ? OH14 Ca Si44 98.31(17) 3_665 3_765 ? O13 Ca Si44 167.60(16) . 3_765 ? OW16 Ca Be44 111.6(2) . 3_765 ? OW17 Ca Be44 95.92(19) . 3_765 ? O2 Ca Be44 31.42(16) . 3_765 ? O1 Ca Be44 114.76(16) 1_565 3_765 ? OH15 Ca Be44 69.39(17) 3_665 3_765 ? O10 Ca Be44 30.86(15) 3_665 3_765 ? OH14 Ca Be44 98.31(17) 3_665 3_765 ? O13 Ca Be44 167.60(16) . 3_765 ? Si44 Ca Be44 0.0(3) 3_765 3_765 ? OW16 Ca Be4 97.70(19) . 3_665 ? OW17 Ca Be4 110.8(2) . 3_665 ? O2 Ca Be4 113.97(16) . 3_665 ? O1 Ca Be4 30.76(17) 1_565 3_665 ? OH15 Ca Be4 97.33(17) 3_665 3_665 ? O10 Ca Be4 166.66(18) 3_665 3_665 ? OH14 Ca Be4 67.84(16) 3_665 3_665 ? O13 Ca Be4 30.56(15) . 3_665 ? Si44 Ca Be4 144.16(14) 3_765 3_665 ? Be44 Ca Be4 144.16(14) 3_765 3_665 ? OW16 Ca Si4 97.70(19) . 3_665 ? OW17 Ca Si4 110.8(2) . 3_665 ? O2 Ca Si4 113.97(16) . 3_665 ? O1 Ca Si4 30.76(17) 1_565 3_665 ? OH15 Ca Si4 97.33(17) 3_665 3_665 ? O10 Ca Si4 166.66(18) 3_665 3_665 ? OH14 Ca Si4 67.84(16) 3_665 3_665 ? O13 Ca Si4 30.56(15) . 3_665 ? Si44 Ca Si4 144.16(14) 3_765 3_665 ? Be44 Ca Si4 144.16(14) 3_765 3_665 ? Be4 Ca Si4 0.0(4) 3_665 3_665 ? OW16 Ca H16A 20.6(12) . . ? OW17 Ca H16A 96.6(13) . . ? O2 Ca H16A 127.2(17) . . ? O1 Ca H16A 103(2) 1_565 . ? OH15 Ca H16A 59.5(12) 3_665 . ? O10 Ca H16A 78(2) 3_665 . ? OH14 Ca H16A 157.5(19) 3_665 . ? O13 Ca H16A 89(2) . . ? Si44 Ca H16A 103(2) 3_765 . ? Be44 Ca H16A 103(2) 3_765 . ? Be4 Ca H16A 97(2) 3_665 . ? Si4 Ca H16A 97(2) 3_665 . ? OW16 Ca H17B 98.4(10) . . ? OW17 Ca H17B 21.8(9) . . ? O2 Ca H17B 89.8(13) . . ? O1 Ca H17B 131(2) 1_565 . ? OH15 Ca H17B 150(2) 3_665 . ? O10 Ca H17B 80(2) 3_665 . ? OH14 Ca H17B 59.1(18) 3_665 . ? O13 Ca H17B 91(2) . . ? Si44 Ca H17B 84(2) 3_765 . ? Be44 Ca H17B 84(2) 3_765 . ? Be4 Ca H17B 113(2) 3_665 . ? Si4 Ca H17B 113(2) 3_665 . ? H16A Ca H17B 117.0(18) . . ? O4 Si1 O3 110.82(18) . . ? O4 Si1 O2 107.1(2) . . ? O3 Si1 O2 112.0(2) . . ? O4 Si1 O1 112.4(2) . . ? O3 Si1 O1 107.4(3) . . ? O2 Si1 O1 107.09(17) . . ? O4 Si1 Si44 137.5(2) . 3_765 ? O3 Si1 Si44 87.8(2) . 3_765 ? O2 Si1 Si44 31.9(2) . 3_765 ? O1 Si1 Si44 96.4(2) . 3_765 ? O4 Si1 Si4 88.2(2) . 3_655 ? O3 Si1 Si4 137.6(2) . 3_655 ? O2 Si1 Si4 96.7(2) . 3_655 ? O1 Si1 Si4 31.7(2) . 3_655 ? Si44 Si1 Si4 103.43(16) 3_765 3_655 ? O7 Si2 O5 113.1(3) . . ? O7 Si2 O6 110.1(3) . . ? O5 Si2 O6 106.4(3) . . ? O7 Si2 O6 106.8(3) . 2_644 ? O5 Si2 O6 109.6(3) . 2_644 ? O6 Si2 O6 110.96(12) . 2_644 ? O9 Si22 O8 111.1(3) . . ? O9 Si22 O5 112.3(3) . . ? O8 Si22 O5 106.9(3) . . ? O9 Si22 O8 106.4(3) . 2_554 ? O8 Si22 O8 110.39(14) . 2_554 ? O5 Si22 O8 109.9(3) . 2_554 ? O10 Si3 O9 108.9(3) 3_565 . ? O10 Si3 O11 108.2(3) 3_565 1_545 ? O9 Si3 O11 109.3(3) . 1_545 ? O10 Si3 O12 114.5(3) 3_565 . ? O9 Si3 O12 110.2(3) . . ? O11 Si3 O12 105.7(3) 1_545 . ? O10 Si3 Si44 28.1(2) 3_565 3_665 ? O9 Si3 Si44 135.3(3) . 3_665 ? O11 Si3 Si44 87.2(3) 1_545 3_665 ? O12 Si3 Si44 104.2(2) . 3_665 ? O11 Si33 O13 116.1(3) . . ? O11 Si33 O7 109.1(3) . . ? O13 Si33 O7 107.6(3) . . ? O11 Si33 O12 103.4(3) . . ? O13 Si33 O12 110.5(2) . . ? O7 Si33 O12 110.0(3) . . ? OH14 Be4 O13 112.6(5) 1_545 3_665 ? OH14 Be4 O4 113.7(5) 1_545 . ? O13 Be4 O4 111.9(5) 3_665 . ? OH14 Be4 O1 110.2(5) 1_545 3_655 ? O13 Be4 O1 105.9(5) 3_665 3_655 ? O4 Be4 O1 101.6(4) . 3_655 ? OH14 Be4 Mn1 139.9(4) 1_545 . ? O13 Be4 Mn1 107.3(4) 3_665 . ? O4 Be4 Mn1 50.8(2) . . ? O1 Be4 Mn1 53.4(2) 3_655 . ? OH14 Be4 Ca 127.8(4) 1_545 3_665 ? O13 Be4 Ca 57.8(3) 3_665 3_665 ? O4 Be4 Ca 117.0(4) . 3_665 ? O1 Be4 Ca 48.1(2) 3_655 3_665 ? Mn1 Be4 Ca 72.26(17) . 3_665 ? O10 Be44 OH15 115.6(5) 1_655 1_665 ? O10 Be44 O3 110.4(5) 1_655 1_565 ? OH15 Be44 O3 113.6(5) 1_665 1_565 ? O10 Be44 O2 104.6(4) 1_655 3_765 ? OH15 Be44 O2 109.4(5) 1_665 3_765 ? O3 Be44 O2 101.9(4) 1_565 3_765 ? O10 Be44 Mn2 104.2(4) 1_655 . ? OH15 Be44 Mn2 140.0(4) 1_665 . ? O3 Be44 Mn2 51.2(2) 1_565 . ? O2 Be44 Mn2 53.6(2) 3_765 . ? O10 Be44 Ca 55.3(3) 1_655 3_765 ? OH15 Be44 Ca 127.1(4) 1_665 3_765 ? O3 Be44 Ca 118.0(4) 1_565 3_765 ? O2 Be44 Ca 49.3(2) 3_765 3_765 ? Mn2 Be44 Ca 72.94(17) . 3_765 ? Si1 O1 Si4 117.0(3) . 3_655 ? Si1 O1 Be4 117.0(3) . 3_655 ? Si4 O1 Be4 0.0(6) 3_655 3_655 ? Si1 O1 Mn1 115.6(2) . 1_545 ? Si4 O1 Mn1 89.5(3) 3_655 1_545 ? Be4 O1 Mn1 89.5(3) 3_655 1_545 ? Si1 O1 Ca 127.2(2) . 1_545 ? Si4 O1 Ca 101.1(3) 3_655 1_545 ? Be4 O1 Ca 101.1(3) 3_655 1_545 ? Mn1 O1 Ca 98.87(16) 1_545 1_545 ? Si1 O2 Si44 117.0(3) . 3_765 ? Si1 O2 Be44 117.0(3) . 3_765 ? Si44 O2 Be44 0.0(5) 3_765 3_765 ? Si1 O2 Mn2 116.6(2) . . ? Si44 O2 Mn2 89.0(3) 3_765 . ? Be44 O2 Mn2 89.0(3) 3_765 . ? Si1 O2 Ca 128.1(2) . . ? Si44 O2 Ca 99.2(3) 3_765 . ? Be44 O2 Ca 99.2(3) 3_765 . ? Mn2 O2 Ca 98.81(16) . . ? Si1 O3 Si44 125.0(4) . 1_545 ? Si1 O3 Be44 125.0(4) . 1_545 ? Si44 O3 Be44 0.0(5) 1_545 1_545 ? Si1 O3 Mn2 121.3(2) . 1_545 ? Si44 O3 Mn2 92.3(3) 1_545 1_545 ? Be44 O3 Mn2 92.3(3) 1_545 1_545 ? Si1 O4 Be4 124.2(4) . . ? Si1 O4 Mn1 120.5(2) . . ? Be4 O4 Mn1 93.2(3) . . ? Si2 O5 Si22 144.8(3) . . ? Si2 O6 Si2 141.0(4) . 2_654 ? Si33 O7 Si2 155.7(4) . . ? Si22 O8 Si22 142.7(4) . 2_544 ? Si22 O9 Si3 160.5(4) . . ? Si3 O10 Si44 124.4(4) 3_565 1_455 ? Si3 O10 Be44 124.4(4) 3_565 1_455 ? Si44 O10 Be44 0.0(6) 1_455 1_455 ? Si3 O10 Ca 139.2(2) 3_565 3_665 ? Si44 O10 Ca 93.9(3) 1_455 3_665 ? Be44 O10 Ca 93.9(3) 1_455 3_665 ? Si33 O11 Si3 153.5(4) . 1_565 ? Si3 O12 Si33 138.5(3) . . ? Si33 O13 Si4 130.0(4) . 3_665 ? Si33 O13 Be4 130.0(4) . 3_665 ? Si4 O13 Be4 0.0(6) 3_665 3_665 ? Si33 O13 Ca 128.0(2) . . ? Si4 O13 Ca 91.7(3) 3_665 . ? Be4 O13 Ca 91.7(3) 3_665 . ? Si4 OH14 Be4 0.0(5) 1_565 1_565 ? Si4 OH14 Mn1 122.1(3) 1_565 . ? Be4 OH14 Mn1 122.1(3) 1_565 . ? Si4 OH14 Ca 120.0(4) 1_565 3_665 ? Be4 OH14 Ca 120.0(4) 1_565 3_665 ? Mn1 OH14 Ca 95.50(17) . 3_665 ? Si4 OH14 H14 97(6) 1_565 . ? Be4 OH14 H14 97(6) 1_565 . ? Mn1 OH14 H14 116(6) . . ? Ca OH14 H14 106(6) 3_665 . ? Si44 OH15 Be44 0.0(7) 1_445 1_445 ? Si44 OH15 Mn2 122.2(4) 1_445 1_455 ? Be44 OH15 Mn2 122.2(4) 1_445 1_455 ? Si44 OH15 Ca 122.3(4) 1_445 3_665 ? Be44 OH15 Ca 122.3(4) 1_445 3_665 ? Mn2 OH15 Ca 95.78(16) 1_455 3_665 ? Si44 OH15 H15 118(6) 1_445 . ? Be44 OH15 H15 118(6) 1_445 . ? Mn2 OH15 H15 107(6) 1_455 . ? Ca OH15 H15 84(6) 3_665 . ? Ca OW16 H16A 100(7) . . ? Ca OW16 H16B 148(6) . . ? H16A OW16 H16B 100(8) . . ? Ca OW17 H17A 132(6) . . ? Ca OW17 H17B 90(6) . . ? H17A OW17 H17B 110(9) . . ? 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 0.980(2) 1.96(2) 2.926(7) 168(9) 3_665 OH15 H15 O10 0.980(2) 2.23(8) 2.933(6) 128(8) . OW16 H16A O10 0.980(2) 2.24(5) 3.132(8) 151(9) 3_675 OW16 H16B O8 0.980(2) 2.12(3) 3.073(9) 164(9) 2_654 OW17 H17B O13 0.960(2) 1.95(5) 2.817(7) 149(9) 1_545 OW17 H17B OW16 0.960(2) 2.54(10) 2.855(7) 99(7) 1_545 OW17 H17A O6 0.969(2) 2.29(8) 3.052(7) 135(8) 2_644 OW17 H17A O7 0.969(2) 2.58(8) 3.277(9) 129(8) . OW17 H17B OH14 0.960(2) 2.56(10) 3.048(7) 112(7) 3_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.118 _refine_diff_density_min -1.088 _refine_diff_density_rms 0.174