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_4332733
_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         'C30 H47 Cu1 K1 N5 O45 Si1 W11'
_chemical_formula_sum            'C30 H47 Cu K N5 O45 Si W11'
_chemical_formula_weight         3350.67
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-04-13T18:49:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                87.227(6)
_cell_angle_beta                 85.004(5)
_cell_angle_gamma                84.328(6)
_cell_formula_units_Z            2
_cell_length_a                   10.8974(7)
_cell_length_b                   13.1029(10)
_cell_length_c                   21.4442(13)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7955
_cell_measurement_theta_min      3.1209
_cell_measurement_wavelength     0.71073
_cell_volume                     3033.0(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
        (compiled Apr  1 2005,17:53:34)
;
_computing_data_collection
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        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
        (compiled Apr  1 2005,17:53:34)
;
_computing_data_reduction
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        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
        (compiled Apr  1 2005,17:53:34)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
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_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_details
;
  1 omega  -54.00   61.00   0.5000   20.0000
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   20.0000
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   20.0000
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   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  270.0000    0.0000    0.0000 230

;
_diffrn_measurement_device_type  Xcalibur
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_diffrn_orient_matrix_UB_12      0.0086767785
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_diffrn_orient_matrix_UB_22      0.008557628
_diffrn_orient_matrix_UB_23      0.0083167598
_diffrn_orient_matrix_UB_31      0.0192206507
_diffrn_orient_matrix_UB_32      -0.0530615084
_diffrn_orient_matrix_UB_33      -0.0025353806
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0541
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_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20408
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    21.304
_exptl_absorpt_correction_T_max  0.46299
_exptl_absorpt_correction_T_min  0.17983
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
        (compiled Apr  1 2005,17:53:34)
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.825
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.813
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         11678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.813
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                6032
_reflns_number_total             11678
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060762gsup1.cif
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