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_4310229
_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            'C44 H70 Cu5 K2 N8 O66 Si W11'
_chemical_formula_weight         4213.4
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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             2005-03-16T20:31:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.777(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4871(11)
_cell_length_b                   20.5817(16)
_cell_length_c                   18.6197(16)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      1.95
_cell_measurement_wavelength     0.71073
_cell_volume                     4684.6(7)
_computing_cell_refinement       'Stoe IPDS Software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS Software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_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_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDS area detector diffractometer'
_diffrn_measurement_method       '200 exposures, \D \f 1.0\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focused sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2121
_diffrn_reflns_av_unetI/netI     0.3724
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30361
_diffrn_reflns_theta_full        25.88
_diffrn_reflns_theta_max         25.88
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    14.763
_exptl_absorpt_correction_T_max  0.592
_exptl_absorpt_correction_T_min  0.082
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3814
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.443
_refine_diff_density_min         -2.776
_refine_diff_density_rms         0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.681
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         9265
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      0.68
_refine_ls_R_factor_all          0.2252
_refine_ls_R_factor_gt           0.0749
_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^)+(0.0728P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1982
_reflns_number_gt                2373
_reflns_number_total             9265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051134msi20051026_104735_2.cif
_cod_data_source_block           comp1
_cod_database_code               4310229