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_4307150
_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_sum            'C44 H68 Cu4 N8 O66 Si W12'
_chemical_formula_weight         4253.5
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2005-03-16T20:54:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 104.440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4400(10)
_cell_length_b                   13.4230(10)
_cell_length_c                   23.497(3)
_cell_measurement_reflns_used    6138
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     4410.5(7)
_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      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   60.80   0.4000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000    0.0000    0.0000    0.0000 287

  2 omega  -54.00   60.80   0.4000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000   90.0000    0.0000    0.0000 287

  3 omega  -54.00   60.80   0.4000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  180.0000    0.0000    0.0000 287

  4 omega  -54.00   60.80   0.4000   25.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       26.0000  -79.0000  270.0000    0.0000    0.0000 287

;
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.0183279728
_diffrn_orient_matrix_UB_12      -0.0440924693
_diffrn_orient_matrix_UB_13      -0.0098176262
_diffrn_orient_matrix_UB_21      -0.0450359986
_diffrn_orient_matrix_UB_22      -0.0090494471
_diffrn_orient_matrix_UB_23      -0.0198027616
_diffrn_orient_matrix_UB_31      0.0144451156
_diffrn_orient_matrix_UB_32      0.0276824260
_diffrn_orient_matrix_UB_33      -0.0219808235
_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  0.0772
_diffrn_reflns_av_unetI/netI     0.2121
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26244
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    16.645
_exptl_absorpt_correction_T_max  0.5879
_exptl_absorpt_correction_T_min  0.1773
_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    3.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3868
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.035
_refine_diff_density_max         1.63
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         8646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.2079
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                3829
_reflns_number_total             8646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061671msi20060904_120536_1.cif
_cod_data_source_block           comp5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4307150