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_4119259
_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
'90(K +),9(C2 H8 N +),(H54 Cu9 Se12 W174 O630 Cl3 99-),246(H2 O)'
_chemical_formula_sum            'C18 H616 Cl3 Cu9 K90 N9 O876 Se12 W174'
_chemical_formula_weight         52113.83
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   46.5979(8)
_cell_length_b                   46.5979(8)
_cell_length_c                   35.8791(11)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      2.27
_cell_volume                     67469(3)
_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 0.768
_diffrn_measured_fraction_theta_max 0.768
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            102203
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    23.380
_exptl_absorpt_correction_T_max  0.4548
_exptl_absorpt_correction_T_min  0.1658
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light cyan'
_exptl_crystal_density_diffrn    3.848
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             69303
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.36
_refine_diff_density_min         -2.18
_refine_diff_density_rms         0.25
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1647
_refine_ls_number_reflns         22653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0725
_reflns_number_gt                16886
_reflns_number_total             22653
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja309237x_si_002_10.cif
_cod_data_source_block           compound10
_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_sg_symbol_H-M      'R -3'
_cod_database_code               4119259