Structure and Properties of the Dendron-Encapsulated Polyoxometalate (C52H60NO12)12[(Mn(H2O))3(SbW9O33)2], a First Generation Dendrizyme
Dirk Volkmer; Björn Bredenkötter; Jörg Tellenbröker; Paul Kögerler; Dirk G. Kurth; Pit Lehmann; Heimo Schnablegger; Dietmar Schwahn; Markus Piepenbrink; Bernt Krebs; Journal of the American Chemical Society 124 (2002) 10489–10496; doi:10.1021/ja017613b

data_4115093
_publ_section_title
;
 Structure and Properties of the Dendron-Encapsulated Polyoxometalate
 (C52H60NO12)12[(Mn(H2O))3(SbW9O33)2], a First Generation Dendrizyme
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10489
_journal_page_last               10496
_journal_paper_doi               10.1021/ja017613b
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'K6 Na6 O92 Sb2 W18 Zn3'
_chemical_formula_weight         5593.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   15.265(2)
_cell_length_b                   15.265(2)
_cell_length_c                   24.461(5)
_cell_measurement_temperature    293(2)
_cell_volume                     4936.3(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.1538
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36960
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         4.27
_exptl_absorpt_coefficient_mu    22.511
_exptl_crystal_density_diffrn    3.763
_exptl_crystal_F_000             4880
_refine_diff_density_max         2.859
_refine_diff_density_min         -4.663
_refine_diff_density_rms         0.529
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.227
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         1832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.227
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+160.8570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                1735
_reflns_number_total             1832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja017613b_s1.cif
_cod_data_source_block           wsbzn
_cod_database_code               4115093