The first three-dimensional vanadium hypophosphite
Maouel, Hind A.; Alonzo, Véronique; Roisnel, Thierry; Rebbah, Houria; Le Fur, Eric; Acta Crystallographica Section C 65 (2009) i36–i38; doi:10.1107/S0108270109021325

data_2017180
_publ_section_title
;
 The first three-dimensional vanadium hypophosphite
;
_journal_coeditor_code           FN3018
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i36
_journal_page_last               i38
_journal_paper_doi               10.1107/S0108270109021325
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'V (H2 P O2)3'
_chemical_formula_moiety         'H12 O12 P6 V2'
_chemical_formula_sum            'H12 O12 P6 V2'
_chemical_formula_weight         491.8
_chemical_name_systematic
;
vanadium hypophosphite
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.807(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4985(3)
_cell_length_b                   11.7771(5)
_cell_length_c                   11.5999(4)
_cell_measurement_reflns_used    9018
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     1547.89(9)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1166
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20258
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.56
_exptl_absorpt_coefficient_mu    1.875
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.11
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.542
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '(SHELXL97; Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+4.0183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                2426
_reflns_number_total             3550
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3018.cif
_cod_data_source_block           I
_cod_database_code               2017180
_cod_database_fobs_code          2017180