#------------------------------------------------------------------------------ #$Date: 2016-02-14 04:40:26 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/81/2008133.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_2008133 loop_ _publ_author_name 'Fratzky, Dietmar' 'Worzala, Horst' 'Goetze, Thomas' 'Meisel, Manfred' _publ_section_title ; NH~4~VO(NH~3~)PO~4~ ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 156 _journal_page_last 157 _journal_paper_doi 10.1107/S0108270198011123 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac 'N H4 V O (N H3) P O4' _chemical_formula_moiety 'H3NO5PV, H4N' _chemical_formula_sum 'H7 N2 O5 P V' _chemical_formula_weight 196.99 _chemical_name_common ' ammonium oxovanadium(IV) phosphate ammonia' _chemical_name_systematic ; ammonium oxovanadium(IV) phosphate ammonia ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _cell_angle_alpha 90.00 _cell_angle_beta 91.11(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.7770(10) _cell_length_b 4.9150(10) _cell_length_c 8.455(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18 _cell_measurement_theta_min 10 _cell_volume 281.57(10) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CORINC (Schollmeyr, 1992)' _computing_molecular_graphics 'DIAMOND (Bergerhoff & Bernd, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997b)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \q/2\q _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 0.027 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1765 _diffrn_reflns_theta_full 29.96 _diffrn_reflns_theta_max 29.96 _diffrn_reflns_theta_min 2.41 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.000 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(CORINC; Schollmeyr, 1992)' _exptl_crystal_colour 'light blue' _exptl_crystal_density_diffrn 2.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 198 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.481 _refine_diff_density_min -0.365 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1646 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.050 _refine_ls_R_factor_gt 0.034 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.7939P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.070 _reflns_number_gt 1426 _reflns_number_total 1646 _reflns_threshold_expression I>2\s(I) _cod_data_source_file br1216.cif _cod_data_source_block nvpo6 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.7939P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0367P)^2^+0.7939P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_Hall 'P 2y1' _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2008133 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol V1 0.35943(9) 0.65672(11) 0.65971(7) 0.01149(14) Uani d . 1 . . V P1 0.63284(13) 1.20466(16) 0.72266(10) 0.00997(19) Uani d . 1 . . P O1 0.5806(4) 0.9019(6) 0.7219(3) 0.0143(5) Uani d . 1 . . O O2 0.4731(4) 0.3768(5) 0.8053(3) 0.0151(6) Uani d . 1 . . O O3 0.3734(4) 0.8256(6) 0.4486(3) 0.0172(6) Uani d . 1 . . O O4 0.1826(4) 0.7966(6) 0.7526(4) 0.0222(6) Uani d . 1 . . O O5 0.8336(4) 1.2412(6) 0.8009(3) 0.0174(6) Uani d . 1 . . O N1 0.1674(6) 0.3495(8) 0.5622(5) 0.0174(7) Uani d . 1 . . N N2 0.1776(5) 0.2194(7) 1.0118(4) 0.0173(7) Uani d . 1 . . N H1 0.109(11) 0.289(17) 0.627(9) 0.06(3) Uiso d . 1 . . H H2 0.235(8) 0.217(15) 0.520(6) 0.037(16) Uiso d . 1 . . H H3 0.099(7) 0.421(10) 0.500(6) 0.008(11) Uiso d . 1 . . H H4 0.169(11) 0.057(17) 1.052(8) 0.06(2) Uiso d . 1 . . H H5 0.079(8) 0.242(12) 0.951(6) 0.025(14) Uiso d . 1 . . H H6 0.170(9) 0.371(14) 1.079(7) 0.039(17) Uiso d . 1 . . H H7 0.284(9) 0.255(12) 0.956(7) 0.033(16) Uiso d . 1 . . 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 V1 0.0138(3) 0.0100(3) 0.0106(2) 0.0003(3) -0.00080(19) 0.0002(3) P1 0.0113(4) 0.0100(5) 0.0085(4) -0.0011(3) -0.0022(3) 0.0002(3) O1 0.0190(14) 0.0111(12) 0.0126(12) -0.0050(10) -0.0056(10) 0.0003(10) O2 0.0169(14) 0.0133(14) 0.0153(13) 0.0027(10) -0.0004(11) 0.0020(11) O3 0.0256(15) 0.0135(13) 0.0122(13) 0.0032(11) -0.0039(11) -0.0005(10) O4 0.0213(14) 0.0224(15) 0.0231(15) 0.0037(12) 0.0039(12) -0.0025(11) O5 0.0149(12) 0.0192(14) 0.0179(13) -0.0013(10) -0.0054(10) 0.0001(10) N1 0.0151(17) 0.0158(17) 0.0211(18) -0.0006(13) -0.0042(15) -0.0004(14) N2 0.0184(16) 0.0169(19) 0.0164(15) -0.0017(13) -0.0048(13) 0.0005(13) 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 O4 V1 O3 . . 108.22(14) O4 V1 O1 . . 100.24(14) O3 V1 O1 . . 86.27(12) O4 V1 O2 . . 106.13(14) O3 V1 O2 . . 145.64(12) O1 V1 O2 . . 88.55(11) O4 V1 N1 . . 92.10(16) O3 V1 N1 . . 89.30(14) O1 V1 N1 . . 167.64(14) O2 V1 N1 . . 88.61(13) O5 P1 O1 . . 108.88(15) O5 P1 O2 . 1_565 111.61(16) O1 P1 O2 . 1_565 111.66(16) O5 P1 O3 . 2_656 111.57(16) O1 P1 O3 . 2_656 111.32(15) O2 P1 O3 1_565 2_656 101.70(15) P1 O1 V1 . . 139.89(18) P1 O2 V1 1_545 . 111.33(15) P1 O3 V1 2_646 . 132.56(17) V1 N1 H1 . . 109(6) V1 N1 H2 . . 111(4) H1 N1 H2 . . 107(7) V1 N1 H3 . . 107(4) H1 N1 H3 . . 111(6) H2 N1 H3 . . 112(5) H4 N2 H5 . . 108(6) H4 N2 H6 . . 119(5) H5 N2 H6 . . 103(5) H4 N2 H7 . . 117(6) H5 N2 H7 . . 107(5) H6 N2 H7 . . 103(5) 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 V1 O4 . 1.601(3) y V1 O3 . 1.972(3) y V1 O1 . 1.986(3) y V1 O2 . 1.991(3) y V1 N1 . 2.148(4) ? P1 O5 . 1.512(3) ? P1 O1 . 1.529(3) ? P1 O2 1_565 1.551(3) ? P1 O3 2_656 1.565(3) ? O2 P1 1_545 1.551(3) ? O3 P1 2_646 1.565(3) ? N1 H1 . 0.74(8) ? N1 H2 . 0.87(7) ? N1 H3 . 0.78(5) ? N2 H4 . 0.87(8) ? N2 H5 . 0.85(6) ? N2 H6 . 0.94(7) ? N2 H7 . 0.89(6) ? 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 N1 H1 O5 1_445 0.74(8) 2.41(8) 3.107(5) 157(8) N1 H2 O3 1_545 0.87(7) 2.23(7) 3.090(5) 168(5) N2 H4 O5 2_637 0.87(8) 1.99(8) 2.836(5) 164(7) N2 H5 O5 1_445 0.85(6) 2.07(6) 2.910(4) 172(5) N2 H6 O5 2_647 0.94(7) 2.08(7) 3.016(5) 171(6) N2 H7 O2 . 0.89(6) 1.92(6) 2.792(5) 167(5)