#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:21:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180258 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/44/7114444.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_7114444
loop_
_publ_author_name
'Barthelet, K.'
'Riou, D.'
'Férey, G.'
_publ_section_title
;
 [VIII(H2O)]3O(O2CC6H4CO2)3·(Cl, 9H2O) (MIL-59): a rare example of
 vanadocarboxylate with a magnetically frustrated three-dimensional hybrid
 framework
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1492
_journal_paper_doi               10.1039/b202749f
_journal_year                    2002
_chemical_formula_sum            'C8 H4 Cl0.33 O8.33 V'
_chemical_formula_weight         296.20
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   19.29070(10)
_cell_length_b                   19.29070(10)
_cell_length_c                   19.29070(10)
_cell_measurement_reflns_used    47867
_cell_measurement_temperature    296(2)
_cell_volume                     7178.67(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamnod Brandenburg'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            47867
_diffrn_reflns_theta_max         29.87
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.880739
_exptl_absorpt_correction_T_min  0.784810
_exptl_absorpt_correction_type   'Semi empirical (SADABS)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_meas      1.670(4)
_exptl_crystal_density_method    pycnometry
_exptl_crystal_description       cubic
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.140
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_obs          0.0513
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0555P)²+11.2419P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1331
_refine_ls_wR_factor_obs         0.1238
_reflns_number_observed          2750
_reflns_number_total             3345
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b202749f.txt
_cod_data_source_block           MIL-59
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+11.2419P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+11.2419P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pa-3
_cod_database_code               7114444
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
V1 V 0.75509(2) 0.39102(2) 0.14242(2) 0.01682(14) Uani 1 d .
O1 O 0.80451(10) 0.48174(9) 0.15148(10) 0.0256(4) Uani 1 d .
O2 O 0.83494(9) 0.33494(9) 0.16506(9) 0.0176(6) Uani 1 d S
O3 O 0.69107(10) 0.30864(10) 0.13710(12) 0.0310(5) Uani 1 d .
O4 O 0.72206(10) 0.39737(11) 0.24087(10) 0.0277(4) Uani 1 d .
O5 O 0.77398(11) 0.39115(10) 0.04025(9) 0.0276(4) Uani 1 d .
O6 O 0.66938(11) 0.45057(11) 0.11735(11) 0.0320(5) Uani 1 d .
C1 C 0.74479(13) 0.36925(14) 0.29530(13) 0.0225(5) Uani 1 d .
C2 C 0.85500(13) 0.50048(13) 0.18967(14) 0.0223(5) Uani 1 d .
C3 C 0.69392(13) 0.33926(15) 0.34526(13) 0.0238(5) Uani 1 d .
C4 C 0.62343(13) 0.34303(14) 0.33040(14) 0.0232(5) Uani 1 d .
H4 H 0.60811(13) 0.36856(14) 0.29249(14) 0.028 Uiso 1 calc R
C5 C 0.80861(15) 0.37225(14) -0.07596(13) 0.0245(5) Uani 1 d .
C6 C 0.7699(2) 0.4287(2) -0.09915(14) 0.0336(7) Uani 1 d .
H6 H 0.7459(2) 0.4560(2) -0.06754(14) 0.040 Uiso 1 calc R
C7 C 0.71669(14) 0.3023(2) 0.4030(2) 0.0327(7) Uani 1 d .
H7 H 0.76362(14) 0.3012(2) 0.4140(2) 0.039 Uiso 1 calc R
C8 C 0.6693(2) 0.2672(2) 0.4441(2) 0.0413(8) Uani 1 d .
H8 H 0.6845(2) 0.2418(2) 0.4822(2) 0.050 Uiso 1 calc R
Cl Cl 0.5638(2) 0.4837(3) 0.2146(2) 0.0484(9) Uani 0.33 d P
OW1 O 0.5634(7) 0.4788(8) 0.2189(8) 0.141(5) Uani 0.67 d P
OW2 O 0.8677(2) 0.5525(2) -0.0074(2) 0.0682(9) Uani 1 d .
OW3 O 0.5756(2) 0.3989(3) 0.0212(3) 0.127(2) Uani 1 d .
OW4 O 0.9419(2) 0.4419(2) 0.0581(2) 0.0598(13) Uani 1 d S
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2 V1 O1 95.17(9) . .
O2 V1 O5 94.47(8) . .
O1 V1 O5 89.90(8) . .
O2 V1 O4 94.21(8) . .
O1 V1 O4 90.87(8) . .
O5 V1 O4 171.18(8) . .
O2 V1 O3 93.36(9) . .
O1 V1 O3 170.52(8) . .
O5 V1 O3 93.57(9) . .
O4 V1 O3 84.36(9) . .
O2 V1 O6 179.47(6) . .
O1 V1 O6 85.16(8) . .
O5 V1 O6 85.11(8) . .
O4 V1 O6 86.19(8) . .
O3 V1 O6 86.34(8) . .
C2 O1 V1 131.6(2) . .
V1 O2 V1 119.995(2) . 11_556
V1 O2 V1 119.996(2) . 8_645
V1 O2 V1 119.996(2) 11_556 8_645
C1 O3 V1 130.2(2) 8_645 .
C1 O4 V1 130.7(2) . .
C2 O5 V1 135.4(2) 8_645 .
O4 C1 O3 123.6(2) . 11_556
O4 C1 C3 118.4(2) . .
O3 C1 C3 117.9(2) 11_556 .
O5 C2 O1 124.5(2) 11_556 .
O5 C2 C5 118.1(2) 11_556 11_556
O1 C2 C5 117.4(2) . 11_556
C4 C3 C7 120.0(2) . .
C4 C3 C1 119.3(2) . .
C7 C3 C1 120.5(2) . .
C5 C4 C3 120.0(2) 18_655 .
C5 C4 H4 120.02(15) 18_655 .
C3 C4 H4 120.0(2) . .
C4 C5 C6 119.9(2) 24_656 .
C4 C5 C2 120.1(2) 24_656 8_645
C6 C5 C2 119.9(2) . 8_645
C8 C6 C5 120.1(3) 24_656 .
C8 C6 H6 120.0(2) 24_656 .
C5 C6 H6 120.0(2) . .
C8 C7 C3 119.9(3) . .
C8 C7 H7 120.0(2) . .
C3 C7 H7 120.0(2) . .
C6 C8 C7 120.2(3) 18_655 .
C6 C8 H8 119.9(2) 18_655 .
C7 C8 H8 119.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O2 1.9322(4) .
V1 O1 2.000(2) .
V1 O5 2.004(2) .
V1 O4 2.007(2) .
V1 O3 2.015(2) .
V1 O6 2.071(2) .
O1 C2 1.274(3) .
O2 V1 1.9323(4) 11_556
O2 V1 1.9323(4) 8_645
O3 C1 1.265(3) 8_645
O4 C1 1.260(3) .
O5 C2 1.263(3) 8_645
C1 O3 1.265(3) 11_556
C1 C3 1.492(4) .
C2 O5 1.263(3) 11_556
C2 C5 1.494(4) 11_556
C3 C4 1.391(4) .
C3 C7 1.394(4) .
C4 C5 1.390(4) 18_655
C4 H4 0.93 .
C5 C4 1.390(4) 24_656
C5 C6 1.394(4) .
C5 C2 1.494(4) 8_645
C6 C8 1.386(4) 24_656
C6 H6 0.93 .
C7 C8 1.387(4) .
C7 H7 0.93 .
C8 C6 1.386(4) 18_655
C8 H8 0.93 .
