Structural and Spectroscopic Evidence for the Formation of Trinuclear and Tetranuclear Vanadium(III)/Carboxylate Complexes of Acetate and Related Derivatives in Aqueous Solution
Riya Mukherjee; Brenda A. Dougan; Fiona H. Fry; Scott D. Bunge; Christopher J. Ziegler; Nicola E. Brasch; Inorganic Chemistry 46 (2007) 1575–1585; doi:10.1021/ic0613210

data_4306968
_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 Cl6 F3 O20 S V3'
_chemical_formula_weight         950.87
_chemical_name_common
'[V3(m3-O)(m-OOCCH2Cl)6(H2O)3][CF3SO3]H2O (7)'
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 107.065(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4904(12)
_cell_length_b                   14.0237(12)
_cell_length_c                   18.0199(16)
_cell_measurement_reflns_used    2235
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.56
_cell_measurement_theta_min      2.15
_cell_volume                     3259.0(5)
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.2100
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37412
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.8530
_exptl_absorpt_correction_T_min  0.7065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   10(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         18278
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.830
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.6249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1946
_reflns_number_gt                9434
_reflns_number_total             18278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0613210si20060918_062623_4.cif
_cod_data_source_block           bd012z
_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_database_code               4306968