A high-nuclearity, beyond "fully reduced" polyoxo(alkoxo)vanadium(III/IV) cage
Tidmarsh, Ian S.; Laye, Rebecca H.; Brearley, Paul R.; Shanmugam, Maheswaran; Sañudo, E. Carolina; Sorace, Lorenzo; Caneschi, Andrea; McInnes, Eric J. L.; Chemical Communications (Cambridge, United Kingdom)  (2006) 2560–2562; doi:10.1039/b605106e

data_7101228
_publ_section_title
;
 A high-nuclearity, beyond "fully reduced" polyoxo(alkoxo)vanadium(III/IV) cage
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   24
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2560
_journal_page_last               2562
_journal_paper_doi               10.1039/b605106e
_journal_year                    2006
_chemical_formula_sum            'C96 H164 O56 V18'
_chemical_formula_weight         3131.19
_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                74.367(7)
_cell_angle_beta                 87.552(7)
_cell_angle_gamma                65.633(9)
_cell_formula_units_Z            1
_cell_length_a                   14.0361(13)
_cell_length_b                   16.0288(13)
_cell_length_c                   16.2151(12)
_cell_measurement_reflns_used    5256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0176
_cell_measurement_theta_min      2.6114
_cell_volume                     3190.4(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++)
(compiled Nov 6 2003,09:43:27)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++)
(compiled Nov 6 2003,09:43:27)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.12 beta (release 06.11.2003 CrysAlis171 VC++)
(compiled Nov 6 2003,09:43:27)
;
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 2'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15920
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.62
_exptl_absorpt_coefficient_mu    1.33279
_exptl_absorpt_correction_T_max  0.85466
_exptl_absorpt_correction_T_min  0.49442
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.23 beta (release 19.07.2004 CrysAlis171 .NET)
(compiled Jul 19 2004,21:00:49)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         7765
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0902
_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^)+(0.1914P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2386
_refine_ls_wR_factor_ref         0.2793
_reflns_number_gt                4785
_reflns_number_total             7765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605106e.txt
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101228