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_4321188
_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            'C45 H35 N9 O21 V8'
_chemical_formula_weight         1445.34
_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                69.5840(10)
_cell_angle_beta                 71.2040(10)
_cell_angle_gamma                84.6400(10)
_cell_formula_units_Z            2
_cell_length_a                   12.2071(7)
_cell_length_b                   13.8855(8)
_cell_length_c                   16.9832(10)
_cell_measurement_temperature    96(2)
_cell_volume                     2553.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11967
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.488
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.307
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         7311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.400
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+3.0885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                5833
_reflns_number_total             7311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991473d_1.cif
_cod_data_source_block           Pam140
_cod_database_code               4321188