Giant Ising-Type Magnetic Anisotropy in Trigonal Bipyramidal Ni(II) Complexes: Experiment and Theory
Renaud Ruamps; Rémi Maurice; Luke Batchelor; Martial Boggio-Pasqua; Régis Guillot; Anne Laure Barra; Junjie Liu; El-Eulmi Bendeif; Sébastien Pillet; Stephen Hill; Talal Mallah; Nathalie Guihéry; Journal of the American Chemical Society 135 (2013) 3017–3026; doi:10.1021/ja308146e

data_4119387
_publ_contact_author_address
;Universit\'e Paris Sud 11, 
UMR CNRS 8182, 
Institut de Chimie Mol\'eculaire et des Mat\'eriaux d'Orsay, 
F-91405 Orsay, 
France.
;
_publ_contact_author_email       talal.mallah@u-psud.fr
_publ_contact_author_name        'Talal Mallah'
_publ_section_title
;
 Giant Ising-Type Magnetic Anisotropy in Trigonal Bipyramidal Ni(II)
 Complexes: Experiment and Theory
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3017
_journal_page_last               3026
_journal_paper_doi               10.1021/ja308146e
_journal_volume                  135
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H30 Cl N4 Ni, Cl O4'
_chemical_formula_sum            'C12 H30 Cl2 N4 Ni O4'
_chemical_formula_weight         423.99
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                120.
_cell_formula_units_Z            6
_cell_length_a                   9.874(5)
_cell_length_b                   9.874(5)
_cell_length_c                   32.962(5)
_cell_measurement_reflns_used    3609
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      36.87
_cell_measurement_theta_min      2.68
_cell_volume                     2783(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            8389
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.93
_diffrn_reflns_theta_min         2.68
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'kappa X8 APEX II Bruker ICMMO'
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.014(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0000P)^2^+0.5446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0609
_reflns_number_gt                1781
_reflns_number_total             2212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308146e_si_002.cif
_cod_data_source_block           1064GuillotICMMO
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4119387