Synthesis and Characterization of a Metal-to-Polyoxometalate Charge Transfer Molecular Chromophore
Chongchao Zhao; Zhuangqun Huang; William Rodríguez-Córdoba; Choon Sung Kambara; Kevin P. O'Halloran; Ken I. Hardcastle; Djamaladdin G. Musaev; Tianquan Lian; Craig L. Hill; Journal of the American Chemical Society 133 (2011) 20134–20137; doi:10.1021/ja209360x

data_4107230
_publ_section_title
;
 Synthesis and Characterization of a Metal-to-Polyoxometalate Charge
 Transfer Molecular Chromophore
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20134
_journal_page_last               20137
_journal_paper_doi               10.1021/ja209360x
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C6 K15 Na O156.50 P4 Re2 W35'
_chemical_formula_sum            'C6 K15 Na O156.5 P4 Re2 W35'
_chemical_formula_weight         10116.58
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.326(4)
_cell_angle_beta                 97.652(4)
_cell_angle_gamma                92.667(4)
_cell_formula_units_Z            2
_cell_length_a                   12.819(3)
_cell_length_b                   22.511(6)
_cell_length_c                   25.188(6)
_cell_measurement_reflns_used    3782
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.24
_cell_volume                     7069(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1886
_diffrn_reflns_av_sigmaI/netI    0.2096
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            119590
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    30.669
_exptl_absorpt_correction_T_max  0.4220
_exptl_absorpt_correction_T_min  0.0457
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.753
_exptl_crystal_description       plate
_exptl_crystal_F_000             8768
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.332
_refine_diff_density_min         -3.789
_refine_diff_density_rms         0.749
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         33843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1750
_refine_ls_R_factor_gt           0.0729
_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^)+(0.0110P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1721
_reflns_number_gt                16073
_reflns_number_total             33843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja209360x_si_002.cif
_cod_data_source_block           zcc_4_25
_cod_original_cell_volume        7068(3)
_cod_original_formula_sum        'C6 K15 Na O156.50 P4 Re2 W35'
_cod_database_code               4107230