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_1515763
_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            'C62 H98 O11 V2'
_chemical_formula_weight         1121.28
_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                105.9570(10)
_cell_angle_beta                 93.7700(10)
_cell_angle_gamma                95.8850(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2421(8)
_cell_length_b                   14.0373(10)
_cell_length_c                   21.6847(16)
_cell_measurement_reflns_used    15525
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.953
_cell_measurement_theta_min      7.269
_cell_volume                     3257.0(4)
_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     0.78480
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57516
_diffrn_reflns_theta_full        31.53
_diffrn_reflns_theta_max         31.53
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue/black
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         15525
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0960P)^2^+0.9810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                13200
_reflns_number_total             15525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0sc00142b.txt
_cod_data_source_block           testpb1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515763