Influence of reaction conditions on the electrochemical-hydrothermal synthesis of two ammonium vanadium phosphates: (NH4)2VO(HPO4)2·H2O and (NH4)2VO(V0.88P1.12O7)
Liu, Lumei; Wang, Xiqu; Bontchev, Ranko; Ross, Kent; Jacobson, Allan J.; Journal of Materials Chemistry 9 (1999) 1585–; doi:10.1039/a901956a

data_7213055
_publ_section_title
;
 Influence of reaction conditions on the electrochemical-hydrothermal
 synthesis of two ammonium vanadium phosphates: (NH4)2VO(HPO4)2&#x00B7;H2O
 and (NH4)2VO(V0.88P1.12O7)
;
_journal_issue                   7
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1585
_journal_paper_doi               10.1039/a901956a
_journal_volume                  9
_journal_year                    1999
_chemical_formula_sum            'H12 N2 O10 P2 V'
_chemical_formula_weight         313.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                73.472(2)
_cell_angle_beta                 80.085(2)
_cell_angle_gamma                85.077(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2499(8)
_cell_length_b                   8.1244(9)
_cell_length_c                   8.6529(9)
_cell_measurement_temperature    293(2)
_cell_volume                     480.94(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.1542
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3034
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    1.410
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_F_000             318
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.237
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.18(7)
_refine_ls_extinction_coef       0.0042(47)
_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   0.995
_refine_ls_goodness_of_fit_obs   1.096
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2509
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.995
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_obs          0.0797
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2045
_refine_ls_wR_factor_obs         0.1937
_reflns_number_observed          1867
_reflns_number_total             2509
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901956asup1.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+0.0000P] 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^)+(0.0980P)^2^+0.0000P] 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               7213055