Formation of a "less stable" polyanion directed and protected by electrophilic internal surface functionalities of a capsule in growth: [{Mo6O19}2– {MoVI72FeIII30O252(ac)20(H2O)92}]4–
Müller, Achim; Todea, Ana Maria; Bögge, Hartmut; van Slageren, Joris; Dressel, Martin; Stammler, Anja; Rusu, Mariana; Chemical Communications (Cambridge, United Kingdom)  (2006) 3066–3068; doi:10.1039/b604977j

data_7101297
_publ_section_title
;
 Formation of a "less stable" polyanion directed and protected by electrophilic
 internal surface functionalities of a capsule in growth:
 [{Mo6O19}2-- {MoVI72FeIII30O252(ac)20(H2O)92}]4--
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   29
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              3066
_journal_page_last               3068
_journal_paper_doi               10.1039/b604977j
_journal_year                    2006
_chemical_formula_moiety
'Na4 [Mo72 Fe30 O252 (CH3COO)20 (H2O)92 (Mo6O19)].120 H2O'
_chemical_formula_sum            'C40 H484 Fe30 Mo78 Na4 O523'
_chemical_formula_weight         18587.05
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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            12
_cell_length_a                   54.6070(17)
_cell_length_b                   54.6070(17)
_cell_length_c                   60.034(3)
_cell_measurement_reflns_used    7416
_cell_measurement_temperature    188(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.18
_cell_volume                     155033(10)
_computing_cell_refinement       'SAINT (Bruker AXS, 2001)'
_computing_data_collection       'SMART (Bruker AXS, 2001)'
_computing_data_reduction        'SAINT (Bruker AXS, 2001)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker AXS SMART 1K'
_diffrn_measurement_method       omega-scan
_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  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            173057
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.763
_exptl_absorpt_correction_T_max  0.6080
_exptl_absorpt_correction_T_min  0.5451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             108096
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3799
_refine_ls_number_reflns         43683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.1851
_refine_ls_R_factor_gt           0.0975
_refine_ls_shift/su_max          0.203
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+13508.1055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2387
_refine_ls_wR_factor_ref         0.3491
_reflns_number_gt                23116
_reflns_number_total             43683
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b604977j.txt
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7101297