#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/70/2007089.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_2007089 loop_ _publ_author_name 'Horst Worzala' 'Goetze, Thomas ' 'Fratzky, Dietmar' 'Manfred Meisel' _publ_section_title ; Redetermination of Monoclinic VOHPO~4~.2H~2~O ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 283 _journal_page_last 285 _journal_paper_doi 10.1107/S0108270197014017 _journal_volume 54 _journal_year 1998 _chemical_formula_analytical (VOHPO4)2H2O _chemical_formula_iupac 'VOHPO4 ,2H2 O' _chemical_formula_moiety '(V O2 +),(H O4 P 2-),2(H2 O)' _chemical_formula_sum 'H5 O7 P V' _chemical_formula_weight 198.95 _chemical_name_common ' \a-vanadium(IV) hydrogenphosphat dihydrat' _chemical_name_systematic ; \a-oxovanadium(IV)hydrogen phosphate dihydrate ; _chemical_temperature_decomposition 393.15 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method 'SHELXL - 97' _cell_angle_alpha 90.00 _cell_angle_beta 95.47(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.597(2) _cell_length_b 7.4220(10) _cell_length_c 9.466(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18 _cell_measurement_theta_min 10 _cell_volume 531.31(19) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'Fair (1990)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Bernd, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.931 _diffrn_measured_fraction_theta_max 0.931 _diffrn_measurement_device_type 'Enraf-Nonius CAD-4 ' _diffrn_measurement_method '\q/2\q 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 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5980 _diffrn_reflns_theta_full 29.99 _diffrn_reflns_theta_max 30 _diffrn_reflns_theta_min 2.69 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.139 _exptl_absorpt_correction_T_max 0.807 _exptl_absorpt_correction_T_min 0.736 _exptl_absorpt_correction_type '\y scan (North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'MolEN (Fair, 1990)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.487 _exptl_crystal_density_meas 2.479(3) _exptl_crystal_density_method pycnometry _exptl_crystal_description prismatic _exptl_crystal_F_000 396 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.367 _refine_diff_density_min -0.330 _refine_ls_extinction_coef 0.0150(12) _refine_ls_extinction_method SHELXL97_(Sheldrick,_1997) _refine_ls_goodness_of_fit_all 1.119 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_hydrogen_treatment 'refall freely' _refine_ls_matrix_type full _refine_ls_number_parameters 103 _refine_ls_number_reflns 1553 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.119 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0178 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.2446P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0464 _refine_ls_wR_factor_ref 0.0464 _reflns_number_observed 1405 _reflns_number_total 1554 _reflns_observed_criterion >2sigma(I) _cod_data_source_file jz1223.cif _cod_data_source_block v2 _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' tag was changed to '_chemical_temperature_decomposition' since the value had been given as 'decomp. 120\%C'. The value 'decomp. 120\%C' was changed to '393.15' - it was converted from degrees Celsius(C) to Kelvins(K). Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana The following automatic conversions were performed: '_chemical_melting_point' tag was changed to '_chemical_temperature_decomposition' since the value had been given as 'decomp. 120\%C'. The value 'decomp. 120\%C' was changed to '393.15' - it was converted from degrees Celsius(C) to Kelvins(K). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value ' calc w = 1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.2446P] 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^)+(0.0219P)^2^+0.2446P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 531.3(2) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2007089 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' '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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol V .47583(3) .14693(3) .24294(2) .00918(7) Uani d . 1 . . V P .71860(4) .15044(4) -.01271(3) .00895(8) Uani d . 1 . . P O1 .69442(12) .13399(13) .14468(9) .01234(17) Uani d . 1 . . O O2 .62124(13) .18385(12) .42377(10) .01402(18) Uani d . 1 . . O O3 .32805(12) .02016(12) .09453(10) .01462(19) Uani d . 1 . . O O4 .92307(13) .18722(15) -.01210(11) .0177(2) Uani d . 1 . . O O5 .28260(14) .08682(15) .37142(11) .0175(2) Uani d . 1 . . O O6 .57351(13) -.14677(12) .29533(10) .01454(18) Uani d . 1 . . O O7 -.02456(15) -.08323(18) .26944(13) .0242(2) Uani d . 1 . . O H1 -.031(4) -.151(3) .330(3) .049(8) Uiso d . 1 . . H H2 -.109(3) -.034(3) .255(3) .040(7) Uiso d . 1 . . H H3 .312(3) .039(3) .447(3) .047(7) Uiso d . 1 . . H H4 .189(3) .041(3) .340(2) .042(6) Uiso d . 1 . . H H5 .957(3) .170(3) -.087(3) .045(7) 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 V .01209(11) .00742(10) .00788(10) -.00026(7) .00026(7) -.00065(7) P .01048(14) .00866(14) .00752(14) -.00021(10) -.00008(10) -.00027(10) O1 .0133(4) .0153(4) .0083(4) .0006(3) .0009(3) .0016(3) O2 .0208(5) .0107(4) .0098(4) -.0028(3) -.0029(3) -.0006(3) O3 .0180(4) .0107(4) .0142(4) .0003(3) -.0037(3) -.0030(3) O4 .0122(4) .0228(5) .0185(5) -.0032(4) .0040(4) -.0045(4) O5 .0164(4) .0218(5) .0145(5) -.0028(4) .0026(4) .0020(4) O6 .0191(4) .0104(4) .0140(4) -.0010(3) .0006(3) .0005(3) O7 .0156(5) .0323(6) .0247(6) .0029(4) .0021(4) .0054(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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 O6 V O3 2_655 . 101.00(5) O6 V O2 2_655 . 99.37(5) O3 V O2 . . 158.39(4) O6 V O1 2_655 . 97.36(5) O3 V O1 . . 95.10(4) O2 V O1 . . 89.37(4) O6 V O5 2_655 . 100.17(5) O3 V O5 . . 85.79(5) O2 V O5 . . 83.58(5) O1 V O5 . . 161.94(4) O6 V O6 2_655 . 174.91(2) O3 V O6 . . 81.53(4) O2 V O6 . . 78.74(4) O1 V O6 . . 77.96(4) O5 V O6 . . 84.36(4) O3 P O1 3_655 . 112.98(6) O3 P O2 3_655 4_565 113.09(6) O1 P O2 . 4_565 110.50(5) O3 P O4 3_655 . 109.29(6) O1 P O4 . . 102.76(6) O2 P O4 4_565 . 107.56(6) P O1 V . . 129.77(6) P O2 V 4_566 . 131.71(6) P O3 V 3_655 . 149.75(6) P O4 H5 . . 112.2(19) V O5 H3 . . 118.0(17) V O5 H4 . . 121.6(16) H3 O5 H4 . . 107(2) V O6 V 2_645 . 140.90(6) H1 O7 H2 . . 110(3) 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 V O6 2_655 1.6094(10) ? V O3 . 1.9541(10) ? V O2 . 1.9660(11) ? V O1 . 1.9815(11) ? V O5 . 2.0429(12) ? V O6 . 2.3406(10) ? P O3 3_655 1.5088(10) ? P O1 . 1.5234(10) ? P O2 4_565 1.5285(10) ? P O4 . 1.5766(11) ? O2 P 4_566 1.5285(10) ? O3 P 3_655 1.5088(10) ? O4 H5 . .79(3) ? O5 H3 . .81(3) ? O5 H4 . .82(2) ? O6 V 2_645 1.6094(10) ? O7 H1 . .77(3) ? O7 H2 . .74(2) ? 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 O7 H1 O4 2_645 0.77(3) 2.20(3) 2.9045(17) 154(3) O7 H2 O1 1_455 0.74(2) 2.14(3) 2.8410(16) 158(2) O5 H3 O2 3_656 0.81(3) 2.09(3) 2.8387(15) 153(2) O5 H4 O7 . 0.82(2) 1.93(2) 2.7460(17) 176(2) O4 H5 O7 3_655 0.79(3) 1.96(3) 2.7354(17) 169(2)