# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 912293' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Be4 O12' _chemical_formula_weight 432.30 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 23.8931(2) _cell_length_b 23.8931(2) _cell_length_c 15.9482(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9104.5(2) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2945 _cell_measurement_theta_min 2.8189 _cell_measurement_theta_max 29.2436 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99466 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Eos' _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 9022 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4004 _reflns_number_gt 2965 _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. REM The guest molecules are highly dirordered in the structure. # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.250 0.032 572 68 ' ' 2 0.000 0.750 -0.038 572 68 ' ' 3 0.500 0.250 0.104 572 68 ' ' 4 0.500 0.750 -0.139 572 68 ' ' _platon_squeeze_details ; _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^)+(0.0770P)^2^+4.8145P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4004 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.29976(13) 0.10607(13) 0.55869(19) 0.0227(7) Uani 1 1 d . . . Be2 Be 0.16813(13) -0.02631(12) 0.75517(18) 0.0210(7) Uani 1 1 d . . . Be3 Be 0.22234(13) 0.05556(12) 0.66415(19) 0.0211(7) Uani 1 1 d . . . Be4 Be 0.34596(13) 0.09272(13) 0.39863(18) 0.0233(7) Uani 1 1 d . . . O1 O 0.21581(7) 0.12102(7) 0.69545(10) 0.0293(4) Uani 1 1 d . . . O2 O 0.26547(7) 0.16034(7) 0.59323(10) 0.0285(4) Uani 1 1 d . . . O3 O 0.20258(7) 0.41527(7) 0.64224(10) 0.0286(4) Uani 1 1 d . . . O4 O 0.25056(7) 0.36478(7) 0.54893(10) 0.0287(4) Uani 1 1 d . . . O5 O 0.36628(7) 0.11024(8) 0.58259(10) 0.0310(4) Uani 1 1 d . . . O6 O 0.40301(7) 0.09710(8) 0.45599(10) 0.0316(4) Uani 1 1 d . . . O7 O 0.65961(7) 0.07324(8) 0.53415(10) 0.0303(4) Uani 1 1 d . . . O8 O 0.60855(7) 0.09879(8) 0.42404(10) 0.0315(4) Uani 1 1 d . . . O9 O 0.29237(7) 0.10640(7) 0.45753(10) 0.0283(4) Uani 1 1 d . . . H1 H 0.2578 0.1143 0.4336 0.034 Uiso 1 1 calc R . . O10 O 0.27631(6) 0.05052(6) 0.60469(10) 0.0229(4) Uani 1 1 d . . . H2 H 0.2938 0.0162 0.5968 0.027 Uiso 1 1 calc R . . O11 O 0.22062(7) 0.01166(7) 0.73683(10) 0.0248(4) Uani 1 1 d . . . H3 H 0.2520 0.0078 0.7708 0.030 Uiso 1 1 calc R . . O12 O 0.15576(7) -0.03381(7) 0.85257(9) 0.0267(4) Uani 1 1 d . . . H4 H 0.1492 -0.0019 0.8844 0.032 Uiso 1 1 calc R . . C1 C 0.23097(10) 0.16250(10) 0.65334(14) 0.0229(5) Uani 1 1 d . . . C2 C 0.22009(10) 0.36955(10) 0.61319(14) 0.0218(5) Uani 1 1 d . . . C3 C 0.20601(10) 0.21773(10) 0.67477(14) 0.0249(5) Uani 1 1 d . . . C4 C 0.22445(10) 0.26607(10) 0.63519(14) 0.0239(5) Uani 1 1 d . . . H5 H 0.2521 0.2639 0.5943 0.029 Uiso 1 1 calc R . . C5 C 0.20182(10) 0.31746(10) 0.65633(14) 0.0248(5) Uani 1 1 d . . . C6 C 0.16051(12) 0.32041(11) 0.71693(17) 0.0394(7) Uani 1 1 d . . . H6 H 0.1454 0.3549 0.7316 0.047 Uiso 1 1 calc R . . C7 C 0.14162(14) 0.27235(12) 0.7557(2) 0.0535(9) Uani 1 1 d . . . H7 H 0.1137 0.2745 0.7963 0.064 Uiso 1 1 calc R . . C8 C 0.16422(13) 0.22103(11) 0.73419(18) 0.0421(7) Uani 1 1 d . . . H8 H 0.1512 0.1886 0.7599 0.051 Uiso 1 1 calc R . . C9 C 0.40729(10) 0.10348(10) 0.53376(14) 0.0229(5) Uani 1 1 d . . . C10 C 0.61439(10) 0.08770(10) 0.50060(14) 0.0235(5) Uani 1 1 d . . . C11 C 0.46420(10) 0.10202(11) 0.57139(15) 0.0282(6) Uani 1 1 d . . . C12 C 0.51107(10) 0.09575(11) 0.52039(15) 0.0277(6) Uani 1 1 d . . . H9 H 0.5068 0.0934 0.4625 0.033 Uiso 1 1 calc R . . C13 C 0.56403(10) 0.09294(11) 0.55524(15) 0.0278(6) Uani 1 1 d . . . C14 C 0.57026(11) 0.09698(13) 0.64192(16) 0.0384(7) Uani 1 1 d . . . H10 H 0.6057 0.0946 0.6657 0.046 Uiso 1 1 calc R . . C15 C 0.52427(12) 0.10446(15) 0.69223(16) 0.0486(9) Uani 1 1 d . . . H11 H 0.5286 0.1082 0.7499 0.058 Uiso 1 1 calc R . . C16 C 0.47149(11) 0.10645(14) 0.65707(16) 0.0417(8) Uani 1 1 d . . . H12 H 0.4404 0.1108 0.6916 0.050 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 0.0211(16) 0.0225(16) 0.0244(16) -0.0024(13) 0.0024(13) 0.0000(13) Be2 0.0224(16) 0.0184(15) 0.0223(15) 0.0028(12) -0.0016(12) -0.0002(12) Be3 0.0213(15) 0.0175(15) 0.0245(15) 0.0012(12) 0.0016(13) 0.0001(12) Be4 0.0269(17) 0.0232(16) 0.0199(15) -0.0009(12) -0.0003(13) -0.0044(14) O1 0.0377(10) 0.0187(9) 0.0314(9) 0.0017(7) 0.0127(8) 0.0005(8) O2 0.0334(10) 0.0216(9) 0.0304(9) 0.0005(7) 0.0139(8) 0.0002(8) O3 0.0409(11) 0.0163(9) 0.0286(9) -0.0003(7) 0.0102(8) 0.0035(8) O4 0.0351(10) 0.0218(9) 0.0291(9) 0.0020(7) 0.0115(8) 0.0028(8) O5 0.0201(9) 0.0491(11) 0.0239(9) -0.0056(8) 0.0028(7) -0.0033(8) O6 0.0215(9) 0.0510(12) 0.0223(9) -0.0073(8) 0.0021(7) -0.0011(8) O7 0.0194(9) 0.0465(11) 0.0250(9) 0.0066(8) -0.0024(7) 0.0049(8) O8 0.0225(9) 0.0505(12) 0.0216(9) 0.0010(8) -0.0011(7) 0.0075(8) O9 0.0220(9) 0.0390(10) 0.0238(9) -0.0023(8) -0.0001(7) 0.0047(8) O10 0.0210(9) 0.0171(8) 0.0305(9) -0.0016(7) 0.0035(7) 0.0019(7) O11 0.0213(9) 0.0242(9) 0.0290(9) 0.0086(7) -0.0079(7) -0.0035(7) O12 0.0371(10) 0.0205(9) 0.0225(9) 0.0003(7) 0.0026(7) 0.0027(8) C1 0.0252(13) 0.0204(12) 0.0230(12) 0.0016(10) 0.0004(10) -0.0027(10) C2 0.0241(12) 0.0200(12) 0.0215(12) 0.0019(10) 0.0002(10) 0.0020(10) C3 0.0309(13) 0.0179(12) 0.0259(12) 0.0007(10) 0.0048(11) 0.0008(11) C4 0.0272(13) 0.0205(12) 0.0241(12) -0.0002(10) 0.0064(10) 0.0018(11) C5 0.0294(13) 0.0190(12) 0.0260(13) 0.0009(10) 0.0029(11) 0.0013(10) C6 0.0480(18) 0.0219(14) 0.0481(17) 0.0019(12) 0.0241(14) 0.0088(13) C7 0.064(2) 0.0298(16) 0.067(2) 0.0067(15) 0.0472(18) 0.0092(15) C8 0.0514(18) 0.0241(14) 0.0509(17) 0.0052(13) 0.0283(15) -0.0002(13) C9 0.0217(12) 0.0244(13) 0.0225(12) -0.0005(10) 0.0034(10) -0.0018(10) C10 0.0197(12) 0.0292(13) 0.0217(12) -0.0013(10) -0.0022(10) 0.0022(10) C11 0.0224(13) 0.0378(15) 0.0244(12) -0.0026(11) 0.0012(10) -0.0008(11) C12 0.0228(13) 0.0402(15) 0.0202(12) -0.0015(11) 0.0003(10) 0.0003(11) C13 0.0236(13) 0.0360(14) 0.0239(12) 0.0017(11) -0.0003(10) 0.0021(11) C14 0.0256(14) 0.0616(19) 0.0279(14) 0.0001(13) -0.0060(11) 0.0061(14) C15 0.0341(16) 0.092(3) 0.0200(13) -0.0012(15) -0.0019(12) 0.0069(17) C16 0.0254(14) 0.074(2) 0.0254(14) 0.0019(14) 0.0072(11) 0.0054(14) _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 1.617(3) . ? Be1 O9 1.623(3) . ? Be1 O2 1.630(3) . ? Be1 O5 1.637(3) . ? Be2 O11 1.575(3) . ? Be2 O12 1.591(3) . ? Be2 O4 1.658(3) 15_556 ? Be2 O7 1.667(3) 12_657 ? Be3 O11 1.564(3) . ? Be3 O10 1.605(3) . ? Be3 O3 1.645(3) 15_556 ? Be3 O1 1.649(3) . ? Be4 O12 1.588(3) 2_554 ? Be4 O9 1.621(3) . ? Be4 O8 1.644(3) 11_666 ? Be4 O6 1.645(3) . ? O1 C1 1.251(3) . ? O2 C1 1.265(3) . ? O3 C2 1.258(3) . ? O3 Be3 1.645(3) 12_667 ? O4 C2 1.262(3) . ? O4 Be2 1.658(3) 12_667 ? O5 C9 1.262(3) . ? O6 C9 1.254(3) . ? O7 C10 1.254(3) . ? O7 Be2 1.667(3) 15_656 ? O8 C10 1.257(3) . ? O8 Be4 1.644(3) 16_656 ? O9 H1 0.9300 . ? O10 H2 0.9300 . ? O11 H3 0.9300 . ? O12 Be4 1.588(3) 2 ? O12 H4 0.9300 . ? C1 C3 1.488(3) . ? C2 C5 1.487(3) . ? C3 C8 1.379(4) . ? C3 C4 1.388(3) . ? C4 C5 1.383(3) . ? C4 H5 0.9300 . ? C5 C6 1.383(3) . ? C6 C7 1.380(4) . ? C6 H6 0.9300 . ? C7 C8 1.383(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C11 1.487(3) . ? C10 C13 1.491(3) . ? C11 C16 1.382(3) . ? C11 C12 1.392(3) . ? C12 C13 1.384(3) . ? C12 H9 0.9300 . ? C13 C14 1.394(3) . ? C14 C15 1.372(4) . ? C14 H10 0.9300 . ? C15 C16 1.381(4) . ? C15 H11 0.9300 . ? C16 H12 0.9300 . ? 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 O9 114.7(2) . . ? O10 Be1 O2 109.00(19) . . ? O9 Be1 O2 106.11(19) . . ? O10 Be1 O5 106.3(2) . . ? O9 Be1 O5 109.68(19) . . ? O2 Be1 O5 111.2(2) . . ? O11 Be2 O12 113.2(2) . . ? O11 Be2 O4 107.56(18) . 15_556 ? O12 Be2 O4 114.0(2) . 15_556 ? O11 Be2 O7 111.12(19) . 12_657 ? O12 Be2 O7 106.67(18) . 12_657 ? O4 Be2 O7 103.90(18) 15_556 12_657 ? O11 Be3 O10 114.1(2) . . ? O11 Be3 O3 107.70(19) . 15_556 ? O10 Be3 O3 109.51(19) . 15_556 ? O11 Be3 O1 114.2(2) . . ? O10 Be3 O1 109.03(19) . . ? O3 Be3 O1 101.50(18) 15_556 . ? O12 Be4 O9 115.2(2) 2_554 . ? O12 Be4 O8 107.62(18) 2_554 11_666 ? O9 Be4 O8 107.3(2) . 11_666 ? O12 Be4 O6 109.6(2) 2_554 . ? O9 Be4 O6 108.62(18) . . ? O8 Be4 O6 108.2(2) 11_666 . ? C1 O1 Be3 124.16(18) . . ? C1 O2 Be1 128.03(19) . . ? C2 O3 Be3 123.90(18) . 12_667 ? C2 O4 Be2 124.56(19) . 12_667 ? C9 O5 Be1 127.02(19) . . ? C9 O6 Be4 128.71(19) . . ? C10 O7 Be2 126.61(18) . 15_656 ? C10 O8 Be4 126.68(19) . 16_656 ? Be4 O9 Be1 119.27(18) . . ? Be4 O9 H1 120.4 . . ? Be1 O9 H1 120.4 . . ? Be3 O10 Be1 119.00(18) . . ? Be3 O10 H2 120.5 . . ? Be1 O10 H2 120.5 . . ? Be3 O11 Be2 123.02(18) . . ? Be3 O11 H3 118.5 . . ? Be2 O11 H3 118.5 . . ? Be4 O12 Be2 123.78(18) 2 . ? Be4 O12 H4 118.1 2 . ? Be2 O12 H4 118.1 . . ? O1 C1 O2 124.3(2) . . ? O1 C1 C3 117.6(2) . . ? O2 C1 C3 118.1(2) . . ? O3 C2 O4 124.7(2) . . ? O3 C2 C5 117.3(2) . . ? O4 C2 C5 118.0(2) . . ? C8 C3 C4 119.7(2) . . ? C8 C3 C1 119.9(2) . . ? C4 C3 C1 120.4(2) . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H5 119.9 . . ? C3 C4 H5 119.9 . . ? C6 C5 C4 119.6(2) . . ? C6 C5 C2 119.3(2) . . ? C4 C5 C2 121.0(2) . . ? C7 C6 C5 120.3(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 119.9(2) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C3 C8 C7 120.3(2) . . ? C3 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? O6 C9 O5 124.2(2) . . ? O6 C9 C11 118.1(2) . . ? O5 C9 C11 117.6(2) . . ? O7 C10 O8 124.6(2) . . ? O7 C10 C13 118.0(2) . . ? O8 C10 C13 117.4(2) . . ? C16 C11 C12 119.0(2) . . ? C16 C11 C9 120.8(2) . . ? C12 C11 C9 120.2(2) . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H9 119.8 . . ? C11 C12 H9 119.8 . . ? C12 C13 C14 119.5(2) . . ? C12 C13 C10 120.5(2) . . ? C14 C13 C10 120.0(2) . . ? C15 C14 C13 120.2(2) . . ? C15 C14 H10 119.9 . . ? C13 C14 H10 119.9 . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H11 120.1 . . ? C16 C15 H11 120.1 . . ? C15 C16 C11 120.9(2) . . ? C15 C16 H12 119.5 . . ? C11 C16 H12 119.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.345 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.059 data_2 _database_code_depnum_ccdc_archive 'CCDC 912294' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H6 Be4 O12' _chemical_formula_weight 354.19 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cccm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z-1/2' '-x, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z-1/2' _cell_length_a 10.3705(4) _cell_length_b 11.2422(6) _cell_length_c 18.4030(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2145.55(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1251 _cell_measurement_theta_min 2.8866 _cell_measurement_theta_max 29.1410 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69498 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Eos' _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 4179 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 24.99 _reflns_number_total 980 _reflns_number_gt 772 _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. REM The guest molecules are highly disordered in the structure. # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.100 0.400 0.000 441 79 ' ' 2 -0.121 0.379 0.500 441 79 ' ' _platon_squeeze_details ; _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^)+(0.0920P)^2^+1.2006P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 980 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _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 0.2500 0.2500 0.3027(2) 0.0206(10) Uani 1 2 d S . . Be2 Be 0.0000 0.2204(4) 0.2500 0.0214(10) Uani 1 2 d S . . O1 O 0.19449(15) 0.14658(16) 0.35995(8) 0.0263(6) Uani 1 1 d . . . O2 O -0.00958(15) 0.13258(15) 0.32197(8) 0.0238(5) Uani 1 1 d . . . O3 O 0.12905(14) 0.29534(15) 0.25815(9) 0.0241(5) Uani 1 1 d . . . H1 H 0.1338 0.3693 0.2357 0.029 Uiso 1 1 calc R . . C1 C 0.0861(3) 0.0938(3) 0.5000 0.0210(8) Uani 1 2 d S . . H2 H 0.1448 0.1564 0.5000 0.025 Uiso 1 2 calc SR . . C2 C 0.0430(2) 0.0479(2) 0.43402(12) 0.0187(6) Uani 1 1 d . . . C3 C 0.0795(2) 0.1120(2) 0.36603(12) 0.0188(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 0.021(2) 0.027(2) 0.013(2) 0.000 0.000 -0.0016(18) Be2 0.025(2) 0.027(2) 0.012(2) 0.000 -0.0029(16) 0.000 O1 0.0203(9) 0.0425(12) 0.0162(9) 0.0100(8) -0.0004(7) -0.0036(8) O2 0.0219(9) 0.0342(11) 0.0153(9) 0.0058(7) -0.0039(7) -0.0056(8) O3 0.0231(9) 0.0284(10) 0.0207(10) 0.0064(7) -0.0040(7) -0.0040(7) C1 0.0213(17) 0.0262(19) 0.0156(18) 0.000 0.000 -0.0048(15) C2 0.0181(11) 0.0266(13) 0.0114(12) 0.0013(9) 0.0003(9) -0.0016(10) C3 0.0207(12) 0.0241(13) 0.0116(13) -0.0040(10) 0.0009(9) -0.0022(10) _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 O3 1.583(3) 6 ? Be1 O3 1.583(3) . ? Be1 O1 1.671(3) 6 ? Be1 O1 1.671(3) . ? Be2 O3 1.589(3) . ? Be2 O3 1.589(3) 3 ? Be2 O2 1.655(3) 3 ? Be2 O2 1.655(3) . ? O1 C3 1.259(3) . ? O2 C3 1.251(3) . ? O3 H1 0.9300 . ? C1 C2 1.393(3) . ? C1 C2 1.393(3) 10_556 ? C1 H2 0.9300 . ? C2 C2 1.397(5) 2 ? C2 C3 1.493(3) . ? 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 O3 Be1 O3 117.6(3) 6 . ? O3 Be1 O1 106.12(8) 6 6 ? O3 Be1 O1 112.06(9) . 6 ? O3 Be1 O1 112.06(9) 6 . ? O3 Be1 O1 106.12(8) . . ? O1 Be1 O1 101.9(2) 6 . ? O3 Be2 O3 115.9(3) . 3 ? O3 Be2 O2 109.96(8) . 3 ? O3 Be2 O2 106.94(8) 3 3 ? O3 Be2 O2 106.94(8) . . ? O3 Be2 O2 109.96(8) 3 . ? O2 Be2 O2 106.8(3) 3 . ? C3 O1 Be1 126.66(17) . . ? C3 O2 Be2 125.77(16) . . ? Be1 O3 Be2 123.06(16) . . ? Be1 O3 H1 118.5 . . ? Be2 O3 H1 118.5 . . ? C2 C1 C2 121.3(3) . 10_556 ? C2 C1 H2 119.4 . . ? C2 C1 H2 119.4 10_556 . ? C1 C2 C2 119.37(16) . 2 ? C1 C2 C3 118.0(2) . . ? C2 C2 C3 122.28(13) 2 . ? O2 C3 O1 125.8(2) . . ? O2 C3 C2 116.4(2) . . ? O1 C3 C2 117.7(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.635 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.068