Hybrid Inorganic−Metalorganic Compounds Containing Copper(II)-Monosubstituted Keggin Polyanions and Polymeric Copper(I) Complexes.
San Felices, Leire; Vitoria, Pablo; Gutiérrez-Zorrilla, Juan M.; Lezama, Luis; Reinoso, Santiago; Inorganic Chemistry 45 (2006) 7748–7757; doi:10.1021/ic060762g

data_4332734
_publ_section_title
;
 Hybrid Inorganic&#x2212;Metalorganic Compounds Containing
 Copper(II)-Monosubstituted Keggin Polyanions and Polymeric Copper(I)
 Complexes.
;
_journal_issue                   19
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7748
_journal_page_last               7757
_journal_paper_doi               10.1021/ic060762g
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H56 Cu8 N12 Na4 O88 P2 W22'
_chemical_formula_sum            'C60 H56 Cu8 N12 Na4 O88 P2 W22'
_chemical_formula_weight         7059.87
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-04-13T19:21:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.790(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.253(2)
_cell_length_b                   21.792(1)
_cell_length_c                   27.105(1)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8568
_cell_measurement_theta_min      2.7984
_cell_measurement_wavelength     0.71073
_cell_volume                     12288.7(14)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
        (compiled Sep 23 2004,08:58:26)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
        (compiled Sep 23 2004,08:58:26)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
        (compiled Sep 23 2004,08:58:26)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -54.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000    0.0000    0.0000    0.0000 230

  2 omega  -54.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000   90.0000    0.0000    0.0000 230

  3 omega  -54.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  180.0000    0.0000    0.0000 230

  4 omega  -54.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  270.0000    0.0000    0.0000 230

;
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.0102380489
_diffrn_orient_matrix_UB_12      0.0265162439
_diffrn_orient_matrix_UB_13      -0.0113758675
_diffrn_orient_matrix_UB_21      0.0080112801
_diffrn_orient_matrix_UB_22      0.0144089243
_diffrn_orient_matrix_UB_23      0.0239342497
_diffrn_orient_matrix_UB_31      0.0315167718
_diffrn_orient_matrix_UB_32      -0.0121925271
_diffrn_orient_matrix_UB_33      0.003519571
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.258
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            66667
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    21.997
_exptl_absorpt_correction_T_max  0.53327
_exptl_absorpt_correction_T_min  0.0894
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.24 beta (release 23.09.2004 CrysAlis171 .NET)
        (compiled Sep 23 2004,08:58:26)
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    3.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             12552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.778
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.326
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         21555
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.807
_refine_ls_R_factor_all          0.2097
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.111
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                7074
_reflns_number_total             21555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060762gsup1.cif
_cod_data_source_block           comp4
_cod_database_code               4332734