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_4332686
_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 H36 Cr3 K3 O68 Si W12'
_chemical_formula_weight         3703.94
_chemical_name_common
;           
Tripotassium triaquahexaformatooxotrichromium 
alpha-dodecatungstosilicate dodecahydrate 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.73(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.258(4)
_cell_length_b                   15.764(6)
_cell_length_c                   17.285(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.515
_cell_measurement_theta_min      17.120
_cell_volume                     7245(3)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Softaware (Molecular Structure 
Corporation, 1993)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Softaware (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_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.499
_diffrn_measured_fraction_theta_max 0.499
_diffrn_measurement_device_type
;
RIGAKU AFC-5R automated four-circle 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    0.1152
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_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            10885
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    19.694
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4545
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
teXsan (Molecular Structure Corporation, 1995)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             6588
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.806
_refine_diff_density_min         -2.794
_refine_diff_density_rms         0.451
_refine_ls_extinction_coef       0.000144(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         10885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0539P)^2^+0.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                6014
_reflns_number_total             10885
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic060684xsup2.cif
_cod_data_source_block           c:\shelx\sx97\mizu01
_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 
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4332686