[VIII(H2O)]3O(O2CC6H4CO2)3·(Cl, 9H2O) (MIL-59): a rare example of vanadocarboxylate with a magnetically frustrated three-dimensional hybrid framework
Barthelet, K.; Riou, D.; Férey, G.; Chemical Communications  (2002) 1492–; doi:10.1039/b202749f

data_7114444
_publ_section_title
;
 [VIII(H2O)]3O(O2CC6H4CO2)3&#x00B7;(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       '\w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0555P)^2^+11.2419P] where P=(Fo^2^+2Fc^2^)/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