Self-Assembly of a Nanosized, Saddle-Shaped, Solution-Stable Polyoxometalate Anion Built from Pentagonal Building Blocks: [H34W119Se8Fe2O420]54-
Jun Yan; Jing Gao; De-Liang Long; Haralampos N. Miras; Leroy Cronin; Journal of the American Chemical Society 132 (2010) 11410–11411; doi:10.1021/ja104043s

data_4102925
_publ_section_title
;
 Self-Assembly of a Nanosized, Saddle-Shaped, Solution-Stable
 Polyoxometalate Anion Built from Pentagonal Building Blocks:
 [H34W119Se8Fe2O420]54-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11410
_journal_page_last               11411
_journal_paper_doi               10.1021/ja104043s
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety
'44(K +), 10(Na +), (H34 W119 Se8 Fe2 O440 54-), 220(H2 O)'
_chemical_formula_sum            'Fe2 H474 K44 Na10 O640 Se8 W119'
_chemical_formula_weight         35289.62
_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                94.990(2)
_cell_angle_beta                 94.485(2)
_cell_angle_gamma                109.091(2)
_cell_formula_units_Z            2
_cell_length_a                   24.8548(3)
_cell_length_b                   33.1678(4)
_cell_length_c                   40.1311(4)
_cell_measurement_reflns_used    113413
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.4
_cell_measurement_theta_min      2.92
_cell_volume                     30944.7(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4383
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            289879
_diffrn_reflns_theta_full        64.54
_diffrn_reflns_theta_max         64.54
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    44.367
_exptl_absorpt_correction_T_max  0.128
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.787
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             31340
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         5.43
_refine_diff_density_min         -2.26
_refine_diff_density_rms         0.44
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5848
_refine_ls_number_reflns         101947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                71639
_reflns_number_total             101947
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja104043s_si_001.cif
_cod_data_source_block           jy4143c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        30944.7(6)
_cod_original_formula_sum        'H474 Fe2 K44 Na10 O640 Se8 W119'
_cod_database_code               4102925