Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2001 data_010316b _database_code_CSD 169726 _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Chen, Zhenxia' 'Sun, Jinyu' 'Weng, Linhong' 'Zhang, Haoyu' 'Zhao, Dongyuan' 'Zhou, Yaming' _publ_contact_author_name 'Prof Dongyuan Zhao' _publ_contact_author_address ; chemistry department fudan university handan road 220 shanghai shanghai 200433 CHINA ; _publ_contact_author_email 'ZHANGHY@FUDAN.EDU.CN' _publ_section_title ; [C6N4H24]CoBe6P6O24=A1.3H2O: a novel three dimensional beryllophosphate zeolite-like structure encapsulating CoII ions ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H5 Be Co0.17 N0.67 O4.50 P' _chemical_formula_weight 148.19 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' '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' 'Co' 'Co' 0.3494 0.9721 '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' _symmetry_cell_setting 'Rhombohedral' _symmetry_space_group_name_H-M 'R-3 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 12.380(3) _cell_length_b 12.380(3) _cell_length_c 14.558(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1932.5(10) _cell_formula_units_Z 18 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1353 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7586 _exptl_absorpt_correction_T_max 0.7997 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 2781 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 756 _reflns_number_gt 750 _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^)+(0.0000P)^2^+91.2179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens NONE _refine_ls_hydrogen_treatment NONE _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 756 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0878 _refine_ls_wR_factor_ref 0.1931 _refine_ls_wR_factor_gt 0.1929 _refine_ls_goodness_of_fit_ref 1.472 _refine_ls_restrained_S_all 1.472 _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 Co1 Co 0.0000 1.0000 0.0000 0.0121(8) Uani 1 6 d S . . Be1 Be 0.2348(10) 1.0069(10) 0.0934(7) 0.016(2) Uani 1 1 d . . . P1 P 0.0044(2) 0.7732(2) 0.09669(15) 0.0146(7) Uani 1 1 d . . . O1 O -0.0739(5) 0.8374(5) 0.0828(4) 0.0145(13) Uani 1 1 d . . . O2 O 0.1338(6) 0.8703(6) 0.1254(4) 0.0199(15) Uani 1 1 d . . . O3 O -0.0496(6) 0.6768(6) 0.1686(4) 0.0215(15) Uani 1 1 d . . . O4 O 0.0061(6) 0.7136(6) 0.0065(4) 0.0224(15) Uani 1 1 d . . . N1 N 0.930(3) 0.470(4) 0.999(3) 0.060(9) Uiso 0.33 1 d P . . N2 N 0.721(4) 0.416(4) 1.024(3) 0.071(11) Uiso 0.33 1 d P . . O5 O 0.214(6) 0.703(5) 0.234(9) 0.58(10) 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 Co1 0.0098(10) 0.0098(10) 0.0167(15) 0.000 0.000 0.0049(5) Be1 0.018(6) 0.014(5) 0.017(5) -0.003(4) -0.003(4) 0.009(5) P1 0.0145(12) 0.0130(12) 0.0158(12) 0.0025(8) 0.0007(8) 0.0065(9) O1 0.012(3) 0.012(3) 0.018(3) 0.003(2) 0.003(2) 0.006(2) O2 0.016(3) 0.014(3) 0.025(3) 0.003(3) -0.003(3) 0.004(3) O3 0.016(3) 0.021(3) 0.027(3) 0.007(3) 0.004(3) 0.009(3) O4 0.029(4) 0.018(3) 0.024(3) 0.002(3) -0.005(3) 0.015(3) O5 0.34(7) 0.24(5) 1.3(3) 0.49(11) 0.62(13) 0.27(6) _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 Co1 O1 2.122(6) 11_455 ? Co1 O1 2.122(6) 12_665 ? Co1 O1 2.122(6) 2_675 ? Co1 O1 2.122(6) 3_465 ? Co1 O1 2.122(6) 10_575 ? Co1 O1 2.122(6) . ? Be1 O3 1.561(12) 14_455 ? Be1 O2 1.589(12) . ? Be1 O4 1.622(12) 12_665 ? Be1 O1 1.660(12) 2_675 ? P1 O3 1.473(6) . ? P1 O2 1.504(6) . ? P1 O4 1.512(7) . ? P1 O1 1.542(6) . ? O1 Be1 1.660(12) 3_465 ? O3 Be1 1.561(12) 15 ? O4 Be1 1.622(12) 11_455 ? N1 N1 1.50(7) 10_767 ? N2 N2 1.55(7) 2_655 ? N2 N2 1.55(7) 3_665 ? 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 Co1 O1 90.9(2) 11_455 12_665 ? O1 Co1 O1 180.000(1) 11_455 2_675 ? O1 Co1 O1 89.1(2) 12_665 2_675 ? O1 Co1 O1 89.1(2) 11_455 3_465 ? O1 Co1 O1 180.000(1) 12_665 3_465 ? O1 Co1 O1 90.9(2) 2_675 3_465 ? O1 Co1 O1 90.9(2) 11_455 10_575 ? O1 Co1 O1 90.9(2) 12_665 10_575 ? O1 Co1 O1 89.1(2) 2_675 10_575 ? O1 Co1 O1 89.1(2) 3_465 10_575 ? O1 Co1 O1 89.1(2) 11_455 . ? O1 Co1 O1 89.1(2) 12_665 . ? O1 Co1 O1 90.9(2) 2_675 . ? O1 Co1 O1 90.9(2) 3_465 . ? O1 Co1 O1 180.000(1) 10_575 . ? O3 Be1 O2 107.8(7) 14_455 . ? O3 Be1 O4 108.0(7) 14_455 12_665 ? O2 Be1 O4 111.7(7) . 12_665 ? O3 Be1 O1 114.8(7) 14_455 2_675 ? O2 Be1 O1 107.5(7) . 2_675 ? O4 Be1 O1 107.1(7) 12_665 2_675 ? O3 P1 O2 108.7(4) . . ? O3 P1 O4 109.5(4) . . ? O2 P1 O4 111.2(4) . . ? O3 P1 O1 111.3(3) . . ? O2 P1 O1 108.5(3) . . ? O4 P1 O1 107.7(3) . . ? P1 O1 Be1 124.0(5) . 3_465 ? P1 O1 Co1 118.6(3) . . ? Be1 O1 Co1 113.4(5) 3_465 . ? P1 O2 Be1 136.6(6) . . ? P1 O3 Be1 175.7(6) . 15 ? P1 O4 Be1 124.0(6) . 11_455 ? N2 N2 N2 60.000(18) 2_655 3_665 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.947 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.192