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_4305734
_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, C24 H20 F O18 P4 V4, C2 H3 N'
_chemical_formula_sum            'C50 H43 F N O18 P5 V4'
_chemical_formula_weight         1323.46
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            4
_cell_length_a                   19.794(7)
_cell_length_b                   14.692(4)
_cell_length_c                   18.587(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      5
_cell_volume                     5405(3)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (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_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-rotation,\f-incr.=1.4\%,157 exposures'
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35186
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  0.7157
_exptl_absorpt_correction_T_min  0.5342
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The program XSHAPE1.02 (Stoe, 1997) was used for crystal optimisation
before the numerical absorption correction basing on a Gaussian algorithsm
and implemented in XRED1.08 (Stoe, 1997) was applied.
In XSHAPE 150 strong reflections with 4 symmetry equivalents in each case
were used for that optimisation. XSHAPE bases on the program HABITUS 
(Herrendorf, W. (1993). PhD thesis. Universit\"at Karlsruhe, Germany).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(11)
_refine_ls_extinction_coef       0.00015(8)
_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   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         9760
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                8573
_reflns_number_total             9760
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic800707v_si_001_1.cif
_cod_data_source_block           Ph4P[(V2O3)2(PhPO3)4F]CH3CN
_cod_database_code               4305734