Antiferromagnetic versus Ferromagnetic Exchange Interactions in Bis(μ-Ooximate)dinickel(II) Units for a Series of Closely Related Cube Shaped Carboxamideoximate-Bridged Ni4 Complexes. A Combined Experimental and Theoretical Magneto-Structural Study
M. A. Palacios; Antonio J. Mota; Jesús E. Perea-Buceta; Fraser J. White; Euan K. Brechin; Enrique Colacio; Inorganic Chemistry 49 (2010) 10156–10165; doi:10.1021/ic101435b

data_4316959
_publ_contact_author_email       fraser.white@ed.ac.uk
_publ_contact_author_name        'Fraser J. White'
_publ_section_title
;
 Antiferromagnetic versus Ferromagnetic Exchange Interactions in
 Bis(\m-Ooximate)dinickel(II) Units for a Series of Closely Related Cube
 Shaped Carboxamideoximate-Bridged Ni4 Complexes. A Combined Experimental
 and Theoretical Magneto-Structural Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10156
_journal_page_last               10165
_journal_paper_doi               10.1021/ic101435b
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'Maria Angeles Palacios Lopez'
_chemical_formula_moiety         'C44 H46 N20 Ni4 O10, 2(Cl O4), 4(C H4 O)'
_chemical_formula_sum            'C48 H62 Cl2 N20 Ni4 O22'
_chemical_formula_weight         1576.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.1300(4)
_cell_length_b                   25.3252(5)
_cell_length_c                   14.4407(5)
_cell_measurement_reflns_used    12844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.9455
_cell_measurement_theta_min      2.4349
_cell_volume                     6630.4(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
;
_computing_molecular_graphics    Shelxp
_computing_publication_material  'Platon, encifer'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxs Sheldrick'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   -6.00   31.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       -1.2622  -89.0000 -111.0000 37

  2 omega  -88.00  -55.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        1.2622  179.0000 -150.0000 33

  3 omega  -82.00  -36.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        1.2622  179.0000   60.0000 46

  4 omega   57.00  150.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       84.3951   45.0000 -150.0000 93

  5 omega   99.00  157.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       84.3951  125.0000 -150.0000 58

  6 omega   30.00  145.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       84.3951  -15.0000 -180.0000 115

  7 omega  -25.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        1.2622   37.0000    0.0000 102

  8 omega  -31.00   78.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        1.2622   72.0000   81.0000 109

  9 omega   51.00  163.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       84.3951   77.0000  -30.0000 112

 10 omega   51.00  142.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       84.3951   77.0000  -90.0000 91

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            25745
_diffrn_reflns_theta_full        62.03
_diffrn_reflns_theta_max         62.03
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.777
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
(compiled Dec  8 2009,17:31:18)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'brown block'
_exptl_crystal_F_000             3248
_exptl_crystal_recrystallization_method 'slow evaporation of MeOH solution'
_exptl_crystal_size_max          0.2062
_exptl_crystal_size_mid          0.1266
_exptl_crystal_size_min          0.1212
_platon_squeeze_details
;
;
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5194
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+1.9406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                4252
_reflns_number_total             5194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101435b_si_001_3.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P n c a'
_cod_database_code               4316959