#------------------------------------------------------------------------------
#$Date: 2008-03-16 14:50:27 +0200 (Sun, 16 Mar 2008) $
#$Revision: 279 $
#$URL: file:///home/coder/svn-repositories/cod/cif/5/5000405.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_5000405
## 'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_chemical_formula_sum          'C42.56 H103.84 N6.28 O36 V15'
_chemical_formula_moiety '5(C8 H20 N 1+), O36 V15 5-, 1.28(C2 H3 N)'
_chemical_formula_weight                            2043.92
_cell_length_a                                    22.105(3)
_cell_length_b                                  13.7840(19)
_cell_length_c                                    26.604(4)
_cell_angle_alpha                                        90
_cell_angle_beta                                 107.560(7)
_cell_angle_gamma                                        90
_cell_volume                                     7728.4(18)
_cell_formula_units_Z                                     4
_cell_measurement_reflns_used                           132
_cell_measurement_theta_min                            10.8
_cell_measurement_theta_max                           15.77
_cell_measurement_temperature                           101
_exptl_crystal_colour                   Black
_exptl_crystal_description              needle
_exptl_crystal_size_max                                 .56
_exptl_crystal_size_mid                                 .16
_exptl_crystal_size_min                                 .14
_exptl_crystal_density_diffrn                         1.757
_exptl_crystal_density_meas             ?
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                                   4143
_exptl_absorpt_coefficient_mu                        1.8029
_exptl_absorpt_correction_type          analytical
_exptl_absorpt_process_details          Tompa
_exptl_absorpt_correction_T_min                       0.714
_exptl_absorpt_correction_T_max                       0.815
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'C 2/c'
loop_
_symmetry_equiv_pos_as_xyz
              x,y,z
      1/2+x,1/2+y,z
         -x,y,1/2-z
  1/2-x,1/2+y,1/2-z
         x,-y,1/2+z
  1/2+x,1/2-y,1/2+z
           -x,-y,-z
     1/2-x,1/2-y,-z
_diffrn_radiation_type                  'Mo K\a'
_diffrn_radiation_wavelength                        0.71069
_diffrn_ambient_temperature                             101
_diffrn_measurement_device_type         'refurbished Picker diffractometer'
_diffrn_measurement_method              '\q/2\q scans'
_diffrn_detector_area_resol_mean        ?
_diffrn_reflns_number                                 13681
_diffrn_reflns_av_R_equivalents                       0.064
_diffrn_reflns_theta_min                                  3
_diffrn_reflns_theta_max                                 25
_diffrn_reflns_theta_full                                25
_diffrn_measured_fraction_theta_max                       1
_diffrn_measured_fraction_theta_full                      1
_diffrn_reflns_limit_h_min              -26
_diffrn_reflns_limit_h_max               26
_diffrn_reflns_limit_k_min               -3
_diffrn_reflns_limit_k_max               16
_diffrn_reflns_limit_l_min              -31
_diffrn_reflns_limit_l_max               31
_diffrn_standards_number                                  4
_diffrn_standards_decay_%                               0.9
_diffrn_standards_interval_count                        300
_reflns_number_total                                   6847
_reflns_number_gt                                      4190
_reflns_threshold_expression            F^2^>2.33\s(F^2^)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
  V V 0.267  0.53 'International Tables Vol. IV (1974) Table 2.2B'
  O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B'
  N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B'
  C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B'
  H H     0     0 'International Tables Vol. IV (1974) Table 2.2B'
_refine_ls_structure_factor_coef        F
_refine_ls_matrix_type                  full
_refine_ls_number_reflns                4190
_refine_ls_number_parameters             329
_refine_ls_hydrogen_treatment           noref
_refine_ls_extinction_coef                        0.3841E-7
_refine_ls_extinction_method            Zachariasen
_refine_ls_extinction_expression
;
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
;
_refine_ls_abs_structure_details        none
_refine_ls_abs_structure_Flack          ?
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details            w^-1^=\s^2^(F)+(.05F)^2^
_refine_ls_R_factor_gt                               0.1111
_refine_ls_wR_factor_ref                             0.1125
_refine_ls_goodness_of_fit_ref                       2.5203
_refine_ls_shift/su_max                              0.2286
_refine_diff_density_max                             1.00
_refine_diff_density_min                            -0.97
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_disorder_group
_atom_site_disorder_assembly
  V1  V           1   0.5392(3)        0.25 0.0275(15) Uani        1 0 .
  V2  V 0.99886(10)   0.4455(2) 0.14682(10) 0.0271(11) Uani        1 0 .
  V3  V 0.87024(10)   0.4098(2) 0.15476(10) 0.0320(11) Uani        1 0 .
  V4  V 1.12870(10)   0.4108(3) 0.21998(10) 0.0354(11) Uani        1 0 .
  V5  V 0.91450(10)   0.2205(2) 0.12556(10) 0.0281(13) Uani        1 0 .
  V6  V 1.08240(10)   0.2219(2) 0.16745(10) 0.0295(13) Uani        1 0 .
  V7  V   0.9991(2)   0.0698(3)   0.1869(2) 0.0621(15) Uani        1 0 .
  V8  V 0.86236(10)   0.1747(2) 0.21602(10) 0.0312(13) Uani        1 0 .
  O9  O   0.9420(5)   0.4912(9)   0.1840(4)   0.030(4) Uani        1 0 .
  O10 O   1.0567(5)   0.4934(8)   0.2116(5)   0.031(4) Uani        1 0 .
  O11 O   0.9372(5)   0.3524(8)   0.1208(4)   0.026(4) Uani        1 0 .
  O12 O   1.0625(5)   0.3549(8)   0.1529(4)   0.024(4) Uani        1 0 .
  O13 O   0.8594(5)   0.2745(8)   0.1629(4)   0.025(4) Uani        1 0 .
  O14 O   0.8420(5)   0.4370(9)   0.2102(4)   0.032(4) Uani        1 0 .
  O15 O   1.1384(5)   0.2753(9)   0.2314(4)   0.031(4) Uani        1 0 .
  O16 O   0.9994(5)   0.1855(8)   0.1354(4)   0.029(4) Uani        1 0 .
  O17 O   0.9174(5)   0.1215(9)   0.1761(4)   0.031(4) Uani        1 0 .
  O18 O   1.0808(5)   0.1219(9)   0.2170(4)   0.032(4) Uani        1 0 .
  O19 O           1  0.0126(15)        0.25   0.061(9) Uani        1 0 .
  O20 O           1  0.6561(12)        0.25   0.035(7) Uani        1 0 .
  O21 O   0.9965(5)   0.5182(9)   0.1001(4)   0.031(4) Uani        1 0 .
  O22 O   0.8174(5)   0.4532(9)   0.1048(5)   0.040(5) Uani        1 0 .
  O23 O   1.1816(6)  0.4543(11)   0.1950(5)   0.055(6) Uani        1 0 .
  O24 O   0.8743(5)  0.1855(10)   0.0690(4)   0.036(5) Uani        1 0 .
  O25 O   1.1246(6)  0.1851(11)   0.1311(5)   0.046(5) Uani        1 0 .
  O26 O   1.0004(7) -0.0214(11)   0.1507(7)   0.072(7) Uani        1 0 .
  O27 O   0.7962(5)  0.1178(10)   0.2001(4)   0.040(5) Uani        1 0 .
  N28 N   1.1743(6)  0.5647(13)   0.0466(5)   0.040(6) Uani        1 0 .
  C29 C  1.1472(10)    0.491(2)  0.0764(11)  0.074(11) Uani        1 0 .
  C30 C  1.1274(14)    0.394(2)  0.0472(12)  0.093(15) Uani        1 0 .
  C31 C  1.1933(11)    0.649(2)  0.0824(10)  0.086(13) Uani        1 0 .
  C32 C  1.2167(12)    0.737(2)  0.0634(13)  0.097(14) Uani        1 0 .
  C33 C   1.1237(9)  0.5958(17)  -0.0015(8)   0.050(8) Uani        1 0 .
  C34 C   1.0631(9)  0.6334(18)   0.0059(7)   0.056(9) Uani        1 0 .
  C35 C   1.2297(8)  0.5303(14)   0.0316(7)   0.034(7) Uani        1 0 .
  C36 C   1.2831(9)  0.4937(17)   0.0746(8)   0.050(8) Uani        1 0 .
  N37 N   1.1498(7) -0.2055(13)   0.2394(6)   0.043(7) Uani        1 0 .
  C38 C  1.1661(16)   -0.312(3)  0.2599(14)   0.060(9) Uiso  0.67351 0 .
  C39 C  1.2228(11) -0.3260(18)  0.3016(10)   0.054(6) Uiso 0.924709 0 .
  C40 C  1.1959(12)   -0.169(2)  0.2143(11)   0.043(6) Uiso  0.75171 0 .
  C41 C  1.1840(15)   -0.063(3)  0.1864(13)   0.055(9) Uiso 0.705677 0 .
  C42 C  1.0815(10) -0.1949(17)   0.2024(9)   0.030(5) Uiso 0.743763 0 .
  C43 C  1.0657(10) -0.2526(15)   0.1528(9)   0.050(5) Uiso 0.998564 0 .
  C44 C  1.1563(15)   -0.128(2)  0.2863(13)   0.065(9) Uiso 0.735977 0 .
  C45 C  1.1161(15)   -0.159(2)  0.3223(13)   0.070(9) Uiso 0.780323 0 .
  C46 C    1.218(5)   -0.232(9)    0.268(5)    0.11(3) Uiso 0.278307 0 .
  C47 C    1.166(3)   -0.105(5)    0.210(3)  0.047(16) Uiso 0.308673 0 .
  C48 C    1.199(3)   -0.121(5)    0.172(3)  0.085(19) Uiso 0.429366 0 .
  C49 C    1.124(3)   -0.284(6)    0.208(3)  0.044(18) Uiso 0.274947 0 .
  C50 C    1.104(2)   -0.183(4)    0.271(2)  0.052(14) Uiso 0.394475 0 .
  N51 N  0.9724(15)   -0.020(3)  0.0018(14)   0.053(9) Uiso      0.5 0 .
  C52 C  1.0204(15)   -0.063(2) -0.0262(12)   0.069(9) Uiso 0.813825 0 .
  C53 C    1.001(4)   -0.134(7)   -0.009(4)    0.14(3) Uiso 0.443147 0 .
  C54 C  0.9519(19)   -0.092(3)  0.0367(17)  0.062(11) Uiso 0.549332 0 .
  C55 C    0.942(3)   -0.184(4)    0.013(2)  0.095(18) Uiso 0.527122 0 .
  C56 C    0.908(2)    0.062(4)   -0.035(2)  0.080(14) Uiso 0.540589 0 .
  C57 C    0.850(3)    0.013(4)   -0.039(2)  0.084(16) Uiso   0.4875 0 .
  C58 C    0.913(2)   -0.010(4) -0.0508(19)  0.089(14) Uiso 0.638486 0 .
  C59 C    0.868(2)    0.674(4)    0.092(2)  0.032(13) Uiso 0.317341 0 .
  C60 C    0.882(4)    0.741(7)    0.072(3)    0.08(2) Uiso 0.317341 0 .
  N61 N    0.897(3)   -0.190(5)    0.057(2)  0.061(16) Uiso 0.317341 0 .
  C62 C    0.719(2)    0.634(4)    0.060(2)  0.033(13) Uiso   0.3273 0 .
  C63 C    0.759(3)    0.702(5)    0.044(2)  0.044(15) Uiso   0.3273 0 .
  N64 N    0.770(3)    0.761(5)    0.018(2)  0.063(16) Uiso   0.3273 0 .
  H1  H      1.1784       0.478      0.1088     0.0867 Uiso        1 0 .
  H2  H      1.1109      0.5192      0.0823     0.0867 Uiso        1 0 .
  H3  H      1.1117      0.3527      0.0691     0.1063 Uiso        1 0 .
  H4  H       1.095      0.4059      0.0152     0.1063 Uiso        1 0 .
  H5  H      1.1629      0.3656      0.0406     0.1063 Uiso        1 0 .
  H6  H       1.157      0.6678      0.0922     0.0976 Uiso        1 0 .
  H7  H      1.2258      0.6281      0.1127     0.0976 Uiso        1 0 .
  H8  H       1.254      0.7219      0.0543     0.1074 Uiso        1 0 .
  H9  H      1.1852      0.7612      0.0334     0.1074 Uiso        1 0 .
  H10 H      1.2264      0.7846      0.0905     0.1074 Uiso        1 0 .
  H11 H       1.141      0.6457     -0.0177       0.06 Uiso        1 0 .
  H12 H      1.1134      0.5414     -0.0247       0.06 Uiso        1 0 .
  H13 H      1.0715      0.6899      0.0273     0.0677 Uiso        1 0 .
  H14 H      1.0337       0.649     -0.0275     0.0677 Uiso        1 0 .
  H15 H      1.0448       0.585      0.0225     0.0677 Uiso        1 0 .
  H16 H      1.2159        0.48      0.0065     0.0429 Uiso        1 0 .
  H17 H      1.2446      0.5835      0.0158     0.0429 Uiso        1 0 .
  H18 H       1.269      0.4417      0.0917     0.0625 Uiso        1 0 .
  H19 H      1.3154      0.4714      0.0608     0.0625 Uiso        1 0 .
  H20 H      1.2993      0.5443      0.0993     0.0625 Uiso        1 0 .