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_4310230
_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 H148 Cu7 K14 N8 O183 Si3 W33'
_chemical_formula_weight         10861.1
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-A 2y'
_symmetry_space_group_name_H-M   'A 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2005-07-07T16:15:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.546(2)
_cell_length_b                   21.303(3)
_cell_length_c                   37.932(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      7.7
_cell_measurement_wavelength     0.71073
_cell_volume                     9737(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.011567
_diffrn_orient_matrix_UB_12      -0.000511
_diffrn_orient_matrix_UB_13      -0.062337
_diffrn_orient_matrix_UB_21      -0.024825
_diffrn_orient_matrix_UB_22      0.000229
_diffrn_orient_matrix_UB_23      -0.054616
_diffrn_orient_matrix_UB_31      0.000214
_diffrn_orient_matrix_UB_32      0.046823
_diffrn_orient_matrix_UB_33      -0.000216
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.1158
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            15207
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        9
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    20.586
_exptl_absorpt_correction_T_max  0.8146
_exptl_absorpt_correction_T_min  0.2508
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        (see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9770
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.933
_refine_diff_density_min         -5.004
_refine_diff_density_rms         0.532
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         14587
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1674
_refine_ls_R_factor_gt           0.0705
_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^)+(0.1185P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1991
_reflns_number_gt                7948
_reflns_number_total             14586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051134msi20051026_104735_3.cif
_cod_data_source_block           comp2
_cod_database_code               4310230
_exptl_absorpt_correction_t_ave  0.6724
_diffrn_standards_decay_corr_max 1.156
_diffrn_standards_decay_corr_min 0.944