#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:35:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179191 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/33/4313316.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_4313316
loop_
_publ_author_name
'K. Barthelet'
'D. Riou'
'M. Nogues'
'G. Férey'
_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       '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  0.0243
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0821P)²+0.4930P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_group
V1 V 0.0000 0.5000 0.5000 0.0119(3) Uani 1 d S .
V2 V 0.0000 0.0000 0.5000 0.0122(3) Uani 1 d S .
O1 O -0.0107(5) 0.2011(4) 0.6076(3) 0.0156(6) Uani 1 d . .
O2 O 0.1933(4) 0.1573(4) 0.3209(3) 0.0181(6) Uani 1 d . .
O3 O 0.1746(4) 0.4887(4) 0.6848(3) 0.0169(6) Uani 1 d . .
O4 O 0.2520(4) -0.1870(4) 0.6310(3) 0.0171(6) Uani 1 d . .
O5 O 0.2683(4) 0.4221(4) 0.3856(3) 0.0178(6) Uani 1 d . .
C1 C 0.3961(6) -0.4561(6) 0.8586(4) 0.0137(7) Uani 1 d . .
C2 C 0.2677(6) -0.3812(6) 0.7113(4) 0.0117(7) Uani 1 d . .
C3 C 0.4060(6) 0.3936(6) 0.1443(4) 0.0136(7) Uani 1 d . .
C4 C 0.2826(6) 0.3141(6) 0.2969(4) 0.0141(7) Uani 1 d . .
C5 C 0.3055(6) 0.4359(6) 0.0034(4) 0.0144(7) Uani 1 d . .
H5 H 0.1756(6) 0.3914(6) 0.0057(4) 0.017 Uiso 1 calc R .
OW1 O -0.1882(12) 0.1032(10) 0.9079(6) 0.102(2) Uani 1 d . .
OW2 O 0.4052(13) 0.0734(11) 0.8065(9) 0.114(3) Uani 1 d . .
HO1 H -0.0657(93) 0.1626(95) 0.6834(69) 0.035(17) Uiso 1 d . .
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'
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 V1 O1 180.0 2_566 . ?
O1 V1 O5 89.03(12) 2_566 2_566 ?
O1 V1 O5 90.98(12) . 2_566 ?
O1 V1 O5 90.97(12) 2_566 . ?
O1 V1 O5 89.02(12) . . ?
O5 V1 O5 179.999(1) 2_566 . ?
O1 V1 O3 88.43(11) 2_566 2_566 ?
O1 V1 O3 91.57(11) . 2_566 ?
O5 V1 O3 90.84(11) 2_566 2_566 ?
O5 V1 O3 89.16(11) . 2_566 ?
O1 V1 O3 91.57(11) 2_566 . ?
O1 V1 O3 88.43(11) . . ?
O5 V1 O3 89.16(11) 2_566 . ?
O5 V1 O3 90.84(11) . . ?
O3 V1 O3 179.999(2) 2_566 . ?
O1 V2 O1 180.0 . 2_556 ?
O1 V2 O4 89.16(12) . 2_556 ?
O1 V2 O4 90.84(12) 2_556 2_556 ?
O1 V2 O4 90.84(12) . . ?
O1 V2 O4 89.16(12) 2_556 . ?
O4 V2 O4 180.0 2_556 . ?
O1 V2 O2 92.46(12) . . ?
O1 V2 O2 87.54(12) 2_556 . ?
O4 V2 O2 87.39(11) 2_556 . ?
O4 V2 O2 92.61(11) . . ?
O1 V2 O2 87.54(12) . 2_556 ?
O1 V2 O2 92.46(12) 2_556 2_556 ?
O4 V2 O2 92.61(11) 2_556 2_556 ?
O4 V2 O2 87.39(11) . 2_556 ?
O2 V2 O2 179.999(1) . 2_556 ?
V2 O1 V1 124.40(15) . . ?
V2 O1 HO1 108.6(48) . . ?
V1 O1 HO1 121.6(48) . . ?
C4 O2 V2 133.4(3) . . ?
C2 O3 V1 134.1(2) 1_565 . ?
C2 O4 V2 126.7(2) . . ?
C4 O5 V1 124.8(2) . . ?
C5 C1 C3 119.3(3) 1_546 2_656 ?
C5 C1 C2 119.4(3) 1_546 . ?
C3 C1 C2 120.7(3) 2_656 . ?
O3 C2 O4 126.2(3) 1_545 . ?
O3 C2 C1 118.0(3) 1_545 . ?
O4 C2 C1 115.6(3) . . ?
C5 C3 C1 119.9(3) . 2_656 ?
C5 C3 C4 118.2(3) . . ?
C1 C3 C4 121.1(3) 2_656 . ?
O2 C4 O5 126.0(3) . . ?
O2 C4 C3 118.3(3) . . ?
O5 C4 C3 115.6(3) . . ?
C3 C5 C1 120.8(3) . 1_564 ?
C3 C5 H5 119.6(2) . . ?
C1 C5 H5 119.6(2) 1_564 . ?
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
V1 O1 1.947(3) 2_566 ?
V1 O1 1.947(3) . ?
V1 O5 2.011(3) 2_566 ?
V1 O5 2.011(3) . ?
V1 O3 2.053(3) 2_566 ?
V1 O3 2.053(3) . ?
V2 O1 1.945(3) . ?
V2 O1 1.945(3) 2_556 ?
V2 O4 2.027(3) 2_556 ?
V2 O4 2.027(3) . ?
V2 O2 2.051(3) . ?
V2 O2 2.051(3) 2_556 ?
O1 HO1 0.73(6) . ?
O2 C4 1.254(5) . ?
O3 C2 1.258(5) 1_565 ?
O4 C2 1.261(5) . ?
O5 C4 1.261(5) . ?
C1 C5 1.389(5) 1_546 ?
C1 C3 1.402(5) 2_656 ?
C1 C2 1.497(5) . ?
C2 O3 1.258(5) 1_545 ?
C3 C5 1.383(5) . ?
C3 C1 1.402(5) 2_656 ?
C3 C4 1.501(5) . ?
C5 C1 1.389(5) 1_564 ?
C5 H5 0.93 . ?
