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_4316958
_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 Lopez'
_chemical_formula_moiety         'C46 H44 N22 Ni4 O6, 2(Cl O4), 2(MeOH)'
_chemical_formula_sum            'C48 H52 Cl2 N22 Ni4 O16'
_chemical_formula_weight         1498.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   13.9395(2)
_cell_length_b                   24.2919(3)
_cell_length_c                   33.8474(4)
_cell_measurement_reflns_used    50885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0536
_cell_measurement_theta_min      2.0660
_cell_volume                     11461.3(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            108383
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.478
_exptl_absorpt_correction_T_max  0.91000
_exptl_absorpt_correction_T_min  0.76686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6144
_exptl_crystal_size_max          0.2868
_exptl_crystal_size_mid          0.1942
_exptl_crystal_size_min          0.0669
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         14565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                11320
_reflns_number_total             14565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101435b_si_001_2.cif
_cod_data_source_block           compound2
_cod_database_code               4316958