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_4316957
_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 Palacios Lopez'
_chemical_formula_moiety         'C46 H42 Cl2 N16 Ni4 O6, 4(C H4 O), 2(Cl O4)'
_chemical_formula_sum            'C50 H58 Cl4 N16 Ni4 O18'
_chemical_formula_weight         1547.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.254(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9186(6)
_cell_length_b                   23.8467(10)
_cell_length_c                   14.5107(6)
_cell_measurement_reflns_used    14416
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0070
_cell_measurement_theta_min      2.2081
_cell_volume                     6190.4(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -68.00  -27.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  132.0000  177.0000 41

  2 omega  -22.00   80.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269   77.0000   90.0000 102

  3 omega    2.00   74.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269    0.0000   60.0000 72

  4 omega  -90.00   23.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.0332  -77.0000 -150.0000 113

  5 omega   34.00   70.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269  179.0000    0.0000 36

  6 omega   34.00  102.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       12.1269  179.0000  120.0000 68

;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17843
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.6415
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3176
_exptl_crystal_recrystallization_method 'slow evaporation of MeOH solution'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         17942
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1124P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                13319
_reflns_number_total             17942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101435b_si_001_1.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4316957