A Vanadium(IV) Phosphite with a Pillared Layered Structure: Hydrothermal Synthesis and Characterization of (VO)4(4,4'-bpy)2(HPO3)4
Zhan Shi; Guanghua Li; Dong Zhang; Jia Hua; Shouhua Feng; Inorganic Chemistry 42 (2003) 2357–2361; doi:10.1021/ic0261676

data_4313435
_publ_contact_author
;
      Feng,Shouhua
      Department of Chemistry
      Jilin University
      Changchun, 130023
      P. R. China
;
_publ_contact_author_email       shfeng@mail.jlu.edu.cn
_publ_contact_author_fax         86-431-5671974
_publ_contact_author_phone       86-431-5671974
_publ_section_title
;
 A Vanadium(IV) Phosphite with a Pillared Layered Structure: Hydrothermal
 Synthesis and Characterization of (VO)4(4,4'-bpy)2(HPO3)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2357
_journal_page_last               2361
_journal_paper_doi               10.1021/ic0261676
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C20 H20 N4 O16 P4 V4'
_chemical_formula_weight         900.04
_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                 101.073(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.970(3)
_cell_length_b                   15.9400(13)
_cell_length_c                   10.7681(7)
_cell_measurement_temperature    293(2)
_cell_volume                     6059.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14502
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.334
_exptl_absorpt_correction_T_min  0.248?
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         4340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0782P)^2^+17.5877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1882
_reflns_number_gt                1933
_reflns_number_total             4340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0261676si20030101_083512.cif
_cod_data_source_block           c2c
_cod_original_cell_volume        6059.0(8)
_cod_database_code               4313435