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_4107401
_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_moiety
'6(C16 H36 N +), (H5 P W18 O62 6-), 3(C2 H3 N)'
_chemical_formula_sum            'C102 H230 N9 O62 P W18'
_chemical_formula_weight         5915.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 102.469(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.239(3)
_cell_length_b                   15.9238(17)
_cell_length_c                   33.430(4)
_cell_measurement_reflns_used    6971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.39
_cell_volume                     16237(3)
_computing_cell_refinement       Bruker
_computing_data_collection       Bruker
_computing_data_reduction        Bruker
_computing_molecular_graphics    Diamond
_computing_publication_material  Wingx
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker Apex 2 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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            102773
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    12.779
_exptl_absorpt_correction_T_max  0.5144
_exptl_absorpt_correction_T_min  0.1359
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.420
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             10992
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.92
_refine_diff_density_min         -2.38
_refine_diff_density_rms         0.25
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         30338
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+237.1901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                22153
_reflns_number_total             30338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075940z-file002.cif
_cod_data_source_block           dl221
_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_database_code               4107401