#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:22:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179107 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/69/4306967.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_4306967
loop_
_publ_author_name
'Riya Mukherjee'
'Brenda A. Dougan'
'Fiona H. Fry'
'Scott D. Bunge'
'Christopher J. Ziegler'
'Nicola E. Brasch'
_publ_section_title
;
Structural and Spectroscopic Evidence for the Formation of Trinuclear and
Tetranuclear Vanadium(III)/Carboxylate Complexes of Acetate and Related
Derivatives in Aqueous Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1575
_journal_page_last               1585
_journal_paper_doi               10.1021/ic0613210
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C13 H20 Br6 F3 O20 S V3'
_chemical_formula_weight         1217.63
_chemical_name_common
'[V3(m3-O)(m-OOCCH2Br)6(OH2)3][CF3SO3]H2O (4)'
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.652(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.699(4)
_cell_length_b                   14.218(4)
_cell_length_c                   18.674(6)
_cell_measurement_reflns_used    4206
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.18
_cell_measurement_theta_min      2.12
_cell_volume                     3465.9(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27435
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    7.859
_exptl_absorpt_correction_T_max  0.5070
_exptl_absorpt_correction_T_min  0.3024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         5.610
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.602
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.602
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.5491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2400
_reflns_number_gt                4471
_reflns_number_total             6110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613210si20060918_062623_3.cif
_cod_data_source_block           rm004_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3466.0(18)
_cod_database_code               4306967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.85951(14) 0.25743(12) 0.22197(10) 0.017(2) Uani 1 1 d . . .
V2 V 0.70017(14) 0.41462(12) 0.11432(10) 0.016(2) Uani 1 1 d . . .
V3 V 0.93932(15) 0.40111(13) 0.10876(11) 0.021(2) Uani 1 1 d . . .
O1 O 0.7981(6) 0.3317(5) 0.2892(4) 0.023(3) Uani 1 1 d . . .
O2 O 0.6994(6) 0.4442(5) 0.2197(4) 0.021(3) Uani 1 1 d . . .
O3 O 0.7277(6) 0.1859(5) 0.1762(4) 0.023(3) Uani 1 1 d . . .
O4 O 0.6198(6) 0.2936(5) 0.1066(4) 0.024(3) Uani 1 1 d . . .
O5 O 0.7475(6) 0.5471(5) 0.1118(4) 0.022(3) Uani 1 1 d . . .
O6 O 0.9115(6) 0.5390(5) 0.1147(4) 0.022(3) Uani 1 1 d . . .
O7 O 0.6845(6) 0.3935(5) 0.0045(4) 0.023(3) Uani 1 1 d . . .
O8 O 0.8463(7) 0.3987(5) 0.0005(5) 0.027(3) Uani 1 1 d . . .
O9 O 1.0434(6) 0.4096(5) 0.2106(5) 0.025(3) Uani 1 1 d . . .
O10 O 1.0016(6) 0.3028(5) 0.2838(5) 0.029(3) Uani 1 1 d . . .
O11 O 0.9866(7) 0.2706(5) 0.0929(5) 0.029(3) Uani 1 1 d . . .
O12 O 0.9189(7) 0.1752(5) 0.1595(4) 0.026(3) Uani 1 1 d . . .
O13 O 0.8838(6) 0.1517(5) 0.3000(4) 0.021(3) Uani 1 1 d . . .
O14 O 0.5596(6) 0.4734(5) 0.0813(4) 0.021(3) Uani 1 1 d . . .
O15 O 1.0522(7) 0.4485(6) 0.0664(5) 0.030(3) Uani 1 1 d . . .
O16 O 0.8341(6) 0.3592(5) 0.1488(4) 0.016(3) Uani 1 1 d . . .
O17 O 0.2333(7) 0.3926(6) 0.0535(5) 0.036(3) Uani 1 1 d . . .
O18 O 0.3647(6) 0.2840(5) 0.0414(5) 0.025(3) Uani 1 1 d . . .
O19 O 0.4078(7) 0.4125(6) 0.1323(5) 0.038(3) Uani 1 1 d . . .
O25 O 0.5269(6) 0.6603(5) 0.0559(4) 0.023(3) Uani 1 1 d . . .
C1 C 0.7426(9) 0.4026(8) 0.2808(7) 0.020(3) Uani 1 1 d . . .
C2 C 0.7171(10) 0.4491(8) 0.3475(6) 0.026(4) Uani 1 1 d . . .
H2A H 0.6468 0.4311 0.3462 0.032 Uiso 1 1 calc R . .
H2B H 0.7188 0.5183 0.3422 0.032 Uiso 1 1 calc R . .
C3 C 1.0584(8) 0.3641(7) 0.2715(7) 0.019(3) Uani 1 1 d . . .
C4 C 1.1566(10) 0.3879(9) 0.3295(7) 0.030(4) Uani 1 1 d . . .
H4A H 1.1691 0.4562 0.3266 0.036 Uiso 1 1 calc R . .
H4B H 1.2128 0.3543 0.3172 0.036 Uiso 1 1 calc R . .
C5 C 0.8335(9) 0.5842(8) 0.1142(6) 0.020(3) Uani 1 1 d . . .
C6 C 0.8350(10) 0.6884(8) 0.1201(7) 0.028(4) Uani 1 1 d . . .
H6A H 0.8368 0.7057 0.1718 0.034 Uiso 1 1 calc R . .
H6B H 0.7703 0.7131 0.0855 0.034 Uiso 1 1 calc R . .
C7 C 0.9672(10) 0.1917(9) 0.1138(7) 0.029(4) Uani 1 1 d . . .
C8 C 1.0009(14) 0.1064(10) 0.0746(10) 0.053(5) Uani 1 1 d . . .
H8A H 1.0508 0.1276 0.0492 0.064 Uiso 1 1 calc R . .
H8B H 0.9406 0.0802 0.0360 0.064 Uiso 1 1 calc R . .
C9 C 0.7519(11) 0.3946(7) -0.0295(6) 0.027(4) Uani 1 1 d . . .
C10 C 0.7024(10) 0.3860(9) -0.1149(6) 0.028(4) Uani 1 1 d . . .
H10A H 0.6650 0.4449 -0.1341 0.034 Uiso 1 1 calc R . .
H10B H 0.6520 0.3340 -0.1254 0.034 Uiso 1 1 calc R . .
C11 C 0.6423(9) 0.2115(8) 0.1333(6) 0.022(4) Uani 1 1 d . . .
C12 C 0.5604(9) 0.1381(7) 0.1068(7) 0.022(4) Uani 1 1 d . . .
H12A H 0.5762 0.0982 0.0683 0.026 Uiso 1 1 calc R . .
H12B H 0.4937 0.1692 0.0833 0.026 Uiso 1 1 calc R . .
C13 C 0.3056(12) 0.2738(11) 0.1609(9) 0.044(5) Uani 1 1 d . . .
Br1 Br 0.55078(10) 0.05978(9) 0.18975(8) 0.033(2) Uani 1 1 d . . .
Br2 Br 1.06278(15) 0.00952(11) 0.14729(14) 0.073(3) Uani 1 1 d . . .
Br3 Br 0.80189(13) 0.36269(12) -0.16762(9) 0.050(3) Uani 1 1 d . . .
Br4 Br 0.94748(12) 0.74926(10) 0.09767(11) 0.053(3) Uani 1 1 d . . .
Br5 Br 0.81206(13) 0.41279(9) 0.44377(7) 0.041(3) Uani 1 1 d . . .
Br6 Br 1.16294(13) 0.35741(11) 0.43231(8) 0.048(3) Uani 1 1 d . . .
F1 F 0.3870(8) 0.2320(7) 0.2010(5) 0.069(4) Uani 1 1 d . . .
F2 F 0.2673(9) 0.3252(7) 0.2054(6) 0.076(4) Uani 1 1 d . . .
F3 F 0.2369(9) 0.2078(7) 0.1296(7) 0.082(4) Uani 1 1 d . . .
S1 S 0.3296(2) 0.3482(2) 0.08851(17) 0.024(3) Uani 1 1 d . . .
H50 H 0.506(15) 0.730(14) 0.022(11) 0.09(6) Uiso 1 1 d . . .
H51 H 0.559(8) 0.678(7) 0.023(6) 0.00(2) Uiso 1 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Br Br -0.2901 2.4595 '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
O16 V1 O12 92.5(3) . . ?
O16 V1 O1 91.6(3) . . ?
O12 V1 O1 175.7(3) . . ?
O16 V1 O3 97.5(3) . . ?
O12 V1 O3 85.9(3) . . ?
O1 V1 O3 92.2(3) . . ?
O16 V1 O10 95.7(3) . . ?
O12 V1 O10 91.6(4) . . ?
O1 V1 O10 89.3(4) . . ?
O3 V1 O10 166.7(3) . . ?
O16 V1 O13 178.7(3) . . ?
O12 V1 O13 88.7(3) . . ?
O1 V1 O13 87.1(3) . . ?
O3 V1 O13 82.1(3) . . ?
O10 V1 O13 84.7(3) . . ?
O16 V2 O5 96.4(3) . . ?
O16 V2 O2 92.6(3) . . ?
O5 V2 O2 85.7(3) . . ?
O16 V2 O14 178.3(3) . . ?
O5 V2 O14 83.6(3) . . ?
O2 V2 O14 85.7(3) . . ?
O16 V2 O7 94.4(3) . . ?
O5 V2 O7 93.0(3) . . ?
O2 V2 O7 173.0(3) . . ?
O14 V2 O7 87.3(3) . . ?
O16 V2 O4 96.8(3) . . ?
O5 V2 O4 166.7(3) . . ?
O2 V2 O4 94.7(3) . . ?
O14 V2 O4 83.2(3) . . ?
O7 V2 O4 85.0(3) . . ?
O16 V3 O9 92.9(3) . . ?
O16 V3 O6 96.0(3) . . ?
O9 V3 O6 88.9(3) . . ?
O16 V3 O11 94.9(3) . . ?
O9 V3 O11 91.5(4) . . ?
O6 V3 O11 169.1(3) . . ?
O16 V3 O8 93.7(3) . . ?
O9 V3 O8 173.4(3) . . ?
O6 V3 O8 89.9(3) . . ?
O11 V3 O8 88.3(3) . . ?
O16 V3 O15 179.0(3) . . ?
O9 V3 O15 86.8(3) . . ?
O6 V3 O15 83.0(3) . . ?
O11 V3 O15 86.1(3) . . ?
O8 V3 O15 86.6(4) . . ?
C1 O1 V1 134.6(7) . . ?
C1 O2 V2 130.2(7) . . ?
C11 O3 V1 131.6(7) . . ?
C11 O4 V2 133.7(7) . . ?
C5 O5 V2 133.6(7) . . ?
C5 O6 V3 132.9(7) . . ?
C9 O7 V2 129.6(8) . . ?
C9 O8 V3 134.4(8) . . ?
C3 O9 V3 134.0(7) . . ?
C3 O10 V1 131.5(8) . . ?
C7 O11 V3 132.5(8) . . ?
C7 O12 V1 133.1(8) . . ?
V3 O16 V2 119.9(4) . . ?
V3 O16 V1 120.7(4) . . ?
V2 O16 V1 119.3(4) . . ?
H50 O25 H51 58(10) . . ?
O1 C1 O2 126.5(10) . . ?
O1 C1 C2 121.6(10) . . ?
O2 C1 C2 111.8(10) . . ?
C1 C2 Br5 112.5(8) . . ?
C1 C2 H2A 109.1 . . ?
Br5 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
Br5 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
O10 C3 O9 125.8(11) . . ?
O10 C3 C4 120.4(11) . . ?
O9 C3 C4 113.7(10) . . ?
C3 C4 Br6 115.4(8) . . ?
C3 C4 H4A 108.4 . . ?
Br6 C4 H4A 108.4 . . ?
C3 C4 H4B 108.4 . . ?
Br6 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
O6 C5 O5 124.5(10) . . ?
O6 C5 C6 121.5(11) . . ?
O5 C5 C6 113.9(10) . . ?
C5 C6 Br4 115.3(9) . . ?
C5 C6 H6A 108.5 . . ?
Br4 C6 H6A 108.4 . . ?
C5 C6 H6B 108.4 . . ?
Br4 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
O11 C7 O12 126.3(11) . . ?
O11 C7 C8 115.7(11) . . ?
O12 C7 C8 117.9(11) . . ?
C7 C8 Br2 110.7(10) . . ?
C7 C8 H8A 109.5 . . ?
Br2 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
Br2 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O8 C9 O7 126.1(11) . . ?
O8 C9 C10 122.8(12) . . ?
O7 C9 C10 111.1(11) . . ?
C9 C10 Br3 112.6(9) . . ?
C9 C10 H10A 109.1 . . ?
Br3 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
Br3 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
O3 C11 O4 125.9(10) . . ?
O3 C11 C12 117.9(10) . . ?
O4 C11 C12 116.2(10) . . ?
C11 C12 Br1 111.1(8) . . ?
C11 C12 H12A 109.4 . . ?
Br1 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
Br1 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
F1 C13 F2 109.1(14) . . ?
F1 C13 F3 107.6(13) . . ?
F2 C13 F3 107.5(13) . . ?
F1 C13 S1 112.4(10) . . ?
F2 C13 S1 109.8(10) . . ?
F3 C13 S1 110.2(11) . . ?
O17 S1 O18 115.5(5) . . ?
O17 S1 O19 113.5(6) . . ?
O18 S1 O19 114.5(5) . . ?
O17 S1 C13 104.3(6) . . ?
O18 S1 C13 104.6(6) . . ?
O19 S1 C13 102.4(7) . . ?
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 O16 1.948(7) . ?
V1 O12 1.991(8) . ?
V1 O1 2.010(8) . ?
V1 O3 2.022(8) . ?
V1 O10 2.043(8) . ?
V1 O13 2.048(7) . ?
V2 O16 1.919(8) . ?
V2 O5 1.997(8) . ?
V2 O2 2.014(8) . ?
V2 O14 2.016(8) . ?
V2 O7 2.018(8) . ?
V2 O4 2.024(8) . ?
V3 O16 1.910(7) . ?
V3 O9 2.004(9) . ?
V3 O6 2.007(7) . ?
V3 O11 2.017(8) . ?
V3 O8 2.036(9) . ?
V3 O15 2.052(9) . ?
O1 C1 1.243(13) . ?
O2 C1 1.262(14) . ?
O3 C11 1.255(14) . ?
O4 C11 1.270(13) . ?
O5 C5 1.280(14) . ?
O6 C5 1.244(14) . ?
O7 C9 1.270(15) . ?
O8 C9 1.246(15) . ?
O9 C3 1.269(14) . ?
O10 C3 1.236(13) . ?
O11 C7 1.242(14) . ?
O12 C7 1.251(15) . ?
O17 S1 1.430(9) . ?
O18 S1 1.447(8) . ?
O19 S1 1.456(10) . ?
O25 H50 1.2(2) . ?
O25 H51 0.89(11) . ?
C1 C2 1.540(16) . ?
C2 Br5 1.942(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.487(17) . ?
C4 Br6 1.944(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.484(15) . ?
C6 Br4 1.921(13) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.558(18) . ?
C8 Br2 1.939(14) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.536(16) . ?
C10 Br3 1.937(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.502(15) . ?
C12 Br1 1.945(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 F1 1.285(17) . ?
C13 F2 1.330(17) . ?
C13 F3 1.332(19) . ?
C13 S1 1.822(13) . ?
