#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:08:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179314 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/11/4321134.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_4321134
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_moiety         '(H4 N 1+)2, V2 P2 O14 H2 C2 2-, (H2 O)'
_chemical_formula_structural     '(N H4)2 (V O (H P O4))2 (C2 O4) (H2 O)'
_chemical_formula_sum            'C0.75 H6 N0.75 O6.38 P0.75 V0.75'
_chemical_formula_weight         189.00
_chemical_name_common            'Vanadium oxalatophosphate'
_chemical_name_systematic
;
 Diammoniumbis(vanadylhydrogenphosphate)oxalatehydrate
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 102.017(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   17.735(2)
_cell_length_b                   6.4180(6)
_cell_length_c                   22.839(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2542.6(4)
_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  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5185
_diffrn_reflns_theta_max         23.99
_diffrn_reflns_theta_min         1.82
_diffrn_standards_interval_count none
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs(Sheldrick, 1997)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.161
_refine_ls_goodness_of_fit_obs   1.478
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         1937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_restrained_S_obs      1.478
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_obs          0.0577
_refine_ls_shift/esd_max         0.335
_refine_ls_shift/esd_mean        0.073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0319P)²+20.4056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1383
_refine_ls_wR_factor_obs         0.1077
_reflns_number_observed          1043
_reflns_number_total             2123
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0000303_4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+20.4056P] 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^)+(0.0319P)^2^+20.4056P] 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        2542.7(4)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4321134
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'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.50094(9) 0.0000 0.31060(8) 0.0082(4) Uani 1 d S .
V2 V 0.33053(10) -0.5000 0.35536(8) 0.0154(5) Uani 1 d S .
V3 V 0.16400(11) 0.0000 0.02331(10) 0.0315(6) Uani 1 d S .
P1 P 0.3106(2) 0.0000 -0.04004(12) 0.0180(7) Uani 1 d S .
P2 P 0.47568(14) -0.5000 0.29234(13) 0.0143(6) Uani 1 d S .
P3 P 0.3560(2) 0.0000 0.37336(14) 0.0209(7) Uani 1 d S .
O1 O 0.6097(4) 0.0000 0.3856(3) 0.017(2) Uani 1 d S .
O2 O 0.2225(4) -0.5000 0.2807(4) 0.030(2) Uani 1 d S .
O3 O 0.3904(4) -0.5000 0.2916(3) 0.020(2) Uani 1 d S .
O4 O 0.4432(4) 0.0000 0.3763(3) 0.023(2) Uani 1 d S .
O5 O 0.2384(4) -0.5000 0.3984(4) 0.030(2) Uani 1 d S .
O6 O 0.5949(3) 0.0000 0.2684(3) 0.014(2) Uani 1 d S .
O7 O 0.5175(3) -0.3078(7) 0.3224(2) 0.0212(12) Uani 1 d . .
O8 O 0.4366(4) 0.0000 0.2495(3) 0.022(2) Uani 1 d S .
O9 O 0.3156(3) -0.8097(7) 0.3434(2) 0.0242(13) Uani 1 d . .
O10 O 0.3945(4) -0.5000 0.4152(4) 0.027(2) Uani 1 d S .
O11 O 0.4803(4) -0.5000 0.2241(3) 0.030(2) Uani 1 d S .
O12 O 0.3524(4) 0.0000 0.4427(4) 0.035(2) Uani 1 d S .
O13 O 0.0569(4) 0.0000 -0.0549(3) 0.020(2) Uani 1 d S .
O14 O 0.2231(4) 0.0000 -0.0420(3) 0.028(2) Uani 1 d S .
O15 O 0.0713(4) 0.0000 0.0651(4) 0.027(2) Uani 1 d S .
O16 O 0.1486(3) 0.3063(8) 0.0101(2) 0.0268(14) Uani 1 d . .
O17 O 0.2284(4) 0.0000 0.0824(4) 0.037(2) Uani 1 d S .
O18 O 0.3146(4) 0.0000 -0.1091(3) 0.032(2) Uani 1 d S .
C1 C 0.1628(6) -0.5000 0.2993(5) 0.017(3) Uani 1 d S .
C2 C 0.6687(6) 0.0000 0.3652(5) 0.017(2) Uani 1 d S .
C3 C -0.0061(6) 0.0000 -0.0366(4) 0.012(2) Uani 1 d S .
N1 N 0.0294(7) 0.2830(18) 0.4777(5) 0.044(5) Uani 0.64(2) d P .
N2 N 0.3614(8) 0.2751(19) 0.1451(7) 0.067(6) Uani 0.70(3) d P .
N3 N 0.3040(7) 0.2885(23) 0.1910(5) 0.053(6) Uani 0.62(2) d P .
N4 N 0.0705(9) 0.1339(27) 0.4482(7) 0.083(8) Uani 0.62(3) d P .
N5 N 0.4017(8) 0.1307(21) 0.1157(5) 0.060(6) Uani 0.65(2) d P .
N6 N 0.2594(8) 0.1163(21) 0.2162(6) 0.059(5) Uani 0.63(2) d P .
N7 N 0.1033(8) 0.1169(25) 0.1887(5) 0.070(6) Uani 0.65(2) d P .
N8 N 0.2280(8) 0.1319(24) 0.4835(7) 0.091(6) Uani 0.68(2) d P .
N9 N 0.5595(9) -0.1135(30) 0.1472(8) 0.107(10) Uani 0.64(2) d P .
N10 N 0.0023(15) 0.5000 0.0367(15) 0.046(12) Uani 0.34(3) d SP .
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'
C C 0.0033 0.0016 '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
O8 V1 O4 105.7(3) . . ?
O8 V1 O7 100.0(2) . . ?
O4 V1 O7 89.01(15) . . ?
O8 V1 O7 100.0(2) . 6 ?
O4 V1 O7 89.0(2) . 6 ?
O7 V1 O7 159.7(3) . 6 ?
O8 V1 O6 95.1(3) . . ?
O4 V1 O6 159.1(3) . . ?
O7 V1 O6 87.34(14) . . ?
O7 V1 O6 87.34(14) 6 . ?
O8 V1 O1 168.7(3) . . ?
O4 V1 O1 85.5(3) . . ?
O7 V1 O1 79.8(2) . . ?
O7 V1 O1 79.84(15) 6 . ?
O6 V1 O1 73.6(2) . . ?
O10 V2 O3 103.8(3) . . ?
O10 V2 O9 99.6(2) . . ?
O3 V2 O9 88.6(2) . . ?
O10 V2 O9 99.6(2) . 6_545 ?
O3 V2 O9 88.6(2) . 6_545 ?
O9 V2 O9 160.6(3) . 6_545 ?
O10 V2 O5 94.8(4) . . ?
O3 V2 O5 161.4(3) . . ?
O9 V2 O5 88.3(2) . . ?
O9 V2 O5 88.3(2) 6_545 . ?
O10 V2 O2 169.3(3) . . ?
O3 V2 O2 86.9(3) . . ?
O9 V2 O2 80.35(15) . . ?
O9 V2 O2 80.35(15) 6_545 . ?
O5 V2 O2 74.5(3) . . ?
O17 V3 O14 103.9(4) . . ?
O17 V3 O16 100.5(2) . . ?
O14 V3 O16 87.9(2) . . ?
O17 V3 O16 100.5(2) . 6 ?
O14 V3 O16 87.9(2) . 6 ?
O16 V3 O16 159.1(3) . 6 ?
O17 V3 O15 96.3(4) . . ?
O14 V3 O15 159.9(3) . . ?
O16 V3 O15 88.5(2) . . ?
O16 V3 O15 88.5(2) 6 . ?
O17 V3 O13 172.0(4) . . ?
O14 V3 O13 84.1(3) . . ?
O16 V3 O13 79.6(2) . . ?
O16 V3 O13 79.6(2) 6 . ?
O15 V3 O13 75.7(3) . . ?
O16 P1 O16 109.0(4) 7 4_545 ?
O16 P1 O14 113.1(3) 7 . ?
O16 P1 O14 113.1(3) 4_545 . ?
O16 P1 O18 109.2(3) 7 . ?
O16 P1 O18 109.2(3) 4_545 . ?
O14 P1 O18 102.8(4) . . ?
O3 P2 O7 113.4(2) . . ?
O3 P2 O7 113.4(2) . 6_545 ?
O7 P2 O7 107.8(4) . 6_545 ?
O3 P2 O11 104.3(4) . . ?
O7 P2 O11 108.9(3) . . ?
O7 P2 O11 108.9(3) 6_545 . ?
O9 P3 O9 108.3(4) 6_545 1_565 ?
O9 P3 O4 113.5(3) 6_545 . ?
O9 P3 O4 113.5(3) 1_565 . ?
O9 P3 O12 109.7(3) 6_545 . ?
O9 P3 O12 109.7(3) 1_565 . ?
O4 P3 O12 101.8(5) . . ?
C2 O1 V1 111.5(7) . . ?
C1 O2 V2 113.3(7) . . ?
P2 O3 V2 133.1(5) . . ?
P3 O4 V1 129.9(5) . . ?
C2 O5 V2 117.9(7) 3_445 . ?
C1 O6 V1 120.1(7) 3 . ?
P2 O7 V1 133.7(3) . . ?
P3 O9 V2 134.5(3) 1_545 . ?
C3 O13 V3 112.3(6) . . ?
P1 O14 V3 131.3(5) . . ?
C3 O15 V3 121.1(7) 5 . ?
P1 O16 V3 134.1(3) 7 . ?
O2 C1 O6 127.1(11) . 3_445 ?
O2 C1 C2 118.0(8) . 3_445 ?
O6 C1 C2 115.0(9) 3_445 3_445 ?
O1 C2 O5 123.7(10) . 3 ?
O1 C2 C1 119.9(9) . 3 ?
O5 C2 C1 116.4(8) 3 3 ?
O15 C3 O13 129.2(9) 5 . ?
O15 C3 C3 117.4(10) 5 5 ?
O13 C3 C3 113.4(11) . 5 ?
N4 N1 N1 138.7(7) . 2_556 ?
N5 N2 N3 142.3(13) . . ?
N6 N3 N2 130.6(12) . . ?
N1 N4 N4 131.3(7) . 6 ?
N2 N5 N5 130.7(8) . 6 ?
N6 N6 N3 135.9(7) 6 . ?
N8 N8 N8 147.5(9) 6 7_556 ?
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 O8 1.609(7) . ?
V1 O4 1.984(7) . ?
V1 O7 2.007(5) . ?
V1 O7 2.007(5) 6 ?
V1 O6 2.091(6) . ?
V1 O1 2.297(7) . ?
V2 O10 1.584(8) . ?
V2 O3 1.973(7) . ?
V2 O9 2.017(5) . ?
V2 O9 2.017(5) 6_545 ?
V2 O5 2.074(8) . ?
V2 O2 2.284(8) . ?
V3 O17 1.576(8) . ?
V3 O14 1.994(8) . ?
V3 O16 1.999(5) . ?
V3 O16 1.999(5) 6 ?
V3 O15 2.066(7) . ?
V3 O13 2.321(7) . ?
P1 O16 1.527(5) 7 ?
P1 O16 1.527(5) 4_545 ?
P1 O14 1.543(8) . ?
P1 O18 1.594(7) . ?
P2 O3 1.509(7) . ?
P2 O7 1.526(5) . ?
P2 O7 1.526(5) 6_545 ?
P2 O11 1.578(8) . ?
P3 O9 1.507(5) 6_545 ?
P3 O9 1.507(5) 1_565 ?
P3 O4 1.535(7) . ?
P3 O12 1.597(9) . ?
O1 C2 1.230(11) . ?
O2 C1 1.218(12) . ?
O5 C2 1.310(12) 3_445 ?
O6 C1 1.263(11) 3 ?
O9 P3 1.507(5) 1_545 ?
O13 C3 1.272(11) . ?
O15 C3 1.204(12) 5 ?
O16 P1 1.527(5) 7 ?
C1 O6 1.263(11) 3_445 ?
C1 C2 1.487(13) 3_445 ?
C2 O5 1.310(12) 3 ?
C2 C1 1.487(13) 3 ?
C3 O15 1.204(12) 5 ?
C3 C3 1.64(2) 5 ?
N1 N4 1.45(2) . ?
N1 N1 1.60(2) 2_556 ?
N2 N5 1.42(2) . ?
N2 N3 1.61(2) . ?
N3 N6 1.54(2) . ?
N4 N4 1.72(4) 6 ?
N5 N5 1.68(3) 6 ?
N6 N6 1.49(3) 6 ?
N7 N7 1.50(3) 6 ?
N8 N8 1.69(3) 6 ?
N8 N8 1.80(3) 7_556 ?
N9 N9 1.46(4) 6 ?
N10 N10 1.66(7) 5_565 ?
