#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:22:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179107 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/69/4306966.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_4306966
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            'C18 H40 Cl O18 V3'
_chemical_formula_weight         732.77
_chemical_name_common            '[V3(m3-O)(m-OOCCH2CH3)6(H2O)3]Cl*2H2O (5)'
_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-97
_cell_angle_alpha                67.527(3)
_cell_angle_beta                 70.775(3)
_cell_angle_gamma                66.979(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0342(18)
_cell_length_b                   11.3901(19)
_cell_length_c                   14.607(2)
_cell_measurement_reflns_used    4304
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.29
_cell_volume                     1526.0(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12299
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_correction_T_min  0.9013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.427
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5388
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.427
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+34.8308P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                4342
_reflns_number_total             5388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613210si20060918_062623_2.cif
_cod_data_source_block           rm001tri
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4306966
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_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 0.93257(5) 0.05954(5) 0.16960(4) 0.01334(14) Uani 1 1 d . A 1
V2 V 0.63916(5) 0.29295(5) 0.20510(4) 0.01232(14) Uani 1 1 d . A 1
V3 V 0.82274(5) 0.14721(5) 0.38062(4) 0.01124(14) Uani 1 1 d . A 1
O1 O 0.9491(2) 0.2140(2) 0.04567(18) 0.0209(5) Uani 1 1 d . A 1
O2 O 0.7429(2) 0.3578(2) 0.06255(17) 0.0193(5) Uani 1 1 d . A 1
O3 O 0.8005(2) 0.0287(2) 0.11799(17) 0.0187(5) Uani 1 1 d . A 1
O4 O 0.5980(2) 0.1605(2) 0.17023(18) 0.0177(5) Uani 1 1 d . A 1
O5 O 0.6541(2) 0.4467(2) 0.23083(18) 0.0193(5) Uani 1 1 d . A 1
O6 O 0.7389(2) 0.3419(2) 0.36990(19) 0.0210(5) Uani 1 1 d . A 1
O7 O 0.5200(2) 0.2532(2) 0.34322(17) 0.0170(5) Uani 1 1 d . A 1
O8 O 0.6453(2) 0.1173(2) 0.45705(17) 0.0171(5) Uani 1 1 d . A 1
O9 O 1.0862(2) 0.0748(2) 0.20549(18) 0.0197(5) Uani 1 1 d . A 1
O10 O 1.0005(2) 0.1816(3) 0.32241(18) 0.0205(5) Uani 1 1 d . A 1
O11 O 0.9374(2) -0.1140(2) 0.28000(17) 0.0194(5) Uani 1 1 d . A 1
O12 O 0.9168(2) -0.0542(2) 0.41362(17) 0.0170(5) Uani 1 1 d . A 1
O13 O 0.7977(2) 0.1651(2) 0.25218(16) 0.0130(5) Uani 1 1 d . A 1
O14 O 1.0782(2) -0.0578(2) 0.08515(18) 0.0214(5) Uani 1 1 d D A 1
O15 O 0.4702(2) 0.4194(2) 0.15460(18) 0.0193(5) Uani 1 1 d D A 1
O16 O 0.8510(2) 0.1223(2) 0.51880(18) 0.0179(5) Uani 1 1 d D A 1
C1 C 0.8609(3) 0.3204(3) 0.0137(3) 0.0185(7) Uani 1 1 d . A 1
C2 C 0.9013(4) 0.4104(4) -0.0909(3) 0.0320(9) Uani 1 1 d . A 1
H2A H 0.8568 0.4035 -0.1367 0.038 Uiso 1 1 calc R A 1
H2B H 0.8619 0.5032 -0.0870 0.038 Uiso 1 1 calc R A 1
C4 C 0.6726(3) 0.0678(3) 0.1321(2) 0.0169(7) Uani 1 1 d . A 1
C5 C 0.6036(4) -0.0006(4) 0.1041(3) 0.0284(9) Uani 1 1 d . A 1
H5A H 0.5413 -0.0360 0.1659 0.034 Uiso 1 1 calc R A 1
H5B H 0.5480 0.0677 0.0553 0.034 Uiso 1 1 calc R A 1
C6 C 0.6902(5) -0.1110(6) 0.0595(5) 0.0571(15) Uani 1 1 d . A 1
H6A H 0.7277 -0.0742 -0.0123 0.086 Uiso 1 1 calc R A 1
H6B H 0.6363 -0.1657 0.0657 0.086 Uiso 1 1 calc R A 1
H6C H 0.7637 -0.1663 0.0955 0.086 Uiso 1 1 calc R A 1
C7 C 0.6864(4) 0.4449(3) 0.3059(3) 0.0244(8) Uani 1 1 d . A 1
C8 C 0.5332(3) 0.1824(3) 0.4319(2) 0.0138(7) Uani 1 1 d . A 1
C9 C 0.4064(3) 0.1761(3) 0.5118(3) 0.0182(7) Uani 1 1 d . A 1
H9A H 0.3611 0.1275 0.4971 0.022 Uiso 1 1 calc R A 1
H9B H 0.3452 0.2681 0.5066 0.022 Uiso 1 1 calc R A 1
C10 C 0.4265(4) 0.1095(4) 0.6197(3) 0.0220(8) Uani 1 1 d . A 1
H10A H 0.4810 0.0160 0.6275 0.033 Uiso 1 1 calc R A 1
H10C H 0.3386 0.1140 0.6665 0.033 Uiso 1 1 calc R A 1
H10B H 0.4728 0.1556 0.6350 0.033 Uiso 1 1 calc R A 1
C11 C 1.0957(3) 0.1371(4) 0.2558(3) 0.0205(8) Uani 1 1 d . A 1
C12 C 1.2273(4) 0.1627(5) 0.2350(3) 0.0386(11) Uani 1 1 d . A 1
H12A H 1.2445 0.2205 0.1645 0.046 Uiso 1 1 calc R A 1
H12B H 1.3003 0.0768 0.2399 0.046 Uiso 1 1 calc R A 1
C13 C 1.2340(5) 0.2274(6) 0.3050(3) 0.0506(14) Uani 1 1 d . A 1
H13A H 1.1628 0.3132 0.3003 0.076 Uiso 1 1 calc R A 1
H13B H 1.3221 0.2419 0.2854 0.076 Uiso 1 1 calc R A 1
H13C H 1.2215 0.1692 0.3748 0.076 Uiso 1 1 calc R A 1
C14 C 0.9427(3) -0.1410(3) 0.3701(2) 0.0164(7) Uani 1 1 d . A 1
C15 C 0.9815(4) -0.2857(3) 0.4320(3) 0.0238(8) Uani 1 1 d . A 1
H15A H 1.0154 -0.2929 0.4895 0.029 Uiso 1 1 calc R A 1
H15B H 0.8993 -0.3143 0.4609 0.029 Uiso 1 1 calc R A 1
C17 C 0.6179(13) 0.5752(7) 0.3399(7) 0.027(3) Uani 0.54(2) 1 d P A 1
C18 C 0.4956(8) 0.5660(8) 0.4271(7) 0.032(3) Uani 0.475(12) 1 d P B 2
C3A C 1.0384(8) 0.3923(9) -0.1387(6) 0.034(3) Uani 0.478(13) 1 d P A 1
C3B C 0.9798(9) 0.4896(10) -0.0916(7) 0.042(3) Uani 0.522(13) 1 d P A 2
C16A C 1.0857(9) -0.3804(7) 0.3759(6) 0.026(3) Uani 0.55(2) 1 d P A 1
C16B C 0.994(3) -0.3811(10) 0.3670(9) 0.060(8) Uani 0.45(2) 1 d P A 2
C17A C 0.7023(13) 0.5771(8) 0.2982(9) 0.024(4) Uani 0.46(2) 1 d P A 2
C18A C 0.8002(10) 0.5634(8) 0.3560(8) 0.045(3) Uani 0.525(12) 1 d P B 1
Cl1 Cl 0.33404(10) 0.71940(9) 0.13944(8) 0.0322(2) Uani 1 1 d . C 1
H19 H 1.119(5) -0.029(5) 0.0184(18) 0.051(15) Uiso 1 1 d D D 1
H20 H 1.150(4) -0.128(4) 0.109(4) 0.048(14) Uiso 1 1 d D E 1
H21 H 0.453(5) 0.408(5) 0.099(3) 0.043(13) Uiso 1 1 d D F 1
H22 H 0.436(6) 0.506(3) 0.157(5) 0.08(2) Uiso 1 1 d D G 1
H23 H 0.786(4) 0.154(6) 0.570(3) 0.070(18) Uiso 1 1 d D H 1
H24 H 0.938(3) 0.095(5) 0.529(4) 0.051(15) Uiso 1 1 d D I 1
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'
Cl Cl 0.1484 0.1585 '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
O13 V1 O1 95.11(10) . . ?
O13 V1 O11 94.10(9) . . ?
O1 V1 O11 170.77(10) . . ?
O13 V1 O9 93.71(9) . . ?
O1 V1 O9 88.62(10) . . ?
O11 V1 O9 91.32(10) . . ?
O13 V1 O3 95.33(9) . . ?
O1 V1 O3 89.82(10) . . ?
O11 V1 O3 88.79(10) . . ?
O9 V1 O3 170.92(10) . . ?
O13 V1 O14 178.27(10) . . ?
O1 V1 O14 86.51(10) . . ?
O11 V1 O14 84.28(10) . . ?
O9 V1 O14 85.72(10) . . ?
O3 V1 O14 85.26(10) . . ?
O13 V2 O5 95.90(9) . . ?
O13 V2 O4 93.44(9) . . ?
O5 V2 O4 170.65(10) . . ?
O13 V2 O7 92.86(9) . . ?
O5 V2 O7 89.25(10) . . ?
O4 V2 O7 90.69(10) . . ?
O13 V2 O15 176.86(10) . . ?
O5 V2 O15 87.22(10) . . ?
O4 V2 O15 83.44(10) . . ?
O7 V2 O15 86.90(10) . . ?
O13 V2 O2 93.52(9) . . ?
O5 V2 O2 86.14(10) . . ?
O4 V2 O2 92.89(10) . . ?
O7 V2 O2 172.48(10) . . ?
O15 V2 O2 86.96(10) . . ?
O13 V3 O10 93.53(10) . . ?
O13 V3 O8 94.56(10) . . ?
O10 V3 O8 171.65(10) . . ?
O13 V3 O6 94.93(10) . . ?
O10 V3 O6 87.73(11) . . ?
O8 V3 O6 89.49(10) . . ?
O13 V3 O16 178.33(10) . . ?
O10 V3 O16 86.85(10) . . ?
O8 V3 O16 85.13(10) . . ?
O6 V3 O16 86.70(10) . . ?
O13 V3 O12 94.83(9) . . ?
O10 V3 O12 90.49(10) . . ?
O8 V3 O12 90.92(10) . . ?
O6 V3 O12 170.16(10) . . ?
O16 V3 O12 83.54(9) . . ?
C1 O1 V1 130.0(2) . . ?
C1 O2 V2 135.8(2) . . ?
C4 O3 V1 133.4(2) . . ?
C4 O4 V2 131.8(2) . . ?
C7 O5 V2 127.2(2) . . ?
C7 O6 V3 136.0(2) . . ?
C8 O7 V2 137.7(2) . . ?
C8 O8 V3 126.7(2) . . ?
C11 O9 V1 135.1(2) . . ?
C11 O10 V3 128.3(2) . . ?
C14 O11 V1 128.2(2) . . ?
C14 O12 V3 134.1(2) . . ?
V1 O13 V3 119.87(11) . . ?
V1 O13 V2 120.37(11) . . ?
V3 O13 V2 119.74(11) . . ?
V1 O14 H19 126(3) . . ?
V1 O14 H20 124(3) . . ?
H19 O14 H20 100(4) . . ?
V2 O15 H21 118(3) . . ?
V2 O15 H22 121(4) . . ?
H21 O15 H22 113(5) . . ?
V3 O16 H23 126(4) . . ?
V3 O16 H24 119(3) . . ?
H23 O16 H24 113(5) . . ?
O2 C1 O1 124.7(3) . . ?
O2 C1 C2 118.0(3) . . ?
O1 C1 C2 117.3(3) . . ?
C3A C2 C1 120.5(5) . . ?
C3A C2 H2A 107.2 . . ?
C1 C2 H2A 107.2 . . ?
C3A C2 H2B 107.2 . . ?
C1 C2 H2B 107.2 . . ?
H2A C2 H2B 106.8 . . ?
O4 C4 O3 123.7(3) . . ?
O4 C4 C5 116.7(3) . . ?
O3 C4 C5 119.7(3) . . ?
C6 C5 C4 117.5(4) . . ?
C6 C5 H5A 107.9 . . ?
C4 C5 H5A 107.9 . . ?
C6 C5 H5B 107.9 . . ?
C4 C5 H5B 107.9 . . ?
H5A C5 H5B 107.2 . . ?
O5 C7 O6 125.3(3) . . ?
O5 C7 C17 116.0(4) . . ?
O6 C7 C17 116.0(4) . . ?
O7 C8 O8 123.9(3) . . ?
O7 C8 C9 117.3(3) . . ?
O8 C8 C9 118.8(3) . . ?
C8 C9 C10 115.2(3) . . ?
C8 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
C8 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
O9 C11 O10 123.8(3) . . ?
O9 C11 C12 118.4(3) . . ?
O10 C11 C12 117.9(3) . . ?
C11 C12 C13 114.8(3) . . ?
C11 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
C11 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.5 . . ?
O11 C14 O12 124.0(3) . . ?
O11 C14 C15 118.6(3) . . ?
O12 C14 C15 117.4(3) . . ?
C16A C15 C14 115.6(4) . . ?
C16A C15 H15A 108.4 . . ?
C14 C15 H15A 108.4 . . ?
C16A C15 H15B 108.4 . . ?
C14 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
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 O13 1.908(2) . ?
V1 O1 2.001(2) . ?
V1 O11 2.012(2) . ?
V1 O9 2.015(2) . ?
V1 O3 2.035(2) . ?
V1 O14 2.041(2) . ?
V2 O13 1.921(2) . ?
V2 O5 2.002(2) . ?
V2 O4 2.004(2) . ?
V2 O7 2.006(2) . ?
V2 O15 2.021(2) . ?
V2 O2 2.027(2) . ?
V3 O13 1.909(2) . ?
V3 O10 1.992(2) . ?
V3 O8 1.997(2) . ?
V3 O6 2.005(2) . ?
V3 O16 2.039(2) . ?
V3 O12 2.048(2) . ?
O1 C1 1.257(4) . ?
O2 C1 1.254(4) . ?
O3 C4 1.272(4) . ?
O4 C4 1.254(4) . ?
O5 C7 1.250(4) . ?
O6 C7 1.255(4) . ?
O7 C8 1.258(4) . ?
O8 C8 1.261(4) . ?
O9 C11 1.251(4) . ?
O10 C11 1.263(4) . ?
O11 C14 1.248(4) . ?
O12 C14 1.266(4) . ?
O14 H19 0.92(2) . ?
O14 H20 0.930(19) . ?
O15 H21 0.946(19) . ?
O15 H22 0.92(2) . ?
O16 H23 0.93(2) . ?
O16 H24 0.930(19) . ?
C1 C2 1.515(5) . ?
C2 C3A 1.410(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C5 1.505(5) . ?
C5 C6 1.482(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C17 1.568(8) . ?
C8 C9 1.504(5) . ?
C9 C10 1.515(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.502(5) . ?
C12 C13 1.503(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.511(5) . ?
C15 C16A 1.498(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.209 0.150 0.701 130.2 40
