Inorganic-Metalorganic Hybrids Based on Copper(II)-Monosubstituted Keggin Polyanions and Dinuclear Copper(II)-Oxalate Complexes. Synthesis, X-ray Structural Characterization, and Magnetic Properties
Santiago Reinoso; Pablo Vitoria; Juan M. Gutiérrez-Zorrilla; Luis Lezama; Leire San Felices; Javier I. Beitia; Inorganic Chemistry 44 (2005) 9731–9742; doi:10.1021/ic051134m

data_4310231
_publ_contact_author             'Guti\'errez-Zorrilla, Juan M.'
_publ_contact_author_address
;
Departamento de Qu\'imica Inorg\'anica. Facultad de Ciencias
Universidad del Pa\'is Vasco,  Apdo. 644, E-48080 Bilbao, Spain
;
_publ_contact_author_email       qipguloj@lg.ehu.es
_publ_contact_author_fax         '+34 94 4648500'
_publ_contact_author_phone       '+34 94 6015522'
_publ_section_title
;
Inorganic-Metalorganic Hybrids Based on Copper(II)-Monosubstituted Keggin
Polyanions and Dinuclear Copper(II)-Oxalate Complexes. Synthesis, X-ray
Structural Characterization, and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9731
_journal_page_last               9742
_journal_paper_doi               10.1021/ic051134m
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_sum            'C22 H54 Cu3 N8 O54 Si W11'
_chemical_formula_weight         3535.8
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2005-03-19T23:49:09-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.194(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6937(5)
_cell_length_b                   18.9350(10)
_cell_length_c                   26.9340(10)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     6473.7(5)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
;
_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    'DIRDIF99.2 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1024 \\times 1024 with blocks 2 \\times 2'
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40536
_diffrn_reflns_theta_full        27.9
_diffrn_reflns_theta_max         27.9
_diffrn_reflns_theta_min         2.77
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    20.560
_exptl_absorpt_correction_T_max  0.4361
_exptl_absorpt_correction_T_min  0.0690
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6356
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.002
_refine_diff_density_min         -3.151
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         13886
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.103
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.091
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                7481
_reflns_number_total             13886
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051134msi20051026_104735_4.cif
_cod_data_source_block           comp3
_cod_database_code               4310231