#------------------------------------------------------------------------------
#$Date: 2016-02-09 20:42:54 +0200 (Tue, 09 Feb 2016) $
#$Revision: 176292 $
#$URL: svn://www.crystallography.net/cod/cif/6/00/04/6000494.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_6000494
loop_
_publ_author_name
'Junghwan Do'
'Ranko P. Bontchev'
'Allan J. Jacobson'
_publ_contact_author_email       ajjacob@uh.edu
_publ_contact_author_fax         '713 743 2787'
_publ_contact_author_phone       '713 743 2785'
_publ_section_title
;
 A Hydrothermal Investigation of the 1/2V₂O₅-H₂C₂O₄ 
 / H₃PO₄ / NH₄OH System: Synthesis and Structures of 
 (NH₄)VOPO₄1.5H₂O, (NH₄) (NH₄)~0.5~VOPO₄1.5H₂O,
 (NH₄)₂[VO(H₂O)₃]₂[VO(H₂O)][VO(PO₄)₂]₂3H₂O, 
 and (NH₄)₂[VO(HPO₄)]₂(C₂O₄)H₂O 
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3230
_journal_page_last               3237
_journal_paper_doi               10.1021/ic0000303
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'H5 N0.5 O6.5 P V'
_chemical_formula_weight         197.96
_chemical_name_common            'Vanadium phosphate'
_chemical_name_systematic
;
Hemiammoniumvanadyl(IV, V)phosphatesesquihydrate
;
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.000
_cell_angle_beta                 105.3470(10)
_cell_angle_gamma                90.000
_cell_formula_units_Z            8
_cell_length_a                   6.9669(6)
_cell_length_b                   17.6627(15)
_cell_length_c                   8.9304(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1059.7(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'MS-DOS 6.22 EDITOR'
_computing_structure_refinement  'SHELXTL 5.03'
_computing_structure_solution    'SHELXTL 5.03'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_method       'Siemens SMART CCD diffractometer'
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4778
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.31
_diffrn_standards_interval_count none
_exptl_absorpt_coefficient_mu    2.140
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.337
_refine_ls_goodness_of_fit_obs   1.368
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         1573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.337
_refine_ls_restrained_S_obs      1.368
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_obs          0.0582
_refine_ls_shift/esd_max         -1.915
_refine_ls_shift/esd_mean        0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+17.7853P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1360
_refine_ls_wR_factor_obs         0.1349
_reflns_number_observed          1489
_reflns_number_total             1573
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+17.7853P] 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^)+(0.0000P)^2^+17.7853P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               6000494
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_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_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V1 V 0.3420(3) 0.7500 0.7149(2) 0.0098(5) Uani 1 d S .
V2 V 0.5204(3) 0.7500 1.2587(2) 0.0091(5) Uani 1 d S .
V3 V 0.4129(2) 0.49538(8) 1.2269(2) 0.0078(4) Uani 1 d . .
P1 P 0.5526(3) 0.37649(12) 1.5124(2) 0.0078(5) Uani 1 d . .
P2 P 0.4345(3) 0.62421(12) 0.9855(2) 0.0080(5) Uani 1 d . .
O1 O 0.2881(8) 0.6693(3) 0.8610(6) 0.0127(13) Uani 1 d . .
O2 O 0.2983(8) 0.6691(3) 0.5487(6) 0.0116(12) Uani 1 d . .
O3 O 0.5548(8) 0.6760(3) 1.1172(6) 0.0121(13) Uani 1 d . .
O4 O 0.8629(13) 0.7500 1.3206(11) 0.013(2) Uani 1 d S .
O5 O 0.5824(8) 0.6749(3) 1.4186(6) 0.0123(13) Uani 1 d . .
O6 O 0.3124(8) 0.5662(3) 1.0533(6) 0.0116(13) Uani 1 d . .
O7 O 0.4066(8) 0.4198(3) 1.3844(6) 0.0143(13) Uani 1 d . .
O8 O 0.4065(8) 0.4153(3) 1.0755(6) 0.0120(13) Uani 1 d . .
O9 O 0.3264(8) 0.5693(3) 1.3612(6) 0.0130(13) Uani 1 d . .
O10 O 0.0691(16) 0.4643(5) 1.1662(10) 0.026(2) Uani 1 d . .
O11 O -0.0004(17) 0.7500 0.6344(18) 0.025(3) Uani 1 d S .
O12 O 0.5807(13) 0.7500 0.7651(10) 0.022(2) Uani 1 d S .
O13 O 0.2877(12) 0.7500 1.2246(10) 0.019(2) Uani 1 d S .
O14 O 0.6431(8) 0.5134(4) 1.2687(7) 0.0191(14) Uani 1 d . .
NH4 N -0.0246(26) 0.5790(9) 0.5534(22) 0.036(3) Uani 1 d . .
OW1 O 0.9545(17) 0.6142(8) 1.2161(16) 0.043(5) Uiso 0.66(3) d P .
OW2 O 0.9448(24) 0.7028(10) 0.9597(19) 0.050(7) Uiso 0.51(3) d P .
OW3 O 0.9606(21) 0.6452(9) 1.1305(20) 0.042(7) Uiso 0.53(3) d P .
H1 H 0.8935(114) 0.7149(48) 1.2792(93) 0.000(21) Uiso 1 d . .
H2 H -0.0529(150) 0.4644(48) 1.1164(100) 0.005(23) Uiso 1 d . .
H3 H 0.1241(213) 0.4664(94) 1.1483(175) 0.023(61) Uiso 1 d . .
H4 H 0.9643(238) 0.7500 1.5707(184) 0.009(59) Uiso 1 d S .
H5 H -0.0846(299) 0.7500 0.6707(224) 0.051(70) Uiso 1 d S .
H6 H 0.0829(149) 0.6006(52) 0.5631(98) 0.007(24) Uiso 1 d . .
H7 H -0.1112(151) 0.5858(60) 0.5085(127) 0.001(33) Uiso 1 d . .
H8 H -0.0216(203) 0.5656(72) 0.5010(139) 0.000(48) Uiso 1 d . .
H9 H -0.0546(156) 0.7500 0.9996(132) 0.000(27) Uiso 1 d S .
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'
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 V1 O2 98.5(3) . . ?
O12 V1 O2 98.5(3) . 4_575 ?
O2 V1 O2 89.8(3) . 4_575 ?
O12 V1 O1 100.1(3) . . ?
O2 V1 O1 87.6(2) . . ?
O2 V1 O1 161.4(2) 4_575 . ?
O12 V1 O1 100.1(3) . 4_575 ?
O2 V1 O1 161.4(2) . 4_575 ?
O2 V1 O1 87.6(2) 4_575 4_575 ?
O1 V1 O1 89.0(3) . 4_575 ?
O12 V1 O11 178.1(5) . . ?
O2 V1 O11 80.1(3) . . ?
O2 V1 O11 80.1(3) 4_575 . ?
O1 V1 O11 81.3(3) . . ?
O1 V1 O11 81.3(3) 4_575 . ?
O13 V2 O3 100.3(3) . . ?
O13 V2 O3 100.3(3) . 4_575 ?
O3 V2 O3 88.3(3) . 4_575 ?
O13 V2 O5 99.3(3) . 4_575 ?
O3 V2 O5 160.4(3) . 4_575 ?
O3 V2 O5 88.6(2) 4_575 4_575 ?
O13 V2 O5 99.3(3) . . ?
O3 V2 O5 88.6(2) . . ?
O3 V2 O5 160.4(3) 4_575 . ?
O5 V2 O5 87.9(3) 4_575 . ?
O13 V2 O4 177.4(4) . . ?
O3 V2 O4 81.5(2) . . ?
O3 V2 O4 81.5(2) 4_575 . ?
O5 V2 O4 78.8(2) 4_575 . ?
O5 V2 O4 78.8(2) . . ?
O14 V3 O8 98.4(3) . . ?
O14 V3 O7 100.6(3) . . ?
O8 V3 O7 90.2(2) . . ?
O14 V3 O6 100.7(3) . . ?
O8 V3 O6 88.6(2) . . ?
O7 V3 O6 158.7(2) . . ?
O14 V3 O9 100.2(3) . . ?
O8 V3 O9 161.4(2) . . ?
O7 V3 O9 86.9(2) . . ?
O6 V3 O9 87.5(2) . . ?
O14 V3 O10 178.2(3) . . ?
O8 V3 O10 80.6(3) . . ?
O7 V3 O10 78.0(3) . . ?
O6 V3 O10 80.8(3) . . ?
O9 V3 O10 80.8(3) . . ?
O7 P1 O2 112.4(3) . 3_667 ?
O7 P1 O5 103.8(3) . 3_668 ?
O2 P1 O5 112.1(3) 3_667 3_668 ?
O7 P1 O9 111.3(3) . 3_668 ?
O2 P1 O9 107.3(3) 3_667 3_668 ?
O5 P1 O9 110.0(3) 3_668 3_668 ?
O1 P2 O8 112.8(3) . 3_667 ?
O1 P2 O3 111.7(3) . . ?
O8 P2 O3 104.1(3) 3_667 . ?
O1 P2 O6 107.5(3) . . ?
O8 P2 O6 111.1(3) 3_667 . ?
O3 P2 O6 109.6(3) . . ?
P2 O1 V1 129.4(3) . . ?
P1 O2 V1 130.6(3) 3_667 . ?
P2 O3 V2 141.5(4) . . ?
P1 O5 V2 131.5(3) 3_668 . ?
P2 O6 V3 127.5(3) . . ?
P1 O7 V3 138.5(4) . . ?
P2 O8 V3 133.9(3) 3_667 . ?
P1 O9 V3 131.2(3) 3_668 . ?
OW2 OW2 OW3 124.1(7) 4_575 . ?
OW1 OW3 OW2 174.1(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O12 1.604(9) . ?
V1 O2 2.024(5) . ?
V1 O2 2.024(5) 4_575 ?
V1 O1 2.033(5) . ?
V1 O1 2.033(5) 4_575 ?
V1 O11 2.302(12) . ?
V2 O13 1.568(9) . ?
V2 O3 1.877(5) . ?
V2 O3 1.877(5) 4_575 ?
V2 O5 1.913(6) 4_575 ?
V2 O5 1.913(6) . ?
V2 O4 2.302(9) . ?
V3 O14 1.580(6) . ?
V3 O8 1.948(6) . ?
V3 O7 1.948(6) . ?
V3 O6 1.971(6) . ?
V3 O9 1.972(6) . ?
V3 O10 2.376(11) . ?
P1 O7 1.520(6) . ?
P1 O2 1.524(6) 3_667 ?
P1 O5 1.547(6) 3_668 ?
P1 O9 1.549(6) 3_668 ?
P2 O1 1.520(6) . ?
P2 O8 1.528(6) 3_667 ?
P2 O3 1.550(6) . ?
P2 O6 1.553(6) . ?
O2 P1 1.524(6) 3_667 ?
O5 P1 1.547(6) 3_668 ?
O8 P2 1.528(6) 3_667 ?
O9 P1 1.549(6) 3_668 ?
OW1 OW3 0.95(2) . ?
OW2 OW2 1.67(4) 4_575 ?
OW2 OW3 1.81(3) . ?
