
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_MIL-47
_database_code_depnum_ccdc_archive 'CCDC 166785'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H4 O5 V'
_chemical_formula_weight         231.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   6.8179(12)
_cell_length_b                   16.143(3)
_cell_length_c                   13.939(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1534.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1260
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      1.013
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_density_method    pycnometry
_exptl_crystal_F_000             460
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_correction_T_min  0.9387
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
'Blessing, Acta Cryst. (1995) A51 33-38'   
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6596
_diffrn_reflns_av_R_equivalents  0.2774
_diffrn_reflns_av_sigmaI/netI    0.1655
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         23.37
_reflns_number_total             1160
_reflns_number_gt                607
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond Brandenburg'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F², conventional R-factors R are based 
on F, with F set to zero for negative F². The threshold expression of 
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F² are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0180P)²+3.3757P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1160
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1799
_refine_ls_R_factor_gt           0.0766
_refine_ls_wR_factor_ref         0.1402
_refine_ls_wR_factor_gt          0.1098
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V V 0.2002(2) 0.2500 0.73916(13) 0.0229(6) Uani 1 2 d S . .
O1 O -0.0249(8) 0.2500 0.6916(4) 0.0194(16) Uani 1 2 d S . .
O2 O 0.3118(7) 0.1632(3) 0.6555(3) 0.0320(14) Uani 1 1 d . . .
O3 O 0.1415(6) 0.1626(3) 0.8335(3) 0.0336(14) Uani 1 1 d . . .
C1 C 0.3225(11) 0.0329(5) 0.5261(6) 0.049(3) Uani 1 1 d . . .
H1 H 0.2015 0.0554 0.5425 0.059 Uiso 1 1 calc R . .
C2 C 0.6675(11) 0.0323(5) 0.5369(6) 0.053(3) Uani 1 1 d . . .
H2 H 0.7830 0.0548 0.5611 0.064 Uiso 1 1 calc R . .
C3 C 0.4911(10) 0.0649(4) 0.5650(5) 0.0281(19) Uani 1 1 d . . .
C4 C 0.4781(12) 0.1366(4) 0.6333(5) 0.030(2) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V 0.0242(10) 0.0182(9) 0.0261(12) 0.000 0.0072(11) 0.000
O1 0.012(4) 0.021(4) 0.025(4) 0.000 -0.002(3) 0.000
O2 0.013(3) 0.037(3) 0.045(3) -0.022(3) 0.003(3) 0.008(3)
O3 0.024(3) 0.036(3) 0.041(4) 0.019(3) -0.001(3) -0.003(3)
C1 0.013(5) 0.063(6) 0.071(7) -0.050(5) 0.001(5) 0.005(5)
C2 0.018(5) 0.060(6) 0.082(7) -0.053(6) 0.007(5) -0.005(5)
C3 0.020(5) 0.023(4) 0.041(5) -0.022(4) 0.001(4) 0.001(4)
C4 0.034(5) 0.024(4) 0.031(5) -0.006(4) 0.006(4) -0.007(4)

_geom_special_details            
; 
All esds (except the esd in the dihedral angle between two l.s. planes) 
are estimated using the full covariance matrix.  The cell esds are taken 
into account individually in the estimation of esds in distances, angles 
and torsion angles; correlations between esds in cell parameters are only 
used when they are defined by crystal symmetry.  An approximate (isotropic) 
treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V O1 1.671(6) . ?
V O3 1.970(5) . ?
V O3 1.970(5) 7_565 ?
V O2 1.975(4) . ?
V O2 1.975(4) 7_565 ?
V O1 2.108(6) 6_657 ?
O1 V 2.108(6) 6_557 ?
O2 C4 1.251(7) . ?
O3 C4 1.277(8) 6_557 ?
C1 C3 1.371(9) . ?
C1 C2 1.373(9) 5_656 ?
C1 H1 0.9300 . ?
C2 C3 1.370(8) . ?
C2 C1 1.373(9) 5_656 ?
C2 H2 0.9300 . ?
C3 C4 1.502(8) . ?
C4 O3 1.277(7) 6_657 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V O3 94.49(19) . . ?
O1 V O3 94.49(19) . 7_565 ?
O3 V O3 91.5(3) . 7_565 ?
O1 V O2 96.9(2) . . ?
O3 V O2 87.93(18) . . ?
O3 V O2 168.6(2) 7_565 . ?
O1 V O2 96.9(2) . 7_565 ?
O3 V O2 168.6(2) . 7_565 ?
O3 V O2 87.93(18) 7_565 7_565 ?
O2 V O2 90.4(3) . 7_565 ?
O1 V O1 176.12(18) . 6_657 ?
O3 V O1 82.82(18) . 6_657 ?
O3 V O1 82.82(18) 7_565 6_657 ?
O2 V O1 85.84(17) . 6_657 ?
O2 V O1 85.84(17) 7_565 6_657 ?
V O1 V 129.4(3) . 6_557 ?
C4 O2 V 137.6(5) . . ?
C4 O3 V 130.8(4) 6_557 . ?
C3 C1 C2 120.0(7) . 5_656 ?
C3 C1 H1 120.0 . . ?
C2 C1 H1 120.0 5_656 . ?
C3 C2 C1 121.4(7) . 5_656 ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 5_656 . ?
C2 C3 C1 118.6(6) . . ?
C2 C3 C4 121.9(7) . . ?
C1 C3 C4 119.4(7) . . ?
O2 C4 O3 126.0(7) . 6_657 ?
O2 C4 C3 118.4(7) . . ?
O3 C4 C3 115.5(7) 6_657 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        23.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.102
#===END  


