Coexistence of Five Different Copper(II)-Phenanthroline Species in the Crystal Packing of Inorganic-Metalorganic Hybrids Based on Keggin Polyoxometalates and Copper(II)-Phenanthroline-Oxalate Complexes
Santiago Reinoso; Pablo Vitoria; Juan M. Gutiérrez-Zorrilla; Luis Lezama; Juan M. Madariaga; Leire San Felices; Amaia Iturrospe; Inorganic Chemistry 46 (2007) 4010–4021; doi:10.1021/ic062367w

data_4307857
_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
;
Coexistence of Five Different Copper(II)-Phenanthroline Species in the
Crystal Packing of Inorganic-Metalorganic Hybrids Based on Keggin
Polyoxometalates and Copper(II)-Phenanthroline-Oxalate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4010
_journal_page_last               4021
_journal_paper_doi               10.1021/ic062367w
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C104 H148 Cu10 N20 O128 Si2 W22'
_chemical_formula_sum            'C104 H148 Cu10 N20 O128 Si2 W22'
_chemical_formula_weight         8462.7
_chemical_name_systematic
;
 ?
;
_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             2006-10-03T13:47:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                71.256(2)
_cell_angle_beta                 86.863(2)
_cell_angle_gamma                71.429(2)
_cell_formula_units_Z            1
_cell_length_a                   13.1529(3)
_cell_length_b                   16.9438(3)
_cell_length_c                   23.0200(5)
_cell_measurement_reflns_used    9488
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.8
_cell_volume                     4598.70(19)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_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 (Beurskens, 1999)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -54.00   60.90   0.3000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000    0.0000    0.0000    0.0000 383

  2 omega  -54.00   60.90   0.3000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000   90.0000    0.0000    0.0000 383

  3 omega  -54.00   60.90   0.3000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  180.0000    0.0000    0.0000 383

  4 omega  -54.00   60.90   0.3000   20.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -79.0000  270.0000    0.0000    0.0000 383

;
_diffrn_orient_matrix_UB_11      -0.0315912639
_diffrn_orient_matrix_UB_12      0.0445356384
_diffrn_orient_matrix_UB_13      -0.013675797
_diffrn_orient_matrix_UB_21      0.0261210269
_diffrn_orient_matrix_UB_22      0.0124679503
_diffrn_orient_matrix_UB_23      0.0200959712
_diffrn_orient_matrix_UB_31      0.0395632265
_diffrn_orient_matrix_UB_32      0.0059623043
_diffrn_orient_matrix_UB_33      -0.0216988611
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.1381
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34858
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    14.949
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.085
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    3.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3882
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.029
_refine_diff_density_max         3.67
_refine_diff_density_min         -2.981
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         20550
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                10181
_reflns_number_total             20550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062367w-file003_1.cif
_cod_data_source_block           Comp2
_cod_database_code               4307857