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_4119257
_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
'36(K +),19(C2 H8 N +),(H33 Zn2 Se8 W118 O416 55-),168(H2 O)'
_chemical_formula_sum            'C39.5 H521 K36 N19 O580 Se8 W118 Zn2'
_chemical_formula_weight         34410.07
_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                74.163(2)
_cell_angle_beta                 77.371(2)
_cell_angle_gamma                72.630(2)
_cell_formula_units_Z            2
_cell_length_a                   24.2676(7)
_cell_length_b                   34.0705(10)
_cell_length_c                   38.7161(11)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.46
_cell_measurement_theta_min      2.26
_cell_volume                     29061.6(15)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            341532
_diffrn_reflns_theta_full        24.02
_diffrn_reflns_theta_max         24.02
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    24.205
_exptl_absorpt_correction_T_max  0.1957
_exptl_absorpt_correction_T_min  0.1220
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.932
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             30558
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.01
_refine_diff_density_min         -4.15
_refine_diff_density_rms         0.60
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5718
_refine_ls_number_reflns         90292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0710P)^2^+1731.9398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.2019
_reflns_number_gt                55203
_reflns_number_total             90292
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja309237x_si_002_08.cif
_cod_data_source_block           compound8
_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_formula_sum        'C39.50 H521 K36 N19 O580 Se8 W118 Zn2'
_cod_database_code               4119257