Synthesis, crystal structure of the ammonium vanadyl oxalatophosphite and its controlled conversion into catalytic vanadyl phosphates
C. Kouvatas; V. Alonzo; T. Bataille; L. Le Polles; C. Roiland; G. Louarn; E. Le Fur; Journal of Solid State Chemistry 253 (2017) 73–77; doi:10.1016/j.jssc.2017.05.026

data_1549272
_publ_section_title
;
 Synthesis, crystal structure of the ammonium vanadyl oxalatophosphite and
 its controlled conversion into catalytic vanadyl phosphates
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              73
_journal_page_last               77
_journal_paper_doi               10.1016/j.jssc.2017.05.026
_journal_volume                  253
_journal_year                    2017
_chemical_formula_sum            'C H7.89 N O7.45 P V'
_chemical_formula_weight         235.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                67.260(4)
_cell_angle_beta                 72.927(4)
_cell_angle_gamma                85.848(3)
_cell_formula_units_Z            2
_cell_length_a                   6.3844(4)
_cell_length_b                   7.2278(4)
_cell_length_c                   9.2965(5)
_cell_measurement_reflns_used    4920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     377.80(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4605
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.031
_diffrn_reflns_theta_min         3.541
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.8613
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_description       prism
_exptl_crystal_F_000             238
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2122
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.3820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1766
_reflns_number_total             2122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2017-253-73-77.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_journal_paper_doi' value
'https://doi.org/10.1016/j.jssc.2017.05.026' was changed to
'10.1016/j.jssc.2017.05.026'.

Automatic conversion script
Id: cif_fix_values 6433 2018-09-21 13:16:33Z andrius 
;
_cod_original_formula_sum        'C1 H7.89 N1 O7.45 P1 V1'
_cod_database_code               1549272
_shelx_res_checksum              19711
_shelx_hkl_checksum              6787