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_4122503
_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            'Fe3 H54 K10 O95 Si2 W18'
_chemical_formula_weight         5498.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                77.370(2)
_cell_angle_beta                 89.658(2)
_cell_angle_gamma                72.081(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6679(2)
_cell_length_b                   18.3023(4)
_cell_length_c                   19.2853(4)
_cell_measurement_reflns_used    24640
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.1490
_cell_measurement_theta_min      3.2040
_cell_volume                     4142.43(15)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            67128
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.839
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    26.048
_exptl_absorpt_correction_T_max  0.242
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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            brown
_exptl_crystal_density_diffrn    4.408
_exptl_crystal_description       needle
_exptl_crystal_F_000             4884
_exptl_crystal_size_max          0.1142
_exptl_crystal_size_mid          0.0975
_exptl_crystal_size_min          0.0776
_refine_diff_density_max         2.447
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         16268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+40.6426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13973
_reflns_number_total             16268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5067916_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4122497--4122503.cif.'
_cod_original_formula_sum        'H54 Fe3 K10 O95 Si2 W18'
_cod_database_code               4122503
_shelxl_version_number           2013-4
_shelx_res_checksum              90545
_shelx_hkl_checksum              56028