New Directions in the Preparation and Redox Chemistry of Fluoride-Templated Tetranuclear Vanadium Phosphonate Cage Compounds, Mn+[(V2O3)2(RPO3)4@F]n
Jabor K. Jabor; Reinhard Stösser; Michael Feist; Petra Neubauer; Manfred Meisel; Inorganic Chemistry 47 (2008) 9293–9302; doi:10.1021/ic800707v

data_4305735
_publ_contact_author_address
;Leibniz-Institut f\"ur Katalyse e. V.
an der Universit\"at Rostock
Branch Berlin (former ACA)
P.O.Box 96 11 56
D-12474 Berlin
;
_publ_contact_author_email       jabor.jabor@catalysis.de
_publ_contact_author_fax         '49 (0)30 6392 4454'
_publ_contact_author_name        'Jabor K. Jabor'
_publ_contact_author_phone       '49 (0)30 6392 4240'
_publ_section_title
;
New Directions in the Preparation and Redox Chemistry of Fluoride-Templated
Tetranuclear Vanadium Phosphonate Cage Compounds, Mn+[(V2O3)2(RPO3)4@F]n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9293
_journal_page_last               9302
_journal_paper_doi               10.1021/ic800707v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C24 H20 P, C4 H12 F O18 P4 V4, 2(C2 H3 N)'
_chemical_formula_sum            'C32 H38 F N2 O18 P5 V4'
_chemical_formula_weight         1116.25
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 94.236(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1308(12)
_cell_length_b                   7.9238(6)
_cell_length_c                   17.2634(17)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      14
_cell_volume                     2200.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5238
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.7513
_exptl_absorpt_correction_T_min  0.5263
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0009(2)
_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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0346P)^2^+2.0099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                3565
_reflns_number_total             4091
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic800707v_si_001_2.cif
_cod_data_source_block           Ph4P[(V2O3)2(MePO3)4F]2CH3CN
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4305735