Ion-Pair Charge-Transfer Complexes Based on (o-Phenylenebis(oxamato))cuprate(II) and Cyclic Diquaternary Cations of 1,10-Phenanthroline and 2,2'-Bipyridine: Synthesis, Crystal Structure, and Physical Properties
Iosu Unamuno; Juan M. Gutiérrez-Zorrilla; Antonio Luque; Pascual Román; Luis Lezama; Rafael Calvo; Teófilo Rojo; Inorganic Chemistry 37 (1998) 6452–6460; doi:10.1021/ic9805224

data_4323201
_publ_contact_author
;
 Juan M. Gutierrez-Zorrilla, Departamento de Quimica Inorganica.
 Facultad de Ciencias Universidad del Pais Vasco,  Apdo. 644,
 E-48080 Bilbao, Spain
;
_publ_contact_author_email       qipguloj@lg.ehu.es
_publ_contact_author_fax         '+34-94-464 85 00'
_publ_contact_author_phone       '+34-94-464 77 00 ext 2450'
_publ_section_title
;
 Ion-Pair Charge-Transfer Complexes Based on
 (o-Phenylenebis(oxamato))cuprate(II) and Cyclic Diquaternary Cations of
 1,10-Phenanthroline and 2,2'-Bipyridine: Synthesis, Crystal Structure,
 and Physical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6452
_journal_page_last               6460
_journal_paper_doi               10.1021/ic9805224
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        'aqueous synthesis'
_chemical_formula_structural
'Na1,0.5(C12 H12 N2),C10 H4 Cu1 N2 O6,2(H2 O)'
_chemical_formula_sum            'C16 H14 Cu N3 Na O8'
_chemical_formula_weight         462.838
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             25-MAY-98
_audit_creation_method           SHELXL
_cell_angle_alpha                111.01(2)
_cell_angle_beta                 102.71(3)
_cell_angle_gamma                93.57(3)
_cell_formula_units_Z            2
_cell_length_a                   6.732(3)
_cell_length_b                   11.169(3)
_cell_length_c                   12.126(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      7
_cell_volume                     820.2(5)
_computing_cell_refinement       'local programs'
_computing_data_collection       'CAD4 programs'
_computing_data_reduction        'XRAY-76 (Stewart, 1976)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'XRAY-76 (Stewart, 1976)'
_computing_structure_solution    'DIRDIF-92 (Beurskens, 1992)'
_diffrn_ambient_temperature      295(1)
_diffrn_measurement_device       'Enraf nonius CAD4 diffractometer'
_diffrn_measurement_method       '\w/2\q mode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4983
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 98
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.42
_exptl_absorpt_correction_T_max  1.762
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   'empirical (Walker and Stuart, 1989)'
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_meas      1.88(1)
_exptl_crystal_density_method    'flotation CCl4:CHBr3'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.41
_refine_diff_density_min         -0.96
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_all   1.49
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4771
_refine_ls_R_factor_all          0.089
_refine_ls_R_factor_obs          0.065
_refine_ls_shift/esd_max         0.20
_refine_ls_shift/esd_mean        0.04
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      'PESOS (Martinez-Ripoll, 1975)'
_refine_ls_wR_factor_all         0.102
_refine_ls_wR_factor_obs         0.079
_reflns_number_observed          3354
_reflns_number_total             4771
_reflns_observed_criterion       I>3sigma(I)
_cod_data_source_file            ic9805224_2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        820.1(5)
_cod_original_formula_sum        'C16 H14 Cu1 N3 Na1 O8'
_cod_database_code               4323201