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_1515761
_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            'C70 H128 O23 V6'
_chemical_formula_weight         1643.36
_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                96.27(3)
_cell_angle_beta                 91.40(3)
_cell_angle_gamma                90.45(3)
_cell_formula_units_Z            1
_cell_length_a                   11.232(2)
_cell_length_b                   13.693(3)
_cell_length_c                   14.106(3)
_cell_measurement_reflns_used    10272
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      65.999
_cell_measurement_theta_min      7.660
_cell_volume                     2155.8(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SAINT'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'w/ rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SMX station 16.2'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79770
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27728
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         3.83
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.9344
_exptl_absorpt_correction_T_min  0.8202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7070
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0550
_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^)+(0.1057P)^2^+2.2814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1540
_reflns_number_gt                6648
_reflns_number_total             7070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00142b.txt
_cod_data_source_block           test2pb1a
_cod_original_cell_volume        2155.9(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515761