Unravelling the Complexities of Polyoxometalates in Solution Using Mass Spectrometry: Protonation versus Heteroatom Inclusion
De-Liang Long; Carsten Streb; Yu-Fei Song; Scott Mitchell; Leroy Cronin; Journal of the American Chemical Society 130 (2008) 1830–1832; doi:10.1021/ja075940z

data_4107402
_publ_section_title
;
 Unravelling the Complexities of Polyoxometalates in Solution Using Mass
 Spectrometry: Protonation versus Heteroatom Inclusion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1830
_journal_page_last               1832
_journal_paper_doi               10.1021/ja075940z
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C102 H225 N9 O62 P2 W18'
_chemical_formula_weight         5941.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           31
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   geom
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   26.780(4)
_cell_length_b                   15.516(2)
_cell_length_c                   19.956(3)
_cell_measurement_reflns_used    5205
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_volume                     8292(2)
_computing_cell_refinement       'Apex 2'
_computing_data_collection       'Apex 2'
_computing_data_reduction        'Apex 2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Apex2'
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28029
_diffrn_reflns_theta_full        23.02
_diffrn_reflns_theta_max         23.02
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    12.521
_exptl_absorpt_correction_T_max  0.3674
_exptl_absorpt_correction_T_min  0.1885
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5516
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.47
_refine_diff_density_min         -1.17
_refine_diff_density_rms         0.22
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.015(19)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10851
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0591P)^2^+86.4389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                9450
_reflns_number_total             10851
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075940z-file003.cif
_cod_data_source_block           TBA6P2W18O62
_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        8292.0(19)
_cod_database_code               4107402