Novel Oxovanadium Phosphate Tubule Incorporating 2,2-Bipyridine Ligands: Hydrothermal Synthesis and Crystal Structure of [(VIVO)3(μ5-PO4)2(2,2'-bpy)(μ-OH2)].1/3H2O
Wenbin Yang; Canzhong Lu; Inorganic Chemistry 41 (2002) 5638–5640; doi:10.1021/ic0257874

data_4318793
_publ_contact_author_address
;
     Fujian Institute of Research  
        on the Structure of Matter,
        Chinese Academy of Sciences,
        Fuzhou, Fujian 350002, 
    P.R.China
;
_publ_contact_author_email       czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax         0086-0591-3714946
_publ_contact_author_name        'Dr. Canzhong Lu'
_publ_contact_author_phone       0591-3711368-2148
_publ_section_title
;
 Novel Oxovanadium Phosphate Tubule Incorporating 2,2-Bipyridine Ligands:
 Hydrothermal Synthesis and Crystal Structure of
 [(VIVO)3(\m5-PO4)2(2,2'-bpy)(\m-OH2)].1/3H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5638
_journal_page_last               5640
_journal_paper_doi               10.1021/ic0257874
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C10 H10.67 N2 O12.33 P2 V3'
_chemical_formula_weight         570.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   29.7600(3)
_cell_length_b                   29.7600(3)
_cell_length_c                   9.5745(2)
_cell_measurement_temperature    293(2)
_cell_volume                     7343.66(19)
_computing_cell_refinement       'Simens CCD SAINT'
_computing_data_collection       'Simens SMART CCD'
_computing_data_reduction        'Simens CCD SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens CCD SMART'
_diffrn_measurement_method       omega-scan
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8422
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.854539
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'sapphire blue'
_exptl_crystal_density_diffrn    2.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexangular columns'
_exptl_crystal_F_000             5082
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.00074(7)
_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   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+27.7409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                2426
_reflns_number_total             2882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0257874_s2.cif
_cod_data_source_block           V3P2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4318793