Novel Vanadium(V) Compounds with a Layer Structure: Synthesis, Crystal Structures, and Solid State NMR Spectroscopy of [(VO2)2(4,4'-bpy)0.5(4,4'-Hbpy)(XO4)].H2O (X = P and As)
Li-Hsun Huang; Hsien-Ming Kao; Kwang-Hwa Lii; Inorganic Chemistry 41 (2002) 2936–2940; doi:10.1021/ic0111841

data_4318015
_publ_section_title
;
 Novel Vanadium(V) Compounds with a Layer Structure: Synthesis, Crystal
 Structures, and Solid State NMR Spectroscopy of
 [(VO2)2(4,4'-bpy)0.5(4,4'-Hbpy)(XO4)].H2O (X = P and As)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2936
_journal_page_last               2940
_journal_paper_doi               10.1021/ic0111841
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '[(VO2)2(4,4'-bpy)0.5(4,4'-Hbpy)(PO4)].H2O'
_chemical_formula_sum            'C15 H15 N3 O9 P V2'
_chemical_formula_weight         514.15
_chemical_name_systematic
;
  ?
;
_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-97
_cell_angle_alpha                113.4652(7)
_cell_angle_beta                 95.7231(7)
_cell_angle_gamma                94.4447(7)
_cell_formula_units_Z            2
_cell_length_a                   7.9063(3)
_cell_length_b                   10.2201(4)
_cell_length_c                   12.1336(5)
_cell_measurement_temperature    294(2)
_cell_volume                     887.46(6)
_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 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9430
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   'empirical based on symmetry equivalents'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.924
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0000(6)
_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   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.9049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                3671
_reflns_number_total             4209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0111841_1.cif
_cod_data_source_block           4044all
_cod_database_code               4318015