Synergetic activation of "silent receptor" sites leading to a new type of inclusion complex: integration of a 64-membered ring comprising K+ and SO~4~^2-^ ions into a molybdenum oxide-based nanoobject
Müller, Achim; Toma, Liviu; Bögge, Hartmut; Schmidtmann, Marc; Kögerler, Paul; Chemical Communications (Cambridge, United Kingdom)  (2003) 2000–2001; doi:10.1039/b305447k

data_7103847
_publ_section_title
;
 Synergetic activation of "silent receptor" sites leading to a new type of
 inclusion complex: integration of a 64-membered ring comprising K+ and
 SO~4~^2-^ ions into a molybdenum oxide-based nanoobject
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   16
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2000
_journal_page_last               2001
_journal_paper_doi               10.1039/b305447k
_journal_year                    2003
_chemical_formula_sum            'H1100 K30 Mo146 Na16 O1043 S16'
_chemical_formula_weight         33857.84
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   51.726(2)
_cell_length_b                   51.726(2)
_cell_length_c                   21.7465(11)
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.18
_cell_volume                     58185.4(41)
_computing_cell_refinement       'Bruker AXS SAINT'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics
'Crystal Impact: DIAMOND; Bruker AXS: SHELXTL'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Bruker AXS SMART'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1144
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            159990
_diffrn_reflns_theta_max         20.04
_diffrn_reflns_theta_min         1.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.768
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             33156
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.166
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2002
_refine_ls_number_reflns         27037
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.166
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_obs          0.0843
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0700P)^2^+2300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2394
_refine_ls_wR_factor_obs         0.1961
_reflns_number_observed          16975
_reflns_number_total             27280
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b305447k.txt
_cod_data_source_block           moox
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0700P)^2^+2300.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0700P)^2^+2300.0000P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7103847