Low-valent vanadium catecholate clusters
Scales, Emma; Sorace, Lorenzo; Dei, Andrea; Caneschi, Andrea; Muryn, Christopher A.; Collison, David; McInnes, Eric J. L.; Chemical Science 1 (2010) 221–; doi:10.1039/c0sc00142b

data_1515762
_publ_section_title
;
 Low-valent vanadium catecholate clusters
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              221
_journal_paper_doi               10.1039/c0sc00142b
_journal_volume                  1
_journal_year                    2010
_chemical_formula_sum            'C98 H124 O24 V6'
_chemical_formula_weight         1991.61
_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                 100.286(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.486(4)
_cell_length_b                   28.417(11)
_cell_length_c                   14.966(5)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      46.520
_cell_measurement_theta_min      4.918
_cell_volume                     4806(3)
_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 0.794
_diffrn_measured_fraction_theta_max 0.794
_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  0.1527
_diffrn_reflns_av_sigmaI/netI    0.2416
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10297
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.9571
_exptl_absorpt_correction_T_min  0.7148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            needle
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blue/black
_exptl_crystal_F_000             2042
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0020(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         5527
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.1574
_refine_ls_R_factor_gt           0.0778
_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^)+(0.0681P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                2521
_reflns_number_total             5527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00142b.txt
_cod_data_source_block           test2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1515762