Oxidation-driven self-assembly gives access to high-nuclearity molecular copper vanadium oxide clusters
Forster, Johannes; Rösner, Benedikt; Fink, Rainer H.; Nye, Leanne C.; Ivanovic-Burmazovic, Ivana; Kastner, Katharina; Tucher, Johannes; Streb, Carsten; Chemical Science 4 (2013) 418–; doi:10.1039/c2sc20942j

data_1514846
_publ_section_title
;
 Oxidation-driven self-assembly gives access to high-nuclearity molecular
 copper vanadium oxide clusters
;
_journal_issue                   1
_journal_name_full               'Chemical Science'
_journal_page_first              418
_journal_paper_doi               10.1039/c2sc20942j
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C10 H30 N2 O12 S5 V'
_chemical_formula_weight         581.60
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                67.27(3)
_cell_angle_beta                 77.71(2)
_cell_angle_gamma                89.25(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4145(19)
_cell_length_b                   11.119(2)
_cell_length_c                   13.183(2)
_cell_measurement_reflns_used    125
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      3.6
_cell_volume                     1240.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Kappa Nonius CCD'
_diffrn_measurement_method       'Omega and Phi Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13758
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.85
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Kappa Nonius CCD'
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0205P)^2^+1.2451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                4469
_reflns_number_total             4904
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2sc20942j.txt
_cod_data_source_block           CS1137
_cod_original_cell_volume        1240.0(4)
_cod_database_code               1514846