Trinuclear Nickel(II) Complex through a 2,3,5,6-Tetrakis(2-pyridyl)pyrazine Ligand with a Linear Exchange Pathway
Lorena M. Callejo; Gotzon Madariaga; Luis Lezama; Luz Fidalgo; Noelia De la Pinta; Roberto Cortés; Inorganic Chemistry 49 (2010) 5353–5355; doi:10.1021/ic100562e

data_4315802
_publ_contact_author_address
;Departamento de Qu\'imica Inorganica
 Facultad de Farmacia
 Apartado 450
 01080 Bilbao, Spain
;
_publ_contact_author_email       roberto.cortes@ehu.es
_publ_contact_author_name        'Cort\'es, Roberto'
_publ_section_title
;
 Trinuclear Nickel(II) Complex through a
 2,3,5,6-Tetrakis(2-pyridyl)pyrazine Ligand with a Linear Exchange Pathway
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5353
_journal_page_last               5355
_journal_paper_doi               10.1021/ic100562e
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'                           C50 H40 N14 Ni3 O4 S2, 4(N O3), 4(O)'
_chemical_formula_sum            'C50 H40 N18 Ni3 O20 S2'
_chemical_formula_weight         1453.25
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-11-14T19:33:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.856(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1116(12)
_cell_length_b                   10.8127(5)
_cell_length_c                   25.2294(13)
_cell_measurement_reflns_used    6044
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.917
_cell_measurement_theta_min      2.7221
_cell_measurement_wavelength     0.71073
_cell_volume                     6111.5(6)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
        (compiled Nov 11 2005,15:50:43)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
        (compiled Nov 11 2005,15:50:43)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
        (compiled Nov 11 2005,15:50:43)
;
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur 2 diffractometer'
_diffrn_measurement_method       'stepwise rotation in omega'
_diffrn_orient_matrix_UB_11      -0.0163819674
_diffrn_orient_matrix_UB_12      -0.0525640725
_diffrn_orient_matrix_UB_13      -0.0158255693
_diffrn_orient_matrix_UB_21      -0.0269966755
_diffrn_orient_matrix_UB_22      0.0297423322
_diffrn_orient_matrix_UB_23      -0.0048238502
_diffrn_orient_matrix_UB_31      -0.0022835361
_diffrn_orient_matrix_UB_32      0.0256050366
_diffrn_orient_matrix_UB_33      -0.0268207175
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            30948
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.98
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.072
_exptl_absorpt_correction_T_max  0.92598
_exptl_absorpt_correction_T_min  0.82984
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)
        (compiled Nov 11 2005,15:50:43)
Analytical numeric absorption correction using a multifaceted crystal
        model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      1.552
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prism
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.08915
_exptl_crystal_size_mid          0.06511
_exptl_crystal_size_min          0.03251
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.083
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         9734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.062
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                5414
_reflns_number_total             9734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100562e_si_002.cif
_cod_data_source_block           379ni4
_cod_database_code               4315802