Preparation and characterization of [Gd(hfac)3(DTBN)(H2O)] (DTBN = di-t-butyl nitroxide). Ferromagnetic Gd3±Gd3+ super-superexchange
Takuya Kanetomo; Takayuki Ishida; Chem.Commun. 50 (2014) 2529–; doi:10.1039/c3cc48326f

data_7112026
_publ_section_title
;
 Preparation and characterization of [Gd(hfac)3(DTBN)(H2O)] (DTBN =
 di-t-butyl nitroxide). Ferromagnetic Gd3+-Gd3+ super-superexchange
;
_journal_name_full               Chem.Commun.
_journal_page_first              2529
_journal_paper_doi               10.1039/c3cc48326f
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C23 H23 F18 Gd N O8'
_chemical_formula_sum            'C23 H23 F18 Gd N O8'
_chemical_formula_weight         940.66
_chemical_melting_point          344
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                107.668(8)
_cell_angle_beta                 101.607(8)
_cell_angle_gamma                101.768(8)
_cell_formula_units_Z            4
_cell_length_a                   9.6620(18)
_cell_length_b                   17.014(4)
_cell_length_c                   22.052(5)
_cell_measurement_reflns_used    28930
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     3244.2(13)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 29.412
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1300
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            53099
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832.00
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.058
_refine_diff_density_max         3.300
_refine_diff_density_min         -2.600
_refine_ls_extinction_coef       55(10)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     980
_refine_ls_number_reflns         14595
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0005Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                8692
_reflns_number_total             14598
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3cc48326f.txt
_cod_data_source_block           '[Gd(hfac)3(DTBN)(H2O)]'
_cod_original_cell_volume        3244.1(12)
_cod_database_code               7112026