Recognition of Small Polar Molecules with an Ionic Crystal of α-Keggin-Type Polyoxometalate with a Macrocation
Uchida, Sayaka; Kawamoto, Ryosuke; Mizuno, Noritaka; Inorganic Chemistry 45 (2006) 5136–5144; doi:10.1021/ic060684x

data_4332687
_publ_section_title
;
 Recognition of Small Polar Molecules with an Ionic Crystal of
 \a-Keggin-Type Polyoxometalate with a Macrocation
;
_journal_issue                   13
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5136
_journal_page_last               5144
_journal_paper_doi               10.1021/ic060684x
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C6 H44 B Cr3 O72 Rb4 W12'
_chemical_formula_weight         3983.30
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   24.680(10)
_cell_length_b                   16.137(5)
_cell_length_c                   17.281(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.30
_cell_measurement_theta_min      17.44
_cell_volume                     6882(5)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure 
Corporation, 1993)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure 
Corporation, 1993)
;
_computing_data_reduction
;
teXsan (Molecular Structure Corporation, 1995)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type
;
RIGAKU four-cricle automatic X-ray diffractometer
;
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2719
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10375
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        -8.5
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    23.352
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3167
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             7076
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.511
_refine_diff_density_min         -3.168
_refine_diff_density_rms         0.512
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         10375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.2496
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                3879
_reflns_number_total             10375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060684xsup3.cif
_cod_data_source_block           '__3a'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'psiscan' changed to
'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] 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^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4332687