"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_4108648
_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         '19(K +), (O134 P3 W39 19-), 30(H2 O)'
_chemical_formula_sum            'H60 K19 O164 P3 W39'
_chemical_formula_weight         10690.44
_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                69.588(4)
_cell_angle_beta                 79.143(3)
_cell_angle_gamma                67.420(4)
_cell_formula_units_Z            2
_cell_length_a                   20.5411(9)
_cell_length_b                   21.1805(11)
_cell_length_c                   22.4460(7)
_cell_measurement_reflns_used    14894
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      3.15
_cell_volume                     8434.1(7)
_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 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Oxford Diffraction Gemini CCD'
_diffrn_measurement_method       '\w $ \p scans'
_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  0.0709
_diffrn_reflns_av_sigmaI/netI    0.1013
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76000
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    27.079
_exptl_absorpt_correction_T_max  0.362
_exptl_absorpt_correction_T_min  0.075
_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    4.210
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             9328
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.56
_refine_diff_density_min         -1.93
_refine_diff_density_rms         0.34
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1805
_refine_ls_number_reflns         26134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                16576
_reflns_number_total             26134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806596j_si_001_3.cif
_cod_data_source_block           compound4a
_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        8434.1(6)
_cod_database_code               4108648