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_4302315
_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
'C42 H54 Gd N4 Ni2 O11, 3(C F3 O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C47 H58 Cl4 F9 Gd N4 Ni2 O20 S3'
_chemical_formula_weight         1682.62
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.645(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8541(3)
_cell_length_b                   16.2088(3)
_cell_length_c                   24.2499(5)
_cell_measurement_reflns_used    22224
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1098
_cell_measurement_theta_min      2.5059
_cell_measurement_wavelength     0.71073
_cell_volume                     6409.5(2)
_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_orient_matrix_UB_11      -0.0208749493
_diffrn_orient_matrix_UB_12      -0.013613937
_diffrn_orient_matrix_UB_13      0.0203385142
_diffrn_orient_matrix_UB_21      0.0374737076
_diffrn_orient_matrix_UB_22      0.0003425005
_diffrn_orient_matrix_UB_23      0.0214057994
_diffrn_orient_matrix_UB_31      -0.0071516152
_diffrn_orient_matrix_UB_32      0.0415779555
_diffrn_orient_matrix_UB_33      0.0064632069
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_limit_h_max       21
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49443
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
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_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3380
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         13089
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                9010
_reflns_number_total             13089
_reflns_threshold_expression     >2\s(I)
_cod_duplicate_entry             4338579
_cod_data_source_file            ic900142h_si_001_2.cif
_cod_data_source_block           complex1
_cod_database_code               4302315