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_4305736
_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, C12 H28 F O18 P4 V4'
_chemical_formula_sum            'C36 H48 F O18 P5 V4'
_chemical_formula_weight         1146.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.421(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.413(2)
_cell_length_b                   17.694(2)
_cell_length_c                   16.559(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      14
_cell_volume                     4729.6(10)
_computing_cell_refinement       'STADI4-1.06 (Stoe & Cie, 1997)'
_computing_data_collection       'STADI4-1.06 (Stoe & Cie, 1997)'
_computing_data_reduction        'XRED1.08 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Stoe STADI4 diffractometer'
_diffrn_measurement_method       2\Q/\w-scan,ratio=1.0,width(\w)=1.35-1.5\%
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13219
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.6884
_exptl_absorpt_correction_T_min  0.5385
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 North,A.C.T., Phillips,D.C., Mathwes,F.S. (1968). Acta Cryst. A24, 351-359.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    no
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.836
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00170(6)
_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   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         10843
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+15.7506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                8678
_reflns_number_total             10843
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic800707v_si_001_3.cif
_cod_data_source_block           Ph4P{[(V2O3)2][iPrPO3]4F}
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4305736