A novel supramolecular organic‒inorganic adduct containing α-Keggin-type [PW~12~O~40~]^3{-^} anions and benzo-15-crown-5 molecules
Almeida Paz, Filipe A.; Sousa, Filipa L.; Soares-Santos, Paula C. R.; Cavaleiro, Ana M. V.; Nogueira, Helena I. S.; Klinowski, Jacek; Trindade, Tito; Acta Crystallographica Section E 60 (2004) m1–m5; doi:10.1107/S1600536803024310

data_2203043
_publ_section_title
;
 A novel supramolecular organic--inorganic adduct containing
 \a-Keggin-type [PW~12~O~40~]^3{-^} anions and benzo-15-crown-5
 molecules
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1
_journal_page_last               m5
_journal_paper_doi               10.1107/S1600536803024310
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac
'(H3 O)3 [P W12 O40], 6C14 H20 O5, C H4 O, H2O'
_chemical_formula_moiety
'3 H3 O +,O40 P W12 3-,6 C14 H20 O5,C H4 O,H2 O'
_chemical_formula_sum            'C85 H135 O75 P W12'
_chemical_formula_weight         4594.10
_chemical_name_systematic
;
tris(hydroxonium)
\m~12~-phosphato-tetracosa-\m~2~-oxo-dodecaoxododecatungsten
hexakis(benzo-15-crown-5)--methanol--water (1/1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 101.66(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.890(3)
_cell_length_b                   42.101(8)
_cell_length_c                   17.393(4)
_cell_measurement_reflns_used    118671
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.00
_cell_volume                     12113(4)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL (Bruker, 2001)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Thin-slice \w and \f'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            71608
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.53
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.463
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 (Sortav; Blessing, 1995)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             8592
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.817
_refine_diff_density_min         -1.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1449
_refine_ls_number_reflns         20465
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0246P)^2^+121.8552P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                16507
_reflns_number_total             20465
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6294.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        12112(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2203043
_cod_database_fobs_code          2203043