Synthesis, Structure, and Magnetic Properties of Two New Vanadocarboxylates with Three-Dimensional Hybrid Frameworks
K. Barthelet; D. Riou; M. Nogues; G. Férey; Inorganic Chemistry 42 (2003) 1739–1743; doi:10.1021/ic026175m

data_4313316
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of Two New
 Vanadocarboxylates with Three-Dimensional Hybrid Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1739
_journal_page_last               1743
_journal_paper_doi               10.1021/ic026175m
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C10 H4 O14 V2'
_chemical_formula_weight         450.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                69.010(2)
_cell_angle_beta                 85.197(2)
_cell_angle_gamma                79.452(2)
_cell_formula_units_Z            1
_cell_length_a                   6.3758(5)
_cell_length_b                   6.8840(5)
_cell_length_c                   9.0254(7)
_cell_measurement_reflns_used    1236
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.60
_cell_measurement_theta_min      2.42
_cell_volume                     363.53(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamond 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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2579
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.236968
_exptl_absorpt_correction_type   'semi-empirical (SADABS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.093
_exptl_crystal_density_meas      2.03(1)
_exptl_crystal_density_method    pycnometry
_exptl_crystal_description       parallelepi
_exptl_crystal_F_000             222
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0235(93)
_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   1.051
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_obs          0.0499
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.4930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1494
_refine_ls_wR_factor_obs         0.1329
_reflns_number_observed          1335
_reflns_number_total             1821
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic026175msi20021213_081706.cif
_cod_data_source_block           kb1878sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.4930P] 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^)+(0.0821P)^2^+0.4930P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4313316