A novel acetated 54-member crown-shaped polyoxomolybdate with unprecedented structural features: Na26[{Na(H2O)2}6({μ3-OH)4MoV20MoVI34O164(μ2-CH3COO)4}]·≈120H2O
Yang, Wenbin; Lu, Canzhong; Lin, Xiang; Zhuang, Honghui; Chemical Communications  (2000) 1623–; doi:10.1039/b004948o

data_7111037
_publ_section_title
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 A novel acetated 54-member crown-shaped polyoxomolybdate with
 unprecedented structural features:
 Na26[{Na(H2O)2}6({\m3-OH)4MoV20MoVI34O164(\m2-CH3COO)4}]&#x00B7;&#x2248;120H2O
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_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1623
_journal_paper_doi               10.1039/b004948o
_journal_year                    2000
_chemical_formula_sum            'C8 H280 Mo54 Na32 O308'
_chemical_formula_weight         11222.76
_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                90.0210(10)
_cell_angle_beta                 102.6470(10)
_cell_angle_gamma                100.41
_cell_formula_units_Z            1
_cell_length_a                   17.6814(6)
_cell_length_b                   19.8620(7)
_cell_length_c                   23.4663(8)
_cell_measurement_temperature    293(2)
_cell_volume                     7901.9(5)
_computing_cell_refinement       'Simens CCD SAINT'
_computing_data_collection       'Simens SMART CCD'
_computing_data_reduction        'Simens CCD SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Simens CCD SMART'
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41201
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         0.89
_exptl_absorpt_coefficient_mu    2.227
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.604480
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'Black red'
_exptl_crystal_density_diffrn    2.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5412
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.306
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1323
_refine_ls_number_reflns         27539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.0718
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1969
_refine_ls_wR_factor_ref         0.2434
_reflns_number_gt                16425
_reflns_number_total             27539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004948osup1.cif
_cod_data_source_block           Mo54
_cod_original_cell_volume        7902.0(5)
_cod_original_sg_symbol_H-M      P(-1)
_cod_database_code               7111037