# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr Mark Weller' _publ_contact_author_email MTW@SOTON.AC.UK _publ_author_name M.Weller # Attachment '- BAF1011.cif' data_BAF1011 _database_code_depnum_ccdc_archive 'CCDC 807052' #TrackingRef '- BAF1011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As3 Be3 H3 O13, C5 H6 N' _chemical_formula_sum 'C5 H9 As3 Be3 N O13' _chemical_formula_weight 542.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.2341(6) _cell_length_b 4.91270(10) _cell_length_c 24.6048(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.7180(10) _cell_angle_gamma 90.00 _cell_volume 2781.01(10) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16959 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 7.242 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 3567 _diffrn_standards_interval_count 10981 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16316 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3197 _reflns_number_gt 2751 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0000P)^2^+42.3673P] 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 3197 _refine_ls_number_parameters 238 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.138 _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 As1 As 0.178692(19) 0.80184(9) 0.24364(2) 0.00591(11) Uani 1 1 d . . . As2 As 0.050636(19) 0.85473(9) 0.34221(2) 0.00650(11) Uani 1 1 d . . . As3 As 0.261890(19) 0.97593(9) 0.56991(2) 0.00630(11) Uani 1 1 d . . . Be1 Be 0.0691(3) 1.0009(13) 0.2379(3) 0.0112(12) Uani 1 1 d . . . Be2 Be 0.1749(2) 1.0171(12) 0.4338(3) 0.0085(11) Uani 1 1 d . . . Be3 Be 0.2582(3) 1.1908(12) 0.6843(3) 0.0094(12) Uani 1 1 d . . . O1 O 0.18458(13) 0.4753(6) 0.26578(14) 0.0080(6) Uani 1 1 d . . . O2 O 0.20313(13) 0.8586(7) 0.19409(14) 0.0107(7) Uani 1 1 d . . . O3 O 0.21855(13) 0.9874(6) 0.31022(14) 0.0083(6) Uani 1 1 d . . . O4 O 0.10901(13) 0.8898(7) 0.21000(14) 0.0086(7) Uani 1 1 d . . . O6 O 0.06560(13) 0.7693(6) 0.28537(14) 0.0084(6) Uani 1 1 d . . . O7 O 0.02791(15) 0.5761(7) 0.36595(16) 0.0116(7) Uani 1 1 d D . . H7 H 0.017(2) 0.439(8) 0.343(2) 0.023(17) Uiso 1 1 d D . . O8 O -0.00367(13) 1.0825(7) 0.31602(14) 0.0086(7) Uani 1 1 d . . . O9 O 0.10604(13) 0.9770(7) 0.40544(14) 0.0094(7) Uani 1 1 d . . . O10 O 0.20408(13) 0.8304(6) 0.39756(14) 0.0082(6) Uani 1 1 d . . . O11 O 0.18967(13) 1.3354(7) 0.43734(15) 0.0088(6) Uani 1 1 d . . . O12 O 0.20297(13) 0.8878(7) 0.50376(14) 0.0089(7) Uani 1 1 d . . . O13 O 0.23599(13) 1.1050(6) 0.61384(14) 0.0086(7) Uani 1 1 d . . . N1 N 0.36866(18) 0.8905(9) 0.46413(19) 0.0151(9) Uani 1 1 d . . . H6 H 0.3465 0.8063 0.4753 0.018 Uiso 1 1 calc R . . C1 C 0.3712(2) 0.8032(10) 0.4138(2) 0.0160(11) Uani 1 1 d . . . H1 H 0.3482 0.6577 0.3909 0.019 Uiso 1 1 calc R . . C2 C 0.4076(2) 0.9285(11) 0.3961(2) 0.0167(11) Uani 1 1 d . . . H2 H 0.4105 0.8653 0.3621 0.020 Uiso 1 1 calc R . . C3 C 0.4399(2) 1.1492(11) 0.4295(2) 0.0171(11) Uani 1 1 d . . . H3 H 0.4643 1.2384 0.4177 0.021 Uiso 1 1 calc R . . C4 C 0.4356(2) 1.2382(11) 0.4812(2) 0.0170(11) Uani 1 1 d . . . H4 H 0.4571 1.3870 0.5041 0.020 Uiso 1 1 calc R . . C5 C 0.3994(2) 1.1033(11) 0.4975(2) 0.0160(11) Uani 1 1 d . . . H5 H 0.3962 1.1598 0.5318 0.019 Uiso 1 1 calc R . . O5 O 0.09870(14) 1.2758(7) 0.27762(16) 0.0104(7) Uani 1 1 d D . . H5A H 0.127(2) 1.322(18) 0.273(4) 0.07(3) Uiso 1 1 d D . . H5B H 0.082(2) 1.419(8) 0.280(3) 0.030(18) 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 As1 0.0061(2) 0.0063(2) 0.0057(2) 0.00015(18) 0.00312(17) 0.00028(17) As2 0.0063(2) 0.0071(2) 0.0063(2) -0.00044(18) 0.00314(18) -0.00002(17) As3 0.0070(2) 0.0064(2) 0.0057(2) -0.00039(18) 0.00317(17) -0.00021(17) Be1 0.009(3) 0.011(3) 0.015(3) 0.001(3) 0.007(2) 0.000(2) Be2 0.008(3) 0.009(3) 0.009(3) 0.001(2) 0.005(2) -0.002(2) Be3 0.011(3) 0.006(3) 0.011(3) -0.002(2) 0.005(2) -0.003(2) O1 0.0070(14) 0.0075(15) 0.0081(15) 0.0033(13) 0.0025(12) -0.0002(12) O2 0.0095(16) 0.0134(17) 0.0099(16) 0.0042(14) 0.0051(13) 0.0021(13) O3 0.0108(15) 0.0067(15) 0.0077(15) -0.0014(13) 0.0047(13) -0.0030(13) O4 0.0054(15) 0.0115(17) 0.0065(15) 0.0010(13) 0.0009(12) 0.0007(13) O6 0.0109(16) 0.0066(15) 0.0084(15) 0.0007(13) 0.0054(13) 0.0004(13) O7 0.0185(17) 0.0062(16) 0.0146(17) -0.0022(14) 0.0116(15) -0.0049(14) O8 0.0047(14) 0.0098(16) 0.0098(16) -0.0002(13) 0.0022(12) 0.0013(12) O9 0.0060(15) 0.0131(17) 0.0074(15) -0.0025(13) 0.0019(12) -0.0011(13) O10 0.0105(15) 0.0083(15) 0.0079(15) -0.0002(13) 0.0061(13) 0.0024(13) O11 0.0093(15) 0.0080(15) 0.0116(16) -0.0002(13) 0.0069(13) -0.0019(13) O12 0.0054(14) 0.0140(17) 0.0052(15) -0.0015(13) 0.0008(12) -0.0027(13) O13 0.0100(15) 0.0075(15) 0.0108(16) -0.0014(13) 0.0070(13) -0.0012(13) N1 0.013(2) 0.021(2) 0.014(2) 0.0041(18) 0.0077(17) -0.0005(18) C1 0.016(2) 0.011(2) 0.016(3) 0.003(2) 0.004(2) 0.002(2) C2 0.020(3) 0.019(3) 0.011(2) 0.004(2) 0.007(2) 0.006(2) C3 0.015(2) 0.017(3) 0.022(3) 0.003(2) 0.011(2) -0.003(2) C4 0.016(2) 0.014(2) 0.018(3) -0.002(2) 0.006(2) -0.003(2) C5 0.016(2) 0.020(3) 0.011(2) -0.001(2) 0.006(2) 0.005(2) O5 0.0107(17) 0.0073(16) 0.0151(17) -0.0034(14) 0.0077(14) -0.0004(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 As1 O2 1.651(3) . ? As1 O4 1.661(3) . ? As1 O1 1.677(3) . ? As1 O3 1.721(3) . ? As2 O9 1.649(3) . ? As2 O6 1.677(3) . ? As2 O8 1.678(3) . ? As2 O7 1.705(3) . ? As3 O11 1.650(3) 7_576 ? As3 O13 1.655(3) . ? As3 O12 1.676(3) . ? As3 O10 1.737(3) 7_566 ? Be1 O4 1.599(7) . ? Be1 O5 1.629(7) . ? Be1 O8 1.636(7) 2 ? Be1 O6 1.664(7) . ? Be2 O11 1.604(7) . ? Be2 O9 1.605(6) . ? Be2 O12 1.640(7) . ? Be2 O10 1.696(7) . ? Be3 O2 1.594(7) 6_576 ? Be3 O13 1.597(7) . ? Be3 O1 1.629(7) 7_566 ? Be3 O3 1.676(7) 7_576 ? O1 Be3 1.629(7) 7_566 ? O2 Be3 1.594(7) 6_575 ? O3 Be3 1.676(7) 7_576 ? O8 Be1 1.636(7) 2 ? O10 As3 1.737(3) 7_566 ? O11 As3 1.650(3) 7_576 ? N1 C5 1.334(7) . ? N1 C1 1.343(7) . ? C1 C2 1.370(7) . ? C2 C3 1.378(7) . ? C3 C4 1.399(7) . ? C4 C5 1.367(7) . ? 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 O2 As1 O4 108.23(15) . . ? O2 As1 O1 113.18(16) . . ? O4 As1 O1 108.56(15) . . ? O2 As1 O3 109.84(16) . . ? O4 As1 O3 110.88(15) . . ? O1 As1 O3 106.16(15) . . ? O9 As2 O6 115.11(15) . . ? O9 As2 O8 108.67(16) . . ? O6 As2 O8 110.02(15) . . ? O9 As2 O7 105.32(16) . . ? O6 As2 O7 110.19(16) . . ? O8 As2 O7 107.17(16) . . ? O11 As3 O13 115.77(16) 7_576 . ? O11 As3 O12 116.04(16) 7_576 . ? O13 As3 O12 104.89(16) . . ? O11 As3 O10 106.53(15) 7_576 7_566 ? O13 As3 O10 108.20(15) . 7_566 ? O12 As3 O10 104.69(16) . 7_566 ? O4 Be1 O5 108.6(4) . . ? O4 Be1 O8 112.6(4) . 2 ? O5 Be1 O8 107.2(4) . 2 ? O4 Be1 O6 109.6(4) . . ? O5 Be1 O6 108.5(4) . . ? O8 Be1 O6 110.3(4) 2 . ? O11 Be2 O9 109.6(4) . . ? O11 Be2 O12 110.2(4) . . ? O9 Be2 O12 104.6(4) . . ? O11 Be2 O10 113.4(4) . . ? O9 Be2 O10 113.8(4) . . ? O12 Be2 O10 104.7(4) . . ? O2 Be3 O13 103.8(4) 6_576 . ? O2 Be3 O1 112.5(4) 6_576 7_566 ? O13 Be3 O1 114.2(4) . 7_566 ? O2 Be3 O3 116.9(4) 6_576 7_576 ? O13 Be3 O3 105.4(4) . 7_576 ? O1 Be3 O3 104.1(4) 7_566 7_576 ? Be3 O1 As1 129.2(3) 7_566 . ? Be3 O2 As1 142.0(3) 6_575 . ? Be3 O3 As1 127.4(3) 7_576 . ? Be1 O4 As1 131.7(3) . . ? Be1 O6 As2 121.8(3) . . ? Be1 O8 As2 120.9(3) 2 . ? Be2 O9 As2 138.8(3) . . ? Be2 O10 As3 119.2(3) . 7_566 ? Be2 O11 As3 136.1(3) . 7_576 ? Be2 O12 As3 131.2(3) . . ? Be3 O13 As3 139.4(3) . . ? C5 N1 C1 122.3(5) . . ? N1 C1 C2 120.0(5) . . ? C1 C2 C3 119.1(5) . . ? C2 C3 C4 119.5(5) . . ? C5 C4 C3 119.0(5) . . ? N1 C5 C4 119.9(5) . . ? 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 O7 H7 O8 0.84(2) 1.86(3) 2.664(5) 161(6) 1_545 N1 H6 O12 0.86 1.87 2.730(5) 177.3 7_566 O5 H5A O1 0.85(2) 1.76(3) 2.598(5) 170(9) 1_565 O5 H5B O6 0.85(2) 1.79(3) 2.613(5) 162(6) 1_565 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.894 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.188 # Attachment '- BAF1013.cif' data_BAF1013 _database_code_depnum_ccdc_archive 'CCDC 807053' #TrackingRef '- BAF1013.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As O4, H O1.07, Sr, Be' _chemical_formula_sum 'As Be H O5.07 Sr' _chemical_formula_weight 253.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 5.0833(2) _cell_length_b 7.9685(3) _cell_length_c 10.2929(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.638(2) _cell_angle_gamma 90.00 _cell_volume 416.90(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5787 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 466 _exptl_absorpt_coefficient_mu 20.714 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; Bruker-Nonius APEX II CCD camera on \k-goniostat ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 1033 _diffrn_standards_interval_count 3808 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5767 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.57 _reflns_number_total 961 _reflns_number_gt 892 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_data_reduction ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0000P)^2^+2.5941P] 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 961 _refine_ls_number_parameters 73 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0478 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.004 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 O1 O 0.3267(6) 0.2932(4) 0.5410(3) 0.0108(6) Uani 1 1 d . . . O4 O 0.3213(5) 0.3417(4) 0.7963(3) 0.0098(6) Uani 1 1 d . . . O2 O -0.2528(5) 0.0913(4) 0.4643(3) 0.0106(6) Uani 1 1 d . . . O3 O 0.3188(6) 0.6003(4) 0.6407(3) 0.0121(6) Uani 1 1 d . . . Be1 Be 0.4532(12) 0.4135(7) 0.6578(6) 0.0156(11) Uiso 1 1 d . . . O5 O 0.7703(6) 0.4117(4) 0.6628(3) 0.0100(6) Uani 1 1 d D . . OW1 O 1.0000 0.5000 0.5000 0.012 Uiso 0.137(10) 2 d SP . . H1 H 0.834(10) 0.448(7) 0.593(3) 0.026(15) Uiso 1 1 d D . . Sr1 Sr 0.00486(7) 0.11367(5) 0.67287(4) 0.00828(11) Uani 1 1 d . . . As1 As 0.52068(8) 0.22921(5) 0.41793(4) 0.00724(12) Uani 1 1 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 O1 0.0123(14) 0.0091(14) 0.0111(15) -0.0027(11) 0.0034(11) -0.0013(12) O4 0.0106(13) 0.0107(14) 0.0079(14) 0.0009(11) -0.0028(11) -0.0004(11) O2 0.0101(14) 0.0096(14) 0.0120(15) -0.0004(11) -0.0009(11) 0.0016(12) O3 0.0116(14) 0.0097(14) 0.0151(16) 0.0012(12) 0.0041(12) -0.0025(12) O5 0.0112(14) 0.0101(14) 0.0088(15) -0.0011(11) 0.0017(11) 0.0001(12) Sr1 0.00795(18) 0.00807(19) 0.0088(2) 0.00027(13) 0.00109(14) 0.00091(14) As1 0.0081(2) 0.0061(2) 0.0075(2) -0.00043(14) 0.00043(15) -0.00026(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 Be1 1.662(7) . ? O1 As1 1.692(3) . ? O1 Sr1 2.572(3) . ? O4 Be1 1.682(7) . ? O4 As1 1.699(3) 4_566 ? O4 Sr1 2.730(3) . ? O4 Sr1 2.749(3) 2_556 ? O2 As1 1.658(3) 1_455 ? O2 Sr1 2.509(3) . ? O2 Sr1 2.508(3) 3_556 ? O3 Be1 1.647(6) . ? O3 As1 1.699(3) 3_666 ? O3 Sr1 2.543(3) 2_556 ? Be1 O5 1.612(7) . ? Be1 Sr1 3.307(6) . ? Be1 Sr1 3.331(6) 2_556 ? Be1 Sr1 3.614(6) 2_656 ? Be1 Sr1 3.686(6) 1_655 ? O5 Sr1 2.591(3) 2_656 ? O5 Sr1 2.659(3) 1_655 ? Sr1 O2 2.508(3) 3_556 ? Sr1 O3 2.543(3) 2_546 ? Sr1 O5 2.591(3) 2_646 ? Sr1 O5 2.659(3) 1_455 ? Sr1 O4 2.749(3) 2_546 ? Sr1 Be1 3.331(6) 2_546 ? Sr1 Be1 3.614(6) 2_646 ? Sr1 Be1 3.686(6) 1_455 ? As1 O2 1.658(3) 1_655 ? As1 O3 1.699(3) 3_666 ? As1 O4 1.699(3) 4_565 ? As1 Sr1 3.6942(6) 1_655 ? As1 Sr1 3.7584(5) 4_665 ? As1 Sr1 3.7690(5) 3_656 ? As1 Sr1 3.8286(6) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Be1 O1 As1 119.4(3) . . ? Be1 O1 Sr1 100.5(2) . . ? As1 O1 Sr1 127.37(14) . . ? Be1 O4 As1 119.8(3) . 4_566 ? Be1 O4 Sr1 94.0(2) . . ? As1 O4 Sr1 117.73(14) 4_566 . ? Be1 O4 Sr1 94.4(2) . 2_556 ? As1 O4 Sr1 122.18(14) 4_566 2_556 ? Sr1 O4 Sr1 103.03(9) . 2_556 ? As1 O2 Sr1 123.61(14) 1_455 . ? As1 O2 Sr1 128.42(15) 1_455 3_556 ? Sr1 O2 Sr1 105.49(10) . 3_556 ? Be1 O3 As1 124.1(3) . 3_666 ? Be1 O3 Sr1 103.2(2) . 2_556 ? As1 O3 Sr1 123.49(15) 3_666 2_556 ? O5 Be1 O3 115.1(4) . . ? O5 Be1 O1 113.4(4) . . ? O3 Be1 O1 106.7(4) . . ? O5 Be1 O4 112.2(4) . . ? O3 Be1 O4 103.2(3) . . ? O1 Be1 O4 105.2(4) . . ? O5 Be1 Sr1 133.0(3) . . ? O3 Be1 Sr1 111.9(3) . . ? O1 Be1 Sr1 49.89(19) . . ? O4 Be1 Sr1 55.46(19) . . ? O5 Be1 Sr1 133.8(3) . 2_556 ? O3 Be1 Sr1 48.03(19) . 2_556 ? O1 Be1 Sr1 112.8(3) . 2_556 ? O4 Be1 Sr1 55.39(19) . 2_556 ? Sr1 Be1 Sr1 80.52(13) . 2_556 ? O5 Be1 Sr1 39.84(18) . 2_656 ? O3 Be1 Sr1 88.0(2) . 2_656 ? O1 Be1 Sr1 152.9(3) . 2_656 ? O4 Be1 Sr1 92.9(2) . 2_656 ? Sr1 Be1 Sr1 144.93(19) . 2_656 ? Sr1 Be1 Sr1 94.01(14) 2_556 2_656 ? O5 Be1 Sr1 39.92(18) . 1_655 ? O3 Be1 Sr1 154.8(3) . 1_655 ? O1 Be1 Sr1 86.8(2) . 1_655 ? O4 Be1 Sr1 93.1(2) . 1_655 ? Sr1 Be1 Sr1 93.11(14) . 1_655 ? Sr1 Be1 Sr1 145.54(19) 2_556 1_655 ? Sr1 Be1 Sr1 71.97(11) 2_656 1_655 ? Be1 O5 Sr1 116.7(3) . 2_656 ? Be1 O5 Sr1 117.2(3) . 1_655 ? Sr1 O5 Sr1 109.58(10) 2_656 1_655 ? O2 Sr1 O2 74.51(10) . 3_556 ? O2 Sr1 O3 107.85(9) . 2_546 ? O2 Sr1 O3 136.95(9) 3_556 2_546 ? O2 Sr1 O1 85.24(9) . . ? O2 Sr1 O1 74.83(9) 3_556 . ? O3 Sr1 O1 147.36(9) 2_546 . ? O2 Sr1 O5 137.45(9) . 2_646 ? O2 Sr1 O5 75.06(9) 3_556 2_646 ? O3 Sr1 O5 76.46(9) 2_546 2_646 ? O1 Sr1 O5 114.29(9) . 2_646 ? O2 Sr1 O5 78.49(9) . 1_455 ? O2 Sr1 O5 141.97(9) 3_556 1_455 ? O3 Sr1 O5 76.89(9) 2_546 1_455 ? O1 Sr1 O5 76.72(9) . 1_455 ? O5 Sr1 O5 140.77(6) 2_646 1_455 ? O2 Sr1 O4 138.13(9) . . ? O2 Sr1 O4 113.46(9) 3_556 . ? O3 Sr1 O4 93.42(9) 2_546 . ? O1 Sr1 O4 60.04(9) . . ? O5 Sr1 O4 81.75(9) 2_646 . ? O5 Sr1 O4 71.66(9) 1_455 . ? O2 Sr1 O4 74.52(9) . 2_546 ? O2 Sr1 O4 81.90(9) 3_556 2_546 ? O3 Sr1 O4 58.93(9) 2_546 2_546 ? O1 Sr1 O4 152.54(9) . 2_546 ? O5 Sr1 O4 72.36(8) 2_646 2_546 ? O5 Sr1 O4 115.97(9) 1_455 2_546 ? O4 Sr1 O4 145.45(4) . 2_546 ? O2 Sr1 Be1 111.40(12) . . ? O2 Sr1 Be1 95.34(12) 3_556 . ? O3 Sr1 Be1 121.17(12) 2_546 . ? O1 Sr1 Be1 29.62(12) . . ? O5 Sr1 Be1 100.38(12) 2_646 . ? O5 Sr1 Be1 70.24(12) 1_455 . ? O4 Sr1 Be1 30.49(12) . . ? O4 Sr1 Be1 172.66(12) 2_546 . ? O2 Sr1 Be1 92.99(12) . 2_546 ? O2 Sr1 Be1 109.96(12) 3_556 2_546 ? O3 Sr1 Be1 28.77(12) 2_546 2_546 ? O1 Sr1 Be1 174.29(12) . 2_546 ? O5 Sr1 Be1 70.54(12) 2_646 2_546 ? O5 Sr1 Be1 97.61(12) 1_455 2_546 ? O4 Sr1 Be1 119.14(12) . 2_546 ? O4 Sr1 Be1 30.23(12) 2_546 2_546 ? Be1 Sr1 Be1 148.96(10) . 2_546 ? O2 Sr1 Be1 140.27(11) . 2_646 ? O2 Sr1 Be1 66.35(11) 3_556 2_646 ? O3 Sr1 Be1 96.53(11) 2_546 2_646 ? O1 Sr1 Be1 90.80(12) . 2_646 ? O5 Sr1 Be1 23.49(11) 2_646 2_646 ? O5 Sr1 Be1 138.77(11) 1_455 2_646 ? O4 Sr1 Be1 68.14(11) . 2_646 ? O4 Sr1 Be1 93.07(11) 2_546 2_646 ? Be1 Sr1 Be1 79.60(7) . 2_646 ? Be1 Sr1 Be1 94.01(14) 2_546 2_646 ? O2 Sr1 Be1 67.69(11) . 1_455 ? O2 Sr1 Be1 141.76(11) 3_556 1_455 ? O3 Sr1 Be1 63.94(11) 2_546 1_455 ? O1 Sr1 Be1 96.06(11) . 1_455 ? O5 Sr1 Be1 139.45(11) 2_646 1_455 ? O5 Sr1 Be1 22.90(11) 1_455 1_455 ? O4 Sr1 Be1 91.84(11) . 1_455 ? O4 Sr1 Be1 93.23(11) 2_546 1_455 ? Be1 Sr1 Be1 93.11(14) . 1_455 ? Be1 Sr1 Be1 78.25(7) 2_546 1_455 ? Be1 Sr1 Be1 151.86(9) 2_646 1_455 ? O2 As1 O1 113.12(14) 1_655 . ? O2 As1 O3 107.32(14) 1_655 3_666 ? O1 As1 O3 108.14(14) . 3_666 ? O2 As1 O4 113.49(14) 1_655 4_565 ? O1 As1 O4 107.69(14) . 4_565 ? O3 As1 O4 106.79(14) 3_666 4_565 ? O2 As1 Sr1 34.44(10) 1_655 1_655 ? O1 As1 Sr1 86.13(10) . 1_655 ? O3 As1 Sr1 97.64(10) 3_666 1_655 ? O4 As1 Sr1 145.90(10) 4_565 1_655 ? O2 As1 Sr1 87.49(10) 1_655 4_665 ? O1 As1 Sr1 142.50(10) . 4_665 ? O3 As1 Sr1 34.36(10) 3_666 4_665 ? O4 As1 Sr1 90.34(10) 4_565 4_665 ? Sr1 As1 Sr1 97.104(13) 1_655 4_665 ? O2 As1 Sr1 31.42(10) 1_655 3_656 ? O1 As1 Sr1 141.59(10) . 3_656 ? O3 As1 Sr1 100.39(10) 3_666 3_656 ? O4 As1 Sr1 87.39(10) 4_565 3_656 ? Sr1 As1 Sr1 64.682(12) 1_655 3_656 ? Sr1 As1 Sr1 69.479(8) 4_665 3_656 ? O2 As1 Sr1 151.01(10) 1_655 4_565 ? O1 As1 Sr1 89.67(10) . 4_565 ? O3 As1 Sr1 80.36(10) 3_666 4_565 ? O4 As1 Sr1 39.15(10) 4_565 4_565 ? Sr1 As1 Sr1 174.539(14) 1_655 4_565 ? Sr1 As1 Sr1 84.129(11) 4_665 4_565 ? Sr1 As1 Sr1 120.608(12) 3_656 4_565 ? O2 As1 Sr1 96.98(10) 1_655 . ? O1 As1 Sr1 32.14(10) . . ? O3 As1 Sr1 140.21(10) 3_666 . ? O4 As1 Sr1 91.00(10) 4_565 . ? Sr1 As1 Sr1 84.806(12) 1_655 . ? Sr1 As1 Sr1 174.368(12) 4_665 . ? Sr1 As1 Sr1 116.047(12) 3_656 . ? Sr1 As1 Sr1 93.481(12) 4_565 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.705 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.162 # Attachment '- BAF1074.cif' data_BAF1074 _database_code_depnum_ccdc_archive 'CCDC 807054' #TrackingRef '- BAF1074.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(As O4), 2(H2 O), 3(Be)' _chemical_formula_sum 'As2 Be3 H4 O10' _chemical_formula_weight 340.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.2789(6) _cell_length_b 4.6530(2) _cell_length_c 9.8544(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.679(2) _cell_angle_gamma 90.00 _cell_volume 744.89(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3769 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 9.010 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; Bruker-Nonius APEX II CCD camera on \k-goniostat ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 955 _diffrn_standards_interval_count 5043 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4382 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 27.53 _reflns_number_total 852 _reflns_number_gt 819 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_data_reduction ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0063P)^2^+4.8264P] 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 852 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0450 _refine_ls_wR_factor_gt 0.0441 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Be1 Be 0.0000 0.1963(11) 0.2500 0.0111(9) Uani 1 2 d S . . Be2 Be 0.2526(2) 0.5560(7) 0.3397(3) 0.0079(6) Uani 1 1 d . . . O5 O 0.04729(13) 0.4232(5) 0.1508(2) 0.0158(4) Uani 1 1 d . . . H1 H 0.080(3) 0.348(9) 0.109(4) 0.029(10) Uiso 1 1 d . . . H2 H 0.052(4) 0.580(14) 0.179(6) 0.09(2) Uiso 1 1 d . . . As1 As 0.154595(14) 0.05257(5) 0.40193(2) 0.00601(10) Uani 1 1 d . . . O2 O 0.16469(10) -0.0775(4) 0.55972(17) 0.0076(3) Uani 1 1 d . . . O4 O 0.17626(11) 0.4018(4) 0.40066(17) 0.0094(4) Uani 1 1 d . . . O1 O 0.06014(11) -0.0164(4) 0.3355(2) 0.0148(4) Uani 1 1 d . . . O3 O 0.22376(10) -0.1105(4) 0.30175(16) 0.0078(3) Uani 1 1 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 Be1 0.010(2) 0.013(2) 0.011(2) 0.000 -0.0019(16) 0.000 Be2 0.0110(15) 0.0042(15) 0.0085(14) 0.0017(10) 0.0004(12) 0.0000(11) O5 0.0156(10) 0.0139(11) 0.0186(10) 0.0033(8) 0.0063(8) 0.0030(8) As1 0.00665(15) 0.00554(16) 0.00569(14) 0.00038(8) -0.00074(9) -0.00031(8) O2 0.0079(8) 0.0100(9) 0.0047(8) 0.0012(6) 0.0001(6) 0.0000(6) O4 0.0103(8) 0.0058(8) 0.0124(9) -0.0003(7) 0.0026(7) -0.0004(7) O1 0.0101(9) 0.0136(9) 0.0194(10) 0.0063(8) -0.0091(7) -0.0039(7) O3 0.0115(8) 0.0070(8) 0.0051(8) 0.0001(6) 0.0014(6) 0.0012(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Be1 O1 1.594(4) 2 ? Be1 O1 1.594(4) . ? Be1 O5 1.661(4) 2 ? Be1 O5 1.661(4) . ? Be2 O4 1.586(4) . ? Be2 O2 1.623(4) 7_556 ? Be2 O3 1.657(3) 1_565 ? Be2 O3 1.662(3) 4 ? As1 O4 1.6629(18) . ? As1 O1 1.6635(18) . ? As1 O2 1.6667(16) . ? As1 O3 1.7207(17) . ? O2 Be2 1.623(4) 7_556 ? O3 Be2 1.657(3) 1_545 ? O3 Be2 1.662(3) 4_545 ? 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 O1 Be1 O1 103.2(3) 2 . ? O1 Be1 O5 114.42(10) 2 2 ? O1 Be1 O5 112.06(11) . 2 ? O1 Be1 O5 112.06(11) 2 . ? O1 Be1 O5 114.42(10) . . ? O5 Be1 O5 101.1(3) 2 . ? O4 Be2 O2 115.9(2) . 7_556 ? O4 Be2 O3 107.0(2) . 1_565 ? O2 Be2 O3 106.99(19) 7_556 1_565 ? O4 Be2 O3 109.6(2) . 4 ? O2 Be2 O3 108.2(2) 7_556 4 ? O3 Be2 O3 108.94(18) 1_565 4 ? O4 As1 O1 112.13(9) . . ? O4 As1 O2 110.70(9) . . ? O1 As1 O2 109.31(9) . . ? O4 As1 O3 106.24(8) . . ? O1 As1 O3 108.14(9) . . ? O2 As1 O3 110.26(8) . . ? Be2 O2 As1 125.13(15) 7_556 . ? Be2 O4 As1 128.08(16) . . ? Be1 O1 As1 127.52(17) . . ? Be2 O3 Be2 123.27(15) 1_545 4_545 ? Be2 O3 As1 118.01(15) 1_545 . ? Be2 O3 As1 118.11(15) 4_545 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.406 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.105 # Attachment '- BAF1125.cif' data_BAF1125 _database_code_depnum_ccdc_archive 'CCDC 807055' #TrackingRef '- BAF1125.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(As O4), 2(H4 N), 2(H O), 3(Be)' _chemical_formula_sum 'As2 Be3 H10 N2 O10' _chemical_formula_weight 374.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9140(3) _cell_length_b 8.5660(3) _cell_length_c 11.1562(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.050(2) _cell_angle_gamma 90.00 _cell_volume 932.88(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10226 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728.0 _exptl_absorpt_coefficient_mu 7.164 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 2279 _diffrn_standards_interval_count 9095 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12090 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2133 _reflns_number_gt 1710 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_data_reduction ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement has been attempted in suggested spg P2(1)/2 - leads to unacceptable bond distances ; _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^)+(0.0000P)^2^+7.1150P] 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 2133 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.007 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 N2 N 0.4168(4) 0.1502(5) 0.5483(4) 0.0101(8) Uani 1 1 d . . . N1 N 0.4194(4) 0.6570(5) 0.0473(4) 0.0118(8) Uani 1 1 d . . . Be2 Be 0.3989(6) 0.0675(7) 0.1644(5) 0.0088(12) Uani 1 1 d . . . Be3 Be 0.0891(6) 0.0647(7) -0.1855(5) 0.0097(12) Uani 1 1 d . . . H1 H 0.383(6) 0.238(8) 0.580(6) 0.026(17) Uiso 1 1 d . . . H2 H 0.363(6) 0.615(7) -0.017(6) 0.019(15) Uiso 1 1 d . . . H3 H 0.437(8) 0.587(10) 0.116(8) 0.06(2) Uiso 1 1 d . . . H4 H 0.367(7) 0.062(9) 0.558(6) 0.04(2) Uiso 1 1 d . . . H6 H 0.504(7) 0.128(7) 0.584(6) 0.028(17) Uiso 1 1 d . . . H5 H 0.406(6) 0.159(7) 0.470(6) 0.016(14) Uiso 1 1 d . . . H7 H 0.488(7) 0.692(7) 0.030(5) 0.019(16) Uiso 1 1 d . . . H9 H 0.113(6) 0.088(8) -0.003(6) 0.022(19) Uiso 1 1 d . . . H10 H 0.374(8) 0.736(11) 0.065(8) 0.06(3) Uiso 1 1 d . . . H8 H 0.378(7) 0.115(8) -0.009(6) 0.02(2) Uiso 1 1 d . . . As1 As 0.68971(4) 0.13389(5) 0.24184(4) 0.00601(13) Uani 1 1 d . . . As2 As 0.20042(4) -0.13923(5) 0.25115(4) 0.00620(13) Uani 1 1 d . . . O8 O 0.1030(3) 0.1453(4) -0.0515(3) 0.0081(6) Uani 1 1 d . . . O9 O 0.3688(3) 0.1619(4) 0.0335(3) 0.0093(7) Uani 1 1 d . . . O6 O 0.2037(3) 0.3694(4) 0.1094(3) 0.0092(6) Uani 1 1 d . . . O5 O 0.2996(3) -0.0908(4) 0.1487(3) 0.0103(7) Uani 1 1 d . . . O1 O 0.2409(3) 0.3953(4) -0.1076(3) 0.0098(7) Uani 1 1 d . . . O7 O 0.0694(3) -0.0128(4) 0.2391(3) 0.0099(7) Uani 1 1 d . . . O2 O 0.5591(3) 0.0123(4) 0.1887(3) 0.0105(7) Uani 1 1 d . . . O3 O 0.8209(3) 0.0979(4) 0.1694(3) 0.0091(7) Uani 1 1 d . . . O10 O 0.3598(3) 0.1775(4) 0.2750(3) 0.0080(6) Uani 1 1 d . . . O4 O 0.6462(3) 0.3221(4) 0.2182(3) 0.0089(6) Uani 1 1 d . . . Be1 Be 0.2289(6) 0.2626(7) -0.0055(5) 0.0105(12) Uani 1 1 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 N2 0.0097(19) 0.012(2) 0.0082(19) 0.0004(17) 0.0007(16) 0.0009(17) N1 0.0092(19) 0.012(2) 0.015(2) -0.0001(18) 0.0025(17) -0.0005(17) Be2 0.013(3) 0.002(3) 0.009(3) 0.000(2) -0.004(2) 0.001(2) Be3 0.009(3) 0.010(3) 0.011(3) 0.000(2) 0.003(2) -0.001(2) As1 0.0064(2) 0.0058(2) 0.0058(2) -0.00026(17) 0.00103(16) 0.00046(17) As2 0.0058(2) 0.0065(2) 0.0063(2) -0.00049(18) 0.00118(16) -0.00064(17) O8 0.0110(15) 0.0070(17) 0.0062(15) 0.0002(14) 0.0010(12) -0.0023(12) O9 0.0109(16) 0.0110(18) 0.0066(16) -0.0023(15) 0.0029(13) 0.0006(13) O6 0.0100(15) 0.0112(17) 0.0055(14) -0.0013(13) -0.0011(12) 0.0014(13) O5 0.0128(15) 0.0126(17) 0.0063(15) -0.0009(13) 0.0042(12) -0.0018(13) O1 0.0135(15) 0.0087(17) 0.0071(15) 0.0021(13) 0.0015(12) -0.0004(13) O7 0.0067(14) 0.0088(17) 0.0137(16) -0.0018(13) 0.0009(12) 0.0010(12) O2 0.0078(15) 0.0061(16) 0.0171(17) -0.0005(13) 0.0010(13) 0.0009(12) O3 0.0100(15) 0.0090(17) 0.0101(15) -0.0007(13) 0.0064(12) 0.0019(12) O10 0.0090(14) 0.0063(16) 0.0088(15) -0.0013(12) 0.0018(12) -0.0015(12) O4 0.0082(14) 0.0068(16) 0.0108(15) 0.0008(13) -0.0006(12) 0.0003(12) Be1 0.014(3) 0.008(3) 0.009(3) 0.000(2) 0.000(2) 0.003(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Be2 O2 1.633(6) . ? Be2 O10 1.652(7) . ? Be2 O9 1.650(7) . ? Be2 O5 1.667(7) . ? Be3 O4 1.621(7) 4_565 ? Be3 O8 1.631(7) . ? Be3 O7 1.642(6) 3 ? Be3 O3 1.647(7) 3_655 ? As1 O3 1.675(3) . ? As1 O4 1.678(3) . ? As1 O2 1.687(3) . ? As1 O1 1.687(3) 4_666 ? As2 O6 1.677(3) 2_545 ? As2 O7 1.678(3) . ? As2 O5 1.684(3) . ? As2 O10 1.687(3) 2_545 ? O8 Be1 1.615(7) . ? O9 Be1 1.627(7) . ? O6 Be1 1.629(7) . ? O6 As2 1.677(3) 2 ? O1 Be1 1.628(7) . ? O1 As1 1.687(3) 4_565 ? O7 Be3 1.642(6) 3 ? O3 Be3 1.647(7) 3_655 ? O10 As2 1.687(3) 2 ? O4 Be3 1.621(7) 4_666 ? 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 O2 Be2 O10 112.9(4) . . ? O2 Be2 O9 108.0(4) . . ? O10 Be2 O9 110.6(4) . . ? O2 Be2 O5 108.7(4) . . ? O10 Be2 O5 109.3(4) . . ? O9 Be2 O5 107.1(3) . . ? O4 Be3 O8 111.8(4) 4_565 . ? O4 Be3 O7 110.1(4) 4_565 3 ? O8 Be3 O7 111.8(4) . 3 ? O4 Be3 O3 109.4(4) 4_565 3_655 ? O8 Be3 O3 107.5(4) . 3_655 ? O7 Be3 O3 106.0(4) 3 3_655 ? O3 As1 O4 107.49(16) . . ? O3 As1 O2 109.28(15) . . ? O4 As1 O2 112.18(15) . . ? O3 As1 O1 109.22(15) . 4_666 ? O4 As1 O1 108.89(16) . 4_666 ? O2 As1 O1 109.71(16) . 4_666 ? O6 As2 O7 110.57(16) 2_545 . ? O6 As2 O5 108.36(15) 2_545 . ? O7 As2 O5 108.75(16) . . ? O6 As2 O10 109.13(16) 2_545 2_545 ? O7 As2 O10 109.96(15) . 2_545 ? O5 As2 O10 110.03(15) . 2_545 ? Be1 O8 Be3 119.4(4) . . ? Be1 O9 Be2 120.7(4) . . ? Be1 O6 As2 124.4(3) . 2 ? Be2 O5 As2 122.2(3) . . ? Be1 O1 As1 123.2(3) . 4_565 ? Be3 O7 As2 122.2(3) 3 . ? Be2 O2 As1 122.9(3) . . ? Be3 O3 As1 123.7(3) 3_655 . ? Be2 O10 As2 121.6(3) . 2 ? Be3 O4 As1 125.5(3) 4_666 . ? O8 Be1 O6 112.5(4) . . ? O8 Be1 O1 111.0(4) . . ? O6 Be1 O1 101.4(4) . . ? O8 Be1 O9 109.3(4) . . ? O6 Be1 O9 109.2(4) . . ? O1 Be1 O9 113.3(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.785 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.161 # Attachment '- BAF1152.cif' data_BAF1152 _database_code_depnum_ccdc_archive 'CCDC 807056' #TrackingRef '- BAF1152.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(As4 Be4 H2 O17), 0.72(C2), 5(N), 3.62(C0.50), 0.84(C)' _chemical_formula_sum 'C4.90 H4 As8 Be8 N5 O34' _chemical_formula_weight 1348.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.9639(6) _cell_length_b 14.0423(6) _cell_length_c 18.6966(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.160(4) _cell_angle_gamma 90.00 _cell_volume 3403.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 7.881 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11010 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.55 _reflns_number_total 3828 _reflns_number_gt 3224 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement attempted in Cmca but has proven to be unconclusive High degree of disorder of templating organic materal ; _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^)+(0.0816P)^2^+34.1023P] 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 3828 _refine_ls_number_parameters 264 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.098 _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 Be3 Be 0.3610(6) 0.3795(6) 0.2014(4) 0.0099(15) Uiso 1 1 d . . . Be1 Be -0.0696(6) 0.3297(6) 0.1554(5) 0.0133(16) Uiso 1 1 d . . . C1 C 0.2565(11) 0.1320(10) 0.2164(8) 0.053(5) Uiso 0.81(4) 1 d P . . N3 N 0.5000 0.8937(7) 0.7500 0.029(2) Uani 1 2 d S . . N4 N 0.7500 0.7500 0.5000 0.025(2) Uani 1 2 d S . . N2 N 0.0000 0.1024(7) 0.2500 0.035(3) Uani 1 2 d S . . N1 N 0.7564(5) 0.5069(4) 0.1025(3) 0.0189(13) Uani 1 1 d . . . C4 C 0.2488(9) 0.2522(9) 0.0394(6) 0.032(4) Uiso 0.72(3) 1 d P . . C2 C 0.3062(14) 0.1878(13) 0.1090(10) 0.037(6) Uiso 0.50(4) 1 d P . . C6 C 0.203(3) 0.187(3) 0.110(2) 0.043(15) Uiso 0.23(4) 1 d P . . C7 C 0.118(3) 0.125(3) 0.154(2) 0.025(13) Uiso 0.19(3) 1 d P . . H1 H 0.382(5) 0.190(4) 0.378(3) 0.007(17) Uiso 1 1 d D . . H2 H -0.113(5) 0.186(4) 0.129(3) 0.010(18) Uiso 1 1 d D . . As1 As 0.00178(5) 0.35983(4) 0.00905(3) 0.00795(17) Uani 1 1 d . . . As2 As 0.13545(5) 0.38092(4) 0.20225(3) 0.00860(17) Uani 1 1 d . . . As3 As 0.36538(5) 0.51121(4) 0.07496(3) 0.00791(17) Uani 1 1 d . . . As4 As 0.43302(5) 0.33203(4) 0.34456(3) 0.00908(17) Uani 1 1 d . . . O1 O 0.3767(3) 0.4051(3) 0.2869(2) 0.0133(9) Uani 1 1 d . . . O2 O 0.4440(3) 0.6076(3) 0.0655(2) 0.0090(8) Uani 1 1 d . . . O3 O -0.0864(3) 0.3676(3) 0.0745(2) 0.0127(9) Uani 1 1 d . . . O4 O 0.2471(3) 0.5535(3) 0.0587(2) 0.0113(9) Uani 1 1 d . . . O5 O 0.4218(4) 0.3790(3) 0.4266(2) 0.0147(10) Uani 1 1 d . . . O6 O 0.1070(3) 0.4258(3) 0.0233(2) 0.0124(9) Uani 1 1 d . . . O7 O 0.3910(3) 0.4238(3) 0.0172(2) 0.0127(9) Uani 1 1 d . . . O8 O 0.3815(3) 0.4799(3) 0.1609(2) 0.0127(9) Uani 1 1 d . . . O9 O 0.3588(3) 0.2293(3) 0.3457(3) 0.0137(9) Uani 1 1 d D . . O10 O 0.0494(3) 0.3013(3) 0.1716(2) 0.0123(9) Uani 1 1 d . . . O11 O 0.2509(3) 0.3324(3) 0.1853(2) 0.0113(9) Uani 1 1 d . . . O12 O 0.1199(3) 0.4026(3) 0.2894(2) 0.0120(9) Uani 1 1 d . . . O13 O -0.1332(3) 0.2250(3) 0.1602(3) 0.0145(9) Uani 1 1 d D . . O14 O 0.5416(4) 0.7482(3) -0.0021(2) 0.0159(9) Uani 1 1 d . . . O15 O 0.0551(3) 0.6058(3) 0.0679(2) 0.0106(9) Uani 1 1 d . . . O16 O 0.1216(3) 0.4874(3) 0.1625(2) 0.0118(9) Uani 1 1 d . . . O19 O 0.4466(3) 0.2986(3) 0.1766(2) 0.0124(9) Uani 1 1 d . . . Be2 Be 0.1325(6) 0.5129(6) 0.0772(5) 0.0105(15) Uiso 1 1 d . . . Be4 Be 0.5048(6) 0.6374(6) -0.0082(5) 0.0137(17) Uiso 1 1 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 N3 0.033(5) 0.028(5) 0.025(5) 0.000 0.014(4) 0.000 N4 0.014(4) 0.017(4) 0.044(6) -0.007(4) 0.002(4) 0.000(3) N2 0.031(5) 0.030(5) 0.044(6) 0.000 -0.026(5) 0.000 N1 0.022(3) 0.022(3) 0.013(3) 0.001(2) 0.003(2) 0.001(2) As1 0.0080(3) 0.0096(3) 0.0062(3) -0.0005(2) 0.0016(2) -0.0004(2) As2 0.0081(3) 0.0119(3) 0.0058(3) 0.0003(2) 0.0014(2) -0.0004(2) As3 0.0082(3) 0.0092(3) 0.0063(3) 0.0006(2) 0.0014(2) -0.0003(2) As4 0.0093(3) 0.0121(3) 0.0059(3) 0.0006(2) 0.0013(2) -0.0008(2) O1 0.017(2) 0.014(2) 0.009(2) 0.0043(17) -0.0014(18) 0.0040(18) O2 0.0040(19) 0.014(2) 0.009(2) 0.0007(17) 0.0018(16) -0.0039(16) O3 0.010(2) 0.021(2) 0.008(2) 0.0027(17) 0.0031(17) 0.0015(17) O4 0.010(2) 0.014(2) 0.010(2) -0.0005(17) 0.0032(17) -0.0014(17) O5 0.012(2) 0.024(2) 0.008(2) -0.0020(18) 0.0015(18) 0.0025(18) O6 0.011(2) 0.013(2) 0.014(2) -0.0054(17) 0.0038(17) -0.0007(17) O7 0.017(2) 0.010(2) 0.011(2) -0.0041(17) 0.0041(17) 0.0000(17) O8 0.017(2) 0.015(2) 0.007(2) 0.0019(17) 0.0016(18) -0.0068(18) O9 0.007(2) 0.013(2) 0.020(2) 0.0067(19) -0.0041(18) 0.0000(17) O10 0.010(2) 0.016(2) 0.011(2) -0.0022(17) 0.0000(17) -0.0012(17) O11 0.008(2) 0.014(2) 0.012(2) 0.0002(17) 0.0012(17) 0.0033(16) O12 0.016(2) 0.013(2) 0.007(2) 0.0016(17) 0.0022(17) -0.0019(17) O13 0.013(2) 0.015(2) 0.016(2) -0.0054(18) 0.0057(18) 0.0014(18) O14 0.018(2) 0.015(2) 0.014(2) 0.0017(18) 0.0057(18) 0.0008(18) O15 0.012(2) 0.012(2) 0.007(2) 0.0001(16) -0.0010(17) 0.0053(17) O16 0.012(2) 0.014(2) 0.009(2) 0.0011(17) 0.0036(17) 0.0023(17) O19 0.013(2) 0.014(2) 0.010(2) -0.0007(17) -0.0005(17) -0.0033(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Be3 O11 1.600(9) . ? Be3 O8 1.623(9) . ? Be3 O1 1.650(9) . ? Be3 O19 1.656(9) . ? Be1 O12 1.593(9) 2 ? Be1 O3 1.617(9) . ? Be1 O10 1.622(9) . ? Be1 O13 1.689(9) . ? C4 C4 1.47(2) 7 ? C4 C6 1.72(5) . ? C4 C2 1.75(2) . ? C2 C6 1.34(5) . ? C6 C7 1.61(6) . ? As1 O14 1.663(5) 3_445 ? As1 O6 1.670(4) . ? As1 O3 1.682(4) . ? As1 O15 1.686(4) 5_565 ? As2 O12 1.670(4) . ? As2 O11 1.676(4) . ? As2 O16 1.679(4) . ? As2 O10 1.679(4) . ? As3 O7 1.669(4) . ? As3 O4 1.672(4) . ? As3 O8 1.678(4) . ? As3 O2 1.704(4) . ? As4 O1 1.657(4) . ? As4 O5 1.677(5) . ? As4 O19 1.677(4) 2_655 ? As4 O9 1.734(4) . ? O2 Be4 1.644(10) . ? O4 Be2 1.630(9) . ? O5 Be4 1.640(9) 6_566 ? O6 Be2 1.618(9) . ? O7 Be4 1.610(9) 5_665 ? O12 Be1 1.593(9) 2 ? O14 Be4 1.631(9) . ? O14 As1 1.663(5) 3 ? O15 Be2 1.654(9) . ? O15 As1 1.686(4) 5_565 ? O16 Be2 1.640(9) . ? O19 As4 1.677(4) 2_655 ? Be4 O7 1.610(9) 5_665 ? Be4 O5 1.640(9) 6_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Be3 O8 114.7(5) . . ? O11 Be3 O1 112.3(5) . . ? O8 Be3 O1 104.1(5) . . ? O11 Be3 O19 105.2(5) . . ? O8 Be3 O19 110.8(5) . . ? O1 Be3 O19 109.9(5) . . ? O12 Be1 O3 109.9(5) 2 . ? O12 Be1 O10 115.3(6) 2 . ? O3 Be1 O10 112.4(5) . . ? O12 Be1 O13 108.9(5) 2 . ? O3 Be1 O13 105.7(5) . . ? O10 Be1 O13 103.9(5) . . ? C4 C4 C6 139.3(19) 7 . ? C4 C4 C2 135.4(14) 7 . ? C6 C4 C2 45.4(16) . . ? C6 C2 C4 66(2) . . ? C2 C6 C7 134(4) . . ? C2 C6 C4 68(2) . . ? C7 C6 C4 155(3) . . ? O14 As1 O6 106.8(2) 3_445 . ? O14 As1 O3 111.4(2) 3_445 . ? O6 As1 O3 113.9(2) . . ? O14 As1 O15 107.3(2) 3_445 5_565 ? O6 As1 O15 109.4(2) . 5_565 ? O3 As1 O15 107.8(2) . 5_565 ? O12 As2 O11 111.7(2) . . ? O12 As2 O16 104.9(2) . . ? O11 As2 O16 111.8(2) . . ? O12 As2 O10 111.8(2) . . ? O11 As2 O10 104.9(2) . . ? O16 As2 O10 111.9(2) . . ? O7 As3 O4 109.1(2) . . ? O7 As3 O8 113.7(2) . . ? O4 As3 O8 112.3(2) . . ? O7 As3 O2 113.4(2) . . ? O4 As3 O2 104.3(2) . . ? O8 As3 O2 103.5(2) . . ? O1 As4 O5 108.2(2) . . ? O1 As4 O19 115.4(2) . 2_655 ? O5 As4 O19 114.1(2) . 2_655 ? O1 As4 O9 106.3(2) . . ? O5 As4 O9 105.5(2) . . ? O19 As4 O9 106.6(2) 2_655 . ? Be3 O1 As4 123.3(4) . . ? Be4 O2 As3 125.3(4) . . ? Be1 O3 As1 124.7(4) . . ? Be2 O4 As3 132.3(4) . . ? Be4 O5 As4 124.5(4) 6_566 . ? Be2 O6 As1 133.2(4) . . ? Be4 O7 As3 129.0(4) 5_665 . ? Be3 O8 As3 130.9(4) . . ? Be1 O10 As2 122.0(4) . . ? Be3 O11 As2 126.4(4) . . ? Be1 O12 As2 124.4(4) 2 . ? Be4 O14 As1 144.8(4) . 3 ? Be2 O15 As1 125.4(4) . 5_565 ? Be2 O16 As2 128.0(4) . . ? Be3 O19 As4 119.9(4) . 2_655 ? O6 Be2 O4 108.4(5) . . ? O6 Be2 O16 115.0(5) . . ? O4 Be2 O16 111.3(5) . . ? O6 Be2 O15 114.1(5) . . ? O4 Be2 O15 104.8(5) . . ? O16 Be2 O15 102.8(5) . . ? O7 Be4 O14 105.7(5) 5_665 . ? O7 Be4 O5 113.3(6) 5_665 6_565 ? O14 Be4 O5 112.1(5) . 6_565 ? O7 Be4 O2 110.8(5) 5_665 . ? O14 Be4 O2 109.0(5) . . ? O5 Be4 O2 105.8(5) 6_565 . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.440 _refine_diff_density_min -1.616 _refine_diff_density_rms 0.305 # Attachment '- BAF2021.cif' data_BAF2021 _database_code_depnum_ccdc_archive 'CCDC 807057' #TrackingRef '- BAF2021.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'As O4, 2(H2 O), H O, 2(Be)' _chemical_formula_sum 'As Be2 H5 O7' _chemical_formula_weight 209.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.4806(2) _cell_length_b 11.0971(4) _cell_length_c 8.4133(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.881(2) _cell_angle_gamma 90.00 _cell_volume 581.96(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6925 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408.50 _exptl_absorpt_coefficient_mu 5.814 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type ; Bruker-Nonius APEX II CCD camera on \k-goniostat ; _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 1413 _diffrn_standards_interval_count 4954 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6693 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1339 _reflns_number_gt 1251 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_data_reduction ; DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0231P)^2^+2.1223P] 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 1339 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0507 _refine_ls_wR_factor_gt 0.0486 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.835 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.005 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 O7 O 0.5780(3) 0.90359(17) 0.6656(2) 0.0108(3) Uani 1 1 d . . . O6 O 0.7668(3) 0.60025(16) 0.5330(2) 0.0108(3) Uani 1 1 d . . . O5 O 0.9501(3) 0.80366(15) 0.6726(2) 0.0090(3) Uani 1 1 d . . . Be1 Be 0.9723(5) 0.6962(3) 0.5524(3) 0.0084(5) Uani 1 1 d . . . Be2 Be 0.8085(4) 0.9236(3) 0.6250(4) 0.0085(5) Uani 1 1 d . . . H2 H 0.479(5) 0.952(3) 0.638(4) 0.021(8) Uiso 1 1 d . . . H1 H 0.555(5) 0.857(3) 0.727(4) 0.023(9) Uiso 1 1 d . . . H3 H 1.025(6) 0.812(3) 0.749(5) 0.027(10) Uiso 1 1 d . . . H4 H 0.720(6) 0.591(3) 0.605(5) 0.026(9) Uiso 1 1 d . . . H5 H 0.781(6) 0.530(4) 0.493(5) 0.041(11) Uiso 1 1 d . . . As1 As 1.12926(3) 1.116449(19) 0.70462(3) 0.00570(9) Uani 1 1 d . . . O3 O 1.1926(3) 0.61910(13) 0.60813(19) 0.0082(3) Uani 1 1 d . . . O2 O 0.9418(3) 0.74315(14) 0.36251(19) 0.0093(3) Uani 1 1 d . . . O1 O 0.9171(2) 1.04075(14) 0.73050(19) 0.0089(3) Uani 1 1 d . . . O4 O 0.7586(2) 0.95244(14) 0.42872(19) 0.0089(3) Uani 1 1 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 O7 0.0075(8) 0.0115(8) 0.0145(8) 0.0067(7) 0.0049(7) 0.0023(7) O6 0.0119(8) 0.0112(8) 0.0114(8) -0.0017(6) 0.0069(7) -0.0025(6) O5 0.0101(8) 0.0099(8) 0.0049(7) -0.0014(6) -0.0012(6) 0.0002(6) Be1 0.0084(13) 0.0081(13) 0.0081(13) -0.0005(10) 0.0013(10) -0.0013(10) Be2 0.0062(13) 0.0098(13) 0.0094(13) 0.0013(10) 0.0018(10) 0.0007(10) As1 0.00594(13) 0.00559(13) 0.00539(13) 0.00019(7) 0.00125(9) -0.00018(7) O3 0.0081(7) 0.0090(8) 0.0059(7) -0.0020(5) -0.0007(6) 0.0017(6) O2 0.0149(8) 0.0053(7) 0.0076(7) 0.0012(6) 0.0032(6) 0.0018(6) O1 0.0067(7) 0.0106(8) 0.0094(7) -0.0014(6) 0.0023(6) -0.0027(6) O4 0.0084(7) 0.0109(8) 0.0076(7) 0.0006(6) 0.0026(6) 0.0025(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O7 Be2 1.636(3) . ? O6 Be1 1.678(3) . ? O5 Be1 1.595(3) . ? O5 Be2 1.604(3) . ? Be1 O3 1.620(3) . ? Be1 O2 1.640(3) . ? Be2 O1 1.622(3) . ? Be2 O4 1.625(3) . ? As1 O1 1.6754(15) . ? As1 O2 1.6781(15) 3_776 ? As1 O3 1.6794(16) 2_756 ? As1 O4 1.6784(15) 3_776 ? O3 As1 1.6794(15) 2_746 ? O2 As1 1.6781(15) 3_776 ? O4 As1 1.6784(15) 3_776 ? 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 Be1 O5 Be2 127.32(18) . . ? O5 Be1 O3 115.87(19) . . ? O5 Be1 O2 111.89(19) . . ? O3 Be1 O2 108.14(18) . . ? O5 Be1 O6 109.22(18) . . ? O3 Be1 O6 107.80(18) . . ? O2 Be1 O6 103.08(17) . . ? O5 Be2 O1 113.30(19) . . ? O5 Be2 O4 111.00(19) . . ? O1 Be2 O4 109.52(19) . . ? O5 Be2 O7 109.13(19) . . ? O1 Be2 O7 106.19(18) . . ? O4 Be2 O7 107.44(18) . . ? O1 As1 O2 110.48(8) . 3_776 ? O1 As1 O3 105.36(8) . 2_756 ? O2 As1 O3 110.75(8) 3_776 2_756 ? O1 As1 O4 112.29(8) . 3_776 ? O2 As1 O4 109.09(8) 3_776 3_776 ? O3 As1 O4 108.83(8) 2_756 3_776 ? Be1 O3 As1 127.30(14) . 2_746 ? Be1 O2 As1 124.85(14) . 3_776 ? Be2 O1 As1 125.41(14) . . ? Be2 O4 As1 125.97(14) . 3_776 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.362 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.095 data_BAF845 _database_code_depnum_ccdc_archive 'CCDC 807058' #TrackingRef '- BAF845.cif' _audit_update_record ; 2010-12-06 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0.50 H0.50 As0.95 Be1.05 N0.16 O4.78' _chemical_formula_weight 165.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Be Be 0.0005 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Al Al 0.0645 0.0514 '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 tetragonal _symmetry_space_group_name_H-M P42/nbc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x+1/2, y, -z' 'x, -y+1/2, -z' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x-1/2, -y, z' '-x, y-1/2, z' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 16.9831(5) _cell_length_b 16.9831(5) _cell_length_c 12.7839(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3687.2(2) _cell_formula_units_Z 32 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 29748 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 6.912 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 4411 _diffrn_standards_interval_count 12103 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23354 _diffrn_reflns_av_R_equivalents 0.2004 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2125 _reflns_number_gt 1293 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Atoms C1 and N1 are part of a heavily disordered pyridine ring. ; _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^)+(0.0801P)^2^+119.8929P] 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 2125 _refine_ls_number_parameters 156 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1499 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.1798 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 2.989 _refine_ls_shift/su_mean 0.096 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 O8 O 0.1364(5) 0.0006(5) 0.2041(6) 0.016(2) Uani 1 1 d . . . O5 O 0.1511(5) 0.1028(5) 0.3681(7) 0.017(2) Uani 1 1 d . . . O4 O 0.1384(5) 0.0055(5) -0.2013(6) 0.015(2) Uani 1 1 d . . . O7 O 0.1468(5) 0.0302(5) -0.0020(7) 0.0157(19) Uani 1 1 d . . . O6 O 0.2508(5) 0.1060(4) 0.1314(7) 0.0155(18) Uani 1 1 d . . . O9 O 0.0989(6) -0.0462(6) 0.3889(8) 0.021(2) Uani 1 1 d . . . O12 O 0.2500 0.2500 0.2500 0.019(6) Uani 0.90(7) 4 d SP . . O2 O 0.2482(5) -0.0184(5) 0.3530(6) 0.0163(18) Uani 1 1 d . . . O1 O 0.4010(5) -0.0438(5) 0.3950(7) 0.019(2) Uani 1 1 d . . . O3 O 0.1080(5) 0.1532(5) -0.1288(7) 0.021(2) Uani 1 1 d . . . Be4 Be 0.1615(3) 0.0159(3) 0.3279(4) 0.0113(17) Uani 0.835(7) 1 d P . . As4 As 0.1615(3) 0.0159(3) 0.3279(4) 0.0113(17) Uani 0.165(7) 1 d P . . Be3 Be 0.1596(3) 0.0720(3) -0.1145(4) 0.0110(18) Uani 0.839(7) 1 d P . . As3 As 0.1596(3) 0.0720(3) -0.1145(4) 0.0110(18) Uani 0.161(7) 1 d P . . O13 O 0.2500 0.180(3) 0.5000 0.101(18) Uani 0.67(6) 2 d SP . . N1 N 0.244(5) 0.826(2) 0.47(2) 0.19(12) Uani 0.33(5) 1 d P . . C1 C 0.1810(16) 0.7892(17) 0.504(11) 0.69(11) Uani 1.00(12) 1 d . . . H1 H 0.093(8) -0.042(8) 0.439(11) 0.00(4) Uiso 1 1 d . . . As1 As 0.15861(9) 0.07114(9) 0.11481(11) 0.0096(5) Uani 0.787(12) 1 d P . . Be1 Be 0.15861(9) 0.07114(9) 0.11481(11) 0.0096(5) Uani 0.213(12) 1 d P . . As2 As 0.33699(9) 0.01739(9) 0.32793(11) 0.0100(5) Uani 0.784(12) 1 d P . . Be2 Be 0.33699(9) 0.01739(9) 0.32793(11) 0.0100(5) Uani 0.216(12) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O8 0.016(4) 0.019(5) 0.013(4) 0.000(4) 0.001(3) -0.007(4) O5 0.014(5) 0.014(4) 0.021(4) -0.007(4) -0.010(4) 0.003(4) O4 0.014(4) 0.022(5) 0.009(4) 0.004(4) 0.004(3) 0.000(4) O7 0.020(4) 0.020(4) 0.007(3) -0.006(4) -0.002(4) -0.005(3) O6 0.006(3) 0.013(4) 0.028(4) -0.010(4) -0.007(4) -0.001(4) O9 0.026(6) 0.026(6) 0.012(5) -0.002(4) -0.004(5) -0.008(4) O12 0.020(8) 0.020(8) 0.017(10) 0.000 0.000 -0.001(10) O2 0.015(4) 0.017(4) 0.017(4) 0.006(3) 0.000(4) 0.002(4) O1 0.025(5) 0.023(5) 0.009(4) 0.008(4) -0.003(4) 0.008(4) O3 0.018(4) 0.019(5) 0.026(5) 0.010(4) 0.000(4) 0.006(4) Be4 0.011(3) 0.010(3) 0.013(3) 0.000(2) 0.000(2) 0.002(2) As4 0.011(3) 0.010(3) 0.013(3) 0.000(2) 0.000(2) 0.002(2) Be3 0.010(3) 0.010(3) 0.013(3) 0.001(2) -0.002(2) 0.002(2) As3 0.010(3) 0.010(3) 0.013(3) 0.001(2) -0.002(2) 0.002(2) O13 0.005(12) 0.26(5) 0.035(15) 0.000 0.023(12) 0.000 N1 0.03(4) 0.00(2) 0.5(3) 0.06(9) 0.02(8) 0.04(3) C1 0.026(16) 0.048(18) 2.0(3) 0.13(7) 0.12(6) -0.008(13) As1 0.0090(8) 0.0119(8) 0.0080(7) -0.0001(6) -0.0005(6) -0.0016(6) Be1 0.0090(8) 0.0119(8) 0.0080(7) -0.0001(6) -0.0005(6) -0.0016(6) As2 0.0108(8) 0.0106(8) 0.0084(7) 0.0010(6) -0.0001(6) -0.0004(6) Be2 0.0108(8) 0.0106(8) 0.0084(7) 0.0010(6) -0.0001(6) -0.0004(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O8 Be4 1.660(9) . ? O8 As1 1.697(9) . ? O5 Be4 1.573(10) . ? O5 Be1 1.670(9) 7 ? O5 As1 1.670(9) 7 ? O4 Be3 1.623(10) . ? O4 Be2 1.685(8) 5 ? O4 As2 1.685(8) 5 ? O7 Be3 1.618(10) . ? O7 As1 1.660(8) . ? O6 As3 1.641(10) 5 ? O6 Be3 1.641(10) 5 ? O6 As1 1.687(9) . ? O9 Be4 1.689(11) . ? O2 Be4 1.615(10) . ? O2 As2 1.658(9) . ? O1 As2 1.732(9) . ? O3 Be2 1.643(9) 4_554 ? O3 As2 1.643(9) 4_554 ? O3 Be3 1.645(10) . ? Be3 O6 1.641(10) 5 ? N1 N1 0.8(5) 5_556 ? N1 C1 1.32(15) . ? N1 C1 1.46(9) 5_556 ? C1 C1 1.34(7) 6_566 ? C1 N1 1.46(9) 5_556 ? As1 O5 1.670(9) 7 ? As2 O3 1.643(9) 3 ? As2 O4 1.685(8) 5 ? As2 As3 2.882(5) 5 ? 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 Be4 O8 As1 118.3(5) . . ? Be4 O5 Be1 131.8(6) . 7 ? Be4 O5 As1 131.8(6) . 7 ? Be1 O5 As1 0.00(11) 7 7 ? Be3 O4 Be2 121.2(6) . 5 ? Be3 O4 As2 121.2(6) . 5 ? Be2 O4 As2 0.00(14) 5 5 ? Be3 O7 As1 126.9(5) . . ? As3 O6 Be3 0.0(5) 5 5 ? As3 O6 As1 136.1(5) 5 . ? Be3 O6 As1 136.1(5) 5 . ? Be4 O2 As2 131.2(5) . . ? Be2 O3 As2 0.00(14) 4_554 4_554 ? Be2 O3 Be3 128.5(6) 4_554 . ? As2 O3 Be3 128.5(6) 4_554 . ? O5 Be4 O2 112.1(5) . . ? O5 Be4 O8 115.4(5) . . ? O2 Be4 O8 111.5(5) . . ? O5 Be4 O9 111.4(6) . . ? O2 Be4 O9 104.9(5) . . ? O8 Be4 O9 100.4(5) . . ? O4 Be3 O6 111.2(5) . 5 ? O4 Be3 O7 105.8(5) . . ? O6 Be3 O7 113.3(5) 5 . ? O4 Be3 O3 112.9(5) . . ? O6 Be3 O3 100.7(5) 5 . ? O7 Be3 O3 113.2(5) . . ? N1 N1 C1 82(10) 5_556 . ? N1 N1 C1 63(10) 5_556 5_556 ? C1 N1 C1 115(10) . 5_556 ? C1 C1 N1 116(8) 6_566 . ? C1 C1 N1 116(4) 6_566 5_556 ? N1 C1 N1 35(10) . 5_556 ? O7 As1 O5 112.9(4) . 7 ? O7 As1 O6 111.9(4) . . ? O5 As1 O6 103.0(4) 7 . ? O7 As1 O8 106.4(4) . . ? O5 As1 O8 111.1(4) 7 . ? O6 As1 O8 111.7(4) . . ? O3 As2 O2 111.8(5) 3 . ? O3 As2 O4 114.2(5) 3 5 ? O2 As2 O4 111.6(4) . 5 ? O3 As2 O1 109.4(5) 3 . ? O2 As2 O1 104.8(4) . . ? O4 As2 O1 104.4(4) 5 . ? O3 As2 As3 90.9(3) 3 5 ? O2 As2 As3 108.6(3) . 5 ? O4 As2 As3 28.8(3) 5 5 ? O1 As2 As3 130.5(3) . 5 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.822 _refine_diff_density_min -1.279 _refine_diff_density_rms 0.283 # Attachment '- BAF847.cif' data_BAF847 _database_code_depnum_ccdc_archive 'CCDC 807059' #TrackingRef '- BAF847.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(As5 Be4 O20), 2(C3 H12 N2), 2(C1.50), 2(H N0.94), 2(O)' _chemical_formula_sum 'C9 H26 As10 Be8 N5.88 O42' _chemical_formula_weight 1709.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.4169(6) _cell_length_b 9.8928(2) _cell_length_c 18.7178(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.1780(10) _cell_angle_gamma 90.00 _cell_volume 4703.08(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20770 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3273 _exptl_absorpt_coefficient_mu 7.130 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'Rint high due to disordered template present in channels' ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 5697 _diffrn_standards_interval_count 23358 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28349 _diffrn_reflns_av_R_equivalents 0.1007 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.56 _reflns_number_total 5390 _reflns_number_gt 3882 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; H atoms not present for OW1 & 2 due to high degree of disorder present. ; _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^)+(0.0000P)^2^+227.2789P] 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 5390 _refine_ls_number_parameters 313 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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 H11 H 0.169(4) 0.726(7) 0.001(4) 0.01(3) Uiso 1 1 d D . . C1 C 0.8490(5) 0.2904(13) 0.4907(6) 0.031(3) Uiso 1 1 d . . . H1A H 0.8140 0.2795 0.4690 0.037 Uiso 1 1 calc R . . H1B H 0.8604 0.3822 0.4816 0.037 Uiso 1 1 calc R . . C2 C 0.8856(5) 0.1944(13) 0.4562(6) 0.035(3) Uiso 1 1 d . . . H2A H 0.8715 0.1038 0.4604 0.042 Uiso 1 1 calc R . . H2B H 0.9191 0.1965 0.4827 0.042 Uiso 1 1 calc R . . C4 C 0.8465(5) 0.2695(14) 0.5698(7) 0.040(3) Uiso 1 1 d . . . H4A H 0.8215 0.3327 0.5890 0.048 Uiso 1 1 calc R . . H4B H 0.8340 0.1787 0.5790 0.048 Uiso 1 1 calc R . . N1 N 0.8955(3) 0.2205(9) 0.3785(4) 0.0207(19) Uiso 1 1 d . . . H5A H 0.9176 0.1583 0.3626 0.031 Uiso 1 1 calc R . . H5B H 0.9097 0.3021 0.3738 0.031 Uiso 1 1 calc R . . H5C H 0.8653 0.2165 0.3531 0.031 Uiso 1 1 calc R . . CN1 N 0.8983(3) 0.2890(9) 0.6065(4) 0.0190(18) Uiso 1 1 d . . . HN1A H 0.8954 0.2757 0.6533 0.028 Uiso 1 1 calc R . . HN1B H 0.9095 0.3728 0.5989 0.028 Uiso 1 1 calc R . . HN1C H 0.9212 0.2302 0.5896 0.028 Uiso 1 1 calc R . . Be1 Be 0.8647(5) 0.4053(12) 0.8140(6) 0.012(2) Uiso 1 1 d . . . Be2 Be 0.8649(4) -0.0868(12) 0.6713(6) 0.008(2) Uiso 1 1 d . . . Be3 Be 0.9729(5) 0.6297(13) 0.5905(7) 0.016(3) Uiso 1 1 d . . . Be4 Be 0.9748(4) 0.1351(11) 0.9097(6) 0.007(2) Uiso 1 1 d . . . O1 O 0.8848(2) 0.5999(7) 0.3973(3) 0.0140(14) Uani 1 1 d . . . O2 O 0.8890(2) -0.2119(6) 0.7193(3) 0.0128(13) Uani 1 1 d . . . O3 O 0.8819(2) -0.0977(6) 0.5888(3) 0.0108(13) Uani 1 1 d . . . O4 O 0.9395(2) -0.4298(7) 0.6591(3) 0.0128(13) Uani 1 1 d . . . O5 O 0.9674(2) 0.0683(6) 0.5803(3) 0.0124(13) Uani 1 1 d . . . O6 O 0.8939(3) 0.2878(6) 0.7675(3) 0.0142(14) Uani 1 1 d . . . O7 O 0.8425(2) 0.0699(7) 0.8352(3) 0.0138(14) Uani 1 1 d . . . O8 O 0.9475(2) 0.0729(7) 0.8324(3) 0.0127(13) Uani 1 1 d . . . O9 O 0.9397(2) 0.5798(7) 0.5204(3) 0.0148(14) Uani 1 1 d . . . O10 O 0.8333(3) -0.4216(8) 0.6465(3) 0.0202(15) Uani 1 1 d . . . O11 O 0.9344(2) -0.1009(6) 0.4702(3) 0.0128(13) Uani 1 1 d . . . O12 O 0.9830(3) -0.2059(7) 0.5957(3) 0.0138(14) Uani 1 1 d . . . O13 O 0.8807(3) 0.5479(7) 0.7798(3) 0.0162(15) Uani 1 1 d . . . O14 O 0.9861(2) 0.7042(6) 0.4015(3) 0.0128(13) Uani 1 1 d . . . O15 O 0.6992(2) 0.4166(7) 0.8334(4) 0.0190(15) Uani 1 1 d . . . O16 O 0.7491(3) 0.5562(7) 0.7269(4) 0.0191(15) Uani 1 1 d . . . O17 O 0.7317(3) 0.2911(8) 0.7096(4) 0.0308(19) Uani 1 1 d . . . O18 O 0.8025(2) 0.3727(7) 0.8176(4) 0.0216(16) Uani 1 1 d . . . O19 O 0.9686(2) 0.4325(6) 0.4022(3) 0.0133(13) Uani 1 1 d . . . O20 O 0.8916(3) 0.0479(7) 0.7047(3) 0.0138(14) Uani 1 1 d . . . As1 As 0.94646(3) 0.58202(9) 0.43157(5) 0.0097(2) Uani 1 1 d . . . As2 As 0.94340(3) -0.08609(9) 0.55941(5) 0.0087(2) Uani 1 1 d . . . As3 As 0.88616(4) -0.37752(9) 0.70152(5) 0.0105(2) Uani 1 1 d . . . As4 As 0.89441(3) 0.12143(9) 0.78439(5) 0.0102(2) Uani 1 1 d . . . As5 As 0.74642(4) 0.41218(10) 0.77481(5) 0.0152(2) Uani 1 1 d . . . OW1 O 0.0000 0.1150(12) 0.2500 0.030(3) Uani 1 2 d S . . OW2 O 0.0000 0.5971(12) 0.2500 0.031(3) Uani 1 2 d S . . N10A N 0.1696(4) 0.7958(11) 0.0324(5) 0.026(3) Uani 0.94(3) 1 d PD . . C11A C 0.2272(9) 0.775(2) 0.0335(12) 0.026(5) Uani 0.50 1 d P . . C12A C 0.2630(8) 0.836(3) 0.0227(12) 0.028(5) Uani 0.50 1 d P . . C10A C 0.2099(9) 0.892(2) 0.0198(11) 0.028(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.008(3) 0.017(4) 0.017(3) -0.001(3) 0.001(2) 0.002(3) O2 0.014(3) 0.006(3) 0.019(4) 0.000(3) -0.001(3) 0.002(3) O3 0.010(3) 0.010(3) 0.012(3) -0.004(2) 0.001(2) -0.005(3) O4 0.010(3) 0.014(3) 0.014(3) 0.003(3) 0.004(2) 0.004(3) O5 0.010(3) 0.010(3) 0.017(3) -0.001(3) 0.000(2) 0.001(3) O6 0.016(3) 0.005(3) 0.022(4) -0.004(3) 0.007(3) -0.001(3) O7 0.013(3) 0.018(4) 0.011(3) 0.000(3) 0.002(2) -0.003(3) O8 0.010(3) 0.018(4) 0.010(3) -0.004(3) 0.000(2) 0.004(3) O9 0.013(3) 0.018(4) 0.014(3) -0.002(3) 0.001(3) 0.001(3) O10 0.016(3) 0.029(4) 0.015(3) -0.005(3) -0.005(3) 0.001(3) O11 0.014(3) 0.014(3) 0.011(3) -0.002(3) 0.002(2) 0.005(3) O12 0.018(3) 0.015(4) 0.008(3) -0.002(3) -0.001(3) 0.002(3) O13 0.024(4) 0.010(3) 0.016(3) 0.001(3) 0.007(3) -0.002(3) O14 0.015(3) 0.009(3) 0.015(3) -0.004(3) 0.008(3) -0.004(3) O15 0.010(3) 0.026(4) 0.021(4) -0.003(3) 0.004(3) 0.001(3) O16 0.011(3) 0.012(4) 0.034(4) 0.005(3) 0.001(3) 0.000(3) O17 0.048(5) 0.018(4) 0.027(4) -0.005(3) 0.005(4) 0.009(4) O18 0.007(3) 0.025(4) 0.032(4) 0.010(3) -0.003(3) 0.001(3) O19 0.014(3) 0.009(3) 0.017(3) -0.005(3) -0.001(3) 0.004(3) O20 0.017(3) 0.013(3) 0.012(3) -0.004(3) 0.000(3) 0.000(3) As1 0.0111(4) 0.0086(4) 0.0093(4) -0.0005(3) 0.0010(3) -0.0009(4) As2 0.0099(4) 0.0072(4) 0.0091(4) -0.0001(3) 0.0006(3) -0.0005(3) As3 0.0116(4) 0.0097(5) 0.0103(4) 0.0002(3) 0.0008(3) -0.0007(4) As4 0.0102(4) 0.0106(5) 0.0096(4) 0.0002(3) -0.0003(3) 0.0000(4) As5 0.0100(4) 0.0129(5) 0.0227(5) 0.0016(4) 0.0018(4) 0.0006(4) OW1 0.025(6) 0.037(7) 0.028(6) 0.000 0.002(5) 0.000 OW2 0.035(6) 0.035(7) 0.024(6) 0.000 0.004(5) 0.000 N10A 0.017(5) 0.037(7) 0.024(6) 0.001(5) -0.003(4) 0.005(4) C11A 0.024(12) 0.021(12) 0.033(13) -0.003(10) -0.006(9) -0.001(10) C12A 0.019(11) 0.040(14) 0.025(12) -0.001(10) -0.007(9) -0.011(10) C10A 0.035(12) 0.025(13) 0.023(11) 0.004(9) -0.003(9) -0.017(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.493(16) . ? C1 C4 1.500(17) . ? C2 N1 1.508(14) . ? C4 CN1 1.474(15) . ? Be1 O13 1.608(14) . ? Be1 O18 1.618(13) . ? Be1 O1 1.622(13) 6_566 ? Be1 O6 1.646(13) . ? Be2 O20 1.611(13) . ? Be2 O3 1.622(12) . ? Be2 O15 1.629(12) 4_646 ? Be2 O2 1.634(13) . ? Be3 O9 1.610(14) . ? Be3 O19 1.612(14) 5_766 ? Be3 O12 1.649(15) 1_565 ? Be3 O4 1.673(14) 1_565 ? Be4 O11 1.595(12) 6_556 ? Be4 O5 1.616(12) 2_756 ? Be4 O14 1.623(13) 6_566 ? Be4 O8 1.698(12) . ? O1 Be1 1.622(13) 6_565 ? O1 As1 1.681(6) . ? O2 As3 1.673(6) . ? O3 As2 1.682(6) . ? O4 Be3 1.673(14) 1_545 ? O4 As3 1.678(6) . ? O5 Be4 1.616(12) 2_756 ? O5 As2 1.684(6) . ? O6 As4 1.676(6) . ? O7 As4 1.732(6) . ? O8 As4 1.663(6) . ? O9 As1 1.679(6) . ? O10 As3 1.717(6) . ? O11 Be4 1.595(12) 6 ? O11 As2 1.682(6) . ? O12 Be3 1.649(15) 1_545 ? O12 As2 1.681(6) . ? O13 As3 1.651(6) 1_565 ? O14 Be4 1.623(13) 6_565 ? O14 As1 1.684(6) . ? O15 Be2 1.629(12) 4_656 ? O15 As5 1.656(6) . ? O16 As5 1.686(7) . ? O17 As5 1.741(8) . ? O18 As5 1.654(6) . ? O19 Be3 1.612(14) 5_766 ? O19 As1 1.683(6) . ? O20 As4 1.658(6) . ? As3 O13 1.651(6) 1_545 ? N10A C10A 1.43(2) . ? N10A C11A 1.48(2) . ? C11A C12A 1.12(3) . ? C11A C10A 1.26(3) . ? C11A C12A 1.55(3) 7_565 ? C11A C11A 1.81(5) 7_565 ? C12A C10A 1.46(3) . ? C12A C11A 1.55(3) 7_565 ? C12A C12A 2.00(5) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C4 113.0(11) . . ? C1 C2 N1 116.0(10) . . ? CN1 C4 C1 111.8(10) . . ? O13 Be1 O18 117.0(8) . . ? O13 Be1 O1 109.6(8) . 6_566 ? O18 Be1 O1 103.1(7) . 6_566 ? O13 Be1 O6 106.4(7) . . ? O18 Be1 O6 110.1(8) . . ? O1 Be1 O6 110.7(8) 6_566 . ? O20 Be2 O3 107.6(7) . . ? O20 Be2 O15 114.2(8) . 4_646 ? O3 Be2 O15 104.6(7) . 4_646 ? O20 Be2 O2 105.6(7) . . ? O3 Be2 O2 111.4(7) . . ? O15 Be2 O2 113.4(7) 4_646 . ? O9 Be3 O19 113.9(8) . 5_766 ? O9 Be3 O12 115.2(8) . 1_565 ? O19 Be3 O12 103.3(8) 5_766 1_565 ? O9 Be3 O4 104.6(8) . 1_565 ? O19 Be3 O4 107.1(8) 5_766 1_565 ? O12 Be3 O4 112.6(8) 1_565 1_565 ? O11 Be4 O5 116.0(7) 6_556 2_756 ? O11 Be4 O14 113.3(7) 6_556 6_566 ? O5 Be4 O14 104.4(7) 2_756 6_566 ? O11 Be4 O8 105.9(7) 6_556 . ? O5 Be4 O8 106.9(7) 2_756 . ? O14 Be4 O8 110.0(7) 6_566 . ? Be1 O1 As1 128.2(6) 6_565 . ? Be2 O2 As3 128.3(6) . . ? Be2 O3 As2 126.2(5) . . ? Be3 O4 As3 134.2(6) 1_545 . ? Be4 O5 As2 135.8(6) 2_756 . ? Be1 O6 As4 126.4(6) . . ? As4 O8 Be4 130.7(5) . . ? Be3 O9 As1 137.2(6) . . ? Be4 O11 As2 130.9(6) 6 . ? Be3 O12 As2 125.6(6) 1_545 . ? Be1 O13 As3 141.0(6) . 1_565 ? Be4 O14 As1 124.2(5) 6_565 . ? Be2 O15 As5 135.4(6) 4_656 . ? Be1 O18 As5 139.3(6) . . ? Be3 O19 As1 128.8(6) 5_766 . ? Be2 O20 As4 135.7(6) . . ? O9 As1 O1 104.5(3) . . ? O9 As1 O19 111.1(3) . . ? O1 As1 O19 106.6(3) . . ? O9 As1 O14 115.2(3) . . ? O1 As1 O14 111.0(3) . . ? O19 As1 O14 108.1(3) . . ? O12 As2 O3 111.7(3) . . ? O12 As2 O11 113.4(3) . . ? O3 As2 O11 103.0(3) . . ? O12 As2 O5 109.9(3) . . ? O3 As2 O5 108.6(3) . . ? O11 As2 O5 110.1(3) . . ? O13 As3 O2 105.5(3) 1_545 . ? O13 As3 O4 112.2(3) 1_545 . ? O2 As3 O4 111.5(3) . . ? O13 As3 O10 109.2(3) 1_545 . ? O2 As3 O10 113.2(3) . . ? O4 As3 O10 105.4(3) . . ? O20 As4 O8 111.4(3) . . ? O20 As4 O6 105.2(3) . . ? O8 As4 O6 112.7(3) . . ? O20 As4 O7 110.9(3) . . ? O8 As4 O7 103.8(3) . . ? O6 As4 O7 113.1(3) . . ? O15 As5 O18 108.5(3) . . ? O15 As5 O16 112.0(3) . . ? O18 As5 O16 113.9(3) . . ? O15 As5 O17 109.9(4) . . ? O18 As5 O17 109.6(4) . . ? O16 As5 O17 102.7(4) . . ? C10A N10A C11A 51.6(14) . . ? C12A C11A C10A 75(2) . . ? C12A C11A N10A 137(2) . . ? C10A C11A N10A 62.2(14) . . ? C12A C11A C12A 96(2) . 7_565 ? C10A C11A C12A 125(2) . 7_565 ? N10A C11A C12A 105.9(16) . 7_565 ? C12A C11A C11A 58.3(18) . 7_565 ? C10A C11A C11A 110(2) . 7_565 ? N10A C11A C11A 134(2) . 7_565 ? C12A C11A C11A 37.9(12) 7_565 7_565 ? C11A C12A C10A 56.9(17) . . ? C11A C12A C11A 84(2) . 7_565 ? C10A C12A C11A 114.8(18) . 7_565 ? C11A C12A C12A 50.2(16) . 7_565 ? C10A C12A C12A 91.1(17) . 7_565 ? C11A C12A C12A 33.7(12) 7_565 7_565 ? C11A C10A N10A 66.2(15) . . ? C11A C10A C12A 47.8(16) . . ? N10A C10A C12A 113.9(19) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.093 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.282