"Bottom-Up" Meets "Top-Down" Assembly in Nanoscale Polyoxometalate Clusters: Self-Assembly of [P4W52O178]24- and Disassembly to [P3W39O134]19-
Chullikkattil P. Pradeep; De-Liang Long; Carsten Streb; Leroy Cronin; Journal of the American Chemical Society 130 (2008) 14946–14947; doi:10.1021/ja806596j

data_4108647
_publ_section_title
;
 "Bottom-Up" Meets "Top-Down" Assembly in Nanoscale Polyoxometalate
 Clusters: Self-Assembly of [P4W52O178]24- and Disassembly to
 [P3W39O134]19-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14946
_journal_page_last               14947
_journal_paper_doi               10.1021/ja806596j
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '20(K +), (P4 W44 O152 20-), 48(H2 O)'
_chemical_formula_sum            'H96 K20 O200 P4 W44'
_chemical_formula_weight         12292.05
_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                76.332(2)
_cell_angle_beta                 88.495(2)
_cell_angle_gamma                65.954(3)
_cell_formula_units_Z            2
_cell_length_a                   18.8407(5)
_cell_length_b                   19.7247(7)
_cell_length_c                   29.5038(8)
_cell_measurement_reflns_used    26575
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.05
_cell_volume                     9699.0(6)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD'
_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    0.0555
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            120026
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    26.551
_exptl_absorpt_correction_T_max  0.035
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.209
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             10784
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.99
_refine_diff_density_min         -2.33
_refine_diff_density_rms         0.32
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2344
_refine_ls_number_reflns         33939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                24556
_reflns_number_total             33939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806596j_si_001_2.cif
_cod_data_source_block           compound2
_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        9699.0(5)
_cod_database_code               4108647