One-Pot versus Sequential Reactions in the Self-Assembly of Gigantic Nanoscale Polyoxotungstates
Jing Gao; Jun Yan; Sebastian Beeg; De-Liang Long; Leroy Cronin; Journal of the American Chemical Society 135 (2013) 1796–1805; doi:10.1021/ja309237x

data_4119252
_publ_section_title
;
 One-Pot versus Sequential Reactions in the Self-Assembly of Gigantic
 Nanoscale Polyoxotungstates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1796
_journal_page_last               1805
_journal_paper_doi               10.1021/ja309237x
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'28(K +),11(C2 H8 N +),0.25(Co 2+),(H10.5 Co Se8 W87 O303 39.5-) 98(H2 O)'
_chemical_formula_sum            'C22 H294.5 Co1.25 K28 N11 O402 Se8 W87'
_chemical_formula_weight         24942.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.3740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.7948(8)
_cell_length_b                   42.6071(13)
_cell_length_c                   32.5874(9)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.27
_cell_volume                     39481(2)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II Quasar 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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0664
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_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            315612
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         0.94
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    26.435
_exptl_absorpt_correction_T_max  0.177
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    4.196
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             43981
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.21
_refine_diff_density_min         -5.16
_refine_diff_density_rms         0.46
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4198
_refine_ls_number_reflns         77563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+2915.2334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                56074
_reflns_number_total             77563
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja309237x_si_002_03.cif
_cod_data_source_block           compound3
_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        39481.3(19)
_cod_original_formula_sum        'C22 H294.50 Co1.25 K28 N11 O402 Se8 W87'
_cod_database_code               4119252