A Hydrothermal Investigation of the 1/2V~2~O~5~-H~2~C~2~O~4~ / H~3~PO~4~ / NH~4~OH System: Synthesis and Structures of (NH~4~)VOPO~4~1.5H~2~O, (NH~4~) (NH~4~)~0.5~VOPO~4~1.5H~2~O, (NH~4~)~2~[VO(H~2~O)~3~]~2~[VO(H~2~O)][VO(PO~4~)~2~]~2~3H~2~O, and (NH~4~)~2~[VO(HPO~4~)]~2~(C~2~O~4~)H~2~O
Junghwan Do; Ranko P. Bontchev; Allan J. Jacobson; Inorganic Chemistry 39 (2000) 3230–3237; doi:10.1021/ic0000303

data_4321133
_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 1/2V~2~O~5~-H~2~C~2~O~4~ / H~3~PO~4~
 / NH~4~OH System: Synthesis and Structures of (NH~4~)VOPO~4~1.5H~2~O,
 (NH~4~) (NH~4~)~0.5~VOPO~4~1.5H~2~O,
 (NH~4~)~2~[VO(H~2~O)~3~]~2~[VO(H~2~O)][VO(PO~4~)~2~]~2~3H~2~O, and
 (NH~4~)~2~[VO(HPO~4~)]~2~(C~2~O~4~)H~2~O
;
_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, V5 P4 O28 H14 2-, 3(H2 O)' 
;
_chemical_formula_structural
;
'(N H4)2 (V O (H2 O)3)2 (V O (H2 O)) (V O (P O4)2)2 (H2 O)3' 
;
_chemical_formula_sum            'H28 N2 O31 P4 V5'
_chemical_formula_weight         930.82
_chemical_name_common            'Vanadium phosphate'
_chemical_name_systematic
; 
 Diammoniumbis(triaquovanadyl)aquovanadylbis(vanadyldiphosphate)
 trihydrate'
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                69.041(2)
_cell_angle_beta                 65.653(2)
_cell_angle_gamma                87.789(2)
_cell_formula_units_Z            10
_cell_length_a                   10.2523(9)
_cell_length_b                   12.2626(11)
_cell_length_c                   12.3615(11)
_cell_measurement_reflns_used    2
_cell_measurement_temperature    293(2)
_cell_volume                     1311.3(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SANIT
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'MS-DOS 6.22 EDITOR'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5756
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.79
_diffrn_standards_interval_count none
_exptl_absorpt_coefficient_mu    2.082
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs(Sheldrick, 1997)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.0026(3)
_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_all   1.149
_refine_ls_goodness_of_fit_obs   1.277
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_restrained_S_obs      1.277
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_obs          0.0715
_refine_ls_shift/esd_max         0.108
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+23.1606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1767
_refine_ls_wR_factor_obs         0.1592
_reflns_number_observed          2699
_reflns_number_total             3642
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0000303_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+23.1606P] 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^)+(0.0283P)^2^+23.1606P] 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               4321133