# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H14 Be N2 O8 P2' _chemical_formula_weight 325.15 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.7297(5) _cell_length_b 14.3257(7) _cell_length_c 21.7040(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2403.4(2) _cell_formula_units_Z 8 _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 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8817 _exptl_absorpt_correction_T_max 0.9532 _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _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 21568 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 26.50 _reflns_number_total 2485 _reflns_number_gt 2213 _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^)+(0.0369P)^2^+3.3747P] 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 2485 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Be1 Be 0.2376(4) 0.0294(2) -0.01844(13) 0.0123(6) Uani 1 1 d . . . P1 P 0.02175(8) 0.07970(4) 0.08432(3) 0.01297(16) Uani 1 1 d . . . P2 P 0.43065(8) -0.09004(4) 0.07044(3) 0.01137(16) Uani 1 1 d . . . O1 O 0.1367(2) 0.05367(13) 0.13824(7) 0.0215(4) Uani 1 1 d . . . O2 O -0.0752(2) 0.17310(12) 0.10081(8) 0.0195(4) Uani 1 1 d . . . H2E H -0.0075 0.2170 0.0982 0.029 Uiso 1 1 calc R . . O3 O -0.1181(2) 0.00741(12) 0.07458(7) 0.0177(4) Uani 1 1 d . . . O4 O 0.1249(2) 0.10004(11) 0.02557(7) 0.0168(4) Uani 1 1 d . . . O5 O 0.3087(2) -0.05837(12) 0.02007(7) 0.0176(4) Uani 1 1 d . . . O6 O 0.4257(2) -0.01899(12) 0.12505(8) 0.0212(4) Uani 1 1 d . . . H6C H 0.3284 0.0034 0.1279 0.032 Uiso 1 1 calc R . . O7 O 0.6163(2) -0.09798(11) 0.04801(8) 0.0171(4) Uani 1 1 d . . . O8 O 0.3715(2) -0.18539(11) 0.09379(8) 0.0178(4) Uani 1 1 d . . . C1 C 0.3763(5) -0.3057(2) -0.26049(12) 0.0373(8) Uani 1 1 d . . . H1A H 0.3526 -0.3291 -0.2996 0.045 Uiso 1 1 calc R . . C2 C 0.4292(6) -0.2158(2) -0.25379(15) 0.0522(11) Uani 1 1 d . . . H2D H 0.4404 -0.1773 -0.2881 0.063 Uiso 1 1 calc R . . C3 C 0.4662(5) -0.1822(2) -0.19579(14) 0.0411(8) Uani 1 1 d . . . H3A H 0.5023 -0.1206 -0.1910 0.049 Uiso 1 1 calc R . . C4 C 0.4503(3) -0.23887(18) -0.14472(11) 0.0202(5) Uani 1 1 d . . . C5 C 0.3943(4) -0.32890(19) -0.15405(12) 0.0241(6) Uani 1 1 d . . . H5A H 0.3812 -0.3685 -0.1204 0.029 Uiso 1 1 calc R . . C6 C 0.4789(4) -0.19864(19) -0.08181(12) 0.0259(6) Uani 1 1 d . . . H6A H 0.5401 -0.1399 -0.0862 0.031 Uiso 1 1 calc R . . H6B H 0.3670 -0.1850 -0.0636 0.031 Uiso 1 1 calc R . . C7 C 0.2948(5) -0.4576(2) -0.21829(14) 0.0388(8) Uani 1 1 d . . . H7A H 0.2749 -0.4702 -0.2612 0.058 Uiso 1 1 calc R . . H7B H 0.1886 -0.4651 -0.1959 0.058 Uiso 1 1 calc R . . H7C H 0.3798 -0.5003 -0.2026 0.058 Uiso 1 1 calc R . . N1 N 0.3580(3) -0.36072(16) -0.21097(10) 0.0236(5) Uani 1 1 d . . . N2 N 0.5764(3) -0.25826(14) -0.03895(9) 0.0196(5) Uani 1 1 d . . . H2A H 0.5871 -0.2293 -0.0029 0.029 Uiso 1 1 calc R . . H2B H 0.6808 -0.2697 -0.0544 0.029 Uiso 1 1 calc R . . H2C H 0.5201 -0.3119 -0.0336 0.029 Uiso 1 1 calc R . . 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 0.0103(14) 0.0137(14) 0.0130(14) 0.0011(11) 0.0010(11) -0.0021(12) P1 0.0124(3) 0.0134(3) 0.0130(3) -0.0024(2) 0.0000(2) 0.0000(2) P2 0.0116(3) 0.0096(3) 0.0129(3) 0.0011(2) 0.0003(2) -0.0003(2) O1 0.0188(9) 0.0299(10) 0.0158(9) -0.0047(7) -0.0034(7) 0.0049(8) O2 0.0166(9) 0.0147(9) 0.0272(9) -0.0039(7) 0.0050(7) -0.0007(7) O3 0.0217(9) 0.0161(9) 0.0153(8) 0.0016(7) -0.0039(7) -0.0053(7) O4 0.0173(9) 0.0143(8) 0.0189(9) -0.0013(7) 0.0043(7) 0.0017(7) O5 0.0197(9) 0.0157(9) 0.0175(8) 0.0024(7) -0.0030(7) 0.0028(7) O6 0.0186(9) 0.0229(9) 0.0223(9) -0.0079(7) -0.0035(7) 0.0051(8) O7 0.0125(8) 0.0165(9) 0.0224(9) 0.0011(7) 0.0031(7) -0.0011(7) O8 0.0168(9) 0.0136(8) 0.0230(9) 0.0058(7) 0.0011(7) -0.0017(7) C1 0.056(2) 0.0423(18) 0.0138(14) 0.0015(12) -0.0019(13) -0.0044(16) C2 0.095(3) 0.0418(19) 0.0199(15) 0.0113(14) -0.0022(17) -0.019(2) C3 0.065(2) 0.0280(16) 0.0302(16) 0.0061(13) -0.0011(16) -0.0140(16) C4 0.0203(13) 0.0203(13) 0.0201(13) 0.0006(10) -0.0002(10) 0.0026(11) C5 0.0325(15) 0.0246(14) 0.0153(12) 0.0038(10) 0.0006(11) -0.0003(12) C6 0.0336(16) 0.0220(13) 0.0222(14) -0.0028(11) -0.0051(12) 0.0080(12) C7 0.055(2) 0.0305(17) 0.0306(16) -0.0052(13) -0.0053(15) -0.0103(15) N1 0.0295(12) 0.0231(12) 0.0183(11) -0.0005(9) -0.0005(9) -0.0014(10) N2 0.0195(11) 0.0212(11) 0.0179(10) -0.0009(9) 0.0008(9) 0.0012(9) _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 Be1 O5 1.606(3) . ? Be1 O3 1.617(3) 5 ? Be1 O7 1.630(3) 5_655 ? Be1 O4 1.642(3) . ? P1 O3 1.5118(17) . ? P1 O1 1.5158(17) . ? P1 O4 1.5319(17) . ? P1 O2 1.5747(17) . ? P2 O5 1.5132(17) . ? P2 O7 1.5192(17) . ? P2 O8 1.5271(17) . ? P2 O6 1.5629(17) . ? O2 H2E 0.8200 . ? O3 Be1 1.617(3) 5 ? O6 H6C 0.8200 . ? O7 Be1 1.630(3) 5_655 ? C1 N1 1.341(4) . ? C1 C2 1.358(4) . ? C1 H1A 0.9300 . ? C2 C3 1.378(5) . ? C2 H2D 0.9300 . ? C3 C4 1.380(4) . ? C3 H3A 0.9300 . ? C4 C5 1.376(4) . ? C4 C6 1.498(3) . ? C5 N1 1.346(3) . ? C5 H5A 0.9300 . ? C6 N2 1.470(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N1 1.480(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? 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 O5 Be1 O3 109.4(2) . 5 ? O5 Be1 O7 116.1(2) . 5_655 ? O3 Be1 O7 107.21(18) 5 5_655 ? O5 Be1 O4 111.17(18) . . ? O3 Be1 O4 109.67(19) 5 . ? O7 Be1 O4 102.99(19) 5_655 . ? O3 P1 O1 111.00(10) . . ? O3 P1 O4 112.71(9) . . ? O1 P1 O4 112.60(10) . . ? O3 P1 O2 105.89(10) . . ? O1 P1 O2 108.20(10) . . ? O4 P1 O2 105.98(9) . . ? O5 P2 O7 112.30(10) . . ? O5 P2 O8 108.74(10) . . ? O7 P2 O8 108.79(10) . . ? O5 P2 O6 109.72(10) . . ? O7 P2 O6 108.35(10) . . ? O8 P2 O6 108.87(10) . . ? P1 O2 H2E 109.5 . . ? P1 O3 Be1 137.46(15) . 5 ? P1 O4 Be1 130.02(15) . . ? P2 O5 Be1 145.46(16) . . ? P2 O6 H6C 109.5 . . ? P2 O7 Be1 137.38(16) . 5_655 ? N1 C1 C2 120.2(3) . . ? N1 C1 H1A 119.9 . . ? C2 C1 H1A 119.9 . . ? C1 C2 C3 119.5(3) . . ? C1 C2 H2D 120.3 . . ? C3 C2 H2D 120.3 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 117.5(2) . . ? C5 C4 C6 122.8(2) . . ? C3 C4 C6 119.5(2) . . ? N1 C5 C4 121.2(2) . . ? N1 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? N2 C6 C4 115.4(2) . . ? N2 C6 H6A 108.4 . . ? C4 C6 H6A 108.4 . . ? N2 C6 H6B 108.4 . . ? C4 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 N1 C5 121.0(2) . . ? C1 N1 C7 120.0(2) . . ? C5 N1 C7 119.0(2) . . ? C6 N2 H2A 109.5 . . ? C6 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C6 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? 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 O2 H2E O8 0.82 1.75 2.571(2) 177.1 8_665 O6 H6C O1 0.82 1.66 2.481(2) 175.5 . N2 H2A O7 0.89 2.19 2.988(3) 148.5 . N2 H2B O8 0.89 1.82 2.697(3) 167.6 4_545 N2 H2C O4 0.89 2.12 2.916(3) 148.3 8_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.302 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 964923' data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H25 Be3 N2 O17.50 P4' _chemical_formula_weight 580.21 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 8.7135(7) _cell_length_b 13.8526(4) _cell_length_c 17.1154(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.947(5) _cell_angle_gamma 90.00 _cell_volume 2040.77(18) _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 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.464 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9295 _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _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 19495 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4219 _reflns_number_gt 3644 _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^)+(0.0802P)^2^+3.2213P] 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 4219 _refine_ls_number_parameters 379 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1531 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.099 _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 Be1 Be 0.2029(5) 0.9892(3) 0.2355(2) 0.0137(8) Uani 1 1 d . . . Be2 Be 0.5999(4) 1.1353(3) 0.1772(2) 0.0123(7) Uani 1 1 d . . . Be3 Be -0.4013(5) 0.8564(3) 0.1942(2) 0.0149(8) Uani 1 1 d . . . P1 P 0.38362(9) 0.99033(5) 0.10078(5) 0.0121(2) Uani 1 1 d . . . P2 P 0.41888(9) 1.13826(5) 0.31303(4) 0.0119(2) Uani 1 1 d . . . P3 P -0.15450(9) 1.00108(5) 0.22442(5) 0.0124(2) Uani 1 1 d . . . P4 P 0.41005(9) 0.85220(5) 0.32192(4) 0.0123(2) Uani 1 1 d . . . O1 O 0.2536(3) 1.00603(17) 0.14779(14) 0.0240(6) Uani 1 1 d . . . O1W O -0.4164(5) 1.2510(3) -0.0135(2) 0.0304(9) Uani 0.70 1 d P . . O1W' O -0.5211(14) 1.2458(8) -0.0106(6) 0.040(2) Uani 0.30 1 d PU . . O2 O 0.4694(3) 0.89524(16) 0.11967(13) 0.0197(5) Uani 1 1 d . . . O2W O -0.2208(17) 1.5034(7) 0.0103(14) 0.167(8) Uani 0.50 1 d P . . O3 O 0.2949(3) 0.98258(17) 0.01209(13) 0.0214(5) Uani 1 1 d . . . H3A H 0.3564 0.9665 -0.0172 0.032 Uiso 1 1 calc R . . O4 O 0.4951(3) 1.07563(16) 0.10242(13) 0.0210(5) Uani 1 1 d . . . O5 O 0.5371(3) 1.11914(17) 0.25898(14) 0.0236(5) Uani 1 1 d . . . O6 O 0.3762(3) 1.24286(15) 0.32098(14) 0.0213(5) Uani 1 1 d . . . O7 O 0.5001(3) 1.10210(17) 0.39823(13) 0.0250(6) Uani 1 1 d . . . H7D H 0.5266 1.1489 0.4264 0.037 Uiso 1 1 calc R . . O8 O 0.2750(3) 1.07623(17) 0.29398(14) 0.0226(5) Uani 1 1 d . . . O9 O 0.2573(3) 0.88473(16) 0.27438(15) 0.0227(5) Uani 1 1 d . . . O10 O 0.4014(3) 0.74791(15) 0.34979(13) 0.0189(5) Uani 1 1 d . . . O11 O 0.4402(3) 0.90763(16) 0.40434(13) 0.0283(6) Uani 1 1 d . . . H11A H 0.4570 0.9648 0.3967 0.042 Uiso 1 1 calc R . . O12 O 0.5477(3) 0.87375(17) 0.28026(13) 0.0210(5) Uani 1 1 d . . . O13 O 0.0163(3) 0.99560(16) 0.22257(17) 0.0261(6) Uani 1 1 d . . . O14 O -0.2242(2) 1.09324(15) 0.18534(13) 0.0186(5) Uani 1 1 d . . . O15 O -0.1738(3) 1.00556(18) 0.31593(15) 0.0279(6) Uani 1 1 d . . . H15A H -0.2526 1.0359 0.3207 0.042 Uiso 1 1 calc R . . O16 O -0.2374(3) 0.91042(16) 0.19059(14) 0.0196(5) Uani 1 1 d . . . C1 C -0.0528(8) 1.1676(4) -0.0455(3) 0.0450(14) Uani 0.80 1 d PU . . C1' C 0.061(2) 1.1602(12) -0.0477(9) 0.020(3) Uani 0.20 1 d PU . . C2 C -0.0260(6) 1.1584(4) 0.0452(3) 0.0337(11) Uani 0.80 1 d PU . . C2' C 0.108(2) 1.1656(12) 0.0421(10) 0.023(4) Uani 0.20 1 d PU . . C3 C 0.1854(6) 1.2621(5) -0.0361(3) 0.0434(13) Uani 0.80 1 d PU . . C3' C 0.097(2) 1.3399(13) -0.0461(10) 0.023(4) Uani 0.20 1 d PU . . C4 C 0.2078(5) 1.2605(4) 0.0549(3) 0.0335(11) Uani 0.80 1 d PU . . C4' C 0.1125(19) 1.3442(12) 0.0417(10) 0.021(3) Uani 0.20 1 d PU . . C5 C -0.0648(7) 1.3443(4) -0.0364(3) 0.0411(13) Uani 0.80 1 d PU . . C5' C -0.1612(19) 1.2678(13) -0.0463(9) 0.020(3) Uani 0.20 1 d PU . . C6 C -0.0488(6) 1.3356(4) 0.0537(3) 0.0359(12) Uani 0.80 1 d P . . C6' C -0.1337(19) 1.2572(12) 0.0419(10) 0.020(3) Uani 0.20 1 d PU . . C7 C -0.0116(6) 1.2644(3) -0.1600(2) 0.0394(10) Uani 1 1 d . . . H7A H 0.0879 1.2603 -0.1772 0.059 Uiso 1 1 calc R . . H7B H -0.0605 1.3244 -0.1774 0.059 Uiso 1 1 calc R . . H7C H -0.0757 1.2117 -0.1819 0.059 Uiso 1 1 calc R . . C8 C 0.0684(6) 1.2457(3) 0.1681(2) 0.0391(10) Uani 1 1 d . . . H8A H 0.1771 1.2425 0.1891 0.059 Uiso 1 1 calc R . . H8B H 0.0172 1.1890 0.1835 0.059 Uiso 1 1 calc R . . H8C H 0.0238 1.3020 0.1884 0.059 Uiso 1 1 calc R . . N1 N 0.0484(3) 1.2513(2) 0.07926(16) 0.0213(6) Uani 1 1 d . . . N2 N 0.0096(4) 1.2594(2) -0.07126(17) 0.0239(6) 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 0.0127(19) 0.0113(18) 0.0179(19) -0.0012(14) 0.0048(15) 0.0006(14) Be2 0.0114(18) 0.0109(18) 0.0148(18) 0.0000(14) 0.0022(14) -0.0003(14) Be3 0.0145(19) 0.0144(19) 0.0164(19) -0.0003(15) 0.0040(15) -0.0015(15) P1 0.0114(4) 0.0137(4) 0.0108(4) -0.0012(3) 0.0003(3) -0.0013(3) P2 0.0151(4) 0.0089(4) 0.0123(4) 0.0001(3) 0.0043(3) -0.0012(3) P3 0.0084(4) 0.0122(4) 0.0165(4) 0.0006(3) 0.0021(3) 0.0000(3) P4 0.0161(4) 0.0087(4) 0.0129(4) 0.0000(3) 0.0044(3) 0.0007(3) O1 0.0180(12) 0.0385(15) 0.0162(12) -0.0010(10) 0.0050(9) 0.0046(10) O1W 0.052(3) 0.0207(19) 0.0162(17) -0.0010(14) -0.0019(18) 0.0004(18) O1W' 0.054(4) 0.035(4) 0.030(4) 0.002(3) -0.001(4) 0.003(4) O2 0.0224(12) 0.0161(11) 0.0188(11) -0.0013(9) -0.0022(9) 0.0026(9) O2W 0.108(11) 0.078(8) 0.33(3) 0.005(9) 0.095(14) -0.026(6) O3 0.0201(12) 0.0309(13) 0.0124(11) -0.0023(9) -0.0003(9) -0.0030(10) O4 0.0237(12) 0.0183(11) 0.0197(11) 0.0010(9) -0.0008(9) -0.0077(9) O5 0.0251(13) 0.0254(13) 0.0236(12) 0.0024(10) 0.0142(10) 0.0018(10) O6 0.0284(13) 0.0109(11) 0.0253(12) 0.0000(9) 0.0065(10) 0.0002(9) O7 0.0401(15) 0.0184(12) 0.0139(11) -0.0003(9) -0.0037(10) -0.0011(10) O8 0.0205(12) 0.0208(12) 0.0275(13) -0.0082(10) 0.0069(10) -0.0082(9) O9 0.0156(11) 0.0141(11) 0.0379(14) 0.0065(10) 0.0024(10) 0.0025(9) O10 0.0274(12) 0.0101(11) 0.0184(11) 0.0007(8) 0.0015(9) 0.0000(9) O11 0.0594(18) 0.0115(11) 0.0159(12) -0.0024(9) 0.0117(11) -0.0028(11) O12 0.0194(12) 0.0278(13) 0.0171(11) -0.0016(9) 0.0073(9) -0.0004(10) O13 0.0096(12) 0.0251(14) 0.0436(16) 0.0037(10) 0.0043(11) 0.0013(9) O14 0.0136(11) 0.0155(11) 0.0277(12) 0.0048(9) 0.0065(9) 0.0031(8) O15 0.0242(14) 0.0422(16) 0.0166(12) 0.0002(10) 0.0014(10) 0.0044(10) O16 0.0151(11) 0.0160(11) 0.0287(13) -0.0027(9) 0.0070(9) -0.0041(9) C1 0.067(3) 0.037(3) 0.030(2) 0.003(2) 0.004(2) -0.018(3) C1' 0.024(5) 0.021(5) 0.016(5) 0.001(4) 0.006(4) 0.010(4) C2 0.046(3) 0.030(2) 0.024(2) -0.0002(18) 0.0034(19) -0.012(2) C2' 0.024(5) 0.022(5) 0.022(5) -0.003(4) 0.000(4) 0.009(4) C3 0.027(2) 0.070(3) 0.035(2) -0.001(2) 0.010(2) -0.001(2) C3' 0.027(5) 0.025(5) 0.019(5) 0.003(4) 0.004(4) -0.008(4) C4 0.022(2) 0.047(3) 0.032(2) 0.003(2) 0.0049(18) -0.0034(19) C4' 0.023(5) 0.021(5) 0.019(5) 0.001(4) -0.002(4) -0.009(4) C5 0.053(3) 0.040(3) 0.030(2) 0.001(2) 0.010(2) 0.017(2) C5' 0.017(5) 0.027(5) 0.018(5) -0.001(4) 0.006(4) 0.000(4) C6 0.049(3) 0.037(3) 0.022(2) 0.001(2) 0.004(2) 0.019(2) C6' 0.016(5) 0.022(5) 0.022(5) 0.004(4) 0.007(4) -0.005(4) C7 0.056(3) 0.044(2) 0.0208(19) 0.0056(17) 0.0131(18) 0.006(2) C8 0.052(3) 0.046(2) 0.0184(18) -0.0029(17) 0.0005(17) -0.008(2) N1 0.0225(15) 0.0218(14) 0.0203(14) -0.0020(11) 0.0055(11) -0.0053(11) N2 0.0300(16) 0.0241(15) 0.0197(14) 0.0017(12) 0.0102(12) 0.0023(12) _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 Be1 O13 1.609(5) . ? Be1 O8 1.629(4) . ? Be1 O9 1.631(4) . ? Be1 O1 1.646(5) . ? Be2 O5 1.595(4) . ? Be2 O14 1.625(4) 1_655 ? Be2 O10 1.627(4) 2_655 ? Be2 O4 1.671(4) . ? Be3 O6 1.614(4) 2_545 ? Be3 O12 1.621(4) 1_455 ? Be3 O16 1.623(4) . ? Be3 O2 1.655(4) 1_455 ? P1 O1 1.504(2) . ? P1 O2 1.524(2) . ? P1 O4 1.527(2) . ? P1 O3 1.597(2) . ? P2 O6 1.507(2) . ? P2 O5 1.511(2) . ? P2 O8 1.513(2) . ? P2 O7 1.599(2) . ? P3 O13 1.496(2) . ? P3 O16 1.518(2) . ? P3 O14 1.523(2) . ? P3 O15 1.602(3) . ? P4 O9 1.517(2) . ? P4 O12 1.517(2) . ? P4 O10 1.527(2) . ? P4 O11 1.592(2) . ? O1W O1W' 0.924(11) . ? O2 Be3 1.655(4) 1_655 ? O3 H3A 0.8200 . ? O6 Be3 1.614(4) 2 ? O7 H7D 0.8200 . ? O10 Be2 1.627(4) 2_645 ? O11 H11A 0.8200 . ? O12 Be3 1.621(4) 1_655 ? O14 Be2 1.625(4) 1_455 ? O15 H15A 0.8200 . ? C1 C1' 1.007(18) . ? C1 N2 1.478(6) . ? C1 C2 1.539(7) . ? C1 C5' 1.678(18) . ? C1 C2' 1.886(18) . ? C1' N2 1.483(16) . ? C1' C2' 1.53(2) . ? C1' C3 1.769(19) . ? C1' C2 1.866(18) . ? C2 C2' 1.179(18) . ? C2 N1 1.516(5) . ? C2 C6' 1.656(17) . ? C2' N1 1.477(16) . ? C2' C4 1.574(18) . ? C3 C3' 1.323(19) . ? C3 C4 1.540(7) . ? C3 N2 1.556(6) . ? C3 C4' 1.933(18) . ? C3' N2 1.379(17) . ? C3' C5 1.443(18) . ? C3' C4' 1.49(2) . ? C4 C4' 1.424(18) . ? C4 N1 1.517(5) . ? C4' C6 1.457(18) . ? C4' N1 1.580(16) . ? C4' C5 1.879(18) . ? C5 C5' 1.345(18) . ? C5 N2 1.509(6) . ? C5 C6 1.531(7) . ? C5 C6' 1.965(17) . ? C5' C6' 1.50(2) . ? C5' N2 1.615(16) . ? C6 C6' 1.312(17) . ? C6 N1 1.469(5) . ? C6' N1 1.618(16) . ? C7 N2 1.502(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.505(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 O13 Be1 O8 109.2(3) . . ? O13 Be1 O9 109.2(2) . . ? O8 Be1 O9 110.3(3) . . ? O13 Be1 O1 105.9(3) . . ? O8 Be1 O1 108.8(2) . . ? O9 Be1 O1 113.3(3) . . ? O5 Be2 O14 108.8(2) . 1_655 ? O5 Be2 O10 113.3(3) . 2_655 ? O14 Be2 O10 109.5(2) 1_655 2_655 ? O5 Be2 O4 112.4(3) . . ? O14 Be2 O4 106.5(2) 1_655 . ? O10 Be2 O4 106.1(2) 2_655 . ? O6 Be3 O12 110.8(3) 2_545 1_455 ? O6 Be3 O16 107.5(3) 2_545 . ? O12 Be3 O16 109.5(3) 1_455 . ? O6 Be3 O2 106.6(2) 2_545 1_455 ? O12 Be3 O2 113.7(3) 1_455 1_455 ? O16 Be3 O2 108.5(3) . 1_455 ? O1 P1 O2 113.39(13) . . ? O1 P1 O4 114.09(14) . . ? O2 P1 O4 112.04(13) . . ? O1 P1 O3 102.97(14) . . ? O2 P1 O3 107.02(13) . . ? O4 P1 O3 106.39(13) . . ? O6 P2 O5 115.15(14) . . ? O6 P2 O8 110.96(14) . . ? O5 P2 O8 112.92(14) . . ? O6 P2 O7 107.41(13) . . ? O5 P2 O7 104.84(14) . . ? O8 P2 O7 104.65(13) . . ? O13 P3 O16 111.46(13) . . ? O13 P3 O14 111.31(13) . . ? O16 P3 O14 113.11(14) . . ? O13 P3 O15 106.18(15) . . ? O16 P3 O15 106.80(13) . . ? O14 P3 O15 107.55(13) . . ? O9 P4 O12 112.44(13) . . ? O9 P4 O10 111.53(13) . . ? O12 P4 O10 114.45(14) . . ? O9 P4 O11 110.02(14) . . ? O12 P4 O11 106.72(14) . . ? O10 P4 O11 100.89(12) . . ? P1 O1 Be1 143.0(2) . . ? P1 O2 Be3 134.2(2) . 1_655 ? P1 O3 H3A 109.5 . . ? P1 O4 Be2 131.8(2) . . ? P2 O5 Be2 150.6(2) . . ? P2 O6 Be3 151.7(2) . 2 ? P2 O7 H7D 109.5 . . ? P2 O8 Be1 141.3(2) . . ? P4 O9 Be1 131.1(2) . . ? P4 O10 Be2 144.8(2) . 2_645 ? P4 O11 H11A 109.5 . . ? P4 O12 Be3 138.2(2) . 1_655 ? P3 O13 Be1 171.0(3) . . ? P3 O14 Be2 130.1(2) . 1_455 ? P3 O15 H15A 109.5 . . ? P3 O16 Be3 137.4(2) . . ? C1' C1 N2 70.4(10) . . ? C1' C1 C2 91.8(10) . . ? N2 C1 C2 111.5(4) . . ? C1' C1 C5' 129.9(12) . . ? N2 C1 C5' 61.2(6) . . ? C2 C1 C5' 94.2(7) . . ? C1' C1 C2' 54.0(11) . . ? N2 C1 C2' 89.3(6) . . ? C2 C1 C2' 38.6(6) . . ? C5' C1 C2' 111.4(8) . . ? C1 C1' N2 69.8(10) . . ? C1 C1' C2' 93.8(14) . . ? N2 C1' C2' 104.5(12) . . ? C1 C1' C3 120.4(13) . . ? N2 C1' C3 56.4(6) . . ? C2' C1' C3 77.7(11) . . ? C1 C1' C2 55.5(9) . . ? N2 C1' C2 95.6(8) . . ? C2' C1' C2 39.1(8) . . ? C3 C1' C2 103.8(8) . . ? C2' C2 N1 65.1(9) . . ? C2' C2 C1 86.8(9) . . ? N1 C2 C1 107.9(4) . . ? C2' C2 C6' 119.2(11) . . ? N1 C2 C6' 61.1(6) . . ? C1 C2 C6' 84.3(7) . . ? C2' C2 C1' 54.8(10) . . ? N1 C2 C1' 96.3(6) . . ? C1 C2 C1' 32.6(6) . . ? C6' C2 C1' 105.3(8) . . ? C2 C2' N1 68.6(9) . . ? C2 C2' C1' 86.1(12) . . ? N1 C2' C1' 114.6(12) . . ? C2 C2' C4 126.5(13) . . ? N1 C2' C4 59.5(7) . . ? C1' C2' C4 103.5(13) . . ? C2 C2' C1 54.6(7) . . ? N1 C2' C1 93.7(8) . . ? C1' C2' C1 32.2(7) . . ? C4 C2' C1 115.1(10) . . ? C3' C3 C4 97.0(8) . . ? C3' C3 N2 56.5(8) . . ? C4 C3 N2 110.7(4) . . ? C3' C3 C1' 107.5(10) . . ? C4 C3 C1' 94.6(6) . . ? N2 C3 C1' 52.5(6) . . ? C3' C3 C4' 50.2(9) . . ? C4 C3 C4' 46.7(5) . . ? N2 C3 C4' 82.6(5) . . ? C1' C3 C4' 106.6(7) . . ? C3 C3' N2 70.3(9) . . ? C3 C3' C5 125.5(13) . . ? N2 C3' C5 64.6(8) . . ? C3 C3' C4' 86.7(12) . . ? N2 C3' C4' 107.9(12) . . ? C5 C3' C4' 79.7(11) . . ? C4' C4 N1 64.9(7) . . ? C4' C4 C3 81.3(8) . . ? N1 C4 C3 107.6(4) . . ? C4' C4 C2' 111.2(9) . . ? N1 C4 C2' 57.1(6) . . ? C3 C4 C2' 83.7(7) . . ? C4 C4' C6 117.6(11) . . ? C4 C4' C3' 95.0(13) . . ? C6 C4' C3' 101.5(12) . . ? C4 C4' N1 60.4(7) . . ? C6 C4' N1 57.7(6) . . ? C3' C4' N1 113.3(12) . . ? C4 C4' C5 120.5(10) . . ? C6 C4' C5 52.8(6) . . ? C3' C4' C5 49.1(9) . . ? N1 C4' C5 89.2(8) . . ? C4 C4' C3 51.9(6) . . ? C6 C4' C3 118.5(10) . . ? C3' C4' C3 43.1(9) . . ? N1 C4' C3 88.6(8) . . ? C5 C4' C3 80.3(7) . . ? C5' C5 C3' 123.6(11) . . ? C5' C5 N2 68.6(7) . . ? C3' C5 N2 55.6(7) . . ? C5' C5 C6 91.3(8) . . ? C3' C5 C6 100.1(8) . . ? N2 C5 C6 111.1(4) . . ? C5' C5 C4' 121.1(9) . . ? C3' C5 C4' 51.2(8) . . ? N2 C5 C4' 85.7(6) . . ? C6 C5 C4' 49.3(6) . . ? C5' C5 C6' 49.6(8) . . ? C3' C5 C6' 117.4(9) . . ? N2 C5 C6' 89.3(6) . . ? C6 C5 C6' 41.8(5) . . ? C4' C5 C6' 79.6(7) . . ? C5 C5' C6' 87.2(11) . . ? C5 C5' N2 60.5(7) . . ? C6' C5' N2 104.5(12) . . ? C5 C5' C1 108.1(10) . . ? C6' C5' C1 84.8(11) . . ? N2 C5' C1 53.3(5) . . ? C6' C6 C4' 125.4(11) . . ? C6' C6 N1 70.9(8) . . ? C4' C6 N1 65.4(7) . . ? C6' C6 C5 87.1(8) . . ? C4' C6 C5 77.9(7) . . ? N1 C6 C5 108.7(4) . . ? C6 C6' C5' 94.1(12) . . ? C6 C6' N1 59.1(7) . . ? C5' C6' N1 113.3(12) . . ? C6 C6' C2 112.1(11) . . ? C5' C6' C2 96.6(11) . . ? N1 C6' C2 55.2(6) . . ? C6 C6' C5 51.1(6) . . ? C5' C6' C5 43.2(8) . . ? N1 C6' C5 85.2(7) . . ? C2 C6' C5 107.4(8) . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 N1 C2' 137.3(7) . . ? C6 N1 C8 108.2(3) . . ? C2' N1 C8 113.6(7) . . ? C6 N1 C2 111.6(4) . . ? C2' N1 C2 46.3(7) . . ? C8 N1 C2 108.7(3) . . ? C6 N1 C4 111.2(3) . . ? C2' N1 C4 63.4(7) . . ? C8 N1 C4 108.4(3) . . ? C2 N1 C4 108.7(3) . . ? C6 N1 C4' 56.9(7) . . ? C2' N1 C4' 108.0(10) . . ? C8 N1 C4' 117.4(6) . . ? C2 N1 C4' 133.8(7) . . ? C4 N1 C4' 54.7(7) . . ? C6 N1 C6' 50.0(6) . . ? C2' N1 C6' 105.0(9) . . ? C8 N1 C6' 110.8(6) . . ? C2 N1 C6' 63.7(6) . . ? C4 N1 C6' 140.4(6) . . ? C4' N1 C6' 100.7(8) . . ? C3' N2 C1 144.4(7) . . ? C3' N2 C1' 122.3(11) . . ? C1 N2 C1' 39.8(7) . . ? C3' N2 C7 104.7(7) . . ? C1 N2 C7 110.3(3) . . ? C1' N2 C7 107.6(7) . . ? C3' N2 C5 59.8(8) . . ? C1 N2 C5 110.6(4) . . ? C1' N2 C5 138.2(7) . . ? C7 N2 C5 111.8(3) . . ? C3' N2 C3 53.2(8) . . ? C1 N2 C3 106.9(4) . . ? C1' N2 C3 71.2(8) . . ? C7 N2 C3 110.4(3) . . ? C5 N2 C3 106.7(4) . . ? C3' N2 C5' 110.1(10) . . ? C1 N2 C5' 65.5(7) . . ? C1' N2 C5' 104.4(9) . . ? C7 N2 C5' 106.9(6) . . ? C5 N2 C5' 50.9(6) . . ? C3 N2 C5' 142.0(6) . . ? 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 O3 H3A O4 0.82 2.17 2.993(3) 175.6 3_675 O7 H7D O1W 0.82 1.75 2.572(4) 179.9 4_686 O7 H7D O1W' 0.82 1.90 2.646(11) 151.1 4_686 O11 H11A O7 0.82 1.94 2.749(3) 170.1 . O15 H15A O5 0.82 2.28 3.001(4) 147.0 1_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.675 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 964924' data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H26 Be2 N2 O16 P4' _chemical_formula_weight 548.21 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7901(5) _cell_length_b 8.8969(3) _cell_length_c 15.0950(2) _cell_angle_alpha 88.590(3) _cell_angle_beta 75.260(4) _cell_angle_gamma 62.810(7) _cell_volume 1009.71(7) _cell_formula_units_Z 2 _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 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.459 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8671 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10009 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4160 _reflns_number_gt 3293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0355P)^2^+1.6600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4160 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Be1 Be 0.7220(5) -0.2272(5) 0.2432(3) 0.0146(8) Uani 1 1 d . . . Be2 Be 0.9976(5) 0.0636(5) 0.2654(3) 0.0144(8) Uani 1 1 d . . . P1 P 1.00677(10) -0.17011(10) 0.12265(5) 0.01430(19) Uani 1 1 d . . . P2 P 0.69350(10) 0.03011(10) 0.37137(5) 0.0161(2) Uani 1 1 d . . . P3 P 0.81662(10) 0.40744(9) 0.21275(5) 0.01513(19) Uani 1 1 d . . . P4 P 1.36148(10) -0.17038(10) 0.28266(5) 0.01464(19) Uani 1 1 d . . . O1 O 0.7249(3) -0.1412(3) 0.33631(14) 0.0216(5) Uani 1 1 d . . . O2 O 0.8431(3) -0.1935(3) 0.15251(14) 0.0214(5) Uani 1 1 d . . . O3 O 0.6008(3) 0.0613(3) 0.47538(15) 0.0320(6) Uani 1 1 d . . . O4 O 0.5594(3) 0.1699(3) 0.32459(18) 0.0336(6) Uani 1 1 d . . . H4A H 0.6025 0.2301 0.3001 0.050 Uiso 1 1 calc R . . O5 O 1.1712(3) -0.3370(3) 0.13291(18) 0.0352(6) Uani 1 1 d . . . H5A H 1.2182 -0.3151 0.1676 0.053 Uiso 1 1 calc R . . O6 O 1.0433(3) -0.1484(3) 0.01867(14) 0.0228(5) Uani 1 1 d . . . H6 H 1.0128 -0.0468 0.0058 0.034 Uiso 0.50 1 d PR . . O7 O 0.8580(3) 0.0516(3) 0.35552(14) 0.0210(5) Uani 1 1 d . . . O8 O 0.9967(3) -0.0208(3) 0.17310(14) 0.0218(5) Uani 1 1 d . . . O9 O 0.9438(3) 0.2609(2) 0.25184(15) 0.0191(5) Uani 1 1 d . . . O10 O 0.7953(3) 0.5720(2) 0.25063(15) 0.0196(5) Uani 1 1 d . . . O11 O 0.8897(3) 0.3949(3) 0.10560(15) 0.0310(6) Uani 1 1 d . . . H11A H 0.8985 0.3084 0.0818 0.046 Uiso 1 1 calc R . . O12 O 0.6377(3) 0.4014(3) 0.23391(17) 0.0284(6) Uani 1 1 d . . . H12A H 0.5572 0.4968 0.2340 0.043 Uiso 1 1 calc R . . O13 O 1.1916(3) -0.0158(3) 0.28391(15) 0.0217(5) Uani 1 1 d . . . O14 O 1.5192(3) -0.1445(3) 0.23377(14) 0.0200(5) Uani 1 1 d . . . O15 O 1.3677(3) -0.3291(3) 0.23943(16) 0.0230(5) Uani 1 1 d . . . O16 O 1.3693(3) -0.2142(3) 0.38350(15) 0.0267(5) Uani 1 1 d . . . H16A H 1.3796 -0.1414 0.4100 0.040 Uiso 1 1 calc R . . C1 C 0.3286(4) 0.0491(4) 0.0610(2) 0.0267(8) Uani 1 1 d . . . H1A H 0.3577 -0.0232 0.1097 0.032 Uiso 1 1 calc R . . H1B H 0.2002 0.1158 0.0764 0.032 Uiso 1 1 calc R . . C2 C 0.6082(4) 0.0604(4) 0.0276(2) 0.0263(8) Uani 1 1 d . . . H2A H 0.6637 0.1340 0.0205 0.032 Uiso 1 1 calc R . . H2B H 0.6451 -0.0113 0.0755 0.032 Uiso 1 1 calc R . . C3 C 0.3569(5) 0.2528(5) 0.1529(2) 0.0362(9) Uani 1 1 d . . . H3A H 0.3987 0.1679 0.1937 0.054 Uiso 1 1 calc R . . H3B H 0.2298 0.3172 0.1741 0.054 Uiso 1 1 calc R . . H3C H 0.4089 0.3273 0.1520 0.054 Uiso 1 1 calc R . . C4 C 0.3447(5) 0.3018(4) -0.0055(2) 0.0313(8) Uani 1 1 d . . . H4B H 0.3778 0.2490 -0.0668 0.047 Uiso 1 1 calc R . . H4C H 0.3971 0.3757 -0.0057 0.047 Uiso 1 1 calc R . . H4D H 0.2176 0.3667 0.0158 0.047 Uiso 1 1 calc R . . C5 C 0.0143(5) 0.5201(5) 0.5907(2) 0.0377(9) Uani 1 1 d . . . H5B H 0.0932 0.4047 0.5993 0.045 Uiso 1 1 calc R . . H5C H -0.0179 0.5920 0.6466 0.045 Uiso 1 1 calc R . . C6 C 0.1484(5) 0.4738(5) 0.4242(2) 0.0365(9) Uani 1 1 d . . . H6A H 0.2033 0.5153 0.3723 0.055 Uiso 1 1 calc R . . H6B H 0.2320 0.3567 0.4268 0.055 Uiso 1 1 calc R . . C7 C 0.0112(5) 0.7650(5) 0.5059(3) 0.0384(9) Uani 1 1 d . . . H7A H 0.0763 0.7968 0.4544 0.058 Uiso 1 1 calc R . . H7B H -0.0041 0.8261 0.5617 0.058 Uiso 1 1 calc R . . H7C H -0.1033 0.7920 0.4980 0.058 Uiso 1 1 calc R . . C8 C 0.2873(5) 0.5389(5) 0.5255(3) 0.0373(9) Uani 1 1 d . . . H8A H 0.3533 0.4192 0.5288 0.056 Uiso 1 1 calc R . . H8B H 0.2689 0.6003 0.5819 0.056 Uiso 1 1 calc R . . H8C H 0.3525 0.5723 0.4750 0.056 Uiso 1 1 calc R . . N1 N 0.4094(4) 0.1678(3) 0.05723(18) 0.0214(6) Uani 1 1 d . . . N2 N 0.1120(4) 0.5778(4) 0.51126(19) 0.0287(7) 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 0.018(2) 0.0147(19) 0.0143(19) 0.0030(15) -0.0054(15) -0.0101(16) Be2 0.0119(18) 0.0145(19) 0.019(2) 0.0030(15) -0.0052(15) -0.0074(15) P1 0.0150(4) 0.0144(4) 0.0147(4) -0.0002(3) -0.0036(3) -0.0080(3) P2 0.0161(4) 0.0175(4) 0.0157(4) -0.0022(3) -0.0003(3) -0.0105(3) P3 0.0153(4) 0.0103(4) 0.0197(4) 0.0018(3) -0.0069(3) -0.0049(3) P4 0.0114(4) 0.0143(4) 0.0182(4) 0.0038(3) -0.0056(3) -0.0053(3) O1 0.0308(13) 0.0178(11) 0.0187(11) -0.0001(9) -0.0081(10) -0.0126(10) O2 0.0236(12) 0.0282(12) 0.0190(11) 0.0063(10) -0.0059(9) -0.0176(10) O3 0.0395(15) 0.0463(15) 0.0174(12) -0.0118(11) 0.0091(10) -0.0340(13) O4 0.0219(13) 0.0249(13) 0.0583(17) 0.0141(12) -0.0152(12) -0.0127(11) O5 0.0313(14) 0.0203(13) 0.0500(16) -0.0075(11) -0.0269(12) 0.0000(11) O6 0.0348(13) 0.0264(12) 0.0120(11) 0.0003(9) -0.0013(9) -0.0207(11) O7 0.0216(12) 0.0295(12) 0.0155(11) 0.0019(9) -0.0023(9) -0.0164(10) O8 0.0298(13) 0.0210(12) 0.0177(11) -0.0018(9) -0.0061(9) -0.0144(10) O9 0.0202(11) 0.0120(10) 0.0272(12) 0.0032(9) -0.0120(9) -0.0064(9) O10 0.0233(12) 0.0122(10) 0.0245(12) 0.0018(9) -0.0080(9) -0.0084(9) O11 0.0472(16) 0.0259(13) 0.0202(12) 0.0007(10) -0.0073(11) -0.0182(12) O12 0.0167(12) 0.0125(11) 0.0563(16) 0.0073(11) -0.0139(11) -0.0052(9) O13 0.0124(11) 0.0192(11) 0.0315(13) 0.0025(10) -0.0082(9) -0.0045(9) O14 0.0138(11) 0.0230(12) 0.0224(12) 0.0074(9) -0.0055(9) -0.0079(9) O15 0.0187(11) 0.0169(11) 0.0349(13) -0.0006(10) -0.0131(10) -0.0066(9) O16 0.0351(14) 0.0361(14) 0.0197(12) 0.0104(10) -0.0118(10) -0.0236(12) C1 0.0176(16) 0.0313(19) 0.0284(19) 0.0052(15) -0.0026(14) -0.0110(15) C2 0.0205(17) 0.0283(19) 0.036(2) 0.0079(16) -0.0133(15) -0.0140(15) C3 0.050(2) 0.030(2) 0.0235(19) -0.0015(16) -0.0110(17) -0.0142(18) C4 0.042(2) 0.0195(18) 0.030(2) 0.0099(15) -0.0153(17) -0.0102(16) C5 0.047(2) 0.057(3) 0.0189(18) 0.0015(17) -0.0064(17) -0.033(2) C6 0.040(2) 0.048(2) 0.0239(19) -0.0051(17) -0.0019(16) -0.026(2) C7 0.032(2) 0.042(2) 0.043(2) 0.0047(19) -0.0155(18) -0.0163(18) C8 0.037(2) 0.037(2) 0.040(2) 0.0078(18) -0.0120(18) -0.0187(18) N1 0.0237(14) 0.0197(14) 0.0214(14) 0.0047(11) -0.0100(11) -0.0087(12) N2 0.0365(17) 0.0368(17) 0.0218(15) 0.0018(13) -0.0068(13) -0.0251(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Be1 O10 1.611(4) 1_545 ? Be1 O2 1.620(4) . ? Be1 O1 1.629(4) . ? Be1 O14 1.633(4) 1_455 ? Be2 O8 1.602(4) . ? Be2 O13 1.617(4) . ? Be2 O9 1.619(4) . ? Be2 O7 1.622(4) . ? P1 O2 1.502(2) . ? P1 O8 1.504(2) . ? P1 O6 1.546(2) . ? P1 O5 1.568(2) . ? P2 O7 1.503(2) . ? P2 O1 1.503(2) . ? P2 O3 1.539(2) . ? P2 O4 1.573(2) . ? P3 O10 1.497(2) . ? P3 O9 1.504(2) . ? P3 O12 1.549(2) . ? P3 O11 1.567(2) . ? P4 O13 1.494(2) . ? P4 O14 1.511(2) . ? P4 O15 1.543(2) . ? P4 O16 1.573(2) . ? O4 H4A 0.8200 . ? O5 H5A 0.8200 . ? O6 H6 0.8500 . ? O10 Be1 1.611(4) 1_565 ? O11 H11A 0.8200 . ? O12 H12A 0.8200 . ? O14 Be1 1.633(4) 1_655 ? O16 H16A 0.8200 . ? C1 C2 1.497(5) 2_655 ? C1 N1 1.512(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C1 1.497(5) 2_655 ? C2 N1 1.505(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.505(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 N1 1.497(4) . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4 H4D 0.9600 . ? C5 C6 1.480(5) 2_566 ? C5 N2 1.512(4) . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 C5 1.480(5) 2_566 ? C6 N2 1.502(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.499(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N2 1.489(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? 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 O10 Be1 O2 110.6(3) 1_545 . ? O10 Be1 O1 108.1(2) 1_545 . ? O2 Be1 O1 110.8(2) . . ? O10 Be1 O14 109.4(2) 1_545 1_455 ? O2 Be1 O14 107.9(2) . 1_455 ? O1 Be1 O14 110.1(2) . 1_455 ? O8 Be2 O13 113.7(3) . . ? O8 Be2 O9 107.1(2) . . ? O13 Be2 O9 105.3(2) . . ? O8 Be2 O7 112.0(2) . . ? O13 Be2 O7 108.8(2) . . ? O9 Be2 O7 109.8(2) . . ? O2 P1 O8 114.84(13) . . ? O2 P1 O6 108.72(12) . . ? O8 P1 O6 108.31(12) . . ? O2 P1 O5 109.10(13) . . ? O8 P1 O5 109.61(13) . . ? O6 P1 O5 105.88(14) . . ? O7 P2 O1 114.94(13) . . ? O7 P2 O3 109.05(13) . . ? O1 P2 O3 108.11(13) . . ? O7 P2 O4 109.21(12) . . ? O1 P2 O4 108.49(13) . . ? O3 P2 O4 106.72(15) . . ? O10 P3 O9 110.36(12) . . ? O10 P3 O12 112.36(13) . . ? O9 P3 O12 108.69(12) . . ? O10 P3 O11 106.31(12) . . ? O9 P3 O11 110.96(13) . . ? O12 P3 O11 108.14(14) . . ? O13 P4 O14 110.53(12) . . ? O13 P4 O15 110.64(12) . . ? O14 P4 O15 112.06(13) . . ? O13 P4 O16 110.62(13) . . ? O14 P4 O16 110.14(12) . . ? O15 P4 O16 102.62(12) . . ? P2 O1 Be1 137.1(2) . . ? P1 O2 Be1 140.4(2) . . ? P2 O4 H4A 109.5 . . ? P1 O5 H5A 109.5 . . ? P1 O6 H6 115.1 . . ? P2 O7 Be2 134.74(19) . . ? P1 O8 Be2 148.9(2) . . ? P3 O9 Be2 139.67(19) . . ? P3 O10 Be1 146.9(2) . 1_565 ? P3 O11 H11A 109.5 . . ? P3 O12 H12A 109.5 . . ? P4 O13 Be2 147.9(2) . . ? P4 O14 Be1 131.95(19) . 1_655 ? P4 O16 H16A 109.5 . . ? C2 C1 N1 113.1(3) 2_655 . ? C2 C1 H1A 109.0 2_655 . ? N1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 2_655 . ? N1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C1 C2 N1 112.5(3) 2_655 . ? C1 C2 H2A 109.1 2_655 . ? N1 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 2_655 . ? N1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C4 H4D 109.5 . . ? H4B C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? C6 C5 N2 112.6(3) 2_566 . ? C6 C5 H5B 109.1 2_566 . ? N2 C5 H5B 109.1 . . ? C6 C5 H5C 109.1 2_566 . ? N2 C5 H5C 109.1 . . ? H5B C5 H5C 107.8 . . ? C5 C6 N2 112.8(3) 2_566 . ? C5 C6 H6A 109.0 2_566 . ? N2 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 2_566 . ? N2 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 N1 C2 112.4(3) . . ? C4 N1 C3 108.8(3) . . ? C2 N1 C3 108.4(3) . . ? C4 N1 C1 111.6(3) . . ? C2 N1 C1 107.2(2) . . ? C3 N1 C1 108.3(3) . . ? C8 N2 C7 108.7(3) . . ? C8 N2 C6 107.2(3) . . ? C7 N2 C6 112.5(3) . . ? C8 N2 C5 108.2(3) . . ? C7 N2 C5 111.7(3) . . ? C6 N2 C5 108.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 P2 O1 Be1 -94.4(3) . . . . ? O3 P2 O1 Be1 143.5(3) . . . . ? O4 P2 O1 Be1 28.1(3) . . . . ? O10 Be1 O1 P2 172.8(2) 1_545 . . . ? O2 Be1 O1 P2 51.5(4) . . . . ? O14 Be1 O1 P2 -67.7(4) 1_455 . . . ? O8 P1 O2 Be1 -60.5(3) . . . . ? O6 P1 O2 Be1 178.0(3) . . . . ? O5 P1 O2 Be1 63.0(3) . . . . ? O10 Be1 O2 P1 -88.6(3) 1_545 . . . ? O1 Be1 O2 P1 31.3(4) . . . . ? O14 Be1 O2 P1 151.8(2) 1_455 . . . ? O1 P2 O7 Be2 68.8(3) . . . . ? O3 P2 O7 Be2 -169.6(3) . . . . ? O4 P2 O7 Be2 -53.3(3) . . . . ? O8 Be2 O7 P2 -22.4(4) . . . . ? O13 Be2 O7 P2 -148.9(2) . . . . ? O9 Be2 O7 P2 96.4(3) . . . . ? O2 P1 O8 Be2 73.4(4) . . . . ? O6 P1 O8 Be2 -164.9(4) . . . . ? O5 P1 O8 Be2 -49.8(4) . . . . ? O13 Be2 O8 P1 73.4(5) . . . . ? O9 Be2 O8 P1 -170.8(3) . . . . ? O7 Be2 O8 P1 -50.4(5) . . . . ? O10 P3 O9 Be2 161.0(3) . . . . ? O12 P3 O9 Be2 37.4(3) . . . . ? O11 P3 O9 Be2 -81.4(3) . . . . ? O8 Be2 O9 P3 40.5(4) . . . . ? O13 Be2 O9 P3 161.8(2) . . . . ? O7 Be2 O9 P3 -81.3(4) . . . . ? O9 P3 O10 Be1 167.8(4) . . . 1_565 ? O12 P3 O10 Be1 -70.8(4) . . . 1_565 ? O11 P3 O10 Be1 47.3(4) . . . 1_565 ? O14 P4 O13 Be2 130.8(4) . . . . ? O15 P4 O13 Be2 6.1(4) . . . . ? O16 P4 O13 Be2 -107.0(4) . . . . ? O8 Be2 O13 P4 -41.4(5) . . . . ? O9 Be2 O13 P4 -158.3(3) . . . . ? O7 Be2 O13 P4 84.1(4) . . . . ? O13 P4 O14 Be1 153.4(2) . . . 1_655 ? O15 P4 O14 Be1 -82.7(3) . . . 1_655 ? O16 P4 O14 Be1 30.8(3) . . . 1_655 ? C1 C2 N1 C4 -68.0(3) 2_655 . . . ? C1 C2 N1 C3 171.7(3) 2_655 . . . ? C1 C2 N1 C1 54.9(4) 2_655 . . . ? C2 C1 N1 C4 68.1(3) 2_655 . . . ? C2 C1 N1 C2 -55.3(4) 2_655 . . . ? C2 C1 N1 C3 -172.2(3) 2_655 . . . ? C5 C6 N2 C8 171.2(3) 2_566 . . . ? C5 C6 N2 C7 -69.4(4) 2_566 . . . ? C5 C6 N2 C5 54.6(5) 2_566 . . . ? C6 C5 N2 C8 -170.4(3) 2_566 . . . ? C6 C5 N2 C7 70.0(4) 2_566 . . . ? C6 C5 N2 C6 -54.5(5) 2_566 . . . ? 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 O4 H4A O12 0.82 1.90 2.696(3) 163.0 . O5 H5A O15 0.82 1.87 2.665(3) 164.2 . O11 H11A O6 0.82 1.91 2.671(3) 154.8 2_755 O12 H12A O15 0.82 1.66 2.470(3) 168.2 1_465 O16 H16A O3 0.82 1.96 2.685(3) 146.5 2_756 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.748 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.077 _database_code_depnum_ccdc_archive 'CCDC 973430' data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H28 Be4 N2 O24 P6' _chemical_formula_weight 758.18 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.3591(6) _cell_length_b 9.3128(5) _cell_length_c 15.1655(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.505(5) _cell_angle_gamma 90.00 _cell_volume 1320.55(11) _cell_formula_units_Z 2 _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 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8691 _exptl_absorpt_correction_T_max 0.9221 _exptl_absorpt_process_details '(SADABS; Sheldrick, G. M., 1996)' _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 12711 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 26.49 _reflns_number_total 2729 _reflns_number_gt 2379 _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^)+(0.0495P)^2^+2.0948P] 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 2729 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Be1 Be 0.9164(4) -0.0944(4) 0.6170(2) 0.0166(7) Uani 1 1 d . . . Be2 Be 0.3328(4) -0.0027(4) 0.6794(2) 0.0139(7) Uani 1 1 d . . . P1 P 0.63697(7) 0.02548(8) 0.63834(5) 0.01658(19) Uani 1 1 d . . . P2 P 0.10889(7) 0.13904(8) 0.57606(4) 0.01335(18) Uani 1 1 d . . . P3 P 0.34847(7) 0.23926(7) 0.81425(4) 0.01244(18) Uani 1 1 d . . . O1 O 0.7542(2) -0.0837(2) 0.64881(13) 0.0211(5) Uani 1 1 d . . . O2 O 0.6376(3) 0.0951(2) 0.54475(14) 0.0304(5) Uani 1 1 d . . . H2A H 0.6729 0.0389 0.5102 0.046 Uiso 1 1 calc R . . O3 O 0.6696(2) 0.1571(3) 0.69931(15) 0.0328(6) Uani 1 1 d . . . H3A H 0.5986 0.1764 0.7269 0.049 Uiso 1 1 calc R . . O4 O 0.4950(2) -0.0389(2) 0.65536(15) 0.0247(5) Uani 1 1 d . . . O5 O 0.2517(2) 0.0592(2) 0.58865(13) 0.0201(5) Uani 1 1 d . . . O6 O 0.0755(2) 0.1698(2) 0.47894(13) 0.0227(5) Uani 1 1 d . . . O7 O -0.0100(2) 0.0611(2) 0.61964(14) 0.0229(5) Uani 1 1 d . . . O8 O 0.1245(2) 0.2934(2) 0.61699(14) 0.0264(5) Uani 1 1 d . . . H8A H 0.1609 0.2876 0.6670 0.040 Uiso 1 1 calc R . . O9 O 0.3275(2) 0.1079(2) 0.75895(15) 0.0262(5) Uani 1 1 d . . . O10 O 0.2381(2) 0.3500(2) 0.78547(14) 0.0213(5) Uani 1 1 d . . . O11 O 0.3210(2) 0.1976(3) 0.91281(14) 0.0305(5) Uani 1 1 d . . . H11A H 0.3867 0.2280 0.9452 0.046 Uiso 1 1 calc R . . O12 O 0.5016(2) 0.2945(2) 0.81194(13) 0.0199(4) Uani 1 1 d . . . C1 C 1.0429(4) -0.0799(4) 0.9257(2) 0.0369(9) Uani 1 1 d . . . H1A H 1.1365 -0.0405 0.9152 0.044 Uiso 1 1 calc R . . H1B H 1.0239 -0.1555 0.8828 0.044 Uiso 1 1 calc R . . C2 C 0.9546(5) 0.1439(4) 0.9834(2) 0.0383(9) Uani 1 1 d . . . H2B H 0.8783 0.2143 0.9783 0.046 Uiso 1 1 calc R . . H2C H 1.0442 0.1937 0.9755 0.046 Uiso 1 1 calc R . . C3 C 0.7814(5) -0.0214(6) 0.9094(4) 0.0692(15) Uani 1 1 d . . . H3B H 0.7634 -0.0670 0.9646 0.104 Uiso 1 1 calc R . . H3C H 0.7692 -0.0900 0.8624 0.104 Uiso 1 1 calc R . . H3D H 0.7155 0.0565 0.8996 0.104 Uiso 1 1 calc R . . C4 C 0.9528(4) 0.1053(4) 0.8243(2) 0.0382(9) Uani 1 1 d . . . H4A H 1.0481 0.1429 0.8225 0.057 Uiso 1 1 calc R . . H4B H 0.8851 0.1821 0.8160 0.057 Uiso 1 1 calc R . . H4C H 0.9377 0.0355 0.7782 0.057 Uiso 1 1 calc R . . N1 N 0.9331(3) 0.0358(3) 0.91190(18) 0.0303(6) 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 0.0101(16) 0.0230(19) 0.0165(17) 0.0031(14) -0.0005(13) 0.0023(14) Be2 0.0102(16) 0.0143(17) 0.0171(17) -0.0006(13) -0.0009(13) -0.0004(13) P1 0.0109(4) 0.0218(4) 0.0172(4) 0.0006(3) 0.0020(3) 0.0023(3) P2 0.0131(3) 0.0151(4) 0.0118(3) 0.0009(3) -0.0008(3) 0.0004(3) P3 0.0111(3) 0.0132(4) 0.0130(3) -0.0024(3) 0.0002(2) 0.0001(3) O1 0.0116(10) 0.0267(11) 0.0253(11) 0.0050(9) 0.0044(8) 0.0027(8) O2 0.0407(14) 0.0299(13) 0.0213(11) 0.0053(9) 0.0068(10) 0.0131(11) O3 0.0228(12) 0.0386(14) 0.0377(14) -0.0155(11) 0.0099(10) -0.0025(10) O4 0.0090(10) 0.0301(12) 0.0353(13) 0.0000(10) 0.0033(9) 0.0022(9) O5 0.0143(10) 0.0284(11) 0.0175(10) 0.0041(8) -0.0008(8) 0.0043(8) O6 0.0279(12) 0.0271(12) 0.0128(10) 0.0013(8) -0.0010(8) 0.0067(9) O7 0.0175(10) 0.0259(12) 0.0258(11) 0.0009(9) 0.0057(8) -0.0032(9) O8 0.0398(13) 0.0163(11) 0.0223(11) -0.0024(9) -0.0080(9) 0.0000(10) O9 0.0274(12) 0.0204(11) 0.0303(12) -0.0109(9) -0.0045(9) 0.0020(9) O10 0.0195(10) 0.0185(11) 0.0255(11) -0.0033(9) -0.0030(8) 0.0064(8) O11 0.0346(13) 0.0406(14) 0.0165(11) 0.0056(10) 0.0033(9) -0.0075(11) O12 0.0132(10) 0.0297(12) 0.0169(10) -0.0071(9) 0.0004(8) -0.0039(9) C1 0.052(2) 0.034(2) 0.0244(17) -0.0101(15) -0.0009(15) 0.0121(17) C2 0.058(2) 0.0244(18) 0.0322(19) -0.0043(15) -0.0053(17) 0.0070(17) C3 0.065(3) 0.083(4) 0.059(3) 0.019(3) -0.002(2) -0.018(3) C4 0.040(2) 0.048(2) 0.0263(18) 0.0073(16) -0.0030(15) -0.0049(18) N1 0.0374(16) 0.0296(15) 0.0238(14) -0.0012(12) -0.0007(12) -0.0007(13) _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 Be1 O7 1.604(4) 1_655 ? Be1 O1 1.615(4) . ? Be1 O6 1.620(4) 3_656 ? Be1 O12 1.658(4) 2_646 ? Be2 O9 1.589(4) . ? Be2 O4 1.612(4) . ? Be2 O10 1.625(4) 2_546 ? Be2 O5 1.646(4) . ? P1 O4 1.491(2) . ? P1 O1 1.499(2) . ? P1 O3 1.557(2) . ? P1 O2 1.561(2) . ? P2 O7 1.505(2) . ? P2 O6 1.519(2) . ? P2 O5 1.534(2) . ? P2 O8 1.570(2) . ? P3 O9 1.491(2) . ? P3 O10 1.510(2) . ? P3 O12 1.525(2) . ? P3 O11 1.576(2) . ? O2 H2A 0.8200 . ? O3 H3A 0.8200 . ? O6 Be1 1.620(4) 3_656 ? O7 Be1 1.604(4) 1_455 ? O8 H8A 0.8200 . ? O10 Be2 1.625(4) 2_556 ? O11 H11A 0.8200 . ? O12 Be1 1.658(4) 2_656 ? C1 N1 1.497(4) . ? C1 C2 1.501(5) 3_757 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N1 1.487(4) . ? C2 C1 1.501(5) 3_757 ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 N1 1.515(5) . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C4 N1 1.497(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? 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 O7 Be1 O1 110.2(2) 1_655 . ? O7 Be1 O6 112.1(2) 1_655 3_656 ? O1 Be1 O6 112.1(2) . 3_656 ? O7 Be1 O12 111.2(2) 1_655 2_646 ? O1 Be1 O12 105.0(2) . 2_646 ? O6 Be1 O12 105.9(2) 3_656 2_646 ? O9 Be2 O4 111.6(2) . . ? O9 Be2 O10 105.7(2) . 2_546 ? O4 Be2 O10 107.4(2) . 2_546 ? O9 Be2 O5 112.3(2) . . ? O4 Be2 O5 106.8(2) . . ? O10 Be2 O5 113.0(2) 2_546 . ? O4 P1 O1 111.29(12) . . ? O4 P1 O3 111.52(13) . . ? O1 P1 O3 110.30(13) . . ? O4 P1 O2 111.32(13) . . ? O1 P1 O2 110.24(12) . . ? O3 P1 O2 101.80(14) . . ? O7 P2 O6 113.06(12) . . ? O7 P2 O5 111.63(12) . . ? O6 P2 O5 110.69(11) . . ? O7 P2 O8 108.98(12) . . ? O6 P2 O8 102.86(12) . . ? O5 P2 O8 109.21(12) . . ? O9 P3 O10 109.01(12) . . ? O9 P3 O12 111.40(12) . . ? O10 P3 O12 113.25(12) . . ? O9 P3 O11 107.95(13) . . ? O10 P3 O11 107.74(12) . . ? O12 P3 O11 107.29(12) . . ? P1 O1 Be1 134.7(2) . . ? P1 O2 H2A 109.5 . . ? P1 O3 H3A 109.5 . . ? P1 O4 Be2 144.1(2) . . ? P2 O5 Be2 129.87(18) . . ? P2 O6 Be1 140.63(19) . 3_656 ? P2 O7 Be1 138.5(2) . 1_455 ? P2 O8 H8A 109.5 . . ? P3 O9 Be2 162.0(2) . . ? P3 O10 Be2 139.98(19) . 2_556 ? P3 O11 H11A 109.5 . . ? P3 O12 Be1 127.19(18) . 2_656 ? N1 C1 C2 113.4(3) . 3_757 ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 3_757 . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 3_757 . ? H1A C1 H1B 107.7 . . ? N1 C2 C1 113.4(3) . 3_757 ? N1 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 3_757 . ? N1 C2 H2C 108.9 . . ? C1 C2 H2C 108.9 3_757 . ? H2B C2 H2C 107.7 . . ? N1 C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 N1 C4 109.7(3) . . ? C2 N1 C1 108.4(3) . . ? C4 N1 C1 109.0(3) . . ? C2 N1 C3 110.7(3) . . ? C4 N1 C3 106.3(3) . . ? C1 N1 C3 112.8(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2A O5 0.82 1.92 2.723(3) 167.5 3_656 O3 H3A O12 0.82 1.95 2.695(3) 150.7 . O8 H8A O10 0.82 1.99 2.775(3) 159.1 . O11 H11A O6 0.82 2.05 2.827(3) 157.6 4_666 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.877 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 973431'