Controlling the minimal self assembly of "complex" polyoxometalate clusters.
Winter, Ross S.; Cameron, Jamie M.; Cronin, Leroy; Journal of the American Chemical Society 136 (2014) 12753–12761; doi:10.1021/ja5067916

data_4122498
_publ_section_title
;
 Controlling the minimal self assembly of &quot;complex&quot;
 polyoxometalate clusters.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12753
_journal_page_last               12761
_journal_paper_doi               10.1021/ja5067916
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'Cl Fe3.5 H51.5 K5 Li6 O83.5 Si1.5 W15'
_chemical_formula_weight         4655.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                106.343(3)
_cell_angle_beta                 101.315(3)
_cell_angle_gamma                109.851(3)
_cell_formula_units_Z            4
_cell_length_a                   20.2088(8)
_cell_length_b                   22.0401(6)
_cell_length_c                   22.1265(9)
_cell_measurement_reflns_used    22034
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2652
_cell_measurement_theta_min      2.7855
_cell_volume                     8417.5(6)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            134497
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.791
_diffrn_source                   'Enhance (Mo) X-ray source'
_exptl_absorpt_coefficient_mu    21.401
_exptl_absorpt_correction_T_max  0.316
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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            yellow
_exptl_crystal_density_diffrn    3.674
_exptl_crystal_description       block
_exptl_crystal_F_000             8286
_exptl_crystal_size_max          0.1874
_exptl_crystal_size_mid          0.1332
_exptl_crystal_size_min          0.0547
_refine_diff_density_max         2.352
_refine_diff_density_min         -2.440
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1900
_refine_ls_number_reflns         33033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+22.5729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22024
_reflns_number_total             33033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5067916_si_008.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4122497--4122503.cif.'
_cod_original_formula_sum        'H51.50 Cl Fe3.50 K5 Li6 O83.50 Si1.50 W15'
_cod_database_code               4122498
_shelxl_version_number           2013-4
_shelx_res_checksum              19017
_shelx_hkl_checksum              53090