Synthesis and characterizations of the first [V16O39Cl]6- (V16O39) polyanion.
Xiao, Li-Na; Xu, Jia-Ning; Hu, Yang-Yang; Wang, La-Mei; Wang, Yan; Ding, Hong; Cui, Xiao-Bing; Xu, Ji-Qing; Dalton transactions (Cambridge, England : 2003) 42 (2013) 5247–5251; doi:10.1039/c3dt33081h

data_7021252
_publ_section_title
;
 Synthesis and characterizations of the first [V16O39Cl]6- (V16O39)
 polyanion.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5247
_journal_page_last               5251
_journal_paper_doi               10.1039/c3dt33081h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C108 H87 Cl Fe3 N18 O46.5 V16'
_chemical_formula_weight         3399.00
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.86(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.042(4)
_cell_length_b                   18.473(4)
_cell_length_c                   37.762(8)
_cell_measurement_temperature    293(2)
_cell_volume                     12570(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.1275
_diffrn_reflns_av_sigmaI/netI    0.1746
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            62423
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    1.575
_exptl_absorpt_correction_T_max  0.6244
_exptl_absorpt_correction_T_min  0.5507
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6784
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         4.419
_refine_diff_density_min         -2.533
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.00006(3)
_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   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1739
_refine_ls_number_reflns         22129
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.2085
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1347P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2748
_reflns_number_gt                9155
_reflns_number_total             22129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt33081h.txt
_cod_data_source_block           k
_cod_depositor_comments          'Adding full bibliography for 7021252.cif.'
_cod_original_cell_volume        12571(4)
_cod_original_sg_symbol_H-M      p2(1)/c
_cod_original_formula_sum        'C108 H87 Cl Fe3 N18 O46.50 V16'
_cod_database_code               7021252