#------------------------------------------------------------------------------ #$Date$ #$Revision$ #$URL$ #------------------------------------------------------------------------------ # # 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_2104204 loop_ _publ_author_name 'Udovenko, Anatoly A.' 'Laptash, Natalia M.' _publ_section_title ; Orientational disorder and phase transitions in crystals of (NH~4~)~2~NbOF~5~ ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 527 _journal_page_last 533 _journal_volume 64 _journal_year 2008 _chemical_formula_moiety 'F5 Nb O, 2(H4 N)' _chemical_formula_sum ' F5 H8 N2 Nb O' _chemical_formula_weight 239.99 _chemical_name_common 'ammonium pentafluorooxoniobate(V)' _chemical_name_systematic 'ammonium pentafluorooxoniobate(V)' _space_group_IT_number 5 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.195(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.4051(9) _cell_length_b 5.9715(3) _cell_length_c 7.2312(3) _cell_measurement_reflns_used 1000 _cell_measurement_temperature 233(2) _cell_measurement_theta_max 39.00 _cell_measurement_theta_min 2.82 _cell_volume 622.02(6) _computing_cell_refinement 'Bruker SAINT v6.02a (Bruker, 2000)' _computing_data_collection 'Bruker Smart v5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT v6.02a (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL v5.1 (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL v5.1 (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL v5.1 (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL v5.1 (Bruker, 1998)' _diffrn_ambient_temperature 233(2) _diffrn_detector_area_resol_mean 8.33 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8132 _diffrn_reflns_theta_full 39.00 _diffrn_reflns_theta_max 39.00 _diffrn_reflns_theta_min 2.82 _exptl_absorpt_coefficient_mu 1.970 _exptl_absorpt_correction_T_max 0.5712 _exptl_absorpt_correction_T_min 0.5712 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS v.2.03; Bruker 1999' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_description sphere _exptl_crystal_F_000 464 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_size_rad 0.16 _refine_diff_density_max 0.985 _refine_diff_density_min -0.971 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_extinction_coef 0.1807(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 84 _refine_ls_number_reflns 3062 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.138 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0188 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0527 _reflns_number_gt 3003 _reflns_number_total 3062 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file bp5012.cif _[local]_cod_data_source_block 233K _[local]_cod_cif_authors_sg_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_type_symbol _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_occupancy Nb Nb1 0.398173(4) 0.50020(11) 0.251190(7) 0.013680(10) Uani d 1 N N1 0.72324(6) 0.4967(6) 0.22971(12) 0.02374(16) Uani d 1 N N2 0.06873(6) 0.4954(5) 0.25705(11) 0.02267(15) Uani d 1 O O1 0.51702(5) 0.5082(6) 0.28252(11) 0.0338(2) Uani d 1 F F1 0.25423(5) 0.5103(5) 0.18836(14) 0.0430(2) Uani d 1 F F2 0.36820(10) 0.26567(15) 0.42853(15) 0.0363(3) Uani d 1 F F3 0.39642(10) 0.25751(17) 0.06887(15) 0.0339(3) Uani d 1 F F4 0.39477(10) 0.72709(15) 0.06373(13) 0.0310(3) Uani d 1 F F5 0.36367(10) 0.72459(16) 0.43338(13) 0.0294(3) Uani d 1 H H1 0.6628 0.5015 0.2412 0.070 Uiso d 1 H H2 0.1238 0.4991 0.2131 0.080 Uiso d 1 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 Nb1 0.01373(3) 0.01358(3) 0.01373(2) 0.00031(6) -0.00045(2) -0.00005(5) N1 0.0211(3) 0.0247(4) 0.0254(3) -0.0053(9) -0.0008(2) 0.0025(9) N2 0.0254(3) 0.0205(3) 0.0221(3) 0.0029(10) 0.0015(2) -0.0035(8) O1 0.0153(2) 0.0595(6) 0.0265(3) -0.0116(8) -0.0023(2) 0.0042(9) F1 0.0144(2) 0.0657(6) 0.0488(4) 0.0051(8) -0.0040(3) -0.0081(10) F2 0.0563(7) 0.0221(4) 0.0305(4) -0.0123(4) -0.0071(4) 0.0145(3) F3 0.0475(6) 0.0225(4) 0.0319(4) -0.0027(4) 0.0097(4) -0.0057(3) F4 0.0499(7) 0.0226(4) 0.0204(3) 0.0047(4) 0.0025(4) 0.0144(3) F5 0.0468(6) 0.0251(5) 0.0163(3) 0.0083(4) 0.0042(4) -0.0021(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Nb1 O1 . 1.7268(8) Nb1 F4 . 1.9171(10) Nb1 F5 . 1.9449(11) Nb1 F2 . 1.9484(11) Nb1 F3 . 1.9593(12) Nb1 F1 . 2.1221(7) N1 F1 3_545 2.954(5) N1 F5 3_545 2.980(2) N1 O1 . 2.9971(12) N1 F2 3 2.998(2) N1 F1 2_655 3.0427(13) N1 F4 2_655 3.043(2) N1 F5 2_656 3.062(2) N1 F3 2_655 3.106(2) N1 F1 3 3.114(5) N1 F2 2_656 3.125(2) N1 F3 3 3.166(2) N1 F4 3_545 3.187(2) N1 H1 . 0.8753 N2 F1 . 2.7209(12) N2 F4 4_545 2.869(2) N2 F3 4 2.875(2) N2 F5 4_546 2.926(2) N2 F2 4_556 2.930(2) N2 O1 3_445 3.009(4) N2 O1 3_455 3.157(4) N2 F3 3_455 3.231(2) N2 F4 3_445 3.283(2) N2 H2 . 0.8559 O1 F4 . 2.701(2) O1 F3 . 2.762(2) O1 F5 . 2.785(2) O1 F2 . 2.797(2) F1 F4 . 2.569(2) F1 F3 . 2.689(2) F1 F5 . 2.691(2) F1 F2 . 2.797(2) F2 F5 . 2.7415(12) F3 F4 . 2.8044(12) F3 N2 4_545 2.875(2) F4 F5 . 2.7118(14) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Nb1 F2 98.94(9) O1 Nb1 F3 96.85(9) O1 Nb1 F4 95.52(9) O1 Nb1 F5 98.49(9) O1 Nb1 F1 174.20(9) F4 Nb1 F1 78.81(8) F5 Nb1 F1 82.75(7) F2 Nb1 F1 86.71(8) F3 Nb1 F1 82.33(8) F4 Nb1 F5 89.20(5) F4 Nb1 F2 165.51(6) F5 Nb1 F2 89.52(4) F2 Nb1 F3 84.77(5) F4 Nb1 F3 92.68(4) F5 Nb1 F3 164.29(6)