#------------------------------------------------------------------------------ #$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/29/2002926.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_2002926 loop_ _publ_author_name 'Srivastava, R. C.' 'Klooster, W. T.' 'Koetzle, T. F.' _publ_section_title ; Neutron structures of ammonium tetrafluoroberyllate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 17 _journal_page_last 23 _journal_paper_doi 10.1107/S010876819800737X _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '(N H4)2 Be F4' _chemical_formula_sum 'Be F4 H8 N2' _chemical_formula_weight 121.093 _chemical_name_systematic ; ammonium tetrafluoroberyllate ; _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_formula_units_Z 8 _cell_length_a 15.017(6) _cell_length_b 5.876(3) _cell_length_c 10.418(4) _cell_measurement_reflns_used 32 _cell_measurement_temperature 163 _cell_measurement_theta_max 27 _cell_measurement_theta_min 20 _cell_volume 919.3(7) _computing_cell_refinement local _computing_data_collection local _computing_data_reduction local _computing_structure_refinement 'UPALS (Lundgren, 1982)' _diffrn_ambient_temperature 163 _diffrn_measurement_device 'beamline H6M, HFBR' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator 'Be (002)' _diffrn_radiation_probe neutron _diffrn_radiation_source reactor _diffrn_radiation_type neutron _diffrn_radiation_wavelength 1.0462 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1972 _diffrn_reflns_theta_max 55 _diffrn_reflns_theta_min 2 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_T_max 0.432 _exptl_absorpt_correction_T_min 0.346 _exptl_absorpt_correction_type analytical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.750 _exptl_crystal_description box _exptl_crystal_size_max 4.0 _exptl_crystal_size_mid 3.9 _exptl_crystal_size_min 3.9 _refine_diff_density_max '1.5 % of maximum' _refine_diff_density_min '1.5 % of maximum' _refine_ls_abs_structure_details ' ?' _refine_ls_extinction_coef 390E1(10) _refine_ls_extinction_method 'type I, isotropic' _refine_ls_goodness_of_fit_all 1.0650 _refine_ls_goodness_of_fit_obs 1.0650 _refine_ls_hydrogen_treatment ref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 271 _refine_ls_number_reflns 1932 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_obs 0.0476 _refine_ls_shift/esd_max .01 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details w=1/[\s^2^(F)+0.0004F^2^] _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0552 _refine_ls_wR_factor_obs 0.0552 _reflns_number_observed 1390 _reflns_number_total 1932 _reflns_observed_criterion I>3\s _cod_data_source_file bk0051.cif _cod_data_source_block II _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 30 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w=1/[\s^2^(F)+0.0004F^2^]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(F)+0.0004F^2^]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 919.2(12) _cod_database_code 2002926 _cod_database_fobs_code 2002926 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,1/2+z 1/2-x,1/2+y,1/2+z 1/2+x,1/2-y,z 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 N11 0.0129(9) 0.0124(8) 0.0146(8) -0.0008(4) 0.0010(8) -0.0006(5) N12 0.0131(9) 0.0153(8) 0.0201(9) 0.0000(4) 0.0000(9) -0.0005(5) N21 0.0115(8) 0.0161(9) 0.0148(9) -0.0001(4) 0.0037(7) -0.0006(5) N22 0.0191(10) 0.0119(9) 0.0147(9) -0.0025(4) 0.0018(8) 0.0002(5) Be1 0.0099(10) 0.0136(9) 0.0093(9) -0.0003(5) -0.0020(7) -0.0004(5) Be2 0.0115(11) 0.0086(8) 0.0156(11) -0.0001(5) -0.0025(8) 0.0005(5) F11 0.0122(13) 0.0308(14) 0.038(2) 0.0010(11) -0.0112(14) -0.0021(15) F12 0.0217(14) 0.0246(10) 0.0112(11) 0.0004(12) 0.0005(10) -0.0014(11) F13 0.0181(11) 0.0116(9) 0.0265(14) 0.0004(9) 0.0060(10) -0.0047(10) F14 0.0203(13) 0.0134(11) 0.0250(14) -0.0002(9) 0.0056(11) 0.0062(10) F21 0.0122(13) 0.0311(13) 0.0313(18) 0.0044(10) 0.0022(13) 0.0016(14) F22 0.0281(17) 0.0288(12) 0.0131(13) 0.0048(13) 0.0003(11) -0.0035(13) F23 0.0233(13) 0.0126(10) 0.0269(15) -0.0027(9) -0.0097(11) -0.0012(10) F24 0.0200(13) 0.0152(11) 0.0315(18) 0.0013(9) -0.0040(11) 0.0102(11) H111 0.040(4) 0.048(3) 0.051(4) -0.013(3) -0.021(3) 0.012(3) H112 0.048(4) 0.050(3) 0.040(4) -0.009(3) 0.024(3) -0.021(3) H113 0.048(4) 0.031(2) 0.075(5) -0.014(2) 0.014(4) -0.020(3) H114 0.034(3) 0.032(2) 0.028(2) 0.005(2) -0.008(2) 0.004(2) H121 0.014(2) 0.045(3) 0.050(3) -0.005(2) 0.005(2) -0.008(3) H122 0.044(4) 0.054(4) 0.048(4) 0.001(3) -0.025(4) 0.002(4) H123 0.041(3) 0.023(2) 0.035(3) -0.003(2) -0.002(2) 0.004(2) H124 0.036(3) 0.056(4) 0.062(5) 0.002(3) 0.001(3) -0.042(4) H211 0.037(2) 0.107(6) 0.014(2) -0.002(4) 0.012(2) -0.001(3) H212 0.026(3) 0.051(4) 0.043(3) 0.006(3) -0.004(2) 0.003(3) H213 0.018(2) 0.031(2) 0.037(2) -0.006(2) 0.006(2) 0.005(2) H214 0.097(6) 0.047(3) 0.033(3) 0.049(4) -0.002(4) -0.014(3) H221 0.078(5) 0.040(3) 0.024(3) -0.020(3) 0.003(3) 0.006(2) H222 0.032(3) 0.048(3) 0.042(4) 0.002(3) 0.018(3) -0.004(3) H223 0.079(5) 0.053(4) 0.045(4) -0.036(4) 0.006(4) 0.002(3) H224 0.058(4) 0.024(2) 0.065(4) 0.004(2) 0.008(3) -0.010(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_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol N11 0.2188(2) 0.2600(3) 0.0990 ? Uani ? ? N N12 0.4691(2) 0.2527(2) 0.39780(10) ? Uani ? ? N N21 0.3534(2) 0.2562(2) 0.8015(3) ? Uani ? ? N N22 0.6025(2) 0.2404(3) 0.6957(3) ? Uani ? ? N Be1 0.2509(2) 0.2536(3) 0.4161(3) ? Uani ? ? Be Be2 0.5008(2) 0.2553(3) 0.0785(4) ? Uani ? ? Be F11 0.1534(3) 0.2299(6) 0.3769(6) ? Uani ? ? F F12 0.2584(3) 0.2867(6) 0.5617(4) ? Uani ? ? F F13 0.2989(2) 0.0333(5) 0.3792(5) ? Uani ? ? F F14 0.2903(2) 0.4609(5) 0.3490(4) ? Uani ? ? F F21 0.4026(3) 0.2750(7) 0.1231(6) ? Uani ? ? F F22 0.5084(3) 0.2235(6) -0.0674(4) ? Uani ? ? F F23 0.5485(3) 0.4767(6) 0.1175(5) ? Uani ? ? F F24 0.5417(3) 0.0452(6) 0.1443(5) ? Uani ? ? F H111 0.2820(6) 0.2840(15) 0.1285(10) ? Uani ? ? H H112 0.1773(6) 0.2828(14) 0.1732(10) ? Uani ? ? H H113 0.2137(6) 0.0995(12) 0.0681(11) ? Uani ? ? H H114 0.2050(4) 0.3645(10) 0.0218(6) ? Uani ? ? H H121 0.5342(4) 0.2658(11) 0.3743(10) ? Uani ? ? H H122 0.4267(7) 0.2783(16) 0.3255(11) ? Uani ? ? H H123 0.4604(4) 0.0883(9) 0.4239(7) ? Uani ? ? H H124 0.4546(5) 0.3666(15) 0.4646(10) ? Uani ? ? H H211 0.3720(5) 0.2607(17) 0.7123(7) ? Uani ? ? H H212 0.4091(6) 0.2233(15) 0.8513(10) ? Uani ? ? H H213 0.3032(3) 0.1444(9) 0.8207(6) ? Uani ? ? H H214 0.3257(7) 0.4022(14) 0.8282(8) ? Uani ? ? H H221 0.6125(7) 0.2383(12) 0.7935(8) ? Uani ? ? H H222 0.6563(6) 0.2190(15) 0.6382(10) ? Uani ? ? H H223 0.5583(8) 0.1183(17) 0.6792(9) ? Uani ? ? H H224 0.5849(5) 0.4021(10) 0.6796(8) ? Uani ? ? H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source H -3.7406 International_Tables_Vol_C Be 7.79 International_Tables_Vol_C N 9.36 International_Tables_Vol_C F 5.654 International_Tables_Vol_C loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 -4 0 0 -2 6 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag F11 Be1 F12 110.3(3) no F11 Be1 F13 107.9(3) no F11 Be1 F14 108.8(3) no F12 Be1 F13 108.7(3) no F12 Be1 F14 108.9(3) no F13 Be1 F14 112.2(3) no F21 Be2 F22 112.1(3) no F21 Be2 F23 107.5(3) no F21 Be2 F24 107.8(3) no F22 Be2 F23 108.3(3) no F22 Be2 F24 109.2(3) no F23 Be2 F24 112.0(3) no H111 N11 H112 109.4(8) no H111 N11 H113 107.6(7) no H111 N11 H114 110.1(7) no H112 N11 H113 109.1(8) no H112 N11 H114 113.3(7) no H113 N11 H114 107.1(7) no H121 N12 H122 115.0(8) no H121 N12 H123 105.2(5) no H121 N12 H124 109.3(7) no H122 N12 H123 105.4(7) no H122 N12 H124 106.8(8) no H123 N12 H124 115.3(7) no H211 N21 H212 105.1(8) no H211 N21 H213 114.7(7) no H211 N21 H214 111.4(8) no H212 N21 H213 113.0(6) no H212 N21 H214 111.8(8) no H213 N21 H214 101.1(7) no H221 N22 H222 117.9(9) no H221 N22 H223 105.0(8) no H221 N22 H224 102.4(7) no H222 N22 H223 110.0(8) no H222 N22 H224 103.3(7) no H223 N22 H224 118.6(8) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Be1 F11 1.526(6) no Be1 F12 1.533(6) no Be1 F13 1.531(4) no Be1 F14 1.524(4) no Be2 F21 1.550(6) no Be2 F22 1.536(6) no Be2 F23 1.540(5) no Be2 F24 1.539(4) no N11 H111 1.008(9) no N11 H112 1.002(10) no N11 H113 .999(8) no N11 H114 1.033(6) no N12 H121 1.012(7) no N12 H122 .997(11) no N12 H123 1.012(6) no N12 H124 .989(10) no N21 H211 .971(8) no N21 H212 1.003(10) no N21 H213 1.020(5) no N21 H214 .993(9) no N22 H221 1.030(9) no N22 H222 1.012(10) no N22 H223 .993(11) no N22 H224 1.001(6) 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 N11 H111 F21 . 1.008(9) 1.813(10) 2.774(5) 158.0(9) yes N11 H113 F12 3_544 .999(8) 1.887(8) 2.829(4) 156.0(9) yes N11 H114 F13 3_554 1.033(6) 1.787(8) 2.810(5) 169.6(5) yes N12 H121 F11 4_555 1.011(7) 1.790(8) 2.779(5) 164.7(9) yes N12 H123 F22 2_655 1.012(6) 1.893(7) 2.842(4) 154.8(6) yes N12 H124 F23 2_665 .989(10) 1.840(11) 2.799(5) 162.3(8) yes N21 H212 F22 1_556 1.003(10) 1.715(10) 2.705(5) 168.6(8) yes N21 H213 F14 3_545 1.020(5) 1.795(6) 2.812(4) 176.1(5) yes N21 H214 F11 3_555 .993(9) 2.016(9) 2.894(4) 146.2(9) yes N21 H214 F13 3_555 .993(9) 2.092(11) 2.921(4) 139.8(8) yes N22 H222 F12 4_555 1.012(10) 1.728(10) 2.730(5) 169.1(9) yes N22 H223 F24 2_655 .993(11) 1.819(11) 2.792(4) 165.7(9) yes N22 H224 F21 2_665 1.001(6) 1.996(7) 2.948(4) 158.0(7) yes