#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012133.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012133 loop_ _publ_author_name 'Harrison, William T. A.' _publ_section_title ; [H~3~N(CH~2~)~2~NH~3~]~0.5~[BePO~4~], a beryllophosphate analogue of aluminosilicate zeolite gismondine ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 891 _journal_page_last 892 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '(C2 H10 N2 )0.5 , (BePO4 )' _chemical_formula_moiety '0.5C2 H10 N2 2+ , BePO4 2- ' _chemical_formula_sum 'C H5 Be N O4 P' _chemical_formula_weight 135.04 _chemical_melting_point ? _chemical_name_common 'beryllophosphate gismondine' _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.951(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 9.6165(7) _cell_length_b 9.0032(7) _cell_length_c 9.6231(7) _cell_measurement_reflns_used 1618 _cell_measurement_temperature 298 _cell_measurement_theta_max 30.00 _cell_measurement_theta_min 3.02 _cell_volume 833.05(11) _computing_cell_refinement SAINT _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298 _diffrn_measured_fraction_theta_full .997 _diffrn_measured_fraction_theta_max .997 _diffrn_measurement_device_type 'Bruker SMART1000 CCD diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .031 _diffrn_reflns_av_sigmaI/netI .039 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 3583 _diffrn_reflns_theta_full 30.01 _diffrn_reflns_theta_max 30.01 _diffrn_reflns_theta_min 3.10 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu .555 _exptl_absorpt_correction_T_max .974 _exptl_absorpt_correction_T_min .912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 552 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .06 _exptl_crystal_size_min .05 _refine_diff_density_max .580 _refine_diff_density_min -.368 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 81 _refine_ls_number_reflns 1227 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.02 _refine_ls_R_factor_all .048 _refine_ls_R_factor_gt .035 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .093 _reflns_number_gt 1001 _reflns_number_total 1227 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gd1154.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M ' I 2/a ' _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not measured' was changed to '?' - the value is undefined or not given. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012133 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Be1 .0888(2) .1478(3) .1311(2) .0111(4) Uani d . 1 Be P1 .38754(5) .10285(5) .16681(4) .00864(14) Uani d . 1 P O1 .23221(15) .06926(16) .17490(15) .0203(3) Uani d . 1 O O2 .42344(15) .18611(16) .03443(13) .0183(3) Uani d . 1 O O3 .43633(17) .19378(16) .29234(14) .0223(3) Uani d . 1 O O4 .46021(15) -.04672(16) .18027(16) .0220(3) Uani d . 1 O N1 .4273(4) .5102(4) .0092(4) .0236(8) Uani d P .50 N H1 .4373 .4069 .0277 .028 Uiso d PR .50 H H2 .4708 .5658 .0810 .028 Uiso d PR .50 H H3 .4681 .5330 -.0773 .028 Uiso d PR .50 H N2 .2559(4) .7428(4) -.1801(3) .0221(7) Uani d P .50 N H4 .2421 .8461 -.1916 .027 Uiso d PR .50 H H5 .3422 .7136 -.2152 .027 Uiso d PR .50 H H6 .1825 .6894 -.2238 .027 Uiso d PR .50 H C1 .2762(4) .5474(4) .0020(5) .0209(9) Uiso d P .50 C H11 .2346 .5268 .0883 .025 Uiso d PR .50 H H12 .2319 .4941 -.0700 .025 Uiso d PR .50 H C2 .2549(5) .7089(4) -.0285(4) .0206(9) Uiso d P .50 C H21 .3265 .7615 .0169 .025 Uiso d PR .50 H H22 .1669 .7373 .0082 .025 Uiso d PR .50 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Be1 .0096(10) .0127(10) .0109(9) -.0003(8) -.0008(8) -.0007(8) P1 .0089(2) .0081(2) .0089(2) .00121(17) -.00107(14) -.00124(15) O1 .0089(6) .0303(8) .0217(7) .0024(6) -.0003(5) .0112(6) O2 .0203(7) .0248(8) .0097(6) -.0086(6) -.0009(5) .0018(5) O3 .0398(9) .0144(7) .0125(6) -.0020(6) -.0067(6) -.0045(5) O4 .0178(7) .0148(7) .0334(8) .0095(6) .0017(6) -.0020(6) N1 .031(2) .0174(17) .0226(16) .0047(15) -.0102(15) -.0069(14) N2 .0229(18) .0184(17) .0252(18) .0038(14) .0044(15) .0043(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Be Be .0005 .0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Be1 O4 . 6 109.56(16) yes O1 Be1 O3 . 7 113.72(16) yes O4 Be1 O3 6 7 103.98(15) yes O1 Be1 O2 . 2 113.48(16) yes O4 Be1 O2 6 2 111.25(16) yes O3 Be1 O2 7 2 104.38(15) yes O4 P1 O2 . . 113.37(9) yes O4 P1 O3 . . 105.81(8) yes O2 P1 O3 . . 109.09(8) yes O4 P1 O1 . . 105.58(8) yes O2 P1 O1 . . 112.06(8) yes O3 P1 O1 . . 110.72(9) yes P1 O1 Be1 . . 137.59(13) yes P1 O2 Be1 . 2 134.33(13) yes P1 O3 Be1 . 7 141.57(13) yes P1 O4 Be1 . 6_655 145.86(14) yes N1 C1 C2 . . 111.0(3) no N2 C2 C1 . . 112.8(3) no C1 N1 H1 . . 108.9 no C1 N1 H2 . . 109.5 no H1 N1 H2 . . 109.8 no C1 N1 H3 . . 109.1 no H1 N1 H3 . . 109.5 no H2 N1 H3 . . 110.1 no C2 N2 H4 . . 108.2 no C2 N2 H5 . . 108.4 no H4 N2 H5 . . 110.9 no C2 N2 H6 . . 108.3 no H4 N2 H6 . . 110.1 no H5 N2 H6 . . 110.8 no N1 C1 H11 . . 109.9 no C2 C1 H11 . . 107.7 no N1 C1 H12 . . 110.4 no C2 C1 H12 . . 107.0 no H11 C1 H12 . . 110.8 no N2 C2 H21 . . 109.6 no C1 C2 H21 . . 107.6 no N2 C2 H22 . . 109.1 no C1 C2 H22 . . 107.8 no H21 C2 H22 . . 109.9 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Be1 O1 . 1.600(3) yes Be1 O4 6 1.613(3) yes Be1 O3 7 1.625(3) yes Be1 O2 2 1.632(3) yes P1 O4 . 1.5216(15) yes P1 O2 . 1.5226(14) yes P1 O3 . 1.5267(13) yes P1 O1 . 1.5273(15) yes N1 N1 5_665 1.423(8) no N1 C1 . 1.492(5) yes N2 N2 7_564 1.355(7) no N2 C2 . 1.491(5) yes C1 C1 2 .505(8) no C1 C2 . 1.496(5) yes C1 C2 2 1.506(5) no C2 C2 2 .557(7) no N1 H1 . .9511 no N1 H2 . .9452 no N1 H3 . .9482 no N2 H4 . .9457 no N2 H5 . .9384 no N2 H6 . .9465 no C1 H11 . .9454 no C1 H12 . .9396 no C2 H21 . .9376 no C2 H22 . .9570 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 O2 . .95 1.99 2.928(4) 167.0 yes N1 H2 O3 4 .95 1.89 2.831(4) 173.0 yes N1 H3 O4 8_554 .95 2.34 3.203(4) 151.7 yes N2 H4 O1 2_565 .95 2.03 2.942(4) 161.3 yes N2 H5 O4 8_554 .94 2.14 2.978(4) 147.5 yes N2 H6 O3 3_454 .95 2.38 3.112(4) 134.3 yes N2 H6 O1 8_554 .95 2.57 3.143(4) 119.1 yes 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_publ_flag N1 C1 C2 N2 85.3(5) no