Experimental Evidence for the Participation of 5d Gd^III^ Orbitals in the Magnetic Interaction in Ni‒Gd Complexes
Costes, Jean-Pierre; Yamaguchi, Tomoka; Kojima, Masaaki; Vendier, Laure; Inorganic Chemistry 48 (2009) 5555–5561; doi:10.1021/ic900142h

data_4302314
_publ_section_title
;
 Experimental Evidence for the Participation of 5d Gd^III^ Orbitals in the
 Magnetic Interaction in Ni--Gd Complexes
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5555
_journal_page_last               5561
_journal_paper_doi               10.1021/ic900142h
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H60 Gd N6 Ni2 O12, N O3'
_chemical_formula_sum            'C58 H60 Gd N7 Ni2 O15'
_chemical_formula_weight         1369.76
_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
_cell_angle_alpha                90
_cell_angle_beta                 110.961(15)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   47.138(6)
_cell_length_b                   24.506(3)
_cell_length_c                   17.806(3)
_cell_measurement_reflns_used    1887
_cell_measurement_temperature    180
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5303
_cell_measurement_wavelength     0.71073
_cell_volume                     19208(5)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_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    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1602
_diffrn_reflns_av_unetI/netI     0.2709
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            70222
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.672
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8364
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.784
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         19602
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.1775
_refine_ls_R_factor_gt           0.066
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                6724
_reflns_number_total             19602
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4338580
_cod_data_source_file            ic900142h_si_001_1.cif
_cod_data_source_block           complex2
_cod_database_code               4302314