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_4332732
_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 H48 Cu4 K3 N6 O50 Si1 W11'
_chemical_formula_sum            'C30 H48 Cu4 K3 N6 O50 Si W11'
_chemical_formula_weight         3714.52
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      54
_symmetry_space_group_name_Hall  '-P 2bc 2b'
_symmetry_space_group_name_H-M   'P b c b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-04-12T16:34:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9722(4)
_cell_length_b                   21.5961(7)
_cell_length_c                   28.0216(8)
_cell_measurement_reflns_used    10997
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.8
_cell_measurement_wavelength     0.71073
_cell_volume                     6639.9(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
        (compiled Mar 23 2006,23:39:28)
;
_computing_data_collection
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        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
        (compiled Mar 23 2006,23:39:28)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
        (compiled Mar 23 2006,23:39:28)
;
_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    'DIRDIF99 (Beurskens et al, 1999)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -54.00   60.90   0.3000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000    0.0000    0.0000    0.0000 383

  2 omega  -54.00   60.90   0.3000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000   90.0000    0.0000    0.0000 383

  3 omega  -54.00   60.90   0.3000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  180.0000    0.0000    0.0000 383

  4 omega  -54.00   60.90   0.3000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  270.0000    0.0000    0.0000 383

;
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.0007918136
_diffrn_orient_matrix_UB_12      0.018788319
_diffrn_orient_matrix_UB_13      0.0207867614
_diffrn_orient_matrix_UB_21      0.0493897754
_diffrn_orient_matrix_UB_22      -0.0172624222
_diffrn_orient_matrix_UB_23      0.0095392616
_diffrn_orient_matrix_UB_31      0.0417017239
_diffrn_orient_matrix_UB_32      0.0206818915
_diffrn_orient_matrix_UB_33      -0.0108465448
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            42394
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    20.536
_exptl_absorpt_correction_T_max  0.174
_exptl_absorpt_correction_T_min  0.043
_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            yellow
_exptl_crystal_density_diffrn    3.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6684
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.94
_refine_diff_density_min         -2.054
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.31
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.31
_refine_ls_R_factor_all          0.098
_refine_ls_R_factor_gt           0.0778
_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^)+(0.0132P)^2^+607.8497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                5115
_reflns_number_total             6526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060762gsup1.cif
_cod_data_source_block           comp1
_cod_database_code               4332732