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_4333426
_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            'C36 H46 O16 V4'
_chemical_formula_weight         938.49
_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                 102.773(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2831(3)
_cell_length_b                   11.1266(4)
_cell_length_c                   19.4966(7)
_cell_measurement_reflns_used    3133
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.7546
_cell_measurement_theta_min      2.8114
_cell_volume                     1963.96(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET)
(compiled Jan 13 2006,17:25:00)
;
_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_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Oxford Diffraction Xcaliber 2'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5126
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         3.89
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.6363
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+1.9234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                2282
_reflns_number_total             2562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7011183sup5.cif
_cod_data_source_block           oejlm66p21nsad
_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 2.4.2 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      P2(1)/n
_cod_database_code               4333426