Tetracyanometalates of Ni, Pd, and Pt with Cyclic Diquaternary Cations of 2,2'-Bipyridine and 1,10-Phenanthroline. A Vibrational, Crystallographic, and Theoretical Study of Intermolecular Weak Interactions
Pablo Vitoria; Javier I. Beitia; Juan Manuel Gutiérrez-Zorrilla; Emilio R. Sáiz; Antonio Luque; Maite Insausti; José J. Blanco; Inorganic Chemistry 41 (2002) 4396–4404; doi:10.1021/ic0200287

data_4318379
_publ_contact_author
;
  'Juan Manuel 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         '+34-944 648 500'
_publ_contact_author_phone       '+34-946 015 522'
_publ_section_title
;
 Tetracyanometalates of Ni, Pd, and Pt with Cyclic Diquaternary Cations of
 2,2'-Bipyridine and 1,10-Phenanthroline. A Vibrational, Crystallographic,
 and Theoretical Study of Intermolecular Weak Interactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4396
_journal_page_last               4404
_journal_paper_doi               10.1021/ic0200287
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'aqueous synthesis'
_chemical_formula_moiety         'C4 N4 Ni, C14 H12 N2'
_chemical_formula_sum            'C18 H12 N6 Ni'
_chemical_formula_weight         371.05
_chemical_name_systematic
;
5,6-dihydrodipyrazino[1,2,3,4-lmn]-1,10-phenanthrolinium 
tetracyanonickelate(ii)
;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2a'
_symmetry_space_group_name_H-M   'P m n m :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.555(2)
_cell_length_b                   9.426(2)
_cell_length_c                   12.436(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.54
_cell_measurement_theta_min      6.33
_cell_volume                     768.4(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'CAD4 programs'
_computing_data_reduction        'XCAD (Harms and Wocadlo,1995)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      293(2)
_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_av_R_equivalents  0
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1330
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2
_diffrn_standards_interval_count 98
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.276
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DIFABS (Walker and Stuart, 1983)'
_exptl_crystal_colour            yellow-red
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_meas      1.61(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_all   1.412
_refine_ls_goodness_of_fit_ref   1.332
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/esd_mean        0.004
_refine_ls_shift/su_max          0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1279P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1354
_refine_ls_wR_factor_ref         0.1545
_reflns_number_gt                830
_reflns_number_total             1259
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic0200287_3.cif
_cod_data_source_block           comp4
_cod_original_sg_symbol_H-M      'P m n m'
_cod_original_formula_sum        'C18 H12 N6 Ni1'
_cod_database_code               4318379