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_4119253
_publ_section_title
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 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
'23(K +), 3(Na +), 17(C2 H8 N +), (H20 Ni2 Se8 W91 O322 Cl 43-), 158(H2 O)'
_chemical_formula_sum            'C34 H472 Cl K23 N17 Na3 Ni2 O480 Se8 W91'
_chemical_formula_weight         27285.46
_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                108.952(3)
_cell_angle_beta                 104.631(3)
_cell_angle_gamma                101.886(3)
_cell_formula_units_Z            2
_cell_length_a                   23.7964(13)
_cell_length_b                   27.8126(16)
_cell_length_c                   41.466(2)
_cell_measurement_reflns_used    9174
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.16
_cell_volume                     23838(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker ApexII 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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0912
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            336217
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    22.874
_exptl_absorpt_correction_T_max  0.3407
_exptl_absorpt_correction_T_min  0.1420
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light greeen'
_exptl_crystal_density_diffrn    3.801
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             24368
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.13
_refine_diff_density_min         -4.20
_refine_diff_density_rms         0.40
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4097
_refine_ls_number_reflns         93534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+1088.9061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                56897
_reflns_number_total             93534
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja309237x_si_002_04.cif
_cod_data_source_block           compound4
_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 
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_cod_database_code               4119253