Synthesis, structural, and magnetic studies on a redox family of tetrametallic vanadium clusters: {VIV4}, {VIII2VIV2}, and {VIII4} butterfly complexes.
Tidmarsh, Ian S.; Scales, Emma; Brearley, Paul R.; Wolowska, Joanna; Sorace, Lorenzo; Caneschi, Andrea; Laye, Rebecca H.; McInnes, Eric J. L.; Inorganic chemistry 46 (2007) 9743–9753; doi:10.1021/ic7011183

data_4333427
_publ_section_title
;
 Synthesis, structural, and magnetic studies on a redox family of
 tetrametallic vanadium clusters: {VIV4}, {VIII2VIV2}, and {VIII4}
 butterfly complexes.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9743
_journal_page_last               9753
_journal_paper_doi               10.1021/ic7011183
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C30 H52 O22 V4'
_chemical_formula_weight         968.48
_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                102.367(14)
_cell_angle_beta                 94.480(13)
_cell_angle_gamma                114.203(12)
_cell_formula_units_Z            2
_cell_length_a                   11.067(8)
_cell_length_b                   12.034(9)
_cell_length_c                   17.256(13)
_cell_measurement_reflns_used    4370
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.37
_cell_volume                     2012(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_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      373(2)
_diffrn_measured_fraction_theta_full 0.879
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'CCD area'
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12398
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.8665
_exptl_absorpt_correction_T_min  0.7246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0618
_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/[\s^2^(Fo^2^)+(0.1051P)^2^+2.0928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1778
_reflns_number_gt                6891
_reflns_number_total             8804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7011183sup6.cif
_cod_data_source_block           bejlm52abs
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

 Adding full bibliography for 4333424--4333430.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333427