#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/29/2002927.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_2002927 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_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 14.997(5) _cell_length_b 5.860(3) _cell_length_c 10.402(4) _cell_measurement_reflns_used 32 _cell_measurement_temperature 20 _cell_measurement_theta_max 27 _cell_measurement_theta_min 20 _cell_volume 914.2(7) _computing_cell_refinement local _computing_data_collection local _computing_data_reduction local _computing_structure_refinement 'UPALS (Lundgren, 1982)' _diffrn_ambient_temperature 20 _diffrn_measurement_device 'beamline H6M, HFBR' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator 'Be (002)' _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 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1516 _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 0.293 _exptl_absorpt_correction_T_max 0.431 _exptl_absorpt_correction_T_min 0.343 _exptl_absorpt_correction_type analytical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.759 _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 % of maximum' _refine_diff_density_min '1 % of maximum' _refine_ls_abs_structure_details ' ?' _refine_ls_extinction_coef 510E1(10) _refine_ls_extinction_method 'type I, isotropic' _refine_ls_goodness_of_fit_all 1.0436 _refine_ls_goodness_of_fit_obs 1.0436 _refine_ls_hydrogen_treatment ref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 271 _refine_ls_number_reflns 1484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_obs 0.0342 _refine_ls_shift/esd_max .01 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme w=1/[\s^2^(F)+0.0004F^2^] _refine_ls_wR_factor_all 0.0405 _refine_ls_wR_factor_obs 0.0405 _reflns_number_observed 1363 _reflns_number_total 1484 _reflns_observed_criterion I>3\s _[local]_cod_data_source_file bk0051.cif _[local]_cod_data_source_block III _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 ; _cod_original_cell_volume 914.1(11) _cod_database_code 2002927 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 0.0069(5) 0.0069(11) 0.0082(6) -0.0002(3) -0.0012(5) -0.0005(4) N12 0.0061(5) 0.0034(11) 0.0073(6) -0.0005(3) -0.0011(5) -0.0004(3) N21 0.0060(5) 0.0050(10) 0.0052(5) 0.0000(3) 0.0015(4) -0.0001(3) N22 0.0076(6) 0.0050(11) 0.0094(6) -0.0008(3) 0.0017(5) -0.0007(4) Be1 0.0070(6) 0.0012(12) 0.0070(7) 0.0005(3) 0.0002(5) 0.0003(3) Be2 0.0032(6) 0.0056(11) 0.0043(7) -0.0001(3) 0.0008(5) -0.0002(3) F11 0.0044(6) 0.0072(12) 0.0081(7) 0.0000(6) -0.0012(5) 0.0002(6) F12 0.0078(6) 0.0064(11) 0.0051(6) -0.0019(8) 0.0007(4) -0.0015(7) F13 0.0056(5) 0.0019(10) 0.0074(6) 0.0003(5) 0.0005(5) 0.0002(6) F14 0.0069(6) 0.0045(11) 0.0080(6) -0.0004(5) 0.0010(5) 0.0015(6) F21 0.0057(6) 0.0061(11) 0.0090(7) 0.0009(7) 0.0009(5) -0.0018(7) F22 0.0074(6) 0.0050(12) 0.0055(6) -0.0009(7) 0.0005(4) -0.0002(7) F23 0.0069(6) 0.0044(11) 0.0080(6) -0.0016(5) -0.0013(5) -0.0010(6) F24 0.0061(5) 0.0051(11) 0.0073(6) 0.0007(5) 0.0003(5) 0.0022(6) H111 0.017(2) 0.028(2) 0.034(2) -0.003(2) -0.0100(10) 0.003(2) H112 0.030(2) 0.033(2) 0.025(2) 0.003(2) 0.0130(10) -0.006(2) H113 0.032(2) 0.015(3) 0.027(2) -0.001(2) -0.0020(10) -0.004(2) H114 0.028(2) 0.028(3) 0.0200(10) -0.0010(10) -0.0040(10) 0.0090(10) H121 0.0130(10) 0.027(3) 0.029(2) -0.0050(10) 0.0050(10) -0.003(2) H122 0.025(2) 0.025(3) 0.024(2) -0.0010(10) -0.0140(10) 0.003(2) H123 0.031(2) 0.008(3) 0.031(2) -0.004(2) -0.0030(10) 0.008(2) H124 0.0250(10) 0.015(3) 0.0230(10) 0.0020(10) 0.0050(10) -0.0100(10) H211 0.047(3) 0.031(3) 0.0070(10) 0.001(2) 0.010(2) -0.0020(10) H212 0.0150(10) 0.024(3) 0.026(2) 0.0010(10) -0.0070(10) 0.003(2) H213 0.0170(10) 0.020(3) 0.0290(10) -0.0060(10) 0.0030(10) 0.0020(10) H214 0.033(2) 0.014(3) 0.030(2) 0.008(2) -0.0010(10) -0.0060(10) H221 0.026(2) 0.041(3) 0.020(2) -0.003(2) -0.002(2) 0.008(2) H222 0.0190(10) 0.029(2) 0.027(2) 0.005(2) 0.0100(10) -0.005(2) H223 0.0200(10) 0.021(3) 0.0250(10) -0.0100(10) 0.0000(10) -0.0030(10) H224 0.033(2) 0.010(3) 0.034(2) 0.007(2) 0.0030(10) 0.003(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 0.21960(10) 0.2666(3) 0.0990 ? Uani ? ? N N12 0.47120(10) 0.2538(2) 0.39410(10) ? Uani ? ? N N21 0.35100(10) 0.2600(2) 0.7972(2) ? Uani ? ? N N22 0.60070(10) 0.2369(2) 0.6937(2) ? Uani ? ? N Be1 0.2517(2) 0.2578(2) 0.4152(2) ? Uani ? ? Be Be2 0.50290(10) 0.2574(2) 0.0774(2) ? Uani ? ? Be F11 0.1544(2) 0.2247(4) 0.3718(3) ? Uani ? ? F F12 0.25650(10) 0.2991(5) 0.5624(3) ? Uani ? ? F F13 0.30280(10) 0.0366(3) 0.3832(3) ? Uani ? ? F F14 0.29050(10) 0.4680(4) 0.3475(3) ? Uani ? ? F F21 0.4054(2) 0.2905(5) 0.1265(3) ? Uani ? ? F F22 0.5049(2) 0.2173(4) -0.0687(3) ? Uani ? ? F F23 0.55400(10) 0.4773(4) 0.1097(3) ? Uani ? ? F F24 0.54210(10) 0.0466(4) 0.1451(3) ? Uani ? ? F H111 0.2832(3) 0.2959(10) 0.1288(6) ? Uani ? ? H H112 0.1754(4) 0.2971(11) 0.1708(5) ? Uani ? ? H H113 0.2151(3) 0.0991(10) 0.0735(5) ? Uani ? ? H H114 0.2058(3) 0.3706(8) 0.0213(4) ? Uani ? ? H H121 0.5369(3) 0.2753(8) 0.3712(6) ? Uani ? ? H H122 0.4319(3) 0.2792(9) 0.3164(5) ? Uani ? ? H H123 0.4622(3) 0.0894(9) 0.4226(5) ? Uani ? ? H H124 0.4534(2) 0.3611(7) 0.4672(4) ? Uani ? ? H H211 0.3634(5) 0.2620(7) 0.7056(5) ? Uani ? ? H H212 0.4066(3) 0.2192(9) 0.8479(5) ? Uani ? ? H H213 0.2997(2) 0.1500(8) 0.8156(4) ? Uani ? ? H H214 0.3332(3) 0.4222(8) 0.8244(4) ? Uani ? ? H H221 0.6183(4) 0.2235(10) 0.7903(6) ? Uani ? ? H H222 0.6563(3) 0.1994(11) 0.6397(5) ? Uani ? ? H H223 0.5494(2) 0.1289(7) 0.6742(4) ? Uani ? ? H H224 0.5835(3) 0.4013(9) 0.6752(5) ? 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 110.6(2) no F11 Be1 F13 107.6(2) no F11 Be1 F14 109.1(2) no F12 Be1 F13 108.7(2) no F12 Be1 F14 108.1(2) no F13 Be1 F14 112.8(2) no F21 Be2 F22 111.1(2) no F21 Be2 F23 107.0(2) no F21 Be2 F24 108.0(2) no F22 Be2 F23 109.5(2) no F22 Be2 F24 108.8(2) no F23 Be2 F24 112.5(2) no H111 N11 H112 111.0(5) no H111 N11 H113 107.6(4) no H111 N11 H114 109.1(4) no H112 N11 H113 108.6(5) no H112 N11 H114 110.0(4) no H113 N11 H114 110.6(4) no H121 N12 H122 111.0(4) no H121 N12 H123 108.2(4) no H121 N12 H124 110.4(4) no H122 N12 H123 107.2(4) no H122 N12 H124 110.6(4) no H123 N12 H124 109.3(4) no H211 N21 H212 110.8(6) no H211 N21 H213 109.6(5) no H211 N21 H214 108.0(4) no H212 N21 H213 111.9(4) no H212 N21 H214 106.8(4) no H213 N21 H214 109.6(4) no H221 N22 H222 107.8(5) no H221 N22 H223 109.7(4) no H221 N22 H224 108.6(4) no H222 N22 H223 111.8(4) no H222 N22 H224 107.8(5) no H223 N22 H224 111.1(4) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Be1 F11 1.539(3) no Be1 F12 1.553(4) no Be1 F13 1.542(3) no Be1 F14 1.533(3) no Be2 F21 1.560(3) no Be2 F22 1.539(4) no Be2 F23 1.537(3) no Be2 F24 1.538(3) no N11 H111 1.018(5) no N11 H112 1.014(6) no N11 H113 1.019(6) no N11 H114 1.033(5) no N12 H121 1.020(5) no N12 H122 1.012(6) no N12 H123 1.017(5) no N12 H124 1.022(5) no N21 H211 .971(6) no N21 H212 1.015(5) no N21 H213 1.023(4) no N21 H214 1.027(5) no N22 H221 1.043(7) no N22 H222 1.028(5) no N22 H223 1.017(4) no N22 H224 1.016(5) 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 . 1.018(5) 1.833(5) 2.805(3) 158.5(5) yes N11 H113 F12 3_544 1.019(8) 1.813(7) 2.789(4) 159.3(4) yes N11 H114 F13 3_554 1.033(5) 1.740(5) 2.767(3) 172.2(4) yes N12 H121 F11 4_555 1.021(5) 1.763(5) 2.760(3) 164.5(5) yes N12 H123 F22 2_655 1.017(5) 1.866(6) 2.811(3) 153.1(4) yes N12 H124 F23 2_665 1.022(5) 1.762(5) 2.767(3) 166.6(3) yes N21 H212 F22 1_556 1.015(5) 1.711(5) 2.708(3) 166.6(5) yes N21 H213 F14 3_545 1.023(4) 1.754(6) 2.777(3) 178.4(4) yes N21 H214 F11 3_555 1.027(5) 1.849(5) 2.833(3) 159.1(4) yes N21 H214 F13 3_555 1.027(5) 2.232(5) 2.958(2) 126.3(4) yes N22 H222 F12 4_555 1.028(5) 1.704(5) 2.715(3) 166.1(6) yes N22 H223 F24 2_655 1.017(4) 1.742(4) 2.757(3) 177.1(4) yes N22 H224 F21 2_665 1.016(5) 1.883(6) 2.858(3) 159.7(4) yes _cod_database_fobs_code 2002927 _journal_paper_doi 10.1107/S010876819800737X