Hydrothermal Synthesis of the First Vanadomolybdenum Polyoxocation with a "Metal-Bonded" Spherical Framework
Wenbin Yang; Canzhong Lu; Xiaoping Zhan; Honghui Zhuang; Inorganic Chemistry 41 (2002) 4621–4623; doi:10.1021/ic025679h

data_4318481
_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       0086-0591-3705794
_publ_section_title
;
 Hydrothermal Synthesis of the First Vanadomolybdenum Polyoxocation with a
 "Metal-Bonded" Spherical Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4621
_journal_page_last               4623
_journal_paper_doi               10.1021/ic025679h
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'H31 Mo12 O66 V7'
_chemical_formula_weight         2595.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           128
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.7305(18)
_cell_length_b                   12.7305(18)
_cell_length_c                   17.788(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2882.8(9)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1478
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    3.716
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.556343
_exptl_crystal_colour            deep-violet
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.761
_refine_diff_density_min         -2.146
_refine_diff_density_rms         0.297
_refine_ls_extinction_coef       0.0017(4)
_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   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0686
_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^)+(0.1495P)^2^+19.2040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2265
_reflns_number_gt                1204
_reflns_number_total             1478
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025679h_s2.cif
_cod_data_source_block           Mo12V7
_cod_original_cell_volume        2882.8(8)
_cod_database_code               4318481