Tetrahydroxy-p-benzoquinone as a Source of Polydentate O-Donor Ligands. Synthesis, Crystal Structure, and Magnetic Properties of the [Cu(bpy)(dhmal)]2 Dimer and the Two-Dimensional [{SiW12O40}{Cu2(bpy)2(H2O)(ox)}2].16H2O Inorganic-Metalorganic Hybrid
Santiago Reinoso; Pablo Vitoria; Leire San Felices; Ainara Montero; Luis Lezama; Juan M. Gutiérrez-Zorrilla; Inorganic Chemistry 46 (2007) 1237–1249; doi:10.1021/ic061671m

data_4307151
_publ_contact_author             'Guti\'errez-Zorrilla, Juan M.'
_publ_contact_author_address
;
Departamento de Qu\'imica Inorg\'anica
Facultad de Ciencia y Tecnolog\'ia
Universidad del Pa\'is Vasco, Apdo. 644, E-48080 Bilbao, Spain
;
_publ_contact_author_email       juanma.zorrilla@ehu.es
_publ_section_title
;
Tetrahydroxy-p-benzoquinone as a Source of Polydentate O-Donor Ligands.
Synthesis, Crystal Structure, and Magnetic Properties of the
[Cu(bpy)(dhmal)]2 Dimer and the Two-Dimensional
[{SiW12O40}{Cu2(bpy)2(H2O)(ox)}2].16H2O Inorganic-Metalorganic Hybrid
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1237
_journal_page_last               1249
_journal_paper_doi               10.1021/ic061671m
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '(C13 H10 Cu1 N2 O6)2'
_chemical_formula_sum            'C26 H20 Cu2 N4 O12'
_chemical_formula_weight         707.56
_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             2006-05-16T16:47:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                60.807(11)
_cell_angle_beta                 68.977(8)
_cell_angle_gamma                88.397(7)
_cell_formula_units_Z            1
_cell_length_a                   8.4965(6)
_cell_length_b                   9.3315(11)
_cell_length_c                   9.7891(10)
_cell_measurement_reflns_used    1592
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.54
_cell_measurement_wavelength     0.71073
_cell_volume                     622.07(14)
_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
;
        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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -54.00   61.00   0.5000   70.0000
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   70.0000
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   70.0000
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   70.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  270.0000    0.0000    0.0000 230

;
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.0702380637
_diffrn_orient_matrix_UB_12      0.0169447173
_diffrn_orient_matrix_UB_13      -0.0250414655
_diffrn_orient_matrix_UB_21      -0.0266886986
_diffrn_orient_matrix_UB_22      0.0443478815
_diffrn_orient_matrix_UB_23      0.0436614247
_diffrn_orient_matrix_UB_31      0.0512054067
_diffrn_orient_matrix_UB_32      0.0747159382
_diffrn_orient_matrix_UB_33      -0.0750524533
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4170
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.791
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
        (compiled Mar 23 2006,23:39:28)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.32
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                1545
_reflns_number_total             2401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061671msi20060904_120536_2.cif
_cod_data_source_block           comp1
_cod_database_code               4307151