Synthesis, Crystal Structure, and Solid State NMR Spectroscopy of NH4[(V2O3)2(4,4'-bpy)2(H2PO4)(PO4)2].0.5H2O, a Mixed-Valence Vanadium(IV,V) Phosphate with a Pillared Layer Structure
Ling-I Hung; Sue-Lein Wang; Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 41 (2002) 3929–3934; doi:10.1021/ic011277i

data_4318242
_publ_section_title
;
 Synthesis, Crystal Structure, and Solid State NMR Spectroscopy of
 NH4[(V2O3)2(4,4'-bpy)2(H2PO4)(PO4)2].0.5H2O, a Mixed-Valence
 Vanadium(IV,V) Phosphate with a Pillared Layer Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3929
_journal_page_last               3934
_journal_paper_doi               10.1021/ic011277i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety
'NH4[(V2O3)2(4,4'-bpy)2(H2PO4)(PO4)2].0.5H2O (bpy = bipyridine)'
_chemical_formula_sum            'C20 H23 N5 O18.5 P3 V4'
_chemical_formula_weight         926.10
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.7130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6354(8)
_cell_length_b                   9.9786(6)
_cell_length_c                   23.3689(14)
_cell_measurement_temperature    294(2)
_cell_volume                     2943.1(3)
_computing_molecular_graphics    'Diamond', 'SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Siemens Smart CCD'
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9271
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.00000(12)
_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_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          3.619
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+6.4434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                2594
_reflns_number_total             3544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011277i.cif
_cod_data_source_block           lyhm
_cod_original_formula_sum        'C20 H23 N5 O18.50 P3 V4'
_cod_database_code               4318242