Structural influences of organonitrogen ligands on vanadium oxide solids. Hydrothermal syntheses and structures of the terpyridine vanadates [V2O4(terpy)(2)](3)[V10O28], [VO2(terpy)][V4O10], and [V9O22(terpy)(3)]
Pamela J. Hagrman; Jon Zubieta; Inorganic Chemistry 39 (2000) 3252–3260; doi:10.1021/ic991473d

data_6000498
_publ_section_title
;
 Structural influences of organonitrogen ligands on vanadium oxide solids.
 Hydrothermal syntheses and structures of the terpyridine vanadates
 [V2O4(terpy)(2)](3)[V10O28], [VO2(terpy)][V4O10], and [V9O22(terpy)(3)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3252
_journal_page_last               3260
_journal_paper_doi               10.1021/ic991473d
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C15 H11 N3 O12 V5'
_chemical_formula_weight         679.97
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.000
_cell_angle_beta                 92.2860(10)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   7.77710(10)
_cell_length_b                   10.3595(2)
_cell_length_c                   25.7150(4)
_cell_measurement_temperature    96(2)
_cell_volume                     2070.13(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12687
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    2.247
_exptl_crystal_colour            Dark_blue
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+7.5623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                4070
_reflns_number_total             4866
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               6000498